# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_gd_bcpm
_database_code_depnum_ccdc_archive 'CCDC 2338720'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H18 Gd3 N O19'
_chemical_formula_sum            'C30 H18 Gd3 N O19'
_chemical_formula_weight         1168.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   30.1356(7)
_cell_length_b                   18.2215(7)
_cell_length_c                   14.6429(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.531(2)
_cell_angle_gamma                90
_cell_volume                     7905.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12327
_cell_measurement_temperature    145.15
_cell_measurement_theta_max      73.4530
_cell_measurement_theta_min      2.8250
_shelx_estimated_absorpt_T_max   0.735
_shelx_estimated_absorpt_T_min   0.179
_exptl_absorpt_coefficient_mu    16.377
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    0.982
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.994
_diffrn_reflns_theta_max         66.994
_diffrn_reflns_theta_min         2.847
_diffrn_ambient_temperature      145.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -21.00   0.50    2.00    --  -42.57 -40.00  66.00  186
  2  ω     21.00  66.00   0.50    2.00    --   42.57  40.00-140.00   90
  3  ω     68.00 120.00   0.50    2.00    --   42.57  40.00-140.00  104
  4  ω    -34.00  46.00   0.50    2.00    --   42.57 -40.00  66.00  160
  5  ω   -177.00 -83.00   0.50   15.00    -- -106.00 -40.00  66.00  188
  6  ω     84.00 173.00   0.50   15.00    --  107.12  40.00-140.00  178
  7  ω    -93.00 -13.00   0.50    2.00    --  -42.57 126.00 -60.00  160
  8  ω    -45.00  34.00   0.50    2.00    --  -42.57  40.00-140.00  158
  9  ω     13.00  84.00   0.50    2.00    --   42.57-126.00   0.00  142
 10  ω    -26.00   4.00   0.50    2.00    --   42.57 -77.00-150.00   60
 11  ω     37.00  66.00   0.50    2.00    --   42.57 -77.00-150.00   58
 12  ω     -3.00  23.00   0.50    2.00    --   42.57 -19.00  90.00   52
 13  ω   -112.00 -34.00   0.50   15.00    -- -106.00 126.00-120.00  156
 14  ω   -170.00 -83.00   0.50   15.00    -- -106.00 -30.00 -60.00  174
 15  ω    -69.00 -43.00   0.50   15.00    -- -106.00  61.00  90.00   52
 16  ω    -93.00 -66.00   0.50   15.00    -- -106.00 152.00-114.93   54
 17  ω    -65.00 -33.00   0.50   15.00    -- -106.00  61.00 -60.00   64
 18  ω   -173.00-128.00   0.50   15.00    -- -106.00   0.00 -90.00   90
 19  ω   -115.00 -29.00   0.50   15.00    -- -106.00   0.00 -90.00  172
 20  ω    -67.00 -33.00   0.50   15.00    -- -106.00  61.00 150.00   68
 21  ω   -130.00 -99.00   0.50   15.00    -- -106.00 152.00-114.93   62
 22  ω    -99.00 -64.00   0.50   15.00    -- -106.00  77.00 -90.00   70
 23  ω   -176.00 -84.00   0.50   15.00    -- -106.00 -45.00 150.00  184
 24  ω    -99.00 -49.00   0.50   15.00    -- -106.00  77.00  30.00  100
 25  ω   -125.00 -85.00   0.50   15.00    -- -106.00 144.00  65.63   80
 26  ω   -145.00 -83.00   0.50   15.00    -- -106.00 -95.00  30.00  124
 27  ω    -66.00 -32.00   0.50   15.00    -- -106.00  61.00  60.00   68
 28  ω    -71.00 -33.00   0.50   15.00    -- -106.00  61.00 -90.00   76
 29  ω     34.00  73.00   0.50   15.00    --  107.12 -95.00  30.00   78
 30  ω     68.00 106.00   0.50   15.00    --  107.12 -95.00-180.00   76
 31  ω     43.00 104.00   0.50   15.00    --  107.12 -95.00 150.00  122
 32  ω     37.00  96.00   0.50   15.00    --  107.12 -95.00  60.00  118
 33  ω     35.00  82.00   0.50   15.00    --  107.12 -95.00 120.00   94
 34  ω     82.00 110.00   0.50   15.00    --  107.12-126.00   0.00   56
 35  ω     44.00  71.00   0.50   15.00    --  107.12-126.00   0.00   54
 36  ω     35.00  77.00   0.50   15.00    --  107.12-126.00-150.00   84
 37  ω     76.00 101.00   0.50   15.00    --  107.12 -95.00  30.00   50
 38  ω     36.00  66.00   0.50   15.00    --  107.12 -61.00-150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4953
_reflns_number_total             7281
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.586
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         7281
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0668
_refine_ls_restrained_S_all      0.962
_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)+(0.1538P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2059
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O6-N1
 1.35 with sigma of 0.001
 N1-O7
 1.35 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O6 \\sim O7 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O6, O7, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C10(H10), C4(H4), C3(H3), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_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
Gd1 Gd 0.51661(2) 0.39178(3) 0.13713(3) 0.0837(2) Uani 1 1 d . . . . .
Gd2 Gd 0.59108(2) 0.500000 -0.01367(4) 0.0881(2) Uani 1 2 d S T P . .
O8 O 0.55660(17) 0.500000 0.1171(4) 0.0650(14) Uani 1 2 d S T P . .
O11 O 0.5117(3) 0.2680(4) 0.0849(8) 0.168(3) Uani 1 1 d . . . . .
O6 O 0.53434(19) 0.4372(3) 0.2907(3) 0.1082(18) Uani 1 1 d D U . . .
O1 O 0.5939(2) 0.6440(4) 0.1797(4) 0.121(2) Uani 1 1 d . . . . .
O9 O 0.54117(14) 0.4005(3) -0.0062(3) 0.0723(11) Uani 1 1 d . . . . .
O2 O 0.6344(2) 0.5809(5) 0.0900(4) 0.121(2) Uani 1 1 d . . . . .
O10 O 0.47333(18) 0.500000 0.1289(4) 0.0697(15) Uani 1 2 d S T P . .
O3 O 0.8171(4) 0.6569(13) 0.4488(8) 0.328(12) Uani 1 1 d . . . . .
O7 O 0.5534(5) 0.500000 0.4381(8) 0.219(7) Uani 1 2 d DS TU P . .
O4 O 0.8914(2) 0.9167(5) 0.1243(5) 0.117(2) Uani 1 1 d . . . . .
O5 O 0.9525(2) 0.8521(4) 0.1959(4) 0.1112(19) Uani 1 1 d . . . . .
N1 N 0.5411(4) 0.500000 0.3402(7) 0.131(4) Uani 1 2 d DS TU P . .
C13 C 0.6710(5) 0.7015(12) 0.2849(8) 0.209(9) Uani 1 1 d . . . . .
H13 H 0.643315 0.724170 0.291060 0.250 Uiso 1 1 calc R U . . .
C12 C 0.7138(4) 0.6145(8) 0.2096(8) 0.149(5) Uani 1 1 d . . . . .
H12 H 0.714623 0.578210 0.163406 0.179 Uiso 1 1 calc R U . . .
C1 C 0.9114(5) 0.8691(8) 0.1796(7) 0.126(4) Uani 1 1 d . . . . .
C11 C 0.7132(5) 0.7218(12) 0.3407(7) 0.205(9) Uani 1 1 d . . . . .
H11 H 0.713607 0.759439 0.385804 0.246 Uiso 1 1 calc R U . . .
C10 C 0.7541(4) 0.6362(10) 0.2664(8) 0.168(6) Uani 1 1 d . . . . .
H10 H 0.781932 0.614373 0.259834 0.201 Uiso 1 1 calc R U . . .
C4 C 0.8405(3) 0.8519(9) 0.2403(8) 0.147(5) Uani 1 1 d . . . . .
H4 H 0.829120 0.895425 0.208787 0.177 Uiso 1 1 calc R U . . .
C3 C 0.8966(5) 0.7602(8) 0.2822(8) 0.143(4) Uani 1 1 d . . . . .
H3 H 0.925969 0.742146 0.280095 0.172 Uiso 1 1 calc R U . . .
C7 C 0.8294(5) 0.7479(12) 0.3398(7) 0.172(7) Uani 1 1 d . . . . .
C8 C 0.7964(5) 0.7139(15) 0.3972(9) 0.269(14) Uani 1 1 d . . . . .
H8 H 0.788388 0.752138 0.440495 0.323 Uiso 1 1 calc R U . . .
C5 C 0.8692(5) 0.7222(9) 0.3300(9) 0.159(5) Uani 1 1 d . . . . .
H5 H 0.878955 0.676137 0.356777 0.191 Uiso 1 1 calc R U . . .
C2 C 0.8815(3) 0.8266(8) 0.2354(6) 0.121(4) Uani 1 1 d . . . . .
C9 C 0.7526(4) 0.6894(10) 0.3315(7) 0.164(7) Uani 1 1 d . . . . .
C14 C 0.6736(3) 0.6442(8) 0.2190(6) 0.125(4) Uani 1 1 d . . . . .
C6 C 0.8137(4) 0.8105(11) 0.2955(10) 0.187(8) Uani 1 1 d . . . . .
H6 H 0.784507 0.827811 0.300640 0.224 Uiso 1 1 calc R U . . .
C15 C 0.6311(3) 0.6197(7) 0.1582(7) 0.116(3) 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
Gd1 Gd1 3.9439(10) 6_565 ?
Gd1 Gd1 3.9573(8) 2_655 ?
Gd1 Gd2 3.9426(6) 5_665 ?
Gd1 Gd2 3.9512(7) . ?
Gd1 O8 2.357(3) . ?
Gd1 O11 2.378(8) . ?
Gd1 O6 2.364(5) . ?
Gd1 O1 2.388(6) 6_565 ?
Gd1 O9 2.355(4) . ?
Gd1 O9 2.348(4) 2_655 ?
Gd1 O10 2.355(3) . ?
Gd1 O5 2.368(6) 3_445 ?
Gd2 O8 2.340(5) . ?
Gd2 O9 2.371(5) 6_565 ?
Gd2 O9 2.371(5) . ?
Gd2 O2 2.337(7) 6_565 ?
Gd2 O2 2.337(7) . ?
Gd2 O10 2.328(5) 5_665 ?
Gd2 O4 2.350(7) 7_665 ?
Gd2 O4 2.350(7) 4_645 ?
O6 N1 1.3496(10) . ?
O1 C15 1.298(13) . ?
O2 C15 1.242(13) . ?
O3 C8 1.37(3) . ?
O7 N1 1.413(9) . ?
O4 C1 1.262(15) . ?
O5 C1 1.254(15) . ?
C13 H13 0.9500 . ?
C13 C11 1.428(17) . ?
C13 C14 1.43(2) . ?
C12 H12 0.9500 . ?
C12 C10 1.396(14) . ?
C12 C14 1.356(17) . ?
C1 C2 1.532(14) . ?
C11 H11 0.9500 . ?
C11 C9 1.36(2) . ?
C10 H10 0.9500 . ?
C10 C9 1.37(2) . ?
C4 H4 0.9500 . ?
C4 C2 1.335(16) . ?
C4 C6 1.453(18) . ?
C3 H3 0.9500 . ?
C3 C5 1.365(15) . ?
C3 C2 1.424(18) . ?
C7 C8 1.544(16) . ?
C7 C5 1.32(2) . ?
C7 C6 1.35(2) . ?
C8 H8 1.0000 . ?
C8 C9 1.549(14) . ?
C5 H5 0.9500 . ?
C14 C15 1.489(13) . ?
C6 H6 0.9500 . ?

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
Gd1 Gd1 Gd1 90.0 6_565 2_655 ?
Gd1 Gd1 Gd2 60.062(8) 6_565 . ?
Gd2 Gd1 Gd1 59.989(8) 5_665 6_565 ?
Gd2 Gd1 Gd1 60.022(12) 5_665 2_655 ?
Gd2 Gd1 Gd1 59.805(12) . 2_655 ?
Gd2 Gd1 Gd2 89.893(15) 5_665 . ?
O8 Gd1 Gd1 33.22(11) . 6_565 ?
O8 Gd1 Gd1 85.07(13) . 2_655 ?
O8 Gd1 Gd2 85.49(11) . 5_665 ?
O8 Gd1 Gd2 32.59(12) . . ?
O8 Gd1 O11 139.2(3) . . ?
O8 Gd1 O6 78.09(19) . . ?
O8 Gd1 O1 76.4(2) . 6_565 ?
O8 Gd1 O5 140.4(2) . 3_445 ?
O11 Gd1 Gd1 161.6(3) . 6_565 ?
O11 Gd1 Gd1 71.6(3) . 2_655 ?
O11 Gd1 Gd2 107.6(2) . . ?
O11 Gd1 Gd2 109.2(3) . 5_665 ?
O11 Gd1 O1 80.0(3) . 6_565 ?
O6 Gd1 Gd1 69.51(14) . 6_565 ?
O6 Gd1 Gd1 159.50(14) . 2_655 ?
O6 Gd1 Gd2 106.57(14) . 5_665 ?
O6 Gd1 Gd2 107.71(14) . . ?
O6 Gd1 O11 128.9(3) . . ?
O6 Gd1 O1 78.9(2) . 6_565 ?
O6 Gd1 O5 79.6(2) . 3_445 ?
O1 Gd1 Gd1 108.58(16) 6_565 2_655 ?
O1 Gd1 Gd1 105.8(2) 6_565 6_565 ?
O1 Gd1 Gd2 69.87(18) 6_565 . ?
O1 Gd1 Gd2 159.67(19) 6_565 5_665 ?
O9 Gd1 Gd1 86.13(11) 2_655 6_565 ?
O9 Gd1 Gd1 86.14(11) . 6_565 ?
O9 Gd1 Gd1 32.64(10) . 2_655 ?
O9 Gd1 Gd1 32.76(10) 2_655 2_655 ?
O9 Gd1 Gd2 85.65(10) . 5_665 ?
O9 Gd1 Gd2 85.53(11) 2_655 . ?
O9 Gd1 Gd2 33.52(11) 2_655 5_665 ?
O9 Gd1 Gd2 33.41(11) . . ?
O9 Gd1 O8 65.28(17) . . ?
O9 Gd1 O8 99.31(17) 2_655 . ?
O9 Gd1 O11 77.8(3) . . ?
O9 Gd1 O11 78.9(3) 2_655 . ?
O9 Gd1 O6 139.30(18) 2_655 . ?
O9 Gd1 O6 140.45(18) . . ?
O9 Gd1 O1 140.68(19) 2_655 6_565 ?
O9 Gd1 O1 78.51(19) . 6_565 ?
O9 Gd1 O9 64.83(17) 2_655 . ?
O9 Gd1 O10 65.21(17) 2_655 . ?
O9 Gd1 O10 99.17(17) . . ?
O9 Gd1 O5 138.99(18) . 3_445 ?
O9 Gd1 O5 77.55(18) 2_655 3_445 ?
O10 Gd1 Gd1 85.02(13) . 2_655 ?
O10 Gd1 Gd1 33.14(11) . 6_565 ?
O10 Gd1 Gd2 32.44(12) . 5_665 ?
O10 Gd1 Gd2 85.38(12) . . ?
O10 Gd1 O8 65.43(16) . . ?
O10 Gd1 O11 140.9(3) . . ?
O10 Gd1 O6 77.42(19) . . ?
O10 Gd1 O1 138.3(2) . 6_565 ?
O10 Gd1 O5 78.1(2) . 3_445 ?
O5 Gd1 Gd1 107.79(19) 3_445 6_565 ?
O5 Gd1 Gd1 107.25(15) 3_445 2_655 ?
O5 Gd1 Gd2 70.19(18) 3_445 5_665 ?
O5 Gd1 Gd2 160.08(18) 3_445 . ?
O5 Gd1 O11 79.6(3) 3_445 . ?
O5 Gd1 O1 130.0(3) 3_445 6_565 ?
Gd1 Gd2 Gd1 90.108(15) 2_655 6_565 ?
Gd1 Gd2 Gd1 60.174(13) 5_665 6_565 ?
Gd1 Gd2 Gd1 90.108(14) 5_665 . ?
Gd1 Gd2 Gd1 60.023(16) 2_655 5_665 ?
Gd1 Gd2 Gd1 60.175(13) 2_655 . ?
Gd1 Gd2 Gd1 59.878(16) . 6_565 ?
O8 Gd2 Gd1 32.87(5) . 6_565 ?
O8 Gd2 Gd1 85.64(11) . 5_665 ?
O8 Gd2 Gd1 85.64(11) . 2_655 ?
O8 Gd2 Gd1 32.87(5) . . ?
O8 Gd2 O9 65.29(12) . 6_565 ?
O8 Gd2 O9 65.29(12) . . ?
O8 Gd2 O4 138.9(2) . 7_665 ?
O8 Gd2 O4 138.9(2) . 4_645 ?
O9 Gd2 Gd1 85.76(11) 6_565 . ?
O9 Gd2 Gd1 33.15(10) . 2_655 ?
O9 Gd2 Gd1 33.15(10) . . ?
O9 Gd2 Gd1 85.86(10) 6_565 2_655 ?
O9 Gd2 Gd1 33.15(10) 6_565 5_665 ?
O9 Gd2 Gd1 33.15(10) 6_565 6_565 ?
O9 Gd2 Gd1 85.86(10) . 5_665 ?
O9 Gd2 Gd1 85.76(11) . 6_565 ?
O9 Gd2 O9 99.8(2) 6_565 . ?
O2 Gd2 Gd1 105.03(16) . . ?
O2 Gd2 Gd1 107.3(2) . 5_665 ?
O2 Gd2 Gd1 107.3(2) 6_565 2_655 ?
O2 Gd2 Gd1 105.03(16) 6_565 6_565 ?
O2 Gd2 Gd1 158.31(17) 6_565 5_665 ?
O2 Gd2 Gd1 158.31(17) . 2_655 ?
O2 Gd2 Gd1 68.25(17) 6_565 . ?
O2 Gd2 Gd1 68.25(17) . 6_565 ?
O2 Gd2 O8 75.39(18) 6_565 . ?
O2 Gd2 O8 75.38(18) . . ?
O2 Gd2 O9 76.8(2) . 6_565 ?
O2 Gd2 O9 137.5(2) 6_565 6_565 ?
O2 Gd2 O9 137.5(2) . . ?
O2 Gd2 O9 76.8(2) 6_565 . ?
O2 Gd2 O2 78.3(4) . 6_565 ?
O2 Gd2 O4 133.3(3) . 4_645 ?
O2 Gd2 O4 133.3(3) 6_565 7_665 ?
O2 Gd2 O4 82.6(2) 6_565 4_645 ?
O2 Gd2 O4 82.6(2) . 7_665 ?
O10 Gd2 Gd1 32.87(5) 5_665 2_655 ?
O10 Gd2 Gd1 32.87(5) 5_665 5_665 ?
O10 Gd2 Gd1 85.51(11) 5_665 6_565 ?
O10 Gd2 Gd1 85.51(12) 5_665 . ?
O10 Gd2 O8 99.05(18) 5_665 . ?
O10 Gd2 O9 65.26(12) 5_665 . ?
O10 Gd2 O9 65.26(12) 5_665 6_565 ?
O10 Gd2 O2 139.8(2) 5_665 . ?
O10 Gd2 O2 139.8(2) 5_665 6_565 ?
O10 Gd2 O4 76.29(19) 5_665 4_645 ?
O10 Gd2 O4 76.29(19) 5_665 7_665 ?
O4 Gd2 Gd1 68.32(18) 4_645 2_655 ?
O4 Gd2 Gd1 106.6(2) 4_645 . ?
O4 Gd2 Gd1 106.6(2) 7_665 6_565 ?
O4 Gd2 Gd1 106.08(17) 4_645 5_665 ?
O4 Gd2 Gd1 158.43(18) 7_665 . ?
O4 Gd2 Gd1 106.08(17) 7_665 2_655 ?
O4 Gd2 Gd1 158.43(18) 4_645 6_565 ?
O4 Gd2 Gd1 68.32(18) 7_665 5_665 ?
O4 Gd2 O9 138.6(2) 7_665 . ?
O4 Gd2 O9 76.2(2) 4_645 . ?
O4 Gd2 O9 138.6(2) 4_645 6_565 ?
O4 Gd2 O9 76.2(2) 7_665 6_565 ?
O4 Gd2 O4 80.5(4) 4_645 7_665 ?
Gd1 O8 Gd1 113.6(2) . 6_565 ?
Gd2 O8 Gd1 114.54(14) . 6_565 ?
Gd2 O8 Gd1 114.54(14) . . ?
N1 O6 Gd1 142.5(6) . . ?
C15 O1 Gd1 133.5(7) . 6_565 ?
Gd1 O9 Gd1 114.60(17) 2_655 . ?
Gd1 O9 Gd2 113.33(18) 2_655 . ?
Gd1 O9 Gd2 113.45(18) . . ?
C15 O2 Gd2 139.7(6) . . ?
Gd1 O10 Gd1 113.7(2) . 6_565 ?
Gd2 O10 Gd1 114.69(14) 5_665 . ?
Gd2 O10 Gd1 114.69(14) 5_665 6_565 ?
C1 O4 Gd2 138.1(7) . 7_665 ?
C1 O5 Gd1 134.2(7) . 3 ?
O6 N1 O6 116.0(9) 6_565 . ?
O6 N1 O7 122.0(5) . . ?
O6 N1 O7 122.0(5) 6_565 . ?
C11 C13 H13 122.6 . . ?
C11 C13 C14 114.9(17) . . ?
C14 C13 H13 122.6 . . ?
C10 C12 H12 119.3 . . ?
C14 C12 H12 119.3 . . ?
C14 C12 C10 121.4(14) . . ?
O4 C1 C2 115.4(11) . . ?
O5 C1 O4 129.2(10) . . ?
O5 C1 C2 115.4(12) . . ?
C13 C11 H11 118.8 . . ?
C9 C11 C13 122.3(16) . . ?
C9 C11 H11 118.8 . . ?
C12 C10 H10 120.6 . . ?
C9 C10 C12 118.8(15) . . ?
C9 C10 H10 120.6 . . ?
C2 C4 H4 121.1 . . ?
C2 C4 C6 117.8(15) . . ?
C6 C4 H4 121.1 . . ?
C5 C3 H3 119.7 . . ?
C5 C3 C2 120.6(13) . . ?
C2 C3 H3 119.7 . . ?
C5 C7 C8 127.2(19) . . ?
C5 C7 C6 119.4(13) . . ?
C6 C7 C8 113.3(17) . . ?
O3 C8 C7 109.3(17) . . ?
O3 C8 H8 108.6 . . ?
O3 C8 C9 112.0(17) . . ?
C7 C8 H8 108.6 . . ?
C7 C8 C9 109.7(9) . . ?
C9 C8 H8 108.6 . . ?
C3 C5 H5 119.2 . . ?
C7 C5 C3 121.5(17) . . ?
C7 C5 H5 119.2 . . ?
C4 C2 C1 119.8(13) . . ?
C4 C2 C3 119.0(10) . . ?
C3 C2 C1 121.3(11) . . ?
C11 C9 C10 121.3(10) . . ?
C11 C9 C8 118.3(16) . . ?
C10 C9 C8 120.4(16) . . ?
C13 C14 C15 118.2(12) . . ?
C12 C14 C13 121.3(11) . . ?
C12 C14 C15 120.5(12) . . ?
C4 C6 H6 119.2 . . ?
C7 C6 C4 121.5(15) . . ?
C7 C6 H6 119.2 . . ?
O1 C15 C14 116.2(10) . . ?
O2 C15 O1 126.1(9) . . ?
O2 C15 C14 117.6(10) . . ?

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 O6 N1 O6 3.9(19) . . . 6_565 ?
Gd1 O6 N1 O7 -177.6(8) . . . . ?
Gd1 O1 C15 O2 19.3(17) 6_565 . . . ?
Gd1 O1 C15 C14 -164.1(7) 6_565 . . . ?
Gd1 O5 C1 O4 -1.5(18) 3 . . . ?
Gd1 O5 C1 C2 179.2(6) 3 . . . ?
Gd2 O2 C15 O1 -22(2) . . . . ?
Gd2 O2 C15 C14 161.1(8) . . . . ?
Gd2 O4 C1 O5 3.2(19) 7_665 . . . ?
Gd2 O4 C1 C2 -177.5(7) 7_665 . . . ?
O3 C8 C9 C11 121(2) . . . . ?
O3 C8 C9 C10 -58.9(18) . . . . ?
O4 C1 C2 C4 -15.5(15) . . . . ?
O4 C1 C2 C3 164.2(10) . . . . ?
O5 C1 C2 C4 163.9(10) . . . . ?
O5 C1 C2 C3 -16.4(15) . . . . ?
C13 C11 C9 C10 1(2) . . . . ?
C13 C11 C9 C8 -178.3(14) . . . . ?
C13 C14 C15 O1 -10.5(16) . . . . ?
C13 C14 C15 O2 166.3(11) . . . . ?
C12 C10 C9 C11 -1(2) . . . . ?
C12 C10 C9 C8 178.8(12) . . . . ?
C12 C14 C15 O1 171.5(10) . . . . ?
C12 C14 C15 O2 -11.6(17) . . . . ?
C11 C13 C14 C12 -2(2) . . . . ?
C11 C13 C14 C15 179.9(11) . . . . ?
C10 C12 C14 C13 3(2) . . . . ?
C10 C12 C14 C15 -179.4(11) . . . . ?
C7 C8 C9 C11 -117.4(19) . . . . ?
C7 C8 C9 C10 63(2) . . . . ?
C8 C7 C5 C3 -175.5(13) . . . . ?
C8 C7 C6 C4 178.1(13) . . . . ?
C5 C3 C2 C1 -178.6(11) . . . . ?
C5 C3 C2 C4 1.1(18) . . . . ?
C5 C7 C8 O3 9(2) . . . . ?
C5 C7 C8 C9 -114.7(19) . . . . ?
C5 C7 C6 C4 -3(2) . . . . ?
C2 C4 C6 C7 -1(2) . . . . ?
C2 C3 C5 C7 -5(2) . . . . ?
C14 C13 C11 C9 0(2) . . . . ?
C14 C12 C10 C9 -1(2) . . . . ?
C6 C4 C2 C1 -178.8(11) . . . . ?
C6 C4 C2 C3 1.4(18) . . . . ?
C6 C7 C8 O3 -172.2(16) . . . . ?
C6 C7 C8 C9 65(2) . . . . ?
C6 C7 C5 C3 5(2) . . . . ?

_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 -0.988 -0.960 -0.281 5212.9 1294.8 ?


_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
;
####################################################################### 
# 
# 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_lk1_44_7
_database_code_depnum_ccdc_archive 'CCDC 2338724'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H18 Er3 N O19'
_chemical_formula_sum            'C30 H18 Er3 N O19'
_chemical_formula_weight         1198.23
_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'
Er Er -9.4367 3.9380 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   29.7195(6)
_cell_length_b                   18.1534(5)
_cell_length_c                   14.5912(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.482(2)
_cell_angle_gamma                90
_cell_volume                     7714.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12210
_cell_measurement_temperature    103.7(6)
_cell_measurement_theta_max      70.9810
_cell_measurement_theta_min      4.8800
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.479
_exptl_absorpt_coefficient_mu    6.158
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.032
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24940
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.998
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         3.877
_diffrn_ambient_temperature      103.85
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  48.00   1.00    2.50    --    0.00 -99.00  90.00   41
  2  ω    -85.00 -28.00   1.00    2.50    --    0.00 -57.00   0.00   57
  3  ω      2.00  30.00   1.00    2.50    --    0.00 -99.00-120.00   28
  4  ω    -13.00  26.00   1.00    2.50    --    0.00 -57.00   0.00   39
  5  ω   -127.00 -87.00   1.00    5.00    --  -54.44 -57.00 -90.00   40
  6  ω   -141.00 -85.00   1.00    5.00    --  -54.44 -99.00 -90.00   56
  7  ω   -146.00 -79.00   1.00    5.00    --  -54.44 -99.00   0.00   67
  8  ω   -136.00 -79.00   1.00    5.00    --  -54.44 -99.00  60.00   57
  9  ω   -126.00 -79.00   1.00    5.00    --  -54.44 -99.00-150.00   47
 10  ω    -64.00 -18.00   1.00    5.00    --  -54.44 125.00  30.00   46
 11  ω    -92.00  34.00   1.00    5.00    --  -54.44  77.00 -90.00  126
 12  ω     24.00 117.00   1.00    5.00    --   54.44-125.00  30.00   93
 13  ω    102.00 131.00   1.00   12.50    --  108.88 -77.00-150.00   29
 14  ω     24.00  81.00   1.00   12.50    --  108.88 -77.00-150.00   57
 15  ω    116.00 145.00   1.00   12.50    --  108.88 111.00  60.00   29
 16  ω    103.00 163.00   1.00   12.50    --  108.88 111.00-150.00   60
 17  ω     30.00 107.00   1.00   12.50    --  108.88-111.00 150.00   77
 18  ω    101.00 141.00   1.00   12.50    --  108.88 111.00-180.00   40
 19  ω     74.00 156.00   1.00   12.50    --  108.88  38.00 -90.00   82
 20  ω     44.00 112.00   1.00   12.50    --  108.88-111.00 -60.00   68
 21  ω    100.00 157.00   1.00   12.50    --  108.88 111.00 -90.00   57
 22  ω     22.00 106.00   1.00   12.50    --  108.88 -92.00-180.00   84
 23  ω     45.00 112.00   1.00   12.50    --  108.88-111.00  90.00   67
 24  ω     69.00 156.00   1.00   12.50    --  108.88  64.00   0.00   87
 25  ω     84.00 145.00   1.00   12.50    --  108.88 178.00 120.00   61
 26  ω     73.00 171.00   1.00   12.50    --  108.88  50.00 -30.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6313
_reflns_number_total             7115
_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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         7115
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0436
_refine_ls_restrained_S_all      1.121
_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)+(0.0937P)²+5.0626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1437
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-O7
 1.35 with sigma of 0.001
3. Rigid bond restraints
 O6, O7, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 C8(H8)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C14(H14), C3(H3), C6(H6), C10(H10), C4(H4), C11(H11)
;
_atom_sites_solution_hydrogens   geom
_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
Er2 Er 0.41008(2) 1.000000 1.01276(2) 0.06917(14) Uani 1 2 d S T P . .
Er1 Er 0.48271(2) 0.89409(2) 0.86485(2) 0.06668(12) Uani 1 1 d . . . . .
O5 O 0.54594(11) 0.8548(2) 0.8086(2) 0.0854(9) Uani 1 1 d . . . . .
O1 O 0.40671(11) 0.8588(2) 0.8237(2) 0.0862(9) Uani 1 1 d . . . . .
O3 O 0.1798(2) 0.8353(5) 0.5477(4) 0.204(4) Uani 1 1 d . . . . .
O8 O 0.44305(11) 1.000000 0.8829(2) 0.0554(8) Uani 1 2 d S T P . .
O4 O 0.39197(11) 1.0812(2) 1.1201(2) 0.0846(9) Uani 1 1 d . . . . .
O11 O 0.48808(18) 0.7732(3) 0.9129(5) 0.1376(18) Uani 1 1 d . . . . .
O6 O 0.46460(11) 0.9359(2) 0.7139(2) 0.0858(9) Uani 1 1 d . U . . .
O10 O 0.54111(9) 0.90130(15) 0.99444(17) 0.0582(6) Uani 1 1 d . . . . .
O7 O 0.4471(3) 1.000000 0.5742(4) 0.176(4) Uani 1 2 d DS TU P . .
O9 O 0.52541(11) 1.000000 0.8714(2) 0.0542(8) Uani 1 2 d S T P . .
O2 O 0.36513(11) 0.9205(2) 0.9112(2) 0.0847(9) Uani 1 1 d . . . . .
N1 N 0.4598(3) 1.000000 0.6684(4) 0.111(2) Uani 1 2 d DS TU P . .
C2 C 0.32558(16) 0.8546(3) 0.7812(3) 0.0821(13) Uani 1 1 d . . . . .
C13 C 0.34035(19) 1.1441(5) 1.2387(4) 0.108(2) Uani 1 1 d . . . . .
H13 H 0.328767 1.101148 1.204719 0.130 Uiso 1 1 calc R U . . .
C1 C 0.36966(16) 0.8806(3) 0.8439(3) 0.0802(13) Uani 1 1 d . . . . .
C7 C 0.28428(19) 0.8847(4) 0.7894(4) 0.0989(18) Uani 1 1 d . . . . .
H7 H 0.283150 0.921550 0.835173 0.119 Uiso 1 1 calc R U . . .
C14 C 0.1863(2) 0.6801(5) 0.7080(4) 0.125(3) Uani 1 1 d . . . . .
H14 H 0.215850 0.661383 0.704853 0.151 Uiso 1 1 calc R U . . .
C3 C 0.3276(2) 0.8005(5) 0.7168(4) 0.112(2) Uani 1 1 d . . . . .
H3 H 0.356291 0.779680 0.711303 0.135 Uiso 1 1 calc R U . . .
C12 C 0.38309(17) 1.1692(4) 1.2340(3) 0.0873(15) Uani 1 1 d . . . . .
C6 C 0.2444(2) 0.8616(5) 0.7313(4) 0.113(2) Uani 1 1 d . . . . .
H6 H 0.215901 0.883192 0.736382 0.136 Uiso 1 1 calc R U . . .
C10 C 0.1284(2) 0.7683(4) 0.6648(4) 0.112(2) Uani 1 1 d . . . . .
H10 H 0.117297 0.811957 0.632005 0.134 Uiso 1 1 calc R U . . .
C4 C 0.2869(2) 0.7761(5) 0.6592(4) 0.124(3) Uani 1 1 d . . . . .
H4 H 0.287908 0.737759 0.615402 0.149 Uiso 1 1 calc R U . . .
C9 C 0.1705(2) 0.7428(5) 0.6593(4) 0.116(3) Uani 1 1 d . . . . .
C5 C 0.24581(19) 0.8069(4) 0.6653(3) 0.109(2) Uani 1 1 d . . . . .
C15 C 0.41240(18) 1.1278(3) 1.1776(3) 0.0828(13) Uani 1 1 d . . . . .
C8 C 0.2014(2) 0.7793(6) 0.6003(4) 0.143(4) Uani 1 1 d . . . . .
H8 H 0.210040 0.741359 0.557321 0.172 Uiso 1 1 calc R U . . .
C11 C 0.3989(2) 1.2323(4) 1.2830(4) 0.1056(18) Uani 1 1 d . . . . .
H11 H 0.428571 1.250858 1.280922 0.127 Uiso 1 1 calc 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
Er2 Er1 3.8436(4) 2_657 ?
Er2 Er1 3.8559(4) 6_575 ?
Er2 Er1 3.8559(4) . ?
Er2 Er1 3.8436(4) 5_677 ?
Er2 O8 2.300(3) . ?
Er2 O4 2.291(3) 6_575 ?
Er2 O4 2.291(3) . ?
Er2 O10 2.321(3) 2_657 ?
Er2 O10 2.321(3) 5_677 ?
Er2 O9 2.290(3) 5_677 ?
Er2 O2 2.296(3) . ?
Er2 O2 2.297(3) 6_575 ?
Er1 Er1 3.8727(5) 2_657 ?
Er1 Er1 3.8452(6) 6_575 ?
Er1 O5 2.308(3) . ?
Er1 O1 2.309(3) . ?
Er1 O8 2.2975(17) . ?
Er1 O11 2.300(5) . ?
Er1 O6 2.291(3) . ?
Er1 O10 2.305(3) 2_657 ?
Er1 O10 2.302(3) . ?
Er1 O9 2.2951(17) . ?
O5 C15 1.255(6) 5_677 ?
O1 C1 1.259(6) . ?
O3 C8 1.355(11) . ?
O4 C15 1.260(7) . ?
O6 N1 1.332(5) . ?
O7 N1 1.3522(10) . ?
O2 C1 1.249(6) . ?
C2 C1 1.516(6) . ?
C2 C7 1.371(8) . ?
C2 C3 1.368(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.382(8) 4_557 ?
C13 C12 1.364(8) . ?
C7 H7 0.9500 . ?
C7 C6 1.377(8) . ?
C14 H14 0.9500 . ?
C14 C9 1.374(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.401(8) . ?
C12 C15 1.511(6) . ?
C12 C11 1.382(9) . ?
C6 H6 0.9500 . ?
C6 C5 1.390(10) . ?
C10 H10 0.9500 . ?
C10 C9 1.351(10) . ?
C10 C11 1.383(8) 4_547 ?
C4 H4 0.9500 . ?
C4 C5 1.361(11) . ?
C9 C8 1.529(7) . ?
C5 C8 1.547(7) . ?
C8 H8 1.0000 . ?
C11 H11 0.9500 . ?

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
Er1 Er2 Er1 59.817(9) . 6_575 ?
Er1 Er2 Er1 60.395(8) 2_657 . ?
Er1 Er2 Er1 90.276(9) 5_677 . ?
Er1 Er2 Er1 60.394(8) 5_677 6_575 ?
Er1 Er2 Er1 90.276(9) 2_657 6_575 ?
Er1 Er2 Er1 60.029(10) 5_677 2_657 ?
O8 Er2 Er1 86.16(7) . 2_657 ?
O8 Er2 Er1 32.98(3) . 6_575 ?
O8 Er2 Er1 86.16(7) . 5_677 ?
O8 Er2 Er1 32.98(3) . . ?
O8 Er2 O10 65.80(8) . 5_677 ?
O8 Er2 O10 65.80(8) . 2_657 ?
O4 Er2 Er1 106.86(9) 6_575 5_677 ?
O4 Er2 Er1 107.19(10) . 6_575 ?
O4 Er2 Er1 107.19(10) 6_575 . ?
O4 Er2 Er1 159.57(9) 6_575 6_575 ?
O4 Er2 Er1 69.30(9) . 5_677 ?
O4 Er2 Er1 69.30(9) 6_575 2_657 ?
O4 Er2 Er1 159.57(9) . . ?
O4 Er2 Er1 106.86(9) . 2_657 ?
O4 Er2 O8 139.43(10) . . ?
O4 Er2 O8 139.43(10) 6_575 . ?
O4 Er2 O4 80.1(2) . 6_575 ?
O4 Er2 O10 139.60(11) 6_575 5_677 ?
O4 Er2 O10 139.60(11) . 2_657 ?
O4 Er2 O10 76.60(12) . 5_677 ?
O4 Er2 O10 76.60(12) 6_575 2_657 ?
O4 Er2 O2 131.26(13) . . ?
O4 Er2 O2 131.26(13) 6_575 6_575 ?
O4 Er2 O2 81.44(13) . 6_575 ?
O4 Er2 O2 81.44(13) 6_575 . ?
O10 Er2 Er1 86.52(6) 5_677 2_657 ?
O10 Er2 Er1 86.27(6) 2_657 6_575 ?
O10 Er2 Er1 33.40(6) 2_657 . ?
O10 Er2 Er1 33.59(6) 2_657 2_657 ?
O10 Er2 Er1 86.52(6) 2_657 5_677 ?
O10 Er2 Er1 33.59(6) 5_677 5_677 ?
O10 Er2 Er1 33.40(6) 5_677 6_575 ?
O10 Er2 Er1 86.27(6) 5_677 . ?
O10 Er2 O10 101.07(13) 5_677 2_657 ?
O9 Er2 Er1 86.18(7) 5_677 . ?
O9 Er2 Er1 33.08(3) 5_677 5_677 ?
O9 Er2 Er1 33.08(3) 5_677 2_657 ?
O9 Er2 Er1 86.18(7) 5_677 6_575 ?
O9 Er2 O8 100.18(12) 5_677 . ?
O9 Er2 O4 76.80(11) 5_677 6_575 ?
O9 Er2 O4 76.80(11) 5_677 . ?
O9 Er2 O10 66.06(8) 5_677 5_677 ?
O9 Er2 O10 66.06(8) 5_677 2_657 ?
O9 Er2 O2 140.39(11) 5_677 6_575 ?
O9 Er2 O2 140.39(10) 5_677 . ?
O2 Er2 Er1 69.16(9) . . ?
O2 Er2 Er1 105.71(8) 6_575 . ?
O2 Er2 Er1 105.71(8) . 6_575 ?
O2 Er2 Er1 159.40(9) 6_575 2_657 ?
O2 Er2 Er1 107.91(10) . 2_657 ?
O2 Er2 Er1 159.40(9) . 5_677 ?
O2 Er2 Er1 107.91(10) 6_575 5_677 ?
O2 Er2 Er1 69.16(9) 6_575 6_575 ?
O2 Er2 O8 75.94(10) . . ?
O2 Er2 O8 75.94(10) 6_575 . ?
O2 Er2 O10 138.11(11) 6_575 2_657 ?
O2 Er2 O10 138.11(11) . 5_677 ?
O2 Er2 O10 76.96(12) 6_575 5_677 ?
O2 Er2 O10 76.96(12) . 2_657 ?
O2 Er2 O2 77.9(2) . 6_575 ?
Er2 Er1 Er2 89.723(9) 5_677 . ?
Er2 Er1 Er1 59.645(7) . 2_657 ?
Er2 Er1 Er1 59.959(7) 5_677 2_657 ?
Er2 Er1 Er1 59.986(5) 5_677 6_575 ?
Er1 Er1 Er2 60.092(5) 6_575 . ?
Er1 Er1 Er1 90.0 6_575 2_657 ?
O5 Er1 Er2 70.21(9) . 5_677 ?
O5 Er1 Er2 159.91(9) . . ?
O5 Er1 Er1 108.01(10) . 6_575 ?
O5 Er1 Er1 106.98(9) . 2_657 ?
O5 Er1 O1 130.18(13) . . ?
O1 Er1 Er2 159.56(9) . 5_677 ?
O1 Er1 Er2 69.90(9) . . ?
O1 Er1 Er1 106.10(10) . 6_575 ?
O1 Er1 Er1 108.21(9) . 2_657 ?
O8 Er1 Er2 85.70(7) . 5_677 ?
O8 Er1 Er2 33.02(8) . . ?
O8 Er1 Er1 85.50(8) . 2_657 ?
O8 Er1 Er1 33.20(7) . 6_575 ?
O8 Er1 O5 140.54(12) . . ?
O8 Er1 O1 76.36(12) . . ?
O8 Er1 O11 140.32(15) . . ?
O8 Er1 O10 100.28(11) . . ?
O8 Er1 O10 66.10(11) . 2_657 ?
O11 Er1 Er2 109.56(15) . 5_677 ?
O11 Er1 Er2 108.53(14) . . ?
O11 Er1 Er1 72.61(17) . 2_657 ?
O11 Er1 Er1 162.60(17) . 6_575 ?
O11 Er1 O5 78.54(17) . . ?
O11 Er1 O1 79.61(18) . . ?
O11 Er1 O10 78.96(18) . . ?
O11 Er1 O10 78.32(17) . 2_657 ?
O6 Er1 Er2 108.81(9) . . ?
O6 Er1 Er2 107.18(9) . 5_677 ?
O6 Er1 Er1 70.64(10) . 6_575 ?
O6 Er1 Er1 160.62(10) . 2_657 ?
O6 Er1 O5 79.21(12) . . ?
O6 Er1 O1 79.12(13) . . ?
O6 Er1 O8 78.76(13) . . ?
O6 Er1 O11 126.8(2) . . ?
O6 Er1 O10 141.52(11) . 2_657 ?
O6 Er1 O10 139.95(11) . . ?
O6 Er1 O9 77.56(13) . . ?
O10 Er1 Er2 33.66(7) 2_657 . ?
O10 Er1 Er2 86.03(6) 2_657 5_677 ?
O10 Er1 Er2 85.78(6) . . ?
O10 Er1 Er2 33.91(7) . 5_677 ?
O10 Er1 Er1 86.74(7) . 6_575 ?
O10 Er1 Er1 86.74(7) 2_657 6_575 ?
O10 Er1 Er1 32.76(6) 2_657 2_657 ?
O10 Er1 Er1 32.81(6) . 2_657 ?
O10 Er1 O5 138.61(11) 2_657 . ?
O10 Er1 O5 77.02(11) . . ?
O10 Er1 O1 77.86(11) 2_657 . ?
O10 Er1 O1 140.18(11) . . ?
O10 Er1 O10 65.17(10) . 2_657 ?
O9 Er1 Er2 85.72(7) . . ?
O9 Er1 Er2 32.99(8) . 5_677 ?
O9 Er1 Er1 85.70(8) . 2_657 ?
O9 Er1 Er1 33.10(7) . 6_575 ?
O9 Er1 O5 77.96(12) . . ?
O9 Er1 O1 138.35(12) . . ?
O9 Er1 O8 65.56(10) . . ?
O9 Er1 O11 141.48(16) . . ?
O9 Er1 O10 66.29(10) . . ?
O9 Er1 O10 100.40(11) . 2_657 ?
C15 O5 Er1 135.5(4) 5_677 . ?
C1 O1 Er1 135.0(3) . . ?
Er1 O8 Er2 114.00(9) . . ?
Er1 O8 Er2 114.00(9) 6_575 . ?
Er1 O8 Er1 113.61(13) . 6_575 ?
C15 O4 Er2 137.8(3) . . ?
N1 O6 Er1 138.5(3) . . ?
Er1 O10 Er2 112.50(11) . 5_677 ?
Er1 O10 Er2 112.94(11) 2_657 5_677 ?
Er1 O10 Er1 114.42(10) . 2_657 ?
Er2 O9 Er1 113.93(9) 5_677 6_575 ?
Er2 O9 Er1 113.93(9) 5_677 . ?
Er1 O9 Er1 113.79(13) 6_575 . ?
C1 O2 Er2 137.0(3) . . ?
O6 N1 O6 121.6(5) . 6_575 ?
O6 N1 O7 119.1(3) . . ?
O6 N1 O7 119.1(3) 6_575 . ?
C7 C2 C1 120.2(5) . . ?
C3 C2 C1 119.1(5) . . ?
C3 C2 C7 120.6(5) . . ?
C14 C13 H13 119.5 4_557 . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 121.0(7) . 4_557 ?
O1 C1 C2 116.8(5) . . ?
O2 C1 O1 127.1(4) . . ?
O2 C1 C2 116.1(5) . . ?
C2 C7 H7 120.0 . . ?
C2 C7 C6 120.0(6) . . ?
C6 C7 H7 120.0 . . ?
C13 C14 H14 119.8 4_547 . ?
C9 C14 C13 120.5(7) . 4_547 ?
C9 C14 H14 119.8 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.1(7) . . ?
C4 C3 H3 120.4 . . ?
C13 C12 C15 120.3(6) . . ?
C13 C12 C11 118.4(5) . . ?
C11 C12 C15 121.3(5) . . ?
C7 C6 H6 119.9 . . ?
C7 C6 C5 120.2(7) . . ?
C5 C6 H6 119.9 . . ?
C9 C10 H10 119.3 . . ?
C9 C10 C11 121.5(7) . 4_547 ?
C11 C10 H10 119.3 4_547 . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(7) . . ?
C5 C4 H4 119.7 . . ?
C14 C9 C8 117.9(7) . . ?
C10 C9 C14 118.6(5) . . ?
C10 C9 C8 123.5(8) . . ?
C6 C5 C8 121.1(7) . . ?
C4 C5 C6 119.3(5) . . ?
C4 C5 C8 119.6(7) . . ?
O5 C15 O4 127.2(5) 5_677 . ?
O5 C15 C12 116.5(5) 5_677 . ?
O4 C15 C12 116.3(5) . . ?
O3 C8 C9 112.0(7) . . ?
O3 C8 C5 110.8(7) . . ?
O3 C8 H8 108.2 . . ?
C9 C8 C5 109.3(4) . . ?
C9 C8 H8 108.2 . . ?
C5 C8 H8 108.2 . . ?
C12 C11 C10 120.0(7) . 4_557 ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 4_557 . ?

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
Er2 O4 C15 O5 1.9(9) . . . 5_677 ?
Er2 O4 C15 C12 179.6(3) . . . . ?
Er2 O2 C1 O1 18.4(10) . . . . ?
Er2 O2 C1 C2 -162.9(4) . . . . ?
Er1 O1 C1 O2 -17.1(9) . . . . ?
Er1 O1 C1 C2 164.2(3) . . . . ?
Er1 O6 N1 O6 -2.6(11) . . . 6_575 ?
Er1 O6 N1 O7 -178.5(5) . . . . ?
C2 C7 C6 C5 1.1(10) . . . . ?
C2 C3 C4 C5 1.5(11) . . . . ?
C13 C14 C9 C10 -0.1(11) 4_547 . . . ?
C13 C14 C9 C8 -179.1(6) 4_547 . . . ?
C13 C12 C15 O5 -166.2(5) . . . 5_677 ?
C13 C12 C15 O4 15.9(8) . . . . ?
C13 C12 C11 C10 0.0(9) . . . 4_557 ?
C1 C2 C7 C6 179.0(5) . . . . ?
C1 C2 C3 C4 179.7(6) . . . . ?
C7 C2 C1 O1 -169.8(5) . . . . ?
C7 C2 C1 O2 11.4(8) . . . . ?
C7 C2 C3 C4 0.0(9) . . . . ?
C7 C6 C5 C4 0.4(10) . . . . ?
C7 C6 C5 C8 179.1(6) . . . . ?
C14 C13 C12 C15 178.1(6) 4_557 . . . ?
C14 C13 C12 C11 -0.8(10) 4_557 . . . ?
C14 C9 C8 O3 172.9(7) . . . . ?
C14 C9 C8 C5 -64.0(10) . . . . ?
C3 C2 C1 O1 10.5(8) . . . . ?
C3 C2 C1 O2 -168.3(5) . . . . ?
C3 C2 C7 C6 -1.3(9) . . . . ?
C3 C4 C5 C6 -1.7(10) . . . . ?
C3 C4 C5 C8 179.6(6) . . . . ?
C6 C5 C8 O3 59.9(8) . . . . ?
C6 C5 C8 C9 -64.0(10) . . . . ?
C10 C9 C8 O3 -6.1(10) . . . . ?
C10 C9 C8 C5 117.1(8) . . . . ?
C4 C5 C8 O3 -121.5(8) . . . . ?
C4 C5 C8 C9 114.6(8) . . . . ?
C15 C12 C11 C10 -178.9(5) . . . 4_557 ?
C11 C12 C15 O5 12.7(8) . . . 5_677 ?
C11 C12 C15 O4 -165.3(5) . . . . ?
C11 C10 C9 C14 -0.8(10) 4_547 . . . ?
C11 C10 C9 C8 178.1(6) 4_547 . . . ?

_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 -0.129 -0.907 -0.648 5070.1 1166.6 ?


_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
;
####################################################################### 
# 
# 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_lk1_44_3
_database_code_depnum_ccdc_archive 'CCDC 2338723'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H18 Ho3 N O19'
_chemical_formula_sum            'C30 H18 Ho3 N O19'
_chemical_formula_weight         1191.24
_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'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   29.5465(5)
_cell_length_b                   18.6021(4)
_cell_length_c                   14.5637(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.304(2)
_cell_angle_gamma                90
_cell_volume                     7820.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11667
_cell_measurement_temperature    101.6(8)
_cell_measurement_theta_max      71.2370
_cell_measurement_theta_min      4.4400
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.377
_exptl_absorpt_coefficient_mu    5.767
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.012
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25371
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.994
_diffrn_reflns_theta_max         66.994
_diffrn_reflns_theta_min         3.870
_diffrn_ambient_temperature      101.75
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  20.00   1.00    2.50    --    0.00  57.00-180.00   53
  2  ω    -14.00  42.00   1.00    2.50    --    0.00  57.00 -60.00   56
  3  ω      1.00  26.00   1.00    2.50    --    0.00 -99.00 150.00   25
  4  ω     46.00  84.00   1.00    2.50    --    0.00  57.00-180.00   38
  5  ω     25.00 116.00   1.00    5.00    --   54.44-125.00 -90.00   91
  6  ω    102.00 142.00   1.00    5.00    --   54.44 125.00-120.00   40
  7  ω    116.00 142.00   1.00    5.00    --   54.44 125.00 -90.00   26
  8  ω    100.00 142.00   1.00    5.00    --   54.44 125.00-180.00   42
  9  ω    100.00 135.00   1.00    5.00    --   54.44 125.00 120.00   35
 10  ω     94.00 119.00   1.00    5.00    --   54.44 125.00 -60.00   25
 11  ω    101.00 139.00   1.00    5.00    --   54.44 125.00  60.00   38
 12  ω    -32.00 151.00   1.00    5.00    --   54.44   0.00  30.00  183
 13  ω     20.00  82.00   1.00   30.00    --  108.88-111.00   0.00   62
 14  ω    122.00 166.00   1.00   30.00    --  108.88  50.00-180.00   44
 15  ω     68.00 149.00   1.00   30.00    --  108.88  38.00-120.00   81
 16  ω     74.00 116.00   1.00   30.00    --  108.88  50.00-180.00   42
 17  ω     85.00 112.00   1.00   30.00    --  108.88-111.00-180.00   27
 18  ω     14.00 145.00   1.00   30.00    --  108.88 -77.00  60.00  131
 19  ω     50.00 178.00   1.00   30.00    --  108.88  25.00 150.00  128
 20  ω     88.00 143.00   1.00   30.00    --  108.88 178.00 -30.00   55
 21  ω     79.00 106.00   1.00   30.00    --  108.88-111.00 120.00   27
 22  ω     54.00 106.00   1.00   30.00    --  108.88 -92.00   0.00   52
 23  ω    121.00 175.00   1.00   30.00    --  108.88  77.00 120.00   54
 24  ω    100.00 163.00   1.00   30.00    --  108.88 111.00  60.00   63
 25  ω    125.00 164.00   1.00   30.00    --  108.88 111.00 150.00   39
 26  ω     71.00 100.00   1.00   30.00    --  108.88  77.00 120.00   29
 27  ω     20.00 112.00   1.00   30.00    --  108.88-111.00 -60.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6136
_reflns_number_total             7197
_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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         7197
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1154P)²+2.8964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1680
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O7-N1
 1.35 with sigma of 0.001
3. Rigid bond restraints
 O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
N1 \\sim O6 \\sim O7: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
5. Rigid body (RIGU) restrains
 N1, O6, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C8(H8)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_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
C1 C 0.63262(16) 0.6175(3) 0.6570(3) 0.0720(12) Uani 1 1 d . . . . .
Ho1 Ho 0.51816(2) 0.60455(2) 0.63634(2) 0.05694(14) Uani 1 1 d . . . . .
N1 N 0.5413(3) 0.500000 0.8325(5) 0.107(2) Uani 1 2 d DS TU P . .
O1 O 0.59492(11) 0.6384(2) 0.6767(2) 0.0777(9) Uani 1 1 d . . . . .
C2 C 0.67633(16) 0.6443(3) 0.7193(3) 0.0716(12) Uani 1 1 d . . . . .
Ho2 Ho 0.59076(2) 0.500000 0.48723(3) 0.05893(16) Uani 1 2 d S T P . .
O2 O 0.63714(11) 0.5769(2) 0.5892(2) 0.0731(8) Uani 1 1 d . . . . .
C3 C 0.6742(2) 0.6974(4) 0.7850(4) 0.0949(19) Uani 1 1 d . . . . .
H3 H 0.645022 0.715812 0.791198 0.114 Uiso 1 1 calc R U . . .
O3 O 0.67600(18) 0.8291(4) 0.0453(3) 0.154(3) Uani 1 1 d . . . . .
C4 C 0.7146(2) 0.7240(4) 0.8417(4) 0.099(2) Uani 1 1 d . . . . .
H4 H 0.713088 0.762020 0.884441 0.119 Uiso 1 1 calc R U . . .
O4 O 0.60872(12) 0.5795(2) 0.3794(2) 0.0746(8) Uani 1 1 d . . . . .
C5 C 0.75660(19) 0.6954(4) 0.8360(3) 0.0896(19) Uani 1 1 d . . . . .
O5 O 0.45450(11) 0.6418(2) 0.6921(2) 0.0773(9) Uani 1 1 d . . . . .
C6 C 0.75842(19) 0.6423(4) 0.7720(4) 0.0973(19) Uani 1 1 d . . . . .
H6 H 0.787637 0.622895 0.767626 0.117 Uiso 1 1 calc R U . . .
O8 O 0.55848(11) 0.500000 0.6203(2) 0.0480(7) Uani 1 2 d S T P . .
C7 C 0.71861(18) 0.6160(3) 0.7133(4) 0.0826(15) Uani 1 1 d . . . . .
H7 H 0.720538 0.578938 0.669402 0.099 Uiso 1 1 calc R U . . .
O9 O 0.47539(11) 0.500000 0.6315(2) 0.0499(7) Uani 1 2 d S T P . .
C8 C 0.6997(2) 0.7747(5) 0.0989(3) 0.115(3) Uani 1 1 d . . . . .
H8 H 0.709041 0.737969 0.056255 0.138 Uiso 1 1 calc R U . . .
O10 O 0.45846(8) 0.59457(14) 0.50495(17) 0.0487(5) Uani 1 1 d . . . . .
C9 C 0.6693(2) 0.7385(4) 0.1583(3) 0.094(2) Uani 1 1 d . . . . .
O11 O 0.51109(17) 0.7212(2) 0.5783(4) 0.1022(13) Uani 1 1 d . . . . .
C10 C 0.6258(2) 0.7628(4) 0.1620(5) 0.102(2) Uani 1 1 d . . . . .
H10 H 0.613851 0.804952 0.128669 0.122 Uiso 1 1 calc R U . . .
O6 O 0.53769(13) 0.5647(3) 0.7892(2) 0.0850(10) Uani 1 1 d . U . . .
C11 C 0.5995(2) 0.7259(4) 0.2142(5) 0.0962(18) Uani 1 1 d . . . . .
H11 H 0.569056 0.742122 0.214822 0.115 Uiso 1 1 calc R U . . .
O7 O 0.5519(4) 0.500000 0.9274(5) 0.218(6) Uani 1 2 d DS TU P . .
C12 C 0.61641(18) 0.6666(4) 0.2649(3) 0.0807(14) Uani 1 1 d . . . . .
C13 C 0.66048(19) 0.6431(4) 0.2619(4) 0.098(2) Uani 1 1 d . . . . .
H13 H 0.672716 0.601499 0.296361 0.117 Uiso 1 1 calc R U . . .
C14 C 0.6867(2) 0.6792(5) 0.2097(5) 0.110(3) Uani 1 1 d . . . . .
H14 H 0.717122 0.663051 0.209108 0.132 Uiso 1 1 calc R U . . .
C15 C 0.58777(18) 0.6250(3) 0.3213(4) 0.0758(13) 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
C1 O1 1.269(6) . ?
C1 C2 1.496(6) . ?
C1 O2 1.274(6) . ?
Ho1 Ho1 3.8897(6) 6_565 ?
Ho1 Ho1 3.8865(6) 2_656 ?
Ho1 O1 2.306(3) . ?
Ho1 Ho2 3.8839(4) . ?
Ho1 Ho2 3.8613(5) 5_666 ?
Ho1 O5 2.308(3) . ?
Ho1 O8 2.3183(17) . ?
Ho1 O9 2.3122(18) . ?
Ho1 O10 2.317(2) . ?
Ho1 O10 2.313(2) 2_656 ?
Ho1 O11 2.322(4) . ?
Ho1 O6 2.300(3) . ?
N1 O6 1.352(5) . ?
N1 O6 1.352(5) 6_565 ?
N1 O7 1.3515(10) . ?
C2 C3 1.386(8) . ?
C2 C7 1.375(8) . ?
Ho2 O2 2.294(3) 6_565 ?
Ho2 O2 2.294(3) . ?
Ho2 O4 2.300(3) 6_565 ?
Ho2 O4 2.300(3) . ?
Ho2 O8 2.335(3) . ?
Ho2 O9 2.317(3) 5_666 ?
Ho2 O10 2.301(3) 2_656 ?
Ho2 O10 2.301(3) 5_666 ?
C3 H3 0.9500 . ?
C3 C4 1.390(8) . ?
O3 C8 1.375(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.368(10) . ?
O4 C15 1.262(7) . ?
C5 C6 1.368(10) . ?
C5 C8 1.534(7) 7_666 ?
O5 C15 1.261(7) 2_656 ?
C6 H6 0.9500 . ?
C6 C7 1.387(8) . ?
C7 H7 0.9500 . ?
C8 H8 1.0000 . ?
C8 C9 1.529(6) . ?
C9 C10 1.374(10) . ?
C9 C14 1.370(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.362(9) . ?
C12 C13 1.383(8) . ?
C12 C15 1.511(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.372(8) . ?
C14 H14 0.9500 . ?

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 C1 C2 116.6(5) . . ?
O1 C1 O2 126.8(4) . . ?
O2 C1 C2 116.6(4) . . ?
Ho1 Ho1 Ho1 90.0 2_656 6_565 ?
O1 Ho1 Ho1 105.86(11) . 6_565 ?
O1 Ho1 Ho1 107.62(9) . 2_656 ?
O1 Ho1 Ho2 158.93(9) . 5_666 ?
O1 Ho1 Ho2 69.45(9) . . ?
O1 Ho1 O5 131.25(13) . . ?
O1 Ho1 O8 75.90(12) . . ?
O1 Ho1 O9 137.65(13) . . ?
O1 Ho1 O10 140.05(11) . . ?
O1 Ho1 O10 77.56(11) . 2_656 ?
O1 Ho1 O11 81.06(16) . . ?
Ho2 Ho1 Ho1 59.952(6) . 6_565 ?
Ho2 Ho1 Ho1 59.593(8) . 2_656 ?
Ho2 Ho1 Ho1 60.171(9) 5_666 2_656 ?
Ho2 Ho1 Ho1 59.757(6) 5_666 6_565 ?
Ho2 Ho1 Ho2 89.542(11) 5_666 . ?
O5 Ho1 Ho1 107.47(10) . 6_565 ?
O5 Ho1 Ho1 106.92(9) . 2_656 ?
O5 Ho1 Ho2 69.78(10) . 5_666 ?
O5 Ho1 Ho2 159.31(10) . . ?
O5 Ho1 O8 139.64(12) . . ?
O5 Ho1 O9 77.41(12) . . ?
O5 Ho1 O10 139.21(11) . 2_656 ?
O5 Ho1 O10 77.31(11) . . ?
O5 Ho1 O11 80.25(16) . . ?
O8 Ho1 Ho1 32.98(6) . 6_565 ?
O8 Ho1 Ho1 86.15(8) . 2_656 ?
O8 Ho1 Ho2 85.74(8) . 5_666 ?
O8 Ho1 Ho2 33.56(7) . . ?
O8 Ho1 O11 139.08(14) . . ?
O9 Ho1 Ho1 86.49(9) . 2_656 ?
O9 Ho1 Ho1 32.74(7) . 6_565 ?
O9 Ho1 Ho2 85.71(8) . . ?
O9 Ho1 Ho2 33.52(8) . 5_666 ?
O9 Ho1 O8 65.20(10) . . ?
O9 Ho1 O10 99.80(11) . 2_656 ?
O9 Ho1 O10 65.95(11) . . ?
O9 Ho1 O11 140.24(14) . . ?
O10 Ho1 Ho1 85.40(7) . 6_565 ?
O10 Ho1 Ho1 85.40(7) 2_656 6_565 ?
O10 Ho1 Ho1 32.90(6) . 2_656 ?
O10 Ho1 Ho1 32.96(6) 2_656 2_656 ?
O10 Ho1 Ho2 84.96(6) . . ?
O10 Ho1 Ho2 85.54(6) 2_656 5_666 ?
O10 Ho1 Ho2 33.13(6) . 5_666 ?
O10 Ho1 Ho2 32.57(6) 2_656 . ?
O10 Ho1 O8 65.53(10) 2_656 . ?
O10 Ho1 O8 99.59(11) . . ?
O10 Ho1 O10 65.05(10) 2_656 . ?
O10 Ho1 O11 77.33(14) . . ?
O10 Ho1 O11 76.82(14) 2_656 . ?
O11 Ho1 Ho1 69.16(13) . 2_656 ?
O11 Ho1 Ho1 159.16(13) . 6_565 ?
O11 Ho1 Ho2 106.38(12) . . ?
O11 Ho1 Ho2 107.44(12) . 5_666 ?
O6 Ho1 Ho1 161.18(12) . 2_656 ?
O6 Ho1 Ho1 71.19(12) . 6_565 ?
O6 Ho1 O1 79.12(14) . . ?
O6 Ho1 Ho2 108.97(10) . . ?
O6 Ho1 Ho2 107.51(11) . 5_666 ?
O6 Ho1 O5 79.15(13) . . ?
O6 Ho1 O8 78.39(13) . . ?
O6 Ho1 O9 77.35(14) . . ?
O6 Ho1 O10 139.74(12) . . ?
O6 Ho1 O10 140.71(11) . 2_656 ?
O6 Ho1 O11 129.66(18) . . ?
O6 N1 O6 125.7(6) . 6_565 ?
O7 N1 O6 117.1(3) . 6_565 ?
O7 N1 O6 117.1(3) . . ?
C1 O1 Ho1 136.2(3) . . ?
C3 C2 C1 119.7(5) . . ?
C7 C2 C1 120.9(5) . . ?
C7 C2 C3 119.5(5) . . ?
Ho1 Ho2 Ho1 90.458(11) 2_656 6_565 ?
Ho1 Ho2 Ho1 60.487(11) 5_666 2_656 ?
Ho1 Ho2 Ho1 60.236(9) 5_666 6_565 ?
Ho1 Ho2 Ho1 60.237(9) 2_656 . ?
Ho1 Ho2 Ho1 90.458(11) 5_666 . ?
Ho1 Ho2 Ho1 60.097(11) . 6_565 ?
O2 Ho2 Ho1 108.14(10) 6_565 5_666 ?
O2 Ho2 Ho1 159.95(9) 6_565 2_656 ?
O2 Ho2 Ho1 69.56(9) . . ?
O2 Ho2 Ho1 105.96(8) 6_565 . ?
O2 Ho2 Ho1 108.14(10) . 2_656 ?
O2 Ho2 Ho1 105.97(8) . 6_565 ?
O2 Ho2 Ho1 69.56(9) 6_565 6_565 ?
O2 Ho2 Ho1 159.95(9) . 5_666 ?
O2 Ho2 O2 77.1(2) 6_565 . ?
O2 Ho2 O4 81.30(13) . . ?
O2 Ho2 O4 130.55(13) . 6_565 ?
O2 Ho2 O4 81.30(13) 6_565 6_565 ?
O2 Ho2 O4 130.55(13) 6_565 . ?
O2 Ho2 O8 75.87(10) 6_565 . ?
O2 Ho2 O8 75.87(10) . . ?
O2 Ho2 O9 140.87(10) . 5_666 ?
O2 Ho2 O9 140.87(10) 6_565 5_666 ?
O2 Ho2 O10 77.76(11) 6_565 5_666 ?
O2 Ho2 O10 137.85(10) 6_565 2_656 ?
O2 Ho2 O10 137.85(10) . 5_666 ?
O2 Ho2 O10 77.76(11) . 2_656 ?
O4 Ho2 Ho1 107.18(10) 6_565 6_565 ?
O4 Ho2 Ho1 69.43(9) 6_565 5_666 ?
O4 Ho2 Ho1 159.88(9) 6_565 . ?
O4 Ho2 Ho1 107.22(9) . 5_666 ?
O4 Ho2 Ho1 107.18(10) . . ?
O4 Ho2 Ho1 159.88(9) . 6_565 ?
O4 Ho2 Ho1 107.22(9) 6_565 2_656 ?
O4 Ho2 Ho1 69.43(9) . 2_656 ?
O4 Ho2 O4 79.99(19) 6_565 . ?
O4 Ho2 O8 139.58(10) . . ?
O4 Ho2 O8 139.58(10) 6_565 . ?
O4 Ho2 O9 76.76(11) . 5_666 ?
O4 Ho2 O9 76.76(11) 6_565 5_666 ?
O4 Ho2 O10 77.44(11) . 2_656 ?
O4 Ho2 O10 139.95(11) 6_565 2_656 ?
O4 Ho2 O10 77.44(11) 6_565 5_666 ?
O4 Ho2 O10 139.95(11) . 5_666 ?
O8 Ho2 Ho1 86.53(7) . 5_666 ?
O8 Ho2 Ho1 33.29(3) . . ?
O8 Ho2 Ho1 86.53(7) . 2_656 ?
O8 Ho2 Ho1 33.29(4) . 6_565 ?
O9 Ho2 Ho1 33.44(3) 5_666 5_666 ?
O9 Ho2 Ho1 86.48(7) 5_666 6_565 ?
O9 Ho2 Ho1 86.48(7) 5_666 . ?
O9 Ho2 Ho1 33.44(3) 5_666 2_656 ?
O9 Ho2 O8 100.98(12) 5_666 . ?
O10 Ho2 Ho1 32.77(6) 5_666 6_565 ?
O10 Ho2 Ho1 32.78(6) 2_656 . ?
O10 Ho2 Ho1 85.70(6) 5_666 . ?
O10 Ho2 Ho1 85.70(6) 2_656 6_565 ?
O10 Ho2 Ho1 86.29(6) 5_666 2_656 ?
O10 Ho2 Ho1 33.39(6) 2_656 2_656 ?
O10 Ho2 Ho1 86.29(6) 2_656 5_666 ?
O10 Ho2 Ho1 33.39(6) 5_666 5_666 ?
O10 Ho2 O8 65.46(8) 5_666 . ?
O10 Ho2 O8 65.46(8) 2_656 . ?
O10 Ho2 O9 66.13(8) 2_656 5_666 ?
O10 Ho2 O9 66.13(8) 5_666 5_666 ?
O10 Ho2 O10 99.75(12) 5_666 2_656 ?
C1 O2 Ho2 136.5(3) . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.3(6) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.1(6) . . ?
C5 C4 H4 120.0 . . ?
C15 O4 Ho2 137.5(3) . . ?
C4 C5 C6 119.3(5) . . ?
C4 C5 C8 118.5(6) . 7_666 ?
C6 C5 C8 122.2(6) . 7_666 ?
C15 O5 Ho1 136.5(4) 2_656 . ?
C5 C6 H6 119.2 . . ?
C5 C6 C7 121.6(6) . . ?
C7 C6 H6 119.2 . . ?
Ho1 O8 Ho1 114.05(13) . 6_565 ?
Ho1 O8 Ho2 113.15(9) 6_565 . ?
Ho1 O8 Ho2 113.15(9) . . ?
C2 C7 C6 119.2(6) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
Ho1 O9 Ho1 114.52(14) . 6_565 ?
Ho1 O9 Ho2 113.04(9) . 5_666 ?
Ho1 O9 Ho2 113.04(9) 6_565 5_666 ?
O3 C8 C5 110.1(6) . 7_666 ?
O3 C8 H8 108.9 . . ?
O3 C8 C9 110.8(6) . . ?
C5 C8 H8 108.9 7_666 . ?
C9 C8 C5 109.2(4) . 7_666 ?
C9 C8 H8 108.9 . . ?
Ho1 O10 Ho1 114.14(10) 2_656 . ?
Ho2 O10 Ho1 113.48(10) 5_666 . ?
Ho2 O10 Ho1 114.66(10) 5_666 2_656 ?
C10 C9 C8 123.1(7) . . ?
C14 C9 C8 117.7(6) . . ?
C14 C9 C10 119.2(5) . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0(7) . . ?
C11 C10 H10 120.0 . . ?
N1 O6 Ho1 135.8(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 C10 121.1(7) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C13 118.6(5) . . ?
C11 C12 C15 121.7(5) . . ?
C13 C12 C15 119.7(6) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.6(7) . . ?
C14 C13 H13 119.7 . . ?
C9 C14 C13 120.5(6) . . ?
C9 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
O4 C15 C12 117.1(5) . . ?
O5 C15 O4 126.7(4) 2_656 . ?
O5 C15 C12 116.1(5) 2_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
C1 C2 C3 C4 -178.4(6) . . . . ?
C1 C2 C7 C6 179.8(5) . . . . ?
O1 C1 C2 C3 -9.4(8) . . . . ?
O1 C1 C2 C7 169.6(5) . . . . ?
O1 C1 O2 Ho2 -15.9(9) . . . . ?
C2 C1 O1 Ho1 -164.8(3) . . . . ?
C2 C1 O2 Ho2 164.9(3) . . . . ?
C2 C3 C4 C5 -3.0(10) . . . . ?
Ho2 O4 C15 O5 2.1(9) . . . 2_656 ?
Ho2 O4 C15 C12 179.0(3) . . . . ?
O2 C1 O1 Ho1 16.0(9) . . . . ?
O2 C1 C2 C3 169.8(5) . . . . ?
O2 C1 C2 C7 -11.1(7) . . . . ?
C3 C2 C7 C6 -1.1(9) . . . . ?
C3 C4 C5 C6 2.1(10) . . . . ?
C3 C4 C5 C8 -178.9(6) . . . 7_666 ?
O3 C8 C9 C10 -5.3(9) . . . . ?
O3 C8 C9 C14 174.6(6) . . . . ?
C4 C5 C6 C7 -0.8(10) . . . . ?
C5 C6 C7 C2 0.3(10) . . . . ?
C5 C8 C9 C10 116.1(7) 7_666 . . . ?
C5 C8 C9 C14 -64.0(9) 7_666 . . . ?
C7 C2 C3 C4 2.5(9) . . . . ?
C8 C5 C6 C7 -179.7(6) 7_666 . . . ?
C8 C9 C10 C11 177.4(6) . . . . ?
C8 C9 C14 C13 -177.9(7) . . . . ?
C9 C10 C11 C12 2.0(11) . . . . ?
C10 C9 C14 C13 2.1(11) . . . . ?
C10 C11 C12 C13 -1.1(10) . . . . ?
C10 C11 C12 C15 -179.1(6) . . . . ?
O6 N1 O6 Ho1 7.3(13) 6_565 . . . ?
C11 C12 C13 C14 0.6(11) . . . . ?
C11 C12 C15 O4 -167.2(6) . . . . ?
C11 C12 C15 O5 10.0(8) . . . 2_656 ?
O7 N1 O6 Ho1 -176.7(7) . . . . ?
C12 C13 C14 C9 -1.1(12) . . . . ?
C13 C12 C15 O4 14.8(8) . . . . ?
C13 C12 C15 O5 -168.0(6) . . . 2_656 ?
C14 C9 C10 C11 -2.5(11) . . . . ?
C15 C12 C13 C14 178.7(6) . . . . ?

_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 -0.534 -0.051 -0.507 5174.3 1091.8 ?


_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
;
####################################################################### 
# 
# 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_lk1_44_1
_database_code_depnum_ccdc_archive 'CCDC 2338721'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_chemical_formula_moiety         'C30 H18 N O19 Tb3'
_chemical_formula_sum            'C30 H18 N1 O19 Tb3'
_chemical_formula_weight         1173.249
_chemical_oxdiff_formula         'Tb F O N C H'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.03110 0.01806 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Tb -9.04748 9.18885 25.89760 18.21850 14.31670 2.95354 2.24256 0.19614 12.66480
115.36200 3.58324 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z

_symmetry_Int_Tables_number      12
_cell_length_a                   29.8060(8)
_cell_length_b                   18.4881(7)
_cell_length_c                   14.6432(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.960(3)
_cell_angle_gamma                90
_cell_volume                     7922.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10565
_cell_measurement_temperature    104(4)
_cell_measurement_theta_max      71.0560
_cell_measurement_theta_min      4.3760
_exptl_absorpt_coefficient_mu    13.269
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_correction_T_min  0.138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       plate
_exptl_crystal_F_000             2113.458
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.9986
_diffrn_reflns_Laue_measured_fraction_max 0.9986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27095
_diffrn_reflns_point_group_measured_fraction_full 0.9986
_diffrn_reflns_point_group_measured_fraction_max 0.9986
_diffrn_reflns_theta_full        66.9974
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.88
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00  49.00   1.00    5.00    --    0.00 -99.00 -60.00   30
  2  ω     53.00  86.00   1.00    5.00    --    0.00  38.00 -60.00   33
  3  ω    -61.00 -36.00   1.00    5.00    --    0.00 178.00  30.00   25
  4  ω    -40.00   6.00   1.00    5.00    --    0.00  38.00 -60.00   46
  5  ω     14.00  44.00   1.00    5.00    --    0.00  38.00 -60.00   30
  6  ω   -133.00 -99.00   1.00    5.00    --  -54.44 -99.00-150.00   34
  7  ω   -139.00-110.00   1.00    5.00    --  -54.44 -99.00 -90.00   29
  8  ω   -146.00  35.00   1.00    5.00    --  -54.44 -19.00  90.00  181
  9  ω   -130.00 -82.00   1.00    5.00    --  -54.44 -99.00 -60.00   48
 10  ω    100.00 137.00   1.00    5.00    --   54.44 125.00 -30.00   37
 11  ω    108.00 142.00   1.00    5.00    --   54.44 125.00  30.00   34
 12  ω     94.00 142.00   1.00    5.00    --   54.44 125.00  60.00   48
 13  ω     37.00 117.00   1.00    5.00    --   54.44-125.00  60.00   80
 14  ω    108.00 142.00   1.00    5.00    --   54.44 125.00-120.00   34
 15  ω     23.00 150.00   1.00   30.00    --  108.88 -38.00 -90.00  127
 16  ω     22.00 106.00   1.00   30.00    --  108.88-111.00-120.00   84
 17  ω     83.00 110.00   1.00   30.00    --  108.88-111.00 -30.00   27
 18  ω    116.00 173.00   1.00   30.00    --  108.88  12.00   0.00   57
 19  ω    101.00 178.00   1.00   30.00    --  108.88 111.00   0.00   77
 20  ω     71.00 163.00   1.00   30.00    --  108.88  38.00 120.00   92
 21  ω     81.00 109.00   1.00   30.00    --  108.88 -92.00   0.00   28
 22  ω     21.00 141.00   1.00   30.00    --  108.88 -77.00 -90.00  120
 23  ω    121.00 170.00   1.00   30.00    --  108.88 111.00 -60.00   49
 24  ω     69.00 112.00   1.00   30.00    --  108.88-111.00 120.00   43
 25  ω     24.00  50.00   1.00   30.00    --  108.88-111.00 120.00   26
 26  ω     60.00 129.00   1.00   30.00    --  108.88 -50.00  30.00   69
 27  ω    138.00 168.00   1.00   30.00    --  108.88 111.00-180.00   30
 28  ω     69.00 106.00   1.00   30.00    --  108.88 -92.00 120.00   37
 29  ω     19.00  81.00   1.00   30.00    --  108.88  12.00   0.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0055999000
_diffrn_orient_matrix_UB_12      0.0026079000
_diffrn_orient_matrix_UB_13      -0.1067941000
_diffrn_orient_matrix_UB_21      0.0187767000
_diffrn_orient_matrix_UB_22      -0.0775748000
_diffrn_orient_matrix_UB_23      0.0001887000
_diffrn_orient_matrix_UB_31      -0.0488692000
_diffrn_orient_matrix_UB_32      -0.0301354000
_diffrn_orient_matrix_UB_33      -0.0096023000
_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         0.0
_reflns_limit_h_max              34
_reflns_limit_h_min              -35
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6092
_reflns_number_total             7291
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.1469
_refine_diff_density_min         -1.5697
_refine_diff_density_rms         0.1339
_refine_ls_d_res_high            0.8375
_refine_ls_d_res_low             11.3945
_refine_ls_goodness_of_fit_ref   0.9938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     247
_refine_ls_number_reflns         7291
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0597
_refine_ls_restrained_S_all      0.9922
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1319P)²+5.8953P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1809
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O7-N1
 1.35 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
O7 \\sim N1 \\sim O6: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O7, N1, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14)
;
_atom_sites_solution_primary     iterative
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.5898(3) 0.3732(4) 0.8219(5) 0.0764(19) Uani 1.000000 1 . . .
C2 C 0.6193(2) 0.3324(4) 0.7661(4) 0.0699(17) Uani 1.000000 1 . . .
C3 C 0.6035(3) 0.2698(5) 0.7167(6) 0.095(2) Uani 1.000000 1 . . .
H3 H 0.5738(3) 0.2519(5) 0.7187(6) 0.114(3) Uiso 1.000000 1 R . .
C4 C 0.6307(3) 0.2340(6) 0.6650(5) 0.098(3) Uani 1.000000 1 . . .
H4 H 0.6198(3) 0.1911(6) 0.6327(5) 0.117(3) Uiso 1.000000 1 R . .
C5 C 0.6729(2) 0.2592(6) 0.6596(4) 0.091(3) Uani 1.000000 1 . . .
C6 C 0.6888(3) 0.3215(7) 0.7078(6) 0.110(3) Uani 1.000000 1 . . .
H6 H 0.7181(3) 0.3400(7) 0.7040(6) 0.132(4) Uiso 1.000000 1 R . .
C7 C 0.6622(2) 0.3568(6) 0.7612(5) 0.094(3) Uani 1.000000 1 . . .
H7 H 0.6738(2) 0.3988(6) 0.7951(5) 0.112(3) Uiso 1.000000 1 R . .
C8 C 0.7044(3) 0.2241(7) 0.6014(5) 0.112(4) Uani 1.000000 1 . . .
H8 H 0.7136(3) 0.2612(7) 0.5589(5) 0.134(5) Uiso 1.000000 1 R . .
C9 C 0.7474(2) 0.1949(5) 0.6664(4) 0.089(3) Uani 1.000000 1 . . .
C10 C 0.7453(3) 0.1436(6) 0.7315(5) 0.098(3) Uani 1.000000 1 . . .
H10 H 0.7164(3) 0.1248(6) 0.7374(5) 0.118(3) Uiso 1.000000 1 R . .
C11 C 0.7842(3) 0.1179(5) 0.7897(5) 0.086(2) Uani 1.000000 1 . . .
H11 H 0.7820(3) 0.0819(5) 0.8350(5) 0.103(3) Uiso 1.000000 1 R . .
C12 C 0.8254(2) 0.1446(4) 0.7812(4) 0.0719(18) Uani 1.000000 1 . . .
C13 C 0.8285(3) 0.1978(6) 0.7169(5) 0.104(3) Uani 1.000000 1 . . .
H13 H 0.8574(3) 0.2168(6) 0.7112(5) 0.125(4) Uiso 1.000000 1 R . .
C14 C 0.7886(3) 0.2236(7) 0.6601(5) 0.111(4) Uani 1.000000 1 . . .
H14 H 0.7903(3) 0.2613(7) 0.6169(5) 0.134(4) Uiso 1.000000 1 R . .
C15 C 0.8686(2) 0.1187(4) 0.8432(4) 0.0733(19) Uani 1.000000 1 . . .
N1 N 0.4599(3) 0.5 0.6656(5) 0.088(2) Uani 1.000000 2 DS TU P
O1 O 0.54799(15) 0.3569(3) 0.8077(3) 0.0750(12) Uani 1.000000 1 . . .
O2 O 0.60955(15) 0.4194(3) 0.8784(3) 0.0709(11) Uani 1.000000 1 . . .
O3 O 0.6817(2) 0.1685(6) 0.5489(4) 0.160(4) Uani 1.000000 1 . . .
O9 O 0.54117(12) 0.4037(2) 0.9941(2) 0.0487(8) Uani 1.000000 1 . . .
O8 O 0.52598(14) 0.5 0.8690(3) 0.0470(10) Uani 1.000000 2 S T P
O5 O 0.63570(15) 0.4208(3) 1.0894(3) 0.0747(12) Uani 1.000000 1 . . .
O11 O 0.4898(2) 0.2759(3) 0.9219(5) 0.1050(18) Uani 1.000000 1 . . .
O4 O 0.40647(15) 0.3599(3) 0.8245(3) 0.0783(13) Uani 1.000000 1 . . .
O10 O 0.44328(15) 0.5 0.8820(3) 0.0461(10) Uani 1.000000 2 S T P
O6 O 0.46497(14) 0.4376(3) 0.7096(3) 0.0727(12) Uani 1.000000 1 . U .
O7 O 0.4475(4) 0.5 0.5719(5) 0.131(4) Uani 1.000000 2 DS TU P
Tb1 Tb 0.483010(10) 0.39399(2) 0.86246(2) 0.05554(15) Uani 1.000000 1 . . .
Tb2 Tb 0.590758(14) 0.5 0.98699(3) 0.05651(17) Uani 1.000000 2 S T P


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
C1 C2 1.511(8) . ?
C1 O1 1.261(9) . ?
C1 O2 1.255(10) . ?
C2 C3 1.398(11) . ?
C2 C7 1.371(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.356(13) . ?
C5 C6 1.388(14) . ?
C5 C8 1.527(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(10) . ?
C7 H7 0.9500 . ?
C8 H8 1.0000 . ?
C8 C9 1.543(8) . ?
C8 O3 1.380(14) . ?
C9 C10 1.353(12) . ?
C9 C14 1.356(13) . ?
C10 H10 0.9500 . ?
C10 C11 1.387(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.350(11) . ?
C12 C13 1.376(12) . ?
C12 C15 1.508(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.399(10) . ?
C14 H14 0.9500 . ?
C15 O5 1.254(9) 7_657 ?
C15 O4 1.273(9) 8 ?
N1 O6 1.316(6) 4_565 ?
N1 O6 1.316(6) . ?
N1 O7 1.3513(10) . ?
O1 Tb1 2.336(4) . ?
O2 Tb2 2.324(4) 4_565 ?
O9 Tb1 2.354(3) 2_657 ?
O9 Tb1 2.341(3) . ?
O9 Tb2 2.329(4) 4_565 ?
O8 Tb1 2.333(2) . ?
O8 Tb1 2.333(2) 4_565 ?
O8 Tb2 2.333(4) . ?
O5 Tb2 2.328(4) 4_565 ?
O11 Tb1 2.345(6) . ?
O4 Tb1 2.330(4) . ?
O10 Tb1 2.335(2) . ?
O10 Tb1 2.335(2) 4_565 ?
O10 Tb2 2.335(4) 2_657 ?
O6 Tb1 2.343(4) . ?
Tb1 Tb1 3.9624(6) 2_657 ?
Tb1 Tb1 3.9200(8) 4_565 ?
Tb1 Tb2 3.9217(5) 3_667 ?
Tb1 Tb2 3.9056(5) 4_565 ?

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 C1 C2 116.7(7) . . ?
O2 C1 C2 116.7(7) . . ?
O2 C1 O1 126.6(6) . . ?
C3 C2 C1 121.3(7) . . ?
C7 C2 C1 120.5(7) . . ?
C7 C2 C3 118.2(6) . . ?
H3 C3 C2 119.9(4) . . ?
C4 C3 C2 120.3(8) . . ?
C4 C3 H3 119.9(6) . . ?
H4 C4 C3 119.5(6) . . ?
C5 C4 C3 121.1(9) . . ?
C5 C4 H4 119.5(5) . . ?
C6 C5 C4 119.1(7) . . ?
C8 C5 C4 124.2(9) . . ?
C8 C5 C6 116.7(8) . . ?
H6 C6 C5 119.9(4) . . ?
C7 C6 C5 120.3(8) . . ?
C7 C6 H6 119.9(6) . . ?
C6 C7 C2 121.1(9) . . ?
H7 C7 C2 119.5(5) . . ?
H7 C7 C6 119.5(6) . . ?
H8 C8 C5 109.2(6) . . ?
C9 C8 C5 109.3(5) . . ?
C9 C8 H8 109.2(6) . . ?
O3 C8 C5 109.9(8) . . ?
O3 C8 H8 109.2(6) . . ?
O3 C8 C9 110.1(8) . . ?
C10 C9 C8 122.4(8) . . ?
C14 C9 C8 118.5(8) . . ?
C14 C9 C10 119.0(6) . . ?
H10 C10 C9 119.0(4) . . ?
C11 C10 C9 121.9(8) . . ?
C11 C10 H10 119.0(6) . . ?
H11 C11 C10 120.5(6) . . ?
C12 C11 C10 119.0(8) . . ?
C12 C11 H11 120.5(4) . . ?
C13 C12 C11 120.4(6) . . ?
C15 C12 C11 121.0(7) . . ?
C15 C12 C13 118.6(7) . . ?
H13 C13 C12 120.3(4) . . ?
C14 C13 C12 119.4(9) . . ?
C14 C13 H13 120.3(6) . . ?
C13 C14 C9 120.2(9) . . ?
H14 C14 C9 119.9(5) . . ?
H14 C14 C13 119.9(6) . . ?
O5 C15 C12 117.1(6) 7_657 . ?
O4 C15 C12 117.5(6) 8 . ?
O4 C15 O5 125.3(5) 8 7_657 ?
O6 N1 O6 122.4(6) . 4_565 ?
O7 N1 O6 118.8(3) . 4_565 ?
O7 N1 O6 118.8(3) . . ?
Tb1 O1 C1 137.0(5) . . ?
Tb2 O2 C1 138.1(4) 4_565 . ?
Tb2 O9 Tb1 113.51(14) 4_565 . ?
Tb2 O9 Tb1 113.74(14) 4_565 2_657 ?
Tb1 O8 Tb1 114.28(17) 4_565 . ?
Tb2 O8 Tb1 113.63(11) . . ?
Tb2 O8 Tb1 113.63(11) . 4_565 ?
Tb2 O5 C15 137.8(4) 4_565 7_657 ?
Tb1 O4 C15 137.0(4) . 8_455 ?
Tb1 O10 Tb1 114.12(17) . 4_565 ?
Tb2 O10 Tb1 114.22(11) 2_657 4_565 ?
Tb2 O10 Tb1 114.22(11) 2_657 . ?
Tb1 O6 N1 138.9(4) . 4_565 ?
O9 Tb1 O1 76.86(14) . . ?
O9 Tb1 O1 138.03(14) 2_657 . ?
O8 Tb1 O1 77.07(17) 4_565 . ?
O8 Tb1 O9 65.61(13) 4_565 . ?
O8 Tb1 O9 99.10(15) 4_565 2_657 ?
O11 Tb1 O1 80.5(2) . . ?
O11 Tb1 O9 76.6(2) . . ?
O11 Tb1 O9 76.09(19) . 2_657 ?
O11 Tb1 O8 139.4(2) . 4_565 ?
O4 Tb1 O1 132.60(18) . . ?
O4 Tb1 O9 139.04(15) . . ?
O4 Tb1 O9 77.37(14) . 2_657 ?
O4 Tb1 O8 137.90(17) . 4_565 ?
O4 Tb1 O11 81.3(2) . . ?
O10 Tb1 O1 139.58(16) 4_565 . ?
O10 Tb1 O9 98.53(14) 4_565 . ?
O10 Tb1 O9 65.06(13) 4_565 2_657 ?
O10 Tb1 O8 64.99(13) 4_565 4_565 ?
O10 Tb1 O11 138.27(19) 4_565 . ?
O10 Tb1 O4 76.11(17) 4_565 . ?
O6 Tb1 O1 80.08(16) . . ?
O6 Tb1 O9 139.41(14) . . ?
O6 Tb1 O9 140.58(14) . 2_657 ?
O6 Tb1 O8 76.97(16) . 4_565 ?
O6 Tb1 O11 131.5(2) . . ?
O6 Tb1 O4 80.15(17) . . ?
O6 Tb1 O10 78.36(16) . 4_565 ?
Tb1 Tb1 O1 107.08(14) 4_565 . ?
Tb1 Tb1 O1 106.31(11) 2_657 . ?
Tb1 Tb1 O9 32.34(8) 2_657 2_657 ?
Tb1 Tb1 O9 85.63(9) 4_565 2_657 ?
Tb1 Tb1 O9 85.60(9) 4_565 . ?
Tb1 Tb1 O9 32.54(8) 2_657 . ?
Tb1 Tb1 O8 32.86(9) 4_565 4_565 ?
Tb1 Tb1 O8 85.76(11) 2_657 4_565 ?
Tb1 Tb1 O11 68.63(17) 2_657 . ?
Tb1 Tb1 O11 158.62(17) 4_565 . ?
Tb1 Tb1 O4 105.70(15) 4_565 . ?
Tb1 Tb1 O4 106.97(12) 2_657 . ?
Tb1 Tb1 O10 32.94(9) 4_565 4_565 ?
Tb1 Tb1 O10 85.02(11) 2_657 4_565 ?
Tb1 Tb1 O6 69.87(13) 4_565 . ?
Tb1 Tb1 O6 159.86(13) 2_657 . ?
Tb2 Tb1 O1 158.43(13) 3_667 . ?
Tb2 Tb1 O1 69.26(13) 4_565 . ?
Tb2 Tb1 O9 33.15(9) 4_565 . ?
Tb2 Tb1 O9 84.58(9) 3_667 . ?
Tb2 Tb1 O9 32.93(9) 3_667 2_657 ?
Tb2 Tb1 O9 84.79(8) 4_565 2_657 ?
Tb2 Tb1 O8 33.19(9) 4_565 4_565 ?
Tb2 Tb1 O8 85.36(10) 3_667 4_565 ?
Tb2 Tb1 O11 106.78(18) 4_565 . ?
Tb2 Tb1 O11 105.97(16) 3_667 . ?
Tb2 Tb1 O4 68.97(12) 3_667 . ?
Tb2 Tb1 O4 158.14(13) 4_565 . ?
Tb2 Tb1 O10 32.89(10) 3_667 4_565 ?
Tb2 Tb1 O10 85.00(10) 4_565 4_565 ?
Tb2 Tb1 O6 106.99(12) 4_565 . ?
Tb2 Tb1 O6 108.27(12) 3_667 . ?
O2 Tb2 O2 79.8(2) . 4_565 ?
O9 Tb2 O2 77.16(15) . . ?
O9 Tb2 O2 77.16(15) 4_565 4_565 ?
O9 Tb2 O2 139.31(14) 4_565 . ?
O9 Tb2 O2 139.31(14) . 4_565 ?
O9 Tb2 O9 99.73(18) . 4_565 ?
O8 Tb2 O2 76.50(14) . 4_565 ?
O8 Tb2 O2 76.50(14) . . ?
O8 Tb2 O9 65.80(10) . 4_565 ?
O8 Tb2 O9 65.80(10) . . ?
O5 Tb2 O2 81.58(17) . . ?
O5 Tb2 O2 131.28(17) 4_565 . ?
O5 Tb2 O2 81.58(17) 4_565 4_565 ?
O5 Tb2 O2 131.28(17) . 4_565 ?
O5 Tb2 O9 77.47(16) 4_565 4_565 ?
O5 Tb2 O9 138.09(14) 4_565 . ?
O5 Tb2 O9 77.47(16) . . ?
O5 Tb2 O9 138.09(14) . 4_565 ?
O5 Tb2 O8 140.41(14) 4_565 . ?
O5 Tb2 O8 140.41(14) . . ?
O5 Tb2 O5 77.9(3) 4_565 . ?
O10 Tb2 O2 139.56(13) 2_657 4_565 ?
O10 Tb2 O2 139.56(13) 2_657 . ?
O10 Tb2 O9 65.47(10) 2_657 . ?
O10 Tb2 O9 65.47(10) 2_657 4_565 ?
O10 Tb2 O8 100.42(16) 2_657 . ?
O10 Tb2 O5 75.95(14) 2_657 . ?
O10 Tb2 O5 75.95(14) 2_657 4_565 ?
Tb1 Tb2 O2 107.33(13) 3_667 4_565 ?
Tb1 Tb2 O2 69.06(11) . . ?
Tb1 Tb2 O2 106.63(11) 4_565 . ?
Tb1 Tb2 O2 159.87(12) 2_657 4_565 ?
Tb1 Tb2 O2 69.06(11) 4_565 4_565 ?
Tb1 Tb2 O2 159.87(12) 3_667 . ?
Tb1 Tb2 O2 107.33(13) 2_657 . ?
Tb1 Tb2 O2 106.63(11) . 4_565 ?
Tb1 Tb2 O9 86.10(8) . 4_565 ?
Tb1 Tb2 O9 86.10(8) 4_565 . ?
Tb1 Tb2 O9 33.35(8) 4_565 4_565 ?
Tb1 Tb2 O9 33.33(8) 3_667 4_565 ?
Tb1 Tb2 O9 85.91(9) 3_667 . ?
Tb1 Tb2 O9 33.33(8) 2_657 . ?
Tb1 Tb2 O9 33.35(8) . . ?
Tb1 Tb2 O9 85.91(9) 2_657 4_565 ?
Tb1 Tb2 O8 86.72(10) 3_667 . ?
Tb1 Tb2 O8 33.18(5) . . ?
Tb1 Tb2 O8 86.72(10) 2_657 . ?
Tb1 Tb2 O8 33.18(5) 4_565 . ?
Tb1 Tb2 O5 105.51(11) 3_667 . ?
Tb1 Tb2 O5 68.85(12) 3_667 4_565 ?
Tb1 Tb2 O5 159.63(12) 4_565 . ?
Tb1 Tb2 O5 107.85(14) 4_565 4_565 ?
Tb1 Tb2 O5 105.51(11) 2_657 4_565 ?
Tb1 Tb2 O5 107.85(14) . . ?
Tb1 Tb2 O5 159.63(12) . 4_565 ?
Tb1 Tb2 O5 68.85(12) 2_657 . ?
Tb1 Tb2 O10 32.90(4) 3_667 2_657 ?
Tb1 Tb2 O10 86.36(9) . 2_657 ?
Tb1 Tb2 O10 32.90(4) 2_657 2_657 ?
Tb1 Tb2 O10 86.36(9) 4_565 2_657 ?
Tb1 Tb2 Tb1 90.810(11) 4_565 2_657 ?
Tb1 Tb2 Tb1 60.244(12) 4_565 . ?
Tb1 Tb2 Tb1 59.972(12) 3_667 2_657 ?
Tb1 Tb2 Tb1 90.810(11) 3_667 . ?

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
C1 C2 C3 C4 178.9(8) . . . . ?
C1 C2 C7 C6 -177.6(8) . . . . ?
C2 C3 C4 C5 -1.2(11) . . . . ?
C2 C7 C6 C5 -1.6(11) . . . . ?
C3 C4 C5 C6 0.6(11) . . . . ?
C3 C4 C5 C8 -177.8(8) . . . . ?
C4 C5 C6 C7 0.8(10) . . . . ?
C4 C5 C8 C9 -115.0(10) . . . . ?
C4 C5 C8 O3 6.0(9) . . . . ?
C5 C8 C9 C10 60.8(11) . . . . ?
C5 C8 C9 C14 -116.8(9) . . . . ?
C8 C9 C10 C11 -179.8(8) . . . . ?
C8 C9 C14 C13 -179.1(8) . . . . ?
C9 C10 C11 C12 -0.1(11) . . . . ?
C9 C14 C13 C12 -2.0(11) . . . . ?
C10 C11 C12 C13 1.4(11) . . . . ?
C10 C11 C12 C15 179.7(8) . . . . ?
C11 C12 C13 C14 -0.4(9) . . . . ?
C11 C12 C15 O5 -9.5(8) . . . 7_657 ?
C11 C12 C15 O4 172.3(7) . . . 8 ?
C12 C15 O5 Tb2 163.0(4) . . 7_657 6_647 ?
C12 C15 O4 Tb1 -163.0(4) . . 8 8 ?

_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 -0.977 -0.656 -0.147 5265.0 1179.2 ?


_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 3.344
_oxdiff_exptl_absorpt_empirical_full_min 0.469
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O7 N1 1 1.3500 0.0010 -0.0013

loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
N1 O6 0.004000 0.001071 -0.000886 0.014165
N1 O7 0.004000 -0.004808 0.004823 -0.017002
O6 O7 0.004000 0.006802 0.018021 -0.043680

loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
N1 O6 0.0400
N1 O7 0.0800

####################################################################### 
# 
# 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_LK1_44_2
_database_code_depnum_ccdc_archive 'CCDC 2338722'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_chemical_formula_moiety         'C30 H18 Dy3 N O19'
_chemical_formula_sum            'C30 H18 Dy3 N1 O19'
_chemical_formula_weight         1183.964
_chemical_oxdiff_formula         'Dy O C H'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Dy -9.77090 9.87219 26.50700 17.63830 14.55960 2.96577 2.18020 0.20217 12.18990
111.87400 4.29728 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.03110 0.01806 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z

_symmetry_Int_Tables_number      12
_cell_length_a                   29.9207(7)
_cell_length_b                   18.2577(5)
_cell_length_c                   14.6257(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.432(2)
_cell_angle_gamma                90
_cell_volume                     7857.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9045
_cell_measurement_temperature    102(1)
_cell_measurement_theta_max      70.8150
_cell_measurement_theta_min      3.9830
_exptl_absorpt_coefficient_mu    15.362
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.001
_exptl_crystal_description       plate
_exptl_crystal_F_000             2118.815
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.9989
_diffrn_reflns_Laue_measured_fraction_max 0.9989
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27408
_diffrn_reflns_point_group_measured_fraction_full 0.9989
_diffrn_reflns_point_group_measured_fraction_max 0.9989
_diffrn_reflns_theta_full        66.9892
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.89
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     51.00  88.00   1.00    2.50    --    0.00  57.00 -30.00   37
  2  ω     15.00  43.00   1.00    2.50    --    0.00 -99.00-180.00   28
  3  ω    -65.00 -37.00   1.00    2.50    --    0.00 178.00  30.00   28
  4  ω      0.00  39.00   1.00    2.50    --    0.00  57.00 -30.00   39
  5  ω    -39.00  -9.00   1.00    2.50    --    0.00  57.00 -30.00   30
  6  ω   -136.00 -79.00   1.00    7.50    --  -54.44 -99.00-150.00   57
  7  ω   -144.00 -83.00   1.00    7.50    --  -54.44 -99.00  60.00   61
  8  ω   -117.00 -91.00   1.00    7.50    --  -54.44 -99.00  30.00   26
  9  ω    -96.00  33.00   1.00    7.50    --  -54.44  77.00  30.00  129
 10  ω     22.00 143.00   1.00    7.50    --   54.44  57.00 -90.00  121
 11  ω     94.00 121.00   1.00    7.50    --   54.44 125.00 -90.00   27
 12  ω     10.00 103.00   1.00    7.50    --   54.44 -99.00  90.00   93
 13  ω    101.00 170.00   1.00   35.00    --  108.88 111.00-180.00   69
 14  ω     26.00 108.00   1.00   35.00    --  108.88 -38.00  90.00   82
 15  ω     28.00 103.00   1.00   35.00    --  108.88 -92.00 -60.00   75
 16  ω    101.00 164.00   1.00   35.00    --  108.88 111.00 150.00   63
 17  ω     84.00 111.00   1.00   35.00    --  108.88-111.00-180.00   27
 18  ω     14.00 150.00   1.00   35.00    --  108.88 -77.00 120.00  136
 19  ω     84.00 178.00   1.00   35.00    --  108.88  38.00-120.00   94
 20  ω     25.00 112.00   1.00   35.00    --  108.88-111.00  30.00   87
 21  ω     40.00  81.00   1.00   35.00    --  108.88 -50.00 -90.00   41
 22  ω     65.00 101.00   1.00   35.00    --  108.88 -92.00-120.00   36
 23  ω     57.00 178.00   1.00   35.00    --  108.88  25.00 -30.00  121
 24  ω     85.00 112.00   1.00   35.00    --  108.88-111.00  60.00   27
 25  ω     30.00  96.00   1.00   35.00    --  108.88-111.00 120.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0259071000
_diffrn_orient_matrix_UB_12      0.0078803000
_diffrn_orient_matrix_UB_13      0.1006547000
_diffrn_orient_matrix_UB_21      0.0453615000
_diffrn_orient_matrix_UB_22      0.0017853000
_diffrn_orient_matrix_UB_23      -0.0357104000
_diffrn_orient_matrix_UB_31      -0.0033917000
_diffrn_orient_matrix_UB_32      0.0839685000
_diffrn_orient_matrix_UB_33      -0.0085932000
_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         0.0
_reflns_limit_h_max              35
_reflns_limit_h_min              -35
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5853
_reflns_number_total             7238
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.1403
_refine_diff_density_min         -0.9640
_refine_diff_density_rms         0.1085
_refine_ls_d_res_high            0.8376
_refine_ls_d_res_low             11.3654
_refine_ls_goodness_of_fit_ref   0.9836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     247
_refine_ls_number_reflns         7238
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      0.9820
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1079P)²+5.2306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1594
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O1-C1 = C8-O3
 1.43 with sigma of 0.02
 O6-N1
 1.35 with sigma of 0.001
3. Rigid bond restraints
 O6, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O7 \\sim O6 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
O6 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
5.a Ternary CH refined with riding coordinates:
 C8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C13(H13), C3(H3), C11(H11), C6(H6), C14(H14), C7(H7), C10(H10)
;
_atom_sites_solution_primary     iterative
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Dy2 Dy 0.410044(14) 0.5 0.01105(3) 0.06257(16) Uani 1.000000 2 S T P
Dy1 Dy 0.515728(10) 0.60681(2) 0.13654(2) 0.06194(14) Uani 1.000000 1 . . .
O4 O 0.13440(14) 0.9210(3) 0.0904(3) 0.0799(12) Uani 1.000000 1 . . .
O10 O 0.54133(11) 0.59845(18) -0.0049(2) 0.0505(7) Uani 1.000000 1 . . .
O3 O 0.3158(2) 0.8352(6) 0.4495(4) 0.178(4) Uani 1.000000 1 D . .
O8 O 0.47279(13) 0.5 0.1294(3) 0.0487(10) Uani 1.000000 2 S T P
O1 O 0.45127(14) 0.6444(3) 0.1909(3) 0.0760(11) Uani 1.000000 1 D . .
O9 O 0.55576(13) 0.5 0.1185(3) 0.0453(9) Uani 1.000000 2 S T P
O5 O 0.09163(14) 0.8586(3) 0.1774(3) 0.0806(12) Uani 1.000000 1 . . .
O11 O 0.5094(2) 0.7272(3) 0.0787(5) 0.1130(18) Uani 1.000000 1 . . .
O7 O 0.5525(3) 0.5 0.4435(9) 0.201(7) Uani 1.000000 2 S TU P
O2 O 0.38952(15) 0.5810(3) 0.1186(3) 0.0771(11) Uani 1.000000 1 . . .
O6 O 0.53308(13) 0.56491(19) 0.2877(2) 0.0716(10) Uani 1.000000 1 D U .
N1 N 0.5399(3) 0.5 0.3320(5) 0.088(2) Uani 1.000000 2 DS TU P
C12 C 0.1723(2) 0.8532(5) 0.2187(4) 0.0824(19) Uani 1.000000 1 . . .
C4 C 0.3661(3) 0.7679(6) 0.3308(6) 0.109(3) Uani 1.000000 1 . . .
H4 H 0.3762(3) 0.8119(6) 0.3628(6) 0.131(3) Uiso 1.000000 1 R . .
C15 C 0.1297(2) 0.8800(4) 0.1576(5) 0.0804(19) Uani 1.000000 1 . . .
C13 C 0.1694(3) 0.7988(6) 0.2821(5) 0.105(3) Uani 1.000000 1 . . .
H13 H 0.1408(3) 0.7785(6) 0.2880(5) 0.126(3) Uiso 1.000000 1 R . .
C3 C 0.3935(3) 0.7338(5) 0.2775(5) 0.097(2) Uani 1.000000 1 . . .
H3 H 0.4218(3) 0.7549(5) 0.2714(5) 0.116(3) Uiso 1.000000 1 R . .
C11 C 0.2138(2) 0.8830(5) 0.2113(6) 0.102(3) Uani 1.000000 1 . . .
H11 H 0.2158(2) 0.9202(5) 0.1669(6) 0.122(3) Uiso 1.000000 1 R . .
C6 C 0.3109(3) 0.6778(6) 0.2920(6) 0.116(3) Uani 1.000000 1 . . .
H6 H 0.2818(3) 0.6589(6) 0.2963(6) 0.139(4) Uiso 1.000000 1 R . .
C14 C 0.2102(3) 0.7732(7) 0.3391(5) 0.119(4) Uani 1.000000 1 . . .
H14 H 0.2092(3) 0.7342(7) 0.3816(5) 0.143(4) Uiso 1.000000 1 R . .
C7 C 0.3370(2) 0.6403(6) 0.2385(5) 0.101(3) Uani 1.000000 1 . . .
H7 H 0.3261(2) 0.5966(6) 0.2067(5) 0.121(3) Uiso 1.000000 1 R . .
C10 C 0.2521(3) 0.8581(6) 0.2691(6) 0.109(3) Uani 1.000000 1 . . .
H10 H 0.2808(3) 0.8787(6) 0.2646(6) 0.131(3) Uiso 1.000000 1 R . .
C2 C 0.3795(2) 0.6683(5) 0.2327(4) 0.083(2) Uani 1.000000 1 . . .
C9 C 0.2498(2) 0.8043(6) 0.3327(5) 0.107(3) Uani 1.000000 1 . . .
C8 C 0.2934(3) 0.7756(6) 0.3976(5) 0.124(4) Uani 1.000000 1 D . .
H8 H 0.2846(3) 0.7385(6) 0.4413(5) 0.148(5) Uiso 1.000000 1 R . .
C1 C 0.4081(2) 0.6266(4) 0.1751(4) 0.0797(19) Uani 1.000000 1 D . .
C5 C 0.3247(2) 0.7396(6) 0.3382(5) 0.099(3) Uani 1.000000 1 . . .


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
Dy2 Dy1 3.8818(5) . ?
Dy2 Dy1 3.8818(5) 4_565 ?
Dy2 Dy1 3.8899(5) 3_665 ?
Dy2 Dy1 3.8899(5) 2_655 ?
Dy2 O4 2.310(4) 7_565 ?
Dy2 O4 2.310(4) 6_545 ?
Dy2 O10 2.325(3) 3_665 ?
Dy2 O10 2.325(3) 2_655 ?
Dy2 O8 2.312(4) . ?
Dy2 O9 2.311(4) 2_655 ?
Dy2 O2 2.322(4) . ?
Dy2 O2 2.322(4) 4_565 ?
Dy1 Dy1 3.9340(6) 2_655 ?
Dy1 Dy1 3.9001(7) 4_565 ?
Dy1 O10 2.335(3) 2_655 ?
Dy1 O10 2.337(3) . ?
Dy1 O8 2.327(2) . ?
Dy1 O1 2.319(4) . ?
Dy1 O9 2.328(2) . ?
Dy1 O5 2.329(4) 8_565 ?
Dy1 O11 2.351(6) . ?
Dy1 O6 2.308(3) . ?
O4 C15 1.263(9) . ?
O3 C8 1.424(11) . ?
O1 C1 1.312(8) . ?
O5 C15 1.287(9) . ?
O7 N1 1.606(13) . ?
O2 C1 1.232(9) . ?
O6 N1 1.3481(10) . ?
C12 C15 1.500(8) . ?
C12 C13 1.371(11) . ?
C12 C11 1.378(11) . ?
C4 H4 0.9500 . ?
C4 C3 1.378(10) . ?
C4 C5 1.365(13) . ?
C13 H13 0.9500 . ?
C13 C14 1.426(9) . ?
C3 H3 0.9500 . ?
C3 C2 1.390(11) . ?
C11 H11 0.9500 . ?
C11 C10 1.374(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(10) . ?
C6 C5 1.340(14) . ?
C14 H14 0.9500 . ?
C14 C9 1.332(14) . ?
C7 H7 0.9500 . ?
C7 C2 1.389(11) . ?
C10 H10 0.9500 . ?
C10 C9 1.363(13) . ?
C2 C1 1.510(8) . ?
C9 C8 1.557(9) . ?
C8 H8 1.0000 . ?
C8 C5 1.536(9) . ?

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
Dy1 Dy2 Dy1 60.312(12) 4_565 . ?
Dy1 Dy2 Dy1 90.925(11) 4_565 2_655 ?
Dy1 Dy2 Dy1 90.925(11) 3_665 . ?
Dy1 Dy2 Dy1 60.174(12) 3_665 2_655 ?
O4 Dy2 Dy1 160.45(11) 7_565 4_565 ?
O4 Dy2 Dy1 69.56(11) 6_545 3_665 ?
O4 Dy2 Dy1 69.56(11) 7_565 2_655 ?
O4 Dy2 Dy1 108.35(13) 6_545 4_565 ?
O4 Dy2 Dy1 160.45(11) 6_545 . ?
O4 Dy2 Dy1 108.35(13) 7_565 . ?
O4 Dy2 Dy1 106.08(11) 6_545 2_655 ?
O4 Dy2 Dy1 106.08(11) 7_565 3_665 ?
O4 Dy2 O4 77.3(3) 7_565 6_545 ?
O10 Dy2 Dy1 33.55(7) 3_665 3_665 ?
O10 Dy2 Dy1 33.55(7) 2_655 2_655 ?
O10 Dy2 Dy1 86.67(8) 2_655 3_665 ?
O10 Dy2 Dy1 86.67(8) 3_665 2_655 ?
O10 Dy2 Dy1 33.68(8) 3_665 4_565 ?
O10 Dy2 Dy1 86.84(8) 3_665 . ?
O10 Dy2 Dy1 33.68(8) 2_655 . ?
O10 Dy2 Dy1 86.84(8) 2_655 4_565 ?
O10 Dy2 O4 77.51(15) 3_665 6_545 ?
O10 Dy2 O4 138.56(13) 2_655 6_545 ?
O10 Dy2 O4 77.51(15) 2_655 7_565 ?
O10 Dy2 O4 138.56(13) 3_665 7_565 ?
O10 Dy2 O10 101.30(16) 3_665 2_655 ?
O8 Dy2 Dy1 33.32(4) . . ?
O8 Dy2 Dy1 33.32(4) . 4_565 ?
O8 Dy2 Dy1 87.01(9) . 2_655 ?
O8 Dy2 Dy1 87.01(9) . 3_665 ?
O8 Dy2 O4 140.89(13) . 6_545 ?
O8 Dy2 O4 140.89(13) . 7_565 ?
O8 Dy2 O10 66.42(10) . 2_655 ?
O8 Dy2 O10 66.42(10) . 3_665 ?
O9 Dy2 Dy1 86.79(8) 2_655 . ?
O9 Dy2 Dy1 86.79(8) 2_655 4_565 ?
O9 Dy2 Dy1 33.16(4) 2_655 2_655 ?
O9 Dy2 Dy1 33.16(4) 2_655 3_665 ?
O9 Dy2 O4 76.25(13) 2_655 6_545 ?
O9 Dy2 O4 76.25(13) 2_655 7_565 ?
O9 Dy2 O10 66.11(9) 2_655 2_655 ?
O9 Dy2 O10 66.11(9) 2_655 3_665 ?
O9 Dy2 O8 101.19(14) 2_655 . ?
O2 Dy2 Dy1 107.00(11) . 4_565 ?
O2 Dy2 Dy1 107.71(12) 4_565 3_665 ?
O2 Dy2 Dy1 160.58(12) . 3_665 ?
O2 Dy2 Dy1 107.00(11) 4_565 . ?
O2 Dy2 Dy1 107.71(12) . 2_655 ?
O2 Dy2 Dy1 69.65(12) . . ?
O2 Dy2 Dy1 69.65(12) 4_565 4_565 ?
O2 Dy2 Dy1 160.58(12) 4_565 2_655 ?
O2 Dy2 O4 129.86(16) . 6_545 ?
O2 Dy2 O4 81.09(16) . 7_565 ?
O2 Dy2 O4 129.86(16) 4_565 7_565 ?
O2 Dy2 O4 81.09(16) 4_565 6_545 ?
O2 Dy2 O10 77.16(15) 4_565 3_665 ?
O2 Dy2 O10 139.74(14) 4_565 2_655 ?
O2 Dy2 O10 77.16(15) . 2_655 ?
O2 Dy2 O10 139.74(14) . 3_665 ?
O2 Dy2 O8 76.77(13) . . ?
O2 Dy2 O8 76.77(13) 4_565 . ?
O2 Dy2 O9 140.03(12) 4_565 2_655 ?
O2 Dy2 O9 140.03(12) . 2_655 ?
O2 Dy2 O2 79.2(2) 4_565 . ?
Dy1 Dy1 Dy2 59.913(6) 4_565 2_655 ?
Dy1 Dy1 Dy2 59.844(6) 4_565 . ?
Dy1 Dy1 Dy2 59.691(9) 2_655 . ?
Dy1 Dy1 Dy2 59.488(9) 2_655 2_655 ?
O10 Dy1 Dy2 85.15(8) 2_655 2_655 ?
O10 Dy1 Dy2 33.34(8) . 2_655 ?
O10 Dy1 Dy2 33.50(8) 2_655 . ?
O10 Dy1 Dy2 85.31(8) . . ?
O8 Dy1 Dy2 33.08(9) . . ?
O8 Dy1 Dy2 85.48(9) . 2_655 ?
O8 Dy1 O10 99.94(13) . . ?
O8 Dy1 O10 66.00(13) . 2_655 ?
O1 Dy1 Dy2 69.76(11) . . ?
O1 Dy1 Dy2 158.83(11) . 2_655 ?
O1 Dy1 O10 138.51(13) . . ?
O1 Dy1 O10 76.88(13) . 2_655 ?
O1 Dy1 O8 77.09(15) . . ?
O9 Dy1 Dy2 85.27(9) . . ?
O9 Dy1 Dy2 32.88(9) . 2_655 ?
O9 Dy1 O10 65.63(12) . . ?
O9 Dy1 O10 99.57(13) . 2_655 ?
O9 Dy1 O8 65.44(12) . . ?
O9 Dy1 O1 139.77(15) . . ?
O5 Dy1 Dy2 158.57(12) 8_565 . ?
O5 Dy1 Dy2 69.54(12) 8_565 2_655 ?
O5 Dy1 O10 77.55(14) 8_565 . ?
O5 Dy1 O10 139.71(14) 8_565 2_655 ?
O5 Dy1 O8 138.05(15) 8_565 . ?
O5 Dy1 O1 131.63(17) 8_565 . ?
O5 Dy1 O9 76.04(16) 8_565 . ?
O11 Dy1 Dy2 107.10(17) . . ?
O11 Dy1 Dy2 106.64(15) . 2_655 ?
O11 Dy1 O10 76.16(18) . . ?
O11 Dy1 O10 76.43(19) . 2_655 ?
O11 Dy1 O8 139.44(19) . . ?
O11 Dy1 O1 80.1(2) . . ?
O11 Dy1 O9 138.79(18) . . ?
O11 Dy1 O5 81.4(2) . 8_565 ?
O6 Dy1 Dy2 108.01(10) . . ?
O6 Dy1 Dy2 108.27(10) . 2_655 ?
O6 Dy1 O10 140.65(13) . . ?
O6 Dy1 O10 140.55(13) . 2_655 ?
O6 Dy1 O8 77.98(14) . . ?
O6 Dy1 O1 80.00(15) . . ?
O6 Dy1 O9 78.45(13) . . ?
O6 Dy1 O5 78.70(15) . 8_565 ?
O6 Dy1 O11 130.08(19) . . ?
C15 O4 Dy2 137.5(4) . 7_565 ?
Dy1 O10 Dy2 113.11(13) . 2_655 ?
Dy1 O10 Dy2 112.82(13) 2_655 2_655 ?
Dy1 O8 Dy2 113.60(11) . . ?
Dy1 O8 Dy2 113.60(11) 4_565 . ?
Dy1 O8 Dy1 113.85(16) 4_565 . ?
C1 O1 Dy1 136.1(4) . . ?
Dy1 O9 Dy2 113.96(10) . 2_655 ?
Dy1 O9 Dy2 113.96(10) 4_565 2_655 ?
Dy1 O9 Dy1 113.76(16) 4_565 . ?
C15 O5 Dy1 136.2(4) . 8_465 ?
C1 O2 Dy2 138.0(4) . . ?
N1 O6 Dy1 137.7(4) . . ?
O6 N1 O7 118.3(3) . . ?
O6 N1 O7 118.3(3) 4_565 . ?
O6 N1 O6 123.1(6) 4_565 . ?
C13 C12 C15 119.4(7) . . ?
C11 C12 C15 120.2(7) . . ?
C11 C12 C13 120.4(7) . . ?
C3 C4 H4 119.5(6) . . ?
C5 C4 H4 119.5(5) . . ?
C5 C4 C3 121.0(9) . . ?
O5 C15 O4 125.7(5) . . ?
C12 C15 O4 117.1(6) . . ?
C12 C15 O5 117.2(7) . . ?
H13 C13 C12 120.6(4) . . ?
C14 C13 C12 118.7(8) . . ?
C14 C13 H13 120.6(6) . . ?
H3 C3 C4 120.1(6) . . ?
C2 C3 C4 119.8(9) . . ?
C2 C3 H3 120.1(4) . . ?
H11 C11 C12 120.5(5) . . ?
C10 C11 C12 119.0(9) . . ?
C10 C11 H11 120.5(6) . . ?
C7 C6 H6 118.3(6) . . ?
C5 C6 H6 118.3(5) . . ?
C5 C6 C7 123.3(9) . . ?
H14 C14 C13 120.1(6) . . ?
C9 C14 C13 119.9(9) . . ?
C9 C14 H14 120.1(5) . . ?
H7 C7 C6 121.0(6) . . ?
C2 C7 C6 118.0(9) . . ?
C2 C7 H7 121.0(5) . . ?
H10 C10 C11 119.4(6) . . ?
C9 C10 C11 121.3(9) . . ?
C9 C10 H10 119.4(5) . . ?
C7 C2 C3 119.2(7) . . ?
C1 C2 C3 123.0(7) . . ?
C1 C2 C7 117.7(8) . . ?
C10 C9 C14 120.6(7) . . ?
C8 C9 C14 118.1(9) . . ?
C8 C9 C10 121.2(8) . . ?
C9 C8 O3 109.2(8) . . ?
H8 C8 O3 109.3(5) . . ?
H8 C8 C9 109.3(6) . . ?
C5 C8 O3 110.6(8) . . ?
C5 C8 C9 109.2(5) . . ?
C5 C8 H8 109.3(6) . . ?
O2 C1 O1 126.5(6) . . ?
C2 C1 O1 114.5(7) . . ?
C2 C1 O2 118.9(6) . . ?
C6 C5 C4 118.6(7) . . ?
C8 C5 C4 122.5(9) . . ?
C8 C5 C6 118.9(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
Dy2 O4 C15 O5 16.6(7) 6 . . . ?
Dy2 O4 C15 O5 16.6(7) 7_565 . . . ?
Dy2 O4 C15 C12 -164.4(7) 7_565 . . . ?
Dy2 O4 C15 C12 -164.4(7) 6 . . . ?
Dy2 O2 C1 O1 0.7(7) . . . . ?
Dy2 O2 C1 O1 0.7(7) 4_565 . . . ?
Dy2 O2 C1 C2 179.9(7) . . . . ?
Dy2 O2 C1 C2 179.9(7) 4_565 . . . ?
Dy1 O1 C1 O2 -2.1(6) . . . . ?
Dy1 O1 C1 C2 178.7(6) . . . . ?
Dy1 O5 C15 O4 -15.7(6) 8_465 . . . ?
Dy1 O5 C15 C12 165.2(6) 8_465 . . . ?
Dy1 O6 N1 O7 179.0(7) . . . . ?
Dy1 O6 N1 O6 -6.6(3) . . . 4_565 ?
O4 C15 C12 C13 -168.6(7) . . . . ?
O4 C15 C12 C11 11.5(8) . . . . ?
O3 C8 C9 C14 -124.5(8) . . . . ?
O3 C8 C9 C10 57.5(8) . . . . ?
O3 C8 C5 C4 -6.7(9) . . . . ?
O3 C8 C5 C6 173.2(7) . . . . ?
O1 C1 C2 C3 18.4(7) . . . . ?
O1 C1 C2 C7 -163.4(6) . . . . ?
O5 C15 C12 C13 10.5(8) . . . . ?
O5 C15 C12 C11 -169.4(7) . . . . ?
O2 C1 C2 C3 -161.0(7) . . . . ?
O2 C1 C2 C7 17.2(8) . . . . ?
C12 C13 C14 C9 2.7(10) . . . . ?
C12 C11 C10 C9 0.5(10) . . . . ?
C4 C3 C2 C7 3.3(10) . . . . ?
C4 C3 C2 C1 -178.5(7) . . . . ?
C4 C5 C6 C7 1.4(9) . . . . ?
C4 C5 C8 C9 113.6(9) . . . . ?
C13 C14 C9 C10 -3.1(11) . . . . ?
C13 C14 C9 C8 178.9(8) . . . . ?
C3 C2 C7 C6 -2.4(8) . . . . ?
C11 C10 C9 C14 1.5(12) . . . . ?
C11 C10 C9 C8 179.4(8) . . . . ?
C6 C7 C2 C1 179.3(7) . . . . ?
C6 C5 C8 C9 -66.6(9) . . . . ?
C14 C9 C8 C5 114.4(9) . . . . ?
C10 C9 C8 C5 -63.6(10) . . . . ?

_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 -0.080 -0.519 -0.924 5196.6 1062.8 ?

_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 1.986
_oxdiff_exptl_absorpt_empirical_full_min 0.502
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O1 C1 1 1.4300 0.0200 0.1177
O6 N1 1 1.3500 0.0010 0.0019
C8 O3 1 1.4300 0.0200 0.0062

loop_
_restr_U_rigid_atom_site_label_1
_restr_U_rigid_atom_site_label_2
_restr_U_rigid_target_weight_param
_restr_U_rigid_U_parallel
_restr_U_rigid_diff
O6 N1 0.0100 0.1144 -0.0309

loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
O7 N1 0.0800
O6 N1 0.0400
O6 N1 0.0400

####################################################################### 
# 
# 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_lk3_23_5abscorr
_database_code_depnum_ccdc_archive 'CCDC 2338725'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H41 N O36 Tb6'
_chemical_formula_sum            'C68 H41 N O36 Tb6'
_chemical_formula_weight         2401.54
_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'
N N 0.0311 0.0180 '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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   29.6087(13)
_cell_length_b                   18.6162(10)
_cell_length_c                   14.9895(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.990(4)
_cell_angle_gamma                90
_cell_volume                     8137.0(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5692
_cell_measurement_temperature    99.98(16)
_cell_measurement_theta_max      75.3160
_cell_measurement_theta_min      4.2520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.915
_exptl_absorpt_correction_T_max  0.251
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2268
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -3 9 0.0452
-2 3 -9 0.0579
-17 -6 2 0.2310
10 -10 -2 0.1348
-11 10 3 0.1371
15 7 0 0.1332

_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.107
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17541
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.995
_diffrn_reflns_theta_max         66.995
_diffrn_reflns_theta_min         3.874
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -81.00 -42.00   1.00   10.00    --  -38.92 125.00   0.00   39
  2  ω    -99.00 -10.00   1.00   10.00    --  -38.92 -57.00-120.00   89
  3  ω    -54.00 -16.00   1.00   10.00    --  -38.92 125.00  90.00   38
  4  ω    -70.00  37.00   1.00   10.00    --  -38.92  57.00  60.00  107
  5  ω     26.00  60.00   1.00   10.00    --   38.92 -99.00-180.00   34
  6  ω     31.00  93.00   1.00   10.00    --   38.92-125.00 120.00   62
  7  ω    105.00 177.00   1.00   45.00    --  116.00 111.00 -30.00   72
  8  ω     35.00  99.00   1.00   45.00    --  116.00 -94.00 -90.00   64
  9  ω    144.00 170.00   1.00   45.00    --  116.00  77.00 120.00   26
 10  ω    132.00 177.00   1.00   45.00    --  116.00  30.00 150.00   45
 11  ω    110.00 147.00   1.00   45.00    --  116.00 -61.00-120.00   37
 12  ω     99.00 131.00   1.00   45.00    --  116.00  30.00 150.00   32
 13  ω     78.00 135.00   1.00   45.00    --  116.00 178.00 -90.00   57
 14  ω     46.00  87.00   1.00   45.00    --  116.00-111.00   0.00   41
 15  ω    120.00 175.00   1.00   45.00    --  116.00  77.00 -90.00   55
 16  ω     55.00 102.00   1.00   45.00    --  116.00 -61.00-120.00   47
 17  ω     90.00 178.00   1.00   45.00    --  116.00  61.00 -60.00   88
 18  ω    102.00 174.00   1.00   45.00    --  116.00  45.00  30.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4829
_reflns_number_total             7448
_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 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         3.323
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         7448
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0903
_refine_ls_restrained_S_all      0.956
_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)+(0.1684P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2392
_refine_ls_wR_factor_ref         0.2502
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C18-N1
 1.35 with sigma of 0.005
 C8-O3A
 1.4 with sigma of 0.005
 C8-O3B
 1.4 with sigma of 0.005
3. Restrained planarity
 C16, C17, C18, H18, N1
 with sigma of 0.1
4. Rigid bond restraints
 N1, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C1 \\sim C7 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C8 \\sim C14
\\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim O3A \\sim O3B \\sim O4: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
6. Others
 Sof(H8B)=Sof(O3A)=1-FVAR(1)
 Sof(H8A)=Sof(O3B)=FVAR(1)
 Fixed Sof: H18(0.75) N1(0.25) H1A(0.25) H1B(0.25)
7.a Ternary CH refined with riding coordinates:
 C8(H8A), C8(H8B)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4(H4), C6(H6), C14(H14), C10(H10), C11(H11), C13(H13),
 C18(H18)
7.c Fitted hexagon refined as free rotating group:
 C7(C2,C3,C4,C5,C6), C14(C9,C10,C11,C12,C13)
7.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_atom_sites_solution_hydrogens   geom
_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
C1 C 0.6281(6) 0.6207(13) 0.6650(10) 0.157(5) Uani 1 1 d . U . . .
C7 C 0.7133(4) 0.6243(6) 0.7184(7) 0.173(5) Uani 1 1 d G U . . .
H7 H 0.717629 0.585597 0.679508 0.208 Uiso 1 1 calc R U . . .
C2 C 0.6694(3) 0.6507(7) 0.7191(6) 0.165(4) Uani 1 1 d G U . . .
C3 C 0.6630(3) 0.7074(7) 0.7760(8) 0.174(5) Uani 1 1 d G U . . .
H3 H 0.633032 0.725454 0.776445 0.208 Uiso 1 1 calc R U . . .
C4 C 0.7004(4) 0.7376(6) 0.8323(7) 0.180(5) Uani 1 1 d G U . . .
H4 H 0.696059 0.776289 0.871194 0.216 Uiso 1 1 calc R U . . .
C5 C 0.7443(3) 0.7111(7) 0.8316(6) 0.175(4) Uani 1 1 d G U . . .
C6 C 0.7507(3) 0.6545(7) 0.7747(8) 0.179(5) Uani 1 1 d G U . . .
H6 H 0.780656 0.636433 0.774259 0.215 Uiso 1 1 calc R U . . .
C8 C 0.7858(6) 0.7461(13) 0.8922(11) 0.181(4) Uani 1 1 d D U . . .
H8A H 0.802221 0.709773 0.935127 0.217 Uiso 0.39(2) 1 calc R U P A 1
H8B H 0.774956 0.784486 0.930159 0.217 Uiso 0.61(2) 1 calc R U P A 2
O3B O 0.7701(9) 0.8027(14) 0.9406(15) 0.178(9) Uani 0.39(2) 1 d D U P A 1
C14 C 0.8635(4) 0.7550(6) 0.8391(7) 0.178(4) Uani 1 1 d G U . . .
H14 H 0.875115 0.717549 0.879736 0.213 Uiso 1 1 calc R U . . .
C9 C 0.8186(4) 0.7785(7) 0.8346(7) 0.177(4) Uani 1 1 d G U . . .
C10 C 0.8015(3) 0.8333(7) 0.7752(8) 0.180(4) Uani 1 1 d G U . . .
H10 H 0.770843 0.849358 0.772127 0.216 Uiso 1 1 calc R U . . .
C11 C 0.8294(4) 0.8645(6) 0.7203(7) 0.169(4) Uani 1 1 d G U . . .
H11 H 0.817728 0.901987 0.679661 0.203 Uiso 1 1 calc R U . . .
C12 C 0.8743(3) 0.8410(7) 0.7248(6) 0.149(4) Uani 1 1 d G U . . .
C13 C 0.8913(3) 0.7863(7) 0.7842(7) 0.162(4) Uani 1 1 d G U . . .
H13 H 0.922000 0.770180 0.787269 0.195 Uiso 1 1 calc R U . . .
C15 C 0.9051(6) 0.8768(10) 0.6675(9) 0.128(3) Uani 1 1 d . U . . .
C16 C 0.5210(6) 0.500000 0.8196(9) 0.084(3) Uani 1 2 d S TU P . .
C17 C 0.5102(6) 0.500000 0.9126(9) 0.088(3) Uani 1 2 d S TU P C .
C18 C 0.5056(5) 0.5621(7) 0.9573(7) 0.094(3) Uani 1 1 d D U . . .
H18 H 0.510296 0.606525 0.929174 0.113 Uiso 0.75 1 calc R U P B 1
N1 N 0.5112(19) 0.6278(15) 0.923(4) 0.18(3) Uani 0.25 1 d D U P C 2
H1A H 0.518130 0.631948 0.868153 0.211 Uiso 0.25 1 calc R U P C 2
H1B H 0.507811 0.666497 0.954593 0.211 Uiso 0.25 1 calc R U P C 2
O8 O 0.5428(2) 0.4033(3) 0.4993(3) 0.0592(13) Uani 1 1 d . . . . .
O9 O 0.5303(3) 0.500000 0.3768(4) 0.0529(17) Uani 1 2 d S T P . .
O6 O 0.5237(2) 0.5607(4) 0.7811(4) 0.0715(16) Uani 1 1 d . . . . .
O10 O 0.5065(4) 0.7245(5) 0.5720(8) 0.143(4) Uani 1 1 d . . . . .
O1 O 0.5888(3) 0.6400(6) 0.6806(6) 0.116(3) Uani 1 1 d . . . . .
O2 O 0.6368(3) 0.5809(5) 0.5991(6) 0.106(3) Uani 1 1 d . . . . .
O4 O 0.8832(4) 0.9215(6) 0.6056(6) 0.113(3) Uani 1 1 d . U . . .
O5 O 0.9451(3) 0.8588(5) 0.6830(6) 0.101(3) Uani 1 1 d . . . . .
O7 O 0.5536(3) 0.500000 0.6207(5) 0.0566(18) Uani 1 2 d S T P . .
Tb2 Tb 0.59237(3) 0.500000 0.49740(5) 0.0730(3) Uani 1 2 d S T P . .
Tb1 Tb 0.51257(2) 0.60547(3) 0.63352(3) 0.0712(2) Uani 1 1 d . . . . .
O3A O 0.8086(7) 0.6924(13) 0.9483(12) 0.197(8) Uani 0.61(2) 1 d D U 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
C1 C2 1.455(15) . ?
C1 O1 1.28(2) . ?
C1 O2 1.30(2) . ?
C7 H7 0.9500 . ?
C7 C2 1.3900 . ?
C7 C6 1.3900 . ?
C2 C3 1.3900 . ?
C3 H3 0.9500 . ?
C3 C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C5 C8 1.539(18) . ?
C6 H6 0.9500 . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C8 O3B 1.403(5) . ?
C8 C9 1.531(16) . ?
C8 O3A 1.401(5) . ?
C14 H14 0.9500 . ?
C14 C9 1.3900 . ?
C14 C13 1.3900 . ?
C9 C10 1.3900 . ?
C10 H10 0.9500 . ?
C10 C11 1.3900 . ?
C11 H11 0.9500 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C15 1.512(13) . ?
C13 H13 0.9500 . ?
C15 O4 1.33(2) . ?
C15 O5 1.21(2) . ?
C16 C17 1.484(17) . ?
C16 O6 1.277(8) 6_565 ?
C16 O6 1.277(8) . ?
C17 C18 1.354(13) . ?
C17 C18 1.354(13) 6_565 ?
C18 C18 1.378(19) 2_657 ?
C18 H18 0.9500 . ?
C18 N1 1.351(5) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
O8 Tb2 2.326(6) . ?
O8 Tb1 2.345(5) 6_565 ?
O8 Tb1 2.355(6) 5_666 ?
O9 Tb2 2.343(7) . ?
O9 Tb1 2.329(4) 5_666 ?
O9 Tb1 2.329(4) 2_656 ?
O6 Tb1 2.333(6) . ?
O10 Tb1 2.394(9) . ?
O1 Tb1 2.336(7) . ?
O2 Tb2 2.372(8) . ?
O4 Tb2 2.331(8) 7_666 ?
O5 Tb1 2.343(7) 8_565 ?
O7 Tb2 2.339(7) . ?
O7 Tb1 2.334(4) . ?
O7 Tb1 2.334(4) 6_565 ?
Tb2 Tb1 3.9045(10) 5_666 ?
Tb2 Tb1 3.9080(8) 6_565 ?
Tb2 Tb1 3.9081(8) . ?
Tb2 Tb1 3.9045(10) 2_656 ?
Tb1 Tb1 3.9268(13) 6_565 ?
Tb1 Tb1 3.9425(10) 2_656 ?

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 C1 C2 119.6(17) . . ?
O1 C1 O2 127.4(13) . . ?
O2 C1 C2 112.7(15) . . ?
C2 C7 H7 120.0 . . ?
C2 C7 C6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C2 C1 123.7(13) . . ?
C7 C2 C3 120.0 . . ?
C3 C2 C1 116.2(13) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C8 119.8(12) . . ?
C6 C5 C8 120.2(12) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C8 H8A 110.1 . . ?
C5 C8 H8B 109.6 . . ?
O3B C8 C5 108.7(18) . . ?
O3B C8 H8A 110.1 . . ?
O3B C8 C9 107.2(15) . . ?
C9 C8 C5 110.7(12) . . ?
C9 C8 H8A 110.1 . . ?
C9 C8 H8B 109.6 . . ?
O3A C8 C5 107.7(16) . . ?
O3A C8 H8B 109.6 . . ?
O3A C8 C9 109.4(15) . . ?
C9 C14 H14 120.0 . . ?
C9 C14 C13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C9 C8 122.9(12) . . ?
C10 C9 C8 117.1(12) . . ?
C10 C9 C14 120.0 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C15 120.0(11) . . ?
C13 C12 C11 120.0 . . ?
C13 C12 C15 119.9(11) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
O4 C15 C12 113.7(14) . . ?
O5 C15 C12 115.8(15) . . ?
O5 C15 O4 130.5(12) . . ?
O6 C16 C17 117.7(6) . . ?
O6 C16 C17 117.7(6) 6_565 . ?
O6 C16 O6 124.3(11) 6_565 . ?
C18 C17 C16 121.4(6) 6_565 . ?
C18 C17 C16 121.4(6) . . ?
C18 C17 C18 117.2(13) . 6_565 ?
C17 C18 C18 121.4(6) . 2_657 ?
C17 C18 H18 119.3 . . ?
C18 C18 H18 119.3 2_657 . ?
N1 C18 C17 124(3) . . ?
C18 N1 H1A 120.0 . . ?
C18 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
Tb2 O8 Tb1 113.6(2) . 6_565 ?
Tb2 O8 Tb1 113.0(2) . 5_666 ?
Tb1 O8 Tb1 114.0(2) 6_565 5_666 ?
Tb1 O9 Tb2 113.39(17) 5_666 . ?
Tb1 O9 Tb2 113.39(17) 2_656 . ?
Tb1 O9 Tb1 114.9(3) 5_666 2_656 ?
C16 O6 Tb1 137.2(7) . . ?
C1 O1 Tb1 136.9(11) . . ?
C1 O2 Tb2 133.8(9) . . ?
C15 O4 Tb2 133.2(9) . 7_666 ?
C15 O5 Tb1 135.9(10) . 8_565 ?
Tb1 O7 Tb2 113.51(18) . . ?
Tb1 O7 Tb2 113.51(18) 6_565 . ?
Tb1 O7 Tb1 114.6(3) 6_565 . ?
O8 Tb2 O8 101.4(3) . 6_565 ?
O8 Tb2 O9 66.26(16) 6_565 . ?
O8 Tb2 O9 66.26(16) . . ?
O8 Tb2 O2 77.4(3) . 6_565 ?
O8 Tb2 O2 139.8(2) . . ?
O8 Tb2 O2 77.4(3) 6_565 . ?
O8 Tb2 O2 139.8(2) 6_565 6_565 ?
O8 Tb2 O4 78.0(3) . 4_646 ?
O8 Tb2 O4 139.7(3) . 7_666 ?
O8 Tb2 O4 78.0(3) 6_565 7_666 ?
O8 Tb2 O4 139.7(3) 6_565 4_646 ?
O8 Tb2 O7 65.97(16) 6_565 . ?
O8 Tb2 O7 65.97(16) . . ?
O8 Tb2 Tb1 33.37(12) 6_565 . ?
O8 Tb2 Tb1 33.70(14) . 5_666 ?
O8 Tb2 Tb1 86.70(14) 6_565 6_565 ?
O8 Tb2 Tb1 33.37(12) . 6_565 ?
O8 Tb2 Tb1 86.93(15) . 2_656 ?
O8 Tb2 Tb1 33.71(14) 6_565 2_656 ?
O8 Tb2 Tb1 86.70(14) . . ?
O8 Tb2 Tb1 86.93(15) 6_565 5_666 ?
O9 Tb2 O2 140.3(3) . . ?
O9 Tb2 O2 140.3(3) . 6_565 ?
O9 Tb2 Tb1 33.20(6) . 2_656 ?
O9 Tb2 Tb1 33.20(6) . 5_666 ?
O9 Tb2 Tb1 86.49(14) . . ?
O9 Tb2 Tb1 86.49(14) . 6_565 ?
O2 Tb2 O2 78.8(5) 6_565 . ?
O2 Tb2 Tb1 107.5(2) 6_565 . ?
O2 Tb2 Tb1 108.0(3) . 2_656 ?
O2 Tb2 Tb1 108.0(3) 6_565 5_666 ?
O2 Tb2 Tb1 161.2(2) 6_565 2_656 ?
O2 Tb2 Tb1 70.3(2) 6_565 6_565 ?
O2 Tb2 Tb1 70.3(2) . . ?
O2 Tb2 Tb1 161.2(2) . 5_666 ?
O2 Tb2 Tb1 107.5(2) . 6_565 ?
O4 Tb2 O9 77.4(3) 4_646 . ?
O4 Tb2 O9 77.4(3) 7_666 . ?
O4 Tb2 O2 128.5(4) 7_666 6_565 ?
O4 Tb2 O2 80.0(3) 7_666 . ?
O4 Tb2 O2 128.5(4) 4_646 . ?
O4 Tb2 O2 80.0(3) 4_646 6_565 ?
O4 Tb2 O4 77.7(5) 4_646 7_666 ?
O4 Tb2 O7 140.8(3) 4_646 . ?
O4 Tb2 O7 140.8(2) 7_666 . ?
O4 Tb2 Tb1 108.4(3) 4_646 6_565 ?
O4 Tb2 Tb1 161.1(3) 7_666 6_565 ?
O4 Tb2 Tb1 70.3(3) 7_666 2_656 ?
O4 Tb2 Tb1 107.1(2) 4_646 2_656 ?
O4 Tb2 Tb1 70.3(3) 4_646 5_666 ?
O4 Tb2 Tb1 161.1(3) 4_646 . ?
O4 Tb2 Tb1 108.4(3) 7_666 . ?
O4 Tb2 Tb1 107.1(2) 7_666 5_666 ?
O7 Tb2 O9 100.5(3) . . ?
O7 Tb2 O2 77.6(3) . 6_565 ?
O7 Tb2 O2 77.6(3) . . ?
O7 Tb2 Tb1 33.20(8) . 6_565 ?
O7 Tb2 Tb1 86.55(16) . 2_656 ?
O7 Tb2 Tb1 33.20(8) . . ?
O7 Tb2 Tb1 86.55(16) . 5_666 ?
Tb1 Tb2 Tb1 60.32(2) 6_565 . ?
Tb1 Tb2 Tb1 60.615(17) 5_666 6_565 ?
Tb1 Tb2 Tb1 60.38(2) 5_666 2_656 ?
Tb1 Tb2 Tb1 90.84(2) 5_666 . ?
Tb1 Tb2 Tb1 60.615(17) 2_656 . ?
Tb1 Tb2 Tb1 90.84(2) 2_656 6_565 ?
O8 Tb1 O8 65.4(2) 6_565 5_666 ?
O8 Tb1 O10 75.4(3) 6_565 . ?
O8 Tb1 O10 75.2(3) 5_666 . ?
O8 Tb1 Tb2 33.25(13) 5_666 5_666 ?
O8 Tb1 Tb2 33.07(14) 6_565 . ?
O8 Tb1 Tb2 85.35(14) 5_666 . ?
O8 Tb1 Tb2 85.56(15) 6_565 5_666 ?
O8 Tb1 Tb1 32.90(13) 5_666 2_656 ?
O8 Tb1 Tb1 33.05(14) 6_565 2_656 ?
O8 Tb1 Tb1 86.01(14) 6_565 6_565 ?
O8 Tb1 Tb1 86.03(14) 5_666 6_565 ?
O9 Tb1 O8 66.0(2) 5_666 5_666 ?
O9 Tb1 O8 99.7(2) 5_666 6_565 ?
O9 Tb1 O6 75.4(2) 5_666 . ?
O9 Tb1 O10 138.7(3) 5_666 . ?
O9 Tb1 O1 137.7(3) 5_666 . ?
O9 Tb1 O5 77.0(3) 5_666 8_465 ?
O9 Tb1 O7 64.6(2) 5_666 . ?
O9 Tb1 Tb2 33.42(16) 5_666 5_666 ?
O9 Tb1 Tb2 85.06(15) 5_666 . ?
O9 Tb1 Tb1 85.85(15) 5_666 2_656 ?
O9 Tb1 Tb1 32.54(16) 5_666 6_565 ?
O6 Tb1 O8 137.8(2) . 5_666 ?
O6 Tb1 O8 140.9(2) . 6_565 ?
O6 Tb1 O10 133.2(3) . . ?
O6 Tb1 O1 80.9(3) . . ?
O6 Tb1 O5 77.9(3) . 8_465 ?
O6 Tb1 Tb2 105.45(17) . 5_666 ?
O6 Tb1 Tb2 108.44(17) . . ?
O6 Tb1 Tb1 69.06(18) . 6_565 ?
O6 Tb1 Tb1 158.96(18) . 2_656 ?
O10 Tb1 Tb2 105.8(3) . 5_666 ?
O10 Tb1 Tb2 106.0(3) . . ?
O10 Tb1 Tb1 67.7(3) . 2_656 ?
O10 Tb1 Tb1 157.7(3) . 6_565 ?
O1 Tb1 O8 77.6(3) . 6_565 ?
O1 Tb1 O8 140.3(3) . 5_666 ?
O1 Tb1 O10 82.3(4) . . ?
O1 Tb1 O5 131.1(4) . 8_465 ?
O1 Tb1 Tb2 159.0(3) . 5_666 ?
O1 Tb1 Tb2 69.9(3) . . ?
O1 Tb1 Tb1 108.0(2) . 2_656 ?
O1 Tb1 Tb1 106.0(3) . 6_565 ?
O5 Tb1 O8 139.8(3) 8_465 6_565 ?
O5 Tb1 O8 77.3(3) 8_465 5_666 ?
O5 Tb1 O10 81.3(4) 8_465 . ?
O5 Tb1 Tb2 69.8(2) 8_465 5_666 ?
O5 Tb1 Tb2 158.9(2) 8_465 . ?
O5 Tb1 Tb1 107.5(2) 8_465 2_656 ?
O5 Tb1 Tb1 106.5(2) 8_465 6_565 ?
O7 Tb1 O8 99.6(2) . 5_666 ?
O7 Tb1 O8 65.8(2) . 6_565 ?
O7 Tb1 O6 77.7(2) . . ?
O7 Tb1 O10 138.7(3) . . ?
O7 Tb1 O1 76.6(3) . . ?
O7 Tb1 O5 138.5(3) . 8_465 ?
O7 Tb1 Tb2 85.14(17) . 5_666 ?
O7 Tb1 Tb2 33.29(15) . . ?
O7 Tb1 Tb1 85.73(17) . 2_656 ?
O7 Tb1 Tb1 32.71(15) . 6_565 ?
Tb2 Tb1 Tb2 89.16(2) 5_666 . ?
Tb2 Tb1 Tb1 59.738(17) 5_666 2_656 ?
Tb2 Tb1 Tb1 59.840(10) . 6_565 ?
Tb2 Tb1 Tb1 59.811(11) 5_666 6_565 ?
Tb2 Tb1 Tb1 59.647(16) . 2_656 ?
Tb1 Tb1 Tb1 90.000(1) 6_565 2_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
C1 C2 C3 C4 177.8(13) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C1 O1 Tb1 -171.6(9) . . . . ?
C2 C1 O2 Tb2 168.7(8) . . . . ?
C2 C7 C6 C5 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C5 C8 178.4(12) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C8 O3B 0.0(17) . . . . ?
C4 C5 C8 C9 -117.4(14) . . . . ?
C4 C5 C8 O3A 123.0(14) . . . . ?
C5 C8 C9 C14 -117.4(14) . . . . ?
C5 C8 C9 C10 61.9(19) . . . . ?
C6 C7 C2 C1 -177.6(13) . . . . ?
C6 C7 C2 C3 0.0 . . . . ?
C6 C5 C8 O3B 178.4(12) . . . . ?
C6 C5 C8 C9 61.0(19) . . . . ?
C6 C5 C8 O3A -58.7(16) . . . . ?
C8 C5 C6 C7 -178.3(12) . . . . ?
C8 C9 C10 C11 -179.3(13) . . . . ?
O3B C8 C9 C14 124.2(16) . . . . ?
O3B C8 C9 C10 -56.5(19) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C9 C14 C13 C12 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C15 -177.8(12) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C11 C12 C15 O4 -10.4(17) . . . . ?
C11 C12 C15 O5 171.8(11) . . . . ?
C12 C15 O4 Tb2 174.9(8) . . . 7_666 ?
C12 C15 O5 Tb1 -174.3(8) . . . 8_565 ?
C13 C14 C9 C8 179.3(14) . . . . ?
C13 C14 C9 C10 0.0 . . . . ?
C13 C12 C15 O4 171.8(10) . . . . ?
C13 C12 C15 O5 -6.0(18) . . . . ?
C15 C12 C13 C14 177.8(12) . . . . ?
C16 C17 C18 C18 178.2(18) . . . 2_657 ?
C16 C17 C18 N1 -1(3) . . . . ?
C17 C16 O6 Tb1 -152.1(9) . . . . ?
C18 C17 C18 C18 -3(3) 6_565 . . 2_657 ?
C18 C17 C18 N1 177(3) 6_565 . . . ?
O6 C16 C17 C18 3(2) 6_565 . . 6_565 ?
O6 C16 C17 C18 -178.5(14) 6_565 . . . ?
O6 C16 C17 C18 -3(2) . . . . ?
O6 C16 C17 C18 178.5(14) . . . 6_565 ?
O6 C16 O6 Tb1 23(2) 6_565 . . . ?
O1 C1 C2 C7 168.3(13) . . . . ?
O1 C1 C2 C3 -9(2) . . . . ?
O1 C1 O2 Tb2 -18(3) . . . . ?
O2 C1 C2 C7 -18(2) . . . . ?
O2 C1 C2 C3 164.6(12) . . . . ?
O2 C1 O1 Tb1 15(3) . . . . ?
O4 C15 O5 Tb1 8(3) . . . 8_565 ?
O5 C15 O4 Tb2 -8(3) . . . 7_666 ?
O3A C8 C9 C14 1(2) . . . . ?
O3A C8 C9 C10 -179.5(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 -0.509 0.046 -0.691 5178.9 794.0 ?

_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
;
# start Validation Reply Form
_vrf_PLAT971_lk3_23_5abscorr     
;
RESPONSE: We report the best dataset collected for this compound. We 
collected data from several crystals and applied absorption correction 
for each dataset but there is still residual density around the metal ions. 
Considering that this compound is a result of a single crystal to single crystal 
post synthetic modification at relatively high temperature it is expected that 
the quality of the single crystals will be significantly worse than that of 
the single crystals of the initial compound.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_lk3_40_5
_database_code_depnum_ccdc_archive 'CCDC 2338726'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H20 O18 Tb3'
_chemical_formula_sum            'C36 H20 O18 Tb3'
_chemical_formula_weight         1217.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Tb O N C H'
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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   18.795(2)
_cell_length_b                   29.712(2)
_cell_length_c                   15.4791(14)
_cell_angle_alpha                90
_cell_angle_beta                 102.312(10)
_cell_angle_gamma                90
_cell_volume                     8445.3(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3784
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.6580
_cell_measurement_theta_min      4.1500
_shelx_estimated_absorpt_T_max   0.816
_shelx_estimated_absorpt_T_min   0.120
_exptl_absorpt_coefficient_mu    12.448
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    0.957
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.2967
_exptl_crystal_size_mid          0.1702
_exptl_crystal_size_min          0.017
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16388
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.995
_diffrn_reflns_theta_max         66.995
_diffrn_reflns_theta_min         3.681
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  14.00   1.00    7.50    --    0.00  77.00  30.00   52
  2  ω     17.00  42.00   1.00    7.50    --    0.00  77.00  30.00   25
  3  ω     20.00  52.00   1.00    7.50    --    0.00 -99.00  60.00   32
  4  ω   -123.00 -89.00   1.00   45.00    --  -61.81 -94.00 -90.00   34
  5  ω   -152.00 -85.00   1.00   45.00    --  -61.81 -77.00  30.00   67
  6  ω    109.00 155.00   1.00   45.00    --   61.81 107.00-100.00   46
  7  ω     16.00 104.00   1.00   45.00    --   61.81 -94.00   0.00   88
  8  ω    123.00 150.00   1.00   45.00    --   61.81 125.00  30.00   27
  9  ω    100.00 142.00   1.00   45.00    --   61.81 125.00  60.00   42
 10  ω    105.00 139.00   1.00   45.00    --   61.81  77.00-120.00   34
 11  ω    105.00 144.00   1.00   45.00    --   61.81  77.00 150.00   39
 12  ω     25.00 104.00   1.00   75.00    --  121.00 -91.00   0.00   79
 13  ω     32.00  99.00   1.00   75.00    --  121.00 -38.00   0.00   67
 14  ω     28.00  93.00   1.00   75.00    --  121.00-111.00   0.00   65
 15  ω    115.00 157.00   1.00   75.00    --  121.00  77.00  90.00   42
 16  ω     81.00 106.00   1.00   75.00    --  121.00 -91.00 -60.00   25
 17  ω     67.00 102.00   1.00   75.00    --  121.00 -91.00-120.00   35
 18  ω     31.00  58.00   1.00   75.00    --  121.00 -91.00-120.00   27
 19  ω     34.00  81.00   1.00   75.00    --  121.00-111.00 -30.00   47
 20  ω     50.00  97.00   1.00   75.00    --  121.00 -91.00  60.00   47
 21  ω     36.00  90.00   1.00   75.00    --  121.00 -50.00-150.00   54
 22  ω    108.00 159.00   1.00   75.00    --  121.00 -50.00-150.00   51
 23  ω     29.00  56.00   1.00   75.00    --  121.00 -91.00 -60.00   27
 24  ω    109.00 174.00   1.00   75.00    --  121.00  12.00-150.00   65
 25  ω     28.00 108.00   1.00   75.00    --  121.00  12.00-150.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0297606000
_diffrn_orient_matrix_UB_12      -0.0010795000
_diffrn_orient_matrix_UB_13      0.0853114000
_diffrn_orient_matrix_UB_21      0.0714727000
_diffrn_orient_matrix_UB_22      -0.0217342000
_diffrn_orient_matrix_UB_23      0.0497534000
_diffrn_orient_matrix_UB_31      0.0322819000
_diffrn_orient_matrix_UB_32      0.0470705000
_diffrn_orient_matrix_UB_33      0.0250089000
_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                5183
_reflns_number_total             7626
_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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         4.132
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     279
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.1170
_refine_ls_restrained_S_all      1.075
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3044
_refine_ls_wR_factor_ref         0.3283
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C9-C8
 1.45 with sigma of 0.02
 C15-O5
 1.35 with sigma of 0.001
 O4-C15
 1.35 with sigma of 0.01
 C12-C15_$2
 1.54 with sigma of 0.001
 C16-O6
 1.3 with sigma of 0.001
 C15_$2-C12
 1.55 with sigma of 0.001
 C16-C20
 1.55 with sigma of 0.02
 O3B-C8
 1.4 with sigma of 0.02
 C16-O7
 1.35 with sigma of 0.02
 C8-C5
 1.45 with sigma of 0.02
 C22-C21
 1.35 with sigma of 0.02
 C21-C18
 1.35 with sigma of 0.02
 C18-C19
 1.35 with sigma of 0.02
 C18-C17
 1.55 with sigma of 0.02
 C19-C20
 1.35 with sigma of 0.02
 C22-C20_$1
 1.35 with sigma of 0.02
 C20-C22_$1
 1.35 with sigma of 0.02
 O8-C17
 1.35 with sigma of 0.02
 C19-C19_$1
 1.35 with sigma of 0.02
 O6-C20
 2.5 with sigma of 0.04
 C19-C16
 2.35 with sigma of 0.04
 C18-C20
 2.35 with sigma of 0.04
 C22-C18
 2.35 with sigma of 0.04
 C21-C19
 2.35 with sigma of 0.04
 C21-C17
 2.35 with sigma of 0.04
 O8-C18
 2.5 with sigma of 0.04
 O7-C18
 2.5 with sigma of 0.04
 C19-C17
 2.35 with sigma of 0.04
 O7-C20
 2.5 with sigma of 0.04
3. Rigid bond restraints
 O11B, Tb3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3A, C8, O3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O6, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C3 \\sim C2 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C8 \\sim C14
\\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C15 \\sim C22 \\sim C18
\\sim C19 \\sim C21 \\sim C16 \\sim C20 \\sim C17 \\sim O6 \\sim O4 \\sim O2
\\sim O7 \\sim O5 \\sim O1 \\sim O8 \\sim O11A \\sim O10 \\sim O9 \\sim O3B
\\sim O12A \\sim O12B \\sim O3A \\sim O11B: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C15 \\sim O4 \\sim O5: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.02 within 2A
Tb2 \\sim O5 \\sim C15 \\sim C12: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
O3A \\sim C8 \\sim O3B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C20) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O11B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O11A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O12A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O12B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
5. Others
 Sof(O12A)=0.5*(1-FVAR(2))
 Sof(O12B)=0.5*FVAR(2)
 Sof(H8B)=Sof(O3B)=1-FVAR(2)
 Sof(H8A)=Sof(O3A)=FVAR(2)
 Sof(O11B)=0.5*(1-FVAR(4))
 Sof(O11A)=0.5*FVAR(4)
 Fixed Sof: C16(0.25) O6(0.25) O8(0.25) C17(0.25)
6.a Ternary CH refined with riding coordinates:
 C8(H8B), C8(H8A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6), C4(H4), C14(H14), C10(H10), C11(H11), C13(H13),
 C22(H22), C21(H21)
6.c Fitted hexagon refined as free rotating group:
 C3(C2,C7,C6,C5,C4), C14(C9,C10,C11,C12,C13)
;
_atom_sites_solution_hydrogens   geom
_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
C1 C 0.6423(10) 0.6129(5) 0.6585(11) 0.096(4) Uani 1 1 d . U . . .
C3 C 0.7543(7) 0.6365(3) 0.7779(8) 0.125(6) Uani 1 1 d G U . . .
H3 H 0.769310 0.605942 0.784214 0.150 Uiso 1 1 calc R U . . .
C2 C 0.6914(7) 0.6483(3) 0.7170(7) 0.102(5) Uani 1 1 d G U . . .
C7 C 0.6695(7) 0.6930(4) 0.7078(8) 0.149(8) Uani 1 1 d G U . . .
H7 H 0.626547 0.701010 0.666155 0.178 Uiso 1 1 calc R U . . .
C6 C 0.7106(8) 0.7260(3) 0.7594(9) 0.148(8) Uani 1 1 d G U . . .
H6 H 0.695597 0.756591 0.753031 0.178 Uiso 1 1 calc R U . . .
C5 C 0.7735(8) 0.7143(3) 0.8202(8) 0.152(8) Uani 1 1 d DG U . . .
C4 C 0.7954(7) 0.6695(4) 0.8295(8) 0.143(7) Uani 1 1 d G U . . .
H4 H 0.838361 0.661524 0.871091 0.172 Uiso 1 1 calc R U . . .
C8 C 0.8206(15) 0.7481(6) 0.8749(11) 0.179(7) Uani 1 1 d D U . . .
H8B H 0.866579 0.732853 0.905380 0.215 Uiso 0.45(3) 1 calc R U P A 2
H8A H 0.790866 0.761014 0.915222 0.215 Uiso 0.55(3) 1 calc R U P A 1
C14 C 0.8805(8) 0.7741(3) 0.7618(8) 0.153(8) Uani 1 1 d G U . . .
H14 H 0.894384 0.743599 0.757659 0.184 Uiso 1 1 calc R U . . .
C9 C 0.8400(9) 0.7867(4) 0.8232(7) 0.157(7) Uani 1 1 d DG U . . .
C10 C 0.8197(9) 0.8314(4) 0.8293(8) 0.156(8) Uani 1 1 d G U . . .
H10 H 0.792054 0.839933 0.871270 0.187 Uiso 1 1 calc R U . . .
C11 C 0.8399(9) 0.8635(3) 0.7738(8) 0.160(8) Uani 1 1 d G U . . .
H11 H 0.826039 0.894050 0.777906 0.192 Uiso 1 1 calc R U . . .
C12 C 0.8804(9) 0.8510(3) 0.7123(7) 0.121(6) Uani 1 1 d DG U . . .
C13 C 0.9007(8) 0.8063(3) 0.7063(8) 0.143(7) Uani 1 1 d G U . . .
H13 H 0.928369 0.797717 0.664294 0.171 Uiso 1 1 calc R U . . .
C15 C 0.4050(7) 0.3884(3) 0.6557(7) 0.0907(18) Uani 1 1 d D U . . .
C22 C 0.3705(16) 0.500000 1.030(2) 0.30(2) Uani 1 2 d DS TU P . .
H22 H 0.327885 0.500000 1.053331 0.365 Uiso 1 2 calc R U P . .
C18 C 0.4301(14) 0.500000 0.9087(15) 0.196(12) Uani 1 2 d DS TU P . .
C19 C 0.4994(15) 0.500000 0.9545(7) 0.191(13) Uani 1 2 d DS TU P . .
C21 C 0.3689(17) 0.500000 0.941(2) 0.295(19) Uani 1 2 d DS TU P . .
H21 H 0.323033 0.500000 0.900517 0.353 Uiso 1 2 calc R U P . .
C16 C 0.5548(8) 0.500000 0.8166(12) 0.067(6) Uani 0.5 2 d DS TU P . .
O6 O 0.6093(7) 0.500000 0.7772(8) 0.037(3) Uani 0.5 2 d DS TU P B .
O4 O 0.3847(6) 0.4295(3) 0.6690(6) 0.0907(18) Uani 1 1 d D U . . .
O2 O 0.5926(5) 0.6275(4) 0.5985(6) 0.087(3) Uani 1 1 d . U . . .
O7 O 0.4834(9) 0.500000 0.7761(8) 0.099(4) Uani 1 2 d DS TU P B .
O5 O 0.4395(5) 0.3709(3) 0.5954(6) 0.0907(18) Uani 1 1 d D U . . .
O1 O 0.6688(6) 0.5718(3) 0.6776(7) 0.094(3) Uani 1 1 d . U . . .
O8 O 0.3446(12) 0.500000 0.7539(15) 0.075(6) Uani 0.5 2 d DS TU P B .
O11A O 0.2824(3) 0.500000 0.6230(4) 0.0062(19) Uani 0.75(2) 2 d S TU P B 1
O10 O 0.4802(4) 0.5420(2) 0.3790(4) 0.0544(15) Uani 1 1 d . . . . .
O9 O 0.4044(3) 0.5426(2) 0.4990(4) 0.0538(15) Uani 1 1 d . . . . .
Tb2 Tb 0.500000 0.59175(3) 0.500000 0.0623(4) Uani 1 2 d S T P B .
Tb3 Tb 0.41537(6) 0.500000 0.62827(6) 0.0639(4) Uani 1 2 d S TU P . .
Tb1 Tb 0.62783(6) 0.500000 0.63166(6) 0.0647(4) Uani 1 2 d S T P . .
O3B O 0.7853(19) 0.7652(9) 0.9399(15) 0.187(9) Uani 0.45(3) 1 d D U P A 2
C20 C 0.5610(14) 0.500000 0.9192(13) 0.166(11) Uani 1 2 d DS TU P . .
C17 C 0.4109(17) 0.500000 0.8076(16) 0.116(11) Uani 0.5 2 d DS TU P B .
O12A O 0.7698(5) 0.500000 0.6366(5) 0.015(3) Uani 0.58(2) 2 d S TU P B 2
O12B O 0.7324(11) 0.500000 0.5693(13) 0.051(6) Uani 0.42(2) 2 d S TU P B 1
O3A O 0.886(2) 0.7268(11) 0.934(2) 0.212(11) Uani 0.55(3) 1 d . U P A 1
O11B O 0.2951(13) 0.500000 0.5805(17) 0.021(6) Uani 0.25(2) 2 d S TU P B 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
C1 C2 1.556(14) . ?
C1 O2 1.25(2) . ?
C1 O1 1.328(19) . ?
C3 H3 0.9500 . ?
C3 C2 1.3900 . ?
C3 C4 1.3900 . ?
C2 C7 1.3900 . ?
C7 H7 0.9500 . ?
C7 C6 1.3900 . ?
C6 H6 0.9500 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C5 C8 1.479(14) . ?
C4 H4 0.9500 . ?
C8 H8B 1.0000 . ?
C8 H8A 1.0000 . ?
C8 C9 1.488(13) . ?
C8 O3B 1.414(19) . ?
C8 O3A 1.50(4) . ?
C14 H14 0.9500 . ?
C14 C9 1.3900 . ?
C14 C13 1.3900 . ?
C9 C10 1.3900 . ?
C10 H10 0.9500 . ?
C10 C11 1.3900 . ?
C11 H11 0.9500 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C15 1.5448 3 ?
C13 H13 0.9500 . ?
C15 O4 1.309(8) . ?
C15 O5 1.3495(10) . ?
C22 H22 0.9500 . ?
C22 C21 1.368(19) . ?
C22 C20 1.359(14) 2_657 ?
C18 C19 1.343(17) . ?
C18 C21 1.348(18) . ?
C18 C17 1.529(17) . ?
C19 C19 1.404(19) 2_657 ?
C19 C20 1.381(17) . ?
C21 H21 0.9500 . ?
C16 O6 1.3000(10) . ?
C16 O7 1.354(16) . ?
C16 C20 1.568(17) . ?
O6 Tb1 2.352(12) . ?
O4 Tb3 2.297(8) . ?
O2 Tb2 2.314(9) . ?
O7 Tb3 2.371(13) . ?
O7 C17 1.54(3) . ?
O5 Tb2 2.328(8) 5_666 ?
O1 Tb1 2.328(9) . ?
O8 Tb3 2.58(2) . ?
O8 C17 1.342(18) . ?
O11A Tb3 2.483(6) . ?
O10 Tb2 2.353(6) . ?
O10 Tb3 2.348(7) 5_666 ?
O10 Tb1 2.358(7) 5_666 ?
O9 Tb2 2.313(7) . ?
O9 Tb3 2.340(7) . ?
O9 Tb1 2.353(6) 5_666 ?
Tb2 Tb3 3.9052(9) . ?
Tb2 Tb3 3.9052(9) 5_666 ?
Tb2 Tb1 3.9076(9) . ?
Tb2 Tb1 3.9076(9) 5_666 ?
Tb3 C17 2.79(3) . ?
Tb3 O11B 2.22(2) . ?
Tb1 O12A 2.654(9) . ?
Tb1 O12B 2.37(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
O2 C1 C2 117.1(13) . . ?
O2 C1 O1 132.3(12) . . ?
O1 C1 C2 110.0(14) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C2 C1 122.6(10) . . ?
C3 C2 C7 120.0 . . ?
C7 C2 C1 117.4(10) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C8 122.5(14) . . ?
C4 C5 C8 117.5(14) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C5 C8 H8B 108.4 . . ?
C5 C8 H8A 105.8 . . ?
C5 C8 C9 113.7(13) . . ?
C5 C8 O3A 111.9(19) . . ?
C9 C8 H8B 108.4 . . ?
C9 C8 H8A 105.8 . . ?
C9 C8 O3A 113(2) . . ?
O3B C8 C5 109.7(19) . . ?
O3B C8 H8B 108.4 . . ?
O3B C8 C9 108.1(18) . . ?
O3A C8 H8A 105.8 . . ?
C9 C14 H14 120.0 . . ?
C9 C14 C13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C9 C8 113.2(14) . . ?
C10 C9 C8 126.8(14) . . ?
C10 C9 C14 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C15 118.0(7) . 3 ?
C13 C12 C15 122.0(8) . 3 ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
O4 C15 C12 117(4) . 3_445 ?
O4 C15 O5 131.8(7) . . ?
O5 C15 C12 111(4) . 3_445 ?
C21 C22 H22 123.2 . . ?
C20 C22 H22 123.2 2_657 . ?
C20 C22 C21 114(3) 2_657 . ?
C19 C18 C21 128(2) . . ?
C19 C18 C17 122.0(17) . . ?
C21 C18 C17 110(2) . . ?
C18 C19 C19 110(3) . 2_657 ?
C18 C19 C20 126.3(14) . . ?
C20 C19 C19 124(3) . 2_657 ?
C22 C21 H21 118.9 . . ?
C18 C21 C22 122(3) . . ?
C18 C21 H21 118.9 . . ?
O6 C16 O7 125.8(17) . . ?
O6 C16 C20 125.4(16) . . ?
O7 C16 C20 108.8(13) . . ?
C16 O6 Tb1 137.9(12) . . ?
C15 O4 Tb3 135.2(7) . . ?
C1 O2 Tb2 132.0(9) . . ?
C16 O7 Tb3 136.4(11) . . ?
C16 O7 C17 135.1(13) . . ?
C17 O7 Tb3 88.5(11) . . ?
C15 O5 Tb2 128.9(6) . 5_666 ?
C1 O1 Tb1 133.7(10) . . ?
C17 O8 Tb3 84.7(16) . . ?
Tb2 O10 Tb1 112.1(2) . 5_666 ?
Tb3 O10 Tb2 112.3(3) 5_666 . ?
Tb3 O10 Tb1 115.6(3) 5_666 5_666 ?
Tb2 O9 Tb3 114.1(3) . . ?
Tb2 O9 Tb1 113.8(2) . 5_666 ?
Tb3 O9 Tb1 113.8(3) . 5_666 ?
O2 Tb2 O2 125.3(6) 2_656 . ?
O2 Tb2 O5 78.4(3) 2_656 6_565 ?
O2 Tb2 O5 76.3(4) 2_656 5_666 ?
O2 Tb2 O5 76.3(4) . 6_565 ?
O2 Tb2 O5 78.4(4) . 5_666 ?
O2 Tb2 O10 141.5(3) 2_656 2_656 ?
O2 Tb2 O10 141.5(3) . . ?
O2 Tb2 O10 78.2(3) . 2_656 ?
O2 Tb2 O10 78.2(3) 2_656 . ?
O2 Tb2 Tb3 109.0(3) 2_656 . ?
O2 Tb2 Tb3 108.4(2) 2_656 5_666 ?
O2 Tb2 Tb3 109.0(3) . 5_666 ?
O2 Tb2 Tb3 108.4(2) . . ?
O2 Tb2 Tb1 163.1(3) 2_656 . ?
O2 Tb2 Tb1 71.6(3) . . ?
O2 Tb2 Tb1 163.1(3) . 5_666 ?
O2 Tb2 Tb1 71.6(3) 2_656 5_666 ?
O5 Tb2 O5 123.1(4) 6_565 5_666 ?
O5 Tb2 O10 79.1(3) 6_565 2_656 ?
O5 Tb2 O10 79.1(3) 5_666 . ?
O5 Tb2 O10 142.1(3) 6_565 . ?
O5 Tb2 O10 142.1(3) 5_666 2_656 ?
O5 Tb2 Tb3 164.2(2) 6_565 5_666 ?
O5 Tb2 Tb3 164.2(2) 5_666 . ?
O5 Tb2 Tb3 72.7(2) 5_666 5_666 ?
O5 Tb2 Tb3 72.7(2) 6_565 . ?
O5 Tb2 Tb1 109.3(2) 6_565 . ?
O5 Tb2 Tb1 109.5(2) 6_565 5_666 ?
O5 Tb2 Tb1 109.3(2) 5_666 5_666 ?
O5 Tb2 Tb1 109.5(2) 5_666 . ?
O10 Tb2 O10 102.1(3) 2_656 . ?
O10 Tb2 Tb3 33.80(17) 2_656 . ?
O10 Tb2 Tb3 87.32(15) 2_656 5_666 ?
O10 Tb2 Tb3 33.79(17) . 5_666 ?
O10 Tb2 Tb3 87.32(15) . . ?
O10 Tb2 Tb1 34.00(16) . 5_666 ?
O10 Tb2 Tb1 34.00(16) 2_656 . ?
O10 Tb2 Tb1 87.24(16) . . ?
O10 Tb2 Tb1 87.24(16) 2_656 5_666 ?
O9 Tb2 O2 140.2(3) . . ?
O9 Tb2 O2 79.1(3) . 2_656 ?
O9 Tb2 O2 140.2(3) 2_656 2_656 ?
O9 Tb2 O2 79.1(3) 2_656 . ?
O9 Tb2 O5 79.7(3) . 6_565 ?
O9 Tb2 O5 79.7(3) 2_656 5_666 ?
O9 Tb2 O5 141.3(3) . 5_666 ?
O9 Tb2 O5 141.3(3) 2_656 6_565 ?
O9 Tb2 O10 66.8(2) . . ?
O9 Tb2 O10 66.4(2) 2_656 . ?
O9 Tb2 O10 66.8(2) 2_656 2_656 ?
O9 Tb2 O10 66.4(2) . 2_656 ?
O9 Tb2 O9 101.7(3) 2_656 . ?
O9 Tb2 Tb3 33.14(15) . . ?
O9 Tb2 Tb3 87.47(16) . 5_666 ?
O9 Tb2 Tb3 87.47(16) 2_656 . ?
O9 Tb2 Tb3 33.14(16) 2_656 5_666 ?
O9 Tb2 Tb1 87.34(16) . . ?
O9 Tb2 Tb1 33.44(15) . 5_666 ?
O9 Tb2 Tb1 33.44(15) 2_656 . ?
O9 Tb2 Tb1 87.34(16) 2_656 5_666 ?
Tb3 Tb2 Tb3 91.46(3) . 5_666 ?
Tb3 Tb2 Tb1 61.29(2) . . ?
Tb3 Tb2 Tb1 60.42(2) . 5_666 ?
Tb3 Tb2 Tb1 60.42(2) 5_666 . ?
Tb3 Tb2 Tb1 61.29(2) 5_666 5_666 ?
Tb1 Tb2 Tb1 91.53(3) . 5_666 ?
O4 Tb3 O4 131.7(5) 6_565 . ?
O4 Tb3 O7 81.4(3) . . ?
O4 Tb3 O7 81.4(3) 6_565 . ?
O4 Tb3 O8 66.0(2) 6_565 . ?
O4 Tb3 O8 66.0(2) . . ?
O4 Tb3 O11A 72.5(3) . . ?
O4 Tb3 O11A 72.5(3) 6_565 . ?
O4 Tb3 O10 139.4(3) . 2_656 ?
O4 Tb3 O10 77.9(3) 6_565 2_656 ?
O4 Tb3 O10 77.9(3) . 5_666 ?
O4 Tb3 O10 139.4(3) 6_565 5_666 ?
O4 Tb3 O9 76.1(3) 6_565 . ?
O4 Tb3 O9 76.1(3) . 6_565 ?
O4 Tb3 O9 138.3(3) 6_565 6_565 ?
O4 Tb3 O9 138.3(3) . . ?
O4 Tb3 Tb2 69.9(2) 6_565 . ?
O4 Tb3 Tb2 158.4(2) . . ?
O4 Tb3 C17 70.4(3) 6_565 . ?
O4 Tb3 C17 70.4(3) . . ?
O7 Tb3 O8 62.0(6) . . ?
O7 Tb3 O11A 111.3(4) . . ?
O7 Tb3 Tb2 107.2(3) . . ?
O7 Tb3 C17 33.5(7) . . ?
O8 Tb3 Tb2 135.62(4) . . ?
O8 Tb3 C17 28.6(5) . . ?
O11A Tb3 O8 49.3(5) . . ?
O11A Tb3 Tb2 119.97(9) . . ?
O11A Tb3 C17 77.8(6) . . ?
O10 Tb3 O7 76.2(4) 2_656 . ?
O10 Tb3 O7 76.2(3) 5_666 . ?
O10 Tb3 O8 127.4(4) 2_656 . ?
O10 Tb3 O8 127.4(4) 5_666 . ?
O10 Tb3 O11A 147.59(16) 2_656 . ?
O10 Tb3 O11A 147.59(16) 5_666 . ?
O10 Tb3 O10 64.1(3) 2_656 5_666 ?
O10 Tb3 Tb2 84.89(15) 5_666 . ?
O10 Tb3 Tb2 33.87(16) 2_656 . ?
O10 Tb3 C17 104.5(5) 2_656 . ?
O10 Tb3 C17 104.5(5) 5_666 . ?
O9 Tb3 O7 139.2(3) . . ?
O9 Tb3 O7 139.2(3) 6_565 . ?
O9 Tb3 O8 132.8(4) 6_565 . ?
O9 Tb3 O8 132.8(4) . . ?
O9 Tb3 O11A 93.9(2) 6_565 . ?
O9 Tb3 O11A 93.9(2) . . ?
O9 Tb3 O10 99.7(2) . 5_666 ?
O9 Tb3 O10 99.7(2) 6_565 2_656 ?
O9 Tb3 O10 66.0(2) . 2_656 ?
O9 Tb3 O10 66.0(2) 6_565 5_666 ?
O9 Tb3 O9 65.5(3) . 6_565 ?
O9 Tb3 Tb2 32.72(16) . . ?
O9 Tb3 Tb2 85.06(16) 6_565 . ?
O9 Tb3 C17 146.5(2) 6_565 . ?
O9 Tb3 C17 146.5(2) . . ?
C17 Tb3 Tb2 127.3(3) . . ?
O11B Tb3 O4 78.1(4) . . ?
O11B Tb3 O7 128.5(8) . . ?
O11B Tb3 O8 66.4(9) . . ?
O11B Tb3 O9 79.5(6) . . ?
O11B Tb3 Tb2 109.0(5) . . ?
O11B Tb3 C17 95.0(9) . . ?
O6 Tb1 O10 76.5(3) . 5_666 ?
O6 Tb1 O10 76.5(3) . 2_656 ?
O6 Tb1 O9 139.4(2) . 2_656 ?
O6 Tb1 O9 139.4(2) . 5_666 ?
O6 Tb1 Tb2 107.4(2) . . ?
O6 Tb1 Tb2 107.4(2) . 5_666 ?
O6 Tb1 Tb3 160.0(3) . 5_666 ?
O6 Tb1 O12A 109.0(4) . . ?
O6 Tb1 O12B 134.1(6) . . ?
O1 Tb1 O6 79.3(3) 6_565 . ?
O1 Tb1 O6 79.3(3) . . ?
O1 Tb1 O1 132.9(5) . 6_565 ?
O1 Tb1 O10 76.1(3) . 2_656 ?
O1 Tb1 O10 136.9(3) 6_565 2_656 ?
O1 Tb1 O10 136.9(3) . 5_666 ?
O1 Tb1 O10 76.1(3) 6_565 5_666 ?
O1 Tb1 O9 77.1(3) 6_565 5_666 ?
O1 Tb1 O9 139.8(3) . 5_666 ?
O1 Tb1 O9 77.1(3) . 2_656 ?
O1 Tb1 O9 139.8(3) 6_565 2_656 ?
O1 Tb1 Tb2 69.3(3) . . ?
O1 Tb1 Tb2 69.3(3) 6_565 5_666 ?
O1 Tb1 Tb2 157.7(3) . 5_666 ?
O1 Tb1 Tb2 157.7(3) 6_565 . ?
O1 Tb1 Tb3 107.2(3) 6_565 5_666 ?
O1 Tb1 Tb3 107.2(3) . 5_666 ?
O1 Tb1 O12A 74.1(3) 6_565 . ?
O1 Tb1 O12A 74.1(3) . . ?
O1 Tb1 O12B 82.8(3) . . ?
O1 Tb1 O12B 82.8(3) 6_565 . ?
O10 Tb1 O10 63.8(3) 5_666 2_656 ?
O10 Tb1 Tb2 84.71(16) 5_666 . ?
O10 Tb1 Tb2 33.92(14) 2_656 . ?
O10 Tb1 Tb2 84.71(16) 2_656 5_666 ?
O10 Tb1 Tb2 33.92(14) 5_666 5_666 ?
O10 Tb1 Tb3 86.64(15) 5_666 5_666 ?
O10 Tb1 Tb3 86.64(15) 2_656 5_666 ?
O10 Tb1 O12A 147.96(16) 5_666 . ?
O10 Tb1 O12A 147.96(16) 2_656 . ?
O10 Tb1 O12B 138.5(3) 2_656 . ?
O10 Tb1 O12B 138.5(3) 5_666 . ?
O9 Tb1 O10 99.5(2) 2_656 5_666 ?
O9 Tb1 O10 99.5(2) 5_666 2_656 ?
O9 Tb1 O10 66.1(2) 5_666 5_666 ?
O9 Tb1 O10 66.1(2) 2_656 2_656 ?
O9 Tb1 O9 65.1(3) 5_666 2_656 ?
O9 Tb1 Tb2 84.84(16) 2_656 5_666 ?
O9 Tb1 Tb2 32.81(16) 2_656 . ?
O9 Tb1 Tb2 32.81(16) 5_666 5_666 ?
O9 Tb1 Tb2 84.84(16) 5_666 . ?
O9 Tb1 Tb3 32.99(17) 2_656 5_666 ?
O9 Tb1 Tb3 32.99(17) 5_666 5_666 ?
O9 Tb1 O12A 95.6(2) 5_666 . ?
O9 Tb1 O12A 95.6(2) 2_656 . ?
O9 Tb1 O12B 74.5(4) 5_666 . ?
O9 Tb1 O12B 74.5(4) 2_656 . ?
Tb2 Tb1 Tb2 88.47(3) . 5_666 ?
Tb2 Tb1 Tb3 59.760(17) 5_666 5_666 ?
Tb2 Tb1 Tb3 59.760(17) . 5_666 ?
O12A Tb1 Tb2 121.18(11) . . ?
O12B Tb1 Tb2 105.0(3) . 5_666 ?
O12B Tb1 Tb2 105.0(3) . . ?
O12B Tb1 Tb3 65.8(5) . 5_666 ?
C22 C20 C19 123(2) 2_657 . ?
C22 C20 C16 117(2) 2_657 . ?
C19 C20 C16 120.8(15) . . ?
C18 C17 O7 107.0(17) . . ?
C18 C17 Tb3 165.0(18) . . ?
O7 C17 Tb3 58.0(10) . . ?
O8 C17 C18 128(2) . . ?
O8 C17 O7 125(2) . . ?
O8 C17 Tb3 66.7(14) . . ?

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
C1 C2 C7 C6 178.9(12) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C2 C1 O2 Tb2 -175.1(8) . . . . ?
C2 C1 O1 Tb1 174.9(8) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C2 C7 C6 C5 0.0 . . . . ?
C7 C6 C5 C4 0.0 . . . . ?
C7 C6 C5 C8 178.0(17) . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
C6 C5 C8 C9 -49(3) . . . . ?
C6 C5 C8 O3B 71.7(19) . . . . ?
C6 C5 C8 O3A -179(2) . . . . ?
C5 C8 C9 C14 -63(3) . . . . ?
C5 C8 C9 C10 114.7(19) . . . . ?
C4 C3 C2 C1 -178.8(12) . . . . ?
C4 C3 C2 C7 0.0 . . . . ?
C4 C5 C8 C9 128.6(18) . . . . ?
C4 C5 C8 O3B -110.3(19) . . . . ?
C4 C5 C8 O3A -1(3) . . . . ?
C8 C5 C4 C3 -178.1(16) . . . . ?
C8 C9 C10 C11 -177.5(17) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C9 C14 C13 C12 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C15 -176.8(13) . . . 3 ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C15 O4 Tb3 168(5) 3_445 . . . ?
C12 C15 O5 Tb2 -173.2(8) 3_445 . . 5_666 ?
C13 C14 C9 C8 177.8(15) . . . . ?
C13 C14 C9 C10 0.0 . . . . ?
C15 C12 C13 C14 176.6(14) 3 . . . ?
C18 C19 C20 C22 180.000(10) . . . 2_657 ?
C18 C19 C20 C16 0.000(8) . . . . ?
C19 C18 C21 C22 0.000(11) . . . . ?
C19 C18 C17 O7 0.000(7) . . . . ?
C19 C18 C17 O8 180.000(7) . . . . ?
C19 C18 C17 Tb3 0.000(16) . . . . ?
C19 C19 C20 C22 0.000(9) 2_657 . . 2_657 ?
C19 C19 C20 C16 180.000(8) 2_657 . . . ?
C21 C18 C19 C19 0.000(6) . . . 2_657 ?
C21 C18 C19 C20 180.000(9) . . . . ?
C21 C18 C17 O7 180.000(7) . . . . ?
C21 C18 C17 O8 0.000(8) . . . . ?
C21 C18 C17 Tb3 180.00(2) . . . . ?
C16 O7 C17 C18 0.000(6) . . . . ?
C16 O7 C17 O8 180.000(7) . . . . ?
C16 O7 C17 Tb3 180.000(8) . . . . ?
O6 C16 O7 Tb3 0.000(6) . . . . ?
O6 C16 O7 C17 180.000(8) . . . . ?
O6 C16 C20 C22 0.000(8) . . . 2_657 ?
O6 C16 C20 C19 180.000(8) . . . . ?
O4 C15 O5 Tb2 13(2) . . . 5_666 ?
O2 C1 C2 C3 -171.1(11) . . . . ?
O2 C1 C2 C7 10.1(17) . . . . ?
O2 C1 O1 Tb1 -14(3) . . . . ?
O7 C16 O6 Tb1 0.000(7) . . . . ?
O7 C16 C20 C22 180.000(8) . . . 2_657 ?
O7 C16 C20 C19 0.000(10) . . . . ?
O5 C15 O4 Tb3 -18(3) . . . . ?
O1 C1 C2 C3 1.3(17) . . . . ?
O1 C1 C2 C7 -177.5(10) . . . . ?
O1 C1 O2 Tb2 15(3) . . . . ?
Tb3 O7 C17 C18 180.000(5) . . . . ?
Tb3 O7 C17 O8 0.000(4) . . . . ?
Tb3 O8 C17 C18 180.000(6) . . . . ?
Tb3 O8 C17 O7 0.000(4) . . . . ?
O3B C8 C9 C14 175.0(16) . . . . ?
O3B C8 C9 C10 -7(2) . . . . ?
C20 C22 C21 C18 0.000(10) 2_657 . . . ?
C20 C16 O6 Tb1 180.000(5) . . . . ?
C20 C16 O7 Tb3 180.000(6) . . . . ?
C20 C16 O7 C17 0.000(8) . . . . ?
C17 C18 C19 C19 180.000(6) . . . 2_657 ?
C17 C18 C19 C20 0.000(8) . . . . ?
C17 C18 C21 C22 180.000(11) . . . . ?
O3A C8 C9 C14 66(2) . . . . ?
O3A C8 C9 C10 -116(2) . . . . ?

_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 -0.249 -0.900 -0.272 5385.4 914.6 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 3.677
_oxdiff_exptl_absorpt_empirical_full_min 0.391


# start Validation Reply Form

_vrf_PLAT971_lk3_40_5            
;
RESPONSE: We report the best dataset collected for this compound. We collected 
data from several crystals and applied absorption correction for each dataset 
but there is still residual density around the metal ions and disordered O 
atoms. Considering that this compound is a result of a single crystal to single 
crystal post synthetic modification at relatively high temperature it is 
expected that the quality of the single crystals will be significantly worse 
than that of the single crystals of the initial compound.
;

_vrf_PLAT973_lk3_40_5            
;
RESPONSE: We report the best dataset collected for this compound. We collected 
data from several crystals and applied absorption correction for each dataset 
but there is still residual density around the metal ions. Considering that 
this compound is a result of a single crystal to single crystal post synthetic 
modification at relatively high temperature it is expected that the quality of 
the single crystals will be significantly worse than that of the single crystals
of the initial compound.
;
_vrf_PLAT220_lk3_40_5            
;
RESPONSE: This alert, is due to the fact that the U(eq) values for some O atoms 
are high and for disordered O atoms of a H2O molecule are too low because of the 
moderate quality of the crystal data. Considering that this compound is a result 
of a single crystal to single crystal post synthetic modification at relatively 
high temperature it is expected that the quality of the single crystals will be 
significantly worse than that of the single crystals of the initial compound.
;

_vrf_PLAT342_lk3_40_5            
;
RESPONSE: This alert is due to the moderate quality of the crystal data despite 
systematic trials to obtain better crystals for X-ray data collection and the 
multiple datasets collected. Considering that this compound is a result of 
a single crystal to single crystal post synthetic modification at relatively 
high temperature it is expected that the quality of the single crystals will be 
significantly worse than that of the single crystals of the initial compound.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_lk3_52_1
_database_code_depnum_ccdc_archive 'CCDC 2338727'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H39 F O36 Tb6'
_chemical_formula_sum            'C68 H39 F O36 Tb6'
_chemical_formula_weight         2404.51
_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'
F F 0.0727 0.0534 '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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   29.7002(6)
_cell_length_b                   18.5497(6)
_cell_length_c                   14.9529(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.273(2)
_cell_angle_gamma                90
_cell_volume                     8106.0(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12549
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      71.8410
_cell_measurement_theta_min      3.8560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.973
_exptl_absorpt_correction_T_max  0.256
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    0.985
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2268
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 -10 1 0.1328
10 10 0 0.1046
-13 8 -2 0.1167
2 0 -10 0.0364
-2 0 10 0.0678
-10 -10 0 0.1079

_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.105
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27258
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.994
_diffrn_reflns_theta_max         66.994
_diffrn_reflns_theta_min         3.865
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_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   -127.00 -98.00   1.00   10.00    --  -35.83 -77.00 -30.00   29
  2  ω    -95.00   1.00   1.00   10.00    --  -35.83 -57.00 -60.00   96
  3  ω   -121.00 -86.00   1.00   10.00    --  -35.83 -77.00 120.00   35
  4  ω   -123.00 -84.00   1.00   10.00    --  -35.83 -77.00-120.00   39
  5  ω   -119.00   1.00   1.00   10.00    --  -35.83 -57.00-180.00  120
  6  ω    -62.00  -9.00   1.00   10.00    --  -35.83 125.00  30.00   53
  7  ω   -120.00 -88.00   1.00   10.00    --  -35.83 -77.00 -90.00   32
  8  ω    -79.00 -27.00   1.00   10.00    --  -35.83 125.00 150.00   52
  9  ω     -2.00  29.00   1.00   10.00    --   35.83  77.00  90.00   31
 10  ω     42.00  73.00   1.00   10.00    --   35.83-125.00   0.00   31
 11  ω     15.00  42.00   1.00   10.00    --   35.83  77.00 -60.00   27
 12  ω     12.00  83.00   1.00   10.00    --   35.83 -99.00 150.00   71
 13  ω     79.00 107.00   1.00   70.00    --  108.11-111.00  90.00   28
 14  ω    114.00 170.00   1.00   70.00    --  108.11  77.00   0.00   56
 15  ω     53.00 109.00   1.00   70.00    --  108.11-111.00 -90.00   56
 16  ω     83.00 109.00   1.00   70.00    --  108.11-111.00 -30.00   26
 17  ω     61.00 136.00   1.00   70.00    --  108.11 178.00  60.00   75
 18  ω    110.00 170.00   1.00   70.00    --  108.11 111.00 -30.00   60
 19  ω     34.00 148.00   1.00   70.00    --  108.11 -30.00 -30.00  114
 20  ω     72.00 109.00   1.00   70.00    --  108.11-111.00-180.00   37
 21  ω    119.00 146.00   1.00   70.00    --  108.11 -77.00 150.00   27
 22  ω     28.00  73.00   1.00   70.00    --  108.11 -77.00 150.00   45
 23  ω    133.00 170.00   1.00   70.00    --  108.11  30.00 120.00   37
 24  ω     72.00 147.00   1.00   70.00    --  108.11  45.00-180.00   75
 25  ω     61.00  99.00   1.00   70.00    --  108.11 178.00  90.00   38
 26  ω    103.00 173.00   1.00   70.00    --  108.11  77.00  30.00   70
 27  ω    115.00 177.00   1.00   70.00    --  108.11  77.00  60.00   62
 28  ω    119.00 146.00   1.00   70.00    --  108.11 178.00 120.00   27
 29  ω     25.00 147.00   1.00   70.00    --  108.11 -77.00   0.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5982
_reflns_number_total             7466
_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 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         5.419
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0893
_refine_ls_restrained_S_all      1.049
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2429
_refine_ls_wR_factor_ref         0.2544
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Tb(H) groups
2. Restrained distances
 C8-O3A
 1.35 with sigma of 0.02
 C18-H18
 0.93 with sigma of 0.001
 C18-F1
 1.35 with sigma of 0.001
 F1-H18
 0.42 with sigma of 0.001
 F1-C17
 2.35 with sigma of 0.001
 H18-C17
 2 with sigma of 0.002
3. Restrained planarity
 C16, C17, C18, H18, F1, O6
 with sigma of 0.1
4. Rigid bond restraints
 O3B, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3A, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C18, F1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Uiso/Uaniso restraints and constraints
O3B \\sim C8: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C8 \\sim O3A \\sim O3B: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.02 within 2A
C18 \\sim F1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C16 \\sim C17 \\sim C18 \\sim F1: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
6. Rigid body (RIGU) restrains
 C8, O3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(O3B)=1-FVAR(1)
 Sof(O3A)=FVAR(1)
 Fixed Sof: H8A(0.5) H8B(0.5) F1(0.25) H18(0.75)
8.a Ternary CH refined with riding coordinates:
 C8(H8A), C8(H8B)
8.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4(H4), C6(H6), C13(H13), C11(H11), C10(H10), C14(H14)
8.c Fitted hexagon refined as free rotating group:
 C7(C2,C3,C4,C5,C6), C13(C12,C11,C10,C9,C14)
;
_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
C1 C 0.5955(3) 0.8780(7) 0.3336(7) 0.085(3) Uani 1 1 d . . . . .
C7 C 0.6696(3) 0.8684(5) 0.2767(6) 0.135(6) Uani 1 1 d G . . . .
H7 H 0.680750 0.907530 0.315401 0.162 Uiso 1 1 calc R U . . .
C2 C 0.6252(2) 0.8438(5) 0.2730(5) 0.110(4) Uani 1 1 d G . . . .
C3 C 0.6089(2) 0.7865(5) 0.2163(6) 0.132(6) Uani 1 1 d G . . . .
H3 H 0.578489 0.769681 0.213748 0.159 Uiso 1 1 calc R U . . .
C4 C 0.6371(3) 0.7540(5) 0.1633(5) 0.132(6) Uani 1 1 d G . . . .
H4 H 0.626022 0.714846 0.124607 0.159 Uiso 1 1 calc R U . . .
C5 C 0.6816(3) 0.7786(6) 0.1671(5) 0.148(6) Uani 1 1 d G U . . .
C6 C 0.6979(2) 0.8358(6) 0.2237(6) 0.167(7) Uani 1 1 d G U . . .
H6 H 0.728284 0.852694 0.226259 0.200 Uiso 1 1 calc R U . . .
C8 C 0.7131(5) 0.7452(12) 0.1081(8) 0.187(7) Uani 1 1 d D U . . .
H8A H 0.696120 0.706698 0.069089 0.225 Uiso 0.5 1 calc R U P A 1
H8B H 0.723843 0.784716 0.071615 0.225 Uiso 0.5 1 calc R U P B 2
C16 C 0.4777(6) 1.000000 0.1833(10) 0.103(2) Uani 1 2 d S TU P . .
C17 C 0.4901(6) 1.000000 0.0889(9) 0.103(2) Uani 1 2 d DS TU P C .
C18 C 0.4931(5) 0.9393(5) 0.0426(7) 0.104(2) Uani 1 1 d D U . . .
F1 F 0.4749(9) 0.8765(4) 0.0647(13) 0.106(3) Uani 0.25 1 d D U P C 2
C13 C 0.8361(2) 0.7124(5) 0.2272(6) 0.135(6) Uani 1 1 d G . . . .
H13 H 0.865617 0.732610 0.228933 0.162 Uiso 1 1 calc R U . . .
C12 C 0.8306(2) 0.6534(5) 0.2816(5) 0.111(4) Uani 1 1 d G . . . .
C11 C 0.7873(3) 0.6238(5) 0.2791(6) 0.133(6) Uani 1 1 d G . . . .
H11 H 0.783565 0.583507 0.316225 0.159 Uiso 1 1 calc R U . . .
C10 C 0.7497(2) 0.6532(6) 0.2222(6) 0.165(8) Uani 1 1 d G . . . .
H10 H 0.720155 0.632972 0.220515 0.198 Uiso 1 1 calc R U . . .
C9 C 0.7552(3) 0.7122(6) 0.1679(5) 0.141(7) Uani 1 1 d G . . . .
C14 C 0.7984(3) 0.7418(5) 0.1704(6) 0.139(7) Uani 1 1 d G . . . .
H14 H 0.802205 0.782076 0.133222 0.166 Uiso 1 1 calc R U . . .
O1 O 0.5543(2) 0.8594(5) 0.3173(4) 0.0891(19) Uani 1 1 d . . . . .
O6 O 0.4745(2) 0.9385(4) 0.2173(3) 0.0747(16) Uani 1 1 d . . . . .
O4 O 0.4108(2) 0.8588(5) 0.3227(5) 0.092(2) Uani 1 1 d . . . . .
O5 O 0.6365(2) 1.0775(4) 0.5985(4) 0.0823(17) Uani 1 1 d . . . . .
O9 O 0.55475(19) 1.000000 0.6205(3) 0.0471(13) Uani 1 2 d S T P . .
O7 O 0.54211(14) 0.9031(3) 0.4987(3) 0.0476(10) Uani 1 1 d . . . . .
O2 O 0.6157(2) 0.9212(4) 0.3924(4) 0.0855(18) Uani 1 1 d . . . . .
O8 O 0.53080(18) 1.000000 0.3757(3) 0.0450(12) Uani 1 2 d S T P . .
O10 O 0.4935(3) 0.7731(4) 0.4287(7) 0.108(3) Uani 1 1 d . . . . .
O3A O 0.7255(7) 0.7997(14) 0.0528(10) 0.201(8) Uani 0.544(17) 1 d D U P D 1
Tb2 Tb 0.59143(2) 1.000000 0.49634(3) 0.0584(2) Uani 1 2 d S T P . .
Tb1 Tb 0.48697(2) 0.89364(3) 0.36617(2) 0.0616(2) Uani 1 1 d . . . . .
H18 H 0.4909(19) 0.89368(19) 0.0670(15) 0.074 Uiso 0.75 1 d D U P E 1
C15 C 0.3723(3) 0.8819(7) 0.3403(7) 0.094(3) Uani 1 1 d . . . . .
O3B O 0.6921(8) 0.6939(19) 0.0485(11) 0.187(7) Uani 0.456(17) 1 d . U P D 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
C1 C2 1.512(9) . ?
C1 O1 1.251(13) . ?
C1 O2 1.260(14) . ?
C7 H7 0.9500 . ?
C7 C2 1.3900 . ?
C7 C6 1.3900 . ?
C2 C3 1.3900 . ?
C3 H3 0.9500 . ?
C3 C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C5 C8 1.526(12) . ?
C6 H6 0.9500 . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C8 C9 1.529(12) . ?
C8 O3A 1.398(18) . ?
C8 O3B 1.38(4) . ?
C16 C17 1.521(17) . ?
C16 O6 1.260(8) 6_575 ?
C16 O6 1.260(8) . ?
C17 C18 1.332(11) . ?
C17 C18 1.333(11) 6_575 ?
C18 C18 1.405(17) 2_655 ?
C18 F1 1.3501(10) . ?
C18 H18 0.9300(10) . ?
C13 H13 0.9500 . ?
C13 C12 1.3900 . ?
C13 C14 1.3900 . ?
C12 C11 1.3900 . ?
C12 C15 1.531(10) 8_565 ?
C11 H11 0.9500 . ?
C11 C10 1.3900 . ?
C10 H10 0.9500 . ?
C10 C9 1.3900 . ?
C9 C14 1.3900 . ?
C14 H14 0.9500 . ?
O1 Tb1 2.336(6) . ?
O6 Tb1 2.343(5) . ?
O4 Tb1 2.330(6) . ?
O4 C15 1.294(14) . ?
O5 Tb2 2.336(6) . ?
O5 C15 1.248(14) 5_676 ?
O9 Tb2 2.315(5) . ?
O9 Tb1 2.357(3) 2_656 ?
O9 Tb1 2.357(3) 5_676 ?
O7 Tb2 2.322(4) . ?
O7 Tb1 2.341(4) . ?
O7 Tb1 2.342(4) 2_656 ?
O2 Tb2 2.339(6) . ?
O8 Tb2 2.310(5) . ?
O8 Tb1 2.354(3) . ?
O8 Tb1 2.354(3) 6_575 ?
O10 Tb1 2.418(8) . ?
Tb2 Tb1 3.9049(6) 5_676 ?
Tb2 Tb1 3.9049(6) 2_656 ?
Tb2 Tb1 3.8927(6) . ?
Tb2 Tb1 3.8926(6) 6_575 ?
Tb1 Tb1 3.9387(7) 2_656 ?
Tb1 Tb1 3.9459(10) 6_575 ?

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 C1 C2 114.9(10) . . ?
O1 C1 O2 129.7(8) . . ?
O2 C1 C2 115.4(9) . . ?
C2 C7 H7 120.0 . . ?
C2 C7 C6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C2 C1 119.3(7) . . ?
C3 C2 C1 120.7(7) . . ?
C3 C2 C7 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C8 121.3(11) . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C8 118.7(11) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C8 H8A 109.3 . . ?
C5 C8 H8B 107.8 . . ?
C5 C8 C9 110.3(9) . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 107.8 . . ?
O3A C8 C5 107.5(14) . . ?
O3A C8 H8A 109.3 . . ?
O3A C8 C9 111.2(14) . . ?
O3B C8 C5 113.7(15) . . ?
O3B C8 H8B 107.8 . . ?
O3B C8 C9 109.3(14) . . ?
O6 C16 C17 115.0(6) . . ?
O6 C16 C17 115.0(6) 6_575 . ?
O6 C16 O6 129.9(12) 6_575 . ?
C18 C17 C16 122.1(6) . . ?
C18 C17 C16 122.1(6) 6_575 . ?
C18 C17 C18 115.2(12) . 6_575 ?
C17 C18 C18 121.9(6) . 2_655 ?
C17 C18 F1 122.3(9) . . ?
C17 C18 H18 123.3(12) . . ?
C18 C18 H18 114.2(12) 2_655 . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C12 C15 120.2(7) . 8_565 ?
C11 C12 C13 120.0 . . ?
C11 C12 C15 119.7(8) . 8_565 ?
C12 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C9 C8 119.1(11) . . ?
C10 C9 C14 120.0 . . ?
C14 C9 C8 120.8(11) . . ?
C13 C14 H14 120.0 . . ?
C9 C14 C13 120.0 . . ?
C9 C14 H14 120.0 . . ?
C1 O1 Tb1 136.5(7) . . ?
C16 O6 Tb1 134.0(7) . . ?
C15 O4 Tb1 134.6(7) . . ?
C15 O5 Tb2 133.0(6) 5_676 . ?
Tb2 O9 Tb1 113.41(14) . 5_676 ?
Tb2 O9 Tb1 113.41(14) . 2_656 ?
Tb1 O9 Tb1 113.7(2) 2_656 5_676 ?
Tb2 O7 Tb1 113.70(17) . 2_656 ?
Tb2 O7 Tb1 113.16(17) . . ?
Tb1 O7 Tb1 114.50(17) . 2_656 ?
C1 O2 Tb2 134.1(6) . . ?
Tb2 O8 Tb1 113.13(14) . . ?
Tb2 O8 Tb1 113.13(14) . 6_575 ?
Tb1 O8 Tb1 113.9(2) . 6_575 ?
O5 Tb2 O5 75.9(4) . 6_575 ?
O5 Tb2 O2 80.9(2) . 6_575 ?
O5 Tb2 O2 80.9(2) 6_575 . ?
O5 Tb2 O2 127.6(3) . . ?
O5 Tb2 O2 127.6(3) 6_575 6_575 ?
O5 Tb2 Tb1 106.98(16) 6_575 5_676 ?
O5 Tb2 Tb1 109.12(19) 6_575 . ?
O5 Tb2 Tb1 109.11(19) . 6_575 ?
O5 Tb2 Tb1 161.98(17) . . ?
O5 Tb2 Tb1 70.76(18) . 5_676 ?
O5 Tb2 Tb1 106.98(16) . 2_656 ?
O5 Tb2 Tb1 70.77(18) 6_575 2_656 ?
O5 Tb2 Tb1 161.98(17) 6_575 6_575 ?
O9 Tb2 O5 76.81(19) . 6_575 ?
O9 Tb2 O5 76.81(19) . . ?
O9 Tb2 O7 66.39(12) . . ?
O9 Tb2 O7 66.39(12) . 6_575 ?
O9 Tb2 O2 141.06(18) . 6_575 ?
O9 Tb2 O2 141.06(18) . . ?
O9 Tb2 Tb1 87.37(12) . 6_575 ?
O9 Tb2 Tb1 33.63(6) . 5_676 ?
O9 Tb2 Tb1 33.63(6) . 2_656 ?
O9 Tb2 Tb1 87.37(12) . . ?
O7 Tb2 O5 139.03(19) 6_575 6_575 ?
O7 Tb2 O5 78.7(2) . 6_575 ?
O7 Tb2 O5 139.03(19) . . ?
O7 Tb2 O5 78.7(2) 6_575 . ?
O7 Tb2 O7 101.4(2) . 6_575 ?
O7 Tb2 O2 139.8(2) 6_575 . ?
O7 Tb2 O2 78.2(2) . . ?
O7 Tb2 O2 78.2(2) 6_575 6_575 ?
O7 Tb2 O2 139.8(2) . 6_575 ?
O7 Tb2 Tb1 33.31(10) . 2_656 ?
O7 Tb2 Tb1 33.57(10) . . ?
O7 Tb2 Tb1 33.57(10) 6_575 6_575 ?
O7 Tb2 Tb1 86.91(11) 6_575 2_656 ?
O7 Tb2 Tb1 87.20(11) 6_575 . ?
O7 Tb2 Tb1 86.91(11) . 5_676 ?
O7 Tb2 Tb1 33.31(10) 6_575 5_676 ?
O7 Tb2 Tb1 87.20(11) . 6_575 ?
O2 Tb2 O2 77.4(4) 6_575 . ?
O2 Tb2 Tb1 107.28(17) . 6_575 ?
O2 Tb2 Tb1 161.59(19) 6_575 2_656 ?
O2 Tb2 Tb1 70.32(19) 6_575 6_575 ?
O2 Tb2 Tb1 161.59(19) . 5_676 ?
O2 Tb2 Tb1 108.48(19) 6_575 5_676 ?
O2 Tb2 Tb1 108.49(19) . 2_656 ?
O2 Tb2 Tb1 107.28(17) 6_575 . ?
O2 Tb2 Tb1 70.33(19) . . ?
O8 Tb2 O5 141.82(19) . 6_575 ?
O8 Tb2 O5 141.82(19) . . ?
O8 Tb2 O9 102.35(19) . . ?
O8 Tb2 O7 66.80(12) . . ?
O8 Tb2 O7 66.80(12) . 6_575 ?
O8 Tb2 O2 76.7(2) . . ?
O8 Tb2 O2 76.7(2) . 6_575 ?
O8 Tb2 Tb1 87.50(11) . 2_656 ?
O8 Tb2 Tb1 33.79(5) . . ?
O8 Tb2 Tb1 33.79(5) . 6_575 ?
O8 Tb2 Tb1 87.50(11) . 5_676 ?
Tb1 Tb2 Tb1 91.287(14) . 5_676 ?
Tb1 Tb2 Tb1 91.287(14) 6_575 2_656 ?
Tb1 Tb2 Tb1 60.907(17) 6_575 . ?
Tb1 Tb2 Tb1 60.678(12) 6_575 5_676 ?
Tb1 Tb2 Tb1 60.678(12) . 2_656 ?
Tb1 Tb2 Tb1 60.697(16) 2_656 5_676 ?
O1 Tb1 O6 78.3(2) . . ?
O1 Tb1 O9 138.3(2) . 5_676 ?
O1 Tb1 O7 139.3(2) . 2_656 ?
O1 Tb1 O7 77.1(2) . . ?
O1 Tb1 O8 75.6(2) . . ?
O1 Tb1 O10 81.7(3) . . ?
O1 Tb1 Tb2 69.13(19) . . ?
O1 Tb1 Tb2 157.82(19) . 5_676 ?
O1 Tb1 Tb1 105.8(2) . 6_575 ?
O1 Tb1 Tb1 107.07(17) . 2_656 ?
O6 Tb1 O9 77.7(2) . 5_676 ?
O6 Tb1 O8 75.6(2) . . ?
O6 Tb1 O10 133.1(3) . . ?
O6 Tb1 Tb2 108.26(16) . 5_676 ?
O6 Tb1 Tb2 105.76(15) . . ?
O6 Tb1 Tb1 159.16(17) . 2_656 ?
O6 Tb1 Tb1 69.22(17) . 6_575 ?
O4 Tb1 O1 132.8(3) . . ?
O4 Tb1 O6 81.5(2) . . ?
O4 Tb1 O9 75.9(3) . 5_676 ?
O4 Tb1 O7 139.0(2) . . ?
O4 Tb1 O7 76.9(2) . 2_656 ?
O4 Tb1 O8 138.4(2) . . ?
O4 Tb1 O10 81.8(3) . . ?
O4 Tb1 Tb2 69.3(2) . 5_676 ?
O4 Tb1 Tb2 158.0(2) . . ?
O4 Tb1 Tb1 106.1(2) . 6_575 ?
O4 Tb1 Tb1 106.78(17) . 2_656 ?
O9 Tb1 O10 138.5(2) 5_676 . ?
O9 Tb1 Tb2 32.95(12) 5_676 5_676 ?
O9 Tb1 Tb2 85.28(12) 5_676 . ?
O9 Tb1 Tb1 85.72(12) 5_676 2_656 ?
O9 Tb1 Tb1 33.17(12) 5_676 6_575 ?
O7 Tb1 O6 138.17(19) . . ?
O7 Tb1 O6 140.67(19) 2_656 . ?
O7 Tb1 O9 99.47(17) . 5_676 ?
O7 Tb1 O9 65.41(17) 2_656 5_676 ?
O7 Tb1 O7 64.78(17) . 2_656 ?
O7 Tb1 O8 65.79(16) . . ?
O7 Tb1 O8 99.78(17) 2_656 . ?
O7 Tb1 O10 75.7(2) 2_656 . ?
O7 Tb1 O10 75.3(3) . . ?
O7 Tb1 Tb2 33.27(11) . . ?
O7 Tb1 Tb2 84.79(11) . 5_676 ?
O7 Tb1 Tb2 33.00(11) 2_656 5_676 ?
O7 Tb1 Tb2 85.07(10) 2_656 . ?
O7 Tb1 Tb1 32.75(10) . 2_656 ?
O7 Tb1 Tb1 85.68(12) . 6_575 ?
O7 Tb1 Tb1 85.69(12) 2_656 6_575 ?
O7 Tb1 Tb1 32.74(10) 2_656 2_656 ?
O8 Tb1 O9 65.59(16) . 5_676 ?
O8 Tb1 O10 138.3(3) . . ?
O8 Tb1 Tb2 85.41(11) . 5_676 ?
O8 Tb1 Tb2 33.08(12) . . ?
O8 Tb1 Tb1 86.11(13) . 2_656 ?
O8 Tb1 Tb1 33.06(11) . 6_575 ?
O10 Tb1 Tb2 106.1(2) . 5_676 ?
O10 Tb1 Tb2 105.9(2) . . ?
O10 Tb1 Tb1 157.6(2) . 6_575 ?
O10 Tb1 Tb1 67.6(2) . 2_656 ?
Tb2 Tb1 Tb2 88.713(14) . 5_676 ?
Tb2 Tb1 Tb1 59.546(8) . 6_575 ?
Tb2 Tb1 Tb1 59.814(12) . 2_656 ?
Tb2 Tb1 Tb1 59.507(11) 5_676 2_656 ?
Tb2 Tb1 Tb1 59.652(8) 5_676 6_575 ?
Tb1 Tb1 Tb1 90.0 2_656 6_575 ?
O4 C15 C12 113(2) . 8_465 ?
O5 C15 C12 115(2) 5_676 8_465 ?
O5 C15 O4 131.0(9) 5_676 . ?

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
C1 C2 C3 C4 -177.7(9) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C2 C1 O1 Tb1 -172.5(6) . . . . ?
C2 C1 O2 Tb2 172.9(6) . . . . ?
C2 C7 C6 C5 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C5 C8 -178.5(11) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C8 C9 -118.6(13) . . . . ?
C4 C5 C8 O3A 120.0(13) . . . . ?
C4 C5 C8 O3B 4.6(19) . . . . ?
C5 C8 C9 C10 65.8(18) . . . . ?
C5 C8 C9 C14 -112.2(14) . . . . ?
C6 C7 C2 C1 177.8(9) . . . . ?
C6 C7 C2 C3 0.0 . . . . ?
C6 C5 C8 C9 62.8(18) . . . . ?
C6 C5 C8 O3A -58.6(13) . . . . ?
C6 C5 C8 O3B -174.0(14) . . . . ?
C8 C5 C6 C7 178.6(10) . . . . ?
C8 C9 C14 C13 178.0(10) . . . . ?
C16 C17 C18 C18 -176.6(18) . . . 2_655 ?
C16 C17 C18 F1 17(2) . . . . ?
C17 C16 O6 Tb1 150.1(9) . . . . ?
C18 C17 C18 C18 11(3) 6_575 . . 2_655 ?
C18 C17 C18 F1 -155.5(16) 6_575 . . . ?
C13 C12 C11 C10 0.0 . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C12 C11 C10 C9 0.0 . . . . ?
C11 C10 C9 C8 -178.0(10) . . . . ?
C11 C10 C9 C14 0.0 . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
C14 C13 C12 C11 0.0 . . . . ?
C14 C13 C12 C15 176.5(9) . . . 8_565 ?
O1 C1 C2 C7 170.9(8) . . . . ?
O1 C1 C2 C3 -11.4(13) . . . . ?
O1 C1 O2 Tb2 -6.7(18) . . . . ?
O6 C16 C17 C18 -177.5(15) 6_575 . . . ?
O6 C16 C17 C18 177.5(15) . . . 6_575 ?
O6 C16 C17 C18 -6.0(18) 6_575 . . 6_575 ?
O6 C16 C17 C18 6.0(18) . . . . ?
O6 C16 O6 Tb1 -26(3) 6_575 . . . ?
O2 C1 C2 C7 -8.8(12) . . . . ?
O2 C1 C2 C3 169.0(8) . . . . ?
O2 C1 O1 Tb1 7.1(19) . . . . ?
O3A C8 C9 C10 -175.0(11) . . . . ?
O3A C8 C9 C14 7.0(16) . . . . ?
Tb1 O4 C15 C12 171(3) . . . 8_465 ?
Tb1 O4 C15 O5 -16.4(19) . . . 5_676 ?
C15 C12 C11 C10 -176.5(8) 8_565 . . . ?
O3B C8 C9 C10 -59.9(16) . . . . ?
O3B C8 C9 C14 122.1(16) . . . . ?

_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 -0.728 -0.968 -0.410 5222.2 1042.5 ?


_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
;
# start Validation Reply Form
_vrf_PLAT971_lk3_52_1            
;
RESPONSE: We report the best dataset collected for this compound. We collected 
data from several crystals and applied absorption correction for each dataset 
but there is still residual density around the metal ions and phenyl rings. 
Considering that this compound is a result of a single crystal to single crystal 
post synthetic modification at relatively high temperature it is expected that 
the quality of the single crystals will be significantly worse than that of the 
single crystals of the initial compound.
;
_vrf_PLAT973_lk3_52_1            
;
RESPONSE: We report the best dataset collected for this compound. We collected 
data from several crystals and applied absorption correction for each dataset 
but there is still residual density around the metal ions. Considering that this 
compound is a result of a single crystal to single crystal post synthetic 
modification at relatively high temperature it is expected that the quality of 
the single crystals will be significantly worse than that of the single crystals 
of the initial compound.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_lk3_8_3_newabscorr
_database_code_depnum_ccdc_archive 'CCDC 2338728'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H20 O18 Tb3'
_chemical_formula_sum            'C34 H20 O18 Tb3'
_chemical_formula_weight         1193.26
_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'
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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   29.812(2)
_cell_length_b                   18.891(3)
_cell_length_c                   14.8342(14)
_cell_angle_alpha                90
_cell_angle_beta                 100.849(10)
_cell_angle_gamma                90
_cell_volume                     8205.0(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4309
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      70.7300
_cell_measurement_theta_min      4.2800
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.804
_exptl_absorpt_correction_T_max  0.104
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2252
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 -11 -1 0.0894
11 10 -1 0.0746
-6 12 0 0.1255
-17 -6 1 0.1393
0 0 9 0.0783
0 0 -9 0.0981
19 1 -1 0.1434
-19 -1 2 0.1672

_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.177
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1156
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24220
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.999
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         3.857
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.4223
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -127.00-102.00   1.00   10.00    --  -35.83 -77.00  90.00   25
  2  ω   -112.00  36.00   1.00   10.00    --  -35.83 -14.00  72.00  148
  3  ω    -71.00 -44.00   1.00   10.00    --  -35.83 125.00 -60.00   27
  4  ω   -127.00 -86.00   1.00   10.00    --  -35.83 -77.00 -90.00   41
  5  ω    -41.00 -12.00   1.00   10.00    --  -35.83 125.00 -60.00   29
  6  ω    -54.00 -15.00   1.00   10.00    --  -35.83 125.00-120.00   39
  7  ω   -121.00 -94.00   1.00   10.00    --  -35.83 -77.00 -60.00   27
  8  ω    -68.00 -14.00   1.00   10.00    --  -35.83 125.00 120.00   54
  9  ω      7.00  40.00   1.00   10.00    --   35.83  77.00 150.00   33
 10  ω     16.00  50.00   1.00   10.00    --   35.83 -99.00  30.00   34
 11  ω     -2.00  30.00   1.00   10.00    --   35.83  77.00 120.00   32
 12  ω     -2.00  36.00   1.00   10.00    --   35.83  77.00 -60.00   38
 13  ω     -4.00  42.00   1.00   10.00    --   35.83  77.00-120.00   46
 14  ω     56.00  83.00   1.00   10.00    --   35.83 -99.00   0.00   27
 15  ω    141.00 178.00   1.00   60.00    --  108.11  77.00 -60.00   37
 16  ω     19.00  56.00   1.00   60.00    --  108.11 -77.00  90.00   37
 17  ω     22.00  49.00   1.00   60.00    --  108.11 -95.00 -30.00   27
 18  ω     82.00 109.00   1.00   60.00    --  108.11-111.00 150.00   27
 19  ω     22.00 109.00   1.00   60.00    --  108.11-111.00 -90.00   87
 20  ω     74.00 109.00   1.00   60.00    --  108.11-111.00  90.00   35
 21  ω     32.00  59.00   1.00   60.00    --  108.11-111.00  90.00   27
 22  ω     29.00 142.00   1.00   60.00    --  108.11 -61.00-120.00  113
 23  ω     72.00 167.00   1.00   60.00    --  108.11  61.00 120.00   95
 24  ω     74.00 142.00   1.00   60.00    --  108.11 178.00 -60.00   68
 25  ω     92.00 144.00   1.00   60.00    --  108.11 -77.00  30.00   52
 26  ω    108.00 152.00   1.00   60.00    --  108.11  77.00-150.00   44
 27  ω    103.00 159.00   1.00   60.00    --  108.11  77.00  60.00   56
 28  ω     69.00 106.00   1.00   60.00    --  108.11 -95.00 -30.00   37
 29  ω    110.00 135.00   1.00   60.00    --  108.11 -77.00  90.00   25
 30  ω     18.00  83.00   1.00   60.00    --  108.11 -77.00  30.00   65
 31  ω     90.00 177.00   1.00   60.00    --  108.11   0.00  30.00   87
 32  ω     14.00  71.00   1.00   60.00    --  108.11   0.00  30.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4252
_reflns_number_total             7508
_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 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.320
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         7508
_refine_ls_number_restraints     298
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.1038
_refine_ls_restrained_S_all      0.967
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2865
_refine_ls_wR_factor_ref         0.3198
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C2
 1.41 with sigma of 0.02
 C7-C6
 1.41 with sigma of 0.02
 C17-C16
 1.45 with sigma of 0.01
 O4-C15
 1.24 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O4 \\sim O5 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
O3 \\sim C8: within 1.6A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 1.6A
Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O1, O2, O4, O5, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14,
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 C8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C3(H3), C10(H10), C11(H11), C13(H13), C14(H14),
 C18(H18)
5.c Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C2,C3), C9(C10,C11,C12,C13,C14)
;
_atom_sites_solution_hydrogens   geom
_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
Tb1 Tb 0.48530(2) 0.60492(5) 0.36464(4) 0.0892(3) Uani 1 1 d . . . . .
Tb2 Tb 0.40869(3) 0.500000 0.50658(6) 0.0884(4) Uani 1 2 d S T P . .
O1 O 0.4082(4) 0.6351(9) 0.3185(8) 0.1588(17) Uani 1 1 d . U . . .
O2 O 0.3633(4) 0.5796(9) 0.4056(8) 0.1589(17) Uani 1 1 d . U . . .
O3 O 0.1891(4) 0.7000(10) 0.0502(8) 0.1671(19) Uani 1 1 d . U . . .
O4 O 0.1137(4) 0.9245(8) 0.3872(8) 0.1575(17) Uani 1 1 d D U . . .
O5 O 0.0527(4) 0.8589(9) 0.3151(7) 0.1569(17) Uani 1 1 d . U . . .
O7 O 0.4461(3) 0.500000 0.3812(6) 0.065(2) Uani 1 2 d S T P . .
O8 O 0.4713(3) 0.500000 0.6255(6) 0.064(2) Uani 1 2 d S T P . .
O9 O 0.4576(2) 0.4055(4) 0.5017(4) 0.0637(15) Uani 1 1 d . . . . .
O10 O 0.4904(5) 0.7236(8) 0.4256(8) 0.148(5) Uani 1 1 d . . . . .
O6 O 0.4724(3) 0.5580(6) 0.2163(5) 0.105(3) Uani 1 1 d . . . . .
C1 C 0.3704(7) 0.6174(14) 0.3379(13) 0.1592(16) Uani 1 1 d . U . . .
C4 C 0.2929(4) 0.7268(7) 0.1666(7) 0.1613(16) Uani 1 1 d G U . . .
H4 H 0.295479 0.763359 0.123991 0.194 Uiso 1 1 calc R U . . .
C5 C 0.2500(3) 0.7014(8) 0.1746(7) 0.1615(15) Uani 1 1 d G U . . .
C6 C 0.2462(3) 0.6478(8) 0.2370(8) 0.1614(16) Uani 1 1 d DG U . . .
H6 H 0.216918 0.630464 0.242475 0.194 Uiso 1 1 calc R U . . .
C7 C 0.2852(4) 0.6197(6) 0.2914(8) 0.1608(16) Uani 1 1 d DG U . . .
H7 H 0.282571 0.583154 0.334097 0.193 Uiso 1 1 calc R U . . .
C2 C 0.3280(3) 0.6452(8) 0.2835(7) 0.1602(16) Uani 1 1 d DG U . . .
C3 C 0.3319(3) 0.6987(8) 0.2211(8) 0.1609(16) Uani 1 1 d G U . . .
H3 H 0.361133 0.716048 0.215615 0.193 Uiso 1 1 calc R U . . .
C8 C 0.2128(7) 0.7454(15) 0.1079(12) 0.1619(15) Uani 1 1 d . U . . .
H8 H 0.225907 0.785194 0.076782 0.194 Uiso 1 1 calc R U . . .
C9 C 0.1784(4) 0.7706(8) 0.1703(8) 0.1612(15) Uani 1 1 d G U . . .
C10 C 0.1961(3) 0.8251(8) 0.2293(8) 0.1609(16) Uani 1 1 d G U . . .
H10 H 0.227155 0.838860 0.234062 0.193 Uiso 1 1 calc R U . . .
C11 C 0.1685(4) 0.8595(7) 0.2812(7) 0.1603(16) Uani 1 1 d G U . . .
H11 H 0.180683 0.896726 0.321550 0.192 Uiso 1 1 calc R U . . .
C12 C 0.1232(4) 0.8393(8) 0.2742(8) 0.1593(16) Uani 1 1 d G U . . .
C13 C 0.1054(3) 0.7848(8) 0.2152(8) 0.1602(16) Uani 1 1 d G U . . .
H13 H 0.074399 0.771050 0.210450 0.192 Uiso 1 1 calc R U . . .
C14 C 0.1330(4) 0.7504(7) 0.1633(7) 0.1608(16) Uani 1 1 d G U . . .
H14 H 0.120870 0.713183 0.122961 0.193 Uiso 1 1 calc R U . . .
C15 C 0.0949(6) 0.8813(10) 0.3293(11) 0.1579(16) Uani 1 1 d D U . . .
C16 C 0.4777(7) 0.500000 0.1803(10) 0.106(3) Uani 1 2 d DS TU P . .
C17 C 0.4890(7) 0.500000 0.0876(10) 0.107(3) Uani 1 2 d DS TU P . .
C18 C 0.4942(5) 0.4371(8) 0.0442(8) 0.107(3) Uani 1 1 d . U . . .
H18 H 0.489888 0.393516 0.073390 0.128 Uiso 1 1 calc 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
Tb1 Tb1 3.9461(13) 2_656 ?
Tb1 Tb1 3.9640(19) 6_565 ?
Tb1 Tb2 3.9228(10) . ?
Tb1 Tb2 3.9109(12) 5_666 ?
Tb1 O1 2.342(12) . ?
Tb1 O5 2.366(11) 8_565 ?
Tb1 O7 2.337(4) . ?
Tb1 O8 2.356(4) 5_666 ?
Tb1 O9 2.343(6) 6_565 ?
Tb1 O9 2.365(7) 5_666 ?
Tb1 O10 2.412(14) . ?
Tb1 O6 2.337(8) . ?
Tb2 O2 2.360(14) 6_565 ?
Tb2 O2 2.360(14) . ?
Tb2 O4 2.314(11) 7_566 ?
Tb2 O4 2.314(11) 4_546 ?
Tb2 O7 2.342(7) . ?
Tb2 O8 2.314(9) . ?
Tb2 O9 2.315(6) . ?
Tb2 O9 2.315(6) 6_565 ?
O1 C1 1.26(2) . ?
O2 C1 1.28(3) . ?
O3 C8 1.32(3) . ?
O4 C15 1.2401(10) . ?
O5 C15 1.31(2) . ?
O6 C16 1.241(11) . ?
C1 C2 1.46(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C5 C6 1.3900 . ?
C5 C8 1.58(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.3900 . ?
C7 H7 0.9500 . ?
C7 C2 1.3900 . ?
C2 C3 1.3900 . ?
C3 H3 0.9500 . ?
C8 H8 1.0000 . ?
C8 C9 1.579(18) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 H10 0.9500 . ?
C10 C11 1.3900 . ?
C11 H11 0.9500 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C15 1.506(17) . ?
C13 H13 0.9500 . ?
C13 C14 1.3900 . ?
C14 H14 0.9500 . ?
C16 C17 1.476(9) . ?
C17 C18 1.374(15) . ?
C17 C18 1.374(15) 6_565 ?
C18 C18 1.418(19) 2_655 ?
C18 H18 0.9500 . ?

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 90.0 2_656 6_565 ?
Tb2 Tb1 Tb1 59.651(14) . 6_565 ?
Tb2 Tb1 Tb1 59.550(15) 5_666 6_565 ?
Tb2 Tb1 Tb1 59.604(19) . 2_656 ?
Tb2 Tb1 Tb1 59.90(2) 5_666 2_656 ?
Tb2 Tb1 Tb2 88.88(2) 5_666 . ?
O1 Tb1 Tb1 108.4(3) . 2_656 ?
O1 Tb1 Tb1 104.1(4) . 6_565 ?
O1 Tb1 Tb2 69.0(4) . . ?
O1 Tb1 Tb2 157.6(4) . 5_666 ?
O1 Tb1 O5 133.1(5) . 8_565 ?
O1 Tb1 O8 136.1(5) . 5_666 ?
O1 Tb1 O9 77.7(3) . 6_565 ?
O1 Tb1 O9 141.0(3) . 5_666 ?
O1 Tb1 O10 82.7(5) . . ?
O5 Tb1 Tb1 106.8(4) 8_565 6_565 ?
O5 Tb1 Tb1 106.1(3) 8_565 2_656 ?
O5 Tb1 Tb2 157.9(4) 8_565 . ?
O5 Tb1 Tb2 69.1(4) 8_565 5_666 ?
O5 Tb1 O10 81.4(5) 8_565 . ?
O7 Tb1 Tb1 31.98(17) . 6_565 ?
O7 Tb1 Tb1 85.0(2) . 2_656 ?
O7 Tb1 Tb2 83.8(2) . 5_666 ?
O7 Tb1 Tb2 33.08(17) . . ?
O7 Tb1 O1 75.8(5) . . ?
O7 Tb1 O5 138.4(5) . 8_565 ?
O7 Tb1 O8 63.9(3) . 5_666 ?
O7 Tb1 O9 64.7(2) . 6_565 ?
O7 Tb1 O9 97.8(3) . 5_666 ?
O7 Tb1 O10 138.3(3) . . ?
O8 Tb1 Tb1 85.5(2) 5_666 2_656 ?
O8 Tb1 Tb1 32.74(17) 5_666 6_565 ?
O8 Tb1 Tb2 84.83(17) 5_666 . ?
O8 Tb1 Tb2 32.80(19) 5_666 5_666 ?
O8 Tb1 O5 76.9(4) 5_666 8_565 ?
O8 Tb1 O9 65.0(3) 5_666 5_666 ?
O8 Tb1 O10 139.8(4) 5_666 . ?
O9 Tb1 Tb1 33.23(16) 6_565 2_656 ?
O9 Tb1 Tb1 85.23(16) 5_666 6_565 ?
O9 Tb1 Tb1 32.87(14) 5_666 2_656 ?
O9 Tb1 Tb1 85.18(17) 6_565 6_565 ?
O9 Tb1 Tb2 32.92(15) 5_666 5_666 ?
O9 Tb1 Tb2 32.41(16) 6_565 . ?
O9 Tb1 Tb2 84.72(15) 5_666 . ?
O9 Tb1 Tb2 85.28(16) 6_565 5_666 ?
O9 Tb1 O5 138.8(3) 6_565 8_565 ?
O9 Tb1 O5 76.4(3) 5_666 8_565 ?
O9 Tb1 O8 98.9(3) 6_565 5_666 ?
O9 Tb1 O9 65.2(2) 6_565 5_666 ?
O9 Tb1 O10 76.1(3) 6_565 . ?
O9 Tb1 O10 77.2(4) 5_666 . ?
O10 Tb1 Tb1 68.4(3) . 2_656 ?
O10 Tb1 Tb1 158.4(3) . 6_565 ?
O10 Tb1 Tb2 107.4(4) . 5_666 ?
O10 Tb1 Tb2 105.7(3) . . ?
O6 Tb1 Tb1 157.5(3) . 2_656 ?
O6 Tb1 Tb1 67.7(3) . 6_565 ?
O6 Tb1 Tb2 107.7(2) . . ?
O6 Tb1 Tb2 104.0(2) . 5_666 ?
O6 Tb1 O1 80.7(4) . . ?
O6 Tb1 O5 79.4(4) . 8_565 ?
O6 Tb1 O7 77.3(3) . . ?
O6 Tb1 O8 74.4(3) . 5_666 ?
O6 Tb1 O9 139.8(3) . 6_565 ?
O6 Tb1 O9 136.3(3) . 5_666 ?
O6 Tb1 O10 133.9(4) . . ?
Tb1 Tb2 Tb1 60.49(2) 5_666 6_565 ?
Tb1 Tb2 Tb1 60.70(3) 6_565 . ?
Tb1 Tb2 Tb1 60.49(2) 2_656 . ?
Tb1 Tb2 Tb1 91.12(2) 5_666 . ?
Tb1 Tb2 Tb1 91.12(2) 2_656 6_565 ?
Tb1 Tb2 Tb1 60.90(3) 2_656 5_666 ?
O2 Tb2 Tb1 161.2(3) 6_565 2_656 ?
O2 Tb2 Tb1 107.5(4) 6_565 5_666 ?
O2 Tb2 Tb1 107.5(4) . 2_656 ?
O2 Tb2 Tb1 107.7(3) . 6_565 ?
O2 Tb2 Tb1 70.1(3) 6_565 6_565 ?
O2 Tb2 Tb1 70.1(3) . . ?
O2 Tb2 Tb1 107.7(3) 6_565 . ?
O2 Tb2 Tb1 161.2(3) . 5_666 ?
O2 Tb2 O2 79.2(8) 6_565 . ?
O4 Tb2 Tb1 109.0(4) 4_546 6_565 ?
O4 Tb2 Tb1 70.4(3) 4_546 5_666 ?
O4 Tb2 Tb1 161.5(3) 7_566 6_565 ?
O4 Tb2 Tb1 161.5(3) 4_546 . ?
O4 Tb2 Tb1 109.0(4) 7_566 . ?
O4 Tb2 Tb1 106.8(3) 7_566 5_666 ?
O4 Tb2 Tb1 70.4(3) 7_566 2_656 ?
O4 Tb2 Tb1 106.8(3) 4_546 2_656 ?
O4 Tb2 O2 128.4(5) 4_546 . ?
O4 Tb2 O2 128.4(5) 7_566 6_565 ?
O4 Tb2 O2 80.5(5) 4_546 6_565 ?
O4 Tb2 O2 80.5(4) 7_566 . ?
O4 Tb2 O4 76.1(7) 7_566 4_546 ?
O4 Tb2 O7 141.4(4) 7_566 . ?
O4 Tb2 O7 141.4(4) 4_546 . ?
O4 Tb2 O8 77.0(3) 7_566 . ?
O4 Tb2 O8 77.0(3) 4_546 . ?
O4 Tb2 O9 139.5(4) 7_566 . ?
O4 Tb2 O9 79.0(4) 4_546 . ?
O4 Tb2 O9 139.5(4) 4_546 6_565 ?
O4 Tb2 O9 79.0(4) 7_566 6_565 ?
O7 Tb2 Tb1 85.7(2) . 5_666 ?
O7 Tb2 Tb1 32.99(9) . 6_565 ?
O7 Tb2 Tb1 85.7(2) . 2_656 ?
O7 Tb2 Tb1 32.99(9) . . ?
O7 Tb2 O2 78.3(3) . . ?
O7 Tb2 O2 78.3(3) . 6_565 ?
O8 Tb2 Tb1 86.64(16) . 6_565 ?
O8 Tb2 Tb1 33.48(8) . 2_656 ?
O8 Tb2 Tb1 33.48(8) . 5_666 ?
O8 Tb2 Tb1 86.64(16) . . ?
O8 Tb2 O2 140.1(4) . . ?
O8 Tb2 O2 140.1(4) . 6_565 ?
O8 Tb2 O7 99.7(3) . . ?
O8 Tb2 O9 66.48(19) . . ?
O8 Tb2 O9 66.49(19) . 6_565 ?
O9 Tb2 Tb1 32.84(15) 6_565 . ?
O9 Tb2 Tb1 87.13(17) . 2_656 ?
O9 Tb2 Tb1 33.73(16) 6_565 2_656 ?
O9 Tb2 Tb1 33.73(16) . 5_666 ?
O9 Tb2 Tb1 86.51(15) . . ?
O9 Tb2 Tb1 86.51(15) 6_565 6_565 ?
O9 Tb2 Tb1 87.13(17) 6_565 5_666 ?
O9 Tb2 Tb1 32.84(15) . 6_565 ?
O9 Tb2 O2 139.5(3) 6_565 6_565 ?
O9 Tb2 O2 77.2(4) . 6_565 ?
O9 Tb2 O2 139.5(3) . . ?
O9 Tb2 O2 77.2(4) 6_565 . ?
O9 Tb2 O7 65.1(2) 6_565 . ?
O9 Tb2 O7 65.1(2) . . ?
O9 Tb2 O9 100.9(3) 6_565 . ?
C1 O1 Tb1 137.6(15) . . ?
C1 O2 Tb2 133.8(12) . . ?
C15 O4 Tb2 136.6(11) . 7_566 ?
C15 O5 Tb1 134.8(12) . 8_465 ?
Tb1 O7 Tb1 116.0(3) 6_565 . ?
Tb1 O7 Tb2 113.9(2) . . ?
Tb1 O7 Tb2 113.9(2) 6_565 . ?
Tb1 O8 Tb1 114.5(3) 2_656 5_666 ?
Tb2 O8 Tb1 113.7(2) . 2_656 ?
Tb2 O8 Tb1 113.7(2) . 5_666 ?
Tb1 O9 Tb1 113.9(2) 6_565 5_666 ?
Tb2 O9 Tb1 113.4(3) . 5_666 ?
Tb2 O9 Tb1 114.7(3) . 6_565 ?
C16 O6 Tb1 136.7(10) . . ?
O1 C1 O2 127.9(19) . . ?
O1 C1 C2 120(2) . . ?
O2 C1 C2 112.3(18) . . ?
C5 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C8 108.3(13) . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C8 131.7(13) . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C2 120.0 . . ?
C2 C7 H7 120.0 . . ?
C7 C2 C1 122.7(14) . . ?
C3 C2 C1 117.3(14) . . ?
C3 C2 C7 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
O3 C8 C5 107(2) . . ?
O3 C8 H8 113.4 . . ?
O3 C8 C9 104.3(16) . . ?
C5 C8 H8 113.4 . . ?
C5 C8 C9 104.5(13) . . ?
C9 C8 H8 113.4 . . ?
C10 C9 C8 112.3(13) . . ?
C10 C9 C14 120.0 . . ?
C14 C9 C8 127.2(12) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C15 116.9(10) . . ?
C13 C12 C15 123.1(10) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C9 C14 H14 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
O4 C15 O5 128.4(15) . . ?
O4 C15 C12 119.7(15) . . ?
O5 C15 C12 111.3(12) . . ?
O6 C16 O6 123.8(13) . 6_565 ?
O6 C16 C17 118.1(6) 6_565 . ?
O6 C16 C17 118.1(6) . . ?
C18 C17 C16 120.1(7) . . ?
C18 C17 C16 120.1(7) 6_565 . ?
C18 C17 C18 119.7(13) . 6_565 ?
C17 C18 C18 120.1(7) . 2_655 ?
C17 C18 H18 119.9 . . ?
C18 C18 H18 119.9 2_655 . ?

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 O1 C1 O2 12(4) . . . . ?
Tb1 O1 C1 C2 -173.1(11) . . . . ?
Tb1 O5 C15 O4 12(4) 8_465 . . . ?
Tb1 O5 C15 C12 -176.5(10) 8_465 . . . ?
Tb1 O6 C16 O6 36(3) . . . 6_565 ?
Tb1 O6 C16 C17 -147.3(13) . . . . ?
Tb2 O2 C1 O1 -18(4) . . . . ?
Tb2 O2 C1 C2 166.2(11) . . . . ?
Tb2 O4 C15 O5 -7(4) 7_566 . . . ?
Tb2 O4 C15 C12 -177.6(11) 7_566 . . . ?
O1 C1 C2 C7 169.8(16) . . . . ?
O1 C1 C2 C3 -10(3) . . . . ?
O2 C1 C2 C7 -14(2) . . . . ?
O2 C1 C2 C3 166.4(14) . . . . ?
O3 C8 C9 C10 -173.2(14) . . . . ?
O3 C8 C9 C14 -2(2) . . . . ?
O6 C16 C17 C18 1(3) . . . 6_565 ?
O6 C16 C17 C18 -1(3) 6_565 . . . ?
O6 C16 C17 C18 178.4(18) 6_565 . . 6_565 ?
O6 C16 C17 C18 -178.4(18) . . . . ?
C1 C2 C3 C4 179.4(15) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C8 O3 120.9(14) . . . . ?
C4 C5 C8 C9 -128.8(14) . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C5 C8 C9 C10 74.5(18) . . . . ?
C5 C8 C9 C14 -113.8(14) . . . . ?
C6 C5 C8 O3 -61.9(17) . . . . ?
C6 C5 C8 C9 48(2) . . . . ?
C6 C7 C2 C1 -179.3(15) . . . . ?
C6 C7 C2 C3 0.0 . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C5 C8 177.6(13) . . . . ?
C8 C5 C6 C7 -176.9(16) . . . . ?
C8 C9 C10 C11 172.3(14) . . . . ?
C8 C9 C14 C13 -171.1(16) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C15 -177.2(14) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C11 C12 C15 O4 -10(2) . . . . ?
C11 C12 C15 O5 178.1(13) . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C13 C12 C15 O4 173.0(15) . . . . ?
C13 C12 C15 O5 1(2) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C15 C12 C13 C14 177.0(15) . . . . ?
C16 C17 C18 C18 -179(2) . . . 2_655 ?
C18 C17 C18 C18 2(4) 6_565 . . 2_655 ?

_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 -0.810 -0.718 -0.533 5401.9 973.3 ?


_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
;
# start Validation Reply Form
_vrf_PLAT973_lk3_8_3_newabscorr  
;
RESPONSE: We report the best dataset collected for this compound. We collected 
data from several crystals and applied absorption correction for each dataset 
but there is still residual density around the metal ions. Considering that 
this compound is a result of a single crystal to single crystal post synthetic 
modification at relatively high temperature it is expected that the quality of 
the single crystals will be significantly worse than that of the single crystals 
of the initial compound.
;
_vrf_PLAT971_lk3_8_3_newabscorr  
;
RESPONSE: We report the best dataset collected for this compound. We collected 
data from several crystals and applied absorption correction for each dataset 
but there is still residual density around the metal ions. Considering that 
this compound is a result of a single crystal to single crystal post synthetic 
modification at relatively high temperature it is expected that the quality of 
the single crystals will be significantly worse than that of the single crystals 
of the initial compound.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_y_bcpm
_database_code_depnum_ccdc_archive 'CCDC 2338729'
loop_
_audit_author_name
_audit_author_address
'Laoura Komodiki'
;University of Cyprus
Cyprus
;
_audit_update_record             
;
2024-03-08 deposited with the CCDC.	2024-04-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H18 N O19 Y3'
_chemical_formula_sum            'C30 H18 N O19 Y3'
_chemical_formula_weight         963.18
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Y O N C H'
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'
N N 0.0311 0.0180 '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'
Y Y -0.2670 2.0244 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   29.6715(3)
_cell_length_b                   18.3115(2)
_cell_length_c                   14.59890(10)
_cell_angle_alpha                90
_cell_angle_beta                 101.9510(10)
_cell_angle_gamma                90
_cell_volume                     7760.09(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23844
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.0470
_cell_measurement_theta_min      2.8520
_shelx_estimated_absorpt_T_max   0.937
_shelx_estimated_absorpt_T_min   0.590
_exptl_absorpt_coefficient_mu    3.276
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    0.824
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42780
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.991
_diffrn_reflns_theta_max         66.991
_diffrn_reflns_theta_min         2.853
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -94.00 -33.00   0.50    0.30    -- -106.00  77.00 -60.00  122
  2  ω    -94.00 -38.00   0.50    0.30    -- -106.00  77.00 -30.00  112
  3  ω    -71.00 -46.00   0.50    0.30    -- -106.00  61.00   0.00   50
  4  ω    -89.00 -34.00   0.50    0.30    -- -106.00  77.00 120.00  110
  5  ω    -63.00 -32.00   0.50    0.30    -- -106.00  56.00 134.00   62
  6  ω    -63.00 -21.00   0.50    0.10    --  -42.57  56.00 134.00   84
  7  ω    -16.00  28.00   0.50    0.10    --  -42.57  56.00 134.00   88
  8  ω    -29.00  34.00   0.50    0.10    --  -42.57  19.00 120.00  126
  9  ω   -115.00 -22.00   0.50    0.10    --  -42.57 -56.00  -7.00  186
 10  ω   -154.00-117.00   0.50    0.30    -- -106.00 -95.00  90.00   74
 11  ω   -177.00 -82.00   0.50    0.30    -- -106.00 -61.00  60.00  190
 12  ω   -176.00 -91.00   0.50    0.30    -- -106.00 -56.00  -7.00  170
 13  ω   -107.00 -33.00   0.50    0.30    -- -106.00 105.00-146.11  148
 14  ω    -90.00 -20.00   0.50    0.10    --  -42.57 126.00-150.00  140
 15  ω    -66.00 -33.00   0.50    0.30    -- -106.00 126.00 -90.00   66
 16  ω   -112.00 -76.00   0.50    0.30    -- -106.00 126.00 -90.00   72
 17  ω   -112.00 -36.00   0.50    0.30    -- -106.00 126.00 120.00  152
 18  ω     29.00  95.00   0.50    0.10    --   42.57-126.00  30.00  132
 19  ω     41.00  67.00   0.50    0.30    --  107.12-126.00  30.00   52
 20  ω     71.00  96.00   0.50    0.30    --  107.12-126.00  30.00   50
 21  ω     80.00 106.00   0.50    0.30    --  107.12 -95.00 -30.00   52
 22  ω     34.00  97.00   0.50    0.30    --  107.12 -95.00  30.00  126
 23  ω     13.00  52.00   0.50    0.10    --   42.57-126.00 -90.00   78
 24  ω     45.00  79.00   0.50    0.30    --  107.12-126.00-120.00   68
 25  ω     85.00 111.00   0.50    0.30    --  107.12-126.00-120.00   52
 26  ω     77.00 102.00   0.50    0.30    --  107.12 -95.00  60.00   50
 27  ω     76.00 101.00   0.50    0.30    --  107.12 -77.00  90.00   50
 28  ω     35.00  60.00   0.50    0.30    --  107.12 -56.00  -7.00   50
 29  ω     46.00  71.00   0.50    0.30    --  107.12 -61.00   0.00   50
 30  ω    -27.00   5.00   0.50    0.10    --   42.57 -56.00  -7.00   64
 31  ω    -35.00  -9.00   0.50    0.10    --   42.57 -19.00-180.00   52
 32  ω     34.00  60.00   0.50    0.30    --  107.12 -61.00-150.00   52
 33  ω    152.00 177.00   0.50    0.30    --  107.12  30.00 -90.00   50
 34  ω     95.00 175.00   0.50    0.30    --  107.12  61.00-180.00  160
 35  ω     87.00 167.00   0.50    0.30    --  107.12  61.00  60.00  160
 36  ω    104.00 168.00   0.50    0.30    --  107.12  45.00  90.00  128
 37  ω     87.00 178.00   0.50    0.30    --  107.12  56.00 134.00  182
 38  ω     26.00 117.00   0.50    0.10    --   42.57  56.00 134.00  182
 39  ω    100.00 141.00   0.50    0.30    --  107.12  30.00 -90.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0158496000
_diffrn_orient_matrix_UB_12      0.0433676000
_diffrn_orient_matrix_UB_13      -0.0914608000
_diffrn_orient_matrix_UB_21      -0.0317127000
_diffrn_orient_matrix_UB_22      0.0467227000
_diffrn_orient_matrix_UB_23      0.0476919000
_diffrn_orient_matrix_UB_31      0.0394786000
_diffrn_orient_matrix_UB_32      0.0548988000
_diffrn_orient_matrix_UB_33      0.0316281000
_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                6351
_reflns_number_total             7147
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.551
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         7147
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1435P)²+6.4481P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.1988
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C8-O3
 1.35 with sigma of 0.01
 O9-Y1
 2.25 with sigma of 0.001
3. Rigid bond restraints
 O6, O7, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
5.a Ternary CH refined with riding coordinates:
 C8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_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
Y1 Y 0.51814(2) 0.60509(2) 0.13514(2) 0.05718(18) Uani 1 1 d D . . . .
Y2 Y 0.40920(2) 0.500000 0.01388(3) 0.06060(19) Uani 1 2 d S T P . .
O1 O 0.45529(11) 0.6445(2) 0.1935(2) 0.0788(8) Uani 1 1 d . . . . .
O2 O 0.39281(11) 0.5814(2) 0.1225(2) 0.0787(8) Uani 1 1 d . . . . .
O3 O 0.32311(18) 0.8332(4) 0.4537(3) 0.189(4) Uani 1 1 d D . . . .
O4 O 0.13604(10) 0.9205(2) 0.0884(2) 0.0754(8) Uani 1 1 d . . . . .
O5 O 0.09438(10) 0.8601(2) 0.1759(2) 0.0790(8) Uani 1 1 d . . . . .
O8 O 0.47568(11) 0.500000 0.1299(2) 0.0497(7) Uani 1 2 d S T P . .
O9 O 0.55582(7) 0.500000 0.1188(2) 0.0485(7) Uani 1 2 d DS T P . .
O10 O 0.54117(8) 0.59753(14) -0.00581(16) 0.0516(6) Uani 1 1 d . . . . .
O11 O 0.51276(18) 0.7250(2) 0.0877(5) 0.1353(19) Uani 1 1 d . . . . .
O6 O 0.53693(12) 0.5650(3) 0.2874(2) 0.0930(11) Uani 1 1 d . U . . .
O7 O 0.5521(4) 0.500000 0.4352(7) 0.207(5) Uani 1 2 d S TU P . .
N1 N 0.5394(3) 0.500000 0.3238(6) 0.113(2) Uani 1 2 d S TU P . .
C1 C 0.41426(17) 0.6284(3) 0.1802(3) 0.0720(11) Uani 1 1 d . . . . .
C2 C 0.38481(16) 0.6696(3) 0.2364(3) 0.0827(14) Uani 1 1 d . . . . .
C3 C 0.4009(2) 0.7298(4) 0.2850(4) 0.0990(17) Uani 1 1 d . . . . .
H3 H 0.430095 0.747241 0.283103 0.119 Uiso 1 1 calc R U . . .
C4 C 0.3738(2) 0.7667(4) 0.3386(4) 0.112(2) Uani 1 1 d . U . . .
H4 H 0.385579 0.807977 0.372374 0.134 Uiso 1 1 calc R U . . .
C5 C 0.33088(19) 0.7435(4) 0.3422(3) 0.105(2) Uani 1 1 d . U . . .
C6 C 0.31502(19) 0.6840(5) 0.2928(4) 0.126(3) Uani 1 1 d . U . . .
H6 H 0.285543 0.667491 0.294250 0.151 Uiso 1 1 calc R U . . .
C7 C 0.34112(18) 0.6456(5) 0.2388(4) 0.104(2) Uani 1 1 d . . . . .
H7 H 0.329048 0.604476 0.205015 0.125 Uiso 1 1 calc R U . . .
C8 C 0.3002(2) 0.7802(5) 0.3995(4) 0.127(3) Uani 1 1 d D . . . .
H8 H 0.291408 0.743200 0.441082 0.153 Uiso 1 1 calc R U . . .
C9 C 0.25652(18) 0.8073(4) 0.3360(3) 0.104(2) Uani 1 1 d . . . . .
C10 C 0.25735(18) 0.8605(4) 0.2705(4) 0.1003(19) Uani 1 1 d . . . . .
H10 H 0.285480 0.880409 0.264913 0.120 Uiso 1 1 calc R U . . .
C11 C 0.21767(18) 0.8852(3) 0.2126(4) 0.0875(15) Uani 1 1 d . . . . .
H11 H 0.219037 0.922155 0.169576 0.105 Uiso 1 1 calc R U . . .
C12 C 0.17561(15) 0.8548(3) 0.2189(3) 0.0744(12) Uani 1 1 d . . . . .
C13 C 0.17471(19) 0.8013(4) 0.2839(4) 0.0977(18) Uani 1 1 d . . . . .
H13 H 0.146965 0.779693 0.288875 0.117 Uiso 1 1 calc R U . . .
C14 C 0.2156(2) 0.7796(4) 0.3425(4) 0.113(2) Uani 1 1 d . . . . .
H14 H 0.214512 0.744501 0.387988 0.135 Uiso 1 1 calc R U . . .
C15 C 0.13185(16) 0.8810(3) 0.1561(3) 0.0707(11) 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
Y1 Y1 3.8488(7) 6_565 ?
Y1 Y1 3.8690(6) 2_655 ?
Y1 Y2 3.8763(5) 5_665 ?
Y1 Y2 3.8622(5) . ?
Y1 O1 2.320(3) . ?
Y1 O5 2.307(3) 8_565 ?
Y1 O8 2.2927(17) . ?
Y1 O9 2.2629(9) . ?
Y1 O10 2.303(2) . ?
Y1 O10 2.303(2) 2_655 ?
Y1 O11 2.298(4) . ?
Y1 O6 2.298(3) . ?
Y2 O2 2.301(3) . ?
Y2 O2 2.301(3) 6_565 ?
Y2 O4 2.307(3) 4_545 ?
Y2 O4 2.307(3) 7_565 ?
Y2 O8 2.318(3) . ?
Y2 O9 2.379(2) 5_665 ?
Y2 O10 2.333(2) 5_665 ?
Y2 O10 2.333(2) 2_655 ?
O1 C1 1.228(6) . ?
O2 C1 1.278(6) . ?
O3 C8 1.343(7) . ?
O4 C15 1.251(6) . ?
O5 C15 1.264(6) . ?
O6 N1 1.299(5) . ?
O7 N1 1.592(12) . ?
C1 C2 1.518(6) . ?
C2 C3 1.345(8) . ?
C2 C7 1.376(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.406(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.353(10) . ?
C5 C6 1.337(11) . ?
C5 C8 1.515(7) . ?
C6 H6 0.9300 . ?
C6 C7 1.404(8) . ?
C7 H7 0.9300 . ?
C8 H8 0.9800 . ?
C8 C9 1.513(7) . ?
C9 C10 1.368(10) . ?
C9 C14 1.336(10) . ?
C10 H10 0.9300 . ?
C10 C11 1.376(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.387(8) . ?
C12 C13 1.367(7) . ?
C12 C15 1.505(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.391(8) . ?
C14 H14 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
Y1 Y1 Y1 90.0 6_565 2_655 ?
Y1 Y1 Y2 59.821(9) 2_655 5_665 ?
Y1 Y1 Y2 60.233(6) 6_565 5_665 ?
Y1 Y1 Y2 60.115(6) 6_565 . ?
Y2 Y1 Y1 60.182(10) . 2_655 ?
Y2 Y1 Y2 90.305(12) . 5_665 ?
O1 Y1 Y1 108.13(9) . 6_565 ?
O1 Y1 Y1 107.42(8) . 2_655 ?
O1 Y1 Y2 160.61(9) . 5_665 ?
O1 Y1 Y2 70.32(9) . . ?
O5 Y1 Y1 108.29(8) 8_565 2_655 ?
O5 Y1 Y1 106.04(10) 8_565 6_565 ?
O5 Y1 Y2 69.64(9) 8_565 5_665 ?
O5 Y1 Y2 159.87(9) 8_565 . ?
O5 Y1 O1 129.75(13) 8_565 . ?
O8 Y1 Y1 32.93(6) . 6_565 ?
O8 Y1 Y1 86.03(8) . 2_655 ?
O8 Y1 Y2 33.32(8) . . ?
O8 Y1 Y2 85.99(7) . 5_665 ?
O8 Y1 O1 78.20(11) . . ?
O8 Y1 O5 138.02(12) . 8_565 ?
O8 Y1 O10 66.46(10) . 2_655 ?
O8 Y1 O10 100.50(10) . . ?
O8 Y1 O11 142.05(16) . . ?
O8 Y1 O6 77.63(14) . . ?
O9 Y1 Y1 31.74(4) . 6_565 ?
O9 Y1 Y1 86.08(8) . 2_655 ?
O9 Y1 Y2 34.34(6) . 5_665 ?
O9 Y1 Y2 85.00(6) . . ?
O9 Y1 O1 139.07(10) . . ?
O9 Y1 O5 77.44(11) . 8_565 ?
O9 Y1 O8 64.07(8) . . ?
O9 Y1 O10 99.95(10) . 2_655 ?
O9 Y1 O10 67.05(9) . . ?
O9 Y1 O11 141.81(14) . . ?
O9 Y1 O6 78.70(13) . . ?
O10 Y1 Y1 86.55(6) . 6_565 ?
O10 Y1 Y1 86.55(6) 2_655 6_565 ?
O10 Y1 Y1 32.86(6) 2_655 2_655 ?
O10 Y1 Y1 32.87(6) . 2_655 ?
O10 Y1 Y2 85.96(6) 2_655 5_665 ?
O10 Y1 Y2 86.30(6) . . ?
O10 Y1 Y2 33.51(6) . 5_665 ?
O10 Y1 Y2 33.84(6) 2_655 . ?
O10 Y1 O1 77.52(10) 2_655 . ?
O10 Y1 O1 139.17(10) . . ?
O10 Y1 O5 140.36(10) 2_655 8_565 ?
O10 Y1 O5 77.89(10) . 8_565 ?
O10 Y1 O10 65.27(10) . 2_655 ?
O11 Y1 Y1 72.88(17) . 2_655 ?
O11 Y1 Y1 162.87(17) . 6_565 ?
O11 Y1 Y2 109.80(15) . . ?
O11 Y1 Y2 108.51(14) . 5_665 ?
O11 Y1 O1 78.59(16) . . ?
O11 Y1 O5 79.44(17) . 8_565 ?
O11 Y1 O10 79.46(18) . 2_655 ?
O11 Y1 O10 78.66(17) . . ?
O6 Y1 Y1 71.36(12) . 6_565 ?
O6 Y1 Y1 161.32(12) . 2_655 ?
O6 Y1 Y2 109.43(10) . 5_665 ?
O6 Y1 Y2 107.26(11) . . ?
O6 Y1 O1 78.26(12) . . ?
O6 Y1 O5 79.07(13) . 8_565 ?
O6 Y1 O10 141.99(11) . . ?
O6 Y1 O10 139.91(12) . 2_655 ?
O6 Y1 O11 125.8(2) . . ?
Y1 Y2 Y1 59.996(10) 6_565 5_665 ?
Y1 Y2 Y1 89.694(12) 6_565 2_655 ?
Y1 Y2 Y1 89.695(12) . 5_665 ?
Y1 Y2 Y1 59.531(12) 5_665 2_655 ?
Y1 Y2 Y1 59.997(10) . 2_655 ?
Y1 Y2 Y1 59.770(12) . 6_565 ?
O2 Y2 Y1 158.45(9) . 5_665 ?
O2 Y2 Y1 68.75(9) 6_565 6_565 ?
O2 Y2 Y1 106.45(8) . 6_565 ?
O2 Y2 Y1 106.45(8) 6_565 . ?
O2 Y2 Y1 68.75(9) . . ?
O2 Y2 Y1 106.67(9) . 2_655 ?
O2 Y2 Y1 158.45(9) 6_565 2_655 ?
O2 Y2 Y1 106.67(9) 6_565 5_665 ?
O2 Y2 O2 80.76(18) 6_565 . ?
O2 Y2 O4 132.64(12) . 4_545 ?
O2 Y2 O4 81.91(12) . 7_565 ?
O2 Y2 O4 81.91(12) 6_565 4_545 ?
O2 Y2 O4 132.64(12) 6_565 7_565 ?
O2 Y2 O8 76.46(10) . . ?
O2 Y2 O8 76.46(10) 6_565 . ?
O2 Y2 O9 138.70(9) 6_565 5_665 ?
O2 Y2 O9 138.70(9) . 5_665 ?
O2 Y2 O10 139.15(10) 6_565 2_655 ?
O2 Y2 O10 139.15(10) . 5_665 ?
O2 Y2 O10 76.38(11) 6_565 5_665 ?
O2 Y2 O10 76.38(11) . 2_655 ?
O4 Y2 Y1 107.56(9) 7_565 . ?
O4 Y2 Y1 105.48(8) 4_545 2_655 ?
O4 Y2 Y1 158.56(8) 7_565 6_565 ?
O4 Y2 Y1 158.56(8) 4_545 . ?
O4 Y2 Y1 68.90(8) 7_565 2_655 ?
O4 Y2 Y1 105.48(8) 7_565 5_665 ?
O4 Y2 Y1 68.90(8) 4_545 5_665 ?
O4 Y2 Y1 107.56(9) 4_545 6_565 ?
O4 Y2 O4 78.30(19) 4_545 7_565 ?
O4 Y2 O8 139.97(9) 4_545 . ?
O4 Y2 O8 139.97(9) 7_565 . ?
O4 Y2 O9 76.51(9) 4_545 5_665 ?
O4 Y2 O9 76.51(9) 7_565 5_665 ?
O4 Y2 O10 76.87(11) 4_545 5_665 ?
O4 Y2 O10 137.68(10) 7_565 5_665 ?
O4 Y2 O10 137.68(10) 4_545 2_655 ?
O4 Y2 O10 76.87(11) 7_565 2_655 ?
O8 Y2 Y1 85.52(7) . 5_665 ?
O8 Y2 Y1 32.91(3) . 6_565 ?
O8 Y2 Y1 32.91(3) . . ?
O8 Y2 Y1 85.52(7) . 2_655 ?
O8 Y2 O9 98.39(10) . 5_665 ?
O8 Y2 O10 65.57(7) . 5_665 ?
O8 Y2 O10 65.57(7) . 2_655 ?
O9 Y2 Y1 84.74(6) 5_665 . ?
O9 Y2 Y1 84.74(6) 5_665 6_565 ?
O9 Y2 Y1 32.45(2) 5_665 2_655 ?
O9 Y2 Y1 32.45(2) 5_665 5_665 ?
O10 Y2 Y1 33.35(6) 2_655 . ?
O10 Y2 Y1 85.84(6) 2_655 6_565 ?
O10 Y2 Y1 33.35(6) 5_665 6_565 ?
O10 Y2 Y1 85.84(6) 5_665 . ?
O10 Y2 Y1 33.02(6) 5_665 5_665 ?
O10 Y2 Y1 85.50(6) 2_655 5_665 ?
O10 Y2 Y1 33.02(6) 2_655 2_655 ?
O10 Y2 Y1 85.50(6) 5_665 2_655 ?
O10 Y2 O9 64.70(7) 2_655 5_665 ?
O10 Y2 O9 64.70(7) 5_665 5_665 ?
O10 Y2 O10 99.90(12) 2_655 5_665 ?
C1 O1 Y1 135.5(3) . . ?
C1 O2 Y2 138.0(3) . . ?
C15 O4 Y2 137.4(3) . 7_565 ?
C15 O5 Y1 136.0(3) . 8_465 ?
Y1 O8 Y1 114.14(13) . 6_565 ?
Y1 O8 Y2 113.77(9) . . ?
Y1 O8 Y2 113.77(9) 6_565 . ?
Y1 O9 Y1 116.51(8) 6_565 . ?
Y1 O9 Y2 113.21(8) 6_565 5_665 ?
Y1 O9 Y2 113.21(8) . 5_665 ?
Y1 O10 Y1 114.27(10) . 2_655 ?
Y1 O10 Y2 113.47(10) . 5_665 ?
Y1 O10 Y2 112.82(10) 2_655 5_665 ?
N1 O6 Y1 132.1(4) . . ?
O6 N1 O6 132.7(7) 6_565 . ?
O6 N1 O7 113.5(4) . . ?
O6 N1 O7 113.5(4) 6_565 . ?
O1 C1 O2 127.5(4) . . ?
O1 C1 C2 117.3(5) . . ?
O2 C1 C2 115.3(4) . . ?
C3 C2 C1 120.8(5) . . ?
C3 C2 C7 118.8(5) . . ?
C7 C2 C1 120.4(5) . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.5(6) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.4(7) . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C8 124.0(7) . . ?
C6 C5 C4 117.6(5) . . ?
C6 C5 C8 118.3(6) . . ?
C5 C6 H6 118.7 . . ?
C5 C6 C7 122.6(6) . . ?
C7 C6 H6 118.7 . . ?
C2 C7 C6 119.1(7) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
O3 C8 C5 110.9(6) . . ?
O3 C8 H8 107.6 . . ?
O3 C8 C9 112.9(6) . . ?
C5 C8 H8 107.6 . . ?
C9 C8 C5 110.0(4) . . ?
C9 C8 H8 107.6 . . ?
C10 C9 C8 121.7(6) . . ?
C14 C9 C8 120.4(6) . . ?
C14 C9 C10 117.9(5) . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 121.8(6) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.6(6) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C15 120.4(5) . . ?
C13 C12 C11 118.7(5) . . ?
C13 C12 C15 120.9(5) . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.4(6) . . ?
C14 C13 H13 120.3 . . ?
C9 C14 C13 122.5(6) . . ?
C9 C14 H14 118.7 . . ?
C13 C14 H14 118.7 . . ?
O4 C15 O5 126.2(4) . . ?
O4 C15 C12 116.8(4) . . ?
O5 C15 C12 116.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C1 O2 -1.9(8) . . . . ?
Y1 O1 C1 C2 179.6(3) . . . . ?
Y1 O5 C15 O4 -17.1(8) 8_465 . . . ?
Y1 O5 C15 C12 164.2(3) 8_465 . . . ?
Y1 O6 N1 O6 8.5(13) . . . 6_565 ?
Y1 O6 N1 O7 -177.5(5) . . . . ?
Y2 O2 C1 O1 0.5(9) . . . . ?
Y2 O2 C1 C2 179.1(3) . . . . ?
Y2 O4 C15 O5 18.6(8) 7_565 . . . ?
Y2 O4 C15 C12 -162.7(3) 7_565 . . . ?
O1 C1 C2 C3 12.1(8) . . . . ?
O1 C1 C2 C7 -167.6(5) . . . . ?
O2 C1 C2 C3 -166.6(5) . . . . ?
O2 C1 C2 C7 13.6(7) . . . . ?
O3 C8 C9 C10 60.4(8) . . . . ?
O3 C8 C9 C14 -119.5(8) . . . . ?
C1 C2 C3 C4 -178.5(5) . . . . ?
C1 C2 C7 C6 178.8(6) . . . . ?
C2 C3 C4 C5 -0.8(10) . . . . ?
C3 C2 C7 C6 -0.9(9) . . . . ?
C3 C4 C5 C6 0.0(10) . . . . ?
C3 C4 C5 C8 179.2(6) . . . . ?
C4 C5 C6 C7 0.3(11) . . . . ?
C4 C5 C8 O3 -6.8(9) . . . . ?
C4 C5 C8 C9 118.8(7) . . . . ?
C5 C6 C7 C2 0.2(11) . . . . ?
C5 C8 C9 C10 -64.0(9) . . . . ?
C5 C8 C9 C14 116.1(7) . . . . ?
C6 C5 C8 O3 172.4(7) . . . . ?
C6 C5 C8 C9 -62.1(9) . . . . ?
C7 C2 C3 C4 1.2(9) . . . . ?
C8 C5 C6 C7 -179.0(6) . . . . ?
C8 C9 C10 C11 -180.0(5) . . . . ?
C8 C9 C14 C13 -178.2(6) . . . . ?
C9 C10 C11 C12 -1.4(9) . . . . ?
C10 C9 C14 C13 1.9(10) . . . . ?
C10 C11 C12 C13 1.0(8) . . . . ?
C10 C11 C12 C15 -179.9(5) . . . . ?
C11 C12 C13 C14 0.8(8) . . . . ?
C11 C12 C15 O4 12.8(7) . . . . ?
C11 C12 C15 O5 -168.4(5) . . . . ?
C12 C13 C14 C9 -2.3(10) . . . . ?
C13 C12 C15 O4 -168.1(5) . . . . ?
C13 C12 C15 O5 10.8(7) . . . . ?
C14 C9 C10 C11 0.0(9) . . . . ?
C15 C12 C13 C14 -178.4(5) . . . . ?

_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 -0.036 -0.954 -0.028 5109.5 1183.8 ?


_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.746
