# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2023

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

data_jo2la_run123
_database_code_depnum_ccdc_archive 'CCDC 2269116'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H19 La O11'
_chemical_formula_sum            'C21 H19 La O11'
_chemical_formula_weight         586.27
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.215(3)
_cell_length_b                   12.467(3)
_cell_length_c                   10.233(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.01(3)
_cell_angle_gamma                90
_cell_volume                     2063.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4098
_cell_measurement_temperature    123
_cell_measurement_theta_max      29
_cell_measurement_theta_min      1
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.250
_exptl_absorpt_coefficient_mu    2.134
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26356
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.075
_diffrn_reflns_theta_min         1.259
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_device_type  'Australian Synchrotron, MX1 beamline'
_diffrn_measurement_method       ?
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4098
_reflns_number_total             4444
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.452
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0207
_refine_ls_restrained_S_all      1.096
_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)+(0.0303P)²+1.6292P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0540
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
1.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C20(H20), C21(H21), C24(H24), C26(H26), C27(H27),
 C28(H28), C31(H31), C32(H32), C33(H33), C34(H34)
1.c Idealised tetrahedral OH refined as rotating group:
 O11(H11), O12(H12), O16(H16)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.01052(2) 0.27004(2) 0.21743(2) 0.01052(5) Uani 1 1 d . . . . .
O7 O -0.05181(9) 0.44265(12) 0.31342(14) 0.0135(3) Uani 1 1 d . . . . .
O5 O 0.12517(10) 0.22808(13) 0.08618(16) 0.0183(3) Uani 1 1 d . . . . .
O4 O -0.07394(9) 0.20267(13) 0.38419(15) 0.0165(3) Uani 1 1 d . . . . .
C8 C 0.15351(12) 0.19097(17) -0.0158(2) 0.0130(4) Uani 1 1 d . . . . .
C9 C -0.12942(12) 0.17761(16) 0.4606(2) 0.0122(4) Uani 1 1 d . . . . .
O11 O 0.50134(9) 0.15888(15) -0.01907(17) 0.0240(4) Uani 1 1 d . . . . .
H11 H 0.515248 0.121471 -0.082169 0.036 Uiso 1 1 calc R U . . .
O12 O -0.45753(10) 0.13251(15) 0.24648(17) 0.0264(4) Uani 1 1 d . . . . .
H12 H -0.459622 0.142334 0.165109 0.040 Uiso 1 1 calc R U . . .
C13 C 0.29723(14) 0.23585(18) 0.0734(2) 0.0184(4) Uani 1 1 d . . . . .
H13 H 0.273888 0.277131 0.139558 0.022 Uiso 1 1 calc R U . . .
C14 C 0.38257(14) 0.23022(19) 0.0701(2) 0.0211(5) Uani 1 1 d . . . . .
H14 H 0.417387 0.269133 0.131777 0.025 Uiso 1 1 calc R U . . .
C15 C -0.18981(12) 0.50252(17) 0.26139(19) 0.0135(4) Uani 1 1 d . . . . .
O16 O -0.44320(9) 0.45907(14) 0.27283(18) 0.0245(4) Uani 1 1 d . . . . .
H16 H -0.469478 0.514739 0.249585 0.037 Uiso 1 1 calc R U . . .
C17 C -0.37654(13) 0.13820(19) 0.2967(2) 0.0195(4) Uani 1 1 d . . . . .
C18 C 0.24539(12) 0.18205(17) -0.01863(19) 0.0136(4) Uani 1 1 d . . . . .
C19 C -0.21523(12) 0.15717(17) 0.4027(2) 0.0139(4) Uani 1 1 d . . . . .
C20 C -0.23185(13) 0.15525(18) 0.2676(2) 0.0169(4) Uani 1 1 d . . . . .
H20 H -0.187766 0.160661 0.211498 0.020 Uiso 1 1 calc R U . . .
C21 C 0.28016(13) 0.12150(18) -0.1155(2) 0.0165(4) Uani 1 1 d . . . . .
H21 H 0.245314 0.085688 -0.179999 0.020 Uiso 1 1 calc R U . . .
C22 C 0.41652(13) 0.16715(19) -0.0242(2) 0.0184(4) Uani 1 1 d . . . . .
C23 C -0.35959(12) 0.47744(18) 0.2681(2) 0.0174(4) Uani 1 1 d . . . . .
C24 C -0.22213(13) 0.42386(17) 0.3400(2) 0.0152(4) Uani 1 1 d . . . . .
H24 H -0.185792 0.378757 0.391986 0.018 Uiso 1 1 calc R U . . .
C26 C -0.36101(13) 0.13615(19) 0.4319(2) 0.0199(4) Uani 1 1 d . . . . .
H26 H -0.405117 0.128094 0.487504 0.024 Uiso 1 1 calc R U . . .
C27 C -0.30691(13) 0.41095(18) 0.3429(2) 0.0174(4) Uani 1 1 d . . . . .
H27 H -0.328665 0.356766 0.395998 0.021 Uiso 1 1 calc R U . . .
C28 C -0.31244(14) 0.14550(19) 0.2145(2) 0.0202(4) Uani 1 1 d . . . . .
H28 H -0.323688 0.143819 0.122144 0.024 Uiso 1 1 calc R U . . .
C30 C -0.09860(12) 0.51199(16) 0.25339(18) 0.0126(4) Uani 1 1 d . . . . .
C31 C -0.28008(13) 0.14603(18) 0.4846(2) 0.0168(4) Uani 1 1 d . . . . .
H31 H -0.268768 0.145213 0.576980 0.020 Uiso 1 1 calc R U . . .
C32 C -0.32866(13) 0.55707(19) 0.1903(2) 0.0200(4) Uani 1 1 d . . . . .
H32 H -0.365188 0.602916 0.139712 0.024 Uiso 1 1 calc R U . . .
C33 C 0.36568(13) 0.11330(18) -0.1180(2) 0.0178(4) Uani 1 1 d . . . . .
H33 H 0.389214 0.071208 -0.183213 0.021 Uiso 1 1 calc R U . . .
C34 C -0.24359(13) 0.56891(18) 0.1873(2) 0.0175(4) Uani 1 1 d . . . . .
H34 H -0.221990 0.623030 0.133962 0.021 Uiso 1 1 calc R U . . .
O3 O -0.11540(9) 0.17141(12) 0.58285(14) 0.0161(3) Uani 1 1 d . . . . .
O6 O 0.10895(9) 0.16162(13) -0.11554(15) 0.0171(3) Uani 1 1 d . . . . .
O8 O -0.07014(9) 0.58817(12) 0.18814(14) 0.0147(3) Uani 1 1 d . . . . .
O1 O 0.06189(10) 0.43903(13) 0.10074(15) 0.0195(3) Uani 1 1 d . . . . .
H1A H 0.062438 0.426546 0.017040 0.029 Uiso 1 1 d R U . . .
H1B H 0.026140 0.490655 0.106402 0.029 Uiso 1 1 d R U . . .
O2 O -0.05309(9) 0.10696(12) 0.08749(14) 0.0158(3) Uani 1 1 d . . . . .
H2A H -0.028840 0.048219 0.115742 0.024 Uiso 1 1 d R U . . .
H2B H -0.041330 0.111505 0.005907 0.024 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O7 2.5992(15) . ?
La1 O5 2.4254(17) . ?
La1 O4 2.4125(16) . ?
La1 O3 2.4910(16) 4_565 ?
La1 O6 2.4110(16) 4_566 ?
La1 O8 2.6227(15) 2_545 ?
La1 O1 2.5878(16) . ?
La1 O2 2.6026(16) . ?
O7 C30 1.279(2) . ?
O5 C8 1.258(3) . ?
O4 C9 1.271(2) . ?
C8 C18 1.496(3) . ?
C8 O6 1.263(3) . ?
C9 C19 1.496(3) . ?
C9 O3 1.258(3) . ?
O11 H11 0.8400 . ?
O11 C22 1.377(2) . ?
O12 H12 0.8400 . ?
O12 C17 1.378(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.388(3) . ?
C13 C18 1.390(3) . ?
C14 H14 0.9500 . ?
C14 C22 1.388(3) . ?
C15 C24 1.394(3) . ?
C15 C30 1.492(3) . ?
C15 C34 1.388(3) . ?
O16 H16 0.8400 . ?
O16 C23 1.379(2) . ?
C17 C26 1.389(3) . ?
C17 C28 1.385(3) . ?
C18 C21 1.396(3) . ?
C19 C20 1.390(3) . ?
C19 C31 1.397(3) . ?
C20 H20 0.9500 . ?
C20 C28 1.385(3) . ?
C21 H21 0.9500 . ?
C21 C33 1.392(3) . ?
C22 C33 1.393(3) . ?
C23 C27 1.383(3) . ?
C23 C32 1.388(3) . ?
C24 H24 0.9500 . ?
C24 C27 1.387(3) . ?
C26 H26 0.9500 . ?
C26 C31 1.389(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C30 O8 1.266(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C32 C34 1.390(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
O1 H1A 0.8712 . ?
O1 H1B 0.8709 . ?
O2 H2A 0.8709 . ?
O2 H2B 0.8711 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 La1 O8 136.02(5) . 2_545 ?
O7 La1 O2 133.56(5) . . ?
O5 La1 O7 136.15(5) . . ?
O5 La1 O3 112.79(5) . 4_565 ?
O5 La1 O8 74.96(5) . 2_545 ?
O5 La1 O1 68.67(5) . . ?
O5 La1 O2 80.81(5) . . ?
O4 La1 O7 76.46(5) . . ?
O4 La1 O5 144.25(6) . . ?
O4 La1 O3 90.52(5) . 4_565 ?
O4 La1 O8 69.59(5) . 2_545 ?
O4 La1 O1 145.77(5) . . ?
O4 La1 O2 82.25(5) . . ?
O3 La1 O7 68.96(5) 4_565 . ?
O3 La1 O8 136.36(5) 4_565 2_545 ?
O3 La1 O1 77.54(5) 4_565 . ?
O3 La1 O2 70.50(5) 4_565 . ?
O6 La1 O7 72.25(5) 4_566 . ?
O6 La1 O5 88.50(5) 4_566 . ?
O6 La1 O4 90.11(5) 4_566 . ?
O6 La1 O3 139.89(5) 4_566 4_565 ?
O6 La1 O8 80.54(5) 4_566 2_545 ?
O6 La1 O1 79.69(5) 4_566 . ?
O6 La1 O2 149.01(5) 4_566 . ?
O1 La1 O7 69.31(5) . . ?
O1 La1 O8 138.73(5) . 2_545 ?
O1 La1 O2 121.94(5) . . ?
O2 La1 O8 68.62(5) . 2_545 ?
C30 O7 La1 127.70(12) . . ?
C8 O5 La1 151.36(15) . . ?
C9 O4 La1 168.99(14) . . ?
O5 C8 C18 117.74(19) . . ?
O5 C8 O6 123.76(19) . . ?
O6 C8 C18 118.50(18) . . ?
O4 C9 C19 118.48(18) . . ?
O3 C9 O4 122.69(19) . . ?
O3 C9 C19 118.81(18) . . ?
C22 O11 H11 109.5 . . ?
C17 O12 H12 109.5 . . ?
C14 C13 H13 119.5 . . ?
C14 C13 C18 121.0(2) . . ?
C18 C13 H13 119.5 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C22 119.3(2) . . ?
C22 C14 H14 120.3 . . ?
C24 C15 C30 120.11(18) . . ?
C34 C15 C24 119.18(18) . . ?
C34 C15 C30 120.67(18) . . ?
C23 O16 H16 109.5 . . ?
O12 C17 C26 118.2(2) . . ?
O12 C17 C28 120.9(2) . . ?
C28 C17 C26 121.0(2) . . ?
C13 C18 C8 120.45(19) . . ?
C13 C18 C21 119.12(19) . . ?
C21 C18 C8 120.41(19) . . ?
C20 C19 C9 120.48(18) . . ?
C20 C19 C31 119.58(19) . . ?
C31 C19 C9 119.84(19) . . ?
C19 C20 H20 119.9 . . ?
C28 C20 C19 120.3(2) . . ?
C28 C20 H20 119.9 . . ?
C18 C21 H21 119.8 . . ?
C33 C21 C18 120.3(2) . . ?
C33 C21 H21 119.8 . . ?
O11 C22 C14 117.3(2) . . ?
O11 C22 C33 122.1(2) . . ?
C14 C22 C33 120.5(2) . . ?
O16 C23 C27 116.9(2) . . ?
O16 C23 C32 122.3(2) . . ?
C27 C23 C32 120.82(19) . . ?
C15 C24 H24 119.7 . . ?
C27 C24 C15 120.5(2) . . ?
C27 C24 H24 119.7 . . ?
C17 C26 H26 120.5 . . ?
C31 C26 C17 119.1(2) . . ?
C31 C26 H26 120.5 . . ?
C23 C27 C24 119.6(2) . . ?
C23 C27 H27 120.2 . . ?
C24 C27 H27 120.2 . . ?
C17 C28 C20 119.7(2) . . ?
C17 C28 H28 120.2 . . ?
C20 C28 H28 120.2 . . ?
O7 C30 C15 118.51(18) . . ?
O8 C30 O7 122.30(18) . . ?
O8 C30 C15 119.19(18) . . ?
C19 C31 H31 119.8 . . ?
C26 C31 C19 120.4(2) . . ?
C26 C31 H31 119.8 . . ?
C23 C32 H32 120.4 . . ?
C23 C32 C34 119.2(2) . . ?
C34 C32 H32 120.4 . . ?
C21 C33 C22 119.6(2) . . ?
C21 C33 H33 120.2 . . ?
C22 C33 H33 120.2 . . ?
C15 C34 C32 120.7(2) . . ?
C15 C34 H34 119.6 . . ?
C32 C34 H34 119.6 . . ?
C9 O3 La1 128.01(13) . 4_566 ?
C8 O6 La1 141.59(14) . 4_565 ?
C30 O8 La1 126.34(12) . 2 ?
La1 O1 H1A 109.5 . . ?
La1 O1 H1B 109.5 . . ?
H1A O1 H1B 104.5 . . ?
La1 O2 H2A 109.5 . . ?
La1 O2 H2B 109.5 . . ?
H2A O2 H2B 104.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O11 H11 O16 0.84 1.95 2.788(2) 175.0 4_665 yes
O12 H12 O11 0.84 1.96 2.772(3) 163.4 1_455 yes
O16 H16 O12 0.84 1.89 2.695(2) 160.5 2_455 yes
O2 H2A O7 0.87 1.96 2.806(2) 164.2 2_545 yes
O2 H2B O7 0.87 2.08 2.873(2) 151.5 4_565 yes

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
La1 O7 C30 C15 96.32(19) . . . . ?
La1 O7 C30 O8 -83.9(2) . . . . ?
La1 O5 C8 C18 -172.9(2) . . . . ?
La1 O5 C8 O6 7.6(5) . . . . ?
La1 O4 C9 C19 38.9(8) . . . . ?
La1 O4 C9 O3 -139.7(7) . . . . ?
O7 C30 O8 La1 -81.5(2) . . . 2 ?
O5 C8 C18 C13 -15.0(3) . . . . ?
O5 C8 C18 C21 166.4(2) . . . . ?
O5 C8 O6 La1 62.4(3) . . . 4_565 ?
O4 C9 C19 C20 6.3(3) . . . . ?
O4 C9 C19 C31 -170.0(2) . . . . ?
O4 C9 O3 La1 10.2(3) . . . 4_566 ?
C8 C18 C21 C33 179.99(19) . . . . ?
C9 C19 C20 C28 -174.4(2) . . . . ?
C9 C19 C31 C26 174.5(2) . . . . ?
O11 C22 C33 C21 177.6(2) . . . . ?
O12 C17 C26 C31 -177.5(2) . . . . ?
O12 C17 C28 C20 177.5(2) . . . . ?
C13 C14 C22 O11 -176.3(2) . . . . ?
C13 C14 C22 C33 2.5(3) . . . . ?
C13 C18 C21 C33 1.4(3) . . . . ?
C14 C13 C18 C8 -178.5(2) . . . . ?
C14 C13 C18 C21 0.1(3) . . . . ?
C14 C22 C33 C21 -1.1(3) . . . . ?
C15 C24 C27 C23 -0.6(3) . . . . ?
C15 C30 O8 La1 98.22(19) . . . 2 ?
O16 C23 C27 C24 178.58(19) . . . . ?
O16 C23 C32 C34 -178.1(2) . . . . ?
C17 C26 C31 C19 -0.4(3) . . . . ?
C18 C8 O6 La1 -117.2(2) . . . 4_565 ?
C18 C13 C14 C22 -2.0(4) . . . . ?
C18 C21 C33 C22 -0.9(3) . . . . ?
C19 C9 O3 La1 -168.34(13) . . . 4_566 ?
C19 C20 C28 C17 0.3(3) . . . . ?
C20 C19 C31 C26 -1.8(3) . . . . ?
C23 C32 C34 C15 -0.3(3) . . . . ?
C24 C15 C30 O7 4.2(3) . . . . ?
C24 C15 C30 O8 -175.53(18) . . . . ?
C24 C15 C34 C32 -0.4(3) . . . . ?
C26 C17 C28 C20 -2.6(4) . . . . ?
C27 C23 C32 C34 0.6(3) . . . . ?
C28 C17 C26 C31 2.7(4) . . . . ?
C30 C15 C24 C27 -176.73(19) . . . . ?
C30 C15 C34 C32 177.2(2) . . . . ?
C31 C19 C20 C28 1.9(3) . . . . ?
C32 C23 C27 C24 -0.1(3) . . . . ?
C34 C15 C24 C27 0.9(3) . . . . ?
C34 C15 C30 O7 -173.35(19) . . . . ?
C34 C15 C30 O8 6.9(3) . . . . ?
O3 C9 C19 C20 -175.1(2) . . . . ?
O3 C9 C19 C31 8.6(3) . . . . ?
O6 C8 C18 C13 164.5(2) . . . . ?
O6 C8 C18 C21 -14.0(3) . . . . ?

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

data_jo204ce_a2_tw
_database_code_depnum_ccdc_archive 'CCDC 2269117'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H19 Ce O11, 3(H2 O)'
_chemical_formula_sum            'C21 H25 Ce O14'
_chemical_formula_weight         641.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ce C H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.36120(10)
_cell_length_b                   10.0317(2)
_cell_length_c                   19.6952(9)
_cell_angle_alpha                104.267(3)
_cell_angle_beta                 93.474(3)
_cell_angle_gamma                96.567(2)
_cell_volume                     1204.91(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12088
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      77.0760
_cell_measurement_theta_min      4.5400
_shelx_estimated_absorpt_T_max   0.311
_shelx_estimated_absorpt_T_min   0.150
_exptl_absorpt_coefficient_mu    15.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.768
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4963
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.359
_diffrn_reflns_theta_min         4.584
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     89.00 178.00   0.50    0.15    --  107.75 134.00 109.00  178
  2  ω     88.00 178.00   0.50    0.15    --  107.75 136.00 -71.00  180
  3  ω     95.00 178.00   0.50    0.15    --  107.75 125.00-120.00  166
  4  ω     95.00 178.00   0.50    0.15    --  107.75 125.00-180.00  166
  5  ω    -60.00  28.00   0.50    0.06    --  -47.64  19.00  30.00  176
  6  ω    -94.00 -19.00   0.50    0.06    --  -47.64 136.00 -71.00  150
  7  ω    -94.00 -19.00   0.50    0.15    --  -86.25 136.00 -71.00  150
  8  ω    -92.00 -18.00   0.50    0.06    --  -47.64 134.00 109.00  148
  9  ω     41.00 101.00   0.50    0.06    --   47.64-136.00-136.00  120
 10  ω     -1.00  81.00   0.50    0.06    --   47.64 -99.00-150.00  164
 11  ω     41.00 120.00   0.50    0.15    --  107.75-136.00-136.00  158
 12  ω     35.00 112.00   0.50    0.15    --  107.75-125.00 -60.00  154
 13  ω     35.00 112.00   0.50    0.15    --  107.75-125.00   0.00  154
 14  ω     39.00 119.00   0.50    0.15    --  107.75-134.00  42.00  160
 15  ω     35.00 112.00   0.50    0.15    --  107.75-125.00 150.00  154
 16  ω     76.00 101.00   0.50    0.15    --  107.75 -94.00  60.00   50
 17  ω     35.00 107.00   0.50    0.15    --  107.75-104.00  64.40  144
 18  ω     39.00 100.00   0.50    0.06    --   47.64-134.00  42.00  122
 19  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00-180.00  142
 20  ω     71.00 102.00   0.50    0.15    --  107.75 -94.00-150.00   62
 21  ω     37.00  68.00   0.50    0.15    --  107.75 -94.00-150.00   62
 22  ω     35.00  68.00   0.50    0.15    --  107.75 -94.00-120.00   66
 23  ω     74.00 106.00   0.50    0.15    --  107.75 -94.00-120.00   64
 24  ω     35.00 131.00   0.50    0.15    --  107.75 -77.00 -30.00  192
 25  ω     35.00 124.00   0.50    0.15    --  107.75 -61.00-150.00  178
 26  ω     36.00  76.00   0.50    0.15    --  107.75 -45.00-120.00   80
 27  ω     33.00  66.00   0.50    0.15    --  107.75 -30.00-180.00   66
 28  ω     33.00  66.00   0.50    0.15    --  107.75 -30.00 -90.00   66
 29  ω     36.00  66.00   0.50    0.15    --  107.75 -30.00-120.00   60
 30  ω     36.00  76.00   0.50    0.15    --  107.75 -45.00 -60.00   80
 31  ω     33.00  66.00   0.50    0.15    --  107.75 -30.00 -30.00   66
 32  ω     33.00  66.00   0.50    0.15    --  107.75 -30.00  30.00   66
 33  ω     33.00 122.00   0.50    0.15    --  107.75 -15.00 -30.00  178
 34  ω     33.00 122.00   0.50    0.15    --  107.75 -15.00  60.00  178
 35  ω     33.00  64.00   0.50    0.15    --  107.75 -30.00  90.00   62
 36  ω     47.00  74.00   0.50    0.15    --  107.75 -45.00 120.00   54
 37  ω     38.00  64.00   0.50    0.15    --  107.75 -30.00 150.00   52
 38  ω   -120.00 -25.00   0.50    0.06    --  -47.64 -77.00  60.00  190
 39  ω   -158.00 -73.00   0.50    0.15    --  -86.25 -45.00  90.00  170
 40  ω   -158.00 -73.00   0.50    0.15    --  -86.25 -45.00  30.00  170
 41  ω   -120.00 -73.00   0.50    0.06    --  -47.64-125.00  90.00   94
 42  ω   -120.00 -68.00   0.50    0.06    --  -47.64-134.00  42.00  104
 43  ω   -159.00 -68.00   0.50    0.15    --  -86.25-134.00  42.00  182
 44  ω   -120.00 -66.00   0.50    0.06    --  -47.64-136.00-136.00  108
 45  ω   -159.00 -66.00   0.50    0.15    --  -86.25-136.00-136.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2080914000
_diffrn_orient_matrix_UB_12      0.0587707000
_diffrn_orient_matrix_UB_13      0.0193006000
_diffrn_orient_matrix_UB_21      0.0752594000
_diffrn_orient_matrix_UB_22      0.0290401000
_diffrn_orient_matrix_UB_23      0.0787185000
_diffrn_orient_matrix_UB_31      0.1047484000
_diffrn_orient_matrix_UB_32      0.1458353000
_diffrn_orient_matrix_UB_33      -0.0007464000
_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                4705
_reflns_number_total             4963
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         13.258
_refine_diff_density_min         -4.594
_refine_diff_density_rms         0.488
_refine_ls_extinction_coef       0.0031(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.358
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4963
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.1128
_refine_ls_restrained_S_all      1.356
_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          0.2826
_refine_ls_wR_factor_ref         0.2855
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6287
 0.3713
2. Restrained distances
 H14B_$2-H9
 2.2 with sigma of 0.02
 H9-H14A_$2
 2.2 with sigma of 0.02
 H14B-H6
 2.2 with sigma of 0.02
 H14A-H6
 2.2 with sigma of 0.02
 H14B_$3-H11B
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16 \\sim C15: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C17 \\sim C16 \\sim C21 \\sim C15: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
4.a Free rotating group:
 O14(H14A,H14B), O13(H13A,H13B), O11(H11A,H11B)
4.b Rotating group:
 O10(H10A,H10B), O12(H12A,H12B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C11(H11), C6(H6A), C17(H17), C21(H21), C14(H14), C3(H3A),
 C13(H13), C4(H4), C20(H20), C18(H18)
4.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O3(H3), O9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce01 Ce 0.50362(6) 0.25828(4) 0.51739(2) 0.0131(3) Uani 1 1 d . . . . .
O10 O 0.1686(11) 0.0844(7) 0.4596(4) 0.0215(14) Uani 1 1 d . . . . .
H10A H 0.181330 0.004607 0.466262 0.032 Uiso 1 1 d R U . . .
H10B H 0.060291 0.108359 0.480849 0.032 Uiso 1 1 d R U . . .
O2 O 0.5806(10) -0.1548(7) 0.3870(4) 0.0189(13) Uani 1 1 d . . . . .
O12 O 0.8080(11) 0.3766(7) 0.4599(4) 0.0222(14) Uani 1 1 d . . . . .
H12A H 0.792292 0.461273 0.464159 0.033 Uiso 1 1 d R U . . .
H12B H 0.926630 0.379680 0.483177 0.033 Uiso 1 1 d R U . . .
O5 O 0.3568(10) 0.5401(7) 0.3873(4) 0.0190(13) Uani 1 1 d . . . . .
O6 O 0.1527(12) 0.0514(8) 0.1090(4) 0.0249(15) Uani 1 1 d . . . . .
H6 H 0.022792 0.032791 0.095037 0.037 Uiso 1 1 calc DR U . . .
O4 O 0.3456(10) 0.3592(7) 0.4334(4) 0.0198(13) Uani 1 1 d . . . . .
O1 O 0.6161(11) 0.0727(7) 0.4339(4) 0.0188(13) Uani 1 1 d . . . . .
O3 O 0.6653(12) 0.0713(9) 0.1145(4) 0.0254(15) Uani 1 1 d . . . . .
H3 H 0.688058 0.000327 0.084414 0.038 Uiso 1 1 calc R U . . .
O7 O 0.1626(9) 0.3514(6) 0.5616(3) 0.0134(12) Uani 1 1 d . . . . .
O8 O -0.1309(10) 0.2101(6) 0.5615(3) 0.0161(12) Uani 1 1 d . . . . .
O14 O 0.0316(13) -0.2287(8) 0.0561(4) 0.0319(17) Uani 1 1 d G . . . .
H14A H 0.098608 -0.176750 0.093807 0.048 Uiso 1 1 d DG U . . .
H14B H -0.077889 -0.190173 0.050195 0.048 Uiso 1 1 d DG U . . .
O13 O 0.7167(15) 0.2879(9) 0.0511(4) 0.0335(18) Uani 1 1 d G . . . .
H13A H 0.669888 0.359869 0.074326 0.050 Uiso 1 1 d G U . . .
H13B H 0.750959 0.245858 0.081843 0.050 Uiso 1 1 d G U . . .
O9 O 0.1087(18) 0.4433(10) 0.8904(4) 0.043(2) Uani 1 1 d . . . . .
H9 H 0.098496 0.370802 0.904695 0.064 Uiso 1 1 calc DR U . . .
C10 C 0.2100(13) 0.1717(9) 0.3012(5) 0.0142(17) Uani 1 1 d . . . . .
H10 H 0.203664 0.135249 0.341363 0.017 Uiso 1 1 calc R U . . .
C1 C 0.6113(13) -0.0310(9) 0.3814(5) 0.0139(16) Uani 1 1 d . . . . .
C7 C 0.6872(13) 0.1291(10) 0.3040(5) 0.0151(17) Uani 1 1 d . . . . .
H7 H 0.713642 0.204707 0.344727 0.018 Uiso 1 1 calc R U . . .
O11 O 0.3208(15) 0.1457(10) -0.0012(5) 0.0378(19) Uani 1 1 d G . . . .
H11A H 0.420775 0.202924 0.024286 0.057 Uiso 1 1 d G U . . .
H11B H 0.253395 0.110777 0.027707 0.057 Uiso 1 1 d DG U . . .
C8 C 0.3237(13) 0.4114(9) 0.3813(5) 0.0126(16) Uani 1 1 d . . . . .
C11 C 0.1710(15) 0.0835(10) 0.2342(5) 0.0178(18) Uani 1 1 d . . . . .
H11 H 0.139616 -0.013807 0.228034 0.021 Uiso 1 1 calc R U . . .
C6 C 0.6956(15) 0.1527(10) 0.2384(5) 0.0165(18) Uani 1 1 d . . . . .
H6A H 0.726842 0.245014 0.234139 0.020 Uiso 1 1 calc R U . . .
C15 C 0.0263(15) 0.2979(9) 0.5929(5) 0.0157(10) Uani 1 1 d . U . . .
C17 C -0.1000(15) 0.2756(9) 0.7096(5) 0.0168(10) Uani 1 1 d . U . . .
H17 H -0.215195 0.209601 0.684620 0.020 Uiso 1 1 calc R U . . .
C16 C 0.0461(15) 0.3368(9) 0.6731(5) 0.0164(9) Uani 1 1 d . U . . .
C21 C 0.2133(15) 0.4356(9) 0.7095(5) 0.0171(10) Uani 1 1 d . U . . .
H21 H 0.311319 0.479014 0.684506 0.020 Uiso 1 1 calc R U . . .
C14 C 0.2564(15) 0.3690(11) 0.2508(5) 0.0206(19) Uani 1 1 d . . . . .
H14 H 0.280688 0.466622 0.256766 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6125(15) -0.1155(10) 0.2506(5) 0.0181(17) Uani 1 1 d . . . . .
H3A H 0.587150 -0.207803 0.255272 0.022 Uiso 1 1 calc R U . . .
C2 C 0.6400(13) -0.0053(9) 0.3106(5) 0.0158(17) Uani 1 1 d . . . . .
C9 C 0.2592(14) 0.3166(9) 0.3096(5) 0.0156(17) Uani 1 1 d . . . . .
C5 C 0.6590(16) 0.0430(11) 0.1778(5) 0.0180(18) Uani 1 1 d . . . . .
C13 C 0.2192(16) 0.2830(11) 0.1842(5) 0.0214(19) Uani 1 1 d . . . . .
H13 H 0.220922 0.320375 0.144334 0.026 Uiso 1 1 calc R U . . .
C12 C 0.1784(16) 0.1390(10) 0.1756(5) 0.0185(18) Uani 1 1 d . . . . .
C4 C 0.6212(16) -0.0932(10) 0.1840(5) 0.0196(18) Uani 1 1 d . . . . .
H4 H 0.601967 -0.169200 0.143409 0.023 Uiso 1 1 calc R U . . .
C19 C 0.0887(17) 0.4085(11) 0.8184(5) 0.0223(19) Uani 1 1 d . . . . .
C20 C 0.2360(17) 0.4701(11) 0.7825(6) 0.023(2) Uani 1 1 d . . . . .
H20 H 0.351555 0.535540 0.807656 0.028 Uiso 1 1 calc R U . . .
C18 C -0.0780(18) 0.3107(12) 0.7830(5) 0.024(2) Uani 1 1 d . . . . .
H18 H -0.176176 0.267950 0.808306 0.029 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
Ce01 O10 2.599(7) . ?
Ce01 O2 2.423(7) 2_656 ?
Ce01 O12 2.615(8) . ?
Ce01 O5 2.433(7) 2_666 ?
Ce01 O4 2.373(6) . ?
Ce01 O1 2.371(7) . ?
Ce01 O7 2.575(6) . ?
Ce01 O8 2.571(6) 1_655 ?
O10 H10A 0.8546 . ?
O10 H10B 0.8548 . ?
O2 C1 1.268(12) . ?
O12 H12A 0.8512 . ?
O12 H12B 0.8519 . ?
O5 C8 1.259(11) . ?
O6 H6 0.8400 . ?
O6 C12 1.376(12) . ?
O4 C8 1.269(11) . ?
O1 C1 1.269(11) . ?
O3 H3 0.8400 . ?
O3 C5 1.346(12) . ?
O7 C15 1.241(11) . ?
O8 C15 1.270(11) . ?
O14 H14A 0.8509 . ?
O14 H14B 0.8498 . ?
O13 H13A 0.8494 . ?
O13 H13B 0.8497 . ?
O9 H9 0.8400 . ?
O9 C19 1.368(14) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(13) . ?
C10 C9 1.418(12) . ?
C1 C2 1.496(13) . ?
C7 H7 0.9500 . ?
C7 C6 1.372(13) . ?
C7 C2 1.388(13) . ?
O11 H11A 0.8498 . ?
O11 H11B 0.8504 . ?
C8 C9 1.499(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.399(13) . ?
C6 H6A 0.9500 . ?
C6 C5 1.396(13) . ?
C15 C16 1.524(14) . ?
C17 H17 0.9500 . ?
C17 C16 1.389(13) . ?
C17 C18 1.395(15) . ?
C16 C21 1.394(13) . ?
C21 H21 0.9500 . ?
C21 C20 1.386(16) . ?
C14 H14 0.9500 . ?
C14 C9 1.384(13) . ?
C14 C13 1.371(15) . ?
C3 H3A 0.9500 . ?
C3 C2 1.392(13) . ?
C3 C4 1.386(13) . ?
C5 C4 1.397(15) . ?
C13 H13 0.9500 . ?
C13 C12 1.404(14) . ?
C4 H4 0.9500 . ?
C19 C20 1.387(15) . ?
C19 C18 1.381(15) . ?
C20 H20 0.9500 . ?
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
O10 Ce01 O12 130.3(2) . . ?
O2 Ce01 O10 79.3(2) 2_656 . ?
O2 Ce01 O12 145.1(2) 2_656 . ?
O2 Ce01 O5 83.2(2) 2_656 2_666 ?
O2 Ce01 O7 74.2(2) 2_656 . ?
O2 Ce01 O8 77.5(2) 2_656 1_655 ?
O5 Ce01 O10 145.4(2) 2_666 . ?
O5 Ce01 O12 78.4(2) 2_666 . ?
O5 Ce01 O7 77.7(2) 2_666 . ?
O5 Ce01 O8 74.2(2) 2_666 1_655 ?
O4 Ce01 O10 75.0(2) . . ?
O4 Ce01 O2 141.8(2) . 2_656 ?
O4 Ce01 O12 71.9(2) . . ?
O4 Ce01 O5 102.6(2) . 2_666 ?
O4 Ce01 O7 70.5(2) . . ?
O4 Ce01 O8 140.6(2) . 1_655 ?
O1 Ce01 O10 72.1(2) . . ?
O1 Ce01 O2 102.8(2) . 2_656 ?
O1 Ce01 O12 75.5(2) . . ?
O1 Ce01 O5 141.4(2) . 2_666 ?
O1 Ce01 O4 95.7(2) . . ?
O1 Ce01 O7 140.9(2) . . ?
O1 Ce01 O8 70.2(2) . 1_655 ?
O7 Ce01 O10 69.0(2) . . ?
O7 Ce01 O12 129.0(2) . . ?
O8 Ce01 O10 129.4(2) 1_655 . ?
O8 Ce01 O12 69.0(2) 1_655 . ?
O8 Ce01 O7 141.93(19) 1_655 . ?
Ce01 O10 H10A 109.7 . . ?
Ce01 O10 H10B 109.7 . . ?
H10A O10 H10B 104.3 . . ?
C1 O2 Ce01 134.0(6) . 2_656 ?
Ce01 O12 H12A 109.5 . . ?
Ce01 O12 H12B 109.5 . . ?
H12A O12 H12B 104.5 . . ?
C8 O5 Ce01 134.6(6) . 2_666 ?
C12 O6 H6 109.5 . . ?
C8 O4 Ce01 160.4(6) . . ?
C1 O1 Ce01 160.7(6) . . ?
C5 O3 H3 109.5 . . ?
C15 O7 Ce01 128.2(6) . . ?
C15 O8 Ce01 127.8(6) . 1_455 ?
H14A O14 H14B 104.5 . . ?
H13A O13 H13B 104.5 . . ?
C19 O9 H9 109.5 . . ?
C11 C10 H10 120.2 . . ?
C11 C10 C9 119.6(8) . . ?
C9 C10 H10 120.2 . . ?
O2 C1 O1 122.1(8) . . ?
O2 C1 C2 119.3(8) . . ?
O1 C1 C2 118.6(8) . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C2 119.9(8) . . ?
C2 C7 H7 120.1 . . ?
H11A O11 H11B 104.5 . . ?
O5 C8 O4 122.5(8) . . ?
O5 C8 C9 118.4(8) . . ?
O4 C8 C9 119.0(7) . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.5(8) . . ?
C12 C11 H11 120.2 . . ?
C7 C6 H6A 119.5 . . ?
C7 C6 C5 121.0(8) . . ?
C5 C6 H6A 119.5 . . ?
O7 C15 O8 123.3(8) . . ?
O7 C15 C16 119.4(8) . . ?
O8 C15 C16 117.3(9) . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(9) . . ?
C18 C17 H17 119.9 . . ?
C17 C16 C15 120.8(9) . . ?
C17 C16 C21 120.2(9) . . ?
C21 C16 C15 119.0(9) . . ?
C16 C21 H21 120.1 . . ?
C20 C21 C16 119.7(10) . . ?
C20 C21 H21 120.1 . . ?
C9 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C13 C14 C9 121.3(9) . . ?
C2 C3 H3A 119.3 . . ?
C4 C3 H3A 119.3 . . ?
C4 C3 C2 121.3(8) . . ?
C7 C2 C1 120.2(8) . . ?
C7 C2 C3 119.3(9) . . ?
C3 C2 C1 120.4(8) . . ?
C10 C9 C8 120.1(8) . . ?
C14 C9 C10 119.6(8) . . ?
C14 C9 C8 120.3(8) . . ?
O3 C5 C6 118.9(8) . . ?
O3 C5 C4 121.5(8) . . ?
C6 C5 C4 119.5(8) . . ?
C14 C13 H13 120.4 . . ?
C14 C13 C12 119.2(9) . . ?
C12 C13 H13 120.4 . . ?
O6 C12 C11 119.7(8) . . ?
O6 C12 C13 119.6(9) . . ?
C11 C12 C13 120.7(9) . . ?
C3 C4 C5 118.8(8) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
O9 C19 C20 119.8(10) . . ?
O9 C19 C18 118.8(10) . . ?
C18 C19 C20 121.4(9) . . ?
C21 C20 C19 119.5(10) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C17 C18 H18 120.5 . . ?
C19 C18 C17 119.0(10) . . ?
C19 C18 H18 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce01 O2 C1 O1 5.2(13) 2_656 . . . ?
Ce01 O2 C1 C2 -173.9(6) 2_656 . . . ?
Ce01 O5 C8 O4 6.7(13) 2_666 . . . ?
Ce01 O5 C8 C9 -172.4(6) 2_666 . . . ?
Ce01 O4 C8 O5 -92.4(19) . . . . ?
Ce01 O4 C8 C9 86.6(19) . . . . ?
Ce01 O1 C1 O2 -94.6(19) . . . . ?
Ce01 O1 C1 C2 85(2) . . . . ?
Ce01 O7 C15 O8 -87.0(10) . . . . ?
Ce01 O7 C15 C16 92.4(10) . . . . ?
Ce01 O8 C15 O7 -87.4(10) 1_455 . . . ?
Ce01 O8 C15 C16 93.2(9) 1_455 . . . ?
O2 C1 C2 C7 -175.9(8) . . . . ?
O2 C1 C2 C3 6.4(13) . . . . ?
O5 C8 C9 C10 -176.7(8) . . . . ?
O5 C8 C9 C14 6.1(13) . . . . ?
O4 C8 C9 C10 4.2(12) . . . . ?
O4 C8 C9 C14 -173.0(8) . . . . ?
O1 C1 C2 C7 4.9(12) . . . . ?
O1 C1 C2 C3 -172.8(8) . . . . ?
O3 C5 C4 C3 -178.7(9) . . . . ?
O7 C15 C16 C17 -178.0(8) . . . . ?
O7 C15 C16 C21 2.2(14) . . . . ?
O8 C15 C16 C17 1.4(14) . . . . ?
O8 C15 C16 C21 -178.3(8) . . . . ?
O9 C19 C20 C21 -179.2(12) . . . . ?
O9 C19 C18 C17 179.5(12) . . . . ?
C10 C11 C12 O6 176.1(9) . . . . ?
C10 C11 C12 C13 -1.7(14) . . . . ?
C7 C6 C5 O3 178.9(9) . . . . ?
C7 C6 C5 C4 -2.5(14) . . . . ?
C11 C10 C9 C8 -173.6(8) . . . . ?
C11 C10 C9 C14 3.5(13) . . . . ?
C6 C7 C2 C1 -174.5(8) . . . . ?
C6 C7 C2 C3 3.3(13) . . . . ?
C6 C5 C4 C3 2.7(14) . . . . ?
C15 C16 C21 C20 -178.8(10) . . . . ?
C17 C16 C21 C20 1.5(15) . . . . ?
C16 C17 C18 C19 1.1(17) . . . . ?
C16 C21 C20 C19 -1.6(17) . . . . ?
C14 C13 C12 O6 -176.4(9) . . . . ?
C14 C13 C12 C11 1.4(15) . . . . ?
C2 C7 C6 C5 -0.5(14) . . . . ?
C2 C3 C4 C5 0.1(15) . . . . ?
C9 C10 C11 C12 -0.8(13) . . . . ?
C9 C14 C13 C12 1.5(15) . . . . ?
C13 C14 C9 C10 -3.9(14) . . . . ?
C13 C14 C9 C8 173.3(9) . . . . ?
C4 C3 C2 C1 174.7(9) . . . . ?
C4 C3 C2 C7 -3.1(14) . . . . ?
C20 C19 C18 C17 -1.2(18) . . . . ?
C18 C17 C16 C15 179.1(10) . . . . ?
C18 C17 C16 C21 -1.2(15) . . . . ?
C18 C19 C20 C21 1.5(18) . . . . ?

# end Validation Reply Form
_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 2.726
_oxdiff_exptl_absorpt_empirical_full_min 0.417
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6287
2 0.3713

# start Validation Reply Form
_vrf_PLAT097_jo204ce_a2_tw       
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      13.26 eA-3  
RESPONSE: the crystal suffers from twinning, no meaningful atom
assignment available.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2269120'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 Gd2 O22, 2(H2 O)'
_chemical_formula_sum            'C42 H42 Gd2 O24'
_chemical_formula_weight         1245.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.4100(3)
_cell_length_b                   14.9000(5)
_cell_length_c                   15.5100(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.9610(10)
_cell_angle_gamma                90
_cell_volume                     2313.00(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4213
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.158
_exptl_absorpt_coefficient_mu    2.930
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38190
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.932
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4070
_reflns_number_total             4213
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4213
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.138
_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)+(0.0271P)²+2.0200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0520
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H12A_$1-H11A
 2.2 with sigma of 0.02
2.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
2.c Tetrahedral OH refined with riding coordinates:
 O9(H9)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.46283(2) 0.14784(2) 0.41844(2) 0.01406(6) Uani 1 1 d . . . . .
O3 O 0.55722(16) 0.28135(10) 0.50862(10) 0.0191(3) Uani 1 1 d . . . . .
O6 O 0.64006(15) -0.00635(10) 0.60400(10) 0.0175(3) Uani 1 1 d . . . . .
O4 O 0.54165(16) 0.28239(10) 0.36510(10) 0.0194(3) Uani 1 1 d . . . . .
O1 O 0.27684(15) 0.18112(11) 0.28656(10) 0.0178(3) Uani 1 1 d . . . . .
O5 O 0.66634(15) 0.08451(11) 0.49583(11) 0.0199(3) Uani 1 1 d . . . . .
O7 O 0.55913(16) 0.10094(11) 0.30063(11) 0.0211(3) Uani 1 1 d . . . . .
H7A H 0.595323 0.048516 0.295617 0.032 Uiso 1 1 d R U . . .
H7B H 0.564152 0.130955 0.253057 0.032 Uiso 1 1 d R U . . .
O8 O 0.43264(16) 0.11296(11) 0.55998(11) 0.0210(3) Uani 1 1 d . . . . .
H8A H 0.442626 0.160496 0.592873 0.031 Uiso 1 1 d R U . . .
H8B H 0.495562 0.077660 0.588538 0.031 Uiso 1 1 d R U . . .
O2 O 0.25505(15) 0.21931(11) 0.41847(10) 0.0192(3) Uani 1 1 d . . . . .
O12 O 0.38087(19) 0.30744(13) 0.19682(12) 0.0223(4) Uani 1 1 d . . . . .
O10 O 0.77522(18) 0.67378(12) 0.44997(13) 0.0241(4) Uani 1 1 d . . . . .
O9 O -0.35310(16) 0.22355(12) 0.18730(11) 0.0232(4) Uani 1 1 d . . . . .
H9 H -0.374366 0.207576 0.133285 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5749(2) 0.32278(15) 0.44103(15) 0.0179(5) Uani 1 1 d . . . . .
C9 C 0.6323(2) 0.41362(15) 0.44728(15) 0.0178(5) Uani 1 1 d . . . . .
C2 C 0.0587(2) 0.22207(15) 0.29403(15) 0.0180(5) Uani 1 1 d . . . . .
C10 C 0.6587(2) 0.45199(16) 0.37138(16) 0.0210(5) Uani 1 1 d . . . . .
H10A H 0.643154 0.418107 0.317607 0.025 Uiso 1 1 calc R U . . .
C16 C 0.8602(2) 0.04108(14) 0.60772(15) 0.0177(5) Uani 1 1 d . . . . .
C14 C 0.6575(2) 0.46420(15) 0.52603(15) 0.0191(5) Uani 1 1 d . . . . .
H14 H 0.640843 0.438756 0.578068 0.023 Uiso 1 1 calc R U . . .
C1 C 0.2031(2) 0.20857(14) 0.33393(15) 0.0170(4) Uani 1 1 d . . . . .
C13 C 0.7064(2) 0.55063(16) 0.52928(16) 0.0196(5) Uani 1 1 d . . . . .
H13 H 0.723632 0.584195 0.583335 0.023 Uiso 1 1 calc R U . . .
C21 C 0.9148(2) 0.00331(16) 0.69246(16) 0.0208(5) Uani 1 1 d . . . . .
H21 H 0.857444 -0.022755 0.723795 0.025 Uiso 1 1 calc R U . . .
C15 C 0.7145(2) 0.03964(14) 0.56626(15) 0.0170(4) Uani 1 1 d . . . . .
C7 C 0.0041(2) 0.21556(15) 0.20106(16) 0.0194(5) Uani 1 1 d . . . . .
H7 H 0.061504 0.209308 0.163247 0.023 Uiso 1 1 calc R U . . .
C12 C 0.7305(2) 0.58861(15) 0.45283(16) 0.0194(5) Uani 1 1 d . . . . .
C17 C 0.9461(2) 0.07965(15) 0.56312(16) 0.0199(5) Uani 1 1 d . . . . .
H17 H 0.910073 0.106215 0.505879 0.024 Uiso 1 1 calc R U . . .
C19 C 1.1347(2) 0.04134(15) 0.68531(16) 0.0196(5) Uani 1 1 d . . . . .
C18 C 1.0831(2) 0.07977(16) 0.60101(16) 0.0209(5) Uani 1 1 d . . . . .
H18 H 1.140919 0.105664 0.569986 0.025 Uiso 1 1 calc R U . . .
C11 C 0.7073(2) 0.53859(16) 0.37401(16) 0.0224(5) Uani 1 1 d . . . . .
H11 H 0.724801 0.564007 0.322217 0.027 Uiso 1 1 calc R U . . .
C3 C -0.0269(2) 0.23355(17) 0.34848(16) 0.0223(5) Uani 1 1 d . . . . .
H3 H 0.009439 0.240189 0.411414 0.027 Uiso 1 1 calc R U . . .
C6 C -0.1327(2) 0.21816(16) 0.16395(16) 0.0204(5) Uani 1 1 d . . . . .
H6 H -0.169081 0.214618 0.100770 0.025 Uiso 1 1 calc R U . . .
C5 C -0.2170(2) 0.22600(16) 0.21941(16) 0.0199(5) Uani 1 1 d . . . . .
C20 C 1.0511(2) 0.00357(16) 0.73099(17) 0.0226(5) Uani 1 1 d . . . . .
H20 H 1.087461 -0.022075 0.788632 0.027 Uiso 1 1 calc R U . . .
C4 C -0.1633(2) 0.23536(17) 0.31211(16) 0.0235(5) Uani 1 1 d . . . . .
H4 H -0.220639 0.242921 0.349762 0.028 Uiso 1 1 calc R U . . .
H12A H 0.445(3) 0.3028(18) 0.245(2) 0.039(9) Uiso 1 1 d . . . . .
H12B H 0.336(4) 0.271(3) 0.196(2) 0.041(11) Uiso 1 1 d . . . . .
H10 H 0.768(3) 0.698(2) 0.493(2) 0.027(8) Uiso 1 1 d . . . . .
O11 O 1.27055(16) 0.03819(11) 0.72538(12) 0.0245(4) Uani 1 1 d . . . . .
H11A H 1.306686 0.084518 0.711841 0.037 Uiso 1 1 calc DR 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
Gd1 O3 2.4746(15) . ?
Gd1 O6 2.3468(15) 3_656 ?
Gd1 O4 2.3979(16) . ?
Gd1 O1 2.4496(15) . ?
Gd1 O5 2.3282(16) . ?
Gd1 O7 2.4166(16) . ?
Gd1 O8 2.3595(16) . ?
Gd1 O2 2.4111(15) . ?
O3 C8 1.273(3) . ?
O6 C15 1.289(3) . ?
O4 C8 1.283(3) . ?
O1 C1 1.267(3) . ?
O5 C15 1.261(3) . ?
O7 H7A 0.8798 . ?
O7 H7B 0.8766 . ?
O8 H8A 0.8623 . ?
O8 H8B 0.8617 . ?
O2 C1 1.283(3) . ?
O12 H12A 0.85(3) . ?
O12 H12B 0.71(4) . ?
O10 C12 1.357(3) . ?
O10 H10 0.79(3) . ?
O9 H9 0.8400 . ?
O9 C5 1.367(3) . ?
C8 C9 1.472(3) . ?
C9 C10 1.402(3) . ?
C9 C14 1.397(3) . ?
C2 C1 1.474(3) . ?
C2 C7 1.400(3) . ?
C2 C3 1.397(3) . ?
C10 H10A 0.9500 . ?
C10 C11 1.382(3) . ?
C16 C21 1.399(3) . ?
C16 C15 1.476(3) . ?
C16 C17 1.396(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.381(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.397(3) . ?
C21 H21 0.9500 . ?
C21 C20 1.381(3) . ?
C7 H7 0.9500 . ?
C7 C6 1.382(3) . ?
C12 C11 1.395(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(3) . ?
C19 C18 1.393(3) . ?
C19 C20 1.384(3) . ?
C19 O11 1.380(3) . ?
C18 H18 0.9500 . ?
C11 H11 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.376(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.393(3) . ?
C5 C4 1.399(3) . ?
C20 H20 0.9500 . ?
C4 H4 0.9500 . ?
O11 H11A 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Gd1 O3 154.17(5) 3_656 . ?
O6 Gd1 O4 152.29(5) 3_656 . ?
O6 Gd1 O1 80.46(5) 3_656 . ?
O6 Gd1 O7 83.99(5) 3_656 . ?
O6 Gd1 O8 76.59(6) 3_656 . ?
O6 Gd1 O2 91.37(5) 3_656 . ?
O4 Gd1 O3 53.31(5) . . ?
O4 Gd1 O1 79.02(5) . . ?
O4 Gd1 O7 74.24(5) . . ?
O4 Gd1 O2 91.31(5) . . ?
O1 Gd1 O3 114.15(5) . . ?
O5 Gd1 O3 82.58(5) . . ?
O5 Gd1 O6 91.48(5) . 3_656 ?
O5 Gd1 O4 99.64(5) . . ?
O5 Gd1 O1 155.61(5) . . ?
O5 Gd1 O7 76.39(6) . . ?
O5 Gd1 O8 76.48(6) . . ?
O5 Gd1 O2 150.24(5) . . ?
O7 Gd1 O3 118.50(5) . . ?
O7 Gd1 O1 79.87(5) . . ?
O8 Gd1 O3 77.58(5) . . ?
O8 Gd1 O4 130.61(6) . . ?
O8 Gd1 O1 122.99(5) . . ?
O8 Gd1 O7 145.99(6) . . ?
O8 Gd1 O2 75.41(6) . . ?
O2 Gd1 O3 82.04(5) . . ?
O2 Gd1 O1 53.67(5) . . ?
O2 Gd1 O7 133.36(5) . . ?
C8 O3 Gd1 92.82(13) . . ?
C15 O6 Gd1 135.81(14) . 3_656 ?
C8 O4 Gd1 96.14(13) . . ?
C1 O1 Gd1 92.69(13) . . ?
C15 O5 Gd1 138.58(15) . . ?
Gd1 O7 H7A 126.9 . . ?
Gd1 O7 H7B 128.5 . . ?
H7A O7 H7B 104.6 . . ?
Gd1 O8 H8A 110.1 . . ?
Gd1 O8 H8B 109.6 . . ?
H8A O8 H8B 104.3 . . ?
C1 O2 Gd1 94.05(13) . . ?
H12A O12 H12B 108(4) . . ?
C12 O10 H10 107(2) . . ?
C5 O9 H9 109.5 . . ?
O3 C8 O4 117.7(2) . . ?
O3 C8 C9 122.7(2) . . ?
O4 C8 C9 119.6(2) . . ?
C10 C9 C8 119.3(2) . . ?
C14 C9 C8 121.9(2) . . ?
C14 C9 C10 118.7(2) . . ?
C7 C2 C1 120.1(2) . . ?
C3 C2 C1 120.6(2) . . ?
C3 C2 C7 119.0(2) . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 C9 120.7(2) . . ?
C11 C10 H10A 119.7 . . ?
C21 C16 C15 120.4(2) . . ?
C17 C16 C21 118.8(2) . . ?
C17 C16 C15 120.8(2) . . ?
C9 C14 H14 119.5 . . ?
C13 C14 C9 120.9(2) . . ?
C13 C14 H14 119.5 . . ?
O1 C1 O2 118.7(2) . . ?
O1 C1 C2 120.7(2) . . ?
O2 C1 C2 120.4(2) . . ?
C14 C13 H13 120.1 . . ?
C14 C13 C12 119.8(2) . . ?
C12 C13 H13 120.1 . . ?
C16 C21 H21 119.7 . . ?
C20 C21 C16 120.6(2) . . ?
C20 C21 H21 119.7 . . ?
O6 C15 C16 118.9(2) . . ?
O5 C15 O6 122.0(2) . . ?
O5 C15 C16 119.0(2) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 C2 120.5(2) . . ?
C6 C7 H7 119.8 . . ?
O10 C12 C13 123.4(2) . . ?
O10 C12 C11 116.7(2) . . ?
C11 C12 C13 119.9(2) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 C16 121.0(2) . . ?
C18 C17 H17 119.5 . . ?
C20 C19 C18 120.9(2) . . ?
O11 C19 C18 121.3(2) . . ?
O11 C19 C20 117.8(2) . . ?
C17 C18 C19 119.0(2) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C10 C11 C12 119.9(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(2) . . ?
C4 C3 H3 119.6 . . ?
C7 C6 H6 120.1 . . ?
C7 C6 C5 119.8(2) . . ?
C5 C6 H6 120.1 . . ?
O9 C5 C6 122.6(2) . . ?
O9 C5 C4 117.3(2) . . ?
C6 C5 C4 120.1(2) . . ?
C21 C20 C19 119.7(2) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C3 C4 C5 119.7(2) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C19 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O3 C8 O4 -0.6(2) . . . . ?
Gd1 O3 C8 C9 179.95(19) . . . . ?
Gd1 O6 C15 O5 81.4(3) 3_656 . . . ?
Gd1 O6 C15 C16 -99.7(2) 3_656 . . . ?
Gd1 O4 C8 O3 0.6(2) . . . . ?
Gd1 O4 C8 C9 -179.91(18) . . . . ?
Gd1 O1 C1 O2 9.3(2) . . . . ?
Gd1 O1 C1 C2 -166.58(18) . . . . ?
Gd1 O5 C15 O6 21.2(3) . . . . ?
Gd1 O5 C15 C16 -157.69(16) . . . . ?
Gd1 O2 C1 O1 -9.5(2) . . . . ?
Gd1 O2 C1 C2 166.42(18) . . . . ?
O3 C8 C9 C10 174.8(2) . . . . ?
O3 C8 C9 C14 -7.2(3) . . . . ?
O4 C8 C9 C10 -4.6(3) . . . . ?
O4 C8 C9 C14 173.4(2) . . . . ?
O10 C12 C11 C10 -178.5(2) . . . . ?
O9 C5 C4 C3 176.7(2) . . . . ?
C8 C9 C10 C11 177.2(2) . . . . ?
C8 C9 C14 C13 -177.4(2) . . . . ?
C9 C10 C11 C12 0.1(4) . . . . ?
C9 C14 C13 C12 0.3(3) . . . . ?
C2 C7 C6 C5 -0.9(3) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C10 C9 C14 C13 0.6(3) . . . . ?
C16 C21 C20 C19 -0.2(4) . . . . ?
C16 C17 C18 C19 -0.6(3) . . . . ?
C14 C9 C10 C11 -0.8(4) . . . . ?
C14 C13 C12 O10 178.3(2) . . . . ?
C14 C13 C12 C11 -1.1(3) . . . . ?
C1 C2 C7 C6 172.8(2) . . . . ?
C1 C2 C3 C4 -172.1(2) . . . . ?
C13 C12 C11 C10 0.9(4) . . . . ?
C21 C16 C15 O6 -8.5(3) . . . . ?
C21 C16 C15 O5 170.5(2) . . . . ?
C21 C16 C17 C18 0.8(3) . . . . ?
C15 C16 C21 C20 179.2(2) . . . . ?
C15 C16 C17 C18 -178.9(2) . . . . ?
C7 C2 C1 O1 -8.0(3) . . . . ?
C7 C2 C1 O2 176.1(2) . . . . ?
C7 C2 C3 C4 2.3(3) . . . . ?
C7 C6 C5 O9 -176.0(2) . . . . ?
C7 C6 C5 C4 2.9(4) . . . . ?
C17 C16 C21 C20 -0.5(3) . . . . ?
C17 C16 C15 O6 171.2(2) . . . . ?
C17 C16 C15 O5 -9.8(3) . . . . ?
C18 C19 C20 C21 0.4(4) . . . . ?
C3 C2 C1 O1 166.3(2) . . . . ?
C3 C2 C1 O2 -9.6(3) . . . . ?
C3 C2 C7 C6 -1.6(3) . . . . ?
C6 C5 C4 C3 -2.3(4) . . . . ?
C20 C19 C18 C17 -0.1(3) . . . . ?
O11 C19 C18 C17 178.8(2) . . . . ?
O11 C19 C20 C21 -178.5(2) . . . . ?

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

data_jo2022_b2
_database_code_depnum_ccdc_archive 'CCDC 2269119'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 Eu2 O22, 2(H2 O)'
_chemical_formula_sum            'C42 H42 Eu2 O24'
_chemical_formula_weight         1234.67
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Eu C H O'
_chemical_oxdiff_usercomment     'Colourless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.4168(3)
_cell_length_b                   14.9277(5)
_cell_length_c                   15.5044(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.9590(10)
_cell_angle_gamma                90
_cell_volume                     2318.00(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14676
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.7900
_cell_measurement_theta_min      4.2000
_shelx_estimated_absorpt_T_max   0.082
_shelx_estimated_absorpt_T_min   0.029
_exptl_absorpt_coefficient_mu    19.940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_preparation       
'Seeded an aqueous solution of the cleaned Eu(4hob)3 precipitate, made by metathesis with Na4hob and EuCl3, with a single crystal of the yttrium dimer, prepared in the same way.'
_exptl_crystal_recrystallization_method 
'From water, seeded with the yttrium analogue.'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24759
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.237
_diffrn_reflns_theta_min         4.191
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00 120.00   0.50    0.06    --   47.64  54.00-138.00  172
  2  ω     94.00 178.00   0.50    0.25    --  107.75  54.00-138.00  168
  3  ω    153.00 178.00   0.50    0.25    --  107.75  30.00   0.00   50
  4  ω    112.00 138.00   0.50    0.25    --  107.75  30.00   0.00   52
  5  ω     51.00 104.00   0.50    0.25    --  107.75 -94.00 -60.00  106
  6  ω     34.00  95.00   0.50    0.06    --   47.64-125.00  60.00  122
  7  ω     36.00  61.00   0.50    0.25    --  107.75-125.00   0.00   50
  8  ω     39.00  92.00   0.50    0.25    --  107.75 -94.00-180.00  106
  9  ω     35.00  98.00   0.50    0.25    --  107.75 -77.00-150.00  126
 10  ω     37.00  62.00   0.50    0.25    --  107.75 -45.00-150.00   50
 11  ω    105.00 131.00   0.50    0.25    --  107.75 -77.00-150.00   52
 12  ω     48.00  74.00   0.50    0.25    --  107.75 -45.00 -90.00   52
 13  ω     36.00  76.00   0.50    0.25    --  107.75 -45.00  30.00   80
 14  ω     35.00  90.00   0.50    0.25    --  107.75 -54.00  78.00  110
 15  ω     36.00  61.00   0.50    0.25    --  107.75 -45.00 120.00   50
 16  ω     33.00  64.00   0.50    0.25    --  107.75 -30.00  60.00   62
 17  ω    -24.00  62.00   0.50    0.06    --   47.64 -54.00  78.00  172
 18  ω     33.00  62.00   0.50    0.25    --  107.75 -30.00 -30.00   58
 19  ω     33.00  66.00   0.50    0.25    --  107.75 -30.00 -60.00   66
 20  ω     41.00  66.00   0.50    0.25    --  107.75 -45.00-120.00   50
 21  ω     37.00  76.00   0.50    0.25    --  107.75 -45.00-180.00   78
 22  ω     33.00  66.00   0.50    0.25    --  107.75 -30.00-150.00   66
 23  ω     33.00  66.00   0.50    0.25    --  107.75 -30.00-120.00   66
 24  ω     34.00  64.00   0.50    0.25    --  107.75 -30.00 -90.00   60
 25  ω     38.00  65.00   0.50    0.25    --  107.75 -30.00   0.00   54
 26  ω     33.00  66.00   0.50    0.25    --  107.75 -30.00  90.00   66
 27  ω     33.00 122.00   0.50    0.25    --  107.75 -15.00  60.00  178
 28  ω    -62.00  25.00   0.50    0.06    --  -47.64  54.00-138.00  174
 29  ω    -92.00 -14.00   0.50    0.25    --  -86.25  54.00-138.00  156
 30  ω   -120.00 -33.00   0.50    0.06    --  -47.64 -54.00  78.00  174
 31  ω   -159.00 -72.00   0.50    0.25    --  -86.25 -54.00  78.00  174
 32  ω   -120.00 -73.00   0.50    0.06    --  -47.64-125.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0868193000
_diffrn_orient_matrix_UB_12      -0.0589138000
_diffrn_orient_matrix_UB_13      0.0753064000
_diffrn_orient_matrix_UB_21      -0.0785147000
_diffrn_orient_matrix_UB_22      0.0337987000
_diffrn_orient_matrix_UB_23      0.0645430000
_diffrn_orient_matrix_UB_31      -0.0997351000
_diffrn_orient_matrix_UB_32      -0.0777280000
_diffrn_orient_matrix_UB_33      -0.0290360000
_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                4587
_reflns_number_total             4842
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.060
_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)+(0.0691P)²+1.3046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.0988
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Free rotating group:
 O12(H12A,H12B)
1.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
1.c Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
1.d Tetrahedral OH refined with riding coordinates:
 O9(H9)
1.e Idealised tetrahedral OH refined as rotating group:
 O10(H10), O11(H11A)
;
_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
Eu1 Eu 0.46326(2) 0.14781(2) 0.41841(2) 0.00872(9) Uani 1 1 d . . . . .
O3 O 0.5584(2) 0.28117(15) 0.50877(14) 0.0113(4) Uani 1 1 d . . . . .
O6 O 0.6401(2) -0.00664(15) 0.60413(14) 0.0102(4) Uani 1 1 d . . . . .
O4 O 0.5413(2) 0.28219(14) 0.36533(14) 0.0116(4) Uani 1 1 d . . . . .
O1 O 0.2776(2) 0.18084(15) 0.28683(14) 0.0102(4) Uani 1 1 d . . . . .
O5 O 0.6661(2) 0.08430(16) 0.49592(14) 0.0125(4) Uani 1 1 d . . . . .
O7 O 0.5600(2) 0.10141(16) 0.30090(15) 0.0136(4) Uani 1 1 d . . . . .
H7A H 0.590421 0.047562 0.293490 0.020 Uiso 1 1 d R U . . .
H7B H 0.570713 0.132954 0.255605 0.020 Uiso 1 1 d R U . . .
O8 O 0.4335(2) 0.11297(16) 0.56021(14) 0.0130(4) Uani 1 1 d . . . . .
H8A H 0.445894 0.159960 0.593197 0.019 Uiso 1 1 d R U . . .
H8B H 0.494778 0.076799 0.588126 0.019 Uiso 1 1 d R U . . .
O2 O 0.2559(2) 0.21957(15) 0.41860(14) 0.0116(4) Uani 1 1 d . . . . .
O12 O 0.3810(2) 0.30744(16) 0.19658(15) 0.0140(4) Uani 1 1 d G . . . .
H12A H 0.441559 0.302993 0.245934 0.021 Uiso 1 1 d G U . . .
H12B H 0.332630 0.261254 0.194962 0.021 Uiso 1 1 d G U . . .
O10 O 0.7739(2) 0.67300(17) 0.44971(16) 0.0162(5) Uani 1 1 d . . . . .
H10 H 0.766089 0.700655 0.493687 0.024 Uiso 1 1 calc R U . . .
O9 O -0.3516(2) 0.22419(17) 0.18780(15) 0.0163(5) Uani 1 1 d . . . . .
H9 H -0.372592 0.208633 0.135049 0.024 Uiso 1 1 calc R U . . .
C8 C 0.5747(3) 0.3223(2) 0.4405(2) 0.0100(6) Uani 1 1 d . . . . .
C9 C 0.6318(3) 0.4132(2) 0.4469(2) 0.0099(6) Uani 1 1 d . . . . .
C2 C 0.0596(3) 0.2222(2) 0.2944(2) 0.0101(6) Uani 1 1 d . . . . .
C10 C 0.6580(3) 0.4518(2) 0.3713(2) 0.0125(6) Uani 1 1 d . . . . .
H10A H 0.642672 0.418706 0.318584 0.015 Uiso 1 1 calc R U . . .
C16 C 0.8602(3) 0.0403(2) 0.6077(2) 0.0101(6) Uani 1 1 d . . . . .
C14 C 0.6575(3) 0.4637(2) 0.5262(2) 0.0112(6) Uani 1 1 d . . . . .
H14 H 0.642082 0.438646 0.577378 0.013 Uiso 1 1 calc R U . . .
C1 C 0.2034(3) 0.2082(2) 0.3342(2) 0.0085(5) Uani 1 1 d . . . . .
C13 C 0.7054(3) 0.5503(2) 0.5291(2) 0.0104(6) Uani 1 1 d . . . . .
H13 H 0.721969 0.583335 0.581877 0.012 Uiso 1 1 calc R U . . .
C21 C 0.9142(3) 0.0027(2) 0.6922(2) 0.0136(6) Uani 1 1 d . . . . .
H21 H 0.858169 -0.023091 0.722700 0.016 Uiso 1 1 calc R U . . .
C15 C 0.7140(3) 0.0396(2) 0.56620(19) 0.0095(6) Uani 1 1 d . . . . .
C7 C 0.0052(3) 0.2156(2) 0.2013(2) 0.0124(6) Uani 1 1 d . . . . .
H7 H 0.061409 0.209151 0.164308 0.015 Uiso 1 1 calc R U . . .
C12 C 0.7290(3) 0.5880(2) 0.4522(2) 0.0123(6) Uani 1 1 d . . . . .
C17 C 0.9453(3) 0.0800(2) 0.5628(2) 0.0125(6) Uani 1 1 d . . . . .
H17 H 0.909659 0.106366 0.506974 0.015 Uiso 1 1 calc R U . . .
C19 C 1.1351(3) 0.0413(2) 0.6849(2) 0.0128(6) Uani 1 1 d . . . . .
C18 C 1.0824(3) 0.0802(2) 0.6009(2) 0.0149(6) Uani 1 1 d . . . . .
H18 H 1.138739 0.106037 0.570597 0.018 Uiso 1 1 calc R U . . .
C11 C 0.7061(3) 0.5380(2) 0.3736(2) 0.0150(6) Uani 1 1 d . . . . .
H11 H 0.723310 0.562725 0.322861 0.018 Uiso 1 1 calc R U . . .
C3 C -0.0259(3) 0.2341(2) 0.3489(2) 0.0134(6) Uani 1 1 d . . . . .
H3 H 0.009927 0.240966 0.410426 0.016 Uiso 1 1 calc R U . . .
C6 C -0.1315(3) 0.2185(2) 0.1641(2) 0.0126(6) Uani 1 1 d . . . . .
H6 H -0.167104 0.215405 0.102157 0.015 Uiso 1 1 calc R U . . .
C5 C -0.2160(3) 0.2261(2) 0.2197(2) 0.0129(6) Uani 1 1 d . . . . .
C20 C 1.0512(3) 0.0036(2) 0.7309(2) 0.0166(6) Uani 1 1 d . . . . .
H20 H 1.086830 -0.020999 0.787521 0.020 Uiso 1 1 calc R U . . .
C4 C -0.1628(3) 0.2360(3) 0.3127(2) 0.0166(7) Uani 1 1 d . . . . .
H4 H -0.218986 0.243715 0.349491 0.020 Uiso 1 1 calc R U . . .
O11 O 1.2699(2) 0.03799(17) 0.72488(17) 0.0181(5) Uani 1 1 d . . . . .
H11A H 1.304431 0.084924 0.715243 0.027 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
Eu1 O3 2.479(2) . ?
Eu1 O6 2.348(2) 3_656 ?
Eu1 O4 2.394(2) . ?
Eu1 O1 2.444(2) . ?
Eu1 O5 2.326(2) . ?
Eu1 O7 2.413(2) . ?
Eu1 O8 2.361(2) . ?
Eu1 H8A 2.7712 . ?
Eu1 H8B 2.7714 . ?
Eu1 O2 2.412(2) . ?
O3 C8 1.274(4) . ?
O6 C15 1.290(4) . ?
O4 C8 1.271(4) . ?
O1 C1 1.271(4) . ?
O5 C15 1.258(4) . ?
O7 H7A 0.8832 . ?
O7 H7B 0.8779 . ?
O8 H8A 0.8567 . ?
O8 H8B 0.8569 . ?
O2 C1 1.283(4) . ?
O12 H12A 0.8502 . ?
O12 H12B 0.8500 . ?
O10 H10 0.8200 . ?
O10 C12 1.357(4) . ?
O9 H9 0.8200 . ?
O9 C5 1.362(4) . ?
C8 C9 1.475(4) . ?
C9 C10 1.398(4) . ?
C9 C14 1.405(4) . ?
C2 C1 1.470(4) . ?
C2 C7 1.402(4) . ?
C2 C3 1.397(4) . ?
C10 H10A 0.9300 . ?
C10 C11 1.378(5) . ?
C16 C21 1.393(4) . ?
C16 C15 1.482(4) . ?
C16 C17 1.400(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.381(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.400(4) . ?
C21 H21 0.9300 . ?
C21 C20 1.388(4) . ?
C7 H7 0.9300 . ?
C7 C6 1.382(4) . ?
C12 C11 1.392(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.388(4) . ?
C19 C18 1.394(5) . ?
C19 C20 1.389(5) . ?
C19 O11 1.370(4) . ?
C18 H18 0.9300 . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.382(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.396(4) . ?
C5 C4 1.403(4) . ?
C20 H20 0.9300 . ?
C4 H4 0.9300 . ?
O11 H11A 0.8200 . ?

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
O3 Eu1 H8A 61.2 . . ?
O3 Eu1 H8B 81.1 . . ?
O6 Eu1 O3 154.21(7) 3_656 . ?
O6 Eu1 O4 152.38(7) 3_656 . ?
O6 Eu1 O1 80.32(7) 3_656 . ?
O6 Eu1 O7 84.24(8) 3_656 . ?
O6 Eu1 O8 76.63(8) 3_656 . ?
O6 Eu1 H8A 93.1 3_656 . ?
O6 Eu1 H8B 74.2 3_656 . ?
O6 Eu1 O2 91.41(8) 3_656 . ?
O4 Eu1 O3 53.16(7) . . ?
O4 Eu1 O1 79.02(7) . . ?
O4 Eu1 O7 74.29(8) . . ?
O4 Eu1 H8A 113.6 . . ?
O4 Eu1 H8B 133.2 . . ?
O4 Eu1 O2 90.99(8) . . ?
O1 Eu1 O3 114.29(7) . . ?
O1 Eu1 H8A 123.6 . . ?
O1 Eu1 H8B 136.9 . . ?
O5 Eu1 O3 82.53(8) . . ?
O5 Eu1 O6 91.45(8) . 3_656 ?
O5 Eu1 O4 99.96(8) . . ?
O5 Eu1 O1 155.66(7) . . ?
O5 Eu1 O7 76.38(7) . . ?
O5 Eu1 O8 76.25(8) . . ?
O5 Eu1 H8A 79.4 . . ?
O5 Eu1 H8B 60.0 . . ?
O5 Eu1 O2 150.11(7) . . ?
O7 Eu1 O3 118.17(7) . . ?
O7 Eu1 O1 80.00(7) . . ?
O7 Eu1 H8A 155.5 . . ?
O7 Eu1 H8B 129.9 . . ?
O8 Eu1 O3 77.59(8) . . ?
O8 Eu1 O4 130.44(8) . . ?
O8 Eu1 O1 123.05(7) . . ?
O8 Eu1 O7 145.97(8) . . ?
O8 Eu1 H8A 16.9 . . ?
O8 Eu1 H8B 16.9 . . ?
O8 Eu1 O2 75.51(7) . . ?
H8A Eu1 H8B 28.2 . . ?
O2 Eu1 O3 82.05(7) . . ?
O2 Eu1 O1 53.72(7) . . ?
O2 Eu1 O7 133.50(7) . . ?
O2 Eu1 H8A 70.8 . . ?
O2 Eu1 H8B 92.4 . . ?
C8 O3 Eu1 92.36(18) . . ?
C15 O6 Eu1 135.97(19) . 3_656 ?
C8 O4 Eu1 96.43(18) . . ?
C1 O1 Eu1 92.85(17) . . ?
C15 O5 Eu1 138.68(19) . . ?
Eu1 O7 H7A 126.8 . . ?
Eu1 O7 H7B 128.4 . . ?
H7A O7 H7B 104.8 . . ?
Eu1 O8 H8A 109.8 . . ?
Eu1 O8 H8B 109.8 . . ?
H8A O8 H8B 104.2 . . ?
C1 O2 Eu1 94.04(17) . . ?
H12A O12 H12B 104.5 . . ?
C12 O10 H10 109.5 . . ?
C5 O9 H9 109.5 . . ?
O3 C8 C9 122.1(3) . . ?
O4 C8 O3 118.0(3) . . ?
O4 C8 C9 119.9(3) . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 C14 118.6(3) . . ?
C14 C9 C8 121.9(3) . . ?
C7 C2 C1 119.9(3) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 C7 119.2(3) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 C9 121.0(3) . . ?
C11 C10 H10A 119.5 . . ?
C21 C16 C15 120.4(3) . . ?
C21 C16 C17 119.4(3) . . ?
C17 C16 C15 120.2(3) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.7(3) . . ?
C13 C14 H14 119.6 . . ?
O1 C1 O2 118.4(3) . . ?
O1 C1 C2 121.0(3) . . ?
O2 C1 C2 120.6(3) . . ?
C14 C13 H13 120.2 . . ?
C14 C13 C12 119.7(3) . . ?
C12 C13 H13 120.2 . . ?
C16 C21 H21 119.9 . . ?
C20 C21 C16 120.2(3) . . ?
C20 C21 H21 119.9 . . ?
O6 C15 C16 118.5(3) . . ?
O5 C15 O6 122.3(3) . . ?
O5 C15 C16 119.2(3) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
O10 C12 C13 122.9(3) . . ?
O10 C12 C11 117.0(3) . . ?
C11 C12 C13 120.1(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.5(3) . . ?
C18 C17 H17 119.8 . . ?
C20 C19 C18 120.4(3) . . ?
O11 C19 C18 121.9(3) . . ?
O11 C19 C20 117.7(3) . . ?
C17 C18 C19 119.5(3) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C10 C11 C12 119.8(3) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C7 C6 H6 120.1 . . ?
C7 C6 C5 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
O9 C5 C6 122.7(3) . . ?
O9 C5 C4 116.9(3) . . ?
C6 C5 C4 120.4(3) . . ?
C21 C20 C19 120.0(3) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C3 C4 C5 119.1(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C19 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O3 C8 O4 -0.9(3) . . . . ?
Eu1 O3 C8 C9 179.9(3) . . . . ?
Eu1 O6 C15 O5 80.8(4) 3_656 . . . ?
Eu1 O6 C15 C16 -99.7(3) 3_656 . . . ?
Eu1 O4 C8 O3 0.9(3) . . . . ?
Eu1 O4 C8 C9 -179.8(2) . . . . ?
Eu1 O1 C1 O2 9.9(3) . . . . ?
Eu1 O1 C1 C2 -167.0(3) . . . . ?
Eu1 O5 C15 O6 21.5(5) . . . . ?
Eu1 O5 C15 C16 -158.0(2) . . . . ?
Eu1 O2 C1 O1 -10.0(3) . . . . ?
Eu1 O2 C1 C2 166.9(2) . . . . ?
O3 C8 C9 C10 174.5(3) . . . . ?
O3 C8 C9 C14 -7.4(5) . . . . ?
O4 C8 C9 C10 -4.8(4) . . . . ?
O4 C8 C9 C14 173.4(3) . . . . ?
O10 C12 C11 C10 -178.7(3) . . . . ?
O9 C5 C4 C3 177.0(3) . . . . ?
C8 C9 C10 C11 177.3(3) . . . . ?
C8 C9 C14 C13 -177.1(3) . . . . ?
C9 C10 C11 C12 -0.2(5) . . . . ?
C9 C14 C13 C12 -0.2(5) . . . . ?
C2 C7 C6 C5 -1.4(5) . . . . ?
C2 C3 C4 C5 -0.3(5) . . . . ?
C10 C9 C14 C13 1.1(5) . . . . ?
C16 C21 C20 C19 -0.7(5) . . . . ?
C16 C17 C18 C19 -0.6(5) . . . . ?
C14 C9 C10 C11 -1.0(5) . . . . ?
C14 C13 C12 O10 178.9(3) . . . . ?
C14 C13 C12 C11 -1.0(5) . . . . ?
C1 C2 C7 C6 172.7(3) . . . . ?
C1 C2 C3 C4 -171.8(3) . . . . ?
C13 C12 C11 C10 1.1(5) . . . . ?
C21 C16 C15 O6 -9.1(4) . . . . ?
C21 C16 C15 O5 170.4(3) . . . . ?
C21 C16 C17 C18 1.4(5) . . . . ?
C15 C16 C21 C20 -179.9(3) . . . . ?
C15 C16 C17 C18 -179.4(3) . . . . ?
C7 C2 C1 O1 -7.6(5) . . . . ?
C7 C2 C1 O2 175.6(3) . . . . ?
C7 C2 C3 C4 2.5(5) . . . . ?
C7 C6 C5 O9 -176.1(3) . . . . ?
C7 C6 C5 C4 3.7(5) . . . . ?
C17 C16 C21 C20 -0.8(5) . . . . ?
C17 C16 C15 O6 171.8(3) . . . . ?
C17 C16 C15 O5 -8.7(4) . . . . ?
C18 C19 C20 C21 1.5(5) . . . . ?
C3 C2 C1 O1 166.7(3) . . . . ?
C3 C2 C1 O2 -10.1(5) . . . . ?
C3 C2 C7 C6 -1.7(5) . . . . ?
C6 C5 C4 C3 -2.8(5) . . . . ?
C20 C19 C18 C17 -0.8(5) . . . . ?
O11 C19 C18 C17 178.6(3) . . . . ?
O11 C19 C20 C21 -178.0(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'Thick hydrocarbon oil.'
_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 2.342
_oxdiff_exptl_absorpt_empirical_full_min 0.566
####################################################################### 
# 
# 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_p1
_database_code_depnum_ccdc_archive 'CCDC 2269118'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C84 H76 O44 Pr4, 4(H2 O)'
_chemical_formula_sum            'C84 H84 O48 Pr4'
_chemical_formula_weight         2425.15
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.0467(3)
_cell_length_b                   14.1840(4)
_cell_length_c                   14.6821(4)
_cell_angle_alpha                93.1860(10)
_cell_angle_beta                 102.7450(10)
_cell_angle_gamma                105.5620(10)
_cell_volume                     2339.57(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7595
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.85
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   0.814
_shelx_estimated_absorpt_T_min   0.674
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4282
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.068
_diffrn_reflns_theta_min         1.433
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10968
_reflns_number_total             13334
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0217(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         13334
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0379P)²+0.2115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0785
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O24-H24A = O24-H24B
 0.85 with sigma of 0.02
 H24A-H24B
 1.34 with sigma of 0.04
 Pr2-H15A \\sim Pr2-H15B
 with sigma of 0.02
2.a Free rotating group:
 O23(H23A,H23B), O15(H15A,H15B)
2.b Rotating group:
 O16(H16A,H16B), O7(H7A,H7B), O8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C24(H24), C14(H14), C6(H6), C11(H11), C34(H34), C39(H39), C31(H31),
 C38(H38), C4(H4), C10(H10), C3(H3), C28(H28), C13(H13), C35(H35), C17(H17A),
 C20(H20A), C32(H32), C25(H25), C18(H18A), C21(H21A), C27(H27), C42(H42),
 C41(H41)
2.d Tetrahedral OH refined with riding coordinates:
 O17(H17), O21(H21)
2.e Idealised tetrahedral OH refined as rotating group:
 O18(H18), O20(H20), O22(H22), O19(H19)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.61657(2) 0.12578(2) 0.63590(2) 0.01731(5) Uani 1 1 d . . . . .
Pr2 Pr 0.79272(2) 0.40009(2) 0.81711(2) 0.01934(5) Uani 1 1 d D . . . .
O1 O 0.77813(15) 0.22987(13) 0.55501(11) 0.0247(4) Uani 1 1 d . . . . .
O2 O 0.59095(15) 0.18097(12) 0.47539(11) 0.0233(4) Uani 1 1 d . . . . .
O6 O 0.81609(16) 0.24261(12) 0.76540(11) 0.0266(4) Uani 1 1 d . . . . .
O16 O 0.87147(16) 0.41438(13) 0.66923(12) 0.0285(4) Uani 1 1 d . . . . .
H16A H 0.844823 0.455348 0.636967 0.043 Uiso 1 1 d R U . . .
H16B H 0.842821 0.359678 0.633366 0.043 Uiso 1 1 d R U . . .
O7 O 0.52080(16) -0.04095(13) 0.67687(12) 0.0297(4) Uani 1 1 d . . . . .
H7A H 0.449112 -0.045446 0.700208 0.045 Uiso 1 1 d R U . . .
H7B H 0.485780 -0.093787 0.623067 0.045 Uiso 1 1 d R U . . .
O10 O 0.58418(17) 0.40847(15) 0.76066(12) 0.0352(5) Uani 1 1 d . . . . .
O9 O 0.62248(16) 0.30589(13) 0.66386(12) 0.0270(4) Uani 1 1 d . . . . .
O18 O -0.11364(16) 0.13612(16) 0.43809(13) 0.0377(5) Uani 1 1 d . . . . .
H18 H -0.123562 0.164132 0.484730 0.057 Uiso 1 1 calc R U . . .
O11 O 0.67628(16) 0.28668(14) 0.90926(12) 0.0302(4) Uani 1 1 d . . . . .
O4 O 0.34786(17) -0.00062(14) 0.45868(13) 0.0313(4) Uani 1 1 d . . . . .
O12 O 0.86237(16) 0.35859(14) 0.98027(12) 0.0343(5) Uani 1 1 d . . . . .
O3 O 0.41026(16) 0.10907(14) 0.58544(13) 0.0310(4) Uani 1 1 d . . . . .
O8 O 0.53600(17) 0.13662(14) 0.78066(12) 0.0333(4) Uani 1 1 d . . . . .
H8A H 0.580565 0.186672 0.818713 0.050 Uiso 1 1 d R U . . .
H8B H 0.469165 0.148391 0.765303 0.050 Uiso 1 1 d R U . . .
O13 O 0.76658(18) 0.54172(13) 0.91387(12) 0.0327(4) Uani 1 1 d . . . . .
O23 O 0.6558(2) 0.48378(16) 1.05416(14) 0.0407(5) Uani 1 1 d G . . . .
H23A H 0.692689 0.513743 1.016248 0.061 Uiso 1 1 d G U . . .
H23B H 0.619079 0.522663 1.070777 0.061 Uiso 1 1 d G U . . .
O14 O 0.80713(19) 0.57203(13) 0.77806(12) 0.0386(5) Uani 1 1 d . . . . .
O20 O 0.19403(19) 0.42241(17) 0.40001(13) 0.0443(5) Uani 1 1 d . . . . .
H20 H 0.205979 0.415158 0.347560 0.066 Uiso 1 1 calc R U . . .
O17 O 0.81099(18) 0.47488(16) 0.20771(14) 0.0450(5) Uani 1 1 d . . . . .
H17 H 0.752389 0.470947 0.165146 0.067 Uiso 1 1 calc R U . . .
O5 O 0.77795(15) 0.08220(12) 0.75476(12) 0.0277(4) Uani 1 1 d . . . . .
O15 O 1.00435(17) 0.49115(16) 0.87582(13) 0.0423(5) Uani 1 1 d G . . . .
H15A H 1.057009 0.503793 0.844490 0.064 Uiso 1 1 d DG U . . .
H15B H 1.034752 0.530811 0.926282 0.064 Uiso 1 1 d DG U . . .
O24 O 0.46591(19) 0.38750(19) 0.89683(15) 0.0475(6) Uani 1 1 d D . . . .
H24A H 0.499(3) 0.409(3) 0.8543(18) 0.071 Uiso 1 1 d D U . . .
H24B H 0.521(3) 0.394(3) 0.9449(17) 0.071 Uiso 1 1 d D U . . .
O22 O 0.6717(2) 0.96066(16) 0.88114(16) 0.0517(6) Uani 1 1 d . . . . .
H22 H 0.700354 0.997985 0.846242 0.077 Uiso 1 1 calc R U . . .
O19 O 1.33852(18) 0.19423(17) 0.84095(17) 0.0491(6) Uani 1 1 d . . . . .
H19 H 1.379875 0.251443 0.857054 0.074 Uiso 1 1 calc R U . . .
O21 O 0.70534(18) 0.06389(15) 1.27246(13) 0.0411(5) Uani 1 1 d . . . . .
H21 H 0.763602 0.080994 1.317334 0.062 Uiso 1 1 calc R U . . .
C9 C 0.2173(2) 0.08750(17) 0.49244(16) 0.0216(5) Uani 1 1 d . . . . .
C2 C 0.7259(2) 0.29546(18) 0.40946(16) 0.0237(5) Uani 1 1 d . . . . .
C22 C 0.5590(2) 0.36047(18) 0.67976(17) 0.0237(5) Uani 1 1 d . . . . .
C15 C 0.8530(2) 0.16594(18) 0.77402(16) 0.0223(5) Uani 1 1 d . . . . .
C7 C 0.6374(2) 0.29814(18) 0.33174(17) 0.0267(5) Uani 1 1 d . . . . .
H7 H 0.559689 0.260001 0.325959 0.032 Uiso 1 1 calc R U . . .
C8 C 0.3321(2) 0.06344(18) 0.51314(16) 0.0223(5) Uani 1 1 d . . . . .
C24 C 0.4518(3) 0.3449(2) 0.51149(17) 0.0351(7) Uani 1 1 d . . . . .
H24 H 0.504568 0.313571 0.495180 0.042 Uiso 1 1 calc R U . . .
C30 C 0.7527(2) 0.23312(19) 1.05527(17) 0.0283(6) Uani 1 1 d . . . . .
C29 C 0.7651(2) 0.29537(18) 0.97838(16) 0.0248(5) Uani 1 1 d . . . . .
C14 C 0.1920(2) 0.1501(2) 0.55639(18) 0.0309(6) Uani 1 1 d . . . . .
H14 H 0.249340 0.179861 0.611288 0.037 Uiso 1 1 calc R U . . .
C6 C 0.6637(2) 0.35672(19) 0.26311(17) 0.0293(6) Uani 1 1 d . . . . .
H6 H 0.604048 0.358216 0.211255 0.035 Uiso 1 1 calc R U . . .
C1 C 0.6963(2) 0.23189(17) 0.48305(15) 0.0207(5) Uani 1 1 d . . . . .
C16 C 0.9809(2) 0.17644(18) 0.79735(17) 0.0251(5) Uani 1 1 d . . . . .
C11 C 0.0224(2) 0.0637(2) 0.39250(18) 0.0310(6) Uani 1 1 d . . . . .
H11 H -0.034349 0.035452 0.336868 0.037 Uiso 1 1 calc R U . . .
C12 C -0.0023(2) 0.12431(19) 0.45768(17) 0.0262(5) Uani 1 1 d . . . . .
C36 C 0.7766(2) 0.59910(18) 0.85055(17) 0.0283(6) Uani 1 1 d . . . . .
C23 C 0.4617(2) 0.37360(18) 0.60518(16) 0.0235(5) Uani 1 1 d . . . . .
C34 C 0.8343(2) 0.1854(2) 1.20404(18) 0.0354(7) Uani 1 1 d . . . . .
H34 H 0.898539 0.191751 1.254888 0.043 Uiso 1 1 calc R U . . .
C26 C 0.2841(2) 0.4056(2) 0.46567(17) 0.0303(6) Uani 1 1 d . . . . .
C39 C 0.7529(3) 0.8516(2) 0.8026(2) 0.0400(7) Uani 1 1 d . . . . .
H39 H 0.772017 0.896281 0.760496 0.048 Uiso 1 1 calc R U . . .
C31 C 0.6444(3) 0.1653(2) 1.05295(19) 0.0395(7) Uani 1 1 d . . . . .
H31 H 0.580360 0.157968 1.001688 0.047 Uiso 1 1 calc R U . . .
C37 C 0.7505(3) 0.69462(19) 0.85854(17) 0.0307(6) Uani 1 1 d . . . . .
C38 C 0.7795(3) 0.7631(2) 0.79700(19) 0.0368(7) Uani 1 1 d . . . . .
H38 H 0.817383 0.749018 0.751428 0.044 Uiso 1 1 calc R U . . .
C33 C 0.7258(3) 0.1202(2) 1.20158(18) 0.0318(6) Uani 1 1 d . . . . .
C4 C 0.8684(2) 0.4113(2) 0.34821(19) 0.0329(6) Uani 1 1 d . . . . .
H4 H 0.946015 0.449396 0.353323 0.039 Uiso 1 1 calc R U . . .
C10 C 0.1313(2) 0.0453(2) 0.41036(17) 0.0290(6) Uani 1 1 d . . . . .
H10 H 0.147305 0.004039 0.366704 0.035 Uiso 1 1 calc R U . . .
C3 C 0.8422(2) 0.35242(19) 0.41714(18) 0.0291(6) Uani 1 1 d . . . . .
H3 H 0.902218 0.350892 0.468661 0.035 Uiso 1 1 calc R U . . .
C28 C 0.3809(3) 0.4189(2) 0.62777(19) 0.0392(7) Uani 1 1 d . . . . .
H28 H 0.386854 0.439186 0.690424 0.047 Uiso 1 1 calc R U . . .
C13 C 0.0827(2) 0.1685(2) 0.53918(18) 0.0336(6) Uani 1 1 d . . . . .
H13 H 0.066559 0.210299 0.582253 0.040 Uiso 1 1 calc R U . . .
C35 C 0.8479(2) 0.2415(2) 1.13096(18) 0.0337(6) Uani 1 1 d . . . . .
H35 H 0.921566 0.285083 1.132722 0.040 Uiso 1 1 calc R U . . .
C17 C 1.0626(2) 0.2638(2) 0.78901(19) 0.0330(6) Uani 1 1 d . . . . .
H17A H 1.036759 0.318436 0.773810 0.040 Uiso 1 1 calc R U . . .
C20 C 1.1425(3) 0.1035(2) 0.8368(2) 0.0405(7) Uani 1 1 d . . . . .
H20A H 1.169676 0.050010 0.853959 0.049 Uiso 1 1 calc R U . . .
C32 C 0.6302(3) 0.1087(2) 1.1251(2) 0.0430(8) Uani 1 1 d . . . . .
H32 H 0.557349 0.063318 1.122537 0.052 Uiso 1 1 calc R U . . .
C25 C 0.3647(3) 0.3623(2) 0.44216(19) 0.0407(7) Uani 1 1 d . . . . .
H25 H 0.360384 0.344668 0.379238 0.049 Uiso 1 1 calc R U . . .
C5 C 0.7791(3) 0.4131(2) 0.27192(18) 0.0301(6) Uani 1 1 d . . . . .
C18 C 1.1806(3) 0.2702(2) 0.8029(2) 0.0375(7) Uani 1 1 d . . . . .
H18A H 1.233966 0.328902 0.796359 0.045 Uiso 1 1 calc R U . . .
C40 C 0.6982(3) 0.8741(2) 0.87029(19) 0.0366(7) Uani 1 1 d . . . . .
C21 C 1.0230(3) 0.0962(2) 0.8215(2) 0.0357(7) Uani 1 1 d . . . . .
H21A H 0.969880 0.037091 0.827280 0.043 Uiso 1 1 calc R U . . .
C27 C 0.2925(3) 0.4340(2) 0.55887(19) 0.0448(8) Uani 1 1 d . . . . .
H27 H 0.238104 0.463480 0.574966 0.054 Uiso 1 1 calc R U . . .
C19 C 1.2212(2) 0.1906(2) 0.82668(19) 0.0363(7) Uani 1 1 d . . . . .
C42 C 0.6944(3) 0.7180(2) 0.9258(2) 0.0448(8) Uani 1 1 d . . . . .
H42 H 0.673825 0.673115 0.967357 0.054 Uiso 1 1 calc R U . . .
C41 C 0.6687(3) 0.8068(2) 0.9320(2) 0.0483(8) Uani 1 1 d . . . . .
H41 H 0.631389 0.821520 0.977771 0.058 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
Pr1 O1 2.6555(16) . ?
Pr1 O2 2.5052(16) . ?
Pr1 O6 2.7630(17) . ?
Pr1 O7 2.5071(17) . ?
Pr1 O9 2.5443(17) . ?
Pr1 O4 2.3791(18) 2_656 ?
Pr1 O3 2.3736(18) . ?
Pr1 O8 2.5372(17) . ?
Pr1 O5 2.5446(17) . ?
Pr2 O6 2.4267(16) . ?
Pr2 O16 2.5515(16) . ?
Pr2 O10 2.5030(19) . ?
Pr2 O9 2.6858(17) . ?
Pr2 O11 2.5008(17) . ?
Pr2 O12 2.5147(17) . ?
Pr2 O13 2.5243(17) . ?
Pr2 O14 2.5056(18) . ?
Pr2 O15 2.4598(19) . ?
O1 C1 1.283(3) . ?
O2 C1 1.258(3) . ?
O6 C15 1.283(3) . ?
O16 H16A 0.8536 . ?
O16 H16B 0.8538 . ?
O7 H7A 0.9853 . ?
O7 H7B 0.9905 . ?
O10 C22 1.267(3) . ?
O9 C22 1.271(3) . ?
O18 H18 0.8200 . ?
O18 C12 1.366(3) . ?
O11 C29 1.275(3) . ?
O4 C8 1.257(3) . ?
O12 C29 1.264(3) . ?
O3 C8 1.260(3) . ?
O8 H8A 0.8505 . ?
O8 H8B 0.8503 . ?
O13 C36 1.274(3) . ?
O23 H23A 0.8496 . ?
O23 H23B 0.8504 . ?
O14 C36 1.272(3) . ?
O20 H20 0.8200 . ?
O20 C26 1.366(3) . ?
O17 H17 0.8200 . ?
O17 C5 1.369(3) . ?
O5 C15 1.258(3) . ?
O15 H15A 0.8503 . ?
O15 H15B 0.8502 . ?
O24 H24A 0.842(17) . ?
O24 H24B 0.834(18) . ?
O22 H22 0.8200 . ?
O22 C40 1.360(3) . ?
O19 H19 0.8200 . ?
O19 C19 1.368(3) . ?
O21 H21 0.8200 . ?
O21 C33 1.372(3) . ?
C9 C8 1.483(3) . ?
C9 C14 1.393(3) . ?
C9 C10 1.386(3) . ?
C2 C7 1.389(3) . ?
C2 C1 1.488(3) . ?
C2 C3 1.393(4) . ?
C22 C23 1.477(3) . ?
C15 C16 1.467(4) . ?
C7 H7 0.9300 . ?
C7 C6 1.378(3) . ?
C24 H24 0.9300 . ?
C24 C23 1.383(3) . ?
C24 C25 1.377(4) . ?
C30 C29 1.480(3) . ?
C30 C31 1.390(4) . ?
C30 C35 1.384(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.382(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.379(4) . ?
C16 C17 1.391(4) . ?
C16 C21 1.398(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.384(3) . ?
C11 C10 1.377(4) . ?
C12 C13 1.380(3) . ?
C36 C37 1.475(4) . ?
C23 C28 1.387(4) . ?
C34 H34 0.9300 . ?
C34 C33 1.375(4) . ?
C34 C35 1.383(3) . ?
C26 C25 1.372(4) . ?
C26 C27 1.379(4) . ?
C39 H39 0.9300 . ?
C39 C38 1.379(4) . ?
C39 C40 1.374(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.377(4) . ?
C37 C38 1.392(3) . ?
C37 C42 1.385(4) . ?
C38 H38 0.9300 . ?
C33 C32 1.387(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.384(3) . ?
C4 C5 1.378(4) . ?
C10 H10 0.9300 . ?
C3 H3 0.9300 . ?
C28 H28 0.9300 . ?
C28 C27 1.369(4) . ?
C13 H13 0.9300 . ?
C35 H35 0.9300 . ?
C17 H17A 0.9300 . ?
C17 C18 1.367(4) . ?
C20 H20A 0.9300 . ?
C20 C21 1.381(4) . ?
C20 C19 1.379(4) . ?
C32 H32 0.9300 . ?
C25 H25 0.9300 . ?
C18 H18A 0.9300 . ?
C18 C19 1.379(4) . ?
C40 C41 1.383(4) . ?
C21 H21A 0.9300 . ?
C27 H27 0.9300 . ?
C42 H42 0.9300 . ?
C42 C41 1.378(4) . ?
C41 H41 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
O1 Pr1 O6 67.43(5) . . ?
O2 Pr1 O1 50.36(5) . . ?
O2 Pr1 O6 113.67(5) . . ?
O2 Pr1 O7 126.79(5) . . ?
O2 Pr1 O9 75.56(5) . . ?
O2 Pr1 O8 139.10(6) . . ?
O2 Pr1 O5 137.28(6) . . ?
O7 Pr1 O1 146.09(6) . . ?
O7 Pr1 O6 117.06(5) . . ?
O7 Pr1 O9 141.29(6) . . ?
O7 Pr1 O8 67.73(6) . . ?
O7 Pr1 O5 74.11(6) . . ?
O9 Pr1 O1 72.44(5) . . ?
O9 Pr1 O6 65.18(5) . . ?
O9 Pr1 O5 112.54(5) . . ?
O4 Pr1 O1 77.90(6) 2_656 . ?
O4 Pr1 O2 75.72(6) 2_656 . ?
O4 Pr1 O6 114.50(6) 2_656 . ?
O4 Pr1 O7 69.82(6) 2_656 . ?
O4 Pr1 O9 147.66(6) 2_656 . ?
O4 Pr1 O8 136.76(6) 2_656 . ?
O4 Pr1 O5 79.93(6) 2_656 . ?
O3 Pr1 O1 123.59(6) . . ?
O3 Pr1 O2 75.50(6) . . ?
O3 Pr1 O6 139.52(6) . . ?
O3 Pr1 O7 76.56(6) . . ?
O3 Pr1 O9 80.77(6) . . ?
O3 Pr1 O4 105.98(6) . 2_656 ?
O3 Pr1 O8 71.78(6) . . ?
O3 Pr1 O5 145.79(6) . . ?
O8 Pr1 O1 140.70(6) . . ?
O8 Pr1 O6 78.79(6) . . ?
O8 Pr1 O9 75.58(6) . . ?
O8 Pr1 O5 81.04(6) . . ?
O5 Pr1 O1 90.62(5) . . ?
O5 Pr1 O6 48.44(5) . . ?
O6 Pr2 O16 70.67(6) . . ?
O6 Pr2 O10 112.51(6) . . ?
O6 Pr2 O9 67.94(6) . . ?
O6 Pr2 O11 78.27(6) . . ?
O6 Pr2 O12 84.89(6) . . ?
O6 Pr2 O13 163.54(6) . . ?
O6 Pr2 O14 144.45(6) . . ?
O6 Pr2 O15 98.25(7) . . ?
O16 Pr2 O9 68.84(5) . . ?
O10 Pr2 O16 103.21(6) . . ?
O10 Pr2 O9 49.63(6) . . ?
O10 Pr2 O12 120.02(6) . . ?
O10 Pr2 O13 71.27(6) . . ?
O10 Pr2 O14 73.35(7) . . ?
O11 Pr2 O16 145.73(6) . . ?
O11 Pr2 O10 75.36(6) . . ?
O11 Pr2 O9 86.51(6) . . ?
O11 Pr2 O12 51.67(6) . . ?
O11 Pr2 O13 87.62(6) . . ?
O11 Pr2 O14 134.77(6) . . ?
O12 Pr2 O16 136.03(6) . . ?
O12 Pr2 O9 134.61(6) . . ?
O12 Pr2 O13 79.68(6) . . ?
O13 Pr2 O16 124.98(6) . . ?
O13 Pr2 O9 120.09(6) . . ?
O14 Pr2 O16 73.86(6) . . ?
O14 Pr2 O9 97.09(6) . . ?
O14 Pr2 O12 123.89(6) . . ?
O14 Pr2 O13 51.71(5) . . ?
O15 Pr2 O16 75.91(6) . . ?
O15 Pr2 O10 147.26(7) . . ?
O15 Pr2 O9 144.65(6) . . ?
O15 Pr2 O11 123.73(6) . . ?
O15 Pr2 O12 72.06(6) . . ?
O15 Pr2 O13 82.47(7) . . ?
O15 Pr2 O14 75.11(8) . . ?
C1 O1 Pr1 90.65(13) . . ?
C1 O2 Pr1 98.37(14) . . ?
Pr2 O6 Pr1 112.47(6) . . ?
C15 O6 Pr1 87.75(14) . . ?
C15 O6 Pr2 155.95(15) . . ?
Pr2 O16 H16A 109.6 . . ?
Pr2 O16 H16B 109.6 . . ?
H16A O16 H16B 104.3 . . ?
Pr1 O7 H7A 114.8 . . ?
Pr1 O7 H7B 115.3 . . ?
H7A O7 H7B 98.6 . . ?
C22 O10 Pr2 98.68(15) . . ?
Pr1 O9 Pr2 111.29(6) . . ?
C22 O9 Pr1 141.87(17) . . ?
C22 O9 Pr2 90.01(14) . . ?
C12 O18 H18 109.5 . . ?
C29 O11 Pr2 94.64(14) . . ?
C8 O4 Pr1 176.40(18) . 2_656 ?
C29 O12 Pr2 94.29(14) . . ?
C8 O3 Pr1 132.29(16) . . ?
Pr1 O8 H8A 109.4 . . ?
Pr1 O8 H8B 109.4 . . ?
H8A O8 H8B 104.5 . . ?
C36 O13 Pr2 93.87(14) . . ?
H23A O23 H23B 104.4 . . ?
C36 O14 Pr2 94.79(15) . . ?
C26 O20 H20 109.5 . . ?
C5 O17 H17 109.5 . . ?
C15 O5 Pr1 98.49(14) . . ?
Pr2 O15 H15A 127.5 . . ?
Pr2 O15 H15B 125.7 . . ?
H15A O15 H15B 104.5 . . ?
H24A O24 H24B 106(3) . . ?
C40 O22 H22 109.5 . . ?
C19 O19 H19 109.5 . . ?
C33 O21 H21 109.5 . . ?
C14 C9 C8 120.8(2) . . ?
C10 C9 C8 120.5(2) . . ?
C10 C9 C14 118.6(2) . . ?
C7 C2 C1 120.1(2) . . ?
C7 C2 C3 119.2(2) . . ?
C3 C2 C1 120.7(2) . . ?
O10 C22 O9 118.7(2) . . ?
O10 C22 C23 119.5(2) . . ?
O9 C22 C23 121.7(2) . . ?
O6 C15 C16 120.0(2) . . ?
O5 C15 O6 118.7(2) . . ?
O5 C15 C16 121.0(2) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.7(2) . . ?
C6 C7 H7 119.7 . . ?
O4 C8 O3 122.8(2) . . ?
O4 C8 C9 119.4(2) . . ?
O3 C8 C9 117.8(2) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C25 C24 C23 120.6(2) . . ?
C31 C30 C29 120.4(2) . . ?
C35 C30 C29 120.9(2) . . ?
C35 C30 C31 118.6(2) . . ?
O11 C29 C30 120.0(2) . . ?
O12 C29 O11 118.8(2) . . ?
O12 C29 C30 121.2(2) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.7(2) . . ?
C13 C14 H14 119.6 . . ?
C7 C6 H6 120.3 . . ?
C7 C6 C5 119.5(2) . . ?
C5 C6 H6 120.3 . . ?
O1 C1 C2 120.0(2) . . ?
O2 C1 O1 119.9(2) . . ?
O2 C1 C2 120.1(2) . . ?
C17 C16 C15 121.1(2) . . ?
C17 C16 C21 118.1(3) . . ?
C21 C16 C15 120.6(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.7(2) . . ?
O18 C12 C11 117.0(2) . . ?
O18 C12 C13 122.6(2) . . ?
C13 C12 C11 120.3(2) . . ?
O13 C36 C37 121.4(2) . . ?
O14 C36 O13 119.0(2) . . ?
O14 C36 C37 119.6(2) . . ?
C24 C23 C22 121.0(2) . . ?
C24 C23 C28 118.6(2) . . ?
C28 C23 C22 120.3(2) . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.1(3) . . ?
C35 C34 H34 120.0 . . ?
O20 C26 C25 122.7(2) . . ?
O20 C26 C27 117.5(2) . . ?
C25 C26 C27 119.8(2) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C40 C39 C38 120.2(3) . . ?
C30 C31 H31 119.4 . . ?
C32 C31 C30 121.3(3) . . ?
C32 C31 H31 119.4 . . ?
C38 C37 C36 120.6(2) . . ?
C42 C37 C36 121.3(2) . . ?
C42 C37 C38 118.1(2) . . ?
C39 C38 C37 121.0(3) . . ?
C39 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
O21 C33 C34 123.2(3) . . ?
O21 C33 C32 116.5(2) . . ?
C34 C33 C32 120.3(2) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C5 C4 C3 119.7(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.0(2) . . ?
C11 C10 H10 119.5 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 H3 120.0 . . ?
C23 C28 H28 119.6 . . ?
C27 C28 C23 120.8(2) . . ?
C27 C28 H28 119.6 . . ?
C14 C13 H13 120.2 . . ?
C12 C13 C14 119.6(2) . . ?
C12 C13 H13 120.2 . . ?
C30 C35 H35 119.8 . . ?
C34 C35 C30 120.5(2) . . ?
C34 C35 H35 119.8 . . ?
C16 C17 H17A 119.7 . . ?
C18 C17 C16 120.7(3) . . ?
C18 C17 H17A 119.7 . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C19 C20 C21 119.6(3) . . ?
C31 C32 C33 119.1(3) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.1(2) . . ?
C26 C25 H25 119.9 . . ?
O17 C5 C6 122.6(2) . . ?
O17 C5 C4 116.5(2) . . ?
C4 C5 C6 120.9(2) . . ?
C17 C18 H18A 119.7 . . ?
C17 C18 C19 120.7(3) . . ?
C19 C18 H18A 119.7 . . ?
O22 C40 C39 123.3(3) . . ?
O22 C40 C41 117.0(3) . . ?
C39 C40 C41 119.6(3) . . ?
C16 C21 H21A 119.5 . . ?
C20 C21 C16 121.0(3) . . ?
C20 C21 H21A 119.5 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.1(3) . . ?
C28 C27 H27 120.0 . . ?
O19 C19 C20 117.8(3) . . ?
O19 C19 C18 122.3(3) . . ?
C20 C19 C18 119.9(3) . . ?
C37 C42 H42 119.5 . . ?
C41 C42 C37 121.0(3) . . ?
C41 C42 H42 119.5 . . ?
C40 C41 H41 119.9 . . ?
C42 C41 C40 120.1(3) . . ?
C42 C41 H41 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pr1 O1 C1 O2 -8.1(2) . . . . ?
Pr1 O1 C1 C2 171.04(19) . . . . ?
Pr1 O2 C1 O1 8.7(2) . . . . ?
Pr1 O2 C1 C2 -170.45(18) . . . . ?
Pr1 O6 C15 O5 -24.8(2) . . . . ?
Pr1 O6 C15 C16 149.6(2) . . . . ?
Pr1 O9 C22 O10 109.3(3) . . . . ?
Pr1 O9 C22 C23 -74.2(3) . . . . ?
Pr1 O3 C8 O4 14.1(4) . . . . ?
Pr1 O3 C8 C9 -165.71(15) . . . . ?
Pr1 O5 C15 O6 27.4(2) . . . . ?
Pr1 O5 C15 C16 -146.95(19) . . . . ?
Pr2 O6 C15 O5 123.5(4) . . . . ?
Pr2 O6 C15 C16 -62.1(5) . . . . ?
Pr2 O10 C22 O9 18.2(3) . . . . ?
Pr2 O10 C22 C23 -158.37(19) . . . . ?
Pr2 O9 C22 O10 -16.7(2) . . . . ?
Pr2 O9 C22 C23 159.8(2) . . . . ?
Pr2 O11 C29 O12 7.8(2) . . . . ?
Pr2 O11 C29 C30 -173.2(2) . . . . ?
Pr2 O12 C29 O11 -7.7(2) . . . . ?
Pr2 O12 C29 C30 173.3(2) . . . . ?
Pr2 O13 C36 O14 -8.0(3) . . . . ?
Pr2 O13 C36 C37 170.3(2) . . . . ?
Pr2 O14 C36 O13 8.1(3) . . . . ?
Pr2 O14 C36 C37 -170.3(2) . . . . ?
O6 C15 C16 C17 -15.2(4) . . . . ?
O6 C15 C16 C21 169.9(2) . . . . ?
O10 C22 C23 C24 162.3(3) . . . . ?
O10 C22 C23 C28 -15.0(4) . . . . ?
O9 C22 C23 C24 -14.1(4) . . . . ?
O9 C22 C23 C28 168.5(3) . . . . ?
O18 C12 C13 C14 177.3(3) . . . . ?
O13 C36 C37 C38 169.8(3) . . . . ?
O13 C36 C37 C42 -11.6(4) . . . . ?
O14 C36 C37 C38 -11.9(4) . . . . ?
O14 C36 C37 C42 166.8(3) . . . . ?
O20 C26 C25 C24 -178.3(3) . . . . ?
O20 C26 C27 C28 179.9(3) . . . . ?
O5 C15 C16 C17 159.1(2) . . . . ?
O5 C15 C16 C21 -15.9(4) . . . . ?
O22 C40 C41 C42 -179.2(3) . . . . ?
O21 C33 C32 C31 178.2(3) . . . . ?
C9 C14 C13 C12 0.0(4) . . . . ?
C2 C7 C6 C5 0.0(4) . . . . ?
C22 C23 C28 C27 178.0(3) . . . . ?
C15 C16 C17 C18 -174.3(2) . . . . ?
C15 C16 C21 C20 175.2(3) . . . . ?
C7 C2 C1 O1 -179.7(2) . . . . ?
C7 C2 C1 O2 -0.5(4) . . . . ?
C7 C2 C3 C4 0.4(4) . . . . ?
C7 C6 C5 O17 -178.3(2) . . . . ?
C7 C6 C5 C4 0.3(4) . . . . ?
C8 C9 C14 C13 -176.7(2) . . . . ?
C8 C9 C10 C11 177.0(2) . . . . ?
C24 C23 C28 C27 0.6(4) . . . . ?
C30 C31 C32 C33 0.3(5) . . . . ?
C29 C30 C31 C32 -178.1(3) . . . . ?
C29 C30 C35 C34 177.8(3) . . . . ?
C14 C9 C8 O4 173.0(2) . . . . ?
C14 C9 C8 O3 -7.1(3) . . . . ?
C14 C9 C10 C11 -0.8(4) . . . . ?
C1 C2 C7 C6 180.0(2) . . . . ?
C1 C2 C3 C4 -180.0(2) . . . . ?
C16 C17 C18 C19 -0.8(4) . . . . ?
C11 C12 C13 C14 -1.4(4) . . . . ?
C12 C11 C10 C9 -0.6(4) . . . . ?
C36 C37 C38 C39 178.5(3) . . . . ?
C36 C37 C42 C41 -179.0(3) . . . . ?
C23 C24 C25 C26 -2.1(5) . . . . ?
C23 C28 C27 C26 -1.1(5) . . . . ?
C34 C33 C32 C31 -1.8(5) . . . . ?
C39 C40 C41 C42 0.2(5) . . . . ?
C31 C30 C29 O11 -0.3(4) . . . . ?
C31 C30 C29 O12 178.7(3) . . . . ?
C31 C30 C35 C34 -1.9(4) . . . . ?
C37 C42 C41 C40 0.3(5) . . . . ?
C38 C39 C40 O22 178.6(3) . . . . ?
C38 C39 C40 C41 -0.8(5) . . . . ?
C38 C37 C42 C41 -0.4(5) . . . . ?
C33 C34 C35 C30 0.5(5) . . . . ?
C10 C9 C8 O4 -4.7(3) . . . . ?
C10 C9 C8 O3 175.1(2) . . . . ?
C10 C9 C14 C13 1.1(4) . . . . ?
C10 C11 C12 O18 -177.1(2) . . . . ?
C10 C11 C12 C13 1.7(4) . . . . ?
C3 C2 C7 C6 -0.4(4) . . . . ?
C3 C2 C1 O1 0.7(4) . . . . ?
C3 C2 C1 O2 179.9(2) . . . . ?
C3 C4 C5 O17 178.4(2) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C35 C30 C29 O11 -179.9(3) . . . . ?
C35 C30 C29 O12 -0.9(4) . . . . ?
C35 C30 C31 C32 1.5(5) . . . . ?
C35 C34 C33 O21 -178.5(3) . . . . ?
C35 C34 C33 C32 1.4(5) . . . . ?
C17 C16 C21 C20 0.1(4) . . . . ?
C17 C18 C19 O19 179.8(3) . . . . ?
C17 C18 C19 C20 -0.2(4) . . . . ?
C25 C24 C23 C22 -176.5(3) . . . . ?
C25 C24 C23 C28 0.9(4) . . . . ?
C25 C26 C27 C28 -0.1(5) . . . . ?
C5 C4 C3 C2 -0.1(4) . . . . ?
C40 C39 C38 C37 0.8(5) . . . . ?
C21 C16 C17 C18 0.8(4) . . . . ?
C21 C20 C19 O19 -178.9(3) . . . . ?
C21 C20 C19 C18 1.2(4) . . . . ?
C27 C26 C25 C24 1.7(5) . . . . ?
C19 C20 C21 C16 -1.1(5) . . . . ?
C42 C37 C38 C39 -0.2(5) . . . . ?

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

data_p21c
_database_code_depnum_ccdc_archive 'CCDC 2269123'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H38 Dy2 O22, 2(H2 O)'
_chemical_formula_sum            'C42 H42 Dy2 O24'
_chemical_formula_weight         1255.75
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.4033(3)
_cell_length_b                   14.8810(5)
_cell_length_c                   15.5628(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.9720(10)
_cell_angle_gamma                90
_cell_volume                     2316.29(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.52
_shelx_estimated_absorpt_T_max   0.494
_shelx_estimated_absorpt_T_min   0.243
_exptl_absorpt_coefficient_mu    3.289
_exptl_absorpt_correction_T_max  0.518
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.930
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4869
_reflns_number_total             5313
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.286
_refine_diff_density_min         -2.725
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.0543(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5313
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      1.119
_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)+(0.0453P)²+0.8293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0821
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H11A_$1-H12A_$2
 2.2 with sigma of 0.02
2.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
2.c Tetrahedral OH refined with riding coordinates:
 O9(H9)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.46228(2) 0.14824(2) 0.42099(2) 0.01900(9) Uani 1 1 d . . . . .
O3 O 0.5584(2) 0.28001(14) 0.50982(14) 0.0297(5) Uani 1 1 d . . . . .
O6 O 0.6385(2) -0.00805(13) 0.60078(14) 0.0275(4) Uani 1 1 d . . . . .
O4 O 0.5403(2) 0.28025(14) 0.36709(14) 0.0314(5) Uani 1 1 d . . . . .
O1 O 0.27973(19) 0.17908(15) 0.29049(14) 0.0260(4) Uani 1 1 d . . . . .
O5 O 0.6629(2) 0.08466(15) 0.49455(15) 0.0313(5) Uani 1 1 d . . . . .
O7 O 0.5561(2) 0.09928(17) 0.30439(16) 0.0379(5) Uani 1 1 d . . . . .
H7A H 0.604216 0.051100 0.303912 0.057 Uiso 1 1 d R U . . .
H7B H 0.549204 0.124835 0.252718 0.057 Uiso 1 1 d R U . . .
O8 O 0.4335(2) 0.11415(16) 0.56102(15) 0.0347(5) Uani 1 1 d . . . . .
H8A H 0.444872 0.161445 0.594262 0.052 Uiso 1 1 d R U . . .
H8B H 0.495635 0.078126 0.589222 0.052 Uiso 1 1 d R U . . .
O2 O 0.2575(2) 0.21947(15) 0.42071(14) 0.0306(5) Uani 1 1 d . . . . .
O12 O 0.3811(3) 0.3046(2) 0.1959(2) 0.0421(6) Uani 1 1 d . . . . .
O10 O 0.7754(3) 0.67129(18) 0.4499(2) 0.0437(7) Uani 1 1 d . . . . .
O9 O -0.3484(2) 0.2246(2) 0.18939(16) 0.0477(7) Uani 1 1 d . . . . .
H9 H -0.369282 0.209061 0.136811 0.072 Uiso 1 1 calc R U . . .
C8 C 0.5749(3) 0.3205(2) 0.44192(19) 0.0240(6) Uani 1 1 d . . . . .
C9 C 0.6327(3) 0.41143(19) 0.4478(2) 0.0250(6) Uani 1 1 d . . . . .
C2 C 0.0617(3) 0.2216(2) 0.2960(2) 0.0252(6) Uani 1 1 d . . . . .
C10 C 0.6583(4) 0.4495(2) 0.3728(2) 0.0366(7) Uani 1 1 d . . . . .
H10A H 0.642777 0.416134 0.320408 0.044 Uiso 1 1 calc R U . . .
C16 C 0.8570(3) 0.04201(19) 0.60552(19) 0.0241(6) Uani 1 1 d . . . . .
C14 C 0.6582(3) 0.4622(2) 0.5259(2) 0.0303(6) Uani 1 1 d . . . . .
H14 H 0.642485 0.437366 0.576940 0.036 Uiso 1 1 calc R U . . .
C1 C 0.2060(3) 0.20770(19) 0.3369(2) 0.0232(6) Uani 1 1 d . . . . .
C13 C 0.7065(3) 0.5487(2) 0.5287(2) 0.0313(7) Uani 1 1 d . . . . .
H13 H 0.723270 0.581772 0.581341 0.038 Uiso 1 1 calc R U . . .
C21 C 0.9115(3) 0.0047(2) 0.6895(2) 0.0350(7) Uani 1 1 d . . . . .
H21 H 0.855556 -0.021117 0.720036 0.042 Uiso 1 1 calc R U . . .
C15 C 0.7114(3) 0.03898(18) 0.56384(19) 0.0236(6) Uani 1 1 d . . . . .
C7 C 0.0083(3) 0.2143(2) 0.2043(2) 0.0290(6) Uani 1 1 d . . . . .
H7 H 0.064741 0.207269 0.167637 0.035 Uiso 1 1 calc R U . . .
C12 C 0.7299(3) 0.5863(2) 0.4529(2) 0.0302(6) Uani 1 1 d . . . . .
C17 C 0.9423(3) 0.0810(2) 0.5613(2) 0.0324(7) Uani 1 1 d . . . . .
H17 H 0.907132 0.106754 0.505322 0.039 Uiso 1 1 calc R U . . .
C19 C 1.1308(3) 0.0440(2) 0.6826(3) 0.0357(7) Uani 1 1 d . . . . .
C18 C 1.0788(3) 0.0818(2) 0.5998(3) 0.0379(8) Uani 1 1 d . . . . .
H18 H 1.135266 0.107885 0.569763 0.045 Uiso 1 1 calc R U . . .
C11 C 0.7064(4) 0.5361(2) 0.3746(2) 0.0396(8) Uani 1 1 d . . . . .
H11 H 0.723068 0.560858 0.323855 0.048 Uiso 1 1 calc R U . . .
C3 C -0.0236(3) 0.2333(3) 0.3503(2) 0.0364(7) Uani 1 1 d . . . . .
H3 H 0.011773 0.239431 0.411775 0.044 Uiso 1 1 calc R U . . .
C6 C -0.1286(3) 0.2175(2) 0.1670(2) 0.0328(7) Uani 1 1 d . . . . .
H6 H -0.163974 0.213484 0.105381 0.039 Uiso 1 1 calc R U . . .
C5 C -0.2127(3) 0.2265(2) 0.2213(2) 0.0341(7) Uani 1 1 d . . . . .
C20 C 1.0480(3) 0.0057(3) 0.7282(3) 0.0436(9) Uani 1 1 d . . . . .
H20 H 1.083832 -0.019198 0.784476 0.052 Uiso 1 1 calc R U . . .
C4 C -0.1605(3) 0.2360(3) 0.3132(2) 0.0431(9) Uani 1 1 d . . . . .
H4 H -0.217271 0.244056 0.349424 0.052 Uiso 1 1 calc R U . . .
H12A H 0.431(5) 0.299(3) 0.249(4) 0.078(18) Uiso 1 1 d . . . . .
H12B H 0.337(5) 0.260(3) 0.190(3) 0.047(13) Uiso 1 1 d . . . . .
H10 H 0.755(5) 0.692(3) 0.486(3) 0.048(14) Uiso 1 1 d . . . . .
O11 O 1.2663(2) 0.04094(19) 0.7232(2) 0.0535(7) Uani 1 1 d . . . . .
H11A H 1.302532 0.084369 0.707231 0.080 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
Dy1 O3 2.449(2) . ?
Dy1 O6 2.317(2) 3_656 ?
Dy1 O4 2.366(2) . ?
Dy1 O1 2.412(2) . ?
Dy1 O5 2.291(2) . ?
Dy1 O7 2.398(2) . ?
Dy1 O8 2.336(2) . ?
Dy1 O2 2.378(2) . ?
O3 C8 1.268(4) . ?
O6 C15 1.279(3) . ?
O4 C8 1.270(4) . ?
O1 C1 1.263(3) . ?
O5 C15 1.257(4) . ?
O7 H7A 0.8756 . ?
O7 H7B 0.8745 . ?
O8 H8A 0.8621 . ?
O8 H8B 0.8611 . ?
O2 C1 1.279(4) . ?
O12 H12A 0.85(6) . ?
O12 H12B 0.80(5) . ?
O10 C12 1.356(4) . ?
O10 H10 0.72(5) . ?
O9 H9 0.8200 . ?
O9 C5 1.362(4) . ?
C8 C9 1.474(4) . ?
C9 C10 1.388(4) . ?
C9 C14 1.394(4) . ?
C2 C1 1.475(4) . ?
C2 C7 1.387(4) . ?
C2 C3 1.394(4) . ?
C10 H10A 0.9300 . ?
C10 C11 1.380(5) . ?
C16 C21 1.389(4) . ?
C16 C15 1.475(4) . ?
C16 C17 1.390(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.377(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.387(5) . ?
C21 H21 0.9300 . ?
C21 C20 1.381(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.382(4) . ?
C12 C11 1.391(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.381(4) . ?
C19 C18 1.374(5) . ?
C19 C20 1.380(5) . ?
C19 O11 1.378(4) . ?
C18 H18 0.9300 . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.382(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.380(4) . ?
C5 C4 1.390(5) . ?
C20 H20 0.9300 . ?
C4 H4 0.9300 . ?
O11 H11A 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Dy1 O3 154.36(7) 3_656 . ?
O6 Dy1 O4 151.79(7) 3_656 . ?
O6 Dy1 O1 80.13(7) 3_656 . ?
O6 Dy1 O7 82.98(8) 3_656 . ?
O6 Dy1 O8 76.82(8) 3_656 . ?
O6 Dy1 O2 91.84(8) 3_656 . ?
O4 Dy1 O3 53.73(7) . . ?
O4 Dy1 O1 79.11(8) . . ?
O4 Dy1 O7 74.52(8) . . ?
O4 Dy1 O2 91.38(8) . . ?
O1 Dy1 O3 115.32(7) . . ?
O5 Dy1 O3 82.77(8) . . ?
O5 Dy1 O6 90.83(8) . 3_656 ?
O5 Dy1 O4 99.53(8) . . ?
O5 Dy1 O1 153.80(8) . . ?
O5 Dy1 O7 75.40(8) . . ?
O5 Dy1 O8 77.12(8) . . ?
O5 Dy1 O2 151.35(8) . . ?
O7 Dy1 O3 118.84(8) . . ?
O7 Dy1 O1 79.09(7) . . ?
O8 Dy1 O3 77.55(8) . . ?
O8 Dy1 O4 130.98(8) . . ?
O8 Dy1 O1 123.62(8) . . ?
O8 Dy1 O7 145.42(9) . . ?
O8 Dy1 O2 75.75(8) . . ?
O2 Dy1 O3 82.57(7) . . ?
O2 Dy1 O1 54.30(7) . . ?
O2 Dy1 O7 133.22(8) . . ?
C8 O3 Dy1 92.15(17) . . ?
C15 O6 Dy1 136.65(19) . 3_656 ?
C8 O4 Dy1 95.98(17) . . ?
C1 O1 Dy1 92.54(17) . . ?
C15 O5 Dy1 138.36(19) . . ?
Dy1 O7 H7A 127.4 . . ?
Dy1 O7 H7B 128.0 . . ?
H7A O7 H7B 104.5 . . ?
Dy1 O8 H8A 110.6 . . ?
Dy1 O8 H8B 109.9 . . ?
H8A O8 H8B 104.1 . . ?
C1 O2 Dy1 93.70(16) . . ?
H12A O12 H12B 102(5) . . ?
C12 O10 H10 102(4) . . ?
C5 O9 H9 109.5 . . ?
O3 C8 O4 118.1(3) . . ?
O3 C8 C9 122.0(3) . . ?
O4 C8 C9 119.8(3) . . ?
C10 C9 C8 119.5(3) . . ?
C10 C9 C14 118.5(3) . . ?
C14 C9 C8 121.9(3) . . ?
C7 C2 C1 120.3(3) . . ?
C7 C2 C3 119.5(3) . . ?
C3 C2 C1 119.9(3) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10A 119.5 . . ?
C21 C16 C15 120.4(3) . . ?
C21 C16 C17 118.8(3) . . ?
C17 C16 C15 120.9(3) . . ?
C9 C14 H14 119.5 . . ?
C13 C14 C9 120.9(3) . . ?
C13 C14 H14 119.5 . . ?
O1 C1 O2 118.6(2) . . ?
O1 C1 C2 120.5(3) . . ?
O2 C1 C2 120.8(3) . . ?
C14 C13 H13 120.1 . . ?
C14 C13 C12 119.9(3) . . ?
C12 C13 H13 120.1 . . ?
C16 C21 H21 119.7 . . ?
C20 C21 C16 120.7(3) . . ?
C20 C21 H21 119.7 . . ?
O6 C15 C16 118.9(3) . . ?
O5 C15 O6 122.3(3) . . ?
O5 C15 C16 118.8(3) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 C2 120.2(3) . . ?
C6 C7 H7 119.9 . . ?
O10 C12 C13 123.4(3) . . ?
O10 C12 C11 116.7(3) . . ?
C13 C12 C11 119.9(3) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 H17 119.7 . . ?
C18 C19 C20 120.7(3) . . ?
C18 C19 O11 122.2(3) . . ?
O11 C19 C20 117.1(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 H18 120.1 . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3 119.9 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 C7 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
O9 C5 C6 122.9(3) . . ?
O9 C5 C4 116.7(3) . . ?
C6 C5 C4 120.4(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 H20 120.2 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C19 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O3 C8 O4 -0.6(3) . . . . ?
Dy1 O3 C8 C9 179.6(2) . . . . ?
Dy1 O6 C15 O5 81.5(4) 3_656 . . . ?
Dy1 O6 C15 C16 -100.4(3) 3_656 . . . ?
Dy1 O4 C8 O3 0.7(3) . . . . ?
Dy1 O4 C8 C9 -179.5(2) . . . . ?
Dy1 O1 C1 O2 9.0(3) . . . . ?
Dy1 O1 C1 C2 -167.1(2) . . . . ?
Dy1 O5 C15 O6 22.2(5) . . . . ?
Dy1 O5 C15 C16 -155.8(2) . . . . ?
Dy1 O2 C1 O1 -9.2(3) . . . . ?
Dy1 O2 C1 C2 166.9(2) . . . . ?
O3 C8 C9 C10 174.8(3) . . . . ?
O3 C8 C9 C14 -7.5(4) . . . . ?
O4 C8 C9 C10 -4.9(4) . . . . ?
O4 C8 C9 C14 172.7(3) . . . . ?
O10 C12 C11 C10 -179.1(4) . . . . ?
O9 C5 C4 C3 176.4(4) . . . . ?
C8 C9 C10 C11 176.9(3) . . . . ?
C8 C9 C14 C13 -176.9(3) . . . . ?
C9 C10 C11 C12 0.1(6) . . . . ?
C9 C14 C13 C12 0.2(5) . . . . ?
C2 C7 C6 C5 -1.0(5) . . . . ?
C2 C3 C4 C5 0.3(6) . . . . ?
C10 C9 C14 C13 0.7(5) . . . . ?
C16 C21 C20 C19 -0.2(6) . . . . ?
C16 C17 C18 C19 -0.2(5) . . . . ?
C14 C9 C10 C11 -0.8(5) . . . . ?
C14 C13 C12 O10 179.0(3) . . . . ?
C14 C13 C12 C11 -0.9(5) . . . . ?
C1 C2 C7 C6 172.8(3) . . . . ?
C1 C2 C3 C4 -172.5(4) . . . . ?
C13 C12 C11 C10 0.8(5) . . . . ?
C21 C16 C15 O6 -8.7(4) . . . . ?
C21 C16 C15 O5 169.4(3) . . . . ?
C21 C16 C17 C18 0.7(5) . . . . ?
C15 C16 C21 C20 178.7(3) . . . . ?
C15 C16 C17 C18 -178.5(3) . . . . ?
C7 C2 C1 O1 -8.1(4) . . . . ?
C7 C2 C1 O2 175.8(3) . . . . ?
C7 C2 C3 C4 1.2(5) . . . . ?
C7 C6 C5 O9 -175.9(3) . . . . ?
C7 C6 C5 C4 2.5(6) . . . . ?
C17 C16 C21 C20 -0.5(5) . . . . ?
C17 C16 C15 O6 170.4(3) . . . . ?
C17 C16 C15 O5 -11.4(4) . . . . ?
C18 C19 C20 C21 0.7(6) . . . . ?
C3 C2 C1 O1 165.5(3) . . . . ?
C3 C2 C1 O2 -10.5(4) . . . . ?
C3 C2 C7 C6 -0.9(5) . . . . ?
C6 C5 C4 C3 -2.1(6) . . . . ?
C20 C19 C18 C17 -0.5(5) . . . . ?
O11 C19 C18 C17 178.4(3) . . . . ?
O11 C19 C20 C21 -178.3(3) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT972_p21c                
;
PROBLEM: Check Calcd Resid. Dens.  0.89Ang From Dy1            -2.83 eA-3  
RESPONSE:These are the ripples (residual density) features that are
very closed to the heavy atom and are typically more pronounced for heavier
atoms, for example element Dy in this case.
;
####################################################################### 
# 
# 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_jo2147_d2
_database_code_depnum_ccdc_archive 'CCDC 2269121'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 O22 Tb2, 2(H2 O)'
_chemical_formula_sum            'C42 H42 O24 Tb2'
_chemical_formula_weight         1248.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Tb C H O'
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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.39280(10)
_cell_length_b                   14.9032(2)
_cell_length_c                   15.4634(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.8680(10)
_cell_angle_gamma                90
_cell_volume                     2303.80(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15987
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      77.0950
_cell_measurement_theta_min      4.1990
_shelx_estimated_absorpt_T_max   0.573
_shelx_estimated_absorpt_T_min   0.356
_exptl_absorpt_coefficient_mu    15.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystallized at room temperature by slow evaporation.'
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24578
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.350
_diffrn_reflns_theta_min         4.199
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     33.00 120.00   0.50    0.05    --   47.70  58.00 100.00  174
  2  ω    116.00 142.00   0.50    0.10    --  107.75 125.00   0.00   52
  3  ω    144.00 172.00   0.50    0.10    --  107.75 125.00   0.00   56
  4  ω     93.00 178.00   0.50    0.10    --  107.75  58.00 100.00  170
  5  ω   -101.00 -14.00   0.50    0.10    --  -86.25  58.00 100.00  174
  6  ω    -63.00  25.00   0.50    0.05    --  -47.70  58.00 100.00  176
  7  ω   -119.00 -32.00   0.50    0.05    --  -47.70 -58.00 -39.00  174
  8  ω   -159.00 -71.00   0.50    0.10    --  -86.25 -58.00 -39.00  176
  9  ω   -119.00 -73.00   0.50    0.05    --  -47.70-125.00  60.00   92
 10  ω   -119.00 -73.00   0.50    0.05    --  -47.70-125.00  90.00   92
 11  ω     43.00  94.00   0.50    0.10    --  107.75 -94.00 -30.00  102
 12  ω     59.00  85.00   0.50    0.10    --  107.75 -94.00-150.00   52
 13  ω     78.00 106.00   0.50    0.10    --  107.75 -94.00  90.00   56
 14  ω     48.00  73.00   0.50    0.10    --  107.75 -94.00  90.00   50
 15  ω     37.00  65.00   0.50    0.10    --  107.75 -77.00  30.00   56
 16  ω     43.00  72.00   0.50    0.10    --  107.75 -45.00  90.00   58
 17  ω    106.00 131.00   0.50    0.10    --  107.75 -77.00  30.00   50
 18  ω     35.00 102.00   0.50    0.10    --  107.75 -58.00 -39.00  134
 19  ω     39.00  64.00   0.50    0.10    --  107.75 -45.00-150.00   50
 20  ω     36.00  76.00   0.50    0.10    --  107.75 -45.00-180.00   80
 21  ω     34.00  66.00   0.50    0.10    --  107.75 -30.00-150.00   64
 22  ω     34.00  66.00   0.50    0.10    --  107.75 -30.00 -60.00   64
 23  ω    -24.00  63.00   0.50    0.05    --   47.70 -58.00 -39.00  174
 24  ω     33.00  66.00   0.50    0.10    --  107.75 -30.00 120.00   66
 25  ω     34.00  64.00   0.50    0.10    --  107.75 -30.00 150.00   60
 26  ω     39.00  76.00   0.50    0.10    --  107.75 -45.00 120.00   74
 27  ω     33.00  66.00   0.50    0.10    --  107.75 -30.00   0.00   66
 28  ω     33.00  58.00   0.50    0.10    --  107.75 -30.00  30.00   50
 29  ω     33.00  66.00   0.50    0.10    --  107.75 -30.00 -30.00   66
 30  ω     33.00  66.00   0.50    0.10    --  107.75 -30.00-180.00   66
 31  ω     87.00 119.00   0.50    0.10    --  107.75 -15.00 -30.00   64
 32  ω     38.00  77.00   0.50    0.10    --  107.75 -15.00 -30.00   78
 33  ω     34.00  60.00   0.50    0.10    --  107.75 -15.00  90.00   52
 34  ω     73.00 120.00   0.50    0.10    --  107.75 -15.00  90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0984804000
_diffrn_orient_matrix_UB_12      -0.0609888000
_diffrn_orient_matrix_UB_13      0.0671454000
_diffrn_orient_matrix_UB_21      0.0535885000
_diffrn_orient_matrix_UB_22      -0.0360888000
_diffrn_orient_matrix_UB_23      -0.0768184000
_diffrn_orient_matrix_UB_31      0.1057495000
_diffrn_orient_matrix_UB_32      0.0752814000
_diffrn_orient_matrix_UB_33      0.0175990000
_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                4552
_reflns_number_total             4808
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4808
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0256
_refine_ls_restrained_S_all      1.050
_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)+(0.0323P)²+2.5692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0649
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Free rotating group:
 O12(H12A,H12B)
1.b Rotating group:
 O11(H11A,H11B), O10(H10A,H10B)
1.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C13(H13), C17(H17), C21(H21), C7(H7A), C20(H20), C11(H11),
  C6(H6), C3(H3), C4(H4), C18(H18)
1.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O7(H7), O9(H9)
;
_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
Tb01 Tb 0.46287(2) 0.14762(2) 0.41905(2) 0.00879(6) Uani 1 1 d . . . . .
O1 O 0.27858(17) 0.18022(12) 0.28785(12) 0.0124(3) Uani 1 1 d . . . . .
O3 O 0.53950(18) 0.28107(12) 0.36567(12) 0.0141(4) Uani 1 1 d . . . . .
O6 O 0.63909(17) -0.00700(12) 0.60348(12) 0.0120(3) Uani 1 1 d . . . . .
O11 O 0.43263(18) 0.11230(13) 0.55962(12) 0.0155(4) Uani 1 1 d . . . . .
H11A H 0.439064 0.159977 0.591516 0.023 Uiso 1 1 d R U . . .
H11B H 0.497415 0.079208 0.589087 0.023 Uiso 1 1 d R U . . .
O4 O 0.55801(18) 0.27994(12) 0.50975(12) 0.0140(4) Uani 1 1 d . . . . .
O5 O 0.66476(17) 0.08462(13) 0.49544(12) 0.0143(4) Uani 1 1 d . . . . .
O8 O 0.7729(2) 0.67270(13) 0.44891(13) 0.0182(4) Uani 1 1 d . . . . .
H8 H 0.768858 0.699777 0.494249 0.027 Uiso 1 1 calc R U . . .
O7 O -0.35127(18) 0.22427(14) 0.18895(12) 0.0187(4) Uani 1 1 d . . . . .
H7 H -0.372220 0.219923 0.134004 0.028 Uiso 1 1 calc R U . . .
O12 O 0.38043(19) 0.19339(13) 0.69601(13) 0.0172(4) Uani 1 1 d G . . . .
H12A H 0.436830 0.196525 0.747407 0.026 Uiso 1 1 d G U . . .
H12B H 0.330719 0.239127 0.693740 0.026 Uiso 1 1 d G U . . .
O2 O 0.25665(17) 0.21956(13) 0.41965(12) 0.0142(4) Uani 1 1 d . . . . .
O9 O 1.27003(18) 0.03819(13) 0.72407(14) 0.0202(4) Uani 1 1 d . . . . .
H9 H 1.305119 0.084226 0.712373 0.030 Uiso 1 1 calc R U . . .
O10 O 0.55841(18) 0.10096(13) 0.30146(12) 0.0153(4) Uani 1 1 d . . . . .
H10A H 0.629320 0.070650 0.323954 0.023 Uiso 1 1 d R U . . .
H10B H 0.585507 0.146909 0.278563 0.023 Uiso 1 1 d R U . . .
C8 C 0.5743(2) 0.32142(17) 0.44147(17) 0.0115(5) Uani 1 1 d . . . . .
C9 C 0.6312(2) 0.41257(17) 0.44730(17) 0.0123(5) Uani 1 1 d . . . . .
C2 C 0.0600(2) 0.22216(17) 0.29505(17) 0.0123(5) Uani 1 1 d . . . . .
C1 C 0.2044(2) 0.20838(16) 0.33511(17) 0.0110(5) Uani 1 1 d . . . . .
C10 C 0.6569(3) 0.45096(18) 0.37116(17) 0.0155(5) Uani 1 1 d . . . . .
H10 H 0.641491 0.417686 0.318432 0.019 Uiso 1 1 calc R U . . .
C14 C 0.6572(3) 0.46284(17) 0.52619(17) 0.0135(5) Uani 1 1 d . . . . .
H14 H 0.641826 0.437737 0.577514 0.016 Uiso 1 1 calc R U . . .
C5 C -0.2152(2) 0.22668(18) 0.22098(18) 0.0147(5) Uani 1 1 d . . . . .
C16 C 0.8596(2) 0.04065(16) 0.60741(17) 0.0115(5) Uani 1 1 d . . . . .
C12 C 0.7282(3) 0.58725(17) 0.45191(18) 0.0143(5) Uani 1 1 d . . . . .
C13 C 0.7057(3) 0.54966(18) 0.52915(17) 0.0148(5) Uani 1 1 d . . . . .
H13 H 0.723063 0.582639 0.582152 0.018 Uiso 1 1 calc R U . . .
C17 C 0.9140(3) 0.00262(18) 0.69170(18) 0.0155(5) Uani 1 1 d . . . . .
H17 H 0.858007 -0.023498 0.722352 0.019 Uiso 1 1 calc R U . . .
C21 C 0.9442(3) 0.08055(18) 0.56205(17) 0.0149(5) Uani 1 1 d . . . . .
H21 H 0.908371 0.107202 0.506271 0.018 Uiso 1 1 calc R U . . .
C7 C 0.0058(3) 0.21563(18) 0.20214(17) 0.0142(5) Uani 1 1 d . . . . .
H7A H 0.062170 0.209305 0.165079 0.017 Uiso 1 1 calc R U . . .
C19 C 1.1342(2) 0.04168(17) 0.68435(18) 0.0148(5) Uani 1 1 d . . . . .
C15 C 0.7124(2) 0.03942(17) 0.56579(16) 0.0123(5) Uani 1 1 d . . . . .
C20 C 1.0815(3) 0.08042(19) 0.60013(18) 0.0169(5) Uani 1 1 d . . . . .
H20 H 1.138029 0.106044 0.569615 0.020 Uiso 1 1 calc R U . . .
C11 C 0.7048(3) 0.53742(18) 0.37321(18) 0.0172(5) Uani 1 1 d . . . . .
H11 H 0.721278 0.562285 0.322128 0.021 Uiso 1 1 calc R U . . .
C6 C -0.1310(3) 0.21849(19) 0.16487(17) 0.0158(5) Uani 1 1 d . . . . .
H6 H -0.166676 0.214987 0.102880 0.019 Uiso 1 1 calc R U . . .
C3 C -0.0251(3) 0.23379(19) 0.35014(18) 0.0164(5) Uani 1 1 d . . . . .
H3 H 0.010751 0.239968 0.411903 0.020 Uiso 1 1 calc R U . . .
C4 C -0.1623(3) 0.2362(2) 0.31364(18) 0.0189(6) Uani 1 1 d . . . . .
H4 H -0.218689 0.244108 0.350511 0.023 Uiso 1 1 calc R U . . .
C18 C 1.0506(3) 0.00347(19) 0.73007(19) 0.0184(5) Uani 1 1 d . . . . .
H18 H 1.086391 -0.021625 0.786614 0.022 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
Tb01 O1 2.4281(17) . ?
Tb01 O3 2.3729(18) . ?
Tb01 O6 2.3311(17) 3_656 ?
Tb01 O11 2.3397(17) . ?
Tb01 O4 2.4647(18) . ?
Tb01 O5 2.3074(17) . ?
Tb01 O2 2.3987(17) . ?
Tb01 O10 2.4006(17) . ?
O1 C1 1.270(3) . ?
O3 C8 1.278(3) . ?
O6 C15 1.282(3) . ?
O11 H11A 0.8571 . ?
O11 H11B 0.8581 . ?
O4 C8 1.274(3) . ?
O5 C15 1.260(3) . ?
O8 H8 0.8200 . ?
O8 C12 1.361(3) . ?
O7 H7 0.8200 . ?
O7 C5 1.365(3) . ?
O12 H12A 0.8501 . ?
O12 H12B 0.8502 . ?
O2 C1 1.282(3) . ?
O9 H9 0.8200 . ?
O9 C19 1.378(3) . ?
O10 H10A 0.8532 . ?
O10 H10B 0.8534 . ?
C8 C9 1.475(4) . ?
C9 C10 1.399(4) . ?
C9 C14 1.393(4) . ?
C2 C1 1.474(3) . ?
C2 C7 1.396(4) . ?
C2 C3 1.396(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.378(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.385(4) . ?
C5 C6 1.397(4) . ?
C5 C4 1.395(4) . ?
C16 C17 1.392(4) . ?
C16 C21 1.399(3) . ?
C16 C15 1.488(3) . ?
C12 C13 1.396(4) . ?
C12 C11 1.389(4) . ?
C13 H13 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.381(4) . ?
C21 H21 0.9300 . ?
C21 C20 1.387(4) . ?
C7 H7A 0.9300 . ?
C7 C6 1.380(4) . ?
C19 C20 1.393(4) . ?
C19 C18 1.384(4) . ?
C20 H20 0.9300 . ?
C11 H11 0.9300 . ?
C6 H6 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.383(4) . ?
C4 H4 0.9300 . ?
C18 H18 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
O1 Tb01 O4 114.67(6) . . ?
O3 Tb01 O1 78.74(6) . . ?
O3 Tb01 O4 53.61(6) . . ?
O3 Tb01 O2 90.69(6) . . ?
O3 Tb01 O10 74.44(6) . . ?
O6 Tb01 O1 80.36(6) 3_656 . ?
O6 Tb01 O3 152.08(6) 3_656 . ?
O6 Tb01 O11 76.44(6) 3_656 . ?
O6 Tb01 O4 154.10(6) 3_656 . ?
O6 Tb01 O2 91.85(6) 3_656 . ?
O6 Tb01 O10 83.78(6) 3_656 . ?
O11 Tb01 O1 123.07(6) . . ?
O11 Tb01 O3 130.91(6) . . ?
O11 Tb01 O4 77.66(6) . . ?
O11 Tb01 O2 75.51(6) . . ?
O11 Tb01 O10 145.78(7) . . ?
O5 Tb01 O1 155.27(6) . . ?
O5 Tb01 O3 100.05(6) . . ?
O5 Tb01 O6 91.33(6) . 3_656 ?
O5 Tb01 O11 76.53(6) . . ?
O5 Tb01 O4 82.36(6) . . ?
O5 Tb01 O2 150.26(6) . . ?
O5 Tb01 O10 76.31(6) . . ?
O2 Tb01 O1 54.01(6) . . ?
O2 Tb01 O4 81.96(6) . . ?
O2 Tb01 O10 133.43(6) . . ?
O10 Tb01 O1 79.64(6) . . ?
O10 Tb01 O4 118.56(6) . . ?
C1 O1 Tb01 92.83(15) . . ?
C8 O3 Tb01 96.49(15) . . ?
C15 O6 Tb01 136.05(16) . 3_656 ?
Tb01 O11 H11A 109.8 . . ?
Tb01 O11 H11B 109.7 . . ?
H11A O11 H11B 104.1 . . ?
C8 O4 Tb01 92.30(15) . . ?
C15 O5 Tb01 138.37(16) . . ?
C12 O8 H8 109.5 . . ?
C5 O7 H7 109.5 . . ?
H12A O12 H12B 104.5 . . ?
C1 O2 Tb01 93.87(14) . . ?
C19 O9 H9 109.5 . . ?
Tb01 O10 H10A 109.6 . . ?
Tb01 O10 H10B 109.5 . . ?
H10A O10 H10B 104.3 . . ?
O3 C8 C9 119.8(2) . . ?
O4 C8 O3 117.6(2) . . ?
O4 C8 C9 122.6(2) . . ?
C10 C9 C8 119.4(2) . . ?
C14 C9 C8 121.8(2) . . ?
C14 C9 C10 118.7(2) . . ?
C7 C2 C1 120.1(2) . . ?
C7 C2 C3 119.5(2) . . ?
C3 C2 C1 120.2(2) . . ?
O1 C1 O2 118.4(2) . . ?
O1 C1 C2 120.9(2) . . ?
O2 C1 C2 120.6(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.5 . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.9(2) . . ?
C13 C14 H14 119.6 . . ?
O7 C5 C6 122.4(2) . . ?
O7 C5 C4 117.0(2) . . ?
C4 C5 C6 120.6(2) . . ?
C17 C16 C21 119.5(2) . . ?
C17 C16 C15 120.4(2) . . ?
C21 C16 C15 120.1(2) . . ?
O8 C12 C13 122.9(2) . . ?
O8 C12 C11 116.8(2) . . ?
C11 C12 C13 120.3(2) . . ?
C14 C13 C12 119.4(2) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.3(2) . . ?
C18 C17 H17 119.8 . . ?
C16 C21 H21 119.9 . . ?
C20 C21 C16 120.1(2) . . ?
C20 C21 H21 119.9 . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 C2 120.5(2) . . ?
C6 C7 H7A 119.8 . . ?
O9 C19 C20 121.7(2) . . ?
O9 C19 C18 117.8(2) . . ?
C18 C19 C20 120.5(2) . . ?
O6 C15 C16 118.6(2) . . ?
O5 C15 O6 122.6(2) . . ?
O5 C15 C16 118.8(2) . . ?
C21 C20 C19 119.6(2) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C10 C11 C12 119.7(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H6 120.3 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 H3 119.7 . . ?
C5 C4 H4 120.3 . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4 120.3 . . ?
C17 C18 C19 120.0(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?

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
Tb01 O1 C1 O2 9.4(2) . . . . ?
Tb01 O1 C1 C2 -166.6(2) . . . . ?
Tb01 O3 C8 O4 0.5(2) . . . . ?
Tb01 O3 C8 C9 -179.68(19) . . . . ?
Tb01 O6 C15 O5 81.0(3) 3_656 . . . ?
Tb01 O6 C15 C16 -99.7(3) 3_656 . . . ?
Tb01 O4 C8 O3 -0.5(2) . . . . ?
Tb01 O4 C8 C9 179.7(2) . . . . ?
Tb01 O5 C15 O6 21.5(4) . . . . ?
Tb01 O5 C15 C16 -157.87(18) . . . . ?
Tb01 O2 C1 O1 -9.5(2) . . . . ?
Tb01 O2 C1 C2 166.5(2) . . . . ?
O3 C8 C9 C10 -5.3(4) . . . . ?
O3 C8 C9 C14 173.0(2) . . . . ?
O4 C8 C9 C10 174.5(2) . . . . ?
O4 C8 C9 C14 -7.1(4) . . . . ?
O8 C12 C13 C14 178.6(2) . . . . ?
O8 C12 C11 C10 -178.8(2) . . . . ?
O7 C5 C6 C7 -175.8(3) . . . . ?
O7 C5 C4 C3 176.3(3) . . . . ?
O9 C19 C20 C21 178.6(2) . . . . ?
O9 C19 C18 C17 -177.9(2) . . . . ?
C8 C9 C10 C11 177.2(2) . . . . ?
C8 C9 C14 C13 -177.4(2) . . . . ?
C9 C10 C11 C12 0.1(4) . . . . ?
C9 C14 C13 C12 0.2(4) . . . . ?
C2 C7 C6 C5 -0.9(4) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C1 C2 C7 C6 172.8(2) . . . . ?
C1 C2 C3 C4 -172.4(3) . . . . ?
C10 C9 C14 C13 1.0(4) . . . . ?
C14 C9 C10 C11 -1.2(4) . . . . ?
C16 C17 C18 C19 -0.5(4) . . . . ?
C16 C21 C20 C19 -1.1(4) . . . . ?
C13 C12 C11 C10 1.1(4) . . . . ?
C17 C16 C21 C20 1.4(4) . . . . ?
C17 C16 C15 O6 -8.8(4) . . . . ?
C17 C16 C15 O5 170.6(2) . . . . ?
C21 C16 C17 C18 -0.6(4) . . . . ?
C21 C16 C15 O6 171.5(2) . . . . ?
C21 C16 C15 O5 -9.1(4) . . . . ?
C7 C2 C1 O1 -8.4(4) . . . . ?
C7 C2 C1 O2 175.7(2) . . . . ?
C7 C2 C3 C4 1.9(4) . . . . ?
C15 C16 C17 C18 179.7(2) . . . . ?
C15 C16 C21 C20 -178.9(2) . . . . ?
C20 C19 C18 C17 0.8(4) . . . . ?
C11 C12 C13 C14 -1.3(4) . . . . ?
C6 C5 C4 C3 -2.6(4) . . . . ?
C3 C2 C1 O1 165.9(2) . . . . ?
C3 C2 C1 O2 -10.0(4) . . . . ?
C3 C2 C7 C6 -1.5(4) . . . . ?
C4 C5 C6 C7 3.0(4) . . . . ?
C18 C19 C20 C21 0.0(4) . . . . ?

_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.790
####################################################################### 
# 
# 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_pcj026
_database_code_depnum_ccdc_archive 'CCDC 2269122'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 O22 Tb2, 4(H2 O)'
_chemical_formula_sum            'C42 H46 O26 Tb2'
_chemical_formula_weight         1284.63
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.0067(7)
_cell_length_b                   11.0069(9)
_cell_length_c                   12.9695(10)
_cell_angle_alpha                91.8950(10)
_cell_angle_beta                 108.879(2)
_cell_angle_gamma                93.5260(10)
_cell_volume                     1212.36(17)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7513
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.982
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.621108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.1012 before and 0.0304 after correction.
The Ratio of minimum to maximum transmission is 0.6211.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 4 sets of ω scans each set at different φ and/or
 2θ angles and each scan (15 s exposure) covering -0.300° degrees in ω.
 The crystal to detector distance was 5.625 cm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8275
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_min         2.561
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5629
_reflns_number_total             5757
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.28A (Bruker, 2002)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.28A (Bruker, 2002)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.842
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0230(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5757
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0278
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0368P)²+1.0722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0723
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Riding coordinates:
 O11(H11A,H11B)
1.b Free rotating group:
 O12(H12A,H12B), O13(H13A,H13B)
1.c Rotating group:
 O10(H10A,H10B)
1.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6A), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21)
1.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6), O9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.75798(2) 0.05652(2) 0.68146(2) 0.02297(7) Uani 1 1 d . . . . .
O1 O 0.9476(2) 0.22952(19) 0.73046(19) 0.0348(4) Uani 1 1 d . . . . .
O2 O 0.7650(3) 0.2323(2) 0.80616(19) 0.0368(5) Uani 1 1 d . . . . .
O3 O 1.0289(3) 0.7906(2) 0.8731(2) 0.0440(6) Uani 1 1 d . . . . .
H3 H 0.950155 0.825928 0.875985 0.066 Uiso 1 1 calc R U . . .
O4 O 0.8092(2) -0.0510(2) 0.84848(18) 0.0330(4) Uani 1 1 d . . . . .
O5 O 0.5671(2) -0.0060(2) 0.77016(17) 0.0329(4) Uani 1 1 d . . . . .
O6 O 0.5045(3) -0.2864(2) 1.1772(2) 0.0420(5) Uani 1 1 d . . . . .
H6 H 0.413190 -0.272282 1.175498 0.063 Uiso 1 1 calc R U . . .
O7 O 0.5401(3) 0.14151(19) 0.57408(17) 0.0335(4) Uani 1 1 d . . . . .
O8 O 0.3428(3) 0.12209(18) 0.41862(18) 0.0329(4) Uani 1 1 d . . . . .
O9 O 0.6983(3) 0.6113(2) 0.3514(2) 0.0514(7) Uani 1 1 d . . . . .
H9 H 0.634860 0.632789 0.292888 0.077 Uiso 1 1 calc R U . . .
O10 O 0.8332(3) 0.0985(2) 0.5280(2) 0.0436(6) Uani 1 1 d . . . . .
H10A H 0.791478 0.042902 0.476508 0.065 Uiso 1 1 d R U . . .
H10B H 0.933035 0.092667 0.543303 0.065 Uiso 1 1 d R U . . .
O11 O 0.9972(3) -0.0430(3) 0.7120(2) 0.0475(6) Uani 1 1 d . . . . .
H11A H 1.025042 -0.115319 0.720589 0.071 Uiso 1 1 d R U . . .
H11B H 1.081202 0.000781 0.709639 0.071 Uiso 1 1 d R U . . .
C1 C 0.8773(3) 0.2877(3) 0.7835(2) 0.0271(5) Uani 1 1 d . . . . .
C2 C 0.9203(3) 0.4192(3) 0.8126(2) 0.0287(5) Uani 1 1 d . . . . .
C3 C 0.8473(4) 0.4845(3) 0.8727(3) 0.0347(6) Uani 1 1 d . . . . .
H3A H 0.773269 0.443404 0.900102 0.042 Uiso 1 1 calc R U . . .
C4 C 0.8807(4) 0.6088(3) 0.8933(3) 0.0382(7) Uani 1 1 d . . . . .
H4 H 0.828825 0.653322 0.933773 0.046 Uiso 1 1 calc R U . . .
C5 C 0.9902(4) 0.6680(3) 0.8547(3) 0.0350(6) Uani 1 1 d . . . . .
C6 C 1.0670(4) 0.6035(3) 0.7969(3) 0.0458(8) Uani 1 1 d . . . . .
H6A H 1.144016 0.644075 0.771858 0.055 Uiso 1 1 calc R U . . .
C7 C 1.0310(4) 0.4798(3) 0.7757(3) 0.0416(7) Uani 1 1 d . . . . .
H7 H 1.082956 0.435486 0.735223 0.050 Uiso 1 1 calc R U . . .
C8 C 0.6676(3) -0.0542(2) 0.8464(2) 0.0263(5) Uani 1 1 d . . . . .
C9 C 0.6216(3) -0.1138(2) 0.9325(2) 0.0267(5) Uani 1 1 d . . . . .
C10 C 0.7363(3) -0.1466(3) 1.0261(2) 0.0298(5) Uani 1 1 d . . . . .
H10 H 0.844222 -0.128780 1.034233 0.036 Uiso 1 1 calc R U . . .
C11 C 0.6967(4) -0.2043(3) 1.1070(2) 0.0313(6) Uani 1 1 d . . . . .
H11 H 0.776310 -0.226850 1.170240 0.038 Uiso 1 1 calc R U . . .
C12 C 0.5391(3) -0.2292(3) 1.0951(2) 0.0286(5) Uani 1 1 d . . . . .
C13 C 0.4229(3) -0.1971(3) 1.0035(3) 0.0342(6) Uani 1 1 d . . . . .
H13 H 0.315151 -0.214383 0.996090 0.041 Uiso 1 1 calc R U . . .
C14 C 0.4643(3) -0.1398(3) 0.9229(2) 0.0330(6) Uani 1 1 d . . . . .
H14 H 0.384260 -0.117727 0.859713 0.040 Uiso 1 1 calc R U . . .
C15 C 0.4676(3) 0.1775(2) 0.4820(2) 0.0249(5) Uani 1 1 d . . . . .
C16 C 0.5270(3) 0.2917(2) 0.4458(2) 0.0282(5) Uani 1 1 d . . . . .
C17 C 0.6498(5) 0.3647(3) 0.5169(3) 0.0492(10) Uani 1 1 d . . . . .
H17 H 0.696054 0.341395 0.589568 0.059 Uiso 1 1 calc R U . . .
C18 C 0.7069(5) 0.4709(3) 0.4848(3) 0.0545(11) Uani 1 1 d . . . . .
H18 H 0.791844 0.520056 0.534656 0.065 Uiso 1 1 calc R U . . .
C19 C 0.6397(4) 0.5048(3) 0.3800(3) 0.0367(6) Uani 1 1 d . . . . .
C20 C 0.5176(5) 0.4333(3) 0.3075(3) 0.0458(8) Uani 1 1 d . . . . .
H20 H 0.472664 0.456436 0.234685 0.055 Uiso 1 1 calc R U . . .
C21 C 0.4605(4) 0.3277(3) 0.3409(3) 0.0417(8) Uani 1 1 d . . . . .
H21 H 0.374638 0.279240 0.291109 0.050 Uiso 1 1 calc R U . . .
O12 O 0.2602(3) 0.0317(3) 0.6658(2) 0.0468(6) Uani 1 1 d G . . . .
H12A H 0.271741 0.105996 0.652027 0.070 Uiso 1 1 d G U . . .
H12B H 0.353439 0.011796 0.696345 0.070 Uiso 1 1 d G U . . .
O13 O 1.0975(6) 0.2134(4) 0.5114(4) 0.0976(16) Uani 1 1 d G . . . .
H13A H 1.121570 0.202800 0.453682 0.146 Uiso 1 1 d G U . . .
H13B H 1.154918 0.276149 0.544432 0.146 Uiso 1 1 d G U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.401(2) . ?
Tb1 O2 2.464(2) . ?
Tb1 O4 2.428(2) . ?
Tb1 O5 2.437(2) . ?
Tb1 O7 2.282(2) . ?
Tb1 O8 2.285(2) 2_656 ?
Tb1 O10 2.351(2) . ?
Tb1 O11 2.401(2) . ?
O1 C1 1.259(4) . ?
O2 C1 1.269(4) . ?
O3 H3 0.8400 . ?
O3 C5 1.367(4) . ?
O4 C8 1.266(3) . ?
O5 C8 1.262(3) . ?
O6 H6 0.8400 . ?
O6 C12 1.364(3) . ?
O7 C15 1.252(3) . ?
O8 C15 1.264(3) . ?
O9 H9 0.8400 . ?
O9 C19 1.369(4) . ?
O10 H10A 0.8627 . ?
O10 H10B 0.8628 . ?
O11 H11A 0.8491 . ?
O11 H11B 0.8811 . ?
C1 C2 1.479(4) . ?
C2 C3 1.382(4) . ?
C2 C7 1.385(4) . ?
C3 H3A 0.9500 . ?
C3 C4 1.381(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(5) . ?
C5 C6 1.380(5) . ?
C6 H6A 0.9500 . ?
C6 C7 1.377(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.470(4) . ?
C9 C10 1.391(4) . ?
C9 C14 1.392(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.375(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.387(4) . ?
C12 C13 1.378(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.378(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.485(4) . ?
C16 C17 1.379(4) . ?
C16 C21 1.380(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.379(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.371(5) . ?
C19 C20 1.374(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.381(5) . ?
C21 H21 0.9500 . ?
O12 H12A 0.8503 . ?
O12 H12B 0.8505 . ?
O13 H13A 0.8505 . ?
O13 H13B 0.8492 . ?

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 Tb1 O2 53.01(7) . . ?
O1 Tb1 O4 104.12(8) . . ?
O1 Tb1 O5 127.74(8) . . ?
O1 Tb1 O11 79.56(9) . . ?
O4 Tb1 O2 82.00(8) . . ?
O4 Tb1 O5 53.31(7) . . ?
O5 Tb1 O2 75.86(8) . . ?
O7 Tb1 O1 101.39(8) . . ?
O7 Tb1 O2 82.26(8) . . ?
O7 Tb1 O4 132.41(7) . . ?
O7 Tb1 O5 79.31(7) . . ?
O7 Tb1 O8 86.92(8) . 2_656 ?
O7 Tb1 O10 79.08(9) . . ?
O7 Tb1 O11 153.42(9) . . ?
O8 Tb1 O1 150.57(8) 2_656 . ?
O8 Tb1 O2 156.23(8) 2_656 . ?
O8 Tb1 O4 89.94(8) 2_656 . ?
O8 Tb1 O5 81.39(8) 2_656 . ?
O8 Tb1 O10 81.89(8) 2_656 . ?
O8 Tb1 O11 80.74(9) 2_656 . ?
O10 Tb1 O1 72.26(8) . . ?
O10 Tb1 O2 116.39(8) . . ?
O10 Tb1 O4 147.19(9) . . ?
O10 Tb1 O5 153.25(8) . . ?
O10 Tb1 O11 75.94(10) . . ?
O11 Tb1 O2 117.10(9) . . ?
O11 Tb1 O4 71.38(8) . . ?
O11 Tb1 O5 121.41(8) . . ?
C1 O1 Tb1 95.22(17) . . ?
C1 O2 Tb1 91.97(17) . . ?
C5 O3 H3 109.5 . . ?
C8 O4 Tb1 93.81(16) . . ?
C8 O5 Tb1 93.47(17) . . ?
C12 O6 H6 109.5 . . ?
C15 O7 Tb1 147.2(2) . . ?
C15 O8 Tb1 143.56(19) . 2_656 ?
C19 O9 H9 109.5 . . ?
Tb1 O10 H10A 110.2 . . ?
Tb1 O10 H10B 109.9 . . ?
H10A O10 H10B 103.8 . . ?
Tb1 O11 H11A 136.7 . . ?
Tb1 O11 H11B 118.0 . . ?
H11A O11 H11B 105.1 . . ?
O1 C1 O2 118.5(3) . . ?
O1 C1 C2 120.0(3) . . ?
O2 C1 C2 121.4(3) . . ?
C3 C2 C1 121.2(3) . . ?
C3 C2 C7 118.9(3) . . ?
C7 C2 C1 119.9(3) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3A 119.6 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
O3 C5 C4 122.1(3) . . ?
O3 C5 C6 117.4(3) . . ?
C6 C5 C4 120.5(3) . . ?
C5 C6 H6A 120.3 . . ?
C7 C6 C5 119.4(3) . . ?
C7 C6 H6A 120.3 . . ?
C2 C7 H7 119.5 . . ?
C6 C7 C2 121.0(3) . . ?
C6 C7 H7 119.5 . . ?
O4 C8 C9 119.9(2) . . ?
O5 C8 O4 119.4(2) . . ?
O5 C8 C9 120.7(2) . . ?
C10 C9 C8 120.1(2) . . ?
C10 C9 C14 118.3(3) . . ?
C14 C9 C8 121.6(2) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 C9 121.3(3) . . ?
C11 C10 H10 119.3 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.1(3) . . ?
C12 C11 H11 120.5 . . ?
O6 C12 C11 117.4(3) . . ?
O6 C12 C13 121.8(3) . . ?
C13 C12 C11 120.8(3) . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.4(3) . . ?
C14 C13 H13 120.3 . . ?
C9 C14 H14 119.5 . . ?
C13 C14 C9 121.0(3) . . ?
C13 C14 H14 119.5 . . ?
O7 C15 O8 122.7(2) . . ?
O7 C15 C16 119.3(2) . . ?
O8 C15 C16 118.0(2) . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 C21 118.5(3) . . ?
C21 C16 C15 121.0(3) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 H18 120.4 . . ?
C19 C18 C17 119.3(3) . . ?
C19 C18 H18 120.4 . . ?
O9 C19 C18 117.6(3) . . ?
O9 C19 C20 121.9(3) . . ?
C18 C19 C20 120.4(3) . . ?
C19 C20 H20 120.1 . . ?
C19 C20 C21 119.8(3) . . ?
C21 C20 H20 120.1 . . ?
C16 C21 C20 120.6(3) . . ?
C16 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
H12A O12 H12B 104.4 . . ?
H13A O13 H13B 104.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O4 0.84 1.88 2.666(3) 155.9 1_565 yes
O6 H6 O2 0.84 1.78 2.608(3) 170.7 2_657 yes
O9 H9 O6 0.84 1.87 2.698(3) 167.8 1_564 yes
O10 H10A O12 0.86 1.90 2.706(4) 155.9 2_656 yes
O10 H10B O13 0.86 2.08 2.700(4) 128.3 . yes
O11 H11A O3 0.85 2.25 2.780(4) 120.3 1_545 yes
O11 H11B O12 0.88 1.89 2.712(3) 154.3 1_655 yes
O12 H12A O13 0.85 2.39 2.981(7) 127.2 1_455 yes
O12 H12B O5 0.85 1.88 2.721(3) 171.0 . yes
O13 H13B O9 0.85 1.91 2.737(5) 165.0 2_766 yes

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 11.7(3) . . . . ?
Tb1 O1 C1 C2 -164.9(2) . . . . ?
Tb1 O2 C1 O1 -11.4(3) . . . . ?
Tb1 O2 C1 C2 165.2(2) . . . . ?
Tb1 O4 C8 O5 -0.8(3) . . . . ?
Tb1 O4 C8 C9 179.2(2) . . . . ?
Tb1 O5 C8 O4 0.8(3) . . . . ?
Tb1 O5 C8 C9 -179.2(2) . . . . ?
Tb1 O7 C15 O8 109.1(4) . . . . ?
Tb1 O7 C15 C16 -72.6(4) . . . . ?
Tb1 O8 C15 O7 -64.2(4) 2_656 . . . ?
Tb1 O8 C15 C16 117.6(3) 2_656 . . . ?
O1 C1 C2 C3 -178.6(3) . . . . ?
O1 C1 C2 C7 4.0(4) . . . . ?
O2 C1 C2 C3 4.8(4) . . . . ?
O2 C1 C2 C7 -172.6(3) . . . . ?
O3 C5 C6 C7 -179.6(3) . . . . ?
O4 C8 C9 C10 11.8(4) . . . . ?
O4 C8 C9 C14 -167.7(3) . . . . ?
O5 C8 C9 C10 -168.2(3) . . . . ?
O5 C8 C9 C14 12.3(4) . . . . ?
O6 C12 C13 C14 -179.8(3) . . . . ?
O7 C15 C16 C17 -7.2(5) . . . . ?
O7 C15 C16 C21 173.1(3) . . . . ?
O8 C15 C16 C17 171.2(3) . . . . ?
O8 C15 C16 C21 -8.6(4) . . . . ?
O9 C19 C20 C21 -178.8(4) . . . . ?
C1 C2 C3 C4 -175.7(3) . . . . ?
C1 C2 C7 C6 176.6(3) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C3 C2 C7 C6 -0.9(5) . . . . ?
C3 C4 C5 O3 -179.6(3) . . . . ?
C3 C4 C5 C6 -0.7(5) . . . . ?
C4 C5 C6 C7 1.5(6) . . . . ?
C5 C6 C7 C2 -0.7(6) . . . . ?
C7 C2 C3 C4 1.7(5) . . . . ?
C8 C9 C10 C11 -178.9(3) . . . . ?
C8 C9 C14 C13 179.2(3) . . . . ?
C9 C10 C11 C12 -0.5(5) . . . . ?
C10 C9 C14 C13 -0.3(5) . . . . ?
C10 C11 C12 O6 -179.9(3) . . . . ?
C10 C11 C12 C13 0.1(5) . . . . ?
C11 C12 C13 C14 0.1(5) . . . . ?
C12 C13 C14 C9 0.0(5) . . . . ?
C14 C9 C10 C11 0.6(4) . . . . ?
C15 C16 C17 C18 179.8(4) . . . . ?
C15 C16 C21 C20 -179.2(3) . . . . ?
C16 C17 C18 C19 0.2(7) . . . . ?
C17 C16 C21 C20 1.0(6) . . . . ?
C17 C18 C19 O9 179.3(4) . . . . ?
C17 C18 C19 C20 -0.5(7) . . . . ?
C18 C19 C20 C21 1.1(6) . . . . ?
C19 C20 C21 C16 -1.3(6) . . . . ?
C21 C16 C17 C18 -0.5(6) . . . . ?

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

data_pcj037
_database_code_depnum_ccdc_archive 'CCDC 2269126'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H42 O24 Y2, 10(H2 O)'
_chemical_formula_sum            'C42 H62 O34 Y2'
_chemical_formula_weight         1288.73
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.7986(9)
_cell_length_b                   11.4256(9)
_cell_length_c                   11.6045(9)
_cell_angle_alpha                90.629(2)
_cell_angle_beta                 100.564(2)
_cell_angle_gamma                105.4750(10)
_cell_volume                     1353.76(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4950
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.808
_shelx_estimated_absorpt_T_min   0.716
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.858918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.0489 before and 0.0150 after correction.
The Ratio of minimum to maximum transmission is 0.8589.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 4 sets of ω scans each set at different φ and/or
 2θ angles and each scan (15 s exposure) covering -0.300° degrees in ω.
 The crystal to detector distance was 5.625 cm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9360
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_min         1.789
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5693
_reflns_number_total             6426
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.28A (Bruker, 2002)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.28A (Bruker, 2002)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.063
_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)+(0.0562P)²+0.4317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0969
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H17B-O15_$1
 1.9 with sigma of 0.02
 H17A-O16_$1
 1.9 with sigma of 0.02
 Y1-H12A \\sim Y1-H12B
 with sigma of 0.02
2.a Free rotating group:
 O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,
 H16B), O17(H17A,H17B)
2.b Rotating group:
 O10(H10A,H10B), O11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6A), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6), O9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.47682(2) 0.60775(2) 0.68224(2) 0.02665(7) Uani 1 1 d D . . . .
O1 O 0.28047(16) 0.64724(14) 0.72050(15) 0.0346(4) Uani 1 1 d . . . . .
O2 O 0.31782(18) 0.47643(16) 0.78047(17) 0.0422(4) Uani 1 1 d . . . . .
O3 O -0.26036(18) 0.39649(17) 0.87028(19) 0.0468(5) Uani 1 1 d . . . . .
H3 H -0.273388 0.329145 0.897127 0.070 Uiso 1 1 calc R U . . .
O4 O 0.33801(16) 0.48828(15) 0.52496(15) 0.0372(4) Uani 1 1 d . . . . .
O5 O 0.34406(16) 0.33708(14) 0.40619(16) 0.0357(4) Uani 1 1 d . . . . .
O6 O -0.23542(17) 0.14365(16) 0.50010(18) 0.0422(4) Uani 1 1 d . . . . .
H6 H -0.256259 0.072379 0.474866 0.063 Uiso 1 1 calc R U . . .
O7 O 0.55403(17) 0.79282(15) 0.77911(18) 0.0436(4) Uani 1 1 d . . . . .
O8 O 0.55510(17) 0.98646(16) 0.78661(18) 0.0451(4) Uani 1 1 d . . . . .
O9 O 1.16319(19) 1.03604(17) 0.8337(2) 0.0532(5) Uani 1 1 d . . . . .
H9 H 1.190978 0.975773 0.838615 0.080 Uiso 1 1 calc R U . . .
O10 O 0.43336(18) 0.74128(16) 0.52732(17) 0.0418(4) Uani 1 1 d . . . . .
H10A H 0.371294 0.770242 0.538629 0.063 Uiso 1 1 d R U . . .
H10B H 0.499203 0.803339 0.532746 0.063 Uiso 1 1 d R U . . .
O11 O 0.54543(18) 0.42369(15) 0.67795(16) 0.0388(4) Uani 1 1 d . . . . .
H11A H 0.606860 0.426502 0.736452 0.058 Uiso 1 1 d R U . . .
H11B H 0.580160 0.420826 0.618282 0.058 Uiso 1 1 d R U . . .
O12 O 0.5959(2) 0.58379(17) 0.87040(16) 0.0470(4) Uani 1 1 d G . . . .
H12A H 0.597267 0.621809 0.934202 0.070 Uiso 1 1 d DG U . . .
H12B H 0.617742 0.520022 0.891921 0.070 Uiso 1 1 d DG U . . .
C1 C 0.2451(2) 0.5473(2) 0.7691(2) 0.0303(4) Uani 1 1 d . . . . .
C2 C 0.1170(2) 0.51353(19) 0.80699(19) 0.0288(4) Uani 1 1 d . . . . .
C3 C 0.0260(2) 0.5796(2) 0.7735(2) 0.0317(5) Uani 1 1 d . . . . .
H3A H 0.049968 0.650755 0.734956 0.038 Uiso 1 1 calc R U . . .
C4 C -0.0987(2) 0.5410(2) 0.7966(2) 0.0339(5) Uani 1 1 d . . . . .
H4 H -0.158400 0.585996 0.774434 0.041 Uiso 1 1 calc R U . . .
C5 C -0.1343(2) 0.4341(2) 0.8535(2) 0.0323(5) Uani 1 1 d . . . . .
C6 C -0.0433(2) 0.3697(2) 0.8916(2) 0.0346(5) Uani 1 1 d . . . . .
H6A H -0.066265 0.300554 0.933044 0.041 Uiso 1 1 calc R U . . .
C7 C 0.0810(2) 0.4091(2) 0.8676(2) 0.0338(5) Uani 1 1 d . . . . .
H7 H 0.141526 0.365411 0.892152 0.041 Uiso 1 1 calc R U . . .
C8 C 0.2866(2) 0.38527(19) 0.47095(19) 0.0274(4) Uani 1 1 d . . . . .
C9 C 0.1501(2) 0.31812(19) 0.48022(18) 0.0269(4) Uani 1 1 d . . . . .
C10 C 0.0735(2) 0.3767(2) 0.5312(2) 0.0303(4) Uani 1 1 d . . . . .
H10 H 0.108835 0.457001 0.560974 0.036 Uiso 1 1 calc R U . . .
C11 C -0.0547(2) 0.3167(2) 0.5381(2) 0.0336(5) Uani 1 1 d . . . . .
H11 H -0.104755 0.356307 0.572725 0.040 Uiso 1 1 calc R U . . .
C12 C -0.1076(2) 0.1971(2) 0.4929(2) 0.0310(4) Uani 1 1 d . . . . .
C13 C -0.0329(2) 0.1366(2) 0.4423(2) 0.0331(5) Uani 1 1 d . . . . .
H13 H -0.068564 0.056296 0.412550 0.040 Uiso 1 1 calc R U . . .
C14 C 0.0956(2) 0.1973(2) 0.4364(2) 0.0315(5) Uani 1 1 d . . . . .
H14 H 0.145967 0.157022 0.402974 0.038 Uiso 1 1 calc R U . . .
C15 C 0.6135(2) 0.9041(2) 0.7893(2) 0.0342(5) Uani 1 1 d . . . . .
C16 C 0.7594(2) 0.9390(2) 0.8059(2) 0.0323(5) Uani 1 1 d . . . . .
C17 C 0.8268(3) 1.0517(2) 0.7739(2) 0.0387(5) Uani 1 1 d . . . . .
H17 H 0.780953 1.107298 0.746308 0.046 Uiso 1 1 calc R U . . .
C18 C 0.9610(3) 1.0821(2) 0.7826(3) 0.0427(6) Uani 1 1 d . . . . .
H18 H 1.004641 1.156644 0.758680 0.051 Uiso 1 1 calc R U . . .
C19 C 1.0304(2) 1.0013(2) 0.8271(2) 0.0379(5) Uani 1 1 d . . . . .
C20 C 0.9653(3) 0.8895(2) 0.8622(2) 0.0403(6) Uani 1 1 d . . . . .
H20 H 1.012091 0.835913 0.893667 0.048 Uiso 1 1 calc R U . . .
C21 C 0.8306(3) 0.8583(2) 0.8501(2) 0.0378(5) Uani 1 1 d . . . . .
H21 H 0.786766 0.782581 0.871672 0.045 Uiso 1 1 calc R U . . .
O13 O 0.30248(19) 0.87562(17) 0.81931(19) 0.0452(4) Uani 1 1 d G . . . .
H13A H 0.279389 0.810829 0.774776 0.068 Uiso 1 1 d G U . . .
H13B H 0.378264 0.912156 0.807397 0.068 Uiso 1 1 d G U . . .
O14 O 0.3967(2) 0.0820(2) 0.5926(2) 0.0573(5) Uani 1 1 d G . . . .
H14A H 0.373436 0.137356 0.625336 0.086 Uiso 1 1 d G U . . .
H14B H 0.460823 0.071613 0.641918 0.086 Uiso 1 1 d G U . . .
O15 O 0.3078(3) 0.2252(2) 0.7309(3) 0.0734(7) Uani 1 1 d G . . . .
H15A H 0.253536 0.174414 0.763241 0.110 Uiso 1 1 d G U . . .
H15B H 0.281777 0.289226 0.729555 0.110 Uiso 1 1 d G U . . .
O16 O 0.6502(3) 0.18224(17) 0.9490(2) 0.0601(6) Uani 1 1 d G . . . .
H16A H 0.678270 0.161228 1.016723 0.090 Uiso 1 1 d G U . . .
H16B H 0.624656 0.116524 0.905852 0.090 Uiso 1 1 d G U . . .
O17 O 0.5255(3) 0.6704(3) 0.0532(3) 0.0902(9) Uani 1 1 d G . . . .
H17A H 0.481706 0.721497 0.034181 0.135 Uiso 1 1 d DG U . . .
H17B H 0.596617 0.705643 0.099673 0.135 Uiso 1 1 d DG 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
Y1 O1 2.3975(16) . ?
Y1 O2 2.4247(17) . ?
Y1 O4 2.3004(16) . ?
Y1 O5 2.2984(16) 2_666 ?
Y1 O7 2.2568(16) . ?
Y1 O10 2.4316(17) . ?
Y1 O11 2.4118(17) . ?
Y1 O12 2.3808(19) . ?
O1 C1 1.276(3) . ?
O2 C1 1.262(3) . ?
O3 H3 0.8200 . ?
O3 C5 1.364(3) . ?
O4 C8 1.262(3) . ?
O5 C8 1.264(3) . ?
O6 H6 0.8200 . ?
O6 C12 1.371(3) . ?
O7 C15 1.256(3) . ?
O8 C15 1.262(3) . ?
O9 H9 0.8200 . ?
O9 C19 1.369(3) . ?
O10 H10A 0.8518 . ?
O10 H10B 0.8519 . ?
O11 H11A 0.8514 . ?
O11 H11B 0.8500 . ?
O12 H12A 0.8501 . ?
O12 H12B 0.8502 . ?
C1 C2 1.482(3) . ?
C2 C3 1.396(3) . ?
C2 C7 1.394(3) . ?
C3 H3A 0.9300 . ?
C3 C4 1.378(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(3) . ?
C5 C6 1.391(3) . ?
C6 H6A 0.9300 . ?
C6 C7 1.379(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.494(3) . ?
C9 C10 1.395(3) . ?
C9 C14 1.397(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.389(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.388(3) . ?
C12 C13 1.391(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.390(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.493(3) . ?
C16 C17 1.392(3) . ?
C16 C21 1.395(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.381(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.384(4) . ?
C19 C20 1.389(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.383(4) . ?
C21 H21 0.9300 . ?
O13 H13A 0.8503 . ?
O13 H13B 0.8506 . ?
O14 H14A 0.8502 . ?
O14 H14B 0.8493 . ?
O15 H15A 0.8518 . ?
O15 H15B 0.8497 . ?
O16 H16A 0.8498 . ?
O16 H16B 0.8495 . ?
O17 H17A 0.8508 . ?
O17 H17B 0.8497 . ?

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 Y1 O2 54.05(6) . . ?
O1 Y1 O10 78.67(6) . . ?
O1 Y1 O11 132.28(6) . . ?
O2 Y1 O10 126.87(6) . . ?
O4 Y1 O1 83.88(6) . . ?
O4 Y1 O2 79.23(7) . . ?
O4 Y1 O10 72.37(6) . . ?
O4 Y1 O11 74.62(6) . . ?
O4 Y1 O12 138.83(6) . . ?
O5 Y1 O1 148.59(6) 2_666 . ?
O5 Y1 O2 156.88(6) 2_666 . ?
O5 Y1 O4 96.17(6) 2_666 . ?
O5 Y1 O10 71.55(6) 2_666 . ?
O5 Y1 O11 76.94(6) 2_666 . ?
O5 Y1 O12 95.78(7) 2_666 . ?
O7 Y1 O1 77.90(6) . . ?
O7 Y1 O2 109.74(7) . . ?
O7 Y1 O4 147.77(7) . . ?
O7 Y1 O5 86.30(6) . 2_666 ?
O7 Y1 O10 78.08(7) . . ?
O7 Y1 O11 136.58(7) . . ?
O7 Y1 O12 72.26(7) . . ?
O11 Y1 O2 80.01(6) . . ?
O11 Y1 O10 130.81(6) . . ?
O12 Y1 O1 104.78(7) . . ?
O12 Y1 O2 74.54(7) . . ?
O12 Y1 O10 148.48(7) . . ?
O12 Y1 O11 70.03(6) . . ?
C1 O1 Y1 93.71(13) . . ?
C1 O2 Y1 92.79(14) . . ?
C5 O3 H3 109.5 . . ?
C8 O4 Y1 150.15(16) . . ?
C8 O5 Y1 138.82(14) . 2_666 ?
C12 O6 H6 109.5 . . ?
C15 O7 Y1 153.86(18) . . ?
C19 O9 H9 109.5 . . ?
Y1 O10 H10A 109.5 . . ?
Y1 O10 H10B 109.4 . . ?
H10A O10 H10B 104.4 . . ?
Y1 O11 H11A 109.5 . . ?
Y1 O11 H11B 109.4 . . ?
H11A O11 H11B 104.5 . . ?
Y1 O12 H12A 125.7 . . ?
Y1 O12 H12B 125.7 . . ?
H12A O12 H12B 104.5 . . ?
O1 C1 C2 119.7(2) . . ?
O2 C1 O1 119.4(2) . . ?
O2 C1 C2 120.8(2) . . ?
C3 C2 C1 120.5(2) . . ?
C7 C2 C1 120.4(2) . . ?
C7 C2 C3 118.9(2) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 C2 121.0(2) . . ?
C4 C3 H3A 119.5 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.3(2) . . ?
C5 C4 H4 120.3 . . ?
O3 C5 C4 117.4(2) . . ?
O3 C5 C6 122.2(2) . . ?
C6 C5 C4 120.4(2) . . ?
C5 C6 H6A 120.2 . . ?
C7 C6 C5 119.7(2) . . ?
C7 C6 H6A 120.2 . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.7(2) . . ?
C6 C7 H7 119.7 . . ?
O4 C8 O5 123.0(2) . . ?
O4 C8 C9 119.03(19) . . ?
O5 C8 C9 117.92(19) . . ?
C10 C9 C8 120.05(19) . . ?
C10 C9 C14 118.8(2) . . ?
C14 C9 C8 121.15(19) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.5(2) . . ?
C12 C11 H11 120.3 . . ?
O6 C12 C11 116.7(2) . . ?
O6 C12 C13 122.6(2) . . ?
C11 C12 C13 120.6(2) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.4(2) . . ?
C14 C13 H13 120.3 . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.8(2) . . ?
C13 C14 H14 119.6 . . ?
O7 C15 O8 122.8(2) . . ?
O7 C15 C16 117.9(2) . . ?
O8 C15 C16 119.3(2) . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 C21 118.6(2) . . ?
C21 C16 C15 121.0(2) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.8(2) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 119.9(2) . . ?
C19 C18 H18 120.0 . . ?
O9 C19 C18 117.5(2) . . ?
O9 C19 C20 122.4(2) . . ?
C18 C19 C20 120.2(2) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.5(2) . . ?
C21 C20 H20 120.2 . . ?
C16 C21 H21 119.6 . . ?
C20 C21 C16 120.9(2) . . ?
C20 C21 H21 119.6 . . ?
H13A O13 H13B 104.4 . . ?
H14A O14 H14B 104.5 . . ?
H15A O15 H15B 104.4 . . ?
H16A O16 H16B 104.5 . . ?
H17A O17 H17B 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O16 0.82 1.82 2.621(3) 163.8 1_455 yes
O6 H6 O14 0.82 2.03 2.773(3) 150.1 2_556 yes
O9 H9 O13 0.82 1.91 2.684(3) 157.8 1_655 yes
O10 H10A O6 0.85 1.96 2.767(2) 156.6 2_566 yes
O10 H10B O14 0.85 2.22 2.898(3) 136.0 2_666 yes
O11 H11A O3 0.85 2.01 2.850(3) 168.5 1_655 yes
O11 H11B O4 0.85 2.17 2.933(2) 149.3 2_666 yes
O12 H12A O17 0.85 1.85 2.647(3) 155.4 1_556 yes
O12 H12B O3 0.85 2.21 2.960(3) 146.8 1_655 yes
O13 H13A O1 0.85 1.97 2.772(2) 156.9 . yes
O13 H13B O8 0.85 1.93 2.781(3) 175.9 . yes
O14 H14A O15 0.85 1.92 2.743(4) 162.9 . yes
O14 H14B O8 0.85 2.18 2.971(3) 155.5 1_545 yes
O15 H15A O9 0.85 1.90 2.733(3) 165.0 1_445 yes
O15 H15B O2 0.85 2.13 2.890(3) 149.5 . yes
O16 H16A O13 0.85 1.94 2.764(3) 163.3 2_667 yes
O16 H16B O8 0.85 1.91 2.754(3) 169.3 1_545 yes
O17 H17A O16 0.85 2.05 2.849(4) 155.9 2_666 yes
O17 H17B O15 0.85 2.08 2.842(4) 148.3 2_666 yes

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 1.7(2) . . . . ?
Y1 O1 C1 C2 -175.72(18) . . . . ?
Y1 O2 C1 O1 -1.7(2) . . . . ?
Y1 O2 C1 C2 175.71(18) . . . . ?
Y1 O4 C8 O5 -80.7(4) . . . . ?
Y1 O4 C8 C9 101.3(3) . . . . ?
Y1 O5 C8 O4 -14.3(4) 2_666 . . . ?
Y1 O5 C8 C9 163.72(16) 2_666 . . . ?
Y1 O7 C15 O8 107.3(4) . . . . ?
Y1 O7 C15 C16 -72.9(5) . . . . ?
O1 C1 C2 C3 10.3(3) . . . . ?
O1 C1 C2 C7 -175.4(2) . . . . ?
O2 C1 C2 C3 -167.1(2) . . . . ?
O2 C1 C2 C7 7.1(3) . . . . ?
O3 C5 C6 C7 177.1(2) . . . . ?
O4 C8 C9 C10 10.5(3) . . . . ?
O4 C8 C9 C14 -170.7(2) . . . . ?
O5 C8 C9 C10 -167.5(2) . . . . ?
O5 C8 C9 C14 11.2(3) . . . . ?
O6 C12 C13 C14 179.0(2) . . . . ?
O7 C15 C16 C17 155.4(2) . . . . ?
O7 C15 C16 C21 -22.6(3) . . . . ?
O8 C15 C16 C17 -24.8(3) . . . . ?
O8 C15 C16 C21 157.2(2) . . . . ?
O9 C19 C20 C21 -178.0(2) . . . . ?
C1 C2 C3 C4 172.5(2) . . . . ?
C1 C2 C7 C6 -172.7(2) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C3 C2 C7 C6 1.6(3) . . . . ?
C3 C4 C5 O3 -177.3(2) . . . . ?
C3 C4 C5 C6 3.0(4) . . . . ?
C4 C5 C6 C7 -3.2(4) . . . . ?
C5 C6 C7 C2 0.9(4) . . . . ?
C7 C2 C3 C4 -1.8(3) . . . . ?
C8 C9 C10 C11 178.5(2) . . . . ?
C8 C9 C14 C13 -178.1(2) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C10 C9 C14 C13 0.7(3) . . . . ?
C10 C11 C12 O6 -178.6(2) . . . . ?
C10 C11 C12 C13 0.8(4) . . . . ?
C11 C12 C13 C14 -0.4(4) . . . . ?
C12 C13 C14 C9 -0.3(4) . . . . ?
C14 C9 C10 C11 -0.3(3) . . . . ?
C15 C16 C17 C18 -176.3(2) . . . . ?
C15 C16 C21 C20 178.2(2) . . . . ?
C16 C17 C18 C19 -2.0(4) . . . . ?
C17 C16 C21 C20 0.1(4) . . . . ?
C17 C18 C19 O9 179.9(3) . . . . ?
C17 C18 C19 C20 0.5(4) . . . . ?
C18 C19 C20 C21 1.4(4) . . . . ?
C19 C20 C21 C16 -1.7(4) . . . . ?
C21 C16 C17 C18 1.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# 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_jo281_a1
_database_code_depnum_ccdc_archive 'CCDC 2269125'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 Ho2 O22, 2(H2 O)'
_chemical_formula_sum            'C42 H42 Ho2 O24'
_chemical_formula_weight         1260.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ho C H O'
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'
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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3692(3)
_cell_length_b                   14.8578(5)
_cell_length_c                   15.4168(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.8910(10)
_cell_angle_gamma                90
_cell_volume                     2284.40(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12995
_cell_measurement_temperature    123.00(13)
_cell_measurement_theta_max      77.1480
_cell_measurement_theta_min      4.2410
_shelx_estimated_absorpt_T_max   0.272
_shelx_estimated_absorpt_T_min   0.101
_exptl_absorpt_coefficient_mu    7.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24375
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.406
_diffrn_reflns_theta_min         4.212
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  -1.00   0.50    0.05    --  -47.64 110.00 -73.00  162
  2  ω     23.00  87.00   0.50    0.05    --   47.64-110.00-168.00  128
  3  ω    -82.00 -13.00   0.50    0.20    --  -86.25 110.00 -73.00  138
  4  ω   -159.00 -82.00   0.50    0.20    --  -86.25-110.00-168.00  154
  5  ω    103.00 178.00   0.50    0.20    --  107.75 110.00 -73.00  150
  6  ω     35.00 108.00   0.50    0.20    --  107.75-110.00-168.00  146
  7  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-120.00   94
  8  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00  90.00   94
  9  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00 -30.00   94
 10  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00   0.00   94
 11  ω    -25.00  61.00   0.50    0.05    --   47.64 -38.00-120.00  172
 12  ω     36.00  76.00   0.50    0.20    --  107.75 -45.00   0.00   80
 13  ω     35.00 127.00   0.50    0.20    --  107.75 -77.00-150.00  184
 14  ω     40.00  66.00   0.50    0.20    --  107.75 -30.00 -60.00   52
 15  ω     35.00 106.00   0.50    0.20    --  107.75 -94.00 -30.00  142
 16  ω     36.00  62.00   0.50    0.20    --  107.75 -30.00  60.00   52
 17  ω     39.00  65.00   0.50    0.20    --  107.75 -30.00-150.00   52
 18  ω     38.00  68.00   0.50    0.20    --  107.75 -94.00-150.00   60
 19  ω     75.00 104.00   0.50    0.20    --  107.75 -94.00-150.00   58
 20  ω     33.00  59.00   0.50    0.20    --  107.75 -30.00  30.00   52
 21  ω     38.00  63.00   0.50    0.20    --  107.75 -45.00  60.00   50
 22  ω     36.00 115.00   0.50    0.20    --  107.75 -77.00 -30.00  158
 23  ω     34.00  66.00   0.50    0.20    --  107.75 -30.00-120.00   64
 24  ω     44.00  76.00   0.50    0.20    --  107.75 -45.00  90.00   64
 25  ω     35.00  63.00   0.50    0.20    --  107.75 -30.00  90.00   56
 26  ω     36.00  71.00   0.50    0.20    --  107.75 -45.00-150.00   70
 27  ω     46.00 106.00   0.50    0.20    --  107.75 -94.00 120.00  120
 28  ω     38.00  63.00   0.50    0.20    --  107.75 -30.00-180.00   50
 29  ω     36.00  62.00   0.50    0.20    --  107.75-125.00-180.00   52
 30  ω     64.00  90.00   0.50    0.20    --  107.75-125.00-180.00   52
 31  ω     36.00  68.00   0.50    0.20    --  107.75 -45.00  30.00   64
 32  ω     42.00  84.00   0.50    0.20    --  107.75 -94.00-120.00   84
 33  ω     33.00  65.00   0.50    0.20    --  107.75 -30.00 -30.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0437087000
_diffrn_orient_matrix_UB_12      0.0518918000
_diffrn_orient_matrix_UB_13      -0.0898607000
_diffrn_orient_matrix_UB_21      -0.0119254000
_diffrn_orient_matrix_UB_22      0.0869542000
_diffrn_orient_matrix_UB_23      0.0517365000
_diffrn_orient_matrix_UB_31      0.1475504000
_diffrn_orient_matrix_UB_32      0.0223840000
_diffrn_orient_matrix_UB_33      0.0072684000
_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                4485
_reflns_number_total             4773
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.120
_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)+(0.0356P)²+2.0426P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0750
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
1.b Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
1.c Tetrahedral OH refined with riding coordinates:
 O9(H9)
1.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.46178(2) 0.14722(2) 0.41975(2) 0.01250(7) Uani 1 1 d . . . . .
O3 O 0.55641(15) 0.27830(11) 0.51049(11) 0.0171(3) Uani 1 1 d . . . . .
O6 O 0.63799(15) -0.00739(11) 0.60326(11) 0.0151(3) Uani 1 1 d . . . . .
O4 O 0.53770(16) 0.27948(11) 0.36616(11) 0.0171(3) Uani 1 1 d . . . . .
O1 O 0.27919(15) 0.17867(11) 0.28894(11) 0.0152(3) Uani 1 1 d . . . . .
O5 O 0.66292(15) 0.08554(12) 0.49533(11) 0.0170(3) Uani 1 1 d . . . . .
O7 O 0.55702(16) 0.10043(12) 0.30335(11) 0.0182(3) Uani 1 1 d . . . . .
H7A H 0.595283 0.048646 0.299216 0.027 Uiso 1 1 d R U . . .
H7B H 0.559985 0.129696 0.255076 0.027 Uiso 1 1 d R U . . .
O8 O 0.43052(16) 0.11165(12) 0.55897(11) 0.0180(3) Uani 1 1 d . . . . .
H8A H 0.434592 0.159811 0.590376 0.027 Uiso 1 1 d R U . . .
H8B H 0.496596 0.079662 0.589187 0.027 Uiso 1 1 d R U . . .
O2 O 0.25847(15) 0.21920(12) 0.42088(11) 0.0170(3) Uani 1 1 d . . . . .
O12 O 0.38002(18) 0.30536(13) 0.19564(12) 0.0203(4) Uani 1 1 d . . . . .
O10 O 0.77264(18) 0.67185(13) 0.44839(12) 0.0214(3) Uani 1 1 d . . . . .
O9 O -0.35161(16) 0.22420(13) 0.19041(11) 0.0217(4) Uani 1 1 d . . . . .
H9 H -0.372672 0.208518 0.137386 0.033 Uiso 1 1 calc R U . . .
C8 C 0.5727(2) 0.32010(16) 0.44204(15) 0.0145(4) Uani 1 1 d . . . . .
C9 C 0.6302(2) 0.41111(16) 0.44784(15) 0.0148(4) Uani 1 1 d . . . . .
C2 C 0.0607(2) 0.22168(16) 0.29607(15) 0.0149(4) Uani 1 1 d . . . . .
C10 C 0.6555(2) 0.44929(17) 0.37103(16) 0.0191(5) Uani 1 1 d . . . . .
H10A H 0.639630 0.415730 0.318229 0.023 Uiso 1 1 calc R U . . .
C16 C 0.8584(2) 0.04132(15) 0.60700(15) 0.0149(4) Uani 1 1 d . . . . .
C14 C 0.6565(2) 0.46192(16) 0.52697(16) 0.0173(4) Uani 1 1 d . . . . .
H14 H 0.640995 0.437033 0.578531 0.021 Uiso 1 1 calc R U . . .
C1 C 0.2055(2) 0.20762(15) 0.33624(15) 0.0144(4) Uani 1 1 d . . . . .
C13 C 0.7054(2) 0.54873(17) 0.52964(16) 0.0176(4) Uani 1 1 d . . . . .
H13 H 0.723367 0.581875 0.582788 0.021 Uiso 1 1 calc R U . . .
C21 C 0.9131(2) 0.00335(17) 0.69126(16) 0.0188(5) Uani 1 1 d . . . . .
H21 H 0.856954 -0.022722 0.722001 0.023 Uiso 1 1 calc R U . . .
C15 C 0.7110(2) 0.03988(15) 0.56530(15) 0.0143(4) Uani 1 1 d . . . . .
C7 C 0.0058(2) 0.21527(16) 0.20296(15) 0.0170(4) Uani 1 1 d . . . . .
H7 H 0.061998 0.208813 0.165601 0.020 Uiso 1 1 calc R U . . .
C12 C 0.7277(2) 0.58648(16) 0.45160(16) 0.0169(4) Uani 1 1 d . . . . .
C17 C 0.9432(2) 0.08100(17) 0.56126(15) 0.0174(4) Uani 1 1 d . . . . .
H17 H 0.906982 0.107464 0.505199 0.021 Uiso 1 1 calc R U . . .
C19 C 1.1335(2) 0.04220(16) 0.68354(16) 0.0171(4) Uani 1 1 d . . . . .
C18 C 1.0804(2) 0.08112(17) 0.59887(16) 0.0195(5) Uani 1 1 d . . . . .
H18 H 1.136821 0.106844 0.568099 0.023 Uiso 1 1 calc R U . . .
C11 C 0.7035(2) 0.53593(17) 0.37269(16) 0.0202(5) Uani 1 1 d . . . . .
H11 H 0.719777 0.560596 0.321248 0.024 Uiso 1 1 calc R U . . .
C3 C -0.0242(2) 0.23366(18) 0.35184(16) 0.0198(5) Uani 1 1 d . . . . .
H3 H 0.011889 0.240502 0.413717 0.024 Uiso 1 1 calc R U . . .
C6 C -0.1314(2) 0.21841(17) 0.16576(15) 0.0185(5) Uani 1 1 d . . . . .
H6 H -0.167385 0.215118 0.103578 0.022 Uiso 1 1 calc R U . . .
C5 C -0.2156(2) 0.22657(17) 0.22222(16) 0.0183(5) Uani 1 1 d . . . . .
C20 C 1.0503(2) 0.00382(18) 0.73012(17) 0.0213(5) Uani 1 1 d . . . . .
H20 H 1.086323 -0.021319 0.786842 0.026 Uiso 1 1 calc R U . . .
C4 C -0.1616(2) 0.23534(19) 0.31506(16) 0.0218(5) Uani 1 1 d . . . . .
H4 H -0.217930 0.242328 0.352264 0.026 Uiso 1 1 calc R U . . .
H12A H 0.438(4) 0.304(3) 0.246(3) 0.050(11) Uiso 1 1 d . . . . .
H12B H 0.333(5) 0.269(3) 0.190(3) 0.054(14) Uiso 1 1 d . . . . .
H10 H 0.765(3) 0.699(3) 0.493(3) 0.033(9) Uiso 1 1 d . . . . .
O11 O 1.26980(15) 0.03886(12) 0.72302(12) 0.0223(4) Uani 1 1 d . . . . .
H11A H 1.305062 0.084263 0.709652 0.033 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
Ho1 O3 2.4415(16) . ?
Ho1 O6 2.3046(16) 3_656 ?
Ho1 O4 2.3495(16) . ?
Ho1 O1 2.4040(15) . ?
Ho1 O5 2.2840(15) . ?
Ho1 O7 2.3770(15) . ?
Ho1 O8 2.3177(16) . ?
Ho1 O2 2.3682(15) . ?
O3 C8 1.275(3) . ?
O6 C15 1.285(3) . ?
O4 C8 1.277(3) . ?
O1 C1 1.267(3) . ?
O5 C15 1.256(3) . ?
O7 H7A 0.8759 . ?
O7 H7B 0.8697 . ?
O8 H8A 0.8585 . ?
O8 H8B 0.8588 . ?
O2 C1 1.281(3) . ?
O12 H12A 0.85(5) . ?
O12 H12B 0.71(5) . ?
O10 C12 1.357(3) . ?
O10 H10 0.82(4) . ?
O9 H9 0.8200 . ?
O9 C5 1.361(3) . ?
C8 C9 1.471(3) . ?
C9 C10 1.401(3) . ?
C9 C14 1.397(3) . ?
C2 C1 1.474(3) . ?
C2 C7 1.395(3) . ?
C2 C3 1.401(3) . ?
C10 H10A 0.9300 . ?
C10 C11 1.378(3) . ?
C16 C21 1.387(3) . ?
C16 C15 1.487(3) . ?
C16 C17 1.399(3) . ?
C14 H14 0.9300 . ?
C14 C13 1.382(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.403(3) . ?
C21 H21 0.9300 . ?
C21 C20 1.384(3) . ?
C7 H7 0.9300 . ?
C7 C6 1.381(3) . ?
C12 C11 1.393(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.382(3) . ?
C19 C18 1.396(3) . ?
C19 C20 1.387(3) . ?
C19 O11 1.378(3) . ?
C18 H18 0.9300 . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.381(3) . ?
C6 H6 0.9300 . ?
C6 C5 1.397(3) . ?
C5 C4 1.393(3) . ?
C20 H20 0.9300 . ?
C4 H4 0.9300 . ?
O11 H11A 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Ho1 O3 154.20(5) 3_656 . ?
O6 Ho1 O4 151.56(6) 3_656 . ?
O6 Ho1 O1 80.14(6) 3_656 . ?
O6 Ho1 O7 83.22(6) 3_656 . ?
O6 Ho1 O8 76.49(6) 3_656 . ?
O6 Ho1 O2 92.59(6) 3_656 . ?
O4 Ho1 O3 54.09(5) . . ?
O4 Ho1 O1 78.77(6) . . ?
O4 Ho1 O7 74.38(6) . . ?
O4 Ho1 O2 90.54(6) . . ?
O1 Ho1 O3 115.23(6) . . ?
O5 Ho1 O3 81.96(6) . . ?
O5 Ho1 O6 91.46(6) . 3_656 ?
O5 Ho1 O4 99.67(6) . . ?
O5 Ho1 O1 154.87(6) . . ?
O5 Ho1 O7 75.97(6) . . ?
O5 Ho1 O8 77.04(6) . . ?
O5 Ho1 O2 150.21(6) . . ?
O7 Ho1 O3 118.75(6) . . ?
O7 Ho1 O1 79.52(5) . . ?
O8 Ho1 O3 77.73(6) . . ?
O8 Ho1 O4 131.42(6) . . ?
O8 Ho1 O1 122.92(5) . . ?
O8 Ho1 O7 145.57(6) . . ?
O8 Ho1 O2 75.27(6) . . ?
O2 Ho1 O3 81.63(5) . . ?
O2 Ho1 O1 54.56(5) . . ?
O2 Ho1 O7 133.82(6) . . ?
C8 O3 Ho1 92.18(13) . . ?
C15 O6 Ho1 135.89(14) . 3_656 ?
C8 O4 Ho1 96.41(13) . . ?
C1 O1 Ho1 92.50(13) . . ?
C15 O5 Ho1 138.34(14) . . ?
Ho1 O7 H7A 127.0 . . ?
Ho1 O7 H7B 128.2 . . ?
H7A O7 H7B 104.7 . . ?
Ho1 O8 H8A 109.5 . . ?
Ho1 O8 H8B 109.6 . . ?
H8A O8 H8B 104.3 . . ?
C1 O2 Ho1 93.79(12) . . ?
H12A O12 H12B 113(5) . . ?
C12 O10 H10 108(3) . . ?
C5 O9 H9 109.5 . . ?
O3 C8 O4 117.3(2) . . ?
O3 C8 C9 122.8(2) . . ?
O4 C8 C9 119.9(2) . . ?
C10 C9 C8 119.2(2) . . ?
C14 C9 C8 121.9(2) . . ?
C14 C9 C10 118.8(2) . . ?
C7 C2 C1 120.3(2) . . ?
C7 C2 C3 119.5(2) . . ?
C3 C2 C1 120.0(2) . . ?
C9 C10 H10A 119.6 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10A 119.6 . . ?
C21 C16 C15 120.5(2) . . ?
C21 C16 C17 119.4(2) . . ?
C17 C16 C15 120.1(2) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.9(2) . . ?
C13 C14 H14 119.6 . . ?
O1 C1 O2 118.28(19) . . ?
O1 C1 C2 120.8(2) . . ?
O2 C1 C2 120.82(19) . . ?
C14 C13 H13 120.2 . . ?
C14 C13 C12 119.5(2) . . ?
C12 C13 H13 120.2 . . ?
C16 C21 H21 119.6 . . ?
C20 C21 C16 120.8(2) . . ?
C20 C21 H21 119.6 . . ?
O6 C15 C16 118.4(2) . . ?
O5 C15 O6 122.78(19) . . ?
O5 C15 C16 118.86(19) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.6(2) . . ?
C6 C7 H7 119.7 . . ?
O10 C12 C13 122.9(2) . . ?
O10 C12 C11 117.0(2) . . ?
C11 C12 C13 120.1(2) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.4(2) . . ?
C18 C17 H17 119.8 . . ?
C20 C19 C18 120.8(2) . . ?
O11 C19 C18 121.5(2) . . ?
O11 C19 C20 117.7(2) . . ?
C17 C18 C19 119.3(2) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C10 C11 C12 119.8(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 H3 120.0 . . ?
C7 C6 H6 120.2 . . ?
C7 C6 C5 119.5(2) . . ?
C5 C6 H6 120.2 . . ?
O9 C5 C6 122.4(2) . . ?
O9 C5 C4 117.3(2) . . ?
C4 C5 C6 120.3(2) . . ?
C21 C20 C19 119.3(2) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C3 C4 C5 120.0(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C19 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O3 C8 O4 -0.52(19) . . . . ?
Ho1 O3 C8 C9 179.97(18) . . . . ?
Ho1 O6 C15 O5 81.1(3) 3_656 . . . ?
Ho1 O6 C15 C16 -99.7(2) 3_656 . . . ?
Ho1 O4 C8 O3 0.5(2) . . . . ?
Ho1 O4 C8 C9 -179.93(17) . . . . ?
Ho1 O1 C1 O2 9.2(2) . . . . ?
Ho1 O1 C1 C2 -166.73(19) . . . . ?
Ho1 O5 C15 O6 20.8(4) . . . . ?
Ho1 O5 C15 C16 -158.32(16) . . . . ?
Ho1 O2 C1 O1 -9.3(2) . . . . ?
Ho1 O2 C1 C2 166.57(19) . . . . ?
O3 C8 C9 C10 174.6(2) . . . . ?
O3 C8 C9 C14 -7.5(3) . . . . ?
O4 C8 C9 C10 -5.0(3) . . . . ?
O4 C8 C9 C14 173.0(2) . . . . ?
O10 C12 C11 C10 -178.8(2) . . . . ?
O9 C5 C4 C3 176.8(2) . . . . ?
C8 C9 C10 C11 177.0(2) . . . . ?
C8 C9 C14 C13 -177.3(2) . . . . ?
C9 C10 C11 C12 0.1(4) . . . . ?
C9 C14 C13 C12 0.6(3) . . . . ?
C2 C7 C6 C5 -1.1(4) . . . . ?
C2 C3 C4 C5 -1.0(4) . . . . ?
C10 C9 C14 C13 0.6(3) . . . . ?
C16 C21 C20 C19 -0.5(4) . . . . ?
C16 C17 C18 C19 -0.8(4) . . . . ?
C14 C9 C10 C11 -1.0(3) . . . . ?
C14 C13 C12 O10 178.5(2) . . . . ?
C14 C13 C12 C11 -1.4(3) . . . . ?
C1 C2 C7 C6 172.8(2) . . . . ?
C1 C2 C3 C4 -171.7(2) . . . . ?
C13 C12 C11 C10 1.1(4) . . . . ?
C21 C16 C15 O6 -9.1(3) . . . . ?
C21 C16 C15 O5 170.1(2) . . . . ?
C21 C16 C17 C18 1.1(4) . . . . ?
C15 C16 C21 C20 179.5(2) . . . . ?
C15 C16 C17 C18 -178.8(2) . . . . ?
C7 C2 C1 O1 -8.9(3) . . . . ?
C7 C2 C1 O2 175.3(2) . . . . ?
C7 C2 C3 C4 2.7(4) . . . . ?
C7 C6 C5 O9 -175.6(2) . . . . ?
C7 C6 C5 C4 2.7(4) . . . . ?
C17 C16 C21 C20 -0.4(4) . . . . ?
C17 C16 C15 O6 170.8(2) . . . . ?
C17 C16 C15 O5 -10.0(3) . . . . ?
C18 C19 C20 C21 0.8(4) . . . . ?
C3 C2 C1 O1 165.5(2) . . . . ?
C3 C2 C1 O2 -10.3(3) . . . . ?
C3 C2 C7 C6 -1.6(4) . . . . ?
C6 C5 C4 C3 -1.7(4) . . . . ?
C20 C19 C18 C17 -0.1(4) . . . . ?
O11 C19 C18 C17 178.6(2) . . . . ?
O11 C19 C20 C21 -177.9(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 2.760
_oxdiff_exptl_absorpt_empirical_full_min 0.729
####################################################################### 
# 
# 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_jo264_b1
_database_code_depnum_ccdc_archive 'CCDC 2269124'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H42 Ho2 O24, 10(H2 O)'
_chemical_formula_sum            'C42 H62 Ho2 O34'
_chemical_formula_weight         1440.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ho C H O'
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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8167(2)
_cell_length_b                   11.3009(2)
_cell_length_c                   11.45320(10)
_cell_angle_alpha                90.5010(10)
_cell_angle_beta                 101.7230(10)
_cell_angle_gamma                105.3020(10)
_cell_volume                     1319.33(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    22764
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      77.0560
_cell_measurement_theta_min      3.9530
_shelx_estimated_absorpt_T_max   0.505
_shelx_estimated_absorpt_T_min   0.404
_exptl_absorpt_coefficient_mu    6.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.125
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26548
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.475
_diffrn_reflns_theta_min         3.951
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 121.00   0.50    0.05    --   47.82  35.00  61.00  172
  2  ω     33.00 119.00   0.50    0.05    --   47.82  57.00 150.00  172
  3  ω     25.00 118.00   0.50    0.05    --   47.82  77.00-150.00  186
  4  ω     95.00 178.00   0.50    0.05    --  107.75 125.00 -60.00  166
  5  ω     95.00 178.00   0.50    0.05    --  107.75 125.00 -90.00  166
  6  ω     95.00 178.00   0.50    0.05    --  107.75 125.00-120.00  166
  7  ω     94.00 178.00   0.50    0.05    --  107.75  15.00-120.00  168
  8  ω     35.00 131.00   0.50    0.05    --  107.75 -77.00-120.00  192
  9  ω     95.00 178.00   0.50    0.05    --  107.75  35.00  61.00  166
 10  ω     94.00 178.00   0.50    0.05    --  107.75  15.00  30.00  168
 11  ω     36.00  76.00   0.50    0.05    --  107.75 -45.00  30.00   80
 12  ω     36.00  76.00   0.50    0.05    --  107.75 -45.00   0.00   80
 13  ω     36.00  76.00   0.50    0.05    --  107.75 -45.00 -60.00   80
 14  ω     33.00  66.00   0.50    0.05    --  107.75 -30.00 -60.00   66
 15  ω     34.00  68.00   0.50    0.05    --  107.75 -35.00 -96.00   68
 16  ω     36.00  76.00   0.50    0.05    --  107.75 -45.00-120.00   80
 17  ω    -25.00  61.00   0.50    0.05    --   47.82 -35.00 -96.00  172
 18  ω    -23.00  63.00   0.50    0.05    --   47.82 -57.00  30.00  172
 19  ω     33.00  66.00   0.50    0.05    --  107.75 -30.00   0.00   66
 20  ω     33.00  66.00   0.50    0.05    --  107.75 -30.00  60.00   66
 21  ω     33.00  66.00   0.50    0.05    --  107.75 -30.00 150.00   66
 22  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00  60.00  142
 23  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00  30.00  142
 24  ω     35.00 112.00   0.50    0.05    --  107.75-125.00 150.00  154
 25  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00   0.00  142
 26  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00 -60.00  142
 27  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00-150.00  142
 28  ω     35.00 112.00   0.50    0.05    --  107.75-125.00-150.00  154
 29  ω     35.00 106.00   0.50    0.05    --  107.75 -96.00-179.32  142
 30  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00-120.00  142
 31  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00 -30.00  142
 32  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00  90.00  142
 33  ω     35.00 106.00   0.50    0.05    --  107.75 -94.00 150.00  142
 34  ω    -85.00 -13.00   0.50    0.05    --  -47.82 125.00 150.00  144
 35  ω    -86.00 -13.00   0.50    0.05    --  -86.25 125.00  90.00  146
 36  ω    -60.00  26.00   0.50    0.05    --  -47.82  35.00  61.00  172
 37  ω    -70.00 -13.00   0.50    0.05    --  -86.25  35.00  61.00  114
 38  ω   -121.00 -35.00   0.50    0.05    --  -47.82 -35.00 -96.00  172
 39  ω   -160.00 -73.00   0.50    0.05    --  -86.25 -35.00 -96.00  174
 40  ω   -119.00 -73.00   0.50    0.05    --  -47.82-125.00-150.00   92
 41  ω   -119.00 -73.00   0.50    0.05    --  -47.82-125.00-120.00   92
 42  ω   -119.00 -25.00   0.50    0.05    --  -47.82 -77.00  30.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0083322000
_diffrn_orient_matrix_UB_12      0.1206527000
_diffrn_orient_matrix_UB_13      -0.0585583000
_diffrn_orient_matrix_UB_21      -0.1412745000
_diffrn_orient_matrix_UB_22      -0.0215878000
_diffrn_orient_matrix_UB_23      0.0183366000
_diffrn_orient_matrix_UB_31      0.0530269000
_diffrn_orient_matrix_UB_32      0.0709878000
_diffrn_orient_matrix_UB_33      0.1232435000
_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'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5470
_reflns_number_total             5499
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5499
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0318
_refine_ls_restrained_S_all      1.083
_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)+(0.0480P)²+2.0072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0826
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H13A-H14A
 2.2 with sigma of 0.02
2.a Free rotating group:
 O16(H16A,H16B), O13(H13A,H13B), O15(H15A,H15B), O17(H17A,H17B), O14(H14A,H14B)
2.b Rotating group:
 O11(H11A,H11B), O10(H10A,H10B), O12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C13(H13), C17(H17), C7(H7A), C20(H20), C10(H10), C3(H3), C4(H4),
 C11(H11), C6(H6), C14(H14), C18(H18)
2.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O7(H7), O9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.52083(2) 0.39276(2) 0.31646(2) 0.00609(7) Uani 1 1 d . . . . .
O3 O 0.66088(16) 0.51353(16) 0.47662(15) 0.0111(3) Uani 1 1 d . . . . .
O11 O 0.45027(17) 0.57668(15) 0.32061(15) 0.0105(3) Uani 1 1 d . . . . .
H11A H 0.384458 0.571863 0.262917 0.016 Uiso 1 1 d R U . . .
H11B H 0.420105 0.581751 0.383557 0.016 Uiso 1 1 d R U . . .
O2 O 0.71754(17) 0.35103(15) 0.28205(15) 0.0103(3) Uani 1 1 d . . . . .
O4 O 0.65840(16) 0.66786(15) 0.59721(15) 0.0105(3) Uani 1 1 d . . . . .
O5 O 0.44636(17) 0.20738(15) 0.21371(16) 0.0123(3) Uani 1 1 d . . . . .
O10 O 0.56617(17) 0.25718(16) 0.47222(16) 0.0136(3) Uani 1 1 d . . . . .
H10A H 0.616744 0.217156 0.453545 0.020 Uiso 1 1 d R U . . .
H10B H 0.495674 0.202257 0.474426 0.020 Uiso 1 1 d R U . . .
O1 O 0.68097(17) 0.52532(15) 0.22183(16) 0.0116(3) Uani 1 1 d . . . . .
O16 O 0.69811(17) 0.12271(16) 0.18533(16) 0.0125(3) Uani 1 1 d G . . . .
H16A H 0.621259 0.080639 0.188711 0.019 Uiso 1 1 d G U . . .
H16B H 0.721831 0.191077 0.226232 0.019 Uiso 1 1 d G U . . .
O12 O 0.40540(18) 0.41885(16) 0.12250(15) 0.0122(3) Uani 1 1 d . . . . .
H12A H 0.431537 0.383380 0.069812 0.018 Uiso 1 1 d R U . . .
H12B H 0.426019 0.494731 0.107982 0.018 Uiso 1 1 d R U . . .
O8 O 1.23468(17) 0.85852(16) 0.50138(16) 0.0124(3) Uani 1 1 d . . . . .
H8 H 1.260094 0.926567 0.537211 0.019 Uiso 1 1 calc R U . . .
O13 O 0.48889(19) 0.33100(17) 0.94388(17) 0.0167(4) Uani 1 1 d G . . . .
H13A H 0.418768 0.300979 0.891718 0.025 Uiso 1 1 d DG U . . .
H13B H 0.532560 0.278293 0.956240 0.025 Uiso 1 1 d G U . . .
O7 O 1.25430(17) 0.60491(16) 0.13332(16) 0.0131(3) Uani 1 1 d . . . . .
H7 H 1.265336 0.671659 0.103628 0.020 Uiso 1 1 calc R U . . .
O6 O 0.44536(17) 0.01073(15) 0.21155(16) 0.0126(3) Uani 1 1 d . . . . .
O15 O 0.3380(2) 0.81673(16) 0.04654(16) 0.0163(4) Uani 1 1 d G . . . .
H15A H 0.322074 0.842566 -0.022917 0.024 Uiso 1 1 d G U . . .
H15B H 0.374902 0.881506 0.092204 0.024 Uiso 1 1 d G U . . .
O9 O -0.16113(18) -0.03603(16) 0.16822(18) 0.0158(4) Uani 1 1 d . . . . .
H9 H -0.188031 0.025315 0.168733 0.024 Uiso 1 1 calc R U . . .
O17 O 0.60303(18) 0.91491(17) 0.40646(16) 0.0153(4) Uani 1 1 d G . . . .
H17A H 0.624140 0.862241 0.366880 0.023 Uiso 1 1 d G U . . .
H17B H 0.547454 0.939334 0.355882 0.023 Uiso 1 1 d G U . . .
C1 C 0.7525(2) 0.4519(2) 0.2325(2) 0.0083(4) Uani 1 1 d . . . . .
O14 O 0.30742(19) 0.22715(17) 0.73528(18) 0.0180(4) Uani 1 1 d G . . . .
H14A H 0.291669 0.295209 0.717059 0.027 Uiso 1 1 d DG U . . .
H14B H 0.249532 0.174049 0.759130 0.027 Uiso 1 1 d G U . . .
C8 C 0.7136(2) 0.6180(2) 0.53147(19) 0.0070(4) Uani 1 1 d . . . . .
C5 C 1.1284(2) 0.5652(2) 0.1477(2) 0.0090(4) Uani 1 1 d . . . . .
C2 C 0.8788(2) 0.4850(2) 0.1936(2) 0.0078(4) Uani 1 1 d . . . . .
C15 C 0.3867(2) 0.0946(2) 0.20707(19) 0.0093(4) Uani 1 1 d . . . . .
C9 C 0.8499(2) 0.6848(2) 0.52106(19) 0.0076(4) Uani 1 1 d . . . . .
C19 C -0.0290(2) -0.0013(2) 0.1734(2) 0.0106(4) Uani 1 1 d . . . . .
C21 C 0.1695(2) 0.1420(2) 0.1469(2) 0.0109(4) Uani 1 1 d . . . . .
H21 H 0.212714 0.217976 0.124244 0.013 Uiso 1 1 calc R U . . .
C16 C 0.2409(2) 0.0595(2) 0.1918(2) 0.0095(4) Uani 1 1 d . . . . .
C13 C 1.0336(2) 0.8672(2) 0.5589(2) 0.0096(4) Uani 1 1 d . . . . .
H13 H 1.069880 0.948692 0.588361 0.012 Uiso 1 1 calc R U . . .
C17 C 0.1755(2) -0.0538(2) 0.2261(2) 0.0113(4) Uani 1 1 d . . . . .
H17 H 0.222098 -0.109747 0.254366 0.014 Uiso 1 1 calc R U . . .
C7 C 0.9127(2) 0.5907(2) 0.1318(2) 0.0102(4) Uani 1 1 d . . . . .
H7A H 0.851302 0.634241 0.106196 0.012 Uiso 1 1 calc R U . . .
C12 C 1.1077(2) 0.8051(2) 0.5086(2) 0.0085(4) Uani 1 1 d . . . . .
C20 C 0.0343(2) 0.1110(2) 0.1360(2) 0.0116(5) Uani 1 1 d . . . . .
H20 H -0.013362 0.164956 0.103979 0.014 Uiso 1 1 calc R U . . .
C10 C 0.9253(2) 0.6243(2) 0.4700(2) 0.0088(4) Uani 1 1 d . . . . .
H10 H 0.889208 0.542869 0.440375 0.011 Uiso 1 1 calc R U . . .
C3 C 0.9697(2) 0.4171(2) 0.2272(2) 0.0091(4) Uani 1 1 d . . . . .
H3 H 0.945963 0.344699 0.265102 0.011 Uiso 1 1 calc R U . . .
C4 C 1.0943(2) 0.4563(2) 0.2047(2) 0.0099(4) Uani 1 1 d . . . . .
H4 H 1.154515 0.410875 0.227133 0.012 Uiso 1 1 calc R U . . .
C11 C 1.0529(2) 0.6836(2) 0.4631(2) 0.0099(4) Uani 1 1 d . . . . .
H11 H 1.101708 0.642558 0.428174 0.012 Uiso 1 1 calc R U . . .
C6 C 1.0372(2) 0.6308(2) 0.1085(2) 0.0108(4) Uani 1 1 d . . . . .
H6 H 1.059672 0.700934 0.067024 0.013 Uiso 1 1 calc R U . . .
C14 C 0.9054(2) 0.8073(2) 0.5651(2) 0.0083(4) Uani 1 1 d . . . . .
H14 H 0.856223 0.848859 0.598702 0.010 Uiso 1 1 calc R U . . .
C18 C 0.0410(2) -0.0835(2) 0.2182(2) 0.0123(5) Uani 1 1 d . . . . .
H18 H -0.002131 -0.158518 0.242933 0.015 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
Ho1 O3 2.2930(16) . ?
Ho1 O11 2.3990(16) . ?
Ho1 O2 2.4026(17) . ?
Ho1 O4 2.3010(17) 2_666 ?
Ho1 O5 2.2592(16) . ?
Ho1 O10 2.4206(17) . ?
Ho1 O1 2.4168(17) . ?
Ho1 O12 2.3790(17) . ?
O3 C8 1.265(3) . ?
O11 H11A 0.8568 . ?
O11 H11B 0.8569 . ?
O2 C1 1.279(3) . ?
O4 C8 1.263(3) . ?
O5 C15 1.261(3) . ?
O10 H10A 0.8520 . ?
O10 H10B 0.8519 . ?
O1 C1 1.267(3) . ?
O16 H16A 0.8505 . ?
O16 H16B 0.8500 . ?
O12 H12A 0.8542 . ?
O12 H12B 0.8540 . ?
O8 H8 0.8200 . ?
O8 C12 1.367(3) . ?
O13 H13A 0.8507 . ?
O13 H13B 0.8490 . ?
O7 H7 0.8200 . ?
O7 C5 1.361(3) . ?
O6 C15 1.268(3) . ?
O15 H15A 0.8502 . ?
O15 H15B 0.8502 . ?
O9 H9 0.8200 . ?
O9 C19 1.367(3) . ?
O17 H17A 0.8491 . ?
O17 H17B 0.8497 . ?
C1 C2 1.479(3) . ?
O14 H14A 0.8495 . ?
O14 H14B 0.8372 . ?
C8 C9 1.498(3) . ?
C5 C4 1.396(3) . ?
C5 C6 1.391(3) . ?
C2 C7 1.396(3) . ?
C2 C3 1.397(3) . ?
C15 C16 1.495(3) . ?
C9 C10 1.399(3) . ?
C9 C14 1.398(3) . ?
C19 C20 1.391(3) . ?
C19 C18 1.386(3) . ?
C21 H21 0.9300 . ?
C21 C16 1.399(3) . ?
C21 C20 1.389(4) . ?
C16 C17 1.392(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.395(3) . ?
C13 C14 1.389(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.388(4) . ?
C7 H7A 0.9300 . ?
C7 C6 1.385(3) . ?
C12 C11 1.394(3) . ?
C20 H20 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.385(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.381(3) . ?
C4 H4 0.9300 . ?
C11 H11 0.9300 . ?
C6 H6 0.9300 . ?
C14 H14 0.9300 . ?
C18 H18 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
O3 Ho1 O11 74.74(6) . . ?
O3 Ho1 O2 83.55(6) . . ?
O3 Ho1 O4 97.28(6) . 2_666 ?
O3 Ho1 O10 72.91(6) . . ?
O3 Ho1 O1 78.19(6) . . ?
O3 Ho1 O12 138.11(6) . . ?
O11 Ho1 O2 133.39(6) . . ?
O11 Ho1 O10 131.03(6) . . ?
O11 Ho1 O1 80.81(6) . . ?
O2 Ho1 O10 77.54(6) . . ?
O2 Ho1 O1 54.29(6) . . ?
O4 Ho1 O11 77.63(6) 2_666 . ?
O4 Ho1 O2 146.86(6) 2_666 . ?
O4 Ho1 O10 71.20(6) 2_666 . ?
O4 Ho1 O1 158.40(6) 2_666 . ?
O4 Ho1 O12 97.27(6) 2_666 . ?
O5 Ho1 O3 148.15(6) . . ?
O5 Ho1 O11 136.45(6) . . ?
O5 Ho1 O2 76.73(6) . . ?
O5 Ho1 O4 86.41(6) . 2_666 ?
O5 Ho1 O10 78.53(6) . . ?
O5 Ho1 O1 108.69(6) . . ?
O5 Ho1 O12 71.84(6) . . ?
O1 Ho1 O10 125.90(6) . . ?
O12 Ho1 O11 70.42(6) . . ?
O12 Ho1 O2 104.06(6) . . ?
O12 Ho1 O10 148.89(6) . . ?
O12 Ho1 O1 74.01(6) . . ?
C8 O3 Ho1 150.25(15) . . ?
Ho1 O11 H11A 109.8 . . ?
Ho1 O11 H11B 109.7 . . ?
H11A O11 H11B 104.2 . . ?
C1 O2 Ho1 93.27(14) . . ?
C8 O4 Ho1 136.66(15) . 2_666 ?
C15 O5 Ho1 150.11(16) . . ?
Ho1 O10 H10A 109.5 . . ?
Ho1 O10 H10B 109.2 . . ?
H10A O10 H10B 104.4 . . ?
C1 O1 Ho1 92.93(14) . . ?
H16A O16 H16B 113.0 . . ?
Ho1 O12 H12A 109.7 . . ?
Ho1 O12 H12B 109.7 . . ?
H12A O12 H12B 104.3 . . ?
C12 O8 H8 109.5 . . ?
H13A O13 H13B 109.5 . . ?
C5 O7 H7 109.5 . . ?
H15A O15 H15B 104.6 . . ?
C19 O9 H9 109.5 . . ?
H17A O17 H17B 104.5 . . ?
O2 C1 C2 120.0(2) . . ?
O1 C1 O2 119.5(2) . . ?
O1 C1 C2 120.4(2) . . ?
H14A O14 H14B 117.8 . . ?
O3 C8 C9 118.6(2) . . ?
O4 C8 O3 123.3(2) . . ?
O4 C8 C9 118.1(2) . . ?
O7 C5 C4 117.3(2) . . ?
O7 C5 C6 121.6(2) . . ?
C6 C5 C4 121.0(2) . . ?
C7 C2 C1 120.0(2) . . ?
C7 C2 C3 119.5(2) . . ?
C3 C2 C1 120.3(2) . . ?
O5 C15 O6 122.7(2) . . ?
O5 C15 C16 118.1(2) . . ?
O6 C15 C16 119.2(2) . . ?
C10 C9 C8 120.3(2) . . ?
C14 C9 C8 120.9(2) . . ?
C14 C9 C10 118.8(2) . . ?
O9 C19 C20 122.4(2) . . ?
O9 C19 C18 117.0(2) . . ?
C18 C19 C20 120.6(2) . . ?
C16 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C16 120.4(2) . . ?
C21 C16 C15 120.2(2) . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 C21 119.4(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C14 C13 C12 119.9(2) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.3(2) . . ?
C18 C17 H17 119.9 . . ?
C2 C7 H7A 119.9 . . ?
C6 C7 C2 120.2(2) . . ?
C6 C7 H7A 119.9 . . ?
O8 C12 C13 122.7(2) . . ?
O8 C12 C11 117.2(2) . . ?
C11 C12 C13 120.2(2) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 C19 119.4(2) . . ?
C21 C20 H20 120.3 . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.0(2) . . ?
C11 C10 H10 119.5 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.6 . . ?
C5 C4 H4 120.5 . . ?
C3 C4 C5 118.9(2) . . ?
C3 C4 H4 120.5 . . ?
C12 C11 H11 120.2 . . ?
C10 C11 C12 119.6(2) . . ?
C10 C11 H11 120.2 . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.4(2) . . ?
C7 C6 H6 120.3 . . ?
C9 C14 H14 119.7 . . ?
C13 C14 C9 120.5(2) . . ?
C13 C14 H14 119.7 . . ?
C19 C18 C17 119.9(2) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O3 C8 O4 81.8(4) . . . . ?
Ho1 O3 C8 C9 -100.0(3) . . . . ?
Ho1 O2 C1 O1 0.1(2) . . . . ?
Ho1 O2 C1 C2 177.02(18) . . . . ?
Ho1 O4 C8 O3 13.7(4) 2_666 . . . ?
Ho1 O4 C8 C9 -164.53(15) 2_666 . . . ?
Ho1 O5 C15 O6 -108.1(3) . . . . ?
Ho1 O5 C15 C16 72.6(4) . . . . ?
Ho1 O1 C1 O2 -0.1(2) . . . . ?
Ho1 O1 C1 C2 -177.00(18) . . . . ?
O3 C8 C9 C10 -11.3(3) . . . . ?
O3 C8 C9 C14 170.6(2) . . . . ?
O2 C1 C2 C7 175.4(2) . . . . ?
O2 C1 C2 C3 -10.1(3) . . . . ?
O4 C8 C9 C10 167.0(2) . . . . ?
O4 C8 C9 C14 -11.1(3) . . . . ?
O5 C15 C16 C21 20.9(3) . . . . ?
O5 C15 C16 C17 -156.8(2) . . . . ?
O1 C1 C2 C7 -7.7(3) . . . . ?
O1 C1 C2 C3 166.7(2) . . . . ?
O8 C12 C11 C10 178.8(2) . . . . ?
O7 C5 C4 C3 176.2(2) . . . . ?
O7 C5 C6 C7 -176.0(2) . . . . ?
O6 C15 C16 C21 -158.4(2) . . . . ?
O6 C15 C16 C17 23.9(3) . . . . ?
O9 C19 C20 C21 178.2(2) . . . . ?
O9 C19 C18 C17 -179.9(2) . . . . ?
C1 C2 C7 C6 171.8(2) . . . . ?
C1 C2 C3 C4 -171.6(2) . . . . ?
C8 C9 C10 C11 -178.0(2) . . . . ?
C8 C9 C14 C13 177.7(2) . . . . ?
C2 C7 C6 C5 -0.3(3) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C15 C16 C17 C18 176.4(2) . . . . ?
C9 C10 C11 C12 0.7(3) . . . . ?
C21 C16 C17 C18 -1.4(4) . . . . ?
C16 C21 C20 C19 1.9(4) . . . . ?
C16 C17 C18 C19 1.5(4) . . . . ?
C13 C12 C11 C10 -1.2(3) . . . . ?
C7 C2 C3 C4 2.9(3) . . . . ?
C12 C13 C14 C9 0.0(3) . . . . ?
C20 C19 C18 C17 0.1(4) . . . . ?
C20 C21 C16 C15 -178.1(2) . . . . ?
C20 C21 C16 C17 -0.3(3) . . . . ?
C10 C9 C14 C13 -0.5(3) . . . . ?
C3 C2 C7 C6 -2.7(3) . . . . ?
C4 C5 C6 C7 3.3(3) . . . . ?
C6 C5 C4 C3 -3.2(3) . . . . ?
C14 C9 C10 C11 0.1(3) . . . . ?
C14 C13 C12 O8 -179.1(2) . . . . ?
C14 C13 C12 C11 0.8(3) . . . . ?
C18 C19 C20 C21 -1.8(4) . . . . ?

_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 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.691
####################################################################### 
# 
# 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_jo289_b2
_database_code_depnum_ccdc_archive 'CCDC 2269127'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H38 O22 Y2, 2(H2 O)'
_chemical_formula_sum            'C42 H42 O24 Y2'
_chemical_formula_weight         1108.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Y C H O'
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'
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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.37330(10)
_cell_length_b                   14.88310(10)
_cell_length_c                   15.43080(10)
_cell_angle_alpha                90
_cell_angle_beta                 105.8630(10)
_cell_angle_gamma                90
_cell_volume                     2291.59(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    32049
_cell_measurement_temperature    122.97(10)
_cell_measurement_theta_max      76.5400
_cell_measurement_theta_min      4.2230
_shelx_estimated_absorpt_T_max   0.616
_shelx_estimated_absorpt_T_min   0.521
_exptl_absorpt_coefficient_mu    4.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.129
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.897
_diffrn_reflns_theta_min         4.207
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     28.00 120.00   0.50    0.05    --   47.64  69.00 -21.00  184
  2  ω     85.00 178.00   0.50    0.05    --  107.11  77.00  60.00  186
  3  ω     91.00 178.00   0.50    0.05    --  107.11  61.00  60.00  174
  4  ω     95.00 178.00   0.50    0.05    --  107.11  45.00  60.00  166
  5  ω     95.00 178.00   0.50    0.05    --  107.11  30.00 120.00  166
  6  ω     88.00 178.00   0.50    0.05    --  107.11  69.00 -21.00  180
  7  ω     94.00 178.00   0.50    0.05    --  107.11  15.00 -90.00  168
  8  ω    124.00 178.00   0.50    0.05    --  107.11  45.00-120.00  108
  9  ω     95.00 178.00   0.50    0.05    --  107.11  45.00 -90.00  166
 10  ω     94.00 178.00   0.50    0.05    --  107.11  15.00 -30.00  168
 11  ω     94.00 178.00   0.50    0.05    --  107.11  15.00  30.00  168
 12  ω     59.00  85.00   0.50    0.05    --  107.11 -94.00 -60.00   52
 13  ω     41.00  74.00   0.50    0.05    --  107.11 -94.00   0.00   66
 14  ω     35.00 106.00   0.50    0.05    --  107.11 -94.00 -90.00  142
 15  ω     35.00 106.00   0.50    0.05    --  107.11 -94.00-150.00  142
 16  ω     34.00  95.00   0.50    0.05    --   47.64-125.00 -30.00  122
 17  ω    -24.00  67.00   0.50    0.05    --   47.64 -69.00-153.00  182
 18  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00 -30.00   68
 19  ω     36.00  70.00   0.50    0.05    --  107.11 -45.00  30.00   68
 20  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00  30.00   68
 21  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00   0.00   68
 22  ω     35.00 127.00   0.50    0.05    --  107.11 -69.00-153.00  184
 23  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00-180.00   68
 24  ω    -27.00  60.00   0.50    0.05    --   47.64 -19.00-180.00  174
 25  ω     36.00  76.00   0.50    0.05    --  107.11 -45.00-120.00   80
 26  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00 -90.00   68
 27  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00 120.00   68
 28  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00  90.00   68
 29  ω    -67.00  25.00   0.50    0.05    --  -47.64  69.00 -21.00  184
 30  ω   -106.00 -13.00   0.50    0.05    --  -86.25  69.00 -21.00  186
 31  ω    -68.00 -11.00   0.50    0.05    --  -86.25  30.00-180.00  114
 32  ω   -159.00 -67.00   0.50    0.05    --  -86.25 -69.00-153.00  184
 33  ω   -120.00 -28.00   0.50    0.05    --  -47.64 -69.00-153.00  184
 34  ω   -161.00 -73.00   0.50    0.05    --  -86.25 -30.00  90.00  176
 35  ω   -158.00 -73.00   0.50    0.05    --  -86.25 -45.00 150.00  170
 36  ω   -159.00 -70.00   0.50    0.05    --  -86.25 -61.00  90.00  178
 37  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00  30.00   94
 38  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00   0.00   94
 39  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-120.00   94
 40  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-180.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0790024000
_diffrn_orient_matrix_UB_12      -0.0034353000
_diffrn_orient_matrix_UB_13      -0.0712285000
_diffrn_orient_matrix_UB_21      -0.0814515000
_diffrn_orient_matrix_UB_22      0.0804191000
_diffrn_orient_matrix_UB_23      -0.0493259000
_diffrn_orient_matrix_UB_31      0.1047387000
_diffrn_orient_matrix_UB_32      0.0650531000
_diffrn_orient_matrix_UB_33      0.0571141000
_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                4729
_reflns_number_total             4773
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0253
_refine_ls_restrained_S_all      1.106
_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)+(0.0402P)²+1.7667P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0702
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Free rotating group:
 O12(H12A,H12B)
1.b Rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
1.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C10(H10A), C20(H20), C14(H14), C3(H3), C6(H6), C7(H7), C17(H17),
 C11(H11A), C13(H13), C18(H18), C4(H4)
1.d Idealised tetrahedral OH refined as rotating group:
 O10(H10), O9(H9), O11(H11)
;
_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
Y001 Y 0.46199(2) 0.85272(2) 0.41997(2) 0.01055(6) Uani 1 1 d . . . . .
O2 O 0.27968(12) 0.82139(8) 0.28896(8) 0.0142(2) Uani 1 1 d . . . . .
O3 O 0.55691(12) 0.72156(8) 0.51074(8) 0.0162(2) Uani 1 1 d . . . . .
O4 O 0.53823(13) 0.72059(8) 0.36625(8) 0.0160(2) Uani 1 1 d . . . . .
O6 O 0.63786(12) 1.00803(8) 0.60290(8) 0.0140(2) Uani 1 1 d . . . . .
O5 O 0.66268(12) 0.91463(9) 0.49541(8) 0.0159(2) Uani 1 1 d . . . . .
O1 O 0.25897(12) 0.78072(9) 0.42100(8) 0.0162(2) Uani 1 1 d . . . . .
O8 O 0.43069(13) 0.88789(9) 0.55918(8) 0.0168(3) Uani 1 1 d . . . . .
H8A H 0.441501 0.840803 0.592005 0.025 Uiso 1 1 d R U . . .
H8B H 0.492681 0.923413 0.587376 0.025 Uiso 1 1 d R U . . .
O7 O 0.55679(12) 0.89957(9) 0.30340(8) 0.0170(3) Uani 1 1 d . . . . .
H7A H 0.624899 0.932565 0.325652 0.026 Uiso 1 1 d R U . . .
H7B H 0.588253 0.854113 0.282524 0.026 Uiso 1 1 d R U . . .
O10 O 0.77209(14) 0.32823(9) 0.44831(9) 0.0207(3) Uani 1 1 d . . . . .
H10 H 0.765850 0.299752 0.493991 0.031 Uiso 1 1 calc R U . . .
O9 O -0.35145(12) 0.77594(10) 0.19058(9) 0.0206(3) Uani 1 1 d . . . . .
H9 H -0.373238 0.781166 0.134235 0.031 Uiso 1 1 calc R U . . .
O11 O 1.26974(12) 0.96132(9) 0.72307(9) 0.0215(3) Uani 1 1 d . . . . .
H11 H 1.306054 0.915408 0.708509 0.032 Uiso 1 1 calc R U . . .
O12 O 0.38005(13) 0.80551(9) 0.69593(9) 0.0192(3) Uani 1 1 d G . . . .
H12A H 0.438781 0.799298 0.746161 0.029 Uiso 1 1 d G U . . .
H12B H 0.329800 0.759667 0.692044 0.029 Uiso 1 1 d G U . . .
C1 C 0.20599(17) 0.79234(11) 0.33633(11) 0.0130(3) Uani 1 1 d . . . . .
C16 C 0.85816(17) 0.95883(11) 0.60665(11) 0.0137(3) Uani 1 1 d . . . . .
C2 C 0.06111(17) 0.77827(12) 0.29615(12) 0.0145(3) Uani 1 1 d . . . . .
C8 C 0.57313(16) 0.68010(12) 0.44230(11) 0.0134(3) Uani 1 1 d . . . . .
C9 C 0.63044(17) 0.58910(12) 0.44793(11) 0.0143(3) Uani 1 1 d . . . . .
C12 C 0.72729(18) 0.41368(12) 0.45177(12) 0.0164(3) Uani 1 1 d . . . . .
C5 C -0.21517(17) 0.77362(12) 0.22233(12) 0.0168(3) Uani 1 1 d . . . . .
C21 C 0.94288(18) 0.91905(12) 0.56122(12) 0.0168(3) Uani 1 1 d . . . . .
H21 H 0.906071 0.892007 0.504029 0.020 Uiso 1 1 calc R U . . .
C10 C 0.65676(17) 0.53834(12) 0.52716(12) 0.0158(3) Uani 1 1 d . . . . .
H10A H 0.641366 0.563809 0.579901 0.019 Uiso 1 1 calc R U . . .
C20 C 1.08068(18) 0.91885(13) 0.59927(13) 0.0182(4) Uani 1 1 d . . . . .
H20 H 1.138354 0.892131 0.568213 0.022 Uiso 1 1 calc R U . . .
C15 C 0.71079(17) 0.96045(11) 0.56523(11) 0.0132(3) Uani 1 1 d . . . . .
C14 C 0.65543(19) 0.55088(12) 0.37114(12) 0.0183(4) Uani 1 1 d . . . . .
H14 H 0.639111 0.585073 0.317232 0.022 Uiso 1 1 calc R U . . .
C3 C -0.02374(18) 0.76649(13) 0.35173(12) 0.0188(4) Uani 1 1 d . . . . .
H3 H 0.013215 0.759858 0.414898 0.023 Uiso 1 1 calc R U . . .
C6 C -0.13098(18) 0.78142(13) 0.16599(12) 0.0171(3) Uani 1 1 d . . . . .
H6 H -0.167752 0.784497 0.102521 0.021 Uiso 1 1 calc R U . . .
C7 C 0.00642(18) 0.78465(12) 0.20311(12) 0.0163(3) Uani 1 1 d . . . . .
H7 H 0.063869 0.791260 0.164995 0.020 Uiso 1 1 calc R U . . .
C17 C 0.91294(18) 0.99693(12) 0.69133(12) 0.0175(3) Uani 1 1 d . . . . .
H17 H 0.855673 1.023470 0.722804 0.021 Uiso 1 1 calc R U . . .
C11 C 0.70504(18) 0.45131(12) 0.52949(12) 0.0166(3) Uani 1 1 d . . . . .
H11A H 0.722944 0.417365 0.583612 0.020 Uiso 1 1 calc R U . . .
C19 C 1.13342(17) 0.95815(12) 0.68333(13) 0.0166(3) Uani 1 1 d . . . . .
C13 C 0.70353(19) 0.46409(13) 0.37275(12) 0.0196(4) Uani 1 1 d . . . . .
H13 H 0.720314 0.438907 0.320309 0.023 Uiso 1 1 calc R U . . .
C18 C 1.05026(18) 0.99634(13) 0.72986(13) 0.0197(4) Uani 1 1 d . . . . .
H18 H 1.087149 1.021934 0.787742 0.024 Uiso 1 1 calc R U . . .
C4 C -0.16135(18) 0.76444(14) 0.31519(12) 0.0203(4) Uani 1 1 d . . . . .
H4 H -0.218837 0.756826 0.353157 0.024 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
Y001 O2 2.4064(12) . ?
Y001 O3 2.4471(12) . ?
Y001 O4 2.3533(12) . ?
Y001 O6 2.3007(12) 3_676 ?
Y001 O5 2.2832(12) . ?
Y001 O1 2.3669(12) . ?
Y001 O8 2.3184(12) . ?
Y001 O7 2.3781(12) . ?
O2 C1 1.269(2) . ?
O3 C8 1.273(2) . ?
O4 C8 1.280(2) . ?
O6 C15 1.285(2) . ?
O5 C15 1.257(2) . ?
O1 C1 1.283(2) . ?
O8 H8A 0.8540 . ?
O8 H8B 0.8540 . ?
O7 H7A 0.8518 . ?
O7 H7B 0.8518 . ?
O10 H10 0.8400 . ?
O10 C12 1.360(2) . ?
O9 H9 0.8400 . ?
O9 C5 1.364(2) . ?
O11 H11 0.8400 . ?
O11 C19 1.380(2) . ?
O12 H12A 0.8499 . ?
O12 H12B 0.8507 . ?
C1 C2 1.476(2) . ?
C16 C21 1.397(2) . ?
C16 C15 1.487(2) . ?
C16 C17 1.395(2) . ?
C2 C3 1.398(2) . ?
C2 C7 1.395(2) . ?
C8 C9 1.472(2) . ?
C9 C10 1.399(2) . ?
C9 C14 1.401(2) . ?
C12 C11 1.399(3) . ?
C12 C13 1.395(3) . ?
C5 C6 1.395(2) . ?
C5 C4 1.395(3) . ?
C21 H21 0.9500 . ?
C21 C20 1.389(2) . ?
C10 H10A 0.9500 . ?
C10 C11 1.386(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.391(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.383(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(2) . ?
C7 H7 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.386(3) . ?
C11 H11A 0.9500 . ?
C19 C18 1.386(3) . ?
C13 H13 0.9500 . ?
C18 H18 0.9500 . ?
C4 H4 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
O2 Y001 O3 115.29(4) . . ?
O4 Y001 O2 78.74(4) . . ?
O4 Y001 O3 54.10(4) . . ?
O4 Y001 O1 90.53(4) . . ?
O4 Y001 O7 74.36(4) . . ?
O6 Y001 O2 80.11(4) 3_676 . ?
O6 Y001 O3 154.19(4) 3_676 . ?
O6 Y001 O4 151.56(4) 3_676 . ?
O6 Y001 O1 92.57(4) 3_676 . ?
O6 Y001 O8 76.56(4) 3_676 . ?
O6 Y001 O7 83.21(4) 3_676 . ?
O5 Y001 O2 154.71(4) . . ?
O5 Y001 O3 82.07(4) . . ?
O5 Y001 O4 99.76(4) . . ?
O5 Y001 O6 91.39(4) . 3_676 ?
O5 Y001 O1 150.25(4) . . ?
O5 Y001 O8 77.03(4) . . ?
O5 Y001 O7 76.08(4) . . ?
O1 Y001 O2 54.66(4) . . ?
O1 Y001 O3 81.63(4) . . ?
O1 Y001 O7 133.67(4) . . ?
O8 Y001 O2 123.04(4) . . ?
O8 Y001 O3 77.65(4) . . ?
O8 Y001 O4 131.35(4) . . ?
O8 Y001 O1 75.27(4) . . ?
O8 Y001 O7 145.71(5) . . ?
O7 Y001 O2 79.28(4) . . ?
O7 Y001 O3 118.81(4) . . ?
C1 O2 Y001 92.35(10) . . ?
C8 O3 Y001 92.04(10) . . ?
C8 O4 Y001 96.23(10) . . ?
C15 O6 Y001 136.29(11) . 3_676 ?
C15 O5 Y001 138.48(11) . . ?
C1 O1 Y001 93.80(10) . . ?
Y001 O8 H8A 109.6 . . ?
Y001 O8 H8B 109.6 . . ?
H8A O8 H8B 104.3 . . ?
Y001 O7 H7A 109.5 . . ?
Y001 O7 H7B 109.5 . . ?
H7A O7 H7B 104.4 . . ?
C12 O10 H10 109.5 . . ?
C5 O9 H9 109.5 . . ?
C19 O11 H11 109.5 . . ?
H12A O12 H12B 104.5 . . ?
O2 C1 O1 118.33(15) . . ?
O2 C1 C2 120.73(15) . . ?
O1 C1 C2 120.81(15) . . ?
C21 C16 C15 120.34(15) . . ?
C17 C16 C21 119.43(16) . . ?
C17 C16 C15 120.24(15) . . ?
C3 C2 C1 119.99(16) . . ?
C7 C2 C1 120.24(16) . . ?
C7 C2 C3 119.52(16) . . ?
O3 C8 O4 117.63(16) . . ?
O3 C8 C9 122.66(15) . . ?
O4 C8 C9 119.71(15) . . ?
C10 C9 C8 121.84(16) . . ?
C10 C9 C14 118.88(16) . . ?
C14 C9 C8 119.25(15) . . ?
O10 C12 C11 123.12(16) . . ?
O10 C12 C13 116.69(16) . . ?
C13 C12 C11 120.19(17) . . ?
O9 C5 C6 122.53(16) . . ?
O9 C5 C4 117.12(16) . . ?
C4 C5 C6 120.35(16) . . ?
C16 C21 H21 119.8 . . ?
C20 C21 C16 120.32(17) . . ?
C20 C21 H21 119.8 . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 C9 120.67(16) . . ?
C11 C10 H10A 119.7 . . ?
C21 C20 H20 120.3 . . ?
C21 C20 C19 119.35(17) . . ?
C19 C20 H20 120.3 . . ?
O6 C15 C16 118.52(15) . . ?
O5 C15 O6 122.78(15) . . ?
O5 C15 C16 118.69(15) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.89(17) . . ?
C13 C14 H14 119.6 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.33(17) . . ?
C4 C3 H3 119.8 . . ?
C5 C6 H6 120.2 . . ?
C7 C6 C5 119.61(16) . . ?
C7 C6 H6 120.2 . . ?
C2 C7 H7 119.8 . . ?
C6 C7 C2 120.44(17) . . ?
C6 C7 H7 119.8 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.47(17) . . ?
C18 C17 H17 119.8 . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 C12 119.69(16) . . ?
C10 C11 H11A 120.2 . . ?
O11 C19 C20 121.51(17) . . ?
O11 C19 C18 117.59(16) . . ?
C18 C19 C20 120.90(16) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.66(17) . . ?
C14 C13 H13 120.2 . . ?
C17 C18 C19 119.52(17) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C5 C4 H4 120.2 . . ?
C3 C4 C5 119.65(16) . . ?
C3 C4 H4 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y001 O2 C1 O1 -9.18(16) . . . . ?
Y001 O2 C1 C2 166.69(14) . . . . ?
Y001 O3 C8 O4 0.57(15) . . . . ?
Y001 O3 C8 C9 -179.82(14) . . . . ?
Y001 O4 C8 O3 -0.59(16) . . . . ?
Y001 O4 C8 C9 179.78(13) . . . . ?
Y001 O6 C15 O5 -81.0(2) 3_676 . . . ?
Y001 O6 C15 C16 99.69(18) 3_676 . . . ?
Y001 O5 C15 O6 -21.1(3) . . . . ?
Y001 O5 C15 C16 158.22(12) . . . . ?
Y001 O1 C1 O2 9.35(16) . . . . ?
Y001 O1 C1 C2 -166.52(14) . . . . ?
O2 C1 C2 C3 -165.28(16) . . . . ?
O2 C1 C2 C7 9.0(3) . . . . ?
O3 C8 C9 C10 7.4(3) . . . . ?
O3 C8 C9 C14 -174.74(16) . . . . ?
O4 C8 C9 C10 -173.03(16) . . . . ?
O4 C8 C9 C14 4.9(2) . . . . ?
O1 C1 C2 C3 10.5(3) . . . . ?
O1 C1 C2 C7 -175.26(16) . . . . ?
O10 C12 C11 C10 -178.73(17) . . . . ?
O10 C12 C13 C14 178.77(17) . . . . ?
O9 C5 C6 C7 175.64(17) . . . . ?
O9 C5 C4 C3 -176.58(18) . . . . ?
O11 C19 C18 C17 178.18(17) . . . . ?
C1 C2 C3 C4 171.94(18) . . . . ?
C1 C2 C7 C6 -172.82(16) . . . . ?
C16 C21 C20 C19 0.4(3) . . . . ?
C16 C17 C18 C19 0.5(3) . . . . ?
C2 C3 C4 C5 0.4(3) . . . . ?
C8 C9 C10 C11 177.06(16) . . . . ?
C8 C9 C14 C13 -177.07(17) . . . . ?
C9 C10 C11 C12 -0.2(3) . . . . ?
C9 C14 C13 C12 0.1(3) . . . . ?
C5 C6 C7 C2 1.3(3) . . . . ?
C21 C16 C15 O6 -170.60(16) . . . . ?
C21 C16 C15 O5 10.1(2) . . . . ?
C21 C16 C17 C18 0.7(3) . . . . ?
C21 C20 C19 O11 -178.61(16) . . . . ?
C21 C20 C19 C18 0.8(3) . . . . ?
C10 C9 C14 C13 0.9(3) . . . . ?
C20 C19 C18 C17 -1.3(3) . . . . ?
C15 C16 C21 C20 178.94(16) . . . . ?
C15 C16 C17 C18 -179.40(17) . . . . ?
C14 C9 C10 C11 -0.8(3) . . . . ?
C3 C2 C7 C6 1.5(3) . . . . ?
C6 C5 C4 C3 2.4(3) . . . . ?
C7 C2 C3 C4 -2.3(3) . . . . ?
C17 C16 C21 C20 -1.2(3) . . . . ?
C17 C16 C15 O6 9.5(2) . . . . ?
C17 C16 C15 O5 -169.84(16) . . . . ?
C11 C12 C13 C14 -1.2(3) . . . . ?
C13 C12 C11 C10 1.3(3) . . . . ?
C4 C5 C6 C7 -3.3(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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.806
####################################################################### 
# 
# 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_jo289_a2
_database_code_depnum_ccdc_archive 'CCDC 2269128'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H15 O9 Y, H2 O'
_chemical_formula_sum            'C21 H17 O10 Y'
_chemical_formula_weight         518.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Y C H O'
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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.29940(10)
_cell_length_b                   12.1464(2)
_cell_length_c                   17.0480(3)
_cell_angle_alpha                92.421(2)
_cell_angle_beta                 97.081(2)
_cell_angle_gamma                101.336(2)
_cell_volume                     1065.25(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11330
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.5600
_cell_measurement_theta_min      3.7080
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.354
_exptl_absorpt_coefficient_mu    4.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.160
_diffrn_reflns_theta_min         3.720
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     33.00 104.00   0.50    0.05    --   47.64  57.00 150.00  142
  2  ω     95.00 178.00   0.50    0.05    --  107.11  45.00   0.00  166
  3  ω     94.00 178.00   0.50    0.05    --  107.11  15.00 -30.00  168
  4  ω     25.00 120.00   0.50    0.05    --   47.64  77.00-120.00  190
  5  ω    -60.00  28.00   0.50    0.05    --  -47.64  19.00 -30.00  176
  6  ω    -68.00 -11.00   0.50    0.05    --  -86.25  30.00  60.00  114
  7  ω    -78.00 -14.00   0.50    0.05    --  -86.25  45.00-180.00  128
  8  ω     41.00 102.00   0.50    0.05    --   47.64-137.00 -58.00  122
  9  ω     35.00 112.00   0.50    0.05    --  107.11-125.00-150.00  154
 10  ω     41.00 121.00   0.50    0.05    --  107.11-137.00 -58.00  160
 11  ω     35.00 109.00   0.50    0.05    --  107.11-113.00 -25.99  148
 12  ω     35.00 106.00   0.50    0.05    --  107.11 -98.00  28.62  142
 13  ω     39.00 117.00   0.50    0.05    --  107.11-133.00 118.00  156
 14  ω     35.00 106.00   0.50    0.05    --  107.11 -94.00 150.00  142
 15  ω     39.00 100.00   0.50    0.05    --   47.64-133.00 118.00  122
 16  ω     35.00 106.00   0.50    0.05    --  107.11 -94.00  30.00  142
 17  ω     35.00 106.00   0.50    0.05    --  107.11 -94.00 -90.00  142
 18  ω     35.00 106.00   0.50    0.05    --  107.11 -94.00-180.00  142
 19  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00  60.00   68
 20  ω     36.00  76.00   0.50    0.05    --  107.11 -45.00  90.00   80
 21  ω     36.00  76.00   0.50    0.05    --  107.11 -45.00 150.00   80
 22  ω    -24.00  63.00   0.50    0.05    --   47.64 -57.00 120.00  174
 23  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00  30.00   68
 24  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00 150.00   68
 25  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00   0.00   68
 26  ω    -25.00  61.00   0.50    0.05    --   47.64 -38.00-120.00  172
 27  ω     32.00  66.00   0.50    0.05    --  107.11 -30.00-150.00   68
 28  ω     36.00  76.00   0.50    0.05    --  107.11 -45.00 -90.00   80
 29  ω     87.00 178.00   0.50    0.05    --  107.11 137.00   4.00  182
 30  ω     95.00 178.00   0.50    0.05    --  107.11 125.00-150.00  166
 31  ω     90.00 178.00   0.50    0.05    --  107.11 133.00-172.00  176
 32  ω    -92.00 -17.00   0.50    0.05    --  -86.25 133.00-172.00  150
 33  ω    -91.00 -17.00   0.50    0.05    --  -47.64 133.00-172.00  148
 34  ω    -95.00 -19.00   0.50    0.05    --  -47.64 137.00   4.00  152
 35  ω    -95.00 -19.00   0.50    0.05    --  -86.25 137.00   4.00  152
 36  ω   -120.00 -73.00   0.50    0.05    --  -47.64-125.00-120.00   94
 37  ω   -120.00 -66.00   0.50    0.05    --  -47.64-137.00 -58.00  108
 38  ω   -159.00 -66.00   0.50    0.05    --  -86.25-137.00 -58.00  186
 39  ω   -120.00 -68.00   0.50    0.05    --  -47.64-133.00 118.00  104
 40  ω   -159.00 -68.00   0.50    0.05    --  -86.25-133.00 118.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0843759000
_diffrn_orient_matrix_UB_12      -0.0654360000
_diffrn_orient_matrix_UB_13      -0.0814415000
_diffrn_orient_matrix_UB_21      -0.0848377000
_diffrn_orient_matrix_UB_22      -0.1090874000
_diffrn_orient_matrix_UB_23      0.0411961000
_diffrn_orient_matrix_UB_31      -0.2742333000
_diffrn_orient_matrix_UB_32      0.0250932000
_diffrn_orient_matrix_UB_33      -0.0010629000
_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                4115
_reflns_number_total             4365
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.115
_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     295
_refine_ls_number_reflns         4365
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0386
_refine_ls_restrained_S_all      1.093
_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)+(0.0761P)²+0.1001P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1076
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Free rotating group:
 O10(H10A,H10B)
1.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C21(H21), C20(H20), C10(H10), C17(H17), C13(H13), C3(H3A),
  C18(H18), C7(H7), C6(H6A), C4(H4)
1.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O3(H3), O9(H9)
;
_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
Y1 Y 0.07173(3) 0.37684(2) 0.43314(2) 0.01338(11) Uani 1 1 d . . . . .
O5 O -0.2777(3) 0.27021(15) 0.46748(11) 0.0181(4) Uani 1 1 d . . . . .
O8 O 0.8372(3) 0.52626(14) 0.44148(10) 0.0149(3) Uani 1 1 d . . . . .
O4 O -0.6730(3) 0.27243(14) 0.49745(11) 0.0177(4) Uani 1 1 d . . . . .
O2 O -0.1544(4) 0.37873(15) 0.30906(11) 0.0226(4) Uani 1 1 d . . . . .
O7 O 0.4158(3) 0.49145(14) 0.39527(11) 0.0167(4) Uani 1 1 d . . . . .
O1 O 0.0788(3) 0.24927(15) 0.32197(11) 0.0198(4) Uani 1 1 d . . . . .
O6 O -0.3974(4) -0.11009(15) 0.71259(11) 0.0217(4) Uani 1 1 d . . . . .
H6 H -0.285962 -0.146960 0.701970 0.033 Uiso 1 1 calc R U . . .
O3 O -0.4848(4) 0.13598(19) -0.03457(12) 0.0327(5) Uani 1 1 d . . . . .
H3 H -0.580859 0.177097 -0.055482 0.049 Uiso 1 1 calc R U . . .
O9 O 0.8487(4) 0.79202(18) 0.12824(13) 0.0316(5) Uani 1 1 d . . . . .
H9 H 0.981730 0.843052 0.140415 0.047 Uiso 1 1 calc R U . . .
O10 O 0.2417(4) 0.96264(18) 0.14219(14) 0.0341(5) Uani 1 1 d G . . . .
H10A H 0.349135 0.958256 0.109642 0.051 Uiso 1 1 d G U . . .
H10B H 0.322453 1.013548 0.177151 0.051 Uiso 1 1 d G U . . .
C9 C -0.4402(5) 0.1459(2) 0.56097(15) 0.0164(5) Uani 1 1 d . . . . .
C15 C 0.6450(5) 0.53480(19) 0.38875(15) 0.0152(5) Uani 1 1 d . . . . .
C11 C -0.2379(5) -0.0065(2) 0.60455(15) 0.0173(5) Uani 1 1 d . . . . .
H11 H -0.112663 -0.051689 0.599569 0.021 Uiso 1 1 calc R U . . .
C14 C -0.6069(4) 0.1242(2) 0.61839(15) 0.0180(5) Uani 1 1 d . . . . .
H14 H -0.734151 0.168571 0.622679 0.022 Uiso 1 1 calc R U . . .
C21 C 0.9464(5) 0.6668(2) 0.31822(15) 0.0181(5) Uani 1 1 d . . . . .
H21 H 1.079839 0.667159 0.360969 0.022 Uiso 1 1 calc R U . . .
C8 C -0.4646(5) 0.2354(2) 0.50543(15) 0.0159(5) Uani 1 1 d . . . . .
C20 C 0.9976(5) 0.7328(2) 0.25520(15) 0.0191(5) Uani 1 1 d . . . . .
H20 H 1.163820 0.779658 0.255362 0.023 Uiso 1 1 calc R U . . .
C12 C -0.4055(5) -0.0274(2) 0.66107(15) 0.0171(5) Uani 1 1 d . . . . .
C10 C -0.2536(4) 0.0803(2) 0.55556(15) 0.0167(5) Uani 1 1 d . . . . .
H10 H -0.135904 0.095565 0.517742 0.020 Uiso 1 1 calc R U . . .
C1 C -0.0796(5) 0.2964(2) 0.27877(16) 0.0186(5) Uani 1 1 d . . . . .
C17 C 0.5088(5) 0.5975(2) 0.25534(16) 0.0198(5) Uani 1 1 d . . . . .
H17 H 0.341008 0.552241 0.255685 0.024 Uiso 1 1 calc R U . . .
C16 C 0.7014(5) 0.60012(19) 0.31927(15) 0.0151(5) Uani 1 1 d . . . . .
C2 C -0.1776(5) 0.2567(2) 0.19549(16) 0.0196(5) Uani 1 1 d . . . . .
C13 C -0.5898(5) 0.0395(2) 0.66897(17) 0.0200(5) Uani 1 1 d . . . . .
H13 H -0.701308 0.026661 0.708645 0.024 Uiso 1 1 calc R U . . .
C3 C -0.3682(6) 0.3041(2) 0.15425(17) 0.0262(6) Uani 1 1 d . . . . .
H3A H -0.427481 0.363687 0.179388 0.031 Uiso 1 1 calc R U . . .
C19 C 0.8048(5) 0.7296(2) 0.19235(17) 0.0222(5) Uani 1 1 d . . . . .
C18 C 0.5610(5) 0.6607(2) 0.19120(17) 0.0241(5) Uani 1 1 d . . . . .
H18 H 0.431368 0.657093 0.146855 0.029 Uiso 1 1 calc R U . . .
C7 C -0.0908(5) 0.1702(2) 0.15718(17) 0.0253(6) Uani 1 1 d . . . . .
H7 H 0.040248 0.137301 0.184434 0.030 Uiso 1 1 calc R U . . .
C5 C -0.3845(5) 0.1789(2) 0.04027(16) 0.0242(5) Uani 1 1 d . . . . .
C6 C -0.1925(6) 0.1319(2) 0.08044(18) 0.0288(6) Uani 1 1 d . . . . .
H6A H -0.131017 0.073205 0.054997 0.035 Uiso 1 1 calc R U . . .
C4 C -0.4732(6) 0.2660(2) 0.07721(17) 0.0274(6) Uani 1 1 d . . . . .
H4 H -0.604099 0.298695 0.049776 0.033 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
Y1 O5 2.1992(17) . ?
Y1 O8 2.3445(17) 2_666 ?
Y1 O8 2.4015(16) 1_455 ?
Y1 O4 2.2508(16) 1_655 ?
Y1 O2 2.3024(19) . ?
Y1 O7 2.2468(16) . ?
Y1 O1 2.4056(18) . ?
O5 C8 1.263(3) . ?
O8 C15 1.296(3) . ?
O4 C8 1.266(3) . ?
O2 C1 1.260(3) . ?
O7 C15 1.245(3) . ?
O1 C1 1.283(3) . ?
O6 H6 0.8400 . ?
O6 C12 1.365(3) . ?
O3 H3 0.8400 . ?
O3 C5 1.360(3) . ?
O9 H9 0.8400 . ?
O9 C19 1.374(3) . ?
O10 H10A 0.8499 . ?
O10 H10B 0.8501 . ?
C9 C14 1.397(3) . ?
C9 C8 1.486(3) . ?
C9 C10 1.395(3) . ?
C15 C16 1.482(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.387(4) . ?
C11 C10 1.381(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.379(4) . ?
C21 H21 0.9500 . ?
C21 C20 1.389(3) . ?
C21 C16 1.391(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.380(4) . ?
C12 C13 1.403(3) . ?
C10 H10 0.9500 . ?
C1 C2 1.477(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.393(4) . ?
C17 C18 1.387(4) . ?
C2 C3 1.391(4) . ?
C2 C7 1.396(4) . ?
C13 H13 0.9500 . ?
C3 H3A 0.9500 . ?
C3 C4 1.384(4) . ?
C19 C18 1.392(4) . ?
C18 H18 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.377(4) . ?
C5 C6 1.386(4) . ?
C5 C4 1.396(4) . ?
C6 H6A 0.9500 . ?
C4 H4 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
O5 Y1 O8 90.83(6) . 2_666 ?
O5 Y1 O8 84.97(6) . 1_455 ?
O5 Y1 O4 91.08(6) . 1_655 ?
O5 Y1 O2 88.40(7) . . ?
O5 Y1 O7 177.10(5) . . ?
O5 Y1 O1 92.46(6) . . ?
O8 Y1 O8 68.06(7) 2_666 1_455 ?
O8 Y1 O1 162.59(6) 2_666 . ?
O8 Y1 O1 129.27(6) 1_455 . ?
O4 Y1 O8 79.64(6) 1_655 2_666 ?
O4 Y1 O8 147.36(6) 1_655 1_455 ?
O4 Y1 O2 138.37(6) 1_655 . ?
O4 Y1 O1 83.21(6) 1_655 . ?
O2 Y1 O8 74.02(6) . 1_455 ?
O2 Y1 O8 141.99(6) . 2_666 ?
O2 Y1 O1 55.25(6) . . ?
O7 Y1 O8 89.47(6) . 2_666 ?
O7 Y1 O8 92.47(6) . 1_455 ?
O7 Y1 O4 91.81(6) . 1_655 ?
O7 Y1 O2 89.59(7) . . ?
O7 Y1 O1 88.11(6) . . ?
C8 O5 Y1 160.55(17) . . ?
Y1 O8 Y1 111.94(7) 2_666 1_655 ?
C15 O8 Y1 122.31(14) . 1_655 ?
C15 O8 Y1 124.19(14) . 2_666 ?
C8 O4 Y1 149.83(16) . 1_455 ?
C1 O2 Y1 95.83(16) . . ?
C15 O7 Y1 160.68(16) . . ?
C1 O1 Y1 90.43(15) . . ?
C12 O6 H6 109.5 . . ?
C5 O3 H3 109.5 . . ?
C19 O9 H9 109.5 . . ?
H10A O10 H10B 104.5 . . ?
C14 C9 C8 120.7(2) . . ?
C10 C9 C14 118.8(2) . . ?
C10 C9 C8 120.5(2) . . ?
O8 C15 C16 118.4(2) . . ?
O7 C15 O8 122.2(2) . . ?
O7 C15 C16 119.3(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.8(2) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 C9 121.1(2) . . ?
C13 C14 H14 119.4 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C16 120.6(2) . . ?
C16 C21 H21 119.7 . . ?
O5 C8 O4 122.9(2) . . ?
O5 C8 C9 118.5(2) . . ?
O4 C8 C9 118.6(2) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 C21 119.4(2) . . ?
C19 C20 H20 120.3 . . ?
O6 C12 C11 123.0(2) . . ?
O6 C12 C13 116.6(2) . . ?
C11 C12 C13 120.3(2) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
O2 C1 O1 118.5(2) . . ?
O2 C1 C2 119.3(2) . . ?
O1 C1 C2 122.2(2) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C18 C17 C16 120.3(2) . . ?
C21 C16 C15 120.1(2) . . ?
C21 C16 C17 119.4(2) . . ?
C17 C16 C15 120.5(2) . . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 C7 118.6(3) . . ?
C7 C2 C1 122.0(2) . . ?
C14 C13 C12 119.1(2) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 C2 121.1(2) . . ?
C4 C3 H3A 119.4 . . ?
O9 C19 C20 121.3(2) . . ?
O9 C19 C18 117.9(2) . . ?
C20 C19 C18 120.8(2) . . ?
C17 C18 C19 119.4(3) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C2 C7 H7 119.6 . . ?
C6 C7 C2 120.9(3) . . ?
C6 C7 H7 119.6 . . ?
O3 C5 C6 118.0(2) . . ?
O3 C5 C4 121.9(2) . . ?
C6 C5 C4 120.1(3) . . ?
C7 C6 C5 120.0(3) . . ?
C7 C6 H6A 120.0 . . ?
C5 C6 H6A 120.0 . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?

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 O5 C8 O4 80.3(6) . . . . ?
Y1 O5 C8 C9 -100.7(5) . . . . ?
Y1 O8 C15 O7 91.5(2) 1_655 . . . ?
Y1 O8 C15 O7 -73.1(3) 2_666 . . . ?
Y1 O8 C15 C16 105.8(2) 2_666 . . . ?
Y1 O8 C15 C16 -89.6(2) 1_655 . . . ?
Y1 O4 C8 O5 8.7(5) 1_455 . . . ?
Y1 O4 C8 C9 -170.3(2) 1_455 . . . ?
Y1 O2 C1 O1 -1.3(2) . . . . ?
Y1 O2 C1 C2 178.2(2) . . . . ?
Y1 O7 C15 O8 -22.9(7) . . . . ?
Y1 O7 C15 C16 158.1(4) . . . . ?
Y1 O1 C1 O2 1.2(2) . . . . ?
Y1 O1 C1 C2 -178.3(2) . . . . ?
O8 C15 C16 C21 -11.4(3) . . . . ?
O8 C15 C16 C17 170.1(2) . . . . ?
O2 C1 C2 C3 -5.8(4) . . . . ?
O2 C1 C2 C7 176.2(2) . . . . ?
O7 C15 C16 C21 167.6(2) . . . . ?
O7 C15 C16 C17 -10.9(3) . . . . ?
O1 C1 C2 C3 173.7(2) . . . . ?
O1 C1 C2 C7 -4.3(4) . . . . ?
O6 C12 C13 C14 -179.9(2) . . . . ?
O3 C5 C6 C7 -178.0(3) . . . . ?
O3 C5 C4 C3 178.3(3) . . . . ?
O9 C19 C18 C17 -179.2(2) . . . . ?
C9 C14 C13 C12 -1.5(4) . . . . ?
C11 C12 C13 C14 1.8(4) . . . . ?
C14 C9 C8 O5 163.7(2) . . . . ?
C14 C9 C8 O4 -17.2(4) . . . . ?
C14 C9 C10 C11 1.7(4) . . . . ?
C21 C20 C19 O9 -178.9(2) . . . . ?
C21 C20 C19 C18 -0.4(4) . . . . ?
C8 C9 C14 C13 178.5(2) . . . . ?
C8 C9 C10 C11 -177.0(2) . . . . ?
C20 C21 C16 C15 -176.7(2) . . . . ?
C20 C21 C16 C17 1.8(4) . . . . ?
C20 C19 C18 C17 2.2(4) . . . . ?
C12 C11 C10 C9 -1.4(4) . . . . ?
C10 C9 C14 C13 -0.2(4) . . . . ?
C10 C9 C8 O5 -17.6(4) . . . . ?
C10 C9 C8 O4 161.5(2) . . . . ?
C10 C11 C12 O6 -178.5(2) . . . . ?
C10 C11 C12 C13 -0.4(4) . . . . ?
C1 C2 C3 C4 -177.2(3) . . . . ?
C1 C2 C7 C6 177.5(3) . . . . ?
C16 C21 C20 C19 -1.6(4) . . . . ?
C16 C17 C18 C19 -2.0(4) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C2 C7 C6 C5 -0.3(5) . . . . ?
C3 C2 C7 C6 -0.4(4) . . . . ?
C18 C17 C16 C15 178.6(2) . . . . ?
C18 C17 C16 C21 0.1(4) . . . . ?
C7 C2 C3 C4 0.8(4) . . . . ?
C6 C5 C4 C3 -0.4(4) . . . . ?
C4 C5 C6 C7 0.7(4) . . . . ?

_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 1.558
_oxdiff_exptl_absorpt_empirical_full_min 0.635
####################################################################### 
# 
# 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_p21c_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2269130'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H38 Er2 O22, 2(H2 O)'
_chemical_formula_sum            'C42 H42 Er2 O24'
_chemical_formula_weight         1265.27
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3698(3)
_cell_length_b                   14.8378(5)
_cell_length_c                   15.5102(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.0290(10)
_cell_angle_gamma                90
_cell_volume                     2293.70(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8026
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   0.456
_shelx_estimated_absorpt_T_min   0.214
_exptl_absorpt_coefficient_mu    3.722
_exptl_absorpt_correction_T_max  0.475
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25669
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.936
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4831
_reflns_number_total             5273
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.323
_refine_diff_density_min         -2.352
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.0447(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0325
_refine_ls_restrained_S_all      1.070
_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)+(0.0491P)²+1.4859P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0872
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H12A_$1-H11A
 2.2 with sigma of 0.02
2.a Free rotating group:
 O12(H12A,H12B)
2.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
2.d Tetrahedral OH refined with riding coordinates:
 O9(H9)
2.e Idealised tetrahedral OH refined as rotating group:
 O10(H10), O11(H11A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.46147(2) 0.14780(2) 0.42158(2) 0.01466(9) Uani 1 1 d . . . . .
O3 O 0.5571(2) 0.27836(17) 0.51042(15) 0.0243(5) Uani 1 1 d . . . . .
O6 O 0.6372(2) -0.00852(16) 0.59982(16) 0.0221(5) Uani 1 1 d . . . . .
O4 O 0.5391(3) 0.27846(18) 0.36770(16) 0.0264(5) Uani 1 1 d . . . . .
O1 O 0.2805(2) 0.17802(18) 0.29131(15) 0.0209(5) Uani 1 1 d . . . . .
O5 O 0.6616(2) 0.08558(18) 0.49403(16) 0.0256(5) Uani 1 1 d . . . . .
O7 O 0.5542(3) 0.0984(2) 0.30626(17) 0.0322(6) Uani 1 1 d . . . . .
H7A H 0.595828 0.047851 0.303517 0.048 Uiso 1 1 d R U . . .
H7B H 0.553760 0.126468 0.256784 0.048 Uiso 1 1 d R U . . .
O8 O 0.4323(3) 0.1136(2) 0.56019(17) 0.0290(6) Uani 1 1 d . . . . .
H8A H 0.437087 0.161698 0.591802 0.044 Uiso 1 1 d R U . . .
H8B H 0.498054 0.081234 0.590158 0.044 Uiso 1 1 d R U . . .
O2 O 0.2588(2) 0.21872(18) 0.42155(16) 0.0256(5) Uani 1 1 d . . . . .
O12 O 0.3807(3) 0.3031(2) 0.1953(2) 0.0355(7) Uani 1 1 d G . . . .
H12A H 0.436213 0.296272 0.246665 0.053 Uiso 1 1 d G U . . .
H12B H 0.327745 0.258453 0.189954 0.053 Uiso 1 1 d G U . . .
O10 O 0.7750(3) 0.6703(2) 0.4495(2) 0.0373(7) Uani 1 1 d . . . . .
H10 H 0.767505 0.698595 0.493203 0.056 Uiso 1 1 calc R U . . .
O9 O -0.3482(2) 0.2247(2) 0.19029(18) 0.0433(8) Uani 1 1 d . . . . .
H9 H -0.369095 0.209153 0.137516 0.065 Uiso 1 1 calc R U . . .
C8 C 0.5742(3) 0.3194(2) 0.4427(2) 0.0189(6) Uani 1 1 d . . . . .
C9 C 0.6316(3) 0.4099(2) 0.4482(2) 0.0210(7) Uani 1 1 d . . . . .
C2 C 0.0625(3) 0.2211(2) 0.2971(2) 0.0211(7) Uani 1 1 d . . . . .
C10 C 0.6571(4) 0.4484(3) 0.3729(3) 0.0309(8) Uani 1 1 d . . . . .
H10A H 0.641515 0.415150 0.320159 0.037 Uiso 1 1 calc R U . . .
C16 C 0.8560(3) 0.0424(2) 0.6051(2) 0.0197(7) Uani 1 1 d . . . . .
C14 C 0.6572(4) 0.4612(2) 0.5263(2) 0.0255(7) Uani 1 1 d . . . . .
H14 H 0.641062 0.436584 0.577428 0.031 Uiso 1 1 calc R U . . .
C1 C 0.2074(3) 0.2068(2) 0.3375(2) 0.0187(6) Uani 1 1 d . . . . .
C13 C 0.7059(4) 0.5479(3) 0.5290(2) 0.0274(8) Uani 1 1 d . . . . .
H13 H 0.722674 0.581287 0.581707 0.033 Uiso 1 1 calc R U . . .
C21 C 0.9107(4) 0.0048(3) 0.6896(3) 0.0304(8) Uani 1 1 d . . . . .
H21 H 0.854925 -0.021509 0.720344 0.036 Uiso 1 1 calc R U . . .
C15 C 0.7101(3) 0.0399(2) 0.5639(2) 0.0193(6) Uani 1 1 d . . . . .
C7 C 0.0087(3) 0.2142(3) 0.2051(2) 0.0252(7) Uani 1 1 d . . . . .
H7 H 0.065175 0.206889 0.168289 0.030 Uiso 1 1 calc R U . . .
C12 C 0.7298(4) 0.5850(2) 0.4529(2) 0.0257(7) Uani 1 1 d . . . . .
C17 C 0.9416(3) 0.0811(3) 0.5607(3) 0.0280(8) Uani 1 1 d . . . . .
H17 H 0.905934 0.106634 0.504327 0.034 Uiso 1 1 calc R U . . .
C19 C 1.1305(3) 0.0442(3) 0.6825(3) 0.0316(8) Uani 1 1 d . . . . .
C18 C 1.0782(4) 0.0824(3) 0.5987(3) 0.0330(9) Uani 1 1 d . . . . .
H18 H 1.134651 0.108514 0.568404 0.040 Uiso 1 1 calc R U . . .
C11 C 0.7050(4) 0.5350(3) 0.3752(3) 0.0345(9) Uani 1 1 d . . . . .
H11 H 0.720801 0.559945 0.324012 0.041 Uiso 1 1 calc R U . . .
C3 C -0.0228(3) 0.2332(3) 0.3511(2) 0.0321(9) Uani 1 1 d . . . . .
H3 H 0.012993 0.239729 0.412735 0.039 Uiso 1 1 calc R U . . .
C6 C -0.1282(3) 0.2182(3) 0.1679(2) 0.0279(8) Uani 1 1 d . . . . .
H6 H -0.163716 0.215334 0.105970 0.034 Uiso 1 1 calc R U . . .
C5 C -0.2128(3) 0.2265(3) 0.2224(2) 0.0299(8) Uani 1 1 d . . . . .
C20 C 1.0473(4) 0.0066(3) 0.7275(3) 0.0388(10) Uani 1 1 d . . . . .
H20 H 1.083491 -0.018011 0.784244 0.047 Uiso 1 1 calc R U . . .
C4 C -0.1600(4) 0.2358(3) 0.3145(3) 0.0378(10) Uani 1 1 d . . . . .
H4 H -0.216651 0.243610 0.351082 0.045 Uiso 1 1 calc R U . . .
O11 O 1.2665(3) 0.0412(2) 0.7222(3) 0.0483(9) Uani 1 1 d . . . . .
H11A H 1.301480 0.087073 0.709637 0.072 Uiso 1 1 calc DR 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
Er1 O3 2.425(2) . ?
Er1 O6 2.289(2) 3_656 ?
Er1 O4 2.340(2) . ?
Er1 O1 2.390(2) . ?
Er1 O5 2.266(2) . ?
Er1 O7 2.368(2) . ?
Er1 O8 2.309(2) . ?
Er1 O2 2.350(2) . ?
O3 C8 1.268(4) . ?
O6 C15 1.277(4) . ?
O4 C8 1.272(4) . ?
O1 C1 1.253(4) . ?
O5 C15 1.259(4) . ?
O7 H7A 0.8729 . ?
O7 H7B 0.8719 . ?
O8 H8A 0.8592 . ?
O8 H8B 0.8585 . ?
O2 C1 1.277(4) . ?
O12 H12A 0.8498 . ?
O12 H12B 0.8501 . ?
O10 H10 0.8200 . ?
O10 C12 1.355(4) . ?
O9 H9 0.8200 . ?
O9 C5 1.355(4) . ?
C8 C9 1.462(5) . ?
C9 C10 1.390(5) . ?
C9 C14 1.393(5) . ?
C2 C1 1.475(4) . ?
C2 C7 1.385(5) . ?
C2 C3 1.387(5) . ?
C10 H10A 0.9300 . ?
C10 C11 1.374(6) . ?
C16 C21 1.394(5) . ?
C16 C15 1.471(4) . ?
C16 C17 1.389(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.378(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.386(5) . ?
C21 H21 0.9300 . ?
C21 C20 1.376(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.378(5) . ?
C12 C11 1.378(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.376(5) . ?
C19 C18 1.385(6) . ?
C19 C20 1.370(6) . ?
C19 O11 1.374(4) . ?
C18 H18 0.9300 . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.380(5) . ?
C6 H6 0.9300 . ?
C6 C5 1.381(5) . ?
C5 C4 1.388(5) . ?
C20 H20 0.9300 . ?
C4 H4 0.9300 . ?
O11 H11A 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Er1 O3 154.15(8) 3_656 . ?
O6 Er1 O4 151.66(8) 3_656 . ?
O6 Er1 O1 80.31(9) 3_656 . ?
O6 Er1 O7 82.50(9) 3_656 . ?
O6 Er1 O8 76.62(9) 3_656 . ?
O6 Er1 O2 92.32(9) 3_656 . ?
O4 Er1 O3 54.13(8) . . ?
O4 Er1 O1 79.05(9) . . ?
O4 Er1 O7 74.64(10) . . ?
O4 Er1 O2 91.42(9) . . ?
O1 Er1 O3 115.66(9) . . ?
O5 Er1 O3 82.46(9) . . ?
O5 Er1 O6 90.89(9) . 3_656 ?
O5 Er1 O4 98.99(9) . . ?
O5 Er1 O1 153.33(9) . . ?
O5 Er1 O7 75.01(9) . . ?
O5 Er1 O8 77.67(9) . . ?
O5 Er1 O2 151.53(9) . . ?
O7 Er1 O3 119.25(9) . . ?
O7 Er1 O1 78.89(8) . . ?
O8 Er1 O3 77.56(9) . . ?
O8 Er1 O4 131.37(9) . . ?
O8 Er1 O1 123.66(8) . . ?
O8 Er1 O7 145.11(10) . . ?
O8 Er1 O2 75.61(9) . . ?
O2 Er1 O3 82.41(9) . . ?
O2 Er1 O1 54.72(8) . . ?
O2 Er1 O7 133.45(9) . . ?
C8 O3 Er1 92.35(19) . . ?
C15 O6 Er1 137.7(2) . 3_656 ?
C8 O4 Er1 96.2(2) . . ?
C1 O1 Er1 92.19(19) . . ?
C15 O5 Er1 137.7(2) . . ?
Er1 O7 H7A 127.8 . . ?
Er1 O7 H7B 127.8 . . ?
H7A O7 H7B 104.4 . . ?
Er1 O8 H8A 110.3 . . ?
Er1 O8 H8B 109.8 . . ?
H8A O8 H8B 104.1 . . ?
C1 O2 Er1 93.40(18) . . ?
H12A O12 H12B 104.5 . . ?
C12 O10 H10 109.5 . . ?
C5 O9 H9 109.5 . . ?
O3 C8 O4 117.3(3) . . ?
O3 C8 C9 122.7(3) . . ?
O4 C8 C9 120.0(3) . . ?
C10 C9 C8 119.9(3) . . ?
C10 C9 C14 118.1(3) . . ?
C14 C9 C8 122.0(3) . . ?
C7 C2 C1 120.0(3) . . ?
C7 C2 C3 119.3(3) . . ?
C3 C2 C1 120.4(3) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 C9 120.9(4) . . ?
C11 C10 H10A 119.5 . . ?
C21 C16 C15 120.0(3) . . ?
C17 C16 C21 118.9(3) . . ?
C17 C16 C15 121.1(3) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 C9 121.2(3) . . ?
C13 C14 H14 119.4 . . ?
O1 C1 O2 118.9(3) . . ?
O1 C1 C2 120.8(3) . . ?
O2 C1 C2 120.2(3) . . ?
C14 C13 H13 120.2 . . ?
C14 C13 C12 119.6(3) . . ?
C12 C13 H13 120.2 . . ?
C16 C21 H21 120.1 . . ?
C20 C21 C16 119.8(3) . . ?
C20 C21 H21 120.1 . . ?
O6 C15 C16 119.1(3) . . ?
O5 C15 O6 122.3(3) . . ?
O5 C15 C16 118.6(3) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 C2 120.2(3) . . ?
C6 C7 H7 119.9 . . ?
O10 C12 C13 123.3(3) . . ?
O10 C12 C11 116.8(3) . . ?
C11 C12 C13 119.8(3) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 C16 121.1(4) . . ?
C18 C17 H17 119.5 . . ?
C20 C19 C18 120.5(3) . . ?
C20 C19 O11 118.1(4) . . ?
O11 C19 C18 121.4(4) . . ?
C17 C18 C19 119.1(3) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C7 C6 H6 119.9 . . ?
C7 C6 C5 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
O9 C5 C6 122.9(3) . . ?
O9 C5 C4 117.0(3) . . ?
C6 C5 C4 120.1(3) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 C21 120.6(4) . . ?
C19 C20 H20 119.7 . . ?
C3 C4 C5 119.3(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C19 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Er1 O3 C8 O4 -0.6(3) . . . . ?
Er1 O3 C8 C9 179.5(3) . . . . ?
Er1 O6 C15 O5 80.9(4) 3_656 . . . ?
Er1 O6 C15 C16 -98.9(4) 3_656 . . . ?
Er1 O4 C8 O3 0.7(3) . . . . ?
Er1 O4 C8 C9 -179.4(3) . . . . ?
Er1 O1 C1 O2 8.9(3) . . . . ?
Er1 O1 C1 C2 -167.1(3) . . . . ?
Er1 O5 C15 O6 23.6(5) . . . . ?
Er1 O5 C15 C16 -156.6(2) . . . . ?
Er1 O2 C1 O1 -9.1(3) . . . . ?
Er1 O2 C1 C2 167.0(3) . . . . ?
O3 C8 C9 C10 175.1(3) . . . . ?
O3 C8 C9 C14 -7.6(5) . . . . ?
O4 C8 C9 C10 -4.8(5) . . . . ?
O4 C8 C9 C14 172.5(3) . . . . ?
O10 C12 C11 C10 -179.0(4) . . . . ?
O9 C5 C4 C3 176.7(4) . . . . ?
C8 C9 C10 C11 176.9(4) . . . . ?
C8 C9 C14 C13 -177.2(3) . . . . ?
C9 C10 C11 C12 0.6(7) . . . . ?
C9 C14 C13 C12 0.1(6) . . . . ?
C2 C7 C6 C5 -1.9(6) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C10 C9 C14 C13 0.2(5) . . . . ?
C16 C21 C20 C19 -0.7(7) . . . . ?
C16 C17 C18 C19 0.1(6) . . . . ?
C14 C9 C10 C11 -0.6(6) . . . . ?
C14 C13 C12 O10 178.6(4) . . . . ?
C14 C13 C12 C11 -0.1(6) . . . . ?
C1 C2 C7 C6 173.2(4) . . . . ?
C1 C2 C3 C4 -172.1(4) . . . . ?
C13 C12 C11 C10 -0.2(6) . . . . ?
C21 C16 C15 O6 -10.5(5) . . . . ?
C21 C16 C15 O5 169.7(3) . . . . ?
C21 C16 C17 C18 0.3(6) . . . . ?
C15 C16 C21 C20 179.4(4) . . . . ?
C15 C16 C17 C18 -179.1(3) . . . . ?
C7 C2 C1 O1 -8.5(5) . . . . ?
C7 C2 C1 O2 175.5(3) . . . . ?
C7 C2 C3 C4 1.9(6) . . . . ?
C7 C6 C5 O9 -175.5(4) . . . . ?
C7 C6 C5 C4 3.5(7) . . . . ?
C17 C16 C21 C20 0.0(6) . . . . ?
C17 C16 C15 O6 168.9(3) . . . . ?
C17 C16 C15 O5 -10.9(5) . . . . ?
C18 C19 C20 C21 1.0(7) . . . . ?
C3 C2 C1 O1 165.5(4) . . . . ?
C3 C2 C1 O2 -10.5(5) . . . . ?
C3 C2 C7 C6 -0.8(6) . . . . ?
C6 C5 C4 C3 -2.4(7) . . . . ?
C20 C19 C18 C17 -0.7(6) . . . . ?
O11 C19 C18 C17 177.9(4) . . . . ?
O11 C19 C20 C21 -177.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# 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_p21c_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2269131'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H38 O22 Yb2, 2(H2 O)'
_chemical_formula_sum            'C42 H42 O24 Yb2'
_chemical_formula_weight         1276.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3616(3)
_cell_length_b                   14.8065(5)
_cell_length_c                   15.4569(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.8930(10)
_cell_angle_gamma                90
_cell_volume                     2280.74(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8074
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   0.422
_shelx_estimated_absorpt_T_min   0.189
_exptl_absorpt_coefficient_mu    4.164
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24650
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.941
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3692
_reflns_number_total             4017
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.056
_refine_diff_density_min         -2.819
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0289(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4017
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.046
_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)+(0.0537P)²+1.3749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0874
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Free rotating group:
 O12(H12A,H12B)
1.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
1.c Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
1.d Tetrahedral OH refined with riding coordinates:
 O9(H9)
1.e Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_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
Yb1 Yb 0.46086(2) 0.14735(2) 0.42226(2) 0.01800(13) Uani 1 1 d . . . . .
O3 O 0.5568(3) 0.27703(18) 0.51130(18) 0.0271(7) Uani 1 1 d . . . . .
O6 O 0.6365(3) -0.00864(18) 0.59949(18) 0.0242(6) Uani 1 1 d . . . . .
O4 O 0.5376(3) 0.27675(18) 0.36845(19) 0.0290(7) Uani 1 1 d . . . . .
O1 O 0.2818(3) 0.1769(2) 0.29286(19) 0.0239(6) Uani 1 1 d . . . . .
O5 O 0.6593(3) 0.0865(2) 0.49383(19) 0.0286(7) Uani 1 1 d . . . . .
O7 O 0.5522(3) 0.0976(2) 0.3074(2) 0.0348(8) Uani 1 1 d . . . . .
H7A H 0.598878 0.048819 0.306433 0.052 Uiso 1 1 d R U . . .
H7B H 0.546819 0.123714 0.256227 0.052 Uiso 1 1 d R U . . .
O8 O 0.4310(3) 0.1130(2) 0.5597(2) 0.0308(7) Uani 1 1 d . . . . .
H8A H 0.448224 0.159256 0.594252 0.046 Uiso 1 1 d R U . . .
H8B H 0.489545 0.073846 0.586232 0.046 Uiso 1 1 d R U . . .
O2 O 0.2600(3) 0.2184(2) 0.42268(19) 0.0275(7) Uani 1 1 d . . . . .
O12 O 0.3803(4) 0.3024(2) 0.1943(2) 0.0384(8) Uani 1 1 d G . . . .
H12A H 0.436927 0.294037 0.245041 0.058 Uiso 1 1 d G U . . .
H12B H 0.335948 0.253398 0.183989 0.058 Uiso 1 1 d G U . . .
O10 O 0.7742(4) 0.6695(2) 0.4492(3) 0.0402(9) Uani 1 1 d . . . . .
O9 O -0.3481(3) 0.2255(3) 0.1915(2) 0.0461(9) Uani 1 1 d . . . . .
H9 H -0.368790 0.209837 0.138613 0.069 Uiso 1 1 calc R U . . .
C8 C 0.5731(4) 0.3178(3) 0.4437(3) 0.0215(9) Uani 1 1 d . . . . .
C9 C 0.6306(4) 0.4088(3) 0.4487(3) 0.0233(9) Uani 1 1 d . . . . .
C2 C 0.0637(4) 0.2210(3) 0.2981(3) 0.0238(9) Uani 1 1 d . . . . .
C10 C 0.6558(5) 0.4473(3) 0.3727(3) 0.0337(11) Uani 1 1 d . . . . .
H10A H 0.639698 0.413633 0.320023 0.040 Uiso 1 1 calc R U . . .
C16 C 0.8544(4) 0.0427(2) 0.6042(3) 0.0216(8) Uani 1 1 d . . . . .
C14 C 0.6563(5) 0.4600(3) 0.5260(3) 0.0295(10) Uani 1 1 d . . . . .
H14 H 0.640452 0.435478 0.577580 0.035 Uiso 1 1 calc R U . . .
C1 C 0.2083(4) 0.2064(3) 0.3386(3) 0.0219(9) Uani 1 1 d . . . . .
C13 C 0.7050(5) 0.5468(3) 0.5284(3) 0.0306(10) Uani 1 1 d . . . . .
H13 H 0.721934 0.580380 0.581137 0.037 Uiso 1 1 calc R U . . .
C21 C 0.9097(5) 0.0048(3) 0.6891(3) 0.0349(11) Uani 1 1 d . . . . .
H21 H 0.854216 -0.021634 0.720101 0.042 Uiso 1 1 calc R U . . .
C15 C 0.7097(4) 0.0399(2) 0.5634(3) 0.0230(9) Uani 1 1 d . . . . .
C7 C 0.0087(5) 0.2142(3) 0.2059(3) 0.0284(10) Uani 1 1 d . . . . .
H7 H 0.064751 0.207360 0.168528 0.034 Uiso 1 1 calc R U . . .
C12 C 0.7283(4) 0.5836(3) 0.4525(3) 0.0274(10) Uani 1 1 d . . . . .
C17 C 0.9401(5) 0.0820(3) 0.5603(3) 0.0315(10) Uani 1 1 d . . . . .
H17 H 0.904484 0.108250 0.504183 0.038 Uiso 1 1 calc R U . . .
C19 C 1.1297(5) 0.0450(3) 0.6816(3) 0.0343(11) Uani 1 1 d . . . . .
C18 C 1.0769(5) 0.0830(3) 0.5980(3) 0.0367(11) Uani 1 1 d . . . . .
H18 H 1.133130 0.109061 0.567258 0.044 Uiso 1 1 calc R U . . .
C11 C 0.7038(6) 0.5333(3) 0.3739(3) 0.0384(12) Uani 1 1 d . . . . .
H11 H 0.719842 0.557964 0.322523 0.046 Uiso 1 1 calc R U . . .
C3 C -0.0220(5) 0.2335(3) 0.3526(3) 0.0360(11) Uani 1 1 d . . . . .
H3 H 0.013465 0.239898 0.414441 0.043 Uiso 1 1 calc R U . . .
C6 C -0.1271(5) 0.2175(3) 0.1694(3) 0.0308(10) Uani 1 1 d . . . . .
H6 H -0.162603 0.213390 0.107425 0.037 Uiso 1 1 calc R U . . .
C5 C -0.2121(4) 0.2268(3) 0.2239(3) 0.0327(10) Uani 1 1 d . . . . .
C20 C 1.0467(5) 0.0066(3) 0.7268(3) 0.0413(13) Uani 1 1 d . . . . .
H20 H 1.083172 -0.018429 0.783424 0.050 Uiso 1 1 calc R U . . .
C4 C -0.1583(5) 0.2365(4) 0.3157(3) 0.0409(12) Uani 1 1 d . . . . .
H4 H -0.214687 0.245096 0.352559 0.049 Uiso 1 1 calc R U . . .
H10 H 0.762(7) 0.695(5) 0.492(5) 0.07(2) Uiso 1 1 d . . . . .
O11 O 1.2657(3) 0.0416(2) 0.7213(3) 0.0515(10) Uani 1 1 d . . . . .
H11A H 1.299748 0.089948 0.713855 0.077 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
Yb1 O3 2.412(3) . ?
Yb1 O6 2.272(3) 3_656 ?
Yb1 O4 2.315(3) . ?
Yb1 O1 2.367(3) . ?
Yb1 O5 2.240(3) . ?
Yb1 O7 2.347(3) . ?
Yb1 O8 2.286(3) . ?
Yb1 H8A 2.7030 . ?
Yb1 H8B 2.6988 . ?
Yb1 O2 2.334(3) . ?
O3 C8 1.259(5) . ?
O6 C15 1.279(5) . ?
O4 C8 1.274(5) . ?
O1 C1 1.251(5) . ?
O5 C15 1.263(5) . ?
O7 H7A 0.8713 . ?
O7 H7B 0.8690 . ?
O8 H8A 0.8571 . ?
O8 H8B 0.8574 . ?
O2 C1 1.275(5) . ?
O12 H12A 0.8500 . ?
O12 H12B 0.8500 . ?
O10 C12 1.364(5) . ?
O10 H10 0.80(7) . ?
O9 H9 0.8200 . ?
O9 C5 1.360(6) . ?
C8 C9 1.466(6) . ?
C9 C10 1.393(6) . ?
C9 C14 1.378(6) . ?
C2 C1 1.473(6) . ?
C2 C7 1.387(6) . ?
C2 C3 1.393(6) . ?
C10 H10A 0.9300 . ?
C10 C11 1.365(6) . ?
C16 C21 1.397(6) . ?
C16 C15 1.460(6) . ?
C16 C17 1.384(6) . ?
C14 H14 0.9300 . ?
C14 C13 1.378(6) . ?
C13 H13 0.9300 . ?
C13 C12 1.373(6) . ?
C21 H21 0.9300 . ?
C21 C20 1.380(7) . ?
C7 H7 0.9300 . ?
C7 C6 1.365(7) . ?
C12 C11 1.387(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.377(7) . ?
C19 C18 1.379(7) . ?
C19 C20 1.370(7) . ?
C19 O11 1.376(6) . ?
C18 H18 0.9300 . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.371(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.383(6) . ?
C5 C4 1.383(6) . ?
C20 H20 0.9300 . ?
C4 H4 0.9300 . ?
O11 H11A 0.8200 . ?

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
O3 Yb1 H8A 60.7 . . ?
O3 Yb1 H8B 82.1 . . ?
O6 Yb1 O3 154.25(9) 3_656 . ?
O6 Yb1 O4 151.32(10) 3_656 . ?
O6 Yb1 O1 80.12(10) 3_656 . ?
O6 Yb1 O7 81.90(11) 3_656 . ?
O6 Yb1 O8 76.62(11) 3_656 . ?
O6 Yb1 H8A 93.7 3_656 . ?
O6 Yb1 H8B 72.8 3_656 . ?
O6 Yb1 O2 92.72(10) 3_656 . ?
O4 Yb1 O3 54.39(9) . . ?
O4 Yb1 O1 79.06(11) . . ?
O4 Yb1 O7 74.86(11) . . ?
O4 Yb1 H8A 114.4 . . ?
O4 Yb1 H8B 135.3 . . ?
O4 Yb1 O2 91.29(11) . . ?
O1 Yb1 O3 116.11(10) . . ?
O1 Yb1 H8A 125.5 . . ?
O1 Yb1 H8B 136.7 . . ?
O5 Yb1 O3 81.92(11) . . ?
O5 Yb1 O6 91.12(10) . 3_656 ?
O5 Yb1 O4 98.71(11) . . ?
O5 Yb1 O1 153.23(10) . . ?
O5 Yb1 O7 75.01(11) . . ?
O5 Yb1 O8 77.92(11) . . ?
O5 Yb1 H8A 80.0 . . ?
O5 Yb1 H8B 61.6 . . ?
O5 Yb1 O2 151.48(10) . . ?
O7 Yb1 O3 119.52(11) . . ?
O7 Yb1 O1 78.71(10) . . ?
O7 Yb1 H8A 154.5 . . ?
O7 Yb1 H8B 128.3 . . ?
O8 Yb1 O3 77.68(10) . . ?
O8 Yb1 O4 131.72(10) . . ?
O8 Yb1 O1 123.52(10) . . ?
O8 Yb1 O7 144.86(11) . . ?
O8 Yb1 H8A 17.3 . . ?
O8 Yb1 H8B 17.4 . . ?
O8 Yb1 O2 75.53(11) . . ?
H8A Yb1 H8B 29.0 . . ?
O2 Yb1 O3 82.43(10) . . ?
O2 Yb1 O1 54.95(10) . . ?
O2 Yb1 O7 133.50(10) . . ?
O2 Yb1 H8A 71.6 . . ?
O2 Yb1 H8B 92.8 . . ?
C8 O3 Yb1 92.1(2) . . ?
C15 O6 Yb1 137.4(2) . 3_656 ?
C8 O4 Yb1 96.3(2) . . ?
C1 O1 Yb1 92.5(2) . . ?
C15 O5 Yb1 138.6(3) . . ?
Yb1 O7 H7A 127.9 . . ?
Yb1 O7 H7B 127.6 . . ?
H7A O7 H7B 104.5 . . ?
Yb1 O8 H8A 110.1 . . ?
Yb1 O8 H8B 109.7 . . ?
H8A O8 H8B 104.1 . . ?
C1 O2 Yb1 93.5(2) . . ?
H12A O12 H12B 104.5 . . ?
C12 O10 H10 106(5) . . ?
C5 O9 H9 109.5 . . ?
O3 C8 O4 117.2(4) . . ?
O3 C8 C9 122.8(4) . . ?
O4 C8 C9 119.9(3) . . ?
C10 C9 C8 119.9(4) . . ?
C14 C9 C8 122.1(4) . . ?
C14 C9 C10 118.0(4) . . ?
C7 C2 C1 120.7(4) . . ?
C7 C2 C3 118.7(4) . . ?
C3 C2 C1 120.4(4) . . ?
C9 C10 H10A 119.3 . . ?
C11 C10 C9 121.4(4) . . ?
C11 C10 H10A 119.3 . . ?
C21 C16 C15 120.2(4) . . ?
C17 C16 C21 118.4(4) . . ?
C17 C16 C15 121.4(4) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 C9 121.2(4) . . ?
C13 C14 H14 119.4 . . ?
O1 C1 O2 118.3(4) . . ?
O1 C1 C2 121.1(4) . . ?
O2 C1 C2 120.5(4) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 C14 119.8(4) . . ?
C12 C13 H13 120.1 . . ?
C16 C21 H21 120.0 . . ?
C20 C21 C16 119.9(4) . . ?
C20 C21 H21 120.0 . . ?
O6 C15 C16 119.3(4) . . ?
O5 C15 O6 121.5(4) . . ?
O5 C15 C16 119.3(4) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.6(4) . . ?
C6 C7 H7 119.7 . . ?
O10 C12 C13 123.1(4) . . ?
O10 C12 C11 116.7(4) . . ?
C13 C12 C11 120.1(4) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.4(4) . . ?
C18 C17 H17 119.3 . . ?
C20 C19 C18 120.3(4) . . ?
C20 C19 O11 117.8(4) . . ?
O11 C19 C18 121.8(4) . . ?
C17 C18 C19 119.3(4) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C7 C6 H6 119.7 . . ?
C7 C6 C5 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
O9 C5 C6 122.9(4) . . ?
O9 C5 C4 117.8(4) . . ?
C6 C5 C4 119.3(4) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 C21 120.6(5) . . ?
C19 C20 H20 119.7 . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C19 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Yb1 O3 C8 O4 -0.8(4) . . . . ?
Yb1 O3 C8 C9 179.3(4) . . . . ?
Yb1 O6 C15 O5 82.0(5) 3_656 . . . ?
Yb1 O6 C15 C16 -98.9(4) 3_656 . . . ?
Yb1 O4 C8 O3 0.8(4) . . . . ?
Yb1 O4 C8 C9 -179.3(3) . . . . ?
Yb1 O1 C1 O2 8.6(4) . . . . ?
Yb1 O1 C1 C2 -167.1(3) . . . . ?
Yb1 O5 C15 O6 22.2(6) . . . . ?
Yb1 O5 C15 C16 -156.9(3) . . . . ?
Yb1 O2 C1 O1 -8.7(4) . . . . ?
Yb1 O2 C1 C2 167.0(3) . . . . ?
O3 C8 C9 C10 174.9(4) . . . . ?
O3 C8 C9 C14 -7.7(7) . . . . ?
O4 C8 C9 C10 -5.0(6) . . . . ?
O4 C8 C9 C14 172.5(4) . . . . ?
O10 C12 C11 C10 -179.0(5) . . . . ?
O9 C5 C4 C3 176.6(5) . . . . ?
C8 C9 C10 C11 177.1(5) . . . . ?
C8 C9 C14 C13 -177.2(4) . . . . ?
C9 C10 C11 C12 0.2(8) . . . . ?
C9 C14 C13 C12 0.1(7) . . . . ?
C2 C7 C6 C5 -0.6(7) . . . . ?
C2 C3 C4 C5 0.2(8) . . . . ?
C10 C9 C14 C13 0.3(7) . . . . ?
C16 C21 C20 C19 -0.3(8) . . . . ?
C16 C17 C18 C19 -0.8(7) . . . . ?
C14 C9 C10 C11 -0.4(7) . . . . ?
C14 C13 C12 O10 178.8(5) . . . . ?
C14 C13 C12 C11 -0.4(8) . . . . ?
C1 C2 C7 C6 172.5(4) . . . . ?
C1 C2 C3 C4 -172.3(5) . . . . ?
C13 C12 C11 C10 0.2(8) . . . . ?
C21 C16 C15 O6 -10.3(6) . . . . ?
C21 C16 C15 O5 168.9(4) . . . . ?
C21 C16 C17 C18 1.0(6) . . . . ?
C15 C16 C21 C20 179.2(4) . . . . ?
C15 C16 C17 C18 -178.7(4) . . . . ?
C7 C2 C1 O1 -8.9(6) . . . . ?
C7 C2 C1 O2 175.5(4) . . . . ?
C7 C2 C3 C4 1.8(7) . . . . ?
C7 C6 C5 O9 -176.3(4) . . . . ?
C7 C6 C5 C4 2.6(7) . . . . ?
C17 C16 C21 C20 -0.5(7) . . . . ?
C17 C16 C15 O6 169.4(4) . . . . ?
C17 C16 C15 O5 -11.5(6) . . . . ?
C18 C19 C20 C21 0.5(8) . . . . ?
C3 C2 C1 O1 165.1(4) . . . . ?
C3 C2 C1 O2 -10.5(6) . . . . ?
C3 C2 C7 C6 -1.6(6) . . . . ?
C6 C5 C4 C3 -2.4(8) . . . . ?
C20 C19 C18 C17 0.0(7) . . . . ?
O11 C19 C18 C17 178.0(4) . . . . ?
O11 C19 C20 C21 -177.5(5) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT972_p21c                
;
PROBLEM: Check Calcd Resid. Dens.  0.91Ang From Yb1            -2.76 eA-3  
RESPONSE: These are the ripples (residual density) features that are
very closed to the heavy atom and are typically more pronounced for heavier
atoms, for example element Yb in this case.
;
####################################################################### 
# 
# 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_jo3025_90_a1
_database_code_depnum_ccdc_archive 'CCDC 2269129'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H42 Er2 O24, 10(H2 O)'
_chemical_formula_sum            'C42 H62 Er2 O34'
_chemical_formula_weight         1445.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Er C H O'
_chemical_oxdiff_usercomment     'Colourless block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.8172(2)
_cell_length_b                   11.3109(2)
_cell_length_c                   11.44570(10)
_cell_angle_alpha                90.5310(10)
_cell_angle_beta                 101.7250(10)
_cell_angle_gamma                105.3210(10)
_cell_volume                     1319.51(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    22689
_cell_measurement_temperature    123.01(13)
_cell_measurement_theta_max      31.9920
_cell_measurement_theta_min      3.6490
_shelx_estimated_absorpt_T_max   0.686
_shelx_estimated_absorpt_T_min   0.599
_exptl_absorpt_coefficient_mu    3.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pinkish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             722
_exptl_crystal_preparation       
'Metathesis of 1:3 Er(NO3)3 + NaL in water at 90C for 2h.'
_exptl_crystal_recrystallization_method 'From the reaction mixture.'
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.125
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36333
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.250
_diffrn_reflns_theta_min         3.644
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(13)
_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 0.858
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  43.00   0.50    0.60    --    9.15 -99.00-120.00  132
  2  ω     -6.00  82.00   0.50    0.60    --    9.15  57.00-180.00  176
  3  ω    -66.00  21.00   0.50    0.60    --    9.15 -22.00 -45.00  174
  4  ω    -23.00  43.00   0.50    0.60    --    9.15 -99.00  60.00  132
  5  ω    -66.00 -41.00   0.50    0.60    --    9.15 -19.00  30.00   50
  6  ω    -63.00  24.00   0.50    0.60    --    9.15 -57.00 150.00  174
  7  ω     -3.00  85.00   0.50    0.60    --    9.15  22.00 119.00  176
  8  ω    -21.00  67.00   0.50    0.60    --   -8.84  22.00 119.00  176
  9  ω    -23.00  25.00   0.50    0.60    --   -8.84 -99.00 120.00   96
 10  ω    -23.00  25.00   0.50    0.60    --   -8.84 -99.00   0.00   96
 11  ω    -23.00  25.00   0.50    0.60    --   -8.84 -99.00 -60.00   96
 12  ω    -23.00  25.00   0.50    0.60    --   -8.84 -99.00-150.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0590269000
_diffrn_orient_matrix_UB_12      0.0351540000
_diffrn_orient_matrix_UB_13      -0.0144476000
_diffrn_orient_matrix_UB_21      -0.0274531000
_diffrn_orient_matrix_UB_22      0.0503085000
_diffrn_orient_matrix_UB_23      -0.0108955000
_diffrn_orient_matrix_UB_31      0.0245907000
_diffrn_orient_matrix_UB_32      0.0219031000
_diffrn_orient_matrix_UB_33      0.0607968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7476
_reflns_number_total             8024
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         8024
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0192P)²+0.3824P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0511
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Free rotating group:
 O16(H16A,H16B), O13(H13A,H13B), O15(H15A,H15B), O17(H17A,H17B), O14(H14A,H14B)
1.b Rotating group:
 O11(H11A,H11B), O10(H10A,H10B), O12(H12A,H12B)
1.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C13(H13), C17(H17), C7(H7A), C20(H20), C10(H10), C3(H3), C4(H4),
 C11(H11), C6(H6), C14(H14), C18(H18)
1.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O7(H7), O9(H9)
;
_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
Er1 Er 0.52089(2) 0.39288(2) 0.31645(2) 0.00907(3) Uani 1 1 d . . . . .
O3 O 0.66014(14) 0.51302(13) 0.47646(12) 0.0135(3) Uani 1 1 d . . . . .
O11 O 0.45092(15) 0.57632(13) 0.32066(12) 0.0135(3) Uani 1 1 d . . . . .
H11A H 0.383585 0.570518 0.264352 0.020 Uiso 1 1 d R U . . .
H11B H 0.423127 0.582559 0.384712 0.020 Uiso 1 1 d R U . . .
O2 O 0.71662(14) 0.35126(13) 0.28235(12) 0.0128(3) Uani 1 1 d . . . . .
O4 O 0.65810(14) 0.66731(13) 0.59736(12) 0.0133(3) Uani 1 1 d . . . . .
O5 O 0.44595(15) 0.20807(13) 0.21432(13) 0.0156(3) Uani 1 1 d . . . . .
O10 O 0.56593(15) 0.25783(14) 0.47191(13) 0.0162(3) Uani 1 1 d . . . . .
H10A H 0.620819 0.221697 0.455770 0.024 Uiso 1 1 d R U . . .
H10B H 0.496758 0.199945 0.470839 0.024 Uiso 1 1 d R U . . .
O1 O 0.68040(15) 0.52517(14) 0.22198(13) 0.0155(3) Uani 1 1 d . . . . .
O16 O 0.30242(15) 0.87679(14) 0.81471(13) 0.0157(3) Uani 1 1 d G . . . .
H16A H 0.378656 0.916599 0.807272 0.024 Uiso 1 1 d G U . . .
H16B H 0.277468 0.805088 0.780000 0.024 Uiso 1 1 d G U . . .
O12 O 0.40552(16) 0.41845(14) 0.12317(12) 0.0157(3) Uani 1 1 d . . . . .
H12A H 0.428582 0.379620 0.070711 0.023 Uiso 1 1 d R U . . .
H12B H 0.429365 0.493668 0.107113 0.023 Uiso 1 1 d R U . . .
O8 O 1.23457(14) 0.85779(14) 0.50170(13) 0.0149(3) Uani 1 1 d . . . . .
H8 H 1.257081 0.928972 0.530087 0.022 Uiso 1 1 calc R U . . .
O13 O 0.48887(18) 0.33199(16) 0.94419(14) 0.0224(3) Uani 1 1 d G . . . .
H13A H 0.417836 0.298778 0.894299 0.034 Uiso 1 1 d G U . . .
H13B H 0.533806 0.280485 0.958976 0.034 Uiso 1 1 d G U . . .
O7 O 1.25507(15) 0.60477(15) 0.13409(13) 0.0165(3) Uani 1 1 d . . . . .
H7 H 1.265985 0.670989 0.103505 0.025 Uiso 1 1 calc R U . . .
O6 O 0.44489(15) 0.01140(14) 0.21229(13) 0.0155(3) Uani 1 1 d . . . . .
O15 O 0.33845(18) 0.81698(14) 0.04709(13) 0.0198(3) Uani 1 1 d G . . . .
H15A H 0.325910 0.843488 -0.022380 0.030 Uiso 1 1 d G U . . .
H15B H 0.368739 0.881524 0.093979 0.030 Uiso 1 1 d G U . . .
O9 O -0.16221(15) -0.03644(14) 0.16784(14) 0.0183(3) Uani 1 1 d . . . . .
H9 H -0.189099 0.024766 0.169359 0.027 Uiso 1 1 calc R U . . .
O17 O 0.60282(16) 0.91481(15) 0.40701(13) 0.0188(3) Uani 1 1 d G . . . .
H17A H 0.623332 0.860054 0.369746 0.028 Uiso 1 1 d G U . . .
H17B H 0.550698 0.940691 0.354033 0.028 Uiso 1 1 d G U . . .
C1 C 0.7519(2) 0.45187(18) 0.23246(16) 0.0107(4) Uani 1 1 d . . . . .
O14 O 0.30752(17) 0.22685(15) 0.73496(15) 0.0223(3) Uani 1 1 d G . . . .
H14A H 0.288573 0.294694 0.723200 0.033 Uiso 1 1 d G U . . .
H14B H 0.254774 0.171123 0.761767 0.033 Uiso 1 1 d G U . . .
C8 C 0.7133(2) 0.61766(18) 0.53118(16) 0.0106(4) Uani 1 1 d . . . . .
C5 C 1.1290(2) 0.56528(19) 0.14838(17) 0.0116(4) Uani 1 1 d . . . . .
C2 C 0.8784(2) 0.48442(19) 0.19349(17) 0.0118(4) Uani 1 1 d . . . . .
C15 C 0.3865(2) 0.09535(19) 0.20723(17) 0.0123(4) Uani 1 1 d . . . . .
C9 C 0.84923(19) 0.68453(18) 0.52083(16) 0.0100(4) Uani 1 1 d . . . . .
C19 C -0.0302(2) -0.00147(19) 0.17323(17) 0.0131(4) Uani 1 1 d . . . . .
C21 C 0.1687(2) 0.14233(19) 0.14704(18) 0.0143(4) Uani 1 1 d . . . . .
H21 H 0.211654 0.218354 0.124364 0.017 Uiso 1 1 calc R U . . .
C16 C 0.2406(2) 0.06041(19) 0.19179(17) 0.0123(4) Uani 1 1 d . . . . .
C13 C 1.0333(2) 0.86702(18) 0.55879(17) 0.0118(4) Uani 1 1 d . . . . .
H13 H 1.069559 0.948476 0.588056 0.014 Uiso 1 1 calc R U . . .
C17 C 0.1752(2) -0.05312(19) 0.22611(18) 0.0140(4) Uani 1 1 d . . . . .
H17 H 0.221866 -0.108945 0.254435 0.017 Uiso 1 1 calc R U . . .
C7 C 0.9128(2) 0.59023(19) 0.13204(17) 0.0132(4) Uani 1 1 d . . . . .
H7A H 0.851565 0.633840 0.106346 0.016 Uiso 1 1 calc R U . . .
C12 C 1.1073(2) 0.80461(19) 0.50869(17) 0.0114(4) Uani 1 1 d . . . . .
C20 C 0.0339(2) 0.1113(2) 0.13615(18) 0.0148(4) Uani 1 1 d . . . . .
H20 H -0.013695 0.165309 0.104312 0.018 Uiso 1 1 calc R U . . .
C10 C 0.9247(2) 0.62397(19) 0.46997(16) 0.0112(4) Uani 1 1 d . . . . .
H10 H 0.888471 0.542689 0.440110 0.013 Uiso 1 1 calc R U . . .
C3 C 0.9694(2) 0.41702(18) 0.22739(17) 0.0120(4) Uani 1 1 d . . . . .
H3 H 0.945918 0.344835 0.265630 0.014 Uiso 1 1 calc R U . . .
C4 C 1.0941(2) 0.45649(19) 0.20471(17) 0.0124(4) Uani 1 1 d . . . . .
H4 H 1.154078 0.410824 0.226844 0.015 Uiso 1 1 calc R U . . .
C11 C 1.0529(2) 0.68310(19) 0.46327(17) 0.0127(4) Uani 1 1 d . . . . .
H11 H 1.101864 0.641968 0.428787 0.015 Uiso 1 1 calc R U . . .
C6 C 1.0376(2) 0.63063(19) 0.10911(17) 0.0124(4) Uani 1 1 d . . . . .
H6 H 1.060067 0.700848 0.067823 0.015 Uiso 1 1 calc R U . . .
C14 C 0.9049(2) 0.80684(19) 0.56476(17) 0.0121(4) Uani 1 1 d . . . . .
H14 H 0.855698 0.848426 0.598335 0.015 Uiso 1 1 calc R U . . .
C18 C 0.0403(2) -0.08319(19) 0.21812(18) 0.0151(4) Uani 1 1 d . . . . .
H18 H -0.002646 -0.158143 0.242921 0.018 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
Er1 O3 2.2848(14) . ?
Er1 O11 2.3923(14) . ?
Er1 O2 2.3908(14) . ?
Er1 O4 2.2973(14) 2_666 ?
Er1 O5 2.2511(14) . ?
Er1 O10 2.4142(14) . ?
Er1 O1 2.4103(15) . ?
Er1 O12 2.3697(14) . ?
O3 C8 1.266(2) . ?
O11 H11A 0.8563 . ?
O11 H11B 0.8559 . ?
O2 C1 1.280(2) . ?
O4 C8 1.264(2) . ?
O5 C15 1.261(3) . ?
O10 H10A 0.8515 . ?
O10 H10B 0.8520 . ?
O1 C1 1.266(3) . ?
O16 H16A 0.8504 . ?
O16 H16B 0.8504 . ?
O12 H12A 0.8541 . ?
O12 H12B 0.8546 . ?
O8 H8 0.8200 . ?
O8 C12 1.368(2) . ?
O13 H13A 0.8501 . ?
O13 H13B 0.8499 . ?
O7 H7 0.8200 . ?
O7 C5 1.363(2) . ?
O6 C15 1.268(3) . ?
O15 H15A 0.8501 . ?
O15 H15B 0.8504 . ?
O9 H9 0.8200 . ?
O9 C19 1.366(3) . ?
O17 H17A 0.8491 . ?
O17 H17B 0.8502 . ?
C1 C2 1.480(3) . ?
O14 H14A 0.8502 . ?
O14 H14B 0.8377 . ?
C8 C9 1.494(3) . ?
C5 C4 1.393(3) . ?
C5 C6 1.392(3) . ?
C2 C7 1.397(3) . ?
C2 C3 1.396(3) . ?
C15 C16 1.494(3) . ?
C9 C10 1.399(3) . ?
C9 C14 1.398(3) . ?
C19 C20 1.396(3) . ?
C19 C18 1.386(3) . ?
C21 H21 0.9300 . ?
C21 C16 1.398(3) . ?
C21 C20 1.385(3) . ?
C16 C17 1.395(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.395(3) . ?
C13 C14 1.391(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.391(3) . ?
C7 H7A 0.9300 . ?
C7 C6 1.385(3) . ?
C12 C11 1.393(3) . ?
C20 H20 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.389(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.383(3) . ?
C4 H4 0.9300 . ?
C11 H11 0.9300 . ?
C6 H6 0.9300 . ?
C14 H14 0.9300 . ?
C18 H18 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
O3 Er1 O11 74.68(5) . . ?
O3 Er1 O2 83.63(5) . . ?
O3 Er1 O4 97.12(5) . 2_666 ?
O3 Er1 O10 72.84(5) . . ?
O3 Er1 O1 78.33(5) . . ?
O3 Er1 O12 138.27(5) . . ?
O11 Er1 O10 131.01(5) . . ?
O11 Er1 O1 80.65(5) . . ?
O2 Er1 O11 133.35(5) . . ?
O2 Er1 O10 77.53(5) . . ?
O2 Er1 O1 54.44(5) . . ?
O4 Er1 O11 77.63(5) 2_666 . ?
O4 Er1 O2 146.88(5) 2_666 . ?
O4 Er1 O10 71.21(5) 2_666 . ?
O4 Er1 O1 158.23(5) 2_666 . ?
O4 Er1 O12 97.14(5) 2_666 . ?
O5 Er1 O3 148.16(5) . . ?
O5 Er1 O11 136.43(5) . . ?
O5 Er1 O2 76.91(5) . . ?
O5 Er1 O4 86.24(5) . 2_666 ?
O5 Er1 O10 78.46(5) . . ?
O5 Er1 O1 108.95(5) . . ?
O5 Er1 O12 71.81(5) . . ?
O1 Er1 O10 126.02(5) . . ?
O12 Er1 O11 70.48(5) . . ?
O12 Er1 O2 104.18(5) . . ?
O12 Er1 O10 148.78(5) . . ?
O12 Er1 O1 74.07(5) . . ?
C8 O3 Er1 150.17(13) . . ?
Er1 O11 H11A 109.7 . . ?
Er1 O11 H11B 109.7 . . ?
H11A O11 H11B 104.2 . . ?
C1 O2 Er1 93.43(12) . . ?
C8 O4 Er1 136.81(13) . 2_666 ?
C15 O5 Er1 150.56(13) . . ?
Er1 O10 H10A 109.5 . . ?
Er1 O10 H10B 109.3 . . ?
H10A O10 H10B 104.4 . . ?
C1 O1 Er1 92.89(12) . . ?
H16A O16 H16B 113.0 . . ?
Er1 O12 H12A 109.6 . . ?
Er1 O12 H12B 109.6 . . ?
H12A O12 H12B 104.3 . . ?
C12 O8 H8 109.5 . . ?
H13A O13 H13B 109.5 . . ?
C5 O7 H7 109.5 . . ?
H15A O15 H15B 104.5 . . ?
C19 O9 H9 109.5 . . ?
H17A O17 H17B 104.5 . . ?
O2 C1 C2 119.99(18) . . ?
O1 C1 O2 119.24(18) . . ?
O1 C1 C2 120.69(18) . . ?
H14A O14 H14B 117.8 . . ?
O3 C8 C9 118.92(17) . . ?
O4 C8 O3 123.05(19) . . ?
O4 C8 C9 118.00(18) . . ?
O7 C5 C4 117.54(18) . . ?
O7 C5 C6 121.82(18) . . ?
C6 C5 C4 120.64(19) . . ?
C7 C2 C1 119.93(19) . . ?
C3 C2 C1 120.54(18) . . ?
C3 C2 C7 119.24(19) . . ?
O5 C15 O6 122.9(2) . . ?
O5 C15 C16 117.96(18) . . ?
O6 C15 C16 119.12(18) . . ?
C10 C9 C8 120.21(18) . . ?
C14 C9 C8 121.04(18) . . ?
C14 C9 C10 118.72(19) . . ?
O9 C19 C20 122.66(19) . . ?
O9 C19 C18 117.13(19) . . ?
C18 C19 C20 120.2(2) . . ?
C16 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C16 120.6(2) . . ?
C21 C16 C15 120.65(19) . . ?
C17 C16 C15 120.12(18) . . ?
C17 C16 C21 119.2(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C14 C13 C12 119.70(19) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.28(19) . . ?
C18 C17 H17 119.9 . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 C2 120.46(19) . . ?
C6 C7 H7A 119.8 . . ?
O8 C12 C13 122.64(19) . . ?
O8 C12 C11 116.99(18) . . ?
C11 C12 C13 120.37(19) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.66(19) . . ?
C21 C20 H20 120.2 . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.15(19) . . ?
C11 C10 H10 119.4 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.68(19) . . ?
C4 C3 H3 119.7 . . ?
C5 C4 H4 120.3 . . ?
C3 C4 C5 119.37(19) . . ?
C3 C4 H4 120.3 . . ?
C12 C11 H11 120.3 . . ?
C10 C11 C12 119.37(18) . . ?
C10 C11 H11 120.3 . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.47(19) . . ?
C7 C6 H6 120.3 . . ?
C9 C14 H14 119.7 . . ?
C13 C14 C9 120.68(18) . . ?
C13 C14 H14 119.7 . . ?
C19 C18 C17 120.0(2) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?

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
Er1 O3 C8 O4 82.7(3) . . . . ?
Er1 O3 C8 C9 -99.4(3) . . . . ?
Er1 O2 C1 O1 0.28(18) . . . . ?
Er1 O2 C1 C2 177.08(15) . . . . ?
Er1 O4 C8 O3 13.2(3) 2_666 . . . ?
Er1 O4 C8 C9 -164.75(13) 2_666 . . . ?
Er1 O5 C15 O6 -107.3(3) . . . . ?
Er1 O5 C15 C16 72.9(3) . . . . ?
Er1 O1 C1 O2 -0.28(18) . . . . ?
Er1 O1 C1 C2 -177.06(15) . . . . ?
O3 C8 C9 C10 -11.4(3) . . . . ?
O3 C8 C9 C14 170.65(18) . . . . ?
O2 C1 C2 C7 175.81(18) . . . . ?
O2 C1 C2 C3 -10.4(3) . . . . ?
O4 C8 C9 C10 166.68(18) . . . . ?
O4 C8 C9 C14 -11.3(3) . . . . ?
O5 C15 C16 C21 21.1(3) . . . . ?
O5 C15 C16 C17 -156.63(18) . . . . ?
O1 C1 C2 C7 -7.4(3) . . . . ?
O1 C1 C2 C3 166.40(18) . . . . ?
O8 C12 C11 C10 178.90(17) . . . . ?
O7 C5 C4 C3 176.17(18) . . . . ?
O7 C5 C6 C7 -176.27(18) . . . . ?
O6 C15 C16 C21 -158.75(18) . . . . ?
O6 C15 C16 C17 23.6(3) . . . . ?
O9 C19 C20 C21 178.29(19) . . . . ?
O9 C19 C18 C17 -179.94(18) . . . . ?
C1 C2 C7 C6 171.37(18) . . . . ?
C1 C2 C3 C4 -171.45(18) . . . . ?
C8 C9 C10 C11 -177.72(17) . . . . ?
C8 C9 C14 C13 177.58(17) . . . . ?
C2 C7 C6 C5 -0.3(3) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
C15 C16 C17 C18 176.39(18) . . . . ?
C9 C10 C11 C12 0.4(3) . . . . ?
C21 C16 C17 C18 -1.3(3) . . . . ?
C16 C21 C20 C19 1.7(3) . . . . ?
C16 C17 C18 C19 1.6(3) . . . . ?
C13 C12 C11 C10 -1.0(3) . . . . ?
C7 C2 C3 C4 2.4(3) . . . . ?
C12 C13 C14 C9 -0.2(3) . . . . ?
C20 C19 C18 C17 -0.2(3) . . . . ?
C20 C21 C16 C15 -178.03(18) . . . . ?
C20 C21 C16 C17 -0.3(3) . . . . ?
C10 C9 C14 C13 -0.4(3) . . . . ?
C3 C2 C7 C6 -2.5(3) . . . . ?
C4 C5 C6 C7 3.4(3) . . . . ?
C6 C5 C4 C3 -3.5(3) . . . . ?
C14 C9 C10 C11 0.3(3) . . . . ?
C14 C13 C12 O8 -179.01(18) . . . . ?
C14 C13 C12 C11 0.9(3) . . . . ?
C18 C19 C20 C21 -1.5(3) . . . . ?

# end Validation Reply Form
_olex2_exptl_crystal_mounting_method 'Thick hydrocarbon oil'
_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 2.145
_oxdiff_exptl_absorpt_empirical_full_min 0.710
# start Validation Reply Form
_vrf_PLAT910_jo3025_90_a1        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: Low-angle reflections rejected because of beam stop and
high background scattering.
;
####################################################################### 
# 
# 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_p21c_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2269132'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H38 Lu2 O22, 2(H2 O)'
_chemical_formula_sum            'C42 H42 Lu2 O24'
_chemical_formula_weight         1280.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3683(3)
_cell_length_b                   14.8139(5)
_cell_length_c                   15.4882(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.9210(10)
_cell_angle_gamma                90
_cell_volume                     2287.66(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8020
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   0.407
_shelx_estimated_absorpt_T_min   0.179
_exptl_absorpt_coefficient_mu    4.379
_exptl_absorpt_correction_T_max  0.335
_exptl_absorpt_correction_T_min  0.141
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36496
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.939
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4786
_reflns_number_total             5243
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.338
_refine_diff_density_min         -1.987
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5243
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.057
_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)+(0.0526P)²+1.2274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0844
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
1.b Aromatic/amide H refined with riding coordinates:
 C10(H10A), C14(H14), C13(H13), C21(H21), C7(H7), C17(H17), C18(H18), C11(H11),
  C3(H3), C6(H6), C20(H20), C4(H4)
1.c Tetrahedral OH refined with riding coordinates:
 O9(H9)
1.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.46046(2) 0.14718(2) 0.42257(2) 0.01988(8) Uani 1 1 d . . . . .
O3 O 0.5560(2) 0.27660(16) 0.51195(16) 0.0300(5) Uani 1 1 d . . . . .
O6 O 0.6359(2) -0.00889(15) 0.59907(16) 0.0267(5) Uani 1 1 d . . . . .
O4 O 0.5375(3) 0.27613(16) 0.36872(16) 0.0312(5) Uani 1 1 d . . . . .
O1 O 0.2821(2) 0.17643(17) 0.29284(16) 0.0270(5) Uani 1 1 d . . . . .
O5 O 0.6595(2) 0.08675(17) 0.49411(17) 0.0305(5) Uani 1 1 d . . . . .
O7 O 0.5516(3) 0.09733(19) 0.30793(18) 0.0370(6) Uani 1 1 d . . . . .
H7A H 0.596504 0.047945 0.306393 0.055 Uiso 1 1 d R U . . .
H7B H 0.547874 0.124155 0.257344 0.055 Uiso 1 1 d R U . . .
O8 O 0.4306(3) 0.11309(18) 0.55973(17) 0.0331(5) Uani 1 1 d . . . . .
H8A H 0.443142 0.160198 0.593202 0.050 Uiso 1 1 d R U . . .
H8B H 0.491985 0.076429 0.587563 0.050 Uiso 1 1 d R U . . .
O2 O 0.2610(2) 0.21844(17) 0.42310(16) 0.0306(5) Uani 1 1 d . . . . .
O12 O 0.3809(3) 0.3020(2) 0.1946(2) 0.0415(7) Uani 1 1 d . . . . .
O10 O 0.7740(3) 0.6696(2) 0.4489(2) 0.0423(7) Uani 1 1 d . . . . .
O9 O -0.3482(3) 0.2254(2) 0.19235(19) 0.0498(8) Uani 1 1 d . . . . .
H9 H -0.369619 0.209792 0.139519 0.075 Uiso 1 1 calc R U . . .
C8 C 0.5723(3) 0.3171(2) 0.4438(2) 0.0243(6) Uani 1 1 d . . . . .
C9 C 0.6303(3) 0.4086(2) 0.4486(2) 0.0264(7) Uani 1 1 d . . . . .
C2 C 0.0634(3) 0.2209(2) 0.2986(2) 0.0261(7) Uani 1 1 d . . . . .
C10 C 0.6552(4) 0.4467(2) 0.3729(3) 0.0359(8) Uani 1 1 d . . . . .
H10A H 0.638584 0.413090 0.320202 0.043 Uiso 1 1 calc R U . . .
C16 C 0.8546(3) 0.0427(2) 0.6044(2) 0.0257(7) Uani 1 1 d . . . . .
C14 C 0.6566(4) 0.4600(2) 0.5267(2) 0.0308(7) Uani 1 1 d . . . . .
H14 H 0.640913 0.435377 0.578153 0.037 Uiso 1 1 calc R U . . .
C1 C 0.2091(3) 0.2059(2) 0.3389(2) 0.0239(6) Uani 1 1 d . . . . .
C13 C 0.7051(4) 0.5466(2) 0.5293(3) 0.0318(8) Uani 1 1 d . . . . .
H13 H 0.722331 0.580043 0.582029 0.038 Uiso 1 1 calc R U . . .
C21 C 0.9098(4) 0.0053(3) 0.6893(3) 0.0360(8) Uani 1 1 d . . . . .
H21 H 0.854102 -0.020616 0.720385 0.043 Uiso 1 1 calc R U . . .
C15 C 0.7081(3) 0.0398(2) 0.5627(2) 0.0246(6) Uani 1 1 d . . . . .
C7 C 0.0093(3) 0.2139(2) 0.2061(2) 0.0311(7) Uani 1 1 d . . . . .
H7 H 0.065689 0.206678 0.169196 0.037 Uiso 1 1 calc R U . . .
C12 C 0.7284(4) 0.5840(2) 0.4526(3) 0.0304(7) Uani 1 1 d . . . . .
C17 C 0.9399(4) 0.0824(2) 0.5598(3) 0.0327(8) Uani 1 1 d . . . . .
H17 H 0.904096 0.108539 0.503685 0.039 Uiso 1 1 calc R U . . .
C19 C 1.1295(4) 0.0449(2) 0.6814(3) 0.0375(9) Uani 1 1 d . . . . .
C18 C 1.0767(4) 0.0835(3) 0.5978(3) 0.0377(8) Uani 1 1 d . . . . .
H18 H 1.133004 0.109989 0.567511 0.045 Uiso 1 1 calc R U . . .
C11 C 0.7042(4) 0.5335(2) 0.3743(3) 0.0390(9) Uani 1 1 d . . . . .
H11 H 0.720929 0.558052 0.323184 0.047 Uiso 1 1 calc R U . . .
C3 C -0.0214(4) 0.2331(3) 0.3531(2) 0.0374(8) Uani 1 1 d . . . . .
H3 H 0.014324 0.239432 0.414776 0.045 Uiso 1 1 calc R U . . .
C6 C -0.1281(4) 0.2176(3) 0.1688(2) 0.0344(8) Uani 1 1 d . . . . .
H6 H -0.163882 0.214164 0.106915 0.041 Uiso 1 1 calc R U . . .
C5 C -0.2121(3) 0.2265(3) 0.2240(3) 0.0359(8) Uani 1 1 d . . . . .
C20 C 1.0472(4) 0.0066(3) 0.7271(3) 0.0436(10) Uani 1 1 d . . . . .
H20 H 1.083833 -0.018492 0.783546 0.052 Uiso 1 1 calc R U . . .
C4 C -0.1590(4) 0.2359(3) 0.3160(3) 0.0435(10) Uani 1 1 d . . . . .
H4 H -0.215623 0.244012 0.352682 0.052 Uiso 1 1 calc R U . . .
H12A H 0.436(7) 0.296(4) 0.237(5) 0.08(2) Uiso 1 1 d . . . . .
H12B H 0.344(6) 0.260(4) 0.184(4) 0.06(2) Uiso 1 1 d . . . . .
H10 H 0.762(5) 0.692(3) 0.490(3) 0.043(14) Uiso 1 1 d . . . . .
O11 O 1.2661(3) 0.0414(2) 0.7209(2) 0.0538(8) Uani 1 1 d . . . . .
H11A H 1.299042 0.091266 0.717895 0.081 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
Lu1 O3 2.413(2) . ?
Lu1 O6 2.263(2) 3_656 ?
Lu1 O4 2.312(2) . ?
Lu1 O1 2.368(2) . ?
Lu1 O5 2.243(2) . ?
Lu1 O7 2.347(3) . ?
Lu1 O8 2.286(3) . ?
Lu1 O2 2.324(2) . ?
O3 C8 1.265(4) . ?
O6 C15 1.277(4) . ?
O4 C8 1.273(4) . ?
O1 C1 1.252(4) . ?
O5 C15 1.255(4) . ?
O7 H7A 0.8712 . ?
O7 H7B 0.8699 . ?
O8 H8A 0.8577 . ?
O8 H8B 0.8576 . ?
O2 C1 1.281(4) . ?
O12 H12A 0.75(7) . ?
O12 H12B 0.72(6) . ?
O10 C12 1.360(4) . ?
O10 H10 0.77(5) . ?
O9 H9 0.8200 . ?
O9 C5 1.361(4) . ?
C8 C9 1.476(5) . ?
C9 C10 1.389(5) . ?
C9 C14 1.392(5) . ?
C2 C1 1.484(4) . ?
C2 C7 1.391(5) . ?
C2 C3 1.388(5) . ?
C10 H10A 0.9300 . ?
C10 C11 1.382(5) . ?
C16 C21 1.397(5) . ?
C16 C15 1.479(4) . ?
C16 C17 1.393(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.375(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.390(5) . ?
C21 H21 0.9300 . ?
C21 C20 1.384(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.384(5) . ?
C12 C11 1.387(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.379(5) . ?
C19 C18 1.384(6) . ?
C19 C20 1.371(6) . ?
C19 O11 1.382(4) . ?
C18 H18 0.9300 . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.385(5) . ?
C6 H6 0.9300 . ?
C6 C5 1.384(5) . ?
C5 C4 1.386(5) . ?
C20 H20 0.9300 . ?
C4 H4 0.9300 . ?
O11 H11A 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Lu1 O3 154.06(8) 3_656 . ?
O6 Lu1 O4 151.19(8) 3_656 . ?
O6 Lu1 O1 80.20(8) 3_656 . ?
O6 Lu1 O7 81.72(9) 3_656 . ?
O6 Lu1 O8 76.75(9) 3_656 . ?
O6 Lu1 O2 93.14(9) 3_656 . ?
O4 Lu1 O3 54.72(8) . . ?
O4 Lu1 O1 79.01(9) . . ?
O4 Lu1 O7 74.73(9) . . ?
O4 Lu1 O2 91.24(9) . . ?
O1 Lu1 O3 116.35(8) . . ?
O5 Lu1 O3 81.74(9) . . ?
O5 Lu1 O6 91.18(8) . 3_656 ?
O5 Lu1 O4 98.40(9) . . ?
O5 Lu1 O1 152.95(9) . . ?
O5 Lu1 O7 75.02(9) . . ?
O5 Lu1 O8 78.08(9) . . ?
O5 Lu1 O2 151.45(9) . . ?
O7 Lu1 O3 119.78(9) . . ?
O7 Lu1 O1 78.37(8) . . ?
O8 Lu1 O3 77.37(9) . . ?
O8 Lu1 O4 131.75(9) . . ?
O8 Lu1 O1 123.76(9) . . ?
O8 Lu1 O7 144.95(10) . . ?
O8 Lu1 O2 75.49(9) . . ?
O2 Lu1 O3 82.12(9) . . ?
O2 Lu1 O1 55.34(8) . . ?
O2 Lu1 O7 133.53(9) . . ?
C8 O3 Lu1 91.49(19) . . ?
C15 O6 Lu1 137.3(2) . 3_656 ?
C8 O4 Lu1 96.0(2) . . ?
C1 O1 Lu1 91.95(19) . . ?
C15 O5 Lu1 137.9(2) . . ?
Lu1 O7 H7A 127.9 . . ?
Lu1 O7 H7B 127.6 . . ?
H7A O7 H7B 104.5 . . ?
Lu1 O8 H8A 110.2 . . ?
Lu1 O8 H8B 109.6 . . ?
H8A O8 H8B 104.1 . . ?
C1 O2 Lu1 93.22(19) . . ?
H12A O12 H12B 109(7) . . ?
C12 O10 H10 103(4) . . ?
C5 O9 H9 109.5 . . ?
O3 C8 O4 117.8(3) . . ?
O3 C8 C9 122.6(3) . . ?
O4 C8 C9 119.6(3) . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 C14 118.4(3) . . ?
C14 C9 C8 121.8(3) . . ?
C7 C2 C1 119.9(3) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C7 119.4(3) . . ?
C9 C10 H10A 119.4 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10A 119.4 . . ?
C21 C16 C15 120.3(3) . . ?
C17 C16 C21 118.9(3) . . ?
C17 C16 C15 120.8(3) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 C9 121.2(3) . . ?
C13 C14 H14 119.4 . . ?
O1 C1 O2 118.7(3) . . ?
O1 C1 C2 121.2(3) . . ?
O2 C1 C2 120.1(3) . . ?
C14 C13 H13 120.2 . . ?
C14 C13 C12 119.7(3) . . ?
C12 C13 H13 120.2 . . ?
C16 C21 H21 120.0 . . ?
C20 C21 C16 120.0(4) . . ?
C20 C21 H21 120.0 . . ?
O6 C15 C16 118.8(3) . . ?
O5 C15 O6 122.6(3) . . ?
O5 C15 C16 118.7(3) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
O10 C12 C13 123.4(3) . . ?
O10 C12 C11 116.6(3) . . ?
C11 C12 C13 120.0(3) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.8(3) . . ?
C18 C17 H17 119.6 . . ?
C20 C19 C18 120.8(3) . . ?
C20 C19 O11 117.6(4) . . ?
O11 C19 C18 121.6(4) . . ?
C17 C18 C19 119.4(4) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C10 C11 C12 119.6(4) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3 119.9 . . ?
C7 C6 H6 120.1 . . ?
C7 C6 C5 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
O9 C5 C6 122.8(3) . . ?
O9 C5 C4 116.9(3) . . ?
C6 C5 C4 120.3(3) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 C21 120.1(4) . . ?
C19 C20 H20 120.0 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C19 O11 H11A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Lu1 O3 C8 O4 -1.0(3) . . . . ?
Lu1 O3 C8 C9 179.5(3) . . . . ?
Lu1 O6 C15 O5 82.2(4) 3_656 . . . ?
Lu1 O6 C15 C16 -99.3(3) 3_656 . . . ?
Lu1 O4 C8 O3 1.0(3) . . . . ?
Lu1 O4 C8 C9 -179.4(3) . . . . ?
Lu1 O1 C1 O2 9.0(3) . . . . ?
Lu1 O1 C1 C2 -167.2(3) . . . . ?
Lu1 O5 C15 O6 21.1(5) . . . . ?
Lu1 O5 C15 C16 -157.4(2) . . . . ?
Lu1 O2 C1 O1 -9.1(3) . . . . ?
Lu1 O2 C1 C2 167.1(3) . . . . ?
O3 C8 C9 C10 175.0(3) . . . . ?
O3 C8 C9 C14 -7.5(5) . . . . ?
O4 C8 C9 C10 -4.5(5) . . . . ?
O4 C8 C9 C14 172.9(3) . . . . ?
O10 C12 C11 C10 -178.7(4) . . . . ?
O9 C5 C4 C3 176.8(4) . . . . ?
C8 C9 C10 C11 177.3(4) . . . . ?
C8 C9 C14 C13 -177.1(3) . . . . ?
C9 C10 C11 C12 -0.4(7) . . . . ?
C9 C14 C13 C12 0.2(6) . . . . ?
C2 C7 C6 C5 -1.3(6) . . . . ?
C2 C3 C4 C5 -0.1(7) . . . . ?
C10 C9 C14 C13 0.4(5) . . . . ?
C16 C21 C20 C19 0.2(6) . . . . ?
C16 C17 C18 C19 -0.2(6) . . . . ?
C14 C9 C10 C11 -0.3(6) . . . . ?
C14 C13 C12 O10 178.8(4) . . . . ?
C14 C13 C12 C11 -0.8(6) . . . . ?
C1 C2 C7 C6 172.7(3) . . . . ?
C1 C2 C3 C4 -172.0(4) . . . . ?
C13 C12 C11 C10 0.9(6) . . . . ?
C21 C16 C15 O6 -10.4(5) . . . . ?
C21 C16 C15 O5 168.1(3) . . . . ?
C21 C16 C17 C18 1.1(5) . . . . ?
C15 C16 C21 C20 178.7(4) . . . . ?
C15 C16 C17 C18 -178.7(3) . . . . ?
C7 C2 C1 O1 -8.7(5) . . . . ?
C7 C2 C1 O2 175.1(3) . . . . ?
C7 C2 C3 C4 1.7(6) . . . . ?
C7 C6 C5 O9 -176.1(4) . . . . ?
C7 C6 C5 C4 3.0(6) . . . . ?
C17 C16 C21 C20 -1.1(6) . . . . ?
C17 C16 C15 O6 169.4(3) . . . . ?
C17 C16 C15 O5 -12.1(5) . . . . ?
C18 C19 C20 C21 0.7(7) . . . . ?
C3 C2 C1 O1 165.0(3) . . . . ?
C3 C2 C1 O2 -11.2(5) . . . . ?
C3 C2 C7 C6 -1.0(5) . . . . ?
C6 C5 C4 C3 -2.3(7) . . . . ?
C20 C19 C18 C17 -0.7(6) . . . . ?
O11 C19 C18 C17 177.6(4) . . . . ?
O11 C19 C20 C21 -177.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# 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_p21n
_database_code_depnum_ccdc_archive 'CCDC 2269133'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C62 H46 N4 O18 Tb2, 4(H2 O), 2(C10 H8 N2)'
_chemical_formula_sum            'C82 H70 N8 O22 Tb2'
_chemical_formula_weight         1837.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.3213(6)
_cell_length_b                   13.1760(4)
_cell_length_c                   19.1799(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.2410(10)
_cell_angle_gamma                90
_cell_volume                     4022.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8095
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   0.772
_shelx_estimated_absorpt_T_min   0.463
_exptl_absorpt_coefficient_mu    1.823
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.118
_diffrn_reflns_theta_min         1.930
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8145
_reflns_number_total             11752
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         11752
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0356P)²+1.1061P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0836
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O11-H11A
 0.8 with sigma of 0.02
 O8-H8
 0.8 with sigma of 0.02
2.a Free rotating group:
 O10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C17(H17), C14(H14), C4(H4), C7(H7A), C18(H18), C6(H6), C10(H10),
 C31(H31), C28(H28), C13(H13), C22(H22), C11(H11), C30(H30), C29(H29), C25(H25),
  C38(H38), C21(H21), C23(H23), C3(H3), C24(H24), C20(H20), C34(H34), C39(H39),
 C33(H33), C32(H32), C40(H40)
2.c Tetrahedral OH refined with riding coordinates:
 O7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.48468(2) 0.45071(2) 0.39123(2) 0.03298(5) Uani 1 1 d . . . . .
O1 O 0.58753(13) 0.33516(16) 0.37749(13) 0.0487(5) Uani 1 1 d . . . . .
O2 O 0.57190(13) 0.48072(16) 0.31821(13) 0.0461(5) Uani 1 1 d . . . . .
O6 O 0.51010(13) 0.67820(15) 0.52382(12) 0.0451(5) Uani 1 1 d . . . . .
O4 O 0.65162(14) 0.54575(17) 0.61220(14) 0.0521(6) Uani 1 1 d . . . . .
O3 O 0.60721(13) 0.4952(2) 0.49268(14) 0.0566(6) Uani 1 1 d . . . . .
O7 O 0.90325(14) 0.30492(19) 0.29318(16) 0.0667(7) Uani 1 1 d . . . . .
H7 H 0.914748 0.244384 0.299955 0.100 Uiso 1 1 calc R U . . .
O5 O 0.47773(14) 0.62330(16) 0.40566(12) 0.0496(5) Uani 1 1 d . . . . .
O9 O 0.6028(2) 1.0645(2) 0.3758(2) 0.0839(10) Uani 1 1 d . . . . .
N2 N 0.38192(16) 0.5114(2) 0.25822(15) 0.0454(6) Uani 1 1 d . . . . .
O11 O 0.9406(2) 0.1137(2) 0.2987(2) 0.0704(8) Uani 1 1 d D . . . .
N1 N 0.40382(17) 0.3144(2) 0.29431(15) 0.0463(6) Uani 1 1 d . . . . .
O10 O 0.67671(18) 1.1949(2) 0.49176(18) 0.0745(8) Uani 1 1 d G . . . .
H10A H 0.657898 1.248320 0.465799 0.112 Uiso 1 1 d G U . . .
H10B H 0.729466 1.197337 0.503910 0.112 Uiso 1 1 d G U . . .
C9 C 0.75022(17) 0.5423(2) 0.55574(18) 0.0398(6) Uani 1 1 d . . . . .
C1 C 0.60994(18) 0.3965(2) 0.33836(17) 0.0409(7) Uani 1 1 d . . . . .
C2 C 0.68314(18) 0.3709(2) 0.31993(17) 0.0409(7) Uani 1 1 d . . . . .
C8 C 0.66365(18) 0.5268(2) 0.55307(19) 0.0422(7) Uani 1 1 d . . . . .
C15 C 0.50337(18) 0.6900(2) 0.45664(18) 0.0401(7) Uani 1 1 d . . . . .
C42 C 0.7259(2) 0.4446(2) 0.2984(2) 0.0492(8) Uani 1 1 d . . . . .
H42 H 0.705561 0.510768 0.290622 0.059 Uiso 1 1 calc R U . . .
C5 C 0.82879(19) 0.3227(3) 0.29917(19) 0.0477(8) Uani 1 1 d . . . . .
C16 C 0.5283(2) 0.7900(2) 0.43594(17) 0.0431(7) Uani 1 1 d . . . . .
N4 N 0.4354(2) 0.5651(3) 0.0574(2) 0.0752(10) Uani 1 1 d . . . . .
C36 C 0.4173(3) 0.3845(3) 0.0599(2) 0.0671(10) Uani 1 1 d . . . . .
C27 C 0.3271(2) 0.4463(3) 0.20966(19) 0.0478(8) Uani 1 1 d . . . . .
C17 C 0.5506(2) 0.8701(3) 0.48529(19) 0.0527(8) Uani 1 1 d . . . . .
H17 H 0.549789 0.862002 0.533154 0.063 Uiso 1 1 calc R U . . .
O8 O 0.9919(2) 0.5809(4) 0.5665(3) 0.1163(13) Uani 1 1 d D . . . .
C14 C 0.81462(19) 0.5717(3) 0.6227(2) 0.0503(8) Uani 1 1 d . . . . .
H14 H 0.803373 0.582450 0.665728 0.060 Uiso 1 1 calc R U . . .
C4 C 0.7986(2) 0.4212(3) 0.2884(2) 0.0521(8) Uani 1 1 d . . . . .
H4 H 0.827260 0.471585 0.274357 0.063 Uiso 1 1 calc R U . . .
N35 N 0.3600(2) 0.3097(3) 0.0414(3) 0.0917(12) Uani 1 1 d . . . . .
C7 C 0.7125(2) 0.2720(3) 0.3278(2) 0.0514(8) Uani 1 1 d . . . . .
H7A H 0.683228 0.221078 0.340681 0.062 Uiso 1 1 calc R U . . .
C18 C 0.5745(2) 0.9629(2) 0.4662(2) 0.0555(9) Uani 1 1 d . . . . .
H18 H 0.588273 1.016129 0.500833 0.067 Uiso 1 1 calc R U . . .
C6 C 0.7842(2) 0.2480(3) 0.3170(2) 0.0543(8) Uani 1 1 d . . . . .
H6 H 0.802548 0.181077 0.321727 0.065 Uiso 1 1 calc R U . . .
C26 C 0.3352(2) 0.3385(3) 0.23258(19) 0.0495(8) Uani 1 1 d . . . . .
C37 C 0.3884(3) 0.4838(3) 0.0237(2) 0.0665(10) Uani 1 1 d . . . . .
C10 C 0.7682(2) 0.5279(3) 0.4928(2) 0.0609(10) Uani 1 1 d . . . . .
H10 H 0.725576 0.509151 0.447081 0.073 Uiso 1 1 calc R U . . .
C31 C 0.3787(2) 0.6084(3) 0.2371(2) 0.0614(10) Uani 1 1 d . . . . .
H31 H 0.416515 0.653601 0.270650 0.074 Uiso 1 1 calc R U . . .
C28 C 0.2688(3) 0.4791(3) 0.1401(2) 0.0676(11) Uani 1 1 d . . . . .
H28 H 0.230871 0.433496 0.107157 0.081 Uiso 1 1 calc R U . . .
C19 C 0.5778(3) 0.9767(3) 0.3978(2) 0.0605(10) Uani 1 1 d . . . . .
C13 C 0.8948(2) 0.5853(3) 0.6268(2) 0.0681(11) Uani 1 1 d . . . . .
H13 H 0.937373 0.605452 0.672159 0.082 Uiso 1 1 calc R U . . .
C22 C 0.4183(2) 0.2169(3) 0.3131(2) 0.0582(9) Uani 1 1 d . . . . .
H22 H 0.466898 0.199779 0.354695 0.070 Uiso 1 1 calc R U . . .
C11 C 0.8493(3) 0.5409(3) 0.4967(3) 0.0768(13) Uani 1 1 d . . . . .
H11 H 0.861064 0.530401 0.453952 0.092 Uiso 1 1 calc R U . . .
C30 C 0.3231(2) 0.6455(3) 0.1688(2) 0.0706(11) Uani 1 1 d . . . . .
H30 H 0.323592 0.713588 0.156353 0.085 Uiso 1 1 calc R U . . .
C12 C 0.9121(2) 0.5694(3) 0.5643(3) 0.0728(12) Uani 1 1 d . . . . .
C29 C 0.2674(3) 0.5800(4) 0.1201(2) 0.0735(12) Uani 1 1 d . . . . .
H29 H 0.228519 0.602795 0.073631 0.088 Uiso 1 1 calc R U . . .
C25 C 0.2772(3) 0.2643(3) 0.1922(2) 0.0719(11) Uani 1 1 d . . . . .
H25 H 0.228630 0.282054 0.150847 0.086 Uiso 1 1 calc R U . . .
C38 C 0.3167(3) 0.4939(5) -0.0418(3) 0.0866(14) Uani 1 1 d . . . . .
H38 H 0.285538 0.436860 -0.064965 0.104 Uiso 1 1 calc R U . . .
C21 C 0.5374(3) 0.8041(3) 0.3678(2) 0.0755(12) Uani 1 1 d . . . . .
H21 H 0.527232 0.749889 0.334260 0.091 Uiso 1 1 calc R U . . .
C23 C 0.3643(3) 0.1394(3) 0.2737(3) 0.0751(12) Uani 1 1 d . . . . .
H23 H 0.377007 0.071947 0.287826 0.090 Uiso 1 1 calc R U . . .
C3 C 0.4985(3) 0.3680(4) 0.1100(3) 0.0934(15) Uani 1 1 d . . . . .
H3 H 0.537194 0.420840 0.122813 0.112 Uiso 1 1 calc R U . . .
C24 C 0.2930(3) 0.1646(4) 0.2145(3) 0.0856(14) Uani 1 1 d . . . . .
H24 H 0.254471 0.114490 0.188741 0.103 Uiso 1 1 calc R U . . .
C20 C 0.5610(3) 0.8962(4) 0.3487(2) 0.0860(15) Uani 1 1 d . . . . .
H20 H 0.565586 0.903931 0.302287 0.103 Uiso 1 1 calc R U . . .
C34 C 0.3857(4) 0.2189(4) 0.0737(4) 0.119(2) Uani 1 1 d . . . . .
H34 H 0.346367 0.166820 0.061810 0.143 Uiso 1 1 calc R U . . .
C39 C 0.2916(4) 0.5885(5) -0.0726(3) 0.1073(18) Uani 1 1 d . . . . .
H39 H 0.243152 0.596300 -0.116455 0.129 Uiso 1 1 calc R U . . .
C41 C 0.4101(4) 0.6554(5) 0.0263(3) 0.0991(17) Uani 1 1 d . . . . .
C33 C 0.4652(4) 0.1984(4) 0.1224(4) 0.116(2) Uani 1 1 d . . . . .
H33 H 0.479873 0.133520 0.142373 0.139 Uiso 1 1 calc R U . . .
C32 C 0.5228(4) 0.2732(4) 0.1415(4) 0.116(2) Uani 1 1 d . . . . .
H32 H 0.577819 0.261214 0.175184 0.139 Uiso 1 1 calc R U . . .
C40 C 0.3389(4) 0.6705(5) -0.0379(3) 0.1114(18) Uani 1 1 d . . . . .
H40 H 0.323158 0.735440 -0.057336 0.134 Uiso 1 1 calc R U . . .
H11A H 0.939(3) 0.080(3) 0.2647(18) 0.078(15) Uiso 1 1 d D . . . .
H11B H 0.970(4) 0.096(4) 0.339(3) 0.11(2) Uiso 1 1 d . . . . .
H9 H 0.616(3) 1.100(3) 0.412(2) 0.063(14) Uiso 1 1 d . . . . .
H8 H 1.020(4) 0.596(7) 0.609(2) 0.20(5) Uiso 1 1 d D . . . .
H41 H 0.447(3) 0.711(4) 0.049(3) 0.118(19) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.435(2) . ?
Tb1 O2 2.464(2) . ?
Tb1 O6 2.331(2) 3_666 ?
Tb1 O4 2.336(2) 3_666 ?
Tb1 O3 2.319(2) . ?
Tb1 O5 2.300(2) . ?
Tb1 N2 2.595(3) . ?
Tb1 N1 2.566(3) . ?
O1 C1 1.264(3) . ?
O2 C1 1.270(4) . ?
O6 C15 1.257(4) . ?
O4 C8 1.256(4) . ?
O3 C8 1.256(4) . ?
O7 H7 0.8200 . ?
O7 C5 1.360(3) . ?
O5 C15 1.258(4) . ?
O9 C19 1.359(4) . ?
O9 H9 0.79(4) . ?
N2 C27 1.345(4) . ?
N2 C31 1.335(5) . ?
O11 H11A 0.779(19) . ?
O11 H11B 0.78(6) . ?
N1 C26 1.344(4) . ?
N1 C22 1.332(4) . ?
O10 H10A 0.8497 . ?
O10 H10B 0.8500 . ?
C9 C8 1.494(4) . ?
C9 C14 1.384(4) . ?
C9 C10 1.374(5) . ?
C1 C2 1.483(4) . ?
C2 C42 1.379(4) . ?
C2 C7 1.386(4) . ?
C15 C16 1.489(4) . ?
C42 H42 0.9300 . ?
C42 C4 1.383(4) . ?
C5 C4 1.383(5) . ?
C5 C6 1.375(4) . ?
C16 C17 1.367(4) . ?
C16 C21 1.389(5) . ?
N4 C37 1.348(5) . ?
N4 C41 1.326(6) . ?
C36 N35 1.343(5) . ?
C36 C37 1.472(6) . ?
C36 C3 1.372(6) . ?
C27 C26 1.477(5) . ?
C27 C28 1.387(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.385(4) . ?
O8 C12 1.374(5) . ?
O8 H8 0.80(2) . ?
C14 H14 0.9300 . ?
C14 C13 1.373(5) . ?
C4 H4 0.9300 . ?
N35 C34 1.340(7) . ?
C7 H7A 0.9300 . ?
C7 C6 1.374(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.348(5) . ?
C6 H6 0.9300 . ?
C26 C25 1.396(5) . ?
C37 C38 1.380(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.387(5) . ?
C31 H31 0.9300 . ?
C31 C30 1.374(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.381(6) . ?
C19 C20 1.371(6) . ?
C13 H13 0.9300 . ?
C13 C12 1.360(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.389(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.377(6) . ?
C30 H30 0.9300 . ?
C30 C29 1.355(6) . ?
C29 H29 0.9300 . ?
C25 H25 0.9300 . ?
C25 C24 1.375(6) . ?
C38 H38 0.9300 . ?
C38 C39 1.375(8) . ?
C21 H21 0.9300 . ?
C21 C20 1.376(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.349(6) . ?
C3 H3 0.9300 . ?
C3 C32 1.379(7) . ?
C24 H24 0.9300 . ?
C20 H20 0.9300 . ?
C34 H34 0.9300 . ?
C34 C33 1.352(8) . ?
C39 H39 0.9300 . ?
C39 C40 1.360(8) . ?
C41 C40 1.371(7) . ?
C41 H41 0.95(5) . ?
C33 H33 0.9300 . ?
C33 C32 1.347(8) . ?
C32 H32 0.9300 . ?
C40 H40 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
O1 Tb1 O2 53.13(7) . . ?
O1 Tb1 N2 109.49(8) . . ?
O1 Tb1 N1 72.41(8) . . ?
O2 Tb1 N2 74.23(8) . . ?
O2 Tb1 N1 88.99(8) . . ?
O6 Tb1 O1 77.99(7) 3_666 . ?
O6 Tb1 O2 130.62(7) 3_666 . ?
O6 Tb1 O4 78.12(8) 3_666 3_666 ?
O6 Tb1 N2 137.24(8) 3_666 . ?
O6 Tb1 N1 81.72(8) 3_666 . ?
O4 Tb1 O1 141.60(8) 3_666 . ?
O4 Tb1 O2 145.12(8) 3_666 . ?
O4 Tb1 N2 70.89(8) 3_666 . ?
O4 Tb1 N1 74.75(8) 3_666 . ?
O3 Tb1 O1 77.44(9) . . ?
O3 Tb1 O2 82.70(8) . . ?
O3 Tb1 O6 80.07(8) . 3_666 ?
O3 Tb1 O4 126.78(9) . 3_666 ?
O3 Tb1 N2 142.45(9) . . ?
O3 Tb1 N1 147.37(9) . . ?
O5 Tb1 O1 134.95(7) . . ?
O5 Tb1 O2 89.01(8) . . ?
O5 Tb1 O6 128.75(7) . 3_666 ?
O5 Tb1 O4 83.30(8) . 3_666 ?
O5 Tb1 O3 73.91(8) . . ?
O5 Tb1 N2 76.43(8) . . ?
O5 Tb1 N1 137.68(8) . . ?
N1 Tb1 N2 62.41(8) . . ?
C1 O1 Tb1 94.22(17) . . ?
C1 O2 Tb1 92.74(17) . . ?
C15 O6 Tb1 140.3(2) . 3_666 ?
C8 O4 Tb1 120.3(2) . 3_666 ?
C8 O3 Tb1 168.4(2) . . ?
C5 O7 H7 109.5 . . ?
C15 O5 Tb1 139.9(2) . . ?
C19 O9 H9 104(3) . . ?
C27 N2 Tb1 120.5(2) . . ?
C31 N2 Tb1 121.6(2) . . ?
C31 N2 C27 117.9(3) . . ?
H11A O11 H11B 117(5) . . ?
C26 N1 Tb1 120.9(2) . . ?
C22 N1 Tb1 119.2(2) . . ?
C22 N1 C26 118.2(3) . . ?
H10A O10 H10B 104.5 . . ?
C14 C9 C8 120.0(3) . . ?
C10 C9 C8 121.6(3) . . ?
C10 C9 C14 118.4(3) . . ?
O1 C1 O2 119.7(3) . . ?
O1 C1 C2 119.2(3) . . ?
O2 C1 C2 121.0(3) . . ?
C42 C2 C1 121.5(3) . . ?
C42 C2 C7 118.6(3) . . ?
C7 C2 C1 119.9(3) . . ?
O4 C8 C9 117.6(3) . . ?
O3 C8 O4 123.5(3) . . ?
O3 C8 C9 118.8(3) . . ?
O6 C15 O5 124.9(3) . . ?
O6 C15 C16 117.6(3) . . ?
O5 C15 C16 117.5(3) . . ?
C2 C42 H42 119.6 . . ?
C2 C42 C4 120.7(3) . . ?
C4 C42 H42 119.6 . . ?
O7 C5 C4 117.6(3) . . ?
O7 C5 C6 122.9(3) . . ?
C6 C5 C4 119.5(3) . . ?
C17 C16 C15 122.1(3) . . ?
C17 C16 C21 116.3(3) . . ?
C21 C16 C15 121.4(3) . . ?
C41 N4 C37 117.9(4) . . ?
N35 C36 C37 116.6(4) . . ?
N35 C36 C3 121.0(4) . . ?
C3 C36 C37 122.4(4) . . ?
N2 C27 C26 116.7(3) . . ?
N2 C27 C28 121.0(3) . . ?
C28 C27 C26 122.3(3) . . ?
C16 C17 H17 119.0 . . ?
C16 C17 C18 122.0(3) . . ?
C18 C17 H17 119.0 . . ?
C12 O8 H8 105(6) . . ?
C9 C14 H14 119.5 . . ?
C13 C14 C9 121.1(4) . . ?
C13 C14 H14 119.5 . . ?
C42 C4 C5 120.0(3) . . ?
C42 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C34 N35 C36 117.2(4) . . ?
C2 C7 H7A 119.6 . . ?
C6 C7 C2 120.9(3) . . ?
C6 C7 H7A 119.6 . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.5(3) . . ?
C19 C18 H18 119.7 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(3) . . ?
C7 C6 H6 119.9 . . ?
N1 C26 C27 115.8(3) . . ?
N1 C26 C25 121.1(3) . . ?
C25 C26 C27 123.0(3) . . ?
N4 C37 C36 116.8(4) . . ?
N4 C37 C38 121.1(5) . . ?
C38 C37 C36 122.1(4) . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.8(4) . . ?
C11 C10 H10 119.6 . . ?
N2 C31 H31 118.0 . . ?
N2 C31 C30 124.0(4) . . ?
C30 C31 H31 118.0 . . ?
C27 C28 H28 120.2 . . ?
C29 C28 C27 119.6(4) . . ?
C29 C28 H28 120.2 . . ?
O9 C19 C20 116.9(4) . . ?
C18 C19 O9 123.9(4) . . ?
C18 C19 C20 119.1(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(4) . . ?
C12 C13 H13 120.0 . . ?
N1 C22 H22 118.4 . . ?
N1 C22 C23 123.2(4) . . ?
C23 C22 H22 118.4 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.4(4) . . ?
C12 C11 H11 120.3 . . ?
C31 C30 H30 120.9 . . ?
C29 C30 C31 118.2(4) . . ?
C29 C30 H30 120.9 . . ?
O8 C12 C11 118.1(5) . . ?
C13 C12 O8 121.6(4) . . ?
C13 C12 C11 120.3(3) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 C28 119.4(4) . . ?
C30 C29 H29 120.3 . . ?
C26 C25 H25 120.5 . . ?
C24 C25 C26 119.0(4) . . ?
C24 C25 H25 120.5 . . ?
C37 C38 H38 120.1 . . ?
C39 C38 C37 119.8(5) . . ?
C39 C38 H38 120.1 . . ?
C16 C21 H21 119.2 . . ?
C20 C21 C16 121.6(4) . . ?
C20 C21 H21 119.2 . . ?
C22 C23 H23 120.9 . . ?
C24 C23 C22 118.3(4) . . ?
C24 C23 H23 120.9 . . ?
C36 C3 H3 119.9 . . ?
C36 C3 C32 120.2(5) . . ?
C32 C3 H3 119.9 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 C25 120.0(4) . . ?
C23 C24 H24 120.0 . . ?
C19 C20 C21 120.3(4) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
N35 C34 H34 118.0 . . ?
N35 C34 C33 124.1(5) . . ?
C33 C34 H34 118.0 . . ?
C38 C39 H39 120.6 . . ?
C40 C39 C38 118.8(5) . . ?
C40 C39 H39 120.6 . . ?
N4 C41 C40 123.7(5) . . ?
N4 C41 H41 116(3) . . ?
C40 C41 H41 120(3) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 C34 119.0(6) . . ?
C32 C33 H33 120.5 . . ?
C3 C32 H32 120.7 . . ?
C33 C32 C3 118.6(6) . . ?
C33 C32 H32 120.7 . . ?
C39 C40 C41 118.6(6) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C1 O2 -4.8(3) . . . . ?
Tb1 O1 C1 C2 172.2(2) . . . . ?
Tb1 O2 C1 O1 4.7(3) . . . . ?
Tb1 O2 C1 C2 -172.2(3) . . . . ?
Tb1 O6 C15 O5 17.0(5) 3_666 . . . ?
Tb1 O6 C15 C16 -162.4(2) 3_666 . . . ?
Tb1 O4 C8 O3 -10.3(4) 3_666 . . . ?
Tb1 O4 C8 C9 170.19(18) 3_666 . . . ?
Tb1 O3 C8 O4 21.1(13) . . . . ?
Tb1 O3 C8 C9 -159.4(10) . . . . ?
Tb1 O5 C15 O6 -36.5(5) . . . . ?
Tb1 O5 C15 C16 142.9(2) . . . . ?
Tb1 N2 C27 C26 -6.6(4) . . . . ?
Tb1 N2 C27 C28 176.4(3) . . . . ?
Tb1 N2 C31 C30 -177.0(3) . . . . ?
Tb1 N1 C26 C27 21.1(4) . . . . ?
Tb1 N1 C26 C25 -160.8(3) . . . . ?
Tb1 N1 C22 C23 163.1(3) . . . . ?
O1 C1 C2 C42 -160.1(3) . . . . ?
O1 C1 C2 C7 16.6(5) . . . . ?
O2 C1 C2 C42 16.9(5) . . . . ?
O2 C1 C2 C7 -166.4(3) . . . . ?
O6 C15 C16 C17 -5.8(4) . . . . ?
O6 C15 C16 C21 168.3(3) . . . . ?
O7 C5 C4 C42 -176.0(3) . . . . ?
O7 C5 C6 C7 175.1(3) . . . . ?
O5 C15 C16 C17 174.7(3) . . . . ?
O5 C15 C16 C21 -11.2(5) . . . . ?
O9 C19 C20 C21 178.4(4) . . . . ?
N2 C27 C26 N1 -9.2(4) . . . . ?
N2 C27 C26 C25 172.7(3) . . . . ?
N2 C27 C28 C29 0.5(6) . . . . ?
N2 C31 C30 C29 0.7(7) . . . . ?
N1 C26 C25 C24 -2.8(6) . . . . ?
N1 C22 C23 C24 -1.4(6) . . . . ?
C9 C14 C13 C12 -0.3(6) . . . . ?
C9 C10 C11 C12 -0.5(6) . . . . ?
C1 C2 C42 C4 173.9(3) . . . . ?
C1 C2 C7 C6 -174.7(3) . . . . ?
C2 C42 C4 C5 0.6(6) . . . . ?
C2 C7 C6 C5 1.0(5) . . . . ?
C8 C9 C14 C13 179.3(3) . . . . ?
C8 C9 C10 C11 -178.9(3) . . . . ?
C15 C16 C17 C18 179.5(3) . . . . ?
C15 C16 C21 C20 -179.5(4) . . . . ?
C42 C2 C7 C6 2.1(5) . . . . ?
C16 C17 C18 C19 -1.2(6) . . . . ?
C16 C21 C20 C19 1.2(8) . . . . ?
N4 C37 C38 C39 -1.3(7) . . . . ?
N4 C41 C40 C39 -0.9(10) . . . . ?
C36 N35 C34 C33 -0.9(9) . . . . ?
C36 C37 C38 C39 178.9(4) . . . . ?
C36 C3 C32 C33 -0.5(9) . . . . ?
C27 N2 C31 C30 -0.2(6) . . . . ?
C27 C26 C25 C24 175.3(4) . . . . ?
C27 C28 C29 C30 0.0(7) . . . . ?
C17 C16 C21 C20 -5.1(6) . . . . ?
C17 C18 C19 O9 -178.1(4) . . . . ?
C17 C18 C19 C20 -2.9(6) . . . . ?
C14 C9 C8 O4 3.0(4) . . . . ?
C14 C9 C8 O3 -176.5(3) . . . . ?
C14 C9 C10 C11 1.0(5) . . . . ?
C14 C13 C12 O8 -179.1(4) . . . . ?
C14 C13 C12 C11 0.8(7) . . . . ?
C4 C5 C6 C7 -3.3(5) . . . . ?
N35 C36 C37 N4 160.5(4) . . . . ?
N35 C36 C37 C38 -19.7(6) . . . . ?
N35 C36 C3 C32 1.0(8) . . . . ?
N35 C34 C33 C32 1.3(11) . . . . ?
C7 C2 C42 C4 -2.9(5) . . . . ?
C18 C19 C20 C21 2.9(7) . . . . ?
C6 C5 C4 C42 2.5(5) . . . . ?
C26 N1 C22 C23 -2.4(5) . . . . ?
C26 C27 C28 C29 -176.4(4) . . . . ?
C26 C25 C24 C23 -1.2(7) . . . . ?
C37 N4 C41 C40 0.2(9) . . . . ?
C37 C36 N35 C34 179.7(5) . . . . ?
C37 C36 C3 C32 -179.0(5) . . . . ?
C37 C38 C39 C40 0.6(8) . . . . ?
C10 C9 C8 O4 -177.1(3) . . . . ?
C10 C9 C8 O3 3.4(5) . . . . ?
C10 C9 C14 C13 -0.6(5) . . . . ?
C10 C11 C12 O8 179.5(4) . . . . ?
C10 C11 C12 C13 -0.4(7) . . . . ?
C31 N2 C27 C26 176.6(3) . . . . ?
C31 N2 C27 C28 -0.4(5) . . . . ?
C31 C30 C29 C28 -0.6(7) . . . . ?
C28 C27 C26 N1 167.8(3) . . . . ?
C28 C27 C26 C25 -10.4(5) . . . . ?
C22 N1 C26 C27 -173.7(3) . . . . ?
C22 N1 C26 C25 4.5(5) . . . . ?
C22 C23 C24 C25 3.1(7) . . . . ?
C38 C39 C40 C41 0.4(9) . . . . ?
C21 C16 C17 C18 5.1(5) . . . . ?
C3 C36 N35 C34 -0.3(7) . . . . ?
C3 C36 C37 N4 -19.5(6) . . . . ?
C3 C36 C37 C38 160.3(5) . . . . ?
C34 C33 C32 C3 -0.5(10) . . . . ?
C41 N4 C37 C36 -179.3(4) . . . . ?
C41 N4 C37 C38 0.9(7) . . . . ?

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

data_p21n_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2269134'
loop_
_audit_author_name
_audit_author_address
'Peter Junk'
;James Cook University
Australia
;
_audit_update_record             
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C62 H46 Dy2 N4 O18, 4(H2 O), 2(C10 H8 N2)'
_chemical_formula_sum            'C82 H70 Dy2 N8 O22'
_chemical_formula_weight         1844.46
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.3138(5)
_cell_length_b                   13.1899(4)
_cell_length_c                   19.1424(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.1660(10)
_cell_angle_gamma                90
_cell_volume                     4019.0(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8103
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.16
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   0.861
_shelx_estimated_absorpt_T_min   0.552
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.929
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6735
_reflns_number_total             9227
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.984
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         9227
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.048
_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)+(0.0416P)²+3.0617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.1014
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N38) = Uanis(C39)
Uanis(C37) = Uanis(N38)
2.a Free rotating group:
 O11(H11A,H11B), O10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7A), C6(H6), C3(H3), C20(H20), C14(H14), C31(H31), C38(H38), C21(H21),
 C22(H22), C30(H30), C29(H29), C28(H28), C10(H10), C11(H11), C13(H13), C23(H23),
  C17(H17), C35(H35), C18(H18), C4(H4), C24(H24), C25(H25), C39(H39), C32(H32),
 C34(H34), C33(H33), C41(H41), C40(H40)
2.c Tetrahedral OH refined with riding coordinates:
 O7(H7)
2.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.51523(2) 0.54958(2) 0.60919(2) 0.03809(7) Uani 1 1 d . . . . .
O1 O 0.41371(18) 0.6657(2) 0.62360(18) 0.0537(7) Uani 1 1 d . . . . .
O2 O 0.42867(18) 0.5199(2) 0.68216(17) 0.0502(7) Uani 1 1 d . . . . .
O6 O 0.48961(18) 0.3233(2) 0.47606(17) 0.0511(7) Uani 1 1 d . . . . .
O4 O 0.35032(18) 0.4558(2) 0.38971(19) 0.0565(8) Uani 1 1 d . . . . .
O5 O 0.52109(18) 0.3771(2) 0.59457(17) 0.0541(7) Uani 1 1 d . . . . .
O3 O 0.39243(18) 0.5065(3) 0.50896(19) 0.0615(8) Uani 1 1 d . . . . .
O7 O 0.09650(19) 0.6962(3) 0.7061(2) 0.0712(10) Uani 1 1 d . . . . .
H7 H 0.090079 0.757496 0.708789 0.107 Uiso 1 1 calc R U . . .
N2 N 0.6177(2) 0.4889(3) 0.7414(2) 0.0513(8) Uani 1 1 d . . . . .
O11 O 0.0591(2) 0.8872(3) 0.7009(2) 0.0745(10) Uani 1 1 d G . . . .
H11A H 0.030568 0.922158 0.662018 0.112 Uiso 1 1 d G U . . .
H11B H 0.065904 0.917357 0.742148 0.112 Uiso 1 1 d G U . . .
N1 N 0.5964(2) 0.6852(3) 0.7050(2) 0.0502(8) Uani 1 1 d . . . . .
O9 O 0.3976(3) -0.0643(3) 0.6236(2) 0.0885(12) Uani 1 1 d . . . . .
H9 H 0.379238 -0.102395 0.586855 0.133 Uiso 1 1 calc R U . . .
C2 C 0.3176(2) 0.6299(3) 0.6808(2) 0.0456(9) Uani 1 1 d . . . . .
C1 C 0.3907(2) 0.6040(3) 0.6619(2) 0.0443(9) Uani 1 1 d . . . . .
O10 O 0.3243(2) 0.8051(3) 0.5081(2) 0.0794(10) Uani 1 1 d G . . . .
H10A H 0.271512 0.807564 0.495873 0.119 Uiso 1 1 d G U . . .
H10B H 0.350760 0.753967 0.533196 0.119 Uiso 1 1 d G U . . .
C8 C 0.3373(2) 0.4751(3) 0.4486(3) 0.0459(10) Uani 1 1 d . . . . .
C9 C 0.2500(2) 0.4584(3) 0.4444(3) 0.0452(9) Uani 1 1 d . . . . .
C5 C 0.1718(3) 0.6782(3) 0.7010(3) 0.0518(10) Uani 1 1 d . . . . .
C7 C 0.2741(3) 0.5558(3) 0.7017(3) 0.0542(11) Uani 1 1 d . . . . .
H7A H 0.293788 0.489408 0.709022 0.065 Uiso 1 1 calc R U . . .
N3 N 0.0650(3) 1.0651(4) 0.4430(3) 0.0812(13) Uani 1 1 d . . . . .
C15 C 0.4957(2) 0.3114(3) 0.5429(3) 0.0457(9) Uani 1 1 d . . . . .
C27 C 0.6731(3) 0.5528(3) 0.7901(3) 0.0519(10) Uani 1 1 d . . . . .
C6 C 0.2014(3) 0.5801(4) 0.7116(3) 0.0578(12) Uani 1 1 d . . . . .
H6 H 0.172428 0.530049 0.725496 0.069 Uiso 1 1 calc R U . . .
C16 C 0.4710(3) 0.2109(3) 0.5638(2) 0.0490(10) Uani 1 1 d . . . . .
N38 N 0.1410(3) 0.8098(4) 0.4596(3) 0.0942(10) Uani 1 1 d . . . . .
O8 O 0.0081(2) 0.4168(5) 0.4316(3) 0.1167(17) Uani 1 1 d . U . . .
H8 H -0.023512 0.399912 0.388596 0.175 Uiso 1 1 calc R U . . .
C3 C 0.2883(3) 0.7289(3) 0.6724(3) 0.0560(11) Uani 1 1 d . . . . .
H3 H 0.317339 0.779329 0.658945 0.067 Uiso 1 1 calc R U . . .
C20 C 0.4255(3) 0.0385(3) 0.5333(3) 0.0604(12) Uani 1 1 d . . . . .
H20 H 0.410825 -0.014093 0.498129 0.072 Uiso 1 1 calc R U . . .
C14 C 0.1861(3) 0.4287(3) 0.3769(3) 0.0561(11) Uani 1 1 d . . . . .
H14 H 0.197729 0.418654 0.333926 0.067 Uiso 1 1 calc R U . . .
C31 C 0.6210(3) 0.3924(4) 0.7626(3) 0.0686(13) Uani 1 1 d . . . . .
H31 H 0.583264 0.347242 0.728973 0.082 Uiso 1 1 calc R U . . .
C36 C 0.1121(4) 0.9839(5) 0.4764(3) 0.0717(14) Uani 1 1 d . . . . .
C38 C 0.2164(3) 0.7536(4) 0.6837(3) 0.0601(12) Uani 1 1 d . . . . .
H38 H 0.198308 0.820619 0.679590 0.072 Uiso 1 1 calc R U . . .
C21 C 0.4500(3) 0.1314(3) 0.5149(3) 0.0579(11) Uani 1 1 d . . . . .
H21 H 0.452187 0.139369 0.467398 0.069 Uiso 1 1 calc R U . . .
C19 C 0.4227(3) 0.0241(4) 0.6025(3) 0.0652(13) Uani 1 1 d . . . . .
C22 C 0.5820(3) 0.7833(3) 0.6863(3) 0.0620(12) Uani 1 1 d . . . . .
H22 H 0.533867 0.800395 0.644279 0.074 Uiso 1 1 calc R U . . .
C37 C 0.0833(4) 0.8840(5) 0.4407(4) 0.0942(10) Uani 1 1 d . . . . .
C30 C 0.6769(3) 0.3551(4) 0.8310(3) 0.0755(15) Uani 1 1 d . . . . .
H30 H 0.676024 0.287061 0.843392 0.091 Uiso 1 1 calc R U . . .
C29 C 0.7330(4) 0.4199(5) 0.8799(3) 0.0793(16) Uani 1 1 d . . . . .
H29 H 0.771852 0.397267 0.926466 0.095 Uiso 1 1 calc R U . . .
C28 C 0.7313(3) 0.5199(5) 0.8590(3) 0.0726(15) Uani 1 1 d . . . . .
H28 H 0.769573 0.565516 0.891563 0.087 Uiso 1 1 calc R U . . .
C10 C 0.2311(3) 0.4726(4) 0.5069(3) 0.0656(13) Uani 1 1 d . . . . .
H10 H 0.273222 0.491171 0.552958 0.079 Uiso 1 1 calc R U . . .
C12 C 0.0880(3) 0.4280(4) 0.4345(4) 0.0732(15) Uani 1 1 d . . . . .
C26 C 0.6654(3) 0.6611(4) 0.7671(3) 0.0534(10) Uani 1 1 d . . . . .
C11 C 0.1494(4) 0.4593(4) 0.5018(4) 0.0814(17) Uani 1 1 d . . . . .
H11 H 0.136391 0.471644 0.543808 0.098 Uiso 1 1 calc R U . . .
C13 C 0.1060(3) 0.4140(4) 0.3727(3) 0.0721(15) Uani 1 1 d . . . . .
H13 H 0.063836 0.394279 0.327005 0.087 Uiso 1 1 calc R U . . .
C23 C 0.6345(4) 0.8597(4) 0.7259(3) 0.0802(16) Uani 1 1 d . . . . .
H23 H 0.621004 0.927143 0.712329 0.096 Uiso 1 1 calc R U . . .
C17 C 0.4623(4) 0.1977(4) 0.6328(3) 0.0799(17) Uani 1 1 d . . . . .
H17 H 0.472500 0.251816 0.666422 0.096 Uiso 1 1 calc R U . . .
C35 C 0.1837(4) 0.9954(6) 0.5422(4) 0.0944(19) Uani 1 1 d . . . . .
H35 H 0.214863 0.938534 0.565857 0.113 Uiso 1 1 calc R U . . .
C18 C 0.4388(4) 0.1047(5) 0.6513(3) 0.0874(19) Uani 1 1 d . . . . .
H18 H 0.433677 0.096743 0.697615 0.105 Uiso 1 1 calc R U . . .
C4 C 0.0019(4) 0.8677(5) 0.3909(4) 0.098(2) Uani 1 1 d . . . . .
H4 H -0.037001 0.920333 0.378281 0.118 Uiso 1 1 calc R U . . .
C24 C 0.7068(4) 0.8352(4) 0.7853(4) 0.0853(17) Uani 1 1 d . . . . .
H24 H 0.745289 0.885416 0.810868 0.102 Uiso 1 1 calc R U . . .
C25 C 0.7228(4) 0.7348(4) 0.8076(3) 0.0773(15) Uani 1 1 d . . . . .
H25 H 0.771311 0.717065 0.849097 0.093 Uiso 1 1 calc R U . . .
C39 C 0.1152(4) 0.7195(5) 0.4265(4) 0.0942(10) Uani 1 1 d . . . . .
H39 H 0.154748 0.667850 0.437627 0.113 Uiso 1 1 calc R U . . .
C32 C 0.0904(5) 1.1551(6) 0.4741(4) 0.103(2) Uani 1 1 d . . . . .
H32 H 0.057728 1.211208 0.451078 0.124 Uiso 1 1 calc R U . . .
C34 C 0.2091(5) 1.0893(8) 0.5729(4) 0.115(2) Uani 1 1 d . . . . .
H34 H 0.257877 1.097342 0.616419 0.138 Uiso 1 1 calc R U . . .
C33 C 0.1613(5) 1.1710(7) 0.5379(5) 0.118(3) Uani 1 1 d . . . . .
H33 H 0.176621 1.236014 0.557141 0.141 Uiso 1 1 calc R U . . .
C41 C -0.0217(5) 0.7735(6) 0.3599(5) 0.120(3) Uani 1 1 d . . . . .
H41 H -0.076946 0.761559 0.326630 0.144 Uiso 1 1 calc R U . . .
C40 C 0.0354(6) 0.6981(6) 0.3778(6) 0.126(3) Uani 1 1 d . . . . .
H40 H 0.020657 0.633476 0.357447 0.152 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
Dy1 O1 2.427(3) . ?
Dy1 O2 2.449(3) . ?
Dy1 O6 2.318(3) 3_666 ?
Dy1 O4 2.321(3) 3_666 ?
Dy1 O5 2.299(3) . ?
Dy1 O3 2.305(3) . ?
Dy1 N2 2.581(4) . ?
Dy1 N1 2.552(3) . ?
O1 C1 1.260(5) . ?
O2 C1 1.271(5) . ?
O6 C15 1.251(5) . ?
O4 C8 1.259(5) . ?
O5 C15 1.257(5) . ?
O3 C8 1.245(5) . ?
O7 H7 0.8200 . ?
O7 C5 1.365(5) . ?
N2 C27 1.340(6) . ?
N2 C31 1.329(6) . ?
O11 H11A 0.8497 . ?
O11 H11B 0.8500 . ?
N1 C22 1.339(6) . ?
N1 C26 1.352(6) . ?
O9 H9 0.8200 . ?
O9 C19 1.360(5) . ?
C2 C1 1.486(5) . ?
C2 C7 1.386(6) . ?
C2 C3 1.387(6) . ?
O10 H10A 0.8499 . ?
O10 H10B 0.8506 . ?
C8 C9 1.498(5) . ?
C9 C14 1.387(6) . ?
C9 C10 1.371(7) . ?
C5 C6 1.377(6) . ?
C5 C38 1.378(6) . ?
C7 H7A 0.9300 . ?
C7 C6 1.381(6) . ?
N3 C36 1.345(7) . ?
N3 C32 1.324(8) . ?
C15 C16 1.495(6) . ?
C27 C28 1.378(7) . ?
C27 C26 1.485(6) . ?
C6 H6 0.9300 . ?
C16 C21 1.358(6) . ?
C16 C17 1.398(7) . ?
N38 C37 1.342(7) . ?
N38 C39 1.341(8) . ?
O8 H8 0.8200 . ?
O8 C12 1.371(5) . ?
C3 H3 0.9300 . ?
C3 C38 1.384(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.387(6) . ?
C20 C19 1.357(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.371(6) . ?
C31 H31 0.9300 . ?
C31 C30 1.377(7) . ?
C36 C37 1.478(9) . ?
C36 C35 1.385(9) . ?
C38 H38 0.9300 . ?
C21 H21 0.9300 . ?
C19 C18 1.370(8) . ?
C22 H22 0.9300 . ?
C22 C23 1.370(7) . ?
C37 C4 1.374(9) . ?
C30 H30 0.9300 . ?
C30 C29 1.355(8) . ?
C29 H29 0.9300 . ?
C29 C28 1.375(8) . ?
C28 H28 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.391(7) . ?
C12 C11 1.372(8) . ?
C12 C13 1.349(8) . ?
C26 C25 1.388(6) . ?
C11 H11 0.9300 . ?
C13 H13 0.9300 . ?
C23 H23 0.9300 . ?
C23 C24 1.359(8) . ?
C17 H17 0.9300 . ?
C17 C18 1.383(7) . ?
C35 H35 0.9300 . ?
C35 C34 1.368(11) . ?
C18 H18 0.9300 . ?
C4 H4 0.9300 . ?
C4 C41 1.368(10) . ?
C24 H24 0.9300 . ?
C24 C25 1.385(8) . ?
C25 H25 0.9300 . ?
C39 H39 0.9300 . ?
C39 C40 1.357(10) . ?
C32 H32 0.9300 . ?
C32 C33 1.365(10) . ?
C34 H34 0.9300 . ?
C34 C33 1.362(11) . ?
C33 H33 0.9300 . ?
C41 H41 0.9300 . ?
C41 C40 1.349(10) . ?
C40 H40 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
O1 Dy1 O2 53.36(9) . . ?
O1 Dy1 N2 109.46(11) . . ?
O1 Dy1 N1 72.21(11) . . ?
O2 Dy1 N2 74.32(10) . . ?
O2 Dy1 N1 89.40(11) . . ?
O6 Dy1 O1 78.26(10) 3_666 . ?
O6 Dy1 O2 131.03(10) 3_666 . ?
O6 Dy1 O4 77.69(11) 3_666 3_666 ?
O6 Dy1 N2 137.33(11) 3_666 . ?
O6 Dy1 N1 81.72(11) 3_666 . ?
O4 Dy1 O1 141.88(10) 3_666 . ?
O4 Dy1 O2 145.76(11) 3_666 . ?
O4 Dy1 N2 71.44(11) 3_666 . ?
O4 Dy1 N1 75.42(11) 3_666 . ?
O5 Dy1 O1 134.96(10) . . ?
O5 Dy1 O2 88.69(10) . . ?
O5 Dy1 O6 128.40(10) . 3_666 ?
O5 Dy1 O4 83.05(10) . 3_666 ?
O5 Dy1 O3 74.06(11) . . ?
O5 Dy1 N2 76.48(11) . . ?
O5 Dy1 N1 137.99(11) . . ?
O3 Dy1 O1 77.17(12) . . ?
O3 Dy1 O2 82.20(11) . . ?
O3 Dy1 O6 79.99(11) . 3_666 ?
O3 Dy1 O4 126.41(12) . 3_666 ?
O3 Dy1 N2 142.45(12) . . ?
O3 Dy1 N1 146.88(12) . . ?
N1 Dy1 N2 62.68(12) . . ?
C1 O1 Dy1 93.9(2) . . ?
C1 O2 Dy1 92.6(2) . . ?
C15 O6 Dy1 140.8(3) . 3_666 ?
C8 O4 Dy1 122.0(3) . 3_666 ?
C15 O5 Dy1 139.4(3) . . ?
C8 O3 Dy1 166.8(3) . . ?
C5 O7 H7 109.5 . . ?
C27 N2 Dy1 120.9(3) . . ?
C31 N2 Dy1 121.7(3) . . ?
C31 N2 C27 117.2(4) . . ?
H11A O11 H11B 112.3 . . ?
C22 N1 Dy1 119.6(3) . . ?
C22 N1 C26 118.0(4) . . ?
C26 N1 Dy1 120.9(3) . . ?
C19 O9 H9 109.5 . . ?
C7 C2 C1 121.4(4) . . ?
C7 C2 C3 118.8(4) . . ?
C3 C2 C1 119.7(4) . . ?
O1 C1 O2 119.8(3) . . ?
O1 C1 C2 119.2(4) . . ?
O2 C1 C2 120.9(4) . . ?
H10A O10 H10B 117.9 . . ?
O4 C8 C9 117.0(4) . . ?
O3 C8 O4 123.8(4) . . ?
O3 C8 C9 119.1(4) . . ?
C14 C9 C8 120.6(4) . . ?
C10 C9 C8 121.1(4) . . ?
C10 C9 C14 118.3(4) . . ?
O7 C5 C6 117.7(4) . . ?
O7 C5 C38 122.2(4) . . ?
C6 C5 C38 120.1(4) . . ?
C2 C7 H7A 119.9 . . ?
C6 C7 C2 120.2(4) . . ?
C6 C7 H7A 119.9 . . ?
C32 N3 C36 117.9(6) . . ?
O6 C15 O5 125.6(4) . . ?
O6 C15 C16 117.8(4) . . ?
O5 C15 C16 116.6(4) . . ?
N2 C27 C28 121.4(5) . . ?
N2 C27 C26 116.3(4) . . ?
C28 C27 C26 122.2(4) . . ?
C5 C6 C7 120.4(4) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C21 C16 C15 121.9(4) . . ?
C21 C16 C17 117.2(4) . . ?
C17 C16 C15 120.8(4) . . ?
C39 N38 C37 116.5(6) . . ?
C12 O8 H8 109.5 . . ?
C2 C3 H3 119.5 . . ?
C38 C3 C2 121.0(4) . . ?
C38 C3 H3 119.5 . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.3(4) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.8(5) . . ?
C13 C14 H14 119.6 . . ?
N2 C31 H31 117.9 . . ?
N2 C31 C30 124.2(5) . . ?
C30 C31 H31 117.9 . . ?
N3 C36 C37 117.3(5) . . ?
N3 C36 C35 120.3(6) . . ?
C35 C36 C37 122.4(6) . . ?
C5 C38 C3 119.4(4) . . ?
C5 C38 H38 120.3 . . ?
C3 C38 H38 120.3 . . ?
C16 C21 C20 122.2(4) . . ?
C16 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
O9 C19 C18 117.7(5) . . ?
C20 C19 O9 123.2(5) . . ?
C20 C19 C18 118.8(4) . . ?
N1 C22 H22 118.3 . . ?
N1 C22 C23 123.4(5) . . ?
C23 C22 H22 118.3 . . ?
N38 C37 C36 116.5(6) . . ?
N38 C37 C4 121.7(7) . . ?
C4 C37 C36 121.9(6) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 C31 118.4(5) . . ?
C29 C30 H30 120.8 . . ?
C30 C29 H29 120.8 . . ?
C30 C29 C28 118.5(5) . . ?
C28 C29 H29 120.8 . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.3(5) . . ?
C29 C28 H28 119.8 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.6(5) . . ?
C11 C10 H10 119.7 . . ?
O8 C12 C11 117.8(6) . . ?
C13 C12 O8 121.9(5) . . ?
C13 C12 C11 120.2(4) . . ?
N1 C26 C27 115.6(4) . . ?
N1 C26 C25 121.2(5) . . ?
C25 C26 C27 123.2(4) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(5) . . ?
C12 C11 H11 120.2 . . ?
C14 C13 H13 119.8 . . ?
C12 C13 C14 120.5(5) . . ?
C12 C13 H13 119.8 . . ?
C22 C23 H23 120.6 . . ?
C24 C23 C22 118.7(5) . . ?
C24 C23 H23 120.6 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.3(5) . . ?
C18 C17 H17 119.8 . . ?
C36 C35 H35 119.7 . . ?
C34 C35 C36 120.7(7) . . ?
C34 C35 H35 119.7 . . ?
C19 C18 C17 120.9(5) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C37 C4 H4 120.2 . . ?
C41 C4 C37 119.6(6) . . ?
C41 C4 H4 120.2 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.5(5) . . ?
C25 C24 H24 120.2 . . ?
C26 C25 H25 120.5 . . ?
C24 C25 C26 119.0(5) . . ?
C24 C25 H25 120.5 . . ?
N38 C39 H39 117.6 . . ?
N38 C39 C40 124.7(6) . . ?
C40 C39 H39 117.6 . . ?
N3 C32 H32 117.9 . . ?
N3 C32 C33 124.2(7) . . ?
C33 C32 H32 117.9 . . ?
C35 C34 H34 120.8 . . ?
C33 C34 C35 118.4(7) . . ?
C33 C34 H34 120.8 . . ?
C32 C33 H33 120.7 . . ?
C34 C33 C32 118.5(7) . . ?
C34 C33 H33 120.7 . . ?
C4 C41 H41 120.1 . . ?
C40 C41 C4 119.7(7) . . ?
C40 C41 H41 120.1 . . ?
C39 C40 H40 121.1 . . ?
C41 C40 C39 117.8(7) . . ?
C41 C40 H40 121.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C1 O2 5.8(4) . . . . ?
Dy1 O1 C1 C2 -172.5(3) . . . . ?
Dy1 O2 C1 O1 -5.7(4) . . . . ?
Dy1 O2 C1 C2 172.5(3) . . . . ?
Dy1 O6 C15 O5 -17.4(7) 3_666 . . . ?
Dy1 O6 C15 C16 162.6(3) 3_666 . . . ?
Dy1 O4 C8 O3 10.4(6) 3_666 . . . ?
Dy1 O4 C8 C9 -169.4(2) 3_666 . . . ?
Dy1 O5 C15 O6 35.6(6) . . . . ?
Dy1 O5 C15 C16 -144.5(3) . . . . ?
Dy1 O3 C8 O4 -20.0(16) . . . . ?
Dy1 O3 C8 C9 159.8(11) . . . . ?
Dy1 N2 C27 C28 -176.2(4) . . . . ?
Dy1 N2 C27 C26 6.6(5) . . . . ?
Dy1 N2 C31 C30 177.1(4) . . . . ?
Dy1 N1 C22 C23 -164.6(4) . . . . ?
Dy1 N1 C26 C27 -20.7(5) . . . . ?
Dy1 N1 C26 C25 161.7(4) . . . . ?
O6 C15 C16 C21 6.1(6) . . . . ?
O6 C15 C16 C17 -168.9(4) . . . . ?
O4 C8 C9 C14 -3.7(6) . . . . ?
O4 C8 C9 C10 176.7(4) . . . . ?
O5 C15 C16 C21 -173.9(4) . . . . ?
O5 C15 C16 C17 11.1(6) . . . . ?
O3 C8 C9 C14 176.5(4) . . . . ?
O3 C8 C9 C10 -3.1(6) . . . . ?
O7 C5 C6 C7 175.2(4) . . . . ?
O7 C5 C38 C3 -174.0(4) . . . . ?
N2 C27 C28 C29 -0.8(8) . . . . ?
N2 C27 C26 N1 8.9(6) . . . . ?
N2 C27 C26 C25 -173.6(4) . . . . ?
N2 C31 C30 C29 -1.0(9) . . . . ?
N1 C22 C23 C24 2.8(8) . . . . ?
N1 C26 C25 C24 2.6(8) . . . . ?
O9 C19 C18 C17 -178.3(6) . . . . ?
C2 C7 C6 C5 -0.1(8) . . . . ?
C2 C3 C38 C5 -2.2(7) . . . . ?
C1 C2 C7 C6 -173.5(4) . . . . ?
C1 C2 C3 C38 174.8(4) . . . . ?
C8 C9 C14 C13 -179.6(4) . . . . ?
C8 C9 C10 C11 178.4(5) . . . . ?
C9 C14 C13 C12 -0.2(8) . . . . ?
C9 C10 C11 C12 2.6(9) . . . . ?
C7 C2 C1 O1 160.2(4) . . . . ?
C7 C2 C1 O2 -18.0(6) . . . . ?
C7 C2 C3 C38 -0.7(7) . . . . ?
N3 C36 C37 N38 160.9(6) . . . . ?
N3 C36 C37 C4 -19.3(9) . . . . ?
N3 C36 C35 C34 -2.1(10) . . . . ?
N3 C32 C33 C34 -0.8(13) . . . . ?
C15 C16 C21 C20 -178.7(4) . . . . ?
C15 C16 C17 C18 179.5(5) . . . . ?
C27 N2 C31 C30 0.7(7) . . . . ?
C27 C26 C25 C24 -174.8(5) . . . . ?
C6 C5 C38 C3 4.0(7) . . . . ?
C16 C17 C18 C19 -0.6(10) . . . . ?
N38 C37 C4 C41 0.4(12) . . . . ?
N38 C39 C40 C41 1.7(13) . . . . ?
O8 C12 C11 C10 -179.4(6) . . . . ?
O8 C12 C13 C14 178.1(5) . . . . ?
C3 C2 C1 O1 -15.1(6) . . . . ?
C3 C2 C1 O2 166.7(4) . . . . ?
C3 C2 C7 C6 1.9(7) . . . . ?
C20 C19 C18 C17 -3.9(10) . . . . ?
C14 C9 C10 C11 -1.3(7) . . . . ?
C31 N2 C27 C28 0.3(7) . . . . ?
C31 N2 C27 C26 -176.9(4) . . . . ?
C31 C30 C29 C28 0.4(9) . . . . ?
C36 N3 C32 C33 0.1(11) . . . . ?
C36 C37 C4 C41 -179.4(7) . . . . ?
C36 C35 C34 C33 1.4(12) . . . . ?
C38 C5 C6 C7 -2.8(8) . . . . ?
C21 C16 C17 C18 4.2(8) . . . . ?
C21 C20 C19 O9 178.6(5) . . . . ?
C21 C20 C19 C18 4.6(8) . . . . ?
C19 C20 C21 C16 -0.8(8) . . . . ?
C22 N1 C26 C27 173.4(4) . . . . ?
C22 N1 C26 C25 -4.2(6) . . . . ?
C22 C23 C24 C25 -4.4(9) . . . . ?
C37 N38 C39 C40 -2.1(11) . . . . ?
C37 C36 C35 C34 178.8(7) . . . . ?
C37 C4 C41 C40 -0.8(13) . . . . ?
C30 C29 C28 C27 0.5(9) . . . . ?
C28 C27 C26 N1 -168.3(4) . . . . ?
C28 C27 C26 C25 9.3(7) . . . . ?
C10 C9 C14 C13 0.1(7) . . . . ?
C26 N1 C22 C23 1.5(7) . . . . ?
C26 C27 C28 C29 176.2(5) . . . . ?
C11 C12 C13 C14 1.5(9) . . . . ?
C13 C12 C11 C10 -2.6(9) . . . . ?
C23 C24 C25 C26 1.8(9) . . . . ?
C17 C16 C21 C20 -3.6(7) . . . . ?
C35 C36 C37 N38 -20.0(9) . . . . ?
C35 C36 C37 C4 159.8(7) . . . . ?
C35 C34 C33 C32 0.0(13) . . . . ?
C4 C41 C40 C39 -0.1(14) . . . . ?
C39 N38 C37 C36 -179.2(6) . . . . ?
C39 N38 C37 C4 1.0(10) . . . . ?
C32 N3 C36 C37 -179.6(6) . . . . ?
C32 N3 C36 C35 1.3(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
