# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_ce545a
_database_code_depnum_ccdc_archive 'CCDC 1937367'
loop_
_audit_author_name
_audit_author_address
'William Harrison'
;University of Aberdeen
United Kingdom
;
_audit_update_record             
;
2019-06-30 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H10 Ce Cl O9'
_chemical_formula_sum            'C8 H10 Ce Cl O9'
_chemical_formula_weight         425.73

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'
Cl Cl 0.3639 0.7018 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.9439(3)
_cell_length_b                   9.7400(4)
_cell_length_c                   10.3973(4)
_cell_angle_alpha                63.431(4)
_cell_angle_beta                 77.659(4)
_cell_angle_gamma                73.969(4)
_cell_volume                     601.15(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4093
_cell_measurement_theta_min      4.76
_cell_measurement_theta_max      70.93

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.352
_exptl_crystal_F_000             410
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    31.740
_shelx_estimated_absorpt_T_min   0.022
_shelx_estimated_absorpt_T_max   0.038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.187
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
#_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku SuperNova CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6012
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.782
_diffrn_reflns_theta_max         71.131
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2291
_reflns_number_gt                2157
_reflns_threshold_expression     'I > 2σ(I)'

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 '
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2291
_refine_ls_number_parameters     174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0640
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.06696(3) 0.23345(2) 1.05100(2) 0.01500(9) Uani 1 1 d . . . . .
C1 C 0.2847(6) 0.3933(5) 0.5614(4) 0.0160(8) Uani 1 1 d . . . . .
C2 C 0.2110(7) 0.5378(5) 0.5701(4) 0.0199(9) Uani 1 1 d . . . . .
H2 H 0.177736 0.541529 0.660176 0.024 Uiso 1 1 calc R U . . .
C3 C 0.1870(7) 0.6755(5) 0.4460(5) 0.0193(9) Uani 1 1 d . . . . .
C4 C 0.2252(6) 0.6707(5) 0.3109(4) 0.0149(8) Uani 1 1 d . . . . .
C5 C 0.3045(6) 0.5259(5) 0.3012(4) 0.0177(9) Uani 1 1 d . . . . .
H5A H 0.333918 0.521766 0.211216 0.021 Uiso 1 1 calc R U . . .
C6 C 0.3387(6) 0.3896(5) 0.4254(4) 0.0159(8) Uani 1 1 d . . . . .
C7 C 0.3000(6) 0.2453(5) 0.6975(4) 0.0182(9) Uani 1 1 d . . . . .
C8 C 0.1785(6) 0.8140(5) 0.1761(4) 0.0165(8) Uani 1 1 d . . . . .
O1 O 0.3909(5) 0.1181(4) 0.6852(3) 0.0292(8) Uani 1 1 d . . . . .
O2 O 0.2215(5) 0.2510(4) 0.8158(3) 0.0274(7) Uani 1 1 d . . . . .
O3 O 0.1829(5) 0.8018(4) 0.0602(3) 0.0215(6) Uani 1 1 d . . . . .
O4 O 0.1359(5) 0.9465(3) 0.1840(3) 0.0246(7) Uani 1 1 d . . . . .
O5 O 0.1198(6) 0.8124(4) 0.4638(3) 0.0326(9) Uani 1 1 d . . . . .
H5 H 0.110889 0.886859 0.384433 0.039 Uiso 1 1 calc R U . . .
O6 O 0.4223(5) 0.2520(3) 0.4095(3) 0.0246(7) Uani 1 1 d . . . . .
H6 H 0.449149 0.180952 0.488356 0.030 Uiso 1 1 calc R U . . .
Cl1 Cl 0.24722(17) 0.50195(12) 0.95183(13) 0.0287(2) Uani 1 1 d . . . . .
O7 O 0.1311(5) 0.1983(4) 1.2916(4) 0.0327(8) Uani 1 1 d . . . . .
H1W H 0.044324 0.186168 1.376061 0.039 Uiso 1 1 d R U . . .
H2W H 0.245224 0.208368 1.318561 0.039 Uiso 1 1 d R U . . .
O8 O -0.2168(5) 0.1380(4) 1.2518(3) 0.0276(7) Uani 1 1 d . . . . .
H3W H -0.322904 0.201307 1.280657 0.033 Uiso 1 1 d R U . . .
H4W H -0.239004 0.046607 1.283757 0.033 Uiso 1 1 d R U . . .
O9 O 0.4333(5) 0.1343(4) 1.0815(4) 0.0324(8) Uani 1 1 d . . . . .
H5W H 0.479046 0.049924 1.160352 0.039 Uiso 1 1 d R U . . .
H6W H 0.521614 0.192824 1.027870 0.039 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
Ce1 O2 2.402(3) . ?
Ce1 O3 2.451(3) 2_566 ?
Ce1 O4 2.457(3) 1_546 ?
Ce1 O7 2.490(3) . ?
Ce1 O9 2.493(3) . ?
Ce1 O8 2.573(3) . ?
Ce1 Cl1 2.8734(11) 2_567 ?
Ce1 Cl1 2.8832(11) . ?
C1 C2 1.395(6) . ?
C1 C6 1.398(5) . ?
C1 C7 1.499(5) . ?
C2 C3 1.383(6) . ?
C2 H2 0.9300 . ?
C3 O5 1.368(5) . ?
C3 C4 1.392(5) . ?
C4 C5 1.406(5) . ?
C4 C8 1.487(5) . ?
C5 C6 1.382(6) . ?
C5 H5A 0.9300 . ?
C6 O6 1.374(5) . ?
C7 O2 1.253(5) . ?
C7 O1 1.275(5) . ?
C8 O3 1.255(5) . ?
C8 O4 1.279(5) . ?
O5 H5 0.8200 . ?
O6 H6 0.8200 . ?
O7 H1W 0.9317 . ?
O7 H2W 0.9376 . ?
O8 H3W 0.9130 . ?
O8 H4W 0.8461 . ?
O9 H5W 0.9018 . ?
O9 H6W 0.8800 . ?

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 Ce1 O3 73.69(11) . 2_566 ?
O2 Ce1 O4 99.00(10) . 1_546 ?
O3 Ce1 O4 85.97(10) 2_566 1_546 ?
O2 Ce1 O7 144.58(12) . . ?
O3 Ce1 O7 139.94(11) 2_566 . ?
O4 Ce1 O7 77.81(11) 1_546 . ?
O2 Ce1 O9 76.02(11) . . ?
O3 Ce1 O9 137.74(11) 2_566 . ?
O4 Ce1 O9 70.40(11) 1_546 . ?
O7 Ce1 O9 69.65(11) . . ?
O2 Ce1 O8 145.00(11) . . ?
O3 Ce1 O8 73.14(10) 2_566 . ?
O4 Ce1 O8 67.83(10) 1_546 . ?
O7 Ce1 O8 66.83(11) . . ?
O9 Ce1 O8 124.26(11) . . ?
O2 Ce1 Cl1 114.44(8) . 2_567 ?
O3 Ce1 Cl1 80.78(7) 2_566 2_567 ?
O4 Ce1 Cl1 138.40(8) 1_546 2_567 ?
O7 Ce1 Cl1 87.48(8) . 2_567 ?
O9 Ce1 Cl1 139.40(9) . 2_567 ?
O8 Ce1 Cl1 70.60(7) . 2_567 ?
O2 Ce1 Cl1 79.04(8) . . ?
O3 Ce1 Cl1 128.20(7) 2_566 . ?
O4 Ce1 Cl1 142.01(8) 1_546 . ?
O7 Ce1 Cl1 82.48(9) . . ?
O9 Ce1 Cl1 72.38(8) . . ?
O8 Ce1 Cl1 131.66(7) . . ?
Cl1 Ce1 Cl1 71.68(4) 2_567 . ?
C2 C1 C6 119.1(4) . . ?
C2 C1 C7 119.5(4) . . ?
C6 C1 C7 121.3(4) . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
O5 C3 C2 116.9(4) . . ?
O5 C3 C4 122.9(4) . . ?
C2 C3 C4 120.2(4) . . ?
C3 C4 C5 119.4(4) . . ?
C3 C4 C8 121.9(4) . . ?
C5 C4 C8 118.7(4) . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
O6 C6 C5 117.5(4) . . ?
O6 C6 C1 122.0(4) . . ?
C5 C6 C1 120.5(4) . . ?
O2 C7 O1 123.3(4) . . ?
O2 C7 C1 119.5(4) . . ?
O1 C7 C1 117.1(4) . . ?
O3 C8 O4 122.6(4) . . ?
O3 C8 C4 119.9(4) . . ?
O4 C8 C4 117.5(4) . . ?
C7 O2 Ce1 173.8(3) . . ?
C8 O3 Ce1 133.6(3) . 2_566 ?
C8 O4 Ce1 146.5(3) . 1_564 ?
C3 O5 H5 109.5 . . ?
C6 O6 H6 109.5 . . ?
Ce1 Cl1 Ce1 108.32(4) 2_567 . ?
Ce1 O7 H1W 130.5 . . ?
Ce1 O7 H2W 129.2 . . ?
H1W O7 H2W 99.8 . . ?
Ce1 O8 H3W 125.2 . . ?
Ce1 O8 H4W 122.6 . . ?
H3W O8 H4W 110.5 . . ?
Ce1 O9 H5W 122.1 . . ?
Ce1 O9 H6W 121.0 . . ?
H5W O9 H6W 115.1 . . ?

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
C6 C1 C2 C3 1.5(7) . . . . ?
C7 C1 C2 C3 -177.1(4) . . . . ?
C1 C2 C3 O5 -178.0(4) . . . . ?
C1 C2 C3 C4 3.7(7) . . . . ?
O5 C3 C4 C5 176.5(4) . . . . ?
C2 C3 C4 C5 -5.3(7) . . . . ?
O5 C3 C4 C8 -5.4(7) . . . . ?
C2 C3 C4 C8 172.7(4) . . . . ?
C3 C4 C5 C6 1.7(7) . . . . ?
C8 C4 C5 C6 -176.4(4) . . . . ?
C4 C5 C6 O6 -178.0(4) . . . . ?
C4 C5 C6 C1 3.6(7) . . . . ?
C2 C1 C6 O6 176.4(4) . . . . ?
C7 C1 C6 O6 -4.9(7) . . . . ?
C2 C1 C6 C5 -5.2(7) . . . . ?
C7 C1 C6 C5 173.4(4) . . . . ?
C2 C1 C7 O2 9.8(7) . . . . ?
C6 C1 C7 O2 -168.8(4) . . . . ?
C2 C1 C7 O1 -171.6(4) . . . . ?
C6 C1 C7 O1 9.8(6) . . . . ?
C3 C4 C8 O3 -168.0(4) . . . . ?
C5 C4 C8 O3 10.0(6) . . . . ?
C3 C4 C8 O4 12.3(6) . . . . ?
C5 C4 C8 O4 -169.6(4) . . . . ?
O4 C8 O3 Ce1 -92.7(5) . . . 2_566 ?
C4 C8 O3 Ce1 87.6(5) . . . 2_566 ?
O3 C8 O4 Ce1 -6.5(8) . . . 1_564 ?
C4 C8 O4 Ce1 173.2(3) . . . 1_564 ?

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
O5 H5 O4 0.82 1.88 2.593(4) 145 . yes
O6 H6 O1 0.82 1.84 2.551(4) 144 . yes
O7 H1W O5 0.93 1.81 2.735(4) 173 2_567 yes
O7 H2W O6 0.94 1.93 2.843(5) 164 1_556 yes
O8 H3W O6 0.91 2.07 2.923(4) 156 1_456 yes
O8 H4W O1 0.85 2.03 2.825(5) 156 2_557 yes
O9 H5W O1 0.90 1.88 2.774(4) 172 2_657 yes
O9 H6W O3 0.88 2.07 2.842(4) 147 2_666 yes
C5 H5A Cl1 0.93 2.98 3.851(4) 156 1_554 yes

_refine_diff_density_max         0.844
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.155

####################################################################### 
# 
# 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_553z
_database_code_depnum_ccdc_archive 'CCDC 1937370'
loop_
_audit_author_name
_audit_author_address
'William Harrison'
;University of Aberdeen
United Kingdom
;
_audit_update_record             
;
2019-06-30 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;

# disorder model 

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 O11 Tb, 3(C2 H6 O), H2 O'
_chemical_formula_sum            'C18 H30 O15 Tb'
_chemical_formula_weight         645.34

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'
Tb Tb -9.1472 9.1891 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.52570(12)
_cell_length_b                   14.44759(14)
_cell_length_c                   14.23151(13)
_cell_angle_alpha                90
_cell_angle_beta                 106.7894(10)
_cell_angle_gamma                90
_cell_volume                     2465.64(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    11667
_cell_measurement_theta_min      4.82
_cell_measurement_theta_max      72.18
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    14.746
_shelx_estimated_absorpt_T_min   0.126
_shelx_estimated_absorpt_T_max   0.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3668
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS '
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17599
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.148
_diffrn_reflns_theta_max         72.262
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4797
_reflns_number_gt                4471
_reflns_threshold_expression     'I > 2σ(I)'

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0399P)²+2.4828P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4797
_refine_ls_number_parameters     343
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.60346(2) 0.46636(2) 0.41532(2) 0.00899(7) Uani 1 1 d . . . . .
C1 C 0.2978(2) 0.2975(2) 0.3721(2) 0.0138(6) Uani 1 1 d . . . . .
C2 C 0.3488(2) 0.2670(2) 0.3022(2) 0.0152(6) Uani 1 1 d . . . . .
H2 H 0.421248 0.288606 0.305007 0.018 Uiso 1 1 calc R U . . .
C3 C 0.2950(2) 0.2057(2) 0.2292(2) 0.0138(6) Uani 1 1 d . . . . .
C4 C 0.1889(2) 0.1716(2) 0.2262(2) 0.0127(6) Uani 1 1 d . . . . .
C5 C 0.1394(2) 0.2002(2) 0.2975(2) 0.0162(6) Uani 1 1 d . . . . .
H5A H 0.068458 0.176370 0.296641 0.019 Uiso 1 1 calc R U . . .
C6 C 0.1925(2) 0.2627(2) 0.3696(2) 0.0161(6) Uani 1 1 d . . . . .
C7 C 0.3542(2) 0.3689(2) 0.4451(2) 0.0130(6) Uani 1 1 d . . . . .
C8 C 0.1264(2) 0.1068(2) 0.1473(2) 0.0134(6) Uani 1 1 d . . . . .
O1 O 0.44423(17) 0.40500(15) 0.44162(15) 0.0156(4) Uani 1 1 d . . . . .
O2 O 0.30662(18) 0.39471(16) 0.50829(16) 0.0173(5) Uani 1 1 d . . . . .
O3 O 0.17095(17) 0.08674(16) 0.07959(15) 0.0157(5) Uani 1 1 d . . . . .
O4 O 0.03486(17) 0.07634(16) 0.15173(15) 0.0159(5) Uani 1 1 d . . . . .
O5 O 0.34788(18) 0.18112(17) 0.16185(16) 0.0205(5) Uani 1 1 d . . . . .
H5 H 0.307022 0.147918 0.120109 0.025 Uiso 1 1 d R U . . .
O6 O 0.13906(19) 0.28958(19) 0.43650(18) 0.0268(6) Uani 1 1 d . . . . .
H6 H 0.174498 0.330851 0.471243 0.032 Uiso 1 1 d R U . . .
C9 C 0.5332(3) 0.4909(2) 0.1020(2) 0.0150(6) Uani 1 1 d . . . . .
C10 C 0.5754(3) 0.5630(2) 0.0580(2) 0.0156(6) Uani 1 1 d . . . . .
H10 H 0.626773 0.605766 0.097425 0.019 Uiso 1 1 calc R U . . .
C11 C 0.5424(3) 0.5722(2) -0.0427(2) 0.0158(6) Uani 1 1 d . . . . .
C12 C 0.5689(3) 0.4818(2) 0.2108(2) 0.0139(6) Uani 1 1 d . . . . .
O7 O 0.5228(2) 0.41717(16) 0.24816(15) 0.0199(5) Uani 1 1 d . . . . .
O8 O 0.63876(19) 0.53420(16) 0.26413(16) 0.0187(5) Uani 1 1 d . . . . .
O9 O 0.58522(19) 0.64434(17) -0.08259(15) 0.0204(5) Uani 1 1 d . . . . .
H9 H 0.559097 0.643746 -0.142281 0.024 Uiso 1 1 d R U . . .
O10 O 0.79636(19) 0.45318(17) 0.42943(19) 0.0237(5) Uani 1 1 d . . . . .
H10A H 0.841054 0.498981 0.414216 0.028 Uiso 1 1 d R U . . .
H10B H 0.839154 0.406481 0.447616 0.028 Uiso 1 1 d R U . . .
O11 O 0.6404(2) 0.30474(16) 0.40260(17) 0.0226(5) Uani 1 1 d . . . . .
H11A H 0.644454 0.261879 0.443342 0.027 Uiso 1 1 d R U . . .
H11B H 0.659455 0.298379 0.346143 0.027 Uiso 1 1 d R U . . .
O12 O 0.95082(19) 0.31559(17) 0.50027(18) 0.0240(5) Uani 1 1 d . . . . .
H12A H 0.942759 0.263962 0.533501 0.029 Uiso 1 1 d R U . . .
H12B H 1.000757 0.294263 0.473902 0.029 Uiso 1 1 d R U . . .
C13 C 0.6820(6) 0.0071(5) 0.5953(7) 0.097(3) Uani 1 1 d . . . . .
H13A H 0.695710 -0.019114 0.536381 0.145 Uiso 1 1 calc R U . . .
H13B H 0.633289 -0.034544 0.618661 0.145 Uiso 1 1 calc R U . . .
H13C H 0.752972 0.014400 0.646643 0.145 Uiso 1 1 calc R U . . .
C14 C 0.6284(5) 0.0968(4) 0.5721(6) 0.079(2) Uani 1 1 d . . . . .
H14A H 0.551832 0.086575 0.528859 0.095 Uiso 1 1 calc R U . . .
H14B H 0.621818 0.124429 0.633809 0.095 Uiso 1 1 calc R U . . .
O13 O 0.6799(2) 0.1607(2) 0.5272(2) 0.0475(8) Uani 1 1 d . . . . .
H13 H 0.749054 0.151301 0.544773 0.071 Uiso 1 1 calc R U . . .
C15 C 1.0183(6) 0.4749(4) 0.3025(6) 0.0762(19) Uani 1 1 d . . . . .
H15B H 1.033694 0.445212 0.245854 0.114 Uiso 1 1 calc R U . . .
H15C H 0.989362 0.428703 0.339315 0.114 Uiso 1 1 calc R U . . .
H15D H 1.087337 0.501523 0.345131 0.114 Uiso 1 1 calc R U . . .
C16 C 0.9363(5) 0.5476(4) 0.2688(5) 0.0617(16) Uani 1 1 d . . . . .
H16A H 0.968907 0.597515 0.238168 0.074 Uiso 1 1 calc R U . . .
H16B H 0.870960 0.522326 0.218378 0.074 Uiso 1 1 calc R U . . .
O14 O 0.9009(2) 0.5853(2) 0.3479(2) 0.0372(7) Uani 1 1 d . . . . .
H14 H 0.954566 0.612617 0.387366 0.045 Uiso 1 1 calc R U . . .
C17 C 0.7860(10) 0.3284(7) 0.1492(7) 0.072(3) Uani 0.676(13) 1 d D . P A 1
H17A H 0.726961 0.302503 0.094472 0.108 Uiso 0.676(13) 1 calc R U P A 1
H17B H 0.851938 0.341332 0.127360 0.108 Uiso 0.676(13) 1 calc R U P A 1
H17C H 0.759739 0.385901 0.171465 0.108 Uiso 0.676(13) 1 calc R U P A 1
C18 C 0.8157(6) 0.2605(5) 0.2316(5) 0.044(2) Uani 0.676(13) 1 d D . P A 1
H18A H 0.849681 0.206245 0.208866 0.053 Uiso 0.676(13) 1 calc R U P A 1
H18B H 0.874683 0.289167 0.285624 0.053 Uiso 0.676(13) 1 calc R U P A 1
O15 O 0.7355(6) 0.2278(5) 0.2711(5) 0.0401(14) Uani 0.676(13) 1 d D . P A 1
H15 H 0.699531 0.185252 0.235522 0.048 Uiso 0.676(13) 1 calc R U P A 1
C17A C 0.8539(14) 0.2826(15) 0.1725(18) 0.073(8) Uani 0.324(13) 1 d D . P A 2
H17D H 0.878822 0.336208 0.142205 0.109 Uiso 0.324(13) 1 calc R U P A 2
H17E H 0.841420 0.230018 0.127174 0.109 Uiso 0.324(13) 1 calc R U P A 2
H17F H 0.911071 0.266423 0.233396 0.109 Uiso 0.324(13) 1 calc R U P A 2
C18A C 0.7491(14) 0.3056(12) 0.1947(14) 0.058(6) Uani 0.324(13) 1 d D . P A 2
H18C H 0.762222 0.364152 0.232433 0.070 Uiso 0.324(13) 1 calc R U P A 2
H18D H 0.693105 0.319324 0.131246 0.070 Uiso 0.324(13) 1 calc R U P A 2
O15A O 0.7015(12) 0.2477(10) 0.2425(11) 0.036(3) Uani 0.324(13) 1 d D U P A 2
H15A H 0.640281 0.229579 0.204891 0.043 Uiso 0.324(13) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.310(2) . ?
Tb1 O4 2.341(2) 2 ?
Tb1 O3 2.372(2) 4_666 ?
Tb1 O10 2.374(2) . ?
Tb1 O11 2.398(2) . ?
Tb1 O2 2.402(2) 3_666 ?
Tb1 O7 2.408(2) . ?
Tb1 O8 2.517(2) . ?
Tb1 C12 2.826(3) . ?
C1 C2 1.399(4) . ?
C1 C6 1.402(4) . ?
C1 C7 1.489(4) . ?
C2 C3 1.383(4) . ?
C2 H2 0.9500 . ?
C3 O5 1.360(3) . ?
C3 C4 1.407(4) . ?
C4 C5 1.396(4) . ?
C4 C8 1.497(4) . ?
C5 C6 1.383(4) . ?
C5 H5A 0.9500 . ?
C6 O6 1.369(3) . ?
C7 O1 1.256(4) . ?
C7 O2 1.270(4) . ?
C8 O4 1.246(4) . ?
C8 O3 1.279(4) . ?
O5 H5 0.8180 . ?
O6 H6 0.8187 . ?
C9 C10 1.396(4) . ?
C9 C11 1.406(5) 3_665 ?
C9 C12 1.488(4) . ?
C10 C11 1.378(4) . ?
C10 H10 0.9500 . ?
C11 O9 1.368(4) . ?
C12 O8 1.238(4) . ?
C12 O7 1.291(4) . ?
O9 H9 0.8174 . ?
O10 H10A 0.9317 . ?
O10 H10B 0.8541 . ?
O11 H11A 0.8398 . ?
O11 H11B 0.9064 . ?
O12 H12A 0.9043 . ?
O12 H12B 0.8733 . ?
C13 C14 1.452(8) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 O13 1.383(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O13 H13 0.8400 . ?
C15 C16 1.451(8) . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15D 0.9800 . ?
C16 O14 1.432(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
O14 H14 0.8400 . ?
C17 C18 1.491(11) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O15 1.370(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
O15 H15 0.8400 . ?
C17A C18A 1.474(16) . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C18A O15A 1.324(16) . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
O15A H15A 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
O1 Tb1 O4 75.79(8) . 2 ?
O1 Tb1 O3 78.15(7) . 4_666 ?
O4 Tb1 O3 129.21(7) 2 4_666 ?
O1 Tb1 O10 149.43(8) . . ?
O4 Tb1 O10 134.77(8) 2 . ?
O3 Tb1 O10 80.00(8) 4_666 . ?
O1 Tb1 O11 80.39(8) . . ?
O4 Tb1 O11 140.04(8) 2 . ?
O3 Tb1 O11 74.80(8) 4_666 . ?
O10 Tb1 O11 73.39(8) . . ?
O1 Tb1 O2 124.14(7) . 3_666 ?
O4 Tb1 O2 79.19(8) 2 3_666 ?
O3 Tb1 O2 80.63(8) 4_666 3_666 ?
O10 Tb1 O2 72.30(8) . 3_666 ?
O11 Tb1 O2 140.56(8) . 3_666 ?
O1 Tb1 O7 84.90(7) . . ?
O4 Tb1 O7 75.38(8) 2 . ?
O3 Tb1 O7 143.77(8) 4_666 . ?
O10 Tb1 O7 100.75(8) . . ?
O11 Tb1 O7 70.91(8) . . ?
O2 Tb1 O7 134.58(8) 3_666 . ?
O1 Tb1 O8 131.39(7) . . ?
O4 Tb1 O8 71.30(7) 2 . ?
O3 Tb1 O8 150.21(7) 4_666 . ?
O10 Tb1 O8 71.20(8) . . ?
O11 Tb1 O8 103.26(8) . . ?
O2 Tb1 O8 83.47(7) 3_666 . ?
O7 Tb1 O8 52.96(7) . . ?
O1 Tb1 C12 108.35(8) . . ?
O4 Tb1 C12 69.61(8) 2 . ?
O3 Tb1 C12 161.05(8) 4_666 . ?
O10 Tb1 C12 86.71(9) . . ?
O11 Tb1 C12 88.53(8) . . ?
O2 Tb1 C12 108.22(8) 3_666 . ?
O7 Tb1 C12 27.08(8) . . ?
O8 Tb1 C12 25.97(8) . . ?
C2 C1 C6 119.2(3) . . ?
C2 C1 C7 119.5(3) . . ?
C6 C1 C7 121.3(3) . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
O5 C3 C2 117.8(3) . . ?
O5 C3 C4 122.4(3) . . ?
C2 C3 C4 119.9(3) . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 C8 119.0(3) . . ?
C3 C4 C8 121.8(3) . . ?
C6 C5 C4 120.9(3) . . ?
C6 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
O6 C6 C5 118.3(3) . . ?
O6 C6 C1 121.7(3) . . ?
C5 C6 C1 120.0(3) . . ?
O1 C7 O2 121.1(3) . . ?
O1 C7 C1 120.7(3) . . ?
O2 C7 C1 118.2(3) . . ?
O4 C8 O3 124.5(3) . . ?
O4 C8 C4 118.2(3) . . ?
O3 C8 C4 117.3(3) . . ?
C7 O1 Tb1 173.0(2) . . ?
C7 O2 Tb1 108.13(19) . 3_666 ?
C8 O3 Tb1 135.00(19) . 4_565 ?
C8 O4 Tb1 143.3(2) . 2_545 ?
C3 O5 H5 109.6 . . ?
C6 O6 H6 109.8 . . ?
C10 C9 C11 119.4(3) . 3_665 ?
C10 C9 C12 119.6(3) . . ?
C11 C9 C12 121.0(3) 3_665 . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
O9 C11 C10 118.0(3) . . ?
O9 C11 C9 121.4(3) . 3_665 ?
C10 C11 C9 120.6(3) . 3_665 ?
O8 C12 O7 120.7(3) . . ?
O8 C12 C9 122.1(3) . . ?
O7 C12 C9 117.2(3) . . ?
O8 C12 Tb1 62.95(16) . . ?
O7 C12 Tb1 58.11(15) . . ?
C9 C12 Tb1 171.6(2) . . ?
C12 O7 Tb1 94.80(18) . . ?
C12 O8 Tb1 91.08(18) . . ?
C11 O9 H9 109.6 . . ?
Tb1 O10 H10A 126.1 . . ?
Tb1 O10 H10B 128.6 . . ?
H10A O10 H10B 105.4 . . ?
Tb1 O11 H11A 129.8 . . ?
Tb1 O11 H11B 105.8 . . ?
H11A O11 H11B 124.0 . . ?
H12A O12 H12B 97.8 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O13 C14 C13 117.0(5) . . ?
O13 C14 H14A 108.0 . . ?
C13 C14 H14A 108.0 . . ?
O13 C14 H14B 108.0 . . ?
C13 C14 H14B 108.0 . . ?
H14A C14 H14B 107.3 . . ?
C14 O13 H13 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C15 H15D 109.5 . . ?
H15B C15 H15D 109.5 . . ?
H15C C15 H15D 109.5 . . ?
O14 C16 C15 111.5(5) . . ?
O14 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
O14 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C16 O14 H14 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O15 C18 C17 120.3(9) . . ?
O15 C18 H18A 107.3 . . ?
C17 C18 H18A 107.3 . . ?
O15 C18 H18B 107.3 . . ?
C17 C18 H18B 107.3 . . ?
H18A C18 H18B 106.9 . . ?
C18 O15 H15 109.5 . . ?
C18A C17A H17D 109.5 . . ?
C18A C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
C18A C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
O15A C18A C17A 122.0(18) . . ?
O15A C18A H18C 106.8 . . ?
C17A C18A H18C 106.8 . . ?
O15A C18A H18D 106.8 . . ?
C17A C18A H18D 106.8 . . ?
H18C C18A H18D 106.7 . . ?
C18A O15A H15A 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
C6 C1 C2 C3 2.3(5) . . . . ?
C7 C1 C2 C3 -175.4(3) . . . . ?
C1 C2 C3 O5 178.0(3) . . . . ?
C1 C2 C3 C4 -1.6(5) . . . . ?
O5 C3 C4 C5 -179.7(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
O5 C3 C4 C8 -0.8(5) . . . . ?
C2 C3 C4 C8 178.7(3) . . . . ?
C3 C4 C5 C6 1.3(5) . . . . ?
C8 C4 C5 C6 -177.6(3) . . . . ?
C4 C5 C6 O6 178.7(3) . . . . ?
C4 C5 C6 C1 -0.6(5) . . . . ?
C2 C1 C6 O6 179.5(3) . . . . ?
C7 C1 C6 O6 -2.9(5) . . . . ?
C2 C1 C6 C5 -1.2(5) . . . . ?
C7 C1 C6 C5 176.4(3) . . . . ?
C2 C1 C7 O1 3.4(5) . . . . ?
C6 C1 C7 O1 -174.2(3) . . . . ?
C2 C1 C7 O2 -179.3(3) . . . . ?
C6 C1 C7 O2 3.1(5) . . . . ?
C5 C4 C8 O4 -4.1(4) . . . . ?
C3 C4 C8 O4 177.0(3) . . . . ?
C5 C4 C8 O3 175.6(3) . . . . ?
C3 C4 C8 O3 -3.3(4) . . . . ?
O1 C7 O2 Tb1 11.2(3) . . . 3_666 ?
C1 C7 O2 Tb1 -166.1(2) . . . 3_666 ?
O4 C8 O3 Tb1 23.1(5) . . . 4_565 ?
C4 C8 O3 Tb1 -156.6(2) . . . 4_565 ?
O3 C8 O4 Tb1 11.5(6) . . . 2_545 ?
C4 C8 O4 Tb1 -168.8(2) . . . 2_545 ?
C11 C9 C10 C11 0.4(5) 3_665 . . . ?
C12 C9 C10 C11 -179.8(3) . . . . ?
C9 C10 C11 O9 179.5(3) . . . . ?
C9 C10 C11 C9 -0.4(5) . . . 3_665 ?
C10 C9 C12 O8 -2.9(5) . . . . ?
C11 C9 C12 O8 177.0(3) 3_665 . . . ?
C10 C9 C12 O7 176.2(3) . . . . ?
C11 C9 C12 O7 -4.0(4) 3_665 . . . ?
O8 C12 O7 Tb1 7.0(3) . . . . ?
C9 C12 O7 Tb1 -172.1(2) . . . . ?
O7 C12 O8 Tb1 -6.7(3) . . . . ?
C9 C12 O8 Tb1 172.3(3) . . . . ?

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
O5 H5 O3 0.82 1.86 2.577(3) 146 . yes
O6 H6 O2 0.82 1.83 2.553(3) 146 . yes
O9 H9 O7 0.82 1.79 2.516(3) 147 3_665 yes
O10 H10A O14 0.93 1.85 2.752(4) 163 . yes
O10 H10B O12 0.85 1.91 2.754(3) 171 . yes
O11 H11A O13 0.84 1.86 2.686(4) 168 . yes
O11 H11B O15 0.91 1.92 2.728(6) 148 . yes
O11 H11B O15A 0.91 1.85 2.732(13) 162 . yes
O12 H12A O9 0.90 1.93 2.829(3) 170 2_645 yes
O12 H12B O6 0.87 1.95 2.786(3) 159 1_655 yes
O13 H13 O9 0.84 1.99 2.827(4) 173 2_645 yes
O14 H14 O12 0.84 1.99 2.802(4) 164 3_766 yes
O15 H15 O14 0.84 2.05 2.891(6) 175 2_645 yes
O15A H15A O14 0.84 2.23 2.803(14) 126 2_645 yes
C2 H2 O7 0.95 2.51 3.319(4) 143 . yes
C17 H17A O6 0.98 2.57 3.498(10) 158 4_665 yes
C18 H18A O8 0.99 2.51 3.317(8) 138 2_645 yes
C17A H17E O2 0.98 2.42 3.403(18) 177 4_665 yes

_refine_diff_density_max         0.819
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.094

####################################################################### 
# 
# 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_551z
_database_code_depnum_ccdc_archive 'CCDC 1937368'
loop_
_audit_author_name
_audit_author_address
'William Harrison'
;University of Aberdeen
United Kingdom
;
_audit_update_record             
;
2019-06-30 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;

# disorder model for ethanol 

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 Eu O11, 3(C2 H6 O), H2 O'
_chemical_formula_sum            'C18 H30 Eu O15'
_chemical_formula_weight         638.38

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.5345(2)
_cell_length_b                   14.4309(2)
_cell_length_c                   14.2786(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.3480(10)
_cell_angle_gamma                90
_cell_volume                     2478.35(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    8533
_cell_measurement_theta_min      4.16
_cell_measurement_theta_max      71.02
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.490
_exptl_crystal_size_min          0.450
_exptl_absorpt_coefficient_mu    18.754
_shelx_estimated_absorpt_T_min   0.035
_shelx_estimated_absorpt_T_max   0.043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3657
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADBAS '
#_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14122
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.153
_diffrn_reflns_theta_max         71.186
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4720
_reflns_number_gt                4293
_reflns_threshold_expression     'I > 2σ(I)'

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0571P)²+1.7628P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4720
_refine_ls_number_parameters     343
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.60352(2) 0.46628(2) 0.41527(2) 0.00776(8) Uani 1 1 d . . . . .
C1 C 0.2970(3) 0.2974(3) 0.3733(2) 0.0139(7) Uani 1 1 d . . . . .
C2 C 0.3483(3) 0.2677(3) 0.3034(2) 0.0149(7) Uani 1 1 d . . . . .
H2 H 0.420505 0.289711 0.306083 0.018 Uiso 1 1 calc R U . . .
C3 C 0.2951(3) 0.2065(3) 0.2304(2) 0.0151(7) Uani 1 1 d . . . . .
C4 C 0.1896(3) 0.1721(3) 0.2276(2) 0.0122(7) Uani 1 1 d . . . . .
C5 C 0.1397(3) 0.2001(3) 0.2989(3) 0.0169(8) Uani 1 1 d . . . . .
H5A H 0.068840 0.176041 0.297939 0.020 Uiso 1 1 calc R U . . .
C6 C 0.1919(3) 0.2620(3) 0.3708(3) 0.0169(8) Uani 1 1 d . . . . .
C7 C 0.3523(3) 0.3684(3) 0.4469(2) 0.0134(7) Uani 1 1 d . . . . .
C8 C 0.1274(3) 0.1076(3) 0.1488(2) 0.0138(7) Uani 1 1 d . . . . .
O1 O 0.4420(2) 0.40579(19) 0.44378(18) 0.0159(5) Uani 1 1 d . . . . .
O2 O 0.3042(2) 0.3929(2) 0.51043(19) 0.0181(6) Uani 1 1 d . . . . .
O3 O 0.1724(2) 0.08871(19) 0.08050(18) 0.0158(5) Uani 1 1 d . . . . .
O4 O 0.0359(2) 0.0772(2) 0.15284(18) 0.0180(6) Uani 1 1 d . . . . .
O5 O 0.3485(2) 0.1825(2) 0.16328(19) 0.0225(6) Uani 1 1 d . . . . .
H5 H 0.307673 0.149281 0.121538 0.027 Uiso 1 1 d R U . . .
O6 O 0.1381(2) 0.2878(2) 0.4380(2) 0.0286(7) Uani 1 1 d . . . . .
H6 H 0.173503 0.329032 0.472793 0.034 Uiso 1 1 d R U . . .
C9 C 0.5328(3) 0.4906(3) 0.1016(3) 0.0145(7) Uani 1 1 d . . . . .
C10 C 0.5762(3) 0.5622(3) 0.0575(3) 0.0173(7) Uani 1 1 d . . . . .
H10 H 0.628423 0.604305 0.096494 0.021 Uiso 1 1 calc R U . . .
C11 C 0.5432(3) 0.5719(3) -0.0431(3) 0.0165(7) Uani 1 1 d . . . . .
C12 C 0.5689(3) 0.4809(3) 0.2096(3) 0.0145(7) Uani 1 1 d . . . . .
O7 O 0.5235(2) 0.4160(2) 0.24729(18) 0.0211(6) Uani 1 1 d . . . . .
O8 O 0.6391(2) 0.5334(2) 0.26240(19) 0.0206(6) Uani 1 1 d . . . . .
O9 O 0.5868(2) 0.6436(2) -0.08302(18) 0.0223(6) Uani 1 1 d . . . . .
H9 H 0.560678 0.643025 -0.142707 0.027 Uiso 1 1 d R U . . .
O10 O 0.7977(2) 0.4512(2) 0.4269(2) 0.0254(7) Uani 1 1 d . . . . .
H10A H 0.842368 0.496962 0.411692 0.030 Uiso 1 1 d R U . . .
H10B H 0.840468 0.404462 0.445092 0.030 Uiso 1 1 d R U . . .
O11 O 0.6389(3) 0.3025(2) 0.40234(19) 0.0245(6) Uani 1 1 d . . . . .
H11A H 0.642882 0.259629 0.443083 0.029 Uiso 1 1 d R U . . .
H11B H 0.657882 0.296129 0.345884 0.029 Uiso 1 1 d R U . . .
O12 O 0.9503(2) 0.3148(2) 0.5015(2) 0.0277(7) Uani 1 1 d . . . . .
H12A H 0.942289 0.263209 0.534772 0.033 Uiso 1 1 d R U . . .
H12B H 1.000288 0.293509 0.475172 0.033 Uiso 1 1 d R U . . .
C13 C 0.6804(9) 0.0058(7) 0.5941(10) 0.116(4) Uani 1 1 d . . . . .
H13A H 0.695393 -0.021710 0.536373 0.174 Uiso 1 1 calc R U . . .
H13B H 0.631697 -0.035366 0.618063 0.174 Uiso 1 1 calc R U . . .
H13C H 0.750567 0.014408 0.645238 0.174 Uiso 1 1 calc R U . . .
C14 C 0.6265(7) 0.0948(6) 0.5685(9) 0.101(4) Uani 1 1 d . . . . .
H14A H 0.552677 0.083425 0.521773 0.122 Uiso 1 1 calc R U . . .
H14B H 0.613330 0.121340 0.628220 0.122 Uiso 1 1 calc R U . . .
O13 O 0.6793(3) 0.1607(3) 0.5288(3) 0.0544(11) Uani 1 1 d . . . . .
H13 H 0.748366 0.152308 0.548616 0.082 Uiso 1 1 calc R U . . .
C15 C 1.0202(8) 0.4735(6) 0.3031(8) 0.083(3) Uani 1 1 d . . . . .
H15B H 1.034461 0.442333 0.246789 0.125 Uiso 1 1 calc R U . . .
H15C H 0.991760 0.428482 0.341461 0.125 Uiso 1 1 calc R U . . .
H15D H 1.089556 0.500502 0.343778 0.125 Uiso 1 1 calc R U . . .
C16 C 0.9379(6) 0.5471(5) 0.2689(6) 0.0614(18) Uani 1 1 d . . . . .
H16A H 0.970644 0.596865 0.238063 0.074 Uiso 1 1 calc R U . . .
H16B H 0.872792 0.521720 0.218980 0.074 Uiso 1 1 calc R U . . .
O14 O 0.9025(3) 0.5848(3) 0.3474(3) 0.0429(9) Uani 1 1 d . . . . .
H14 H 0.958150 0.603687 0.391197 0.051 Uiso 1 1 calc R U . . .
C17 C 0.7864(12) 0.3298(9) 0.1522(8) 0.082(4) Uani 0.705(15) 1 d D . P A 1
H17A H 0.728990 0.303301 0.097331 0.123 Uiso 0.705(15) 1 calc R U P A 1
H17B H 0.852213 0.345009 0.131074 0.123 Uiso 0.705(15) 1 calc R U P A 1
H17C H 0.757814 0.386124 0.174920 0.123 Uiso 0.705(15) 1 calc R U P A 1
C18 C 0.8171(7) 0.2610(6) 0.2334(6) 0.045(2) Uani 0.705(15) 1 d D . P A 1
H18A H 0.852387 0.207703 0.210172 0.054 Uiso 0.705(15) 1 calc R U P A 1
H18B H 0.874958 0.289912 0.287482 0.054 Uiso 0.705(15) 1 calc R U P A 1
O15 O 0.7372(7) 0.2263(5) 0.2722(6) 0.0424(16) Uani 0.705(15) 1 d D . P A 1
H15 H 0.709055 0.178644 0.241149 0.051 Uiso 0.705(15) 1 calc R U P A 1
C17A C 0.8566(17) 0.2810(17) 0.173(2) 0.069(9) Uani 0.295(15) 1 d D . P A 2
H17D H 0.880470 0.334475 0.141231 0.104 Uiso 0.295(15) 1 calc R U P A 2
H17E H 0.844477 0.227798 0.128032 0.104 Uiso 0.295(15) 1 calc R U P A 2
H17F H 0.914305 0.265619 0.232697 0.104 Uiso 0.295(15) 1 calc R U P A 2
C18A C 0.7518(18) 0.3036(13) 0.1960(17) 0.052(6) Uani 0.295(15) 1 d D . P A 2
H18C H 0.766078 0.360900 0.235682 0.062 Uiso 0.295(15) 1 calc R U P A 2
H18D H 0.696839 0.319877 0.133545 0.062 Uiso 0.295(15) 1 calc R U P A 2
O15A O 0.7009(15) 0.2447(12) 0.2418(13) 0.035(4) Uani 0.295(15) 1 d D U P A 2
H15A H 0.642085 0.225336 0.202429 0.041 Uiso 0.295(15) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag


# Eu1 Eu1 4.1317(3) 3_666 ?

Eu1 O1 2.343(2) . ?
Eu1 O4 2.367(3) 2 ?
Eu1 O10 2.402(3) . ?
Eu1 O3 2.407(2) 4_666 ?
Eu1 O11 2.421(3) . ?
Eu1 O2 2.429(3) 3_666 ?
Eu1 O7 2.435(3) . ?
Eu1 O8 2.540(3) . ?
C1 C2 1.398(5) . ?
C1 C6 1.404(5) . ?
C1 C7 1.492(5) . ?
C2 C3 1.386(5) . ?
C2 H2 0.9500 . ?
C3 O5 1.359(4) . ?
C3 C4 1.402(5) . ?
C4 C5 1.397(5) . ?
C4 C8 1.499(5) . ?
C5 C6 1.379(5) . ?
C5 H5A 0.9500 . ?
C6 O6 1.371(4) . ?
C7 O1 1.260(5) . ?
C7 O2 1.273(4) . ?
C8 O4 1.244(4) . ?
C8 O3 1.286(4) . ?
O5 H5 0.8217 . ?
O6 H6 0.8211 . ?
C9 C10 1.398(5) . ?
C9 C11 1.404(5) 3_665 ?
C9 C12 1.486(5) . ?
C10 C11 1.384(5) . ?
C10 H10 0.9500 . ?
C11 O9 1.368(5) . ?
C12 O8 1.243(5) . ?
C12 O7 1.289(5) . ?
O9 H9 0.8226 . ?
O10 H10A 0.9308 . ?
O10 H10B 0.8550 . ?
O11 H11A 0.8408 . ?
O11 H11B 0.9075 . ?
O12 H12A 0.9040 . ?
O12 H12B 0.8724 . ?
C13 C14 1.449(12) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 O13 1.370(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O13 H13 0.8400 . ?
C15 C16 1.466(11) . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15D 0.9800 . ?
C16 O14 1.424(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
O14 H14 0.8400 . ?
C17 C18 1.492(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O15 1.368(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
O15 H15 0.8400 . ?
C17A C18A 1.481(18) . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C18A O15A 1.338(17) . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
O15A H15A 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
O1 Eu1 O4 75.48(9) . 2 ?
O1 Eu1 O10 149.56(10) . . ?
O4 Eu1 O10 134.93(10) 2 . ?
O1 Eu1 O3 78.21(9) . 4_666 ?
O4 Eu1 O3 130.16(9) 2 4_666 ?
O10 Eu1 O3 79.95(9) . 4_666 ?
O1 Eu1 O11 80.50(10) . . ?
O4 Eu1 O11 139.32(10) 2 . ?
O10 Eu1 O11 73.33(10) . . ?
O3 Eu1 O11 74.34(9) 4_666 . ?
O1 Eu1 O2 124.36(9) . 3_666 ?
O4 Eu1 O2 79.62(10) 2 3_666 ?
O10 Eu1 O2 72.35(10) . 3_666 ?
O3 Eu1 O2 81.51(9) 4_666 3_666 ?
O11 Eu1 O2 140.79(10) . 3_666 ?
O1 Eu1 O7 85.63(9) . . ?
O4 Eu1 O7 75.22(10) 2 . ?
O10 Eu1 O7 99.76(10) . . ?
O3 Eu1 O7 143.30(10) 4_666 . ?
O11 Eu1 O7 70.60(10) . . ?
O2 Eu1 O7 133.84(9) 3_666 . ?
O1 Eu1 O8 131.36(9) . . ?
O4 Eu1 O8 71.15(9) 2 . ?
O10 Eu1 O8 71.01(10) . . ?
O3 Eu1 O8 150.10(9) 4_666 . ?
O11 Eu1 O8 103.11(9) . . ?
O2 Eu1 O8 83.04(9) 3_666 . ?
O7 Eu1 O8 52.44(9) . . ?
C2 C1 C6 119.1(3) . . ?
C2 C1 C7 119.8(3) . . ?
C6 C1 C7 121.0(3) . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
O5 C3 C2 117.7(3) . . ?
O5 C3 C4 122.5(3) . . ?
C2 C3 C4 119.8(3) . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 C8 118.8(3) . . ?
C3 C4 C8 121.9(3) . . ?
C6 C5 C4 120.9(3) . . ?
C6 C5 H5A 119.5 . . ?
C4 C5 H5A 119.5 . . ?
O6 C6 C5 118.2(3) . . ?
O6 C6 C1 121.8(3) . . ?
C5 C6 C1 120.0(3) . . ?
O1 C7 O2 120.9(3) . . ?
O1 C7 C1 120.8(3) . . ?
O2 C7 C1 118.3(3) . . ?
O1 C7 Eu1 71.7(2) . 3_666 ?
O2 C7 Eu1 50.04(18) . 3_666 ?
C1 C7 Eu1 163.4(3) . 3_666 ?
O4 C8 O3 124.5(3) . . ?
O4 C8 C4 118.5(3) . . ?
O3 C8 C4 117.0(3) . . ?
C7 O1 Eu1 171.7(2) . . ?
C7 O1 Eu1 84.0(2) . 3_666 ?
Eu1 O1 Eu1 103.39(9) . 3_666 ?
C7 O2 Eu1 106.3(2) . 3_666 ?
C8 O3 Eu1 134.5(2) . 4_565 ?
C8 O4 Eu1 143.4(2) . 2_545 ?
C3 O5 H5 109.3 . . ?
C6 O6 H6 109.3 . . ?
C10 C9 C11 119.5(3) . 3_665 ?
C10 C9 C12 119.6(3) . . ?
C11 C9 C12 121.0(3) 3_665 . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
O9 C11 C10 118.1(3) . . ?
O9 C11 C9 121.4(3) . 3_665 ?
C10 C11 C9 120.5(4) . 3_665 ?
O8 C12 O7 120.6(3) . . ?
O8 C12 C9 121.9(3) . . ?
O7 C12 C9 117.4(3) . . ?
O8 C12 Eu1 62.86(19) . . ?
O7 C12 Eu1 58.23(18) . . ?
C9 C12 Eu1 171.3(3) . . ?
C12 O7 Eu1 95.0(2) . . ?
C12 O8 Eu1 91.3(2) . . ?
C11 O9 H9 109.6 . . ?
Eu1 O10 H10A 125.7 . . ?
Eu1 O10 H10B 129.0 . . ?
H10A O10 H10B 105.3 . . ?
Eu1 O11 H11A 129.9 . . ?
Eu1 O11 H11B 105.4 . . ?
H11A O11 H11B 124.1 . . ?
H12A O12 H12B 97.8 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O13 C14 C13 118.3(8) . . ?
O13 C14 H14A 107.7 . . ?
C13 C14 H14A 107.7 . . ?
O13 C14 H14B 107.7 . . ?
C13 C14 H14B 107.7 . . ?
H14A C14 H14B 107.1 . . ?
C14 O13 H13 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C15 H15D 109.5 . . ?
H15B C15 H15D 109.5 . . ?
H15C C15 H15D 109.5 . . ?
O14 C16 C15 111.2(7) . . ?
O14 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
O14 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C16 O14 H14 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O15 C18 C17 120.0(10) . . ?
O15 C18 H18A 107.3 . . ?
C17 C18 H18A 107.3 . . ?
O15 C18 H18B 107.3 . . ?
C17 C18 H18B 107.3 . . ?
H18A C18 H18B 106.9 . . ?
C18 O15 H15 109.5 . . ?
C18A C17A H17D 109.5 . . ?
C18A C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
C18A C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
O15A C18A C17A 123(2) . . ?
O15A C18A H18C 106.6 . . ?
C17A C18A H18C 106.6 . . ?
O15A C18A H18D 106.6 . . ?
C17A C18A H18D 106.6 . . ?
H18C C18A H18D 106.5 . . ?
C18A O15A H15A 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
C6 C1 C2 C3 2.2(6) . . . . ?
C7 C1 C2 C3 -175.6(3) . . . . ?
C1 C2 C3 O5 178.3(3) . . . . ?
C1 C2 C3 C4 -1.5(6) . . . . ?
O5 C3 C4 C5 -179.9(4) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
O5 C3 C4 C8 -1.2(6) . . . . ?
C2 C3 C4 C8 178.6(3) . . . . ?
C3 C4 C5 C6 1.1(6) . . . . ?
C8 C4 C5 C6 -177.6(4) . . . . ?
C4 C5 C6 O6 179.1(4) . . . . ?
C4 C5 C6 C1 -0.4(6) . . . . ?
C2 C1 C6 O6 179.3(4) . . . . ?
C7 C1 C6 O6 -3.0(6) . . . . ?
C2 C1 C6 C5 -1.2(6) . . . . ?
C7 C1 C6 C5 176.6(4) . . . . ?
C2 C1 C7 O1 3.9(5) . . . . ?
C6 C1 C7 O1 -173.9(4) . . . . ?
C2 C1 C7 O2 -179.0(3) . . . . ?
C6 C1 C7 O2 3.3(5) . . . . ?
C2 C1 C7 Eu1 139.5(7) . . . 3_666 ?
C6 C1 C7 Eu1 -38.2(10) . . . 3_666 ?
C5 C4 C8 O4 -3.8(5) . . . . ?
C3 C4 C8 O4 177.5(4) . . . . ?
C5 C4 C8 O3 175.1(3) . . . . ?
C3 C4 C8 O3 -3.6(5) . . . . ?
O2 C7 O1 Eu1 -9.2(3) . . . 3_666 ?
C1 C7 O1 Eu1 167.8(3) . . . 3_666 ?
O1 C7 O2 Eu1 11.5(4) . . . 3_666 ?
C1 C7 O2 Eu1 -165.7(3) . . . 3_666 ?
O4 C8 O3 Eu1 20.9(6) . . . 4_565 ?
C4 C8 O3 Eu1 -158.0(2) . . . 4_565 ?
O3 C8 O4 Eu1 12.5(7) . . . 2_545 ?
C4 C8 O4 Eu1 -168.7(3) . . . 2_545 ?
C11 C9 C10 C11 0.8(6) 3_665 . . . ?
C12 C9 C10 C11 180.0(3) . . . . ?
C9 C10 C11 O9 179.2(3) . . . . ?
C9 C10 C11 C9 -0.8(6) . . . 3_665 ?
C10 C9 C12 O8 -1.8(6) . . . . ?
C11 C9 C12 O8 177.4(4) 3_665 . . . ?
C10 C9 C12 O7 177.4(3) . . . . ?
C11 C9 C12 O7 -3.4(5) 3_665 . . . ?
O8 C12 O7 Eu1 7.9(4) . . . . ?
C9 C12 O7 Eu1 -171.3(3) . . . . ?
O7 C12 O8 Eu1 -7.5(4) . . . . ?
C9 C12 O8 Eu1 171.6(3) . . . . ?

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
O5 H5 O3 0.82 1.85 2.576(4) 147 . yes
O6 H6 O2 0.82 1.82 2.548(4) 146 . yes
O9 H9 O7 0.82 1.78 2.516(4) 147 3_665 yes
O10 H10A O14 0.93 1.85 2.753(5) 164 . yes
O10 H10B O12 0.85 1.90 2.742(4) 170 . yes
O11 H11A O13 0.84 1.85 2.682(5) 169 . yes
O11 H11B O15 0.91 1.92 2.734(7) 148 . yes
O11 H11B O15A 0.91 1.87 2.749(15) 162 . yes
O12 H12A O9 0.90 1.93 2.825(4) 170 2_645 yes
O12 H12B O6 0.87 1.95 2.777(4) 159 1_655 yes
O13 H13 O9 0.84 1.99 2.824(5) 173 2_645 yes
O14 H14 O12 0.84 2.01 2.812(5) 159 3_766 yes
O15 H15 O14 0.84 2.10 2.910(8) 163 2_645 yes
O15A H15A O14 0.84 2.17 2.775(17) 129 2_645 yes
C2 H2 O7 0.95 2.51 3.323(4) 144 . yes
C16 H16A O5 0.99 2.62 3.235(8) 121 2_655 yes
C17 H17A O6 0.98 2.60 3.533(12) 160 4_665 yes
C18 H18A O8 0.99 2.54 3.327(10) 136 2_645 yes
C17A H17E O2 0.98 2.37 3.35(2) 175 4_665 yes

_refine_diff_density_max         0.791
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.114

####################################################################### 
# 
# 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_gd552
_database_code_depnum_ccdc_archive 'CCDC 1937369'
loop_
_audit_author_name
_audit_author_address
'William Harrison'
;University of Aberdeen
United Kingdom
;
_audit_update_record             
;
2019-06-30 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 Gd O11, 3(C2 H6 O), H2 O'
_chemical_formula_sum            'C18 H30 Gd O15'
_chemical_formula_weight         643.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   12.53408(13)
_cell_length_b                   14.43816(18)
_cell_length_c                   14.25451(16)
_cell_angle_alpha                90
_cell_angle_beta                 106.5332(12)
_cell_angle_gamma                90
_cell_volume                     2472.97(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11585
_cell_measurement_theta_min      4.1380
_cell_measurement_theta_max      72.2570
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.490
_exptl_absorpt_coefficient_mu    17.986
_shelx_estimated_absorpt_T_min   0.034
_shelx_estimated_absorpt_T_max   0.041
_exptl_absorpt_correction_T_min  0.34037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
#_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20744
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.151
_diffrn_reflns_theta_max         71.261
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4756
_reflns_number_gt                4447
_reflns_threshold_expression     'I > 2σ(I)'

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0296P)²+1.3712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4756
_refine_ls_number_parameters     343
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0596
_refine_ls_wR_factor_gt          0.0582
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.60347(2) 0.46626(2) 0.41531(2) 0.00619(6) Uani 1 1 d . . . . .
C1 C 0.2976(2) 0.29719(19) 0.3731(2) 0.0110(5) Uani 1 1 d . . . . .
C2 C 0.3488(2) 0.26764(19) 0.3035(2) 0.0120(5) Uani 1 1 d . . . . .
H2 H 0.420945 0.289775 0.306227 0.014 Uiso 1 1 calc R U . . .
C3 C 0.2954(2) 0.2061(2) 0.2302(2) 0.0114(5) Uani 1 1 d . . . . .
C4 C 0.1893(2) 0.17204(19) 0.22696(19) 0.0098(5) Uani 1 1 d . . . . .
C5 C 0.1396(2) 0.2003(2) 0.2987(2) 0.0137(6) Uani 1 1 d . . . . .
H5A H 0.068712 0.176353 0.297828 0.016 Uiso 1 1 calc R U . . .
C6 C 0.1921(2) 0.2623(2) 0.3707(2) 0.0137(6) Uani 1 1 d . . . . .
C7 C 0.3528(2) 0.36872(19) 0.4460(2) 0.0108(5) Uani 1 1 d . . . . .
C8 C 0.1270(2) 0.10720(19) 0.1484(2) 0.0109(5) Uani 1 1 d . . . . .
O1 O 0.44293(16) 0.40561(14) 0.44336(14) 0.0127(4) Uani 1 1 d . . . . .
O2 O 0.30473(16) 0.39388(14) 0.50957(15) 0.0153(4) Uani 1 1 d . . . . .
O3 O 0.17175(16) 0.08786(14) 0.08031(14) 0.0134(4) Uani 1 1 d . . . . .
O4 O 0.03556(16) 0.07703(14) 0.15275(14) 0.0144(4) Uani 1 1 d . . . . .
O5 O 0.34850(17) 0.18179(16) 0.16280(15) 0.0195(5) Uani 1 1 d . . . . .
H5 H 0.307639 0.148587 0.121059 0.023 Uiso 1 1 d R U . . .
O6 O 0.13857(18) 0.28843(17) 0.43762(17) 0.0250(5) Uani 1 1 d . . . . .
H6 H 0.174013 0.329702 0.472362 0.030 Uiso 1 1 d R U . . .
C9 C 0.5330(2) 0.4905(2) 0.1015(2) 0.0116(5) Uani 1 1 d . . . . .
C10 C 0.5756(2) 0.5624(2) 0.0578(2) 0.0139(6) Uani 1 1 d . . . . .
H10 H 0.627206 0.604878 0.097139 0.017 Uiso 1 1 calc R U . . .
C11 C 0.5426(2) 0.5720(2) -0.0430(2) 0.0133(6) Uani 1 1 d . . . . .
C12 C 0.5688(2) 0.4810(2) 0.2105(2) 0.0121(6) Uani 1 1 d . . . . .
O7 O 0.52336(18) 0.41617(15) 0.24749(14) 0.0182(4) Uani 1 1 d . . . . .
O8 O 0.63892(17) 0.53391(15) 0.26348(15) 0.0172(4) Uani 1 1 d . . . . .
O9 O 0.58603(18) 0.64420(15) -0.08286(14) 0.0191(5) Uani 1 1 d . . . . .
H9 H 0.559905 0.643604 -0.142555 0.023 Uiso 1 1 d R U . . .
O10 O 0.79737(17) 0.45179(15) 0.42775(18) 0.0226(5) Uani 1 1 d . . . . .
H10A H 0.842059 0.497583 0.412537 0.027 Uiso 1 1 d R U . . .
H10B H 0.840159 0.405083 0.445937 0.027 Uiso 1 1 d R U . . .
O11 O 0.63930(19) 0.30298(15) 0.40266(15) 0.0207(5) Uani 1 1 d . . . . .
H11A H 0.643329 0.260124 0.443399 0.025 Uiso 1 1 d R U . . .
H11B H 0.658329 0.296624 0.346200 0.025 Uiso 1 1 d R U . . .
O12 O 0.95074(18) 0.31510(16) 0.50148(17) 0.0240(5) Uani 1 1 d . . . . .
H12A H 0.942686 0.263477 0.534705 0.029 Uiso 1 1 d R U . . .
H12B H 1.000686 0.293777 0.475105 0.029 Uiso 1 1 d R U . . .
C13 C 0.6809(6) 0.0072(4) 0.5954(7) 0.104(3) Uani 1 1 d . . . . .
H13A H 0.694954 -0.020488 0.537236 0.156 Uiso 1 1 calc R U . . .
H13B H 0.632302 -0.033747 0.619715 0.156 Uiso 1 1 calc R U . . .
H13C H 0.751631 0.015375 0.646298 0.156 Uiso 1 1 calc R U . . .
C14 C 0.6278(5) 0.0957(4) 0.5703(6) 0.091(2) Uani 1 1 d . . . . .
H14A H 0.552898 0.084700 0.524875 0.109 Uiso 1 1 calc R U . . .
H14B H 0.617093 0.123017 0.630679 0.109 Uiso 1 1 calc R U . . .
O13 O 0.6798(2) 0.1607(2) 0.5284(3) 0.0483(8) Uani 1 1 d . . . . .
H13 H 0.748760 0.150977 0.545880 0.072 Uiso 1 1 calc R U . . .
C15 C 1.0194(6) 0.4741(4) 0.3026(5) 0.0758(19) Uani 1 1 d . . . . .
H15B H 1.038248 0.446353 0.246584 0.114 Uiso 1 1 calc R U . . .
H15C H 0.988879 0.426455 0.336536 0.114 Uiso 1 1 calc R U . . .
H15D H 1.086551 0.500656 0.347672 0.114 Uiso 1 1 calc R U . . .
C16 C 0.9369(5) 0.5470(4) 0.2681(4) 0.0598(14) Uani 1 1 d . . . . .
H16A H 0.968997 0.596711 0.236770 0.072 Uiso 1 1 calc R U . . .
H16B H 0.871423 0.521279 0.218554 0.072 Uiso 1 1 calc R U . . .
O14 O 0.9026(2) 0.5847(2) 0.3476(2) 0.0381(6) Uani 1 1 d . . . . .
H14 H 0.957388 0.609573 0.387919 0.046 Uiso 1 1 calc R U . . .
C17 C 0.7863(9) 0.3287(6) 0.1510(6) 0.075(3) Uani 0.713(12) 1 d D . P A 1
H17A H 0.724336 0.304144 0.098345 0.113 Uiso 0.713(12) 1 calc R U P A 1
H17B H 0.850638 0.339110 0.126115 0.113 Uiso 0.713(12) 1 calc R U P A 1
H17C H 0.764135 0.387327 0.174484 0.113 Uiso 0.713(12) 1 calc R U P A 1
C18 C 0.8165(6) 0.2611(5) 0.2327(5) 0.0453(19) Uani 0.713(12) 1 d D . P A 1
H18A H 0.852097 0.207556 0.210338 0.054 Uiso 0.713(12) 1 calc R U P A 1
H18B H 0.874068 0.290486 0.286930 0.054 Uiso 0.713(12) 1 calc R U P A 1
O15 O 0.7354(6) 0.2267(4) 0.2714(5) 0.0400(12) Uani 0.713(12) 1 d D . P A 1
H15 H 0.707364 0.178878 0.240608 0.048 Uiso 0.713(12) 1 calc R U P A 1
C17A C 0.8559(13) 0.2836(13) 0.1730(16) 0.059(6) Uani 0.287(12) 1 d D . P A 2
H17D H 0.878978 0.338629 0.143546 0.088 Uiso 0.287(12) 1 calc R U P A 2
H17E H 0.845554 0.231635 0.127070 0.088 Uiso 0.287(12) 1 calc R U P A 2
H17F H 0.913407 0.267759 0.233457 0.088 Uiso 0.287(12) 1 calc R U P A 2
C18A C 0.7497(13) 0.3029(11) 0.1957(13) 0.049(5) Uani 0.287(12) 1 d D . P A 2
H18C H 0.760914 0.361957 0.232594 0.059 Uiso 0.287(12) 1 calc R U P A 2
H18D H 0.694151 0.315807 0.132189 0.059 Uiso 0.287(12) 1 calc R U P A 2
O15A O 0.7013(12) 0.2469(9) 0.2427(10) 0.030(3) Uani 0.287(12) 1 d D U P A 2
H15A H 0.640354 0.228976 0.204980 0.036 Uiso 0.287(12) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

Gd1 O1 2.3310(19) . ?
Gd1 O4 2.3607(19) 2 ?
Gd1 O3 2.3936(19) 4_666 ?
Gd1 O10 2.395(2) . ?
Gd1 O11 2.416(2) . ?
Gd1 O2 2.418(2) 3_666 ?
Gd1 O7 2.426(2) . ?
Gd1 O8 2.526(2) . ?
Gd1 O1 2.913(2) 3_666 ?
C1 C2 1.392(4) . ?
C1 C6 1.406(4) . ?
C1 C7 1.489(4) . ?
C2 C3 1.389(4) . ?
C2 H2 0.9500 . ?
C3 O5 1.362(3) . ?
C3 C4 1.407(4) . ?
C4 C5 1.401(4) . ?
C4 C8 1.498(4) . ?
C5 C6 1.379(4) . ?
C5 H5A 0.9500 . ?
C6 O6 1.367(3) . ?
C7 O1 1.260(3) . ?
C7 O2 1.275(3) . ?
C8 O4 1.244(3) . ?
C8 O3 1.282(3) . ?
O5 H5 0.8201 . ?
O6 H6 0.8201 . ?
C9 C10 1.394(4) . ?
C9 C11 1.399(4) 3_665 ?
C9 C12 1.495(4) . ?
C10 C11 1.384(4) . ?
C10 H10 0.9500 . ?
C11 O9 1.372(3) . ?
C12 O8 1.244(4) . ?
C12 O7 1.285(4) . ?
O9 H9 0.8202 . ?
O10 H10A 0.9312 . ?
O10 H10B 0.8547 . ?
O11 H11A 0.8403 . ?
O11 H11B 0.9068 . ?
O12 H12A 0.9040 . ?
O12 H12B 0.8728 . ?
C13 C14 1.439(8) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 O13 1.372(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O13 H13 0.8400 . ?
C15 C16 1.459(8) . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15D 0.9800 . ?
C16 O14 1.429(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
O14 H14 0.8400 . ?
C17 C18 1.483(10) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O15 1.380(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
O15 H15 0.8400 . ?
C17A C18A 1.483(16) . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C18A O15A 1.305(16) . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
O15A H15A 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


O1 Gd1 O4 75.68(7) . 2 ?
O1 Gd1 O3 78.09(7) . 4_666 ?
O4 Gd1 O3 129.84(7) 2 4_666 ?
O1 Gd1 O10 149.52(7) . . ?
O4 Gd1 O10 134.77(7) 2 . ?
O3 Gd1 O10 80.05(7) 4_666 . ?
O1 Gd1 O11 80.46(7) . . ?
O4 Gd1 O11 139.60(8) 2 . ?
O3 Gd1 O11 74.50(7) 4_666 . ?
O10 Gd1 O11 73.39(8) . . ?
O1 Gd1 O2 124.26(7) . 3_666 ?
O4 Gd1 O2 79.56(7) 2 3_666 ?
O3 Gd1 O2 81.11(7) 4_666 3_666 ?
O10 Gd1 O2 72.25(7) . 3_666 ?
O11 Gd1 O2 140.60(7) . 3_666 ?
O1 Gd1 O7 85.52(7) . . ?
O4 Gd1 O7 75.33(7) 2 . ?
O3 Gd1 O7 143.46(7) 4_666 . ?
O10 Gd1 O7 99.99(8) . . ?
O11 Gd1 O7 70.68(7) . . ?
O2 Gd1 O7 134.17(7) 3_666 . ?
O1 Gd1 O8 131.53(7) . . ?
O4 Gd1 O8 71.05(7) 2 . ?
O3 Gd1 O8 150.12(7) 4_666 . ?
O10 Gd1 O8 71.04(7) . . ?
O11 Gd1 O8 103.39(7) . . ?
O2 Gd1 O8 83.04(7) 3_666 . ?
O7 Gd1 O8 52.77(7) . . ?
O1 Gd1 C12 108.56(7) . . ?
O4 Gd1 C12 69.34(7) 2 . ?
O3 Gd1 C12 160.67(7) 4_666 . ?
O10 Gd1 C12 86.42(8) . . ?
O11 Gd1 C12 88.49(8) . . ?
O2 Gd1 C12 107.90(8) 3_666 . ?
O7 Gd1 C12 26.86(8) . . ?
O8 Gd1 C12 26.03(8) . . ?
O1 Gd1 O1 76.58(7) . 3_666 ?
O4 Gd1 O1 65.46(6) 2 3_666 ?
O3 Gd1 O1 67.27(6) 4_666 3_666 ?
O10 Gd1 O1 113.72(7) . 3_666 ?
O11 Gd1 O1 138.52(6) . 3_666 ?
O2 Gd1 O1 47.69(6) 3_666 3_666 ?
O7 Gd1 O1 139.74(7) . 3_666 ?
O8 Gd1 O1 117.73(6) . 3_666 ?
C12 Gd1 O1 131.48(7) . 3_666 ?
C2 C1 C6 119.6(3) . . ?
C2 C1 C7 119.5(2) . . ?
C6 C1 C7 120.8(2) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
O5 C3 C2 117.9(2) . . ?
O5 C3 C4 122.3(2) . . ?
C2 C3 C4 119.8(2) . . ?
C5 C4 C3 119.1(2) . . ?
C5 C4 C8 118.9(2) . . ?
C3 C4 C8 122.0(2) . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5A 119.5 . . ?
C4 C5 H5A 119.5 . . ?
O6 C6 C5 118.2(2) . . ?
O6 C6 C1 121.9(3) . . ?
C5 C6 C1 119.8(3) . . ?
O1 C7 O2 120.7(3) . . ?
O1 C7 C1 121.0(2) . . ?
O2 C7 C1 118.3(2) . . ?
O1 C7 Gd1 72.00(15) . 3_666 ?
O2 C7 Gd1 49.45(13) . 3_666 ?
C1 C7 Gd1 163.41(19) . 3_666 ?
O4 C8 O3 124.7(3) . . ?
O4 C8 C4 118.2(2) . . ?
O3 C8 C4 117.1(2) . . ?
C7 O1 Gd1 171.75(19) . . ?
C7 O1 Gd1 83.71(16) . 3_666 ?
Gd1 O1 Gd1 103.42(7) . 3_666 ?
C7 O2 Gd1 106.93(17) . 3_666 ?
C8 O3 Gd1 134.70(18) . 4_565 ?
C8 O4 Gd1 143.06(19) . 2_545 ?
C3 O5 H5 109.4 . . ?
C6 O6 H6 109.5 . . ?
C10 C9 C11 119.6(3) . 3_665 ?
C10 C9 C12 119.5(3) . . ?
C11 C9 C12 120.9(3) 3_665 . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
O9 C11 C10 118.0(3) . . ?
O9 C11 C9 121.6(3) . 3_665 ?
C10 C11 C9 120.4(3) . 3_665 ?
O8 C12 O7 121.1(3) . . ?
O8 C12 C9 121.8(3) . . ?
O7 C12 C9 117.1(3) . . ?
O8 C12 Gd1 63.00(15) . . ?
O7 C12 Gd1 58.54(14) . . ?
C9 C12 Gd1 171.60(19) . . ?
C12 O7 Gd1 94.61(16) . . ?
C12 O8 Gd1 90.98(17) . . ?
C11 O9 H9 109.5 . . ?
Gd1 O10 H10A 125.9 . . ?
Gd1 O10 H10B 128.9 . . ?
H10A O10 H10B 105.3 . . ?
Gd1 O11 H11A 130.0 . . ?
Gd1 O11 H11B 105.5 . . ?
H11A O11 H11B 124.0 . . ?
H12A O12 H12B 97.8 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O13 C14 C13 118.2(6) . . ?
O13 C14 H14A 107.8 . . ?
C13 C14 H14A 107.8 . . ?
O13 C14 H14B 107.8 . . ?
C13 C14 H14B 107.8 . . ?
H14A C14 H14B 107.1 . . ?
C14 O13 H13 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C15 H15D 109.5 . . ?
H15B C15 H15D 109.5 . . ?
H15C C15 H15D 109.5 . . ?
O14 C16 C15 110.7(5) . . ?
O14 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
O14 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C16 O14 H14 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O15 C18 C17 119.9(8) . . ?
O15 C18 H18A 107.3 . . ?
C17 C18 H18A 107.3 . . ?
O15 C18 H18B 107.3 . . ?
C17 C18 H18B 107.3 . . ?
H18A C18 H18B 106.9 . . ?
C18 O15 H15 109.5 . . ?
C18A C17A H17D 109.5 . . ?
C18A C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
C18A C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
O15A C18A C17A 125.0(18) . . ?
O15A C18A H18C 106.1 . . ?
C17A C18A H18C 106.1 . . ?
O15A C18A H18D 106.1 . . ?
C17A C18A H18D 106.1 . . ?
H18C C18A H18D 106.3 . . ?
C18A O15A H15A 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
C6 C1 C2 C3 1.8(4) . . . . ?
C7 C1 C2 C3 -175.2(3) . . . . ?
C1 C2 C3 O5 178.2(3) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
O5 C3 C4 C5 -179.9(3) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
O5 C3 C4 C8 -0.6(4) . . . . ?
C2 C3 C4 C8 178.7(3) . . . . ?
C3 C4 C5 C6 1.5(4) . . . . ?
C8 C4 C5 C6 -177.8(3) . . . . ?
C4 C5 C6 O6 178.9(3) . . . . ?
C4 C5 C6 C1 -0.7(5) . . . . ?
C2 C1 C6 O6 179.5(3) . . . . ?
C7 C1 C6 O6 -3.5(4) . . . . ?
C2 C1 C6 C5 -1.0(4) . . . . ?
C7 C1 C6 C5 176.1(3) . . . . ?
C2 C1 C7 O1 2.9(4) . . . . ?
C6 C1 C7 O1 -174.2(3) . . . . ?
C2 C1 C7 O2 -179.3(3) . . . . ?
C6 C1 C7 O2 3.7(4) . . . . ?
C2 C1 C7 Gd1 141.8(6) . . . 3_666 ?
C6 C1 C7 Gd1 -35.2(8) . . . 3_666 ?
C5 C4 C8 O4 -3.7(4) . . . . ?
C3 C4 C8 O4 177.0(3) . . . . ?
C5 C4 C8 O3 175.4(3) . . . . ?
C3 C4 C8 O3 -3.9(4) . . . . ?
O2 C7 O1 Gd1 -9.2(2) . . . 3_666 ?
C1 C7 O1 Gd1 168.6(2) . . . 3_666 ?
O1 C7 O2 Gd1 11.6(3) . . . 3_666 ?
C1 C7 O2 Gd1 -166.34(19) . . . 3_666 ?
O4 C8 O3 Gd1 21.8(4) . . . 4_565 ?
C4 C8 O3 Gd1 -157.22(18) . . . 4_565 ?
O3 C8 O4 Gd1 12.1(5) . . . 2_545 ?
C4 C8 O4 Gd1 -168.9(2) . . . 2_545 ?
C11 C9 C10 C11 0.3(5) 3_665 . . . ?
C12 C9 C10 C11 -179.8(3) . . . . ?
C9 C10 C11 O9 179.5(3) . . . . ?
C9 C10 C11 C9 -0.3(5) . . . 3_665 ?
C10 C9 C12 O8 -2.5(4) . . . . ?
C11 C9 C12 O8 177.4(3) 3_665 . . . ?
C10 C9 C12 O7 176.9(3) . . . . ?
C11 C9 C12 O7 -3.2(4) 3_665 . . . ?
O8 C12 O7 Gd1 7.6(3) . . . . ?
C9 C12 O7 Gd1 -171.8(2) . . . . ?
O7 C12 O8 Gd1 -7.3(3) . . . . ?
C9 C12 O8 Gd1 172.0(2) . . . . ?

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
O5 H5 O3 0.82 1.86 2.578(3) 146 . yes
O6 H6 O2 0.82 1.82 2.548(3) 146 . yes
O9 H9 O7 0.82 1.78 2.513(3) 147 3_665 yes
O10 H10A O14 0.93 1.85 2.754(4) 164 . yes
O10 H10B O12 0.85 1.90 2.747(3) 170 . yes
O11 H11A O13 0.84 1.85 2.679(3) 168 . yes
O11 H11B O15 0.91 1.92 2.729(5) 148 . yes
O11 H11B O15A 0.91 1.85 2.732(12) 163 . yes
O12 H12A O9 0.90 1.93 2.820(3) 170 2_645 yes
O12 H12B O6 0.87 1.95 2.782(3) 159 1_655 yes
O13 H13 O9 0.84 1.99 2.824(4) 173 2_645 yes
O14 H14 O12 0.84 1.99 2.801(4) 162 3_766 yes
O15 H15 O14 0.84 2.08 2.899(6) 163 2_645 yes
O15A H15A O14 0.84 2.23 2.808(12) 126 2_645 yes
C2 H2 O7 0.95 2.51 3.320(3) 143 . yes
C18 H18A O8 0.99 2.53 3.326(7) 137 2_645 yes
C17A H17E O2 0.98 2.42 3.399(19) 176 4_665 yes

_refine_diff_density_max         0.548
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.085

