# 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_du
_database_code_depnum_ccdc_archive 'CCDC 1942126'
loop_
_audit_author_name
_audit_author_address
'xueting Wang'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2020-01-13 deposited with the CCDC.	2020-01-30 downloaded from the CCDC.
;
_audit_creation_date             2020-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(C64 H32 Gd4 O40), H2 O, 0.5(H6 O2)'
_chemical_formula_sum            'C16 H13 Gd O12'
_chemical_formula_weight         554.51
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   9.1964(18)
_cell_length_b                   13.197(3)
_cell_length_c                   14.447(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1753.4(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7463
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1141
_cell_measurement_theta_min      2.6277
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18298
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.016
_diffrn_reflns_theta_min         3.905
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3122
_reflns_number_total             3311
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_refine_diff_density_max         0.523
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3212
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0233
_refine_ls_restrained_S_all      1.135
_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)+(0.0173P)²+2.6345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0534
_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,H,H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 H6-H6_$1
 1.39 with sigma of 0.01
3. Others
 Fixed Sof: O8(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
4.a Riding coordinates:
 O7(H7A), O8(H8A,H8B,H8C)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.250000 0.000000 0.59592(2) 0.01487(4) Uani 1 2 d S T P . .
O1 O 0.69941(16) 0.39091(11) 0.23110(10) 0.0236(3) Uani 1 1 d . . . . .
O2 O 0.5298(2) 0.50627(12) 0.20757(13) 0.0323(4) Uani 1 1 d . . . . .
O3 O 0.39492(18) 0.14174(10) 0.55953(11) 0.0269(3) Uani 1 1 d . . . . .
O4 O 0.5692(2) 0.11190(12) 0.45720(13) 0.0363(4) Uani 1 1 d . . . . .
O5 O 0.250000 0.500000 0.51370(15) 0.0263(5) Uani 1 2 d S T P . .
O6 O 0.250000 0.000000 0.4166(2) 0.0498(8) Uani 1 2 d DS T P . .
O7 O -0.0748(4) 0.250000 0.250000 0.0592(9) Uani 1 2 d S T P . .
H7A H -0.129187 0.301540 0.243090 0.089 Uiso 1 1 d R . . . .
C1 C 0.5821(2) 0.43469(14) 0.25455(14) 0.0222(3) Uani 1 1 d . . . . .
C2 C 0.5054(2) 0.40025(13) 0.34047(13) 0.0194(3) Uani 1 1 d . . . . .
C3 C 0.5305(2) 0.30393(13) 0.37660(13) 0.0195(3) Uani 1 1 d . . . . .
H3 H 0.595713 0.260301 0.347713 0.023 Uiso 1 1 calc R . . . .
C4 C 0.4573(2) 0.27340(12) 0.45635(12) 0.0178(3) Uani 1 1 d . . . . .
C5 C 0.3614(2) 0.33951(13) 0.50006(13) 0.0206(3) Uani 1 1 d . . . . .
H5 H 0.312201 0.319238 0.553177 0.025 Uiso 1 1 calc R . . . .
C6 C 0.3394(2) 0.43584(13) 0.46400(13) 0.0199(3) Uani 1 1 d . . . . .
C7 C 0.4097(2) 0.46646(13) 0.38393(14) 0.0217(3) Uani 1 1 d . . . . .
H7 H 0.392992 0.530623 0.359514 0.026 Uiso 1 1 calc R . . . .
C8 C 0.4767(2) 0.16743(13) 0.49368(12) 0.0192(3) Uani 1 1 d . . . . .
O8 O 0.2015(8) 0.2008(7) 0.3060(7) 0.145(4) Uani 0.5 1 d . . . . .
H8A H 0.109098 0.202250 0.304376 0.217 Uiso 0.5 1 d R . . . .
H8B H 0.232658 0.239610 0.263466 0.217 Uiso 0.5 1 d R . . . .
H8C H 0.229748 0.140680 0.294826 0.217 Uiso 0.5 1 d R . . . .
H6 H 0.3252(10) -0.005(6) 0.3828(13) 0.217 Uiso 1 1 d DR . . . .


_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 2.4705(14) 8_656 ?
Gd1 O1 2.4705(14) 7_566 ?
Gd1 O2 2.5904(18) 8_656 ?
Gd1 O2 2.5904(18) 7_566 ?
Gd1 O3 2.3562(15) 2 ?
Gd1 O3 2.3562(15) . ?
Gd1 O4 2.3525(15) 6_556 ?
Gd1 O4 2.3525(15) 5_656 ?
Gd1 O6 2.590(3) . ?
Gd1 C1 2.8945(19) 8_656 ?
Gd1 C1 2.8945(19) 7_566 ?
O1 C1 1.269(2) . ?
O2 C1 1.259(2) . ?
O3 C8 1.259(2) . ?
O4 C8 1.241(2) . ?
O5 C6 1.381(2) . ?
O5 C6 1.381(2) 2_565 ?
O6 H6 0.850(10) . ?
O6 H6 0.850(10) 2 ?
O7 H7A 0.8499 . ?
O7 H7A 0.8499 4 ?
C1 C2 1.498(3) . ?
C2 C3 1.393(2) . ?
C2 C7 1.390(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.394(2) . ?
C4 C5 1.392(2) . ?
C4 C8 1.509(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(2) . ?
C6 C7 1.386(3) . ?
C7 H7 0.9300 . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8499 . ?
O8 H8C 0.8500 . ?

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 O1 75.53(7) 7_566 8_656 ?
O1 Gd1 O2 68.67(6) 7_566 8_656 ?
O1 Gd1 O2 51.61(5) 7_566 7_566 ?
O1 Gd1 O2 51.61(5) 8_656 8_656 ?
O1 Gd1 O2 68.67(6) 8_656 7_566 ?
O1 Gd1 O6 142.24(4) 7_566 . ?
O1 Gd1 O6 142.24(4) 8_656 . ?
O1 Gd1 C1 25.86(5) 8_656 8_656 ?
O1 Gd1 C1 69.39(6) 8_656 7_566 ?
O1 Gd1 C1 69.39(6) 7_566 8_656 ?
O1 Gd1 C1 25.86(5) 7_566 7_566 ?
O2 Gd1 O2 102.97(9) 8_656 7_566 ?
O2 Gd1 O6 128.52(4) 7_566 . ?
O2 Gd1 O6 128.52(4) 8_656 . ?
O2 Gd1 C1 25.78(5) 7_566 7_566 ?
O2 Gd1 C1 85.09(6) 8_656 7_566 ?
O2 Gd1 C1 85.09(6) 7_566 8_656 ?
O2 Gd1 C1 25.78(5) 8_656 8_656 ?
O3 Gd1 O1 122.18(5) . 8_656 ?
O3 Gd1 O1 122.18(5) 2 7_566 ?
O3 Gd1 O1 79.65(5) 2 8_656 ?
O3 Gd1 O1 79.65(5) . 7_566 ?
O3 Gd1 O2 70.82(5) 2 7_566 ?
O3 Gd1 O2 70.82(5) . 8_656 ?
O3 Gd1 O2 127.34(5) . 7_566 ?
O3 Gd1 O2 127.34(5) 2 8_656 ?
O3 Gd1 O3 154.21(8) 2 . ?
O3 Gd1 O6 77.11(4) 2 . ?
O3 Gd1 O6 77.11(4) . . ?
O3 Gd1 C1 96.40(6) 2 7_566 ?
O3 Gd1 C1 104.00(5) 2 8_656 ?
O3 Gd1 C1 104.00(5) . 7_566 ?
O3 Gd1 C1 96.40(6) . 8_656 ?
O4 Gd1 O1 76.05(6) 5_656 8_656 ?
O4 Gd1 O1 76.05(6) 6_556 7_566 ?
O4 Gd1 O1 139.18(6) 5_656 7_566 ?
O4 Gd1 O1 139.18(6) 6_556 8_656 ?
O4 Gd1 O2 137.37(6) 5_656 7_566 ?
O4 Gd1 O2 137.37(6) 6_556 8_656 ?
O4 Gd1 O2 70.77(7) 6_556 7_566 ?
O4 Gd1 O2 70.77(7) 5_656 8_656 ?
O4 Gd1 O3 80.13(6) 5_656 2 ?
O4 Gd1 O3 91.48(6) 5_656 . ?
O4 Gd1 O3 91.47(6) 6_556 2 ?
O4 Gd1 O3 80.13(6) 6_556 . ?
O4 Gd1 O4 141.92(9) 6_556 5_656 ?
O4 Gd1 O6 70.96(5) 6_556 . ?
O4 Gd1 O6 70.96(5) 5_656 . ?
O4 Gd1 C1 72.21(6) 6_556 7_566 ?
O4 Gd1 C1 145.30(6) 5_656 7_566 ?
O4 Gd1 C1 72.21(6) 5_656 8_656 ?
O4 Gd1 C1 145.30(6) 6_556 8_656 ?
O6 Gd1 C1 142.35(4) . 8_656 ?
O6 Gd1 C1 142.35(4) . 7_566 ?
C1 Gd1 C1 75.30(8) 8_656 7_566 ?
C1 O1 Gd1 96.07(11) . 7_665 ?
C1 O2 Gd1 90.74(13) . 7_665 ?
C8 O3 Gd1 136.07(13) . . ?
C8 O4 Gd1 173.84(15) . 5_656 ?
C6 O5 C6 117.4(2) . 2_565 ?
Gd1 O6 H6 125.2(11) . . ?
Gd1 O6 H6 125.2(11) . 2 ?
H6 O6 H6 110(2) . 2 ?
H7A O7 H7A 108.0 . 4 ?
O1 C1 Gd1 58.07(9) . 7_665 ?
O1 C1 C2 118.88(16) . . ?
O2 C1 Gd1 63.49(11) . 7_665 ?
O2 C1 O1 121.50(18) . . ?
O2 C1 C2 119.62(18) . . ?
C2 C1 Gd1 175.83(14) . 7_665 ?
C3 C2 C1 120.60(16) . . ?
C7 C2 C1 118.80(16) . . ?
C7 C2 C3 120.60(16) . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.55(16) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C8 120.41(15) . . ?
C5 C4 C3 120.00(15) . . ?
C5 C4 C8 119.55(15) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.72(17) . . ?
C6 C5 H5 120.1 . . ?
O5 C6 C5 116.93(16) . . ?
O5 C6 C7 122.20(16) . . ?
C7 C6 C5 120.81(16) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 C2 119.30(16) . . ?
C6 C7 H7 120.4 . . ?
O3 C8 C4 116.69(15) . . ?
O4 C8 O3 124.86(17) . . ?
O4 C8 C4 118.45(16) . . ?
H8A O8 H8B 107.7 . . ?
H8A O8 H8C 108.8 . . ?
H8B O8 H8C 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O1 C1 O2 3.0(2) 7_665 . . . ?
Gd1 O1 C1 C2 -176.70(15) 7_665 . . . ?
Gd1 O2 C1 O1 -2.8(2) 7_665 . . . ?
Gd1 O2 C1 C2 176.85(16) 7_665 . . . ?
Gd1 O3 C8 O4 -45.7(3) . . . . ?
Gd1 O3 C8 C4 133.30(16) . . . . ?
O1 C1 C2 C3 -21.4(3) . . . . ?
O1 C1 C2 C7 158.09(19) . . . . ?
O2 C1 C2 C3 158.9(2) . . . . ?
O2 C1 C2 C7 -21.6(3) . . . . ?
O5 C6 C7 C2 175.88(18) . . . . ?
C1 C2 C3 C4 -179.66(18) . . . . ?
C1 C2 C7 C6 -179.29(19) . . . . ?
C2 C3 C4 C5 -0.9(3) . . . . ?
C2 C3 C4 C8 176.65(18) . . . . ?
C3 C2 C7 C6 0.2(3) . . . . ?
C3 C4 C5 C6 -0.2(3) . . . . ?
C3 C4 C8 O3 -172.22(19) . . . . ?
C3 C4 C8 O4 6.8(3) . . . . ?
C4 C5 C6 O5 -176.04(17) . . . . ?
C4 C5 C6 C7 1.2(3) . . . . ?
C5 C4 C8 O3 5.3(3) . . . . ?
C5 C4 C8 O4 -175.6(2) . . . . ?
C5 C6 C7 C2 -1.2(3) . . . . ?
C6 O5 C6 C5 -143.3(2) 2_565 . . . ?
C6 O5 C6 C7 39.49(16) 2_565 . . . ?
C7 C2 C3 C4 0.9(3) . . . . ?
C8 C4 C5 C6 -177.72(18) . . . . ?

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

data_du_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1942127'
loop_
_audit_author_name
_audit_author_address
'xueting Wang'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2020-01-13 deposited with the CCDC.	2020-01-30 downloaded from the CCDC.
;
_audit_creation_date             2020-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C64 H32 Eu4 O40), H2 O, 0.5(H6 O2)'
_chemical_formula_sum            'C16 H13 Eu O12'
_chemical_formula_weight         549.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Eu Eu -0.1578 3.6682 '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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   9.2104(18)
_cell_length_b                   13.203(3)
_cell_length_c                   14.465(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1759.0(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7322
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.3515
_cell_measurement_theta_min      1.5423
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.634
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18527
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.349
_diffrn_reflns_theta_min         4.051
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3137
_reflns_number_total             3427
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3197
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+2.9765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0531
_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,H,H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 H6-H6_$1
 1.39 with sigma of 0.01
3. Others
 Fixed Sof: O8(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
4.a Riding coordinates:
 O7(H7A), O8(H8A,H8B,H8C)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.250000 0.000000 0.59606(2) 0.01400(4) Uani 1 2 d S T P . .
O1 O 0.69872(16) 0.39047(11) 0.23164(10) 0.0232(3) Uani 1 1 d . . . . .
O2 O 0.5300(2) 0.50632(12) 0.20790(12) 0.0318(4) Uani 1 1 d . . . . .
O3 O 0.39529(19) 0.14226(11) 0.56002(10) 0.0264(3) Uani 1 1 d . . . . .
O4 O 0.5684(2) 0.11220(12) 0.45732(13) 0.0355(4) Uani 1 1 d . . . . .
O5 O 0.250000 0.500000 0.51351(15) 0.0242(4) Uani 1 2 d S T P . .
O6 O 0.250000 0.000000 0.4160(2) 0.0504(9) Uani 1 2 d DS T P . .
O7 O -0.0753(4) 0.250000 0.250000 0.0567(8) Uani 1 2 d S T P . .
H7A H -0.129694 0.301540 0.243090 0.085 Uiso 1 1 d R . . . .
C1 C 0.5821(2) 0.43447(14) 0.25491(14) 0.0215(3) Uani 1 1 d . . . . .
C2 C 0.5052(2) 0.40033(14) 0.34086(13) 0.0187(3) Uani 1 1 d . . . . .
C3 C 0.5302(2) 0.30411(13) 0.37685(13) 0.0187(3) Uani 1 1 d . . . . .
H3 H 0.595182 0.260466 0.347918 0.022 Uiso 1 1 calc R . . . .
C4 C 0.4572(2) 0.27365(13) 0.45659(12) 0.0171(3) Uani 1 1 d . . . . .
C5 C 0.3613(2) 0.33975(14) 0.50025(13) 0.0198(3) Uani 1 1 d . . . . .
H5 H 0.312296 0.319579 0.553355 0.024 Uiso 1 1 calc R . . . .
C6 C 0.3394(2) 0.43592(13) 0.46400(13) 0.0184(3) Uani 1 1 d . . . . .
C7 C 0.4096(2) 0.46646(14) 0.38409(14) 0.0202(3) Uani 1 1 d . . . . .
H7 H 0.392932 0.530550 0.359624 0.024 Uiso 1 1 calc R . . . .
C8 C 0.4763(2) 0.16799(13) 0.49389(12) 0.0185(3) Uani 1 1 d . . . . .
O8 O 0.2008(8) 0.1993(8) 0.3074(7) 0.143(4) Uani 0.5 1 d . . . . .
H8A H 0.108411 0.200740 0.305760 0.215 Uiso 0.5 1 d R . . . .
H8B H 0.231971 0.238100 0.264850 0.215 Uiso 0.5 1 d R . . . .
H8C H 0.229061 0.139170 0.296210 0.215 Uiso 0.5 1 d R . . . .
H6 H 0.3243(19) -0.009(7) 0.3822(13) 0.215 Uiso 1 1 d DR . . . .


_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 O1 2.4821(14) 8_656 ?
Eu1 O1 2.4821(14) 7_566 ?
Eu1 O2 2.5945(18) 8_656 ?
Eu1 O2 2.5945(18) 7_566 ?
Eu1 O3 2.3644(16) 2 ?
Eu1 O3 2.3645(16) . ?
Eu1 O4 2.3639(15) 6_556 ?
Eu1 O4 2.3639(15) 5_656 ?
Eu1 O6 2.605(3) . ?
Eu1 C1 2.9016(19) 8_656 ?
Eu1 C1 2.9016(19) 7_566 ?
O1 C1 1.266(2) . ?
O2 C1 1.262(2) . ?
O3 C8 1.260(2) . ?
O4 C8 1.242(2) . ?
O5 C6 1.381(2) . ?
O5 C6 1.381(2) 2_565 ?
O6 H6 0.849(10) . ?
O6 H6 0.849(10) 2 ?
O7 H7A 0.8507 . ?
O7 H7A 0.8506 4 ?
C1 C2 1.500(3) . ?
C2 C3 1.392(2) . ?
C2 C7 1.389(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.394(2) . ?
C4 C5 1.393(2) . ?
C4 C8 1.506(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(2) . ?
C6 C7 1.385(3) . ?
C7 H7 0.9300 . ?
O8 H8A 0.8513 . ?
O8 H8B 0.8508 . ?
O8 H8C 0.8505 . ?

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 O1 75.60(7) 7_566 8_656 ?
O1 Eu1 O2 68.73(6) 7_566 8_656 ?
O1 Eu1 O2 51.49(5) 7_566 7_566 ?
O1 Eu1 O2 51.49(5) 8_656 8_656 ?
O1 Eu1 O2 68.73(6) 8_656 7_566 ?
O1 Eu1 O6 142.20(4) 7_566 . ?
O1 Eu1 O6 142.20(4) 8_656 . ?
O1 Eu1 C1 25.73(5) 8_656 8_656 ?
O1 Eu1 C1 69.47(6) 8_656 7_566 ?
O1 Eu1 C1 69.47(6) 7_566 8_656 ?
O1 Eu1 C1 25.73(5) 7_566 7_566 ?
O2 Eu1 O2 102.85(9) 8_656 7_566 ?
O2 Eu1 O6 128.58(4) 7_566 . ?
O2 Eu1 O6 128.58(4) 8_656 . ?
O2 Eu1 C1 25.78(5) 7_566 7_566 ?
O2 Eu1 C1 85.00(6) 8_656 7_566 ?
O2 Eu1 C1 85.00(6) 7_566 8_656 ?
O2 Eu1 C1 25.78(5) 8_656 8_656 ?
O3 Eu1 O1 121.96(5) . 8_656 ?
O3 Eu1 O1 121.96(5) 2 7_566 ?
O3 Eu1 O1 79.58(5) 2 8_656 ?
O3 Eu1 O1 79.58(5) . 7_566 ?
O3 Eu1 O2 70.72(5) 2 7_566 ?
O3 Eu1 O2 70.72(5) . 8_656 ?
O3 Eu1 O2 127.24(5) . 7_566 ?
O3 Eu1 O2 127.24(5) 2 8_656 ?
O3 Eu1 O3 154.52(8) 2 . ?
O3 Eu1 O6 77.26(4) 2 . ?
O3 Eu1 O6 77.26(4) . . ?
O3 Eu1 C1 96.31(6) 2 7_566 ?
O3 Eu1 C1 103.85(5) 2 8_656 ?
O3 Eu1 C1 103.85(5) . 7_566 ?
O3 Eu1 C1 96.31(6) . 8_656 ?
O4 Eu1 O1 76.02(6) 5_656 8_656 ?
O4 Eu1 O1 76.02(6) 6_556 7_566 ?
O4 Eu1 O1 139.27(6) 5_656 7_566 ?
O4 Eu1 O1 139.27(6) 6_556 8_656 ?
O4 Eu1 O2 137.41(6) 5_656 7_566 ?
O4 Eu1 O2 137.41(6) 6_556 8_656 ?
O4 Eu1 O2 70.80(7) 6_556 7_566 ?
O4 Eu1 O2 70.80(7) 5_656 8_656 ?
O4 Eu1 O3 80.24(7) 5_656 2 ?
O4 Eu1 O3 91.45(6) 5_656 . ?
O4 Eu1 O3 91.45(6) 6_556 2 ?
O4 Eu1 O3 80.24(7) 6_556 . ?
O4 Eu1 O4 141.87(9) 6_556 5_656 ?
O4 Eu1 O6 70.93(5) 6_556 . ?
O4 Eu1 O6 70.93(5) 5_656 . ?
O4 Eu1 C1 72.23(6) 6_556 7_566 ?
O4 Eu1 C1 145.34(6) 5_656 7_566 ?
O4 Eu1 C1 72.23(6) 5_656 8_656 ?
O4 Eu1 C1 145.34(6) 6_556 8_656 ?
O6 Eu1 C1 142.37(4) . 8_656 ?
O6 Eu1 C1 142.37(4) . 7_566 ?
C1 Eu1 C1 75.27(8) 8_656 7_566 ?
C1 O1 Eu1 95.98(11) . 7_665 ?
C1 O2 Eu1 90.83(13) . 7_665 ?
C8 O3 Eu1 135.79(13) . . ?
C8 O4 Eu1 173.83(15) . 5_656 ?
C6 O5 C6 117.5(2) . 2_565 ?
Eu1 O6 H6 125.1(11) . . ?
Eu1 O6 H6 125.1(11) . 2 ?
H6 O6 H6 110(2) . 2 ?
H7A O7 H7A 107.9 . 4 ?
O1 C1 Eu1 58.29(10) . 7_665 ?
O1 C1 C2 118.88(16) . . ?
O2 C1 Eu1 63.39(11) . 7_665 ?
O2 C1 O1 121.62(18) . . ?
O2 C1 C2 119.50(18) . . ?
C2 C1 Eu1 175.94(14) . 7_665 ?
C3 C2 C1 120.38(16) . . ?
C7 C2 C1 118.92(16) . . ?
C7 C2 C3 120.70(16) . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.51(16) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C8 120.48(15) . . ?
C5 C4 C3 120.01(16) . . ?
C5 C4 C8 119.46(15) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.60(17) . . ?
C6 C5 H5 120.2 . . ?
O5 C6 C5 116.83(16) . . ?
O5 C6 C7 122.22(16) . . ?
C7 C6 C5 120.89(16) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 C2 119.28(16) . . ?
C6 C7 H7 120.4 . . ?
O3 C8 C4 116.91(16) . . ?
O4 C8 O3 124.62(17) . . ?
O4 C8 C4 118.46(16) . . ?
H8A O8 H8B 107.7 . . ?
H8A O8 H8C 108.8 . . ?
H8B O8 H8C 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O1 C1 O2 3.0(2) 7_665 . . . ?
Eu1 O1 C1 C2 -176.62(16) 7_665 . . . ?
Eu1 O2 C1 O1 -2.9(2) 7_665 . . . ?
Eu1 O2 C1 C2 176.77(17) 7_665 . . . ?
Eu1 O3 C8 O4 -46.1(3) . . . . ?
Eu1 O3 C8 C4 133.05(16) . . . . ?
O1 C1 C2 C3 -21.3(3) . . . . ?
O1 C1 C2 C7 158.29(19) . . . . ?
O2 C1 C2 C3 159.1(2) . . . . ?
O2 C1 C2 C7 -21.4(3) . . . . ?
O5 C6 C7 C2 175.92(18) . . . . ?
C1 C2 C3 C4 -179.75(18) . . . . ?
C1 C2 C7 C6 -179.30(19) . . . . ?
C2 C3 C4 C5 -0.7(3) . . . . ?
C2 C3 C4 C8 176.65(18) . . . . ?
C3 C2 C7 C6 0.3(3) . . . . ?
C3 C4 C5 C6 -0.2(3) . . . . ?
C3 C4 C8 O3 -172.48(19) . . . . ?
C3 C4 C8 O4 6.7(3) . . . . ?
C4 C5 C6 O5 -176.12(17) . . . . ?
C4 C5 C6 C7 1.1(3) . . . . ?
C5 C4 C8 O3 4.9(3) . . . . ?
C5 C4 C8 O4 -175.9(2) . . . . ?
C5 C6 C7 C2 -1.2(3) . . . . ?
C6 O5 C6 C5 -143.3(2) 2_565 . . . ?
C6 O5 C6 C7 39.48(15) 2_565 . . . ?
C7 C2 C3 C4 0.7(3) . . . . ?
C8 C4 C5 C6 -177.58(18) . . . . ?

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

data_du_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1942128'
loop_
_audit_author_name
_audit_author_address
'xueting Wang'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2020-01-13 deposited with the CCDC.	2020-01-30 downloaded from the CCDC.
;
_audit_creation_date             2020-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C64 H32 O40 Tb4), H2 O, 0.5(H6 O2)'
_chemical_formula_sum            'C16 H13 O12 Tb'
_chemical_formula_weight         556.19
_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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   9.1988(18)
_cell_length_b                   13.161(3)
_cell_length_c                   14.406(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1744.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7008
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1601
_cell_measurement_theta_min      2.0960
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.124
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17928
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.105
_diffrn_reflns_theta_min         3.912
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3093
_reflns_number_total             3317
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3172
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0293
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0304P)²+3.2718P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0736
_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,H,H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 H6-H6_$1
 1.39 with sigma of 0.01
3. Others
 Fixed Sof: O8(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
4.a Riding coordinates:
 O7(H7A), O8(H8A,H8B,H8C)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.250000 0.000000 0.59552(2) 0.01575(6) Uani 1 2 d S T P . .
O1 O 0.6997(2) 0.39098(13) 0.23025(12) 0.0245(3) Uani 1 1 d . . . . .
O2 O 0.5303(3) 0.50695(14) 0.20696(16) 0.0334(5) Uani 1 1 d . . . . .
O3 O 0.3938(2) 0.14073(13) 0.55882(13) 0.0282(4) Uani 1 1 d . . . . .
O4 O 0.5699(2) 0.11119(15) 0.45741(16) 0.0371(5) Uani 1 1 d . . . . .
O5 O 0.250000 0.500000 0.5135(2) 0.0277(6) Uani 1 2 d S T P . .
O6 O 0.250000 0.000000 0.4163(3) 0.0518(12) Uani 1 2 d DS T P . .
O7 O -0.0737(4) 0.250000 0.250000 0.0607(10) Uani 1 2 d S T P . .
H7A H -0.128027 0.301540 0.243090 0.091 Uiso 1 1 d R . . . .
C1 C 0.5824(3) 0.43512(17) 0.25399(16) 0.0238(4) Uani 1 1 d . . . . .
C2 C 0.5060(2) 0.40057(16) 0.34020(15) 0.0204(4) Uani 1 1 d . . . . .
C3 C 0.5314(2) 0.30384(16) 0.37640(15) 0.0207(4) Uani 1 1 d . . . . .
H3 H 0.597097 0.260333 0.347635 0.025 Uiso 1 1 calc R . . . .
C4 C 0.4574(2) 0.27293(15) 0.45607(15) 0.0186(4) Uani 1 1 d . . . . .
C5 C 0.3616(2) 0.33932(16) 0.49998(16) 0.0221(4) Uani 1 1 d . . . . .
H5 H 0.312596 0.319097 0.553349 0.027 Uiso 1 1 calc R . . . .
C6 C 0.3396(3) 0.43572(16) 0.46371(15) 0.0212(4) Uani 1 1 d . . . . .
C7 C 0.4101(3) 0.46675(17) 0.38363(17) 0.0235(4) Uani 1 1 d . . . . .
H7 H 0.393402 0.531128 0.359249 0.028 Uiso 1 1 calc R . . . .
C8 C 0.4767(3) 0.16687(17) 0.49328(14) 0.0199(4) Uani 1 1 d . . . . .
O8 O 0.2003(9) 0.1982(9) 0.3064(10) 0.150(5) Uani 0.5 1 d . . . . .
H8A H 0.107944 0.199676 0.304767 0.226 Uiso 0.5 1 d R . . . .
H8B H 0.231504 0.237036 0.263857 0.226 Uiso 0.5 1 d R . . . .
H8C H 0.228594 0.138106 0.295217 0.226 Uiso 0.5 1 d R . . . .
H6 H 0.3250(14) -0.006(8) 0.3824(13) 0.226 Uiso 1 1 d DR . . . .


_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 2.4577(17) 8_656 ?
Tb1 O1 2.4577(17) 7_566 ?
Tb1 O2 2.582(2) 8_656 ?
Tb1 O2 2.582(2) 7_566 ?
Tb1 O3 2.3366(18) 2 ?
Tb1 O3 2.3366(18) . ?
Tb1 O4 2.3384(18) 6_556 ?
Tb1 O4 2.3384(18) 5_656 ?
Tb1 O6 2.583(4) . ?
Tb1 C1 2.884(2) 8_656 ?
Tb1 C1 2.884(2) 7_566 ?
O1 C1 1.272(3) . ?
O2 C1 1.258(3) . ?
O3 C8 1.262(3) . ?
O4 C8 1.240(3) . ?
O5 C6 1.382(3) 2_565 ?
O5 C6 1.382(3) . ?
O6 H6 0.849(10) . ?
O6 H6 0.849(10) 2 ?
O7 H7A 0.8485 . ?
O7 H7A 0.8485 4 ?
C1 C2 1.498(3) . ?
C2 C3 1.395(3) . ?
C2 C7 1.389(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.395(3) . ?
C4 C5 1.393(3) . ?
C4 C8 1.506(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.387(3) . ?
C6 C7 1.385(3) . ?
C7 H7 0.9300 . ?
O8 H8A 0.8502 . ?
O8 H8B 0.8478 . ?
O8 H8C 0.8479 . ?

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 O1 75.68(9) 7_566 8_656 ?
O1 Tb1 O2 68.64(7) 7_566 8_656 ?
O1 Tb1 O2 51.86(6) 8_656 8_656 ?
O1 Tb1 O2 51.86(6) 7_566 7_566 ?
O1 Tb1 O2 68.64(7) 8_656 7_566 ?
O1 Tb1 O6 142.16(4) 8_656 . ?
O1 Tb1 O6 142.16(4) 7_566 . ?
O1 Tb1 C1 69.41(7) 8_656 7_566 ?
O1 Tb1 C1 69.41(7) 7_566 8_656 ?
O1 Tb1 C1 26.01(6) 7_566 7_566 ?
O1 Tb1 C1 26.01(6) 8_656 8_656 ?
O2 Tb1 O2 103.13(11) 8_656 7_566 ?
O2 Tb1 O6 128.44(6) 7_566 . ?
O2 Tb1 O6 128.44(6) 8_656 . ?
O2 Tb1 C1 25.86(6) 7_566 7_566 ?
O2 Tb1 C1 85.16(8) 7_566 8_656 ?
O2 Tb1 C1 25.86(6) 8_656 8_656 ?
O2 Tb1 C1 85.16(8) 8_656 7_566 ?
O3 Tb1 O1 122.34(6) . 8_656 ?
O3 Tb1 O1 122.34(6) 2 7_566 ?
O3 Tb1 O1 79.78(6) 2 8_656 ?
O3 Tb1 O1 79.78(6) . 7_566 ?
O3 Tb1 O2 70.71(6) . 8_656 ?
O3 Tb1 O2 127.71(6) 2 8_656 ?
O3 Tb1 O2 70.71(6) 2 7_566 ?
O3 Tb1 O2 127.71(6) . 7_566 ?
O3 Tb1 O3 153.84(9) . 2 ?
O3 Tb1 O4 91.21(7) . 5_656 ?
O3 Tb1 O4 80.29(8) 2 5_656 ?
O3 Tb1 O4 91.21(7) 2 6_556 ?
O3 Tb1 O4 80.29(8) . 6_556 ?
O3 Tb1 O6 76.92(5) 2 . ?
O3 Tb1 O6 76.92(5) . . ?
O3 Tb1 C1 104.30(6) . 7_566 ?
O3 Tb1 C1 104.30(6) 2 8_656 ?
O3 Tb1 C1 96.39(7) 2 7_566 ?
O3 Tb1 C1 96.39(7) . 8_656 ?
O4 Tb1 O1 76.04(7) 6_556 7_566 ?
O4 Tb1 O1 76.04(7) 5_656 8_656 ?
O4 Tb1 O1 139.14(8) 5_656 7_566 ?
O4 Tb1 O1 139.14(8) 6_556 8_656 ?
O4 Tb1 O2 137.31(7) 5_656 7_566 ?
O4 Tb1 O2 137.31(7) 6_556 8_656 ?
O4 Tb1 O2 70.76(8) 5_656 8_656 ?
O4 Tb1 O2 70.76(8) 6_556 7_566 ?
O4 Tb1 O4 141.94(11) 6_556 5_656 ?
O4 Tb1 O6 70.97(6) 5_656 . ?
O4 Tb1 O6 70.97(6) 6_556 . ?
O4 Tb1 C1 145.30(7) 5_656 7_566 ?
O4 Tb1 C1 72.19(8) 5_656 8_656 ?
O4 Tb1 C1 72.19(8) 6_556 7_566 ?
O4 Tb1 C1 145.30(7) 6_556 8_656 ?
O6 Tb1 C1 142.34(5) . 8_656 ?
O6 Tb1 C1 142.34(5) . 7_566 ?
C1 Tb1 C1 75.32(10) 8_656 7_566 ?
C1 O1 Tb1 96.05(13) . 7_665 ?
C1 O2 Tb1 90.57(16) . 7_665 ?
C8 O3 Tb1 136.70(16) . . ?
C8 O4 Tb1 174.34(18) . 5_656 ?
C6 O5 C6 117.4(3) 2_565 . ?
Tb1 O6 H6 125.1(11) . . ?
Tb1 O6 H6 125.1(11) . 2 ?
H6 O6 H6 110(2) . 2 ?
H7A O7 H7A 107.8 . 4 ?
O1 C1 Tb1 57.94(11) . 7_665 ?
O1 C1 C2 118.8(2) . . ?
O2 C1 Tb1 63.56(14) . 7_665 ?
O2 C1 O1 121.4(2) . . ?
O2 C1 C2 119.7(2) . . ?
C2 C1 Tb1 175.69(17) . 7_665 ?
C3 C2 C1 120.5(2) . . ?
C7 C2 C1 118.78(19) . . ?
C7 C2 C3 120.7(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.46(19) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C8 120.38(18) . . ?
C5 C4 C3 119.96(19) . . ?
C5 C4 C8 119.63(18) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.7(2) . . ?
C6 C5 H5 120.2 . . ?
O5 C6 C5 116.8(2) . . ?
O5 C6 C7 122.1(2) . . ?
C7 C6 C5 121.0(2) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 C2 119.2(2) . . ?
C6 C7 H7 120.4 . . ?
O3 C8 C4 116.60(19) . . ?
O4 C8 O3 124.6(2) . . ?
O4 C8 C4 118.74(19) . . ?
H8A O8 H8B 107.7 . . ?
H8A O8 H8C 108.8 . . ?
H8B O8 H8C 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C1 O2 3.0(3) 7_665 . . . ?
Tb1 O1 C1 C2 -176.66(19) 7_665 . . . ?
Tb1 O2 C1 O1 -2.9(3) 7_665 . . . ?
Tb1 O2 C1 C2 176.8(2) 7_665 . . . ?
Tb1 O3 C8 O4 -45.3(4) . . . . ?
Tb1 O3 C8 C4 133.6(2) . . . . ?
O1 C1 C2 C3 -21.2(3) . . . . ?
O1 C1 C2 C7 158.4(2) . . . . ?
O2 C1 C2 C3 159.1(2) . . . . ?
O2 C1 C2 C7 -21.3(4) . . . . ?
O5 C6 C7 C2 175.8(2) . . . . ?
C1 C2 C3 C4 -179.2(2) . . . . ?
C1 C2 C7 C6 -179.6(2) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
C2 C3 C4 C8 176.5(2) . . . . ?
C3 C2 C7 C6 0.0(4) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C3 C4 C8 O3 -171.9(2) . . . . ?
C3 C4 C8 O4 7.0(4) . . . . ?
C4 C5 C6 O5 -176.2(2) . . . . ?
C4 C5 C6 C7 0.8(4) . . . . ?
C5 C4 C8 O3 6.1(3) . . . . ?
C5 C4 C8 O4 -175.0(2) . . . . ?
C5 C6 C7 C2 -1.1(4) . . . . ?
C6 O5 C6 C5 -143.3(2) 2_565 . . . ?
C6 O5 C6 C7 39.70(19) 2_565 . . . ?
C7 C2 C3 C4 1.2(4) . . . . ?
C8 C4 C5 C6 -177.6(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
