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

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

data_Tb
_database_code_depnum_ccdc_archive 'CCDC 2326140'
_audit_update_record             
;
2024-01-17 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H12 O12 Tb'
_chemical_formula_sum            'C12 H12 O12 Tb'
_chemical_formula_weight         507.14
_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                   10.3636(17)
_cell_length_b                   11.0274(16)
_cell_length_c                   11.1750(17)
_cell_angle_alpha                85.893(5)
_cell_angle_beta                 76.937(5)
_cell_angle_gamma                63.663(5)
_cell_volume                     1114.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    304.00
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.661
_shelx_estimated_absorpt_T_min   0.390
_exptl_absorpt_coefficient_mu    3.219
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_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       -14
_diffrn_reflns_number            32186
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         2.062
_diffrn_ambient_temperature      304.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_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                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4776
_reflns_number_total             5091
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0184
_refine_ls_restrained_S_all      1.084
_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)+(0.0179P)²+0.5155P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0448
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Tb1-H7A \\sim Tb1-H7B
 with sigma of 0.02
 Tb1-H9A \\sim Tb1-H9B
 with sigma of 0.02
 Tb1-H12A \\sim Tb1-H12B
 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B), O9(H9A,H9B), O12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5A)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O18(H18)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.53580(2) 0.50509(2) 0.29515(2) 0.01690(4) Uani 1 1 d D . . . .
O1 O 0.4566(2) 0.32745(17) 0.59400(15) 0.0294(4) Uani 1 1 d . . . . .
O2 O 1.0242(3) -0.1645(3) -0.1864(3) 0.0846(11) Uani 1 1 d . . . . .
H2 H 1.106110 -0.229189 -0.201188 0.127 Uiso 1 1 calc R U . . .
O4 O 0.23116(18) 0.59162(18) 0.64414(15) 0.0280(4) Uani 1 1 d . . . . .
O5 O 0.4317(5) -0.0987(3) 0.72616(19) 0.0928(12) Uani 1 1 d . . . . .
H5 H 0.451002 -0.178921 0.720369 0.139 Uiso 1 1 calc R U . . .
O6 O 0.5327(2) 0.30778(18) 0.38984(16) 0.0327(4) Uani 1 1 d . . . . .
O7 O 0.3718(3) 0.7199(2) 0.22891(18) 0.0523(6) Uani 1 1 d G . . . .
H7A H 0.355541 0.736783 0.156928 0.078 Uiso 1 1 d DG U . . .
H7B H 0.302104 0.785972 0.273511 0.078 Uiso 1 1 d DG U . . .
O8 O 0.31891(18) 0.57367(19) 0.44232(16) 0.0308(4) Uani 1 1 d . . . . .
O9 O 0.6813(3) 0.5726(2) 0.13277(19) 0.0492(6) Uani 1 1 d G . . . .
H9A H 0.678714 0.650619 0.121710 0.074 Uiso 1 1 d DG U . . .
H9B H 0.751457 0.522672 0.075816 0.074 Uiso 1 1 d DG U . . .
O10 O 0.70946(18) 0.30960(17) 0.16409(14) 0.0273(4) Uani 1 1 d . . . . .
O12 O 0.4093(2) 0.4626(2) 0.16076(17) 0.0384(5) Uani 1 1 d G . . . .
H12A H 0.460033 0.410118 0.098130 0.058 Uiso 1 1 d DG U . . .
H12B H 0.336387 0.524361 0.135991 0.058 Uiso 1 1 d DG U . . .
O14 O 0.6237(2) 0.2651(2) 0.01656(18) 0.0479(6) Uani 1 1 d . . . . .
C1 C 0.1073(3) 0.5359(3) 0.5187(2) 0.0266(5) Uani 1 1 d . . . . .
C2 C 0.4645(4) 0.0738(3) 0.6062(2) 0.0407(7) Uani 1 1 d . . . . .
H2A H 0.440872 0.123181 0.678534 0.049 Uiso 1 1 calc R U . . .
C3 C 0.8846(3) 0.0284(3) -0.0553(3) 0.0409(7) Uani 1 1 d . . . . .
H3 H 0.806273 0.047163 -0.092393 0.049 Uiso 1 1 calc R U . . .
C4 C 0.4981(3) 0.1276(2) 0.4955(2) 0.0268(5) Uani 1 1 d . . . . .
C5 C 0.1081(3) 0.4995(3) 0.4021(2) 0.0390(7) Uani 1 1 d . . . . .
H5A H 0.181488 0.498635 0.336008 0.047 Uiso 1 1 calc R U . . .
C6 C 0.4952(3) 0.2640(2) 0.4941(2) 0.0241(5) Uani 1 1 d . . . . .
C7 C 0.0017(3) 0.4646(3) 0.3826(2) 0.0387(7) Uani 1 1 d . . . . .
O18 O 0.0091(3) 0.4304(4) 0.26560(18) 0.0802(11) Uani 1 1 d . . . . .
H18 H -0.062290 0.416920 0.264134 0.120 Uiso 1 1 calc R U . . .
C9 C 0.4650(4) -0.0527(3) 0.6125(2) 0.0410(7) Uani 1 1 d . . . . .
C10 C 0.7234(3) 0.2384(2) 0.0737(2) 0.0266(5) Uani 1 1 d . . . . .
C11 C 1.0158(3) -0.0854(3) -0.0936(3) 0.0382(7) Uani 1 1 d . . . . .
C12 C 0.2272(2) 0.5706(2) 0.5347(2) 0.0236(5) Uani 1 1 d . . . . .
C13 C 0.8670(3) 0.1154(2) 0.0371(2) 0.0261(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.3349(16) 2_666 ?
Tb1 O4 2.4046(16) 2_666 ?
Tb1 O6 2.3603(16) . ?
Tb1 O7 2.407(2) . ?
Tb1 O8 2.3082(17) . ?
Tb1 O9 2.3842(18) . ?
Tb1 O10 2.4186(16) . ?
Tb1 O12 2.3941(18) . ?
O1 C6 1.248(3) . ?
O2 H2 0.8200 . ?
O2 C11 1.365(3) . ?
O4 C12 1.275(3) . ?
O5 H5 0.8200 . ?
O5 C9 1.362(3) . ?
O6 C6 1.274(3) . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8504 . ?
O8 C12 1.245(3) . ?
O9 H9A 0.8502 . ?
O9 H9B 0.8502 . ?
O10 C10 1.267(3) . ?
O12 H12A 0.8501 . ?
O12 H12B 0.8498 . ?
O14 C10 1.250(3) . ?
C1 C5 1.387(3) . ?
C1 C7 1.391(3) 2_566 ?
C1 C12 1.501(3) . ?
C2 H2A 0.9300 . ?
C2 C4 1.374(3) . ?
C2 C9 1.390(3) . ?
C3 H3 0.9300 . ?
C3 C11 1.381(4) . ?
C3 C13 1.385(3) . ?
C4 C6 1.490(3) . ?
C4 C9 1.392(3) 2_656 ?
C5 H5A 0.9300 . ?
C5 C7 1.381(3) . ?
C7 O18 1.364(3) . ?
O18 H18 0.8200 . ?
C10 C13 1.496(3) . ?
C11 C13 1.395(3) 2_755 ?

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 72.52(6) 2_666 2_666 ?
O1 Tb1 O6 121.20(6) 2_666 . ?
O1 Tb1 O7 73.06(7) 2_666 . ?
O1 Tb1 O9 82.55(7) 2_666 . ?
O1 Tb1 O10 137.47(6) 2_666 . ?
O1 Tb1 O12 144.57(7) 2_666 . ?
O4 Tb1 O7 137.74(8) 2_666 . ?
O4 Tb1 O10 70.15(5) 2_666 . ?
O6 Tb1 O4 79.53(6) . 2_666 ?
O6 Tb1 O7 140.49(8) . . ?
O6 Tb1 O9 140.46(7) . . ?
O6 Tb1 O10 70.74(6) . . ?
O6 Tb1 O12 83.49(7) . . ?
O7 Tb1 O10 126.19(6) . . ?
O8 Tb1 O1 77.94(6) . 2_666 ?
O8 Tb1 O4 120.07(6) . 2_666 ?
O8 Tb1 O6 73.18(7) . . ?
O8 Tb1 O7 74.93(8) . . ?
O8 Tb1 O9 146.23(7) . . ?
O8 Tb1 O10 139.59(6) . . ?
O8 Tb1 O12 87.00(6) . . ?
O9 Tb1 O4 78.78(8) . 2_666 ?
O9 Tb1 O7 73.13(9) . . ?
O9 Tb1 O10 70.93(7) . . ?
O9 Tb1 O12 93.42(8) . . ?
O12 Tb1 O4 141.36(6) . 2_666 ?
O12 Tb1 O7 72.10(8) . . ?
O12 Tb1 O10 71.53(6) . . ?
C6 O1 Tb1 147.51(15) . 2_666 ?
C11 O2 H2 109.5 . . ?
C12 O4 Tb1 119.38(15) . 2_666 ?
C9 O5 H5 109.5 . . ?
C6 O6 Tb1 141.65(15) . . ?
Tb1 O7 H7A 125.8 . . ?
Tb1 O7 H7B 127.7 . . ?
H7A O7 H7B 104.5 . . ?
C12 O8 Tb1 159.84(18) . . ?
Tb1 O9 H9A 127.8 . . ?
Tb1 O9 H9B 127.6 . . ?
H9A O9 H9B 104.5 . . ?
C10 O10 Tb1 142.98(15) . . ?
Tb1 O12 H12A 118.6 . . ?
Tb1 O12 H12B 123.5 . . ?
H12A O12 H12B 104.5 . . ?
C5 C1 C7 119.1(2) . 2_566 ?
C5 C1 C12 118.8(2) . . ?
C7 C1 C12 122.1(2) 2_566 . ?
C4 C2 H2A 119.3 . . ?
C4 C2 C9 121.5(2) . . ?
C9 C2 H2A 119.3 . . ?
C11 C3 H3 119.2 . . ?
C11 C3 C13 121.6(2) . . ?
C13 C3 H3 119.2 . . ?
C2 C4 C6 119.2(2) . . ?
C2 C4 C9 119.1(2) . 2_656 ?
C9 C4 C6 121.7(2) 2_656 . ?
C1 C5 H5A 119.4 . . ?
C7 C5 C1 121.1(2) . . ?
C7 C5 H5A 119.4 . . ?
O1 C6 O6 124.5(2) . . ?
O1 C6 C4 118.4(2) . . ?
O6 C6 C4 117.2(2) . . ?
C5 C7 C1 119.8(2) . 2_566 ?
O18 C7 C1 122.3(2) . 2_566 ?
O18 C7 C5 117.9(2) . . ?
C7 O18 H18 109.5 . . ?
O5 C9 C2 117.5(2) . . ?
O5 C9 C4 123.0(2) . 2_656 ?
C2 C9 C4 119.5(2) . 2_656 ?
O10 C10 C13 116.9(2) . . ?
O14 C10 O10 123.4(2) . . ?
O14 C10 C13 119.7(2) . . ?
O2 C11 C3 117.7(2) . . ?
O2 C11 C13 122.8(2) . 2_755 ?
C3 C11 C13 119.5(2) . 2_755 ?
O4 C12 C1 117.2(2) . . ?
O8 C12 O4 123.6(2) . . ?
O8 C12 C1 119.2(2) . . ?
C3 C13 C10 119.4(2) . . ?
C3 C13 C11 118.9(2) . 2_755 ?
C11 C13 C10 121.7(2) 2_755 . ?

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 C6 O6 -23.1(5) 2_666 . . . ?
Tb1 O1 C6 C4 156.8(2) 2_666 . . . ?
Tb1 O4 C12 O8 -41.7(3) 2_666 . . . ?
Tb1 O4 C12 C1 136.21(18) 2_666 . . . ?
Tb1 O6 C6 O1 -10.0(4) . . . . ?
Tb1 O6 C6 C4 170.06(19) . . . . ?
Tb1 O8 C12 O4 78.9(5) . . . . ?
Tb1 O8 C12 C1 -99.0(5) . . . . ?
Tb1 O10 C10 O14 3.1(5) . . . . ?
Tb1 O10 C10 C13 -175.96(17) . . . . ?
O10 C10 C13 C3 175.4(3) . . . . ?
O10 C10 C13 C11 -4.5(4) . . . 2_755 ?
O14 C10 C13 C3 -3.7(4) . . . . ?
O14 C10 C13 C11 176.4(3) . . . 2_755 ?
C1 C5 C7 C1 -0.8(5) . . . 2_566 ?
C1 C5 C7 O18 179.8(3) . . . . ?
C2 C4 C6 O1 -2.7(4) . . . . ?
C2 C4 C6 O6 177.3(3) . . . . ?
C4 C2 C9 O5 179.4(3) . . . . ?
C4 C2 C9 C4 0.7(5) . . . 2_656 ?
C5 C1 C12 O4 -173.8(3) . . . . ?
C5 C1 C12 O8 4.2(4) . . . . ?
C7 C1 C5 C7 0.8(5) 2_566 . . . ?
C7 C1 C12 O4 4.3(4) 2_566 . . . ?
C7 C1 C12 O8 -177.7(3) 2_566 . . . ?
C9 C2 C4 C6 179.7(3) . . . . ?
C9 C2 C4 C9 -0.7(5) . . . 2_656 ?
C9 C4 C6 O1 177.8(3) 2_656 . . . ?
C9 C4 C6 O6 -2.3(4) 2_656 . . . ?
C11 C3 C13 C10 179.1(3) . . . . ?
C11 C3 C13 C11 -1.0(5) . . . 2_755 ?
C12 C1 C5 C7 179.0(3) . . . . ?
C13 C3 C11 O2 -179.1(3) . . . . ?
C13 C3 C11 C13 1.0(5) . . . 2_755 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.458 0.076 -0.221 442.3 125.5 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT420_Tb                  
;
PROBLEM: D-H Bond Without Acceptor  O7       --H7B      .     Please Check 
RESPONSE: It is very difficult to locate hydrogen atoms accurately using X-ray
data because these atoms have low scattering power.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Gd
_database_code_depnum_ccdc_archive 'CCDC 2326141'
_audit_update_record             
;
2024-01-17 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H24 Gd2 O24'
_chemical_formula_sum            'C24 H24 Gd2 O24'
_chemical_formula_weight         1010.93
_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      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                   10.766(4)
_cell_length_b                   11.043(3)
_cell_length_c                   11.240(4)
_cell_angle_alpha                89.621(14)
_cell_angle_beta                 80.36(2)
_cell_angle_gamma                64.452(14)
_cell_volume                     1185.4(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    306.00
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.72
_shelx_estimated_absorpt_T_max   0.709
_shelx_estimated_absorpt_T_min   0.404
_exptl_absorpt_coefficient_mu    2.841
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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       -14
_diffrn_reflns_number            34605
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.582
_diffrn_reflns_theta_min         2.654
_diffrn_ambient_temperature      306.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_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                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5231
_reflns_number_total             5426
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.609
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         5426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.114
_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)+(0.0182P)²+2.6350P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0685
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B} of O5
 At 1.5 times of:
  All O(H) groups, {H4A,H4B} of O4, {H6A,H6B} of O6
2.a Riding coordinates:
 O5(H5A,H5B)
2.b Rotating group:
 O4(H4A,H4B), O6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11A), C13(H13)
2.d Idealised tetrahedral OH refined as rotating group:
 O10(H10), O11(H11), O12(H12)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.53082(2) 0.48848(2) 0.30155(2) 0.01821(6) Uani 1 1 d . . . . .
O1 O 0.3262(3) 0.5401(3) 0.4416(3) 0.0351(6) Uani 1 1 d . . . . .
O2 O 0.5211(3) 0.6765(2) 0.4051(2) 0.0339(6) Uani 1 1 d . . . . .
O3 O 0.7097(3) 0.2961(2) 0.1723(2) 0.0310(5) Uani 1 1 d . . . . .
O4 O 0.6420(4) 0.5726(3) 0.1400(3) 0.0534(8) Uani 1 1 d . . . . .
H4A H 0.623418 0.662242 0.128071 0.080 Uiso 1 1 d R U . . .
H4B H 0.713668 0.522873 0.075465 0.080 Uiso 1 1 d R U . . .
O5 O 0.3469(4) 0.6871(3) 0.2367(3) 0.0548(9) Uani 1 1 d . . . . .
H5A H 0.348523 0.678142 0.158361 0.066 Uiso 1 1 d R U . . .
H5B H 0.362993 0.758502 0.243811 0.066 Uiso 1 1 d R U . . .
O6 O 0.4205(3) 0.4200(3) 0.1623(3) 0.0486(8) Uani 1 1 d . . . . .
H6A H 0.474572 0.394627 0.091672 0.073 Uiso 1 1 d R U . . .
H6B H 0.346453 0.488853 0.148296 0.073 Uiso 1 1 d R U . . .
O7 O 0.6455(3) 0.2651(3) 0.0030(3) 0.0491(8) Uani 1 1 d . . . . .
O8 O 0.2453(3) 0.5769(3) 0.6393(2) 0.0318(5) Uani 1 1 d . . . . .
O9 O 0.4399(3) 0.7112(2) 0.6037(2) 0.0350(6) Uani 1 1 d . . . . .
O10 O 1.0467(3) -0.1388(4) -0.2182(3) 0.0588(10) Uani 1 1 d . . . . .
H10 H 1.126712 -0.199012 -0.234488 0.088 Uiso 1 1 calc R U . . .
O11 O 0.0095(4) 0.5715(5) 0.7306(3) 0.0667(12) Uani 1 1 d . . . . .
H11 H 0.081695 0.579062 0.732552 0.100 Uiso 1 1 calc R U . . .
O12 O 0.6302(5) 1.0576(3) 0.2878(3) 0.0612(11) Uani 1 1 d . . . . .
H12 H 0.634729 1.129079 0.297032 0.092 Uiso 1 1 calc R U . . .
C1 C 0.4838(4) 0.7457(3) 0.5030(3) 0.0268(7) Uani 1 1 d . . . . .
C2 C 0.1032(4) 0.4890(5) 0.4028(3) 0.0357(8) Uani 1 1 d . . . . .
H2 H 0.172105 0.481481 0.337183 0.043 Uiso 1 1 calc R U . . .
C4 C 0.2360(3) 0.5493(3) 0.5323(3) 0.0249(7) Uani 1 1 d . . . . .
C5 C 1.0283(4) -0.0736(4) -0.1097(3) 0.0332(8) Uani 1 1 d . . . . .
C6 C 0.1132(3) 0.5249(4) 0.5170(3) 0.0271(7) Uani 1 1 d . . . . .
C7 C 0.5644(5) 1.0329(4) 0.3928(3) 0.0350(8) Uani 1 1 d . . . . .
C8 C 0.4906(4) 0.8775(3) 0.5029(3) 0.0277(7) Uani 1 1 d . . . . .
C9 C 0.0083(4) 0.5362(5) 0.6156(3) 0.0360(9) Uani 1 1 d . . . . .
C10 C 0.7320(4) 0.2331(3) 0.0712(3) 0.0288(7) Uani 1 1 d . . . . .
C11 C 0.9006(4) 0.0390(4) -0.0722(3) 0.0359(9) Uani 1 1 d . . . . .
H11A H 0.833577 0.064994 -0.121595 0.043 Uiso 1 1 calc R U . . .
C12 C 0.8711(4) 0.1129(3) 0.0365(3) 0.0276(7) Uani 1 1 d . . . . .
C13 C 0.5541(4) 0.9117(4) 0.3983(3) 0.0334(8) Uani 1 1 d . . . . .
H13 H 0.590740 0.851593 0.330041 0.040 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
Gd1 O1 2.329(3) . ?
Gd1 O2 2.341(2) . ?
Gd1 O3 2.431(2) . ?
Gd1 O4 2.408(3) . ?
Gd1 O5 2.445(3) . ?
Gd1 O6 2.418(3) . ?
Gd1 O8 2.409(3) 2_666 ?
Gd1 O9 2.362(3) 2_666 ?
O1 C4 1.256(4) . ?
O2 C1 1.246(4) . ?
O3 C10 1.268(4) . ?
O4 H4A 0.9357 . ?
O4 H4B 0.9359 . ?
O5 H5A 0.8834 . ?
O5 H5B 0.8841 . ?
O6 H6A 0.8691 . ?
O6 H6B 0.8692 . ?
O7 C10 1.237(5) . ?
O8 C4 1.273(4) . ?
O9 C1 1.273(4) . ?
O10 H10 0.8200 . ?
O10 C5 1.361(4) . ?
O11 H11 0.8200 . ?
O11 C9 1.358(4) . ?
O12 H12 0.8200 . ?
O12 C7 1.361(5) . ?
C1 C8 1.489(4) . ?
C2 H2 0.9300 . ?
C2 C6 1.381(5) . ?
C2 C9 1.390(5) 2_566 ?
C4 C6 1.495(4) . ?
C5 C11 1.397(5) . ?
C5 C12 1.388(5) 2_755 ?
C6 C9 1.407(5) . ?
C7 C8 1.408(5) 2_676 ?
C7 C13 1.389(5) . ?
C8 C13 1.393(5) . ?
C10 C12 1.501(5) . ?
C11 H11A 0.9300 . ?
C11 C12 1.386(5) . ?
C13 H13 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 Gd1 O2 81.39(10) . . ?
O1 Gd1 O3 138.39(10) . . ?
O1 Gd1 O4 144.50(11) . . ?
O1 Gd1 O5 73.04(11) . . ?
O1 Gd1 O6 85.93(11) . . ?
O1 Gd1 O8 122.46(10) . 2_666 ?
O1 Gd1 O9 73.42(10) . 2_666 ?
O2 Gd1 O3 136.38(10) . . ?
O2 Gd1 O4 80.13(11) . . ?
O2 Gd1 O5 72.99(11) . . ?
O2 Gd1 O6 143.13(11) . . ?
O2 Gd1 O8 72.72(9) . 2_666 ?
O2 Gd1 O9 122.24(10) . 2_666 ?
O3 Gd1 O5 126.59(10) . . ?
O4 Gd1 O3 72.25(10) . . ?
O4 Gd1 O5 72.67(13) . . ?
O4 Gd1 O6 91.00(13) . . ?
O4 Gd1 O8 79.94(12) . 2_666 ?
O6 Gd1 O3 71.48(10) . . ?
O6 Gd1 O5 70.21(12) . . ?
O8 Gd1 O3 69.74(9) 2_666 . ?
O8 Gd1 O5 139.01(12) 2_666 . ?
O8 Gd1 O6 141.13(9) 2_666 . ?
O9 Gd1 O3 70.70(9) 2_666 . ?
O9 Gd1 O4 141.72(11) 2_666 . ?
O9 Gd1 O5 139.96(12) 2_666 . ?
O9 Gd1 O6 86.22(11) 2_666 . ?
O9 Gd1 O8 78.64(10) 2_666 2_666 ?
C4 O1 Gd1 166.2(2) . . ?
C1 O2 Gd1 146.7(2) . . ?
C10 O3 Gd1 140.9(2) . . ?
Gd1 O4 H4A 127.7 . . ?
Gd1 O4 H4B 127.8 . . ?
H4A O4 H4B 104.6 . . ?
Gd1 O5 H5A 110.9 . . ?
Gd1 O5 H5B 110.8 . . ?
H5A O5 H5B 103.1 . . ?
Gd1 O6 H6A 110.3 . . ?
Gd1 O6 H6B 110.1 . . ?
H6A O6 H6B 103.6 . . ?
C4 O8 Gd1 121.4(2) . 2_666 ?
C1 O9 Gd1 138.5(2) . 2_666 ?
C5 O10 H10 109.5 . . ?
C9 O11 H11 109.5 . . ?
C7 O12 H12 109.5 . . ?
O2 C1 O9 124.3(3) . . ?
O2 C1 C8 118.3(3) . . ?
O9 C1 C8 117.4(3) . . ?
C6 C2 H2 119.5 . . ?
C6 C2 C9 120.9(3) . 2_566 ?
C9 C2 H2 119.5 2_566 . ?
O1 C4 O8 122.6(3) . . ?
O1 C4 C6 119.9(3) . . ?
O8 C4 C6 117.5(3) . . ?
O10 C5 C11 117.1(3) . . ?
O10 C5 C12 123.5(3) . 2_755 ?
C12 C5 C11 119.4(3) 2_755 . ?
C2 C6 C4 118.9(3) . . ?
C2 C6 C9 119.1(3) . . ?
C9 C6 C4 122.0(3) . . ?
O12 C7 C8 123.2(3) . 2_676 ?
O12 C7 C13 118.4(3) . . ?
C13 C7 C8 118.4(3) . 2_676 ?
C7 C8 C1 121.1(3) 2_676 . ?
C13 C8 C1 119.4(3) . . ?
C13 C8 C7 119.5(3) . 2_676 ?
O11 C9 C2 117.0(3) . 2_566 ?
O11 C9 C6 122.9(3) . . ?
C2 C9 C6 120.0(3) 2_566 . ?
O3 C10 C12 116.6(3) . . ?
O7 C10 O3 123.4(3) . . ?
O7 C10 C12 120.0(3) . . ?
C5 C11 H11A 119.1 . . ?
C12 C11 C5 121.9(3) . . ?
C12 C11 H11A 119.1 . . ?
C5 C12 C10 122.1(3) 2_755 . ?
C11 C12 C5 118.8(3) . 2_755 ?
C11 C12 C10 119.2(3) . . ?
C7 C13 C8 122.1(3) . . ?
C7 C13 H13 119.0 . . ?
C8 C13 H13 119.0 . . ?

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
Gd1 O1 C4 O8 50.7(12) . . . . ?
Gd1 O1 C4 C6 -128.1(9) . . . . ?
Gd1 O2 C1 O9 10.0(7) . . . . ?
Gd1 O2 C1 C8 -170.0(3) . . . . ?
Gd1 O3 C10 O7 -0.5(7) . . . . ?
Gd1 O3 C10 C12 -179.7(3) . . . . ?
Gd1 O8 C4 O1 -30.2(5) 2_666 . . . ?
Gd1 O8 C4 C6 148.5(2) 2_666 . . . ?
Gd1 O9 C1 O2 28.2(6) 2_666 . . . ?
Gd1 O9 C1 C8 -151.8(3) 2_666 . . . ?
O1 C4 C6 C2 1.6(5) . . . . ?
O1 C4 C6 C9 -179.0(4) . . . . ?
O2 C1 C8 C7 172.9(4) . . . 2_676 ?
O2 C1 C8 C13 -8.0(5) . . . . ?
O3 C10 C12 C5 -1.1(6) . . . 2_755 ?
O3 C10 C12 C11 179.1(4) . . . . ?
O7 C10 C12 C5 179.7(4) . . . 2_755 ?
O7 C10 C12 C11 -0.1(6) . . . . ?
O8 C4 C6 C2 -177.2(4) . . . . ?
O8 C4 C6 C9 2.2(5) . . . . ?
O9 C1 C8 C7 -7.1(5) . . . 2_676 ?
O9 C1 C8 C13 172.0(4) . . . . ?
O10 C5 C11 C12 -179.8(4) . . . . ?
O12 C7 C13 C8 178.8(4) . . . . ?
C1 C8 C13 C7 -179.6(4) . . . . ?
C2 C6 C9 O11 -179.7(4) . . . . ?
C2 C6 C9 C2 0.1(7) . . . 2_566 ?
C4 C6 C9 O11 0.9(7) . . . . ?
C4 C6 C9 C2 -179.3(4) . . . 2_566 ?
C5 C11 C12 C5 0.0(7) . . . 2_755 ?
C5 C11 C12 C10 179.8(4) . . . . ?
C7 C8 C13 C7 -0.5(7) 2_676 . . . ?
C8 C7 C13 C8 0.5(7) 2_676 . . . ?
C9 C2 C6 C4 179.3(4) 2_566 . . . ?
C9 C2 C6 C9 -0.1(7) 2_566 . . . ?
C12 C5 C11 C12 0.0(7) 2_755 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.439 -0.089 -0.317 510.2 67.8 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT420_Gd                  
;
PROBLEM: D-H Bond Without Acceptor  O4       --H4A      .     Please Check 
RESPONSE: It is very difficult to locate hydrogen atoms accurately using X-ray
data because these atoms have low scattering power.
;
# end Validation Reply Form
