# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1473240'
_audit_update_record             
;
2017-08-21 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form 
_vrf_PLAT043_7                   
; 
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      14.11 Check 
RESPONSE: The difference results from the hydrogens of lattice water 
molecules which were not located and included to refinement, 
however, they were included to final formula to calculate 
actual cell metric values. 
;
_vrf_PLAT306_7                   
; 
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check 
RESPONSE: Due to huge disorder on lattice O-atom, H-atoms can not be fixed. 
;
_vrf_PLAT430_7                   
; 
PROBLEM: Short Inter D...A Contact  O3W    ..  O4W     ..       2.70 Ang. 
RESPONSE: This is H bond contact to the O atom from water molecule which 
may be slightly shortened due to disorder of the solvent. 
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C23 H19 Lu O10, 3.5(H2O))'
_chemical_formula_sum            'C46 H52 Lu2 O27'
_chemical_formula_weight         1386.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.535(5)
_cell_length_b                   23.826(5)
_cell_length_c                   8.463(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.280(5)
_cell_angle_gamma                90
_cell_volume                     2644.9(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.798
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7622
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.709
_diffrn_reflns_theta_max         25.106
_diffrn_reflns_theta_full        25.106
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2425
_reflns_number_gt                1982
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0637P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         2425
_refine_ls_number_parameters     183
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.0955
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.067
_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
Lu1 Lu 0.87873(4) 0.500000 0.16628(6) 0.02663(19) Uani 1 2 d S T P A .
O4A O 0.8810(11) 0.5487(5) 0.3985(18) 0.037(2) Uani 0.5 1 d . . P A 2
O1 O 0.4315(5) 0.9268(2) 1.0498(8) 0.0460(17) Uani 1 1 d . . . . .
O4B O 0.9005(11) 0.5743(5) 0.3662(18) 0.037(2) Uani 0.5 1 d . . P A 1
O1W O 1.0527(6) 0.500000 0.2939(11) 0.046(2) Uani 1 2 d S T P A .
H1W H 1.064502 0.477850 0.375106 0.068 Uiso 0.5 1 d R U P B -1
H1WA H 1.099282 0.500000 0.242406 0.068 Uiso 1 2 d R U P . .
O2 O 0.6020(5) 0.7195(2) 0.8137(7) 0.0413(16) Uani 1 1 d . . . . .
O2W O 0.7727(7) 0.500000 -0.0980(11) 0.047(2) Uani 1 2 d S T P A .
H2W H 0.724536 0.524310 -0.145256 0.070 Uiso 1 1 d R U . . .
O3 O 0.7498(5) 0.5625(3) 0.2030(9) 0.0542(18) Uani 1 1 d . . . . .
C1 C 0.500000 0.9024(4) 1.000000 0.029(2) Uani 1 2 d S T P . .
C2 C 0.500000 0.8393(4) 1.000000 0.021(2) Uani 1 2 d S T P . .
C3 C 0.5552(6) 0.8112(3) 0.9052(8) 0.0232(16) Uani 1 1 d . . . . .
H3 H 0.591932 0.830883 0.843718 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5537(6) 0.7529(3) 0.9053(9) 0.0266(17) Uani 1 1 d . . . . .
C5 C 0.500000 0.7238(4) 1.000000 0.031(3) Uani 1 2 d S T P . .
H5 H 0.499998 0.684744 1.000001 0.037 Uiso 1 2 calc R U P . .
C6 C 0.6530(7) 0.7487(3) 0.7060(11) 0.041(2) Uani 1 1 d . . . . .
H6A H 0.708442 0.771462 0.768275 0.049 Uiso 1 1 calc R U . . .
H6B H 0.605556 0.772739 0.631375 0.049 Uiso 1 1 calc R U . . .
C7 C 0.6931(7) 0.7034(3) 0.6142(12) 0.0377(19) Uani 1 1 d . . . . .
C8 C 0.7885(7) 0.6809(4) 0.6728(13) 0.052(3) Uani 1 1 d . . . . .
H8 H 0.829183 0.692403 0.772783 0.063 Uiso 1 1 calc R U . . .
C9 C 0.8237(7) 0.6403(4) 0.5796(11) 0.040(2) Uani 1 1 d . . . . .
H9 H 0.888784 0.625404 0.617354 0.048 Uiso 1 1 calc R U . . .
C10 C 0.7645(6) 0.6226(3) 0.4366(10) 0.0305(17) Uani 1 1 d . . . . .
C11 C 0.6679(7) 0.6459(4) 0.3764(11) 0.042(2) Uani 1 1 d . . . . .
H11 H 0.627550 0.633805 0.276779 0.050 Uiso 1 1 calc R U . . .
C12 C 0.6319(7) 0.6864(4) 0.4630(11) 0.046(2) Uani 1 1 d . . . . .
H12 H 0.567955 0.702247 0.422108 0.056 Uiso 1 1 calc R U . . .
C13 C 0.8031(7) 0.5799(4) 0.3304(10) 0.0344(18) Uani 1 1 d . . . . .
O3W O 0.6265(8) 0.5826(5) -0.208(2) 0.169(6) Uani 1 1 d . . . . .
O5W O 0.438(3) 0.500000 -0.214(5) 0.127(12) Uiso 0.45 2 d S . P . .
O4W O 0.529(2) 0.5660(10) 0.031(4) 0.122(11) Uiso 0.375 1 d . . P . .
O6W O 0.486(5) 0.530(2) -0.449(8) 0.10(2) Uiso 0.15 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O1 2.206(5) 3_544 ?
Lu1 O1 2.206(5) 8_564 ?
Lu1 O4A 2.277(14) 6_565 ?
Lu1 O4A 2.277(14) . ?
Lu1 O1W 2.336(9) . ?
Lu1 O2W 2.341(9) . ?
Lu1 O3 2.372(6) 6_565 ?
Lu1 O3 2.372(6) . ?
Lu1 O4B 2.415(14) 6_565 ?
Lu1 O4B 2.415(14) . ?
Lu1 C13 2.702(8) . ?
Lu1 C13 2.702(8) 6_565 ?
O4A C13 1.301(16) . ?
O1 C1 1.253(7) . ?
O4B C13 1.285(16) . ?
O1W H1W 0.8501 . ?
O1W H1WA 0.8499 . ?
O2 C4 1.383(8) . ?
O2 C6 1.448(9) . ?
O2W H2W 0.8896 . ?
O2W H2W 0.8896 6_565 ?
O3 C13 1.212(10) . ?
C1 C2 1.503(14) . ?
C2 C3 1.396(8) . ?
C2 C3 1.396(8) 2_657 ?
C3 C4 1.389(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.507(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.372(13) . ?
C7 C12 1.402(13) . ?
C8 C9 1.404(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.344(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.395(12) . ?
C10 C13 1.534(10) . ?
C11 C12 1.371(12) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
O4W O4W 0.82(6) 2_655 ?
O6W O6W 1.02(11) 2_654 ?
O6W O6W 1.41(11) 6_565 ?
O6W O6W 1.74(10) 5_664 ?

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 Lu1 O1 104.4(3) 3_544 8_564 ?
O1 Lu1 O4A 92.6(4) 3_544 6_565 ?
O1 Lu1 O4A 148.4(4) 8_564 6_565 ?
O1 Lu1 O4A 148.4(4) 3_544 . ?
O1 Lu1 O4A 92.6(4) 8_564 . ?
O4A Lu1 O4A 61.3(6) 6_565 . ?
O1 Lu1 O1W 78.8(2) 3_544 . ?
O1 Lu1 O1W 78.8(2) 8_564 . ?
O4A Lu1 O1W 78.7(4) 6_565 . ?
O4A Lu1 O1W 78.7(4) . . ?
O1 Lu1 O2W 76.3(2) 3_544 . ?
O1 Lu1 O2W 76.3(2) 8_564 . ?
O4A Lu1 O2W 134.4(4) 6_565 . ?
O4A Lu1 O2W 134.4(4) . . ?
O1W Lu1 O2W 138.8(3) . . ?
O1 Lu1 O3 83.8(2) 3_544 6_565 ?
O1 Lu1 O3 152.2(2) 8_564 6_565 ?
O1W Lu1 O3 129.0(2) . 6_565 ?
O2W Lu1 O3 80.1(2) . 6_565 ?
O1 Lu1 O3 152.2(2) 3_544 . ?
O1 Lu1 O3 83.8(2) 8_564 . ?
O4A Lu1 O3 93.5(4) 6_565 . ?
O4A Lu1 O3 54.6(4) . . ?
O1W Lu1 O3 129.0(2) . . ?
O2W Lu1 O3 80.1(2) . . ?
O3 Lu1 O3 77.8(4) 6_565 . ?
O1 Lu1 O4B 74.7(4) 3_544 6_565 ?
O1 Lu1 O4B 153.5(4) 8_564 6_565 ?
O1W Lu1 O4B 75.0(4) . 6_565 ?
O2W Lu1 O4B 127.5(3) . 6_565 ?
O3 Lu1 O4B 54.2(4) 6_565 6_565 ?
O3 Lu1 O4B 109.6(4) . 6_565 ?
O1 Lu1 O4B 153.5(4) 3_544 . ?
O1 Lu1 O4B 74.7(4) 8_564 . ?
O1W Lu1 O4B 75.0(4) . . ?
O2W Lu1 O4B 127.5(3) . . ?
O3 Lu1 O4B 109.6(4) 6_565 . ?
O3 Lu1 O4B 54.2(4) . . ?
O4B Lu1 O4B 94.2(6) 6_565 . ?
O1 Lu1 C13 172.6(2) 3_544 . ?
O1 Lu1 C13 83.0(2) 8_564 . ?
O4A Lu1 C13 80.9(4) 6_565 . ?
O4A Lu1 C13 28.7(4) . . ?
O1W Lu1 C13 103.2(2) . . ?
O2W Lu1 C13 105.7(3) . . ?
O3 Lu1 C13 89.5(3) 6_565 . ?
O3 Lu1 C13 26.6(2) . . ?
O4B Lu1 C13 98.8(4) 6_565 . ?
O4B Lu1 C13 28.4(4) . . ?
O1 Lu1 C13 83.0(2) 3_544 6_565 ?
O1 Lu1 C13 172.6(2) 8_564 6_565 ?
O1W Lu1 C13 103.2(2) . 6_565 ?
O2W Lu1 C13 105.7(3) . 6_565 ?
O3 Lu1 C13 26.6(2) 6_565 6_565 ?
O3 Lu1 C13 89.5(3) . 6_565 ?
O4B Lu1 C13 28.4(4) 6_565 6_565 ?
O4B Lu1 C13 98.8(4) . 6_565 ?
C13 Lu1 C13 89.6(4) . 6_565 ?
C13 O4A Lu1 94.1(9) . . ?
C1 O1 Lu1 150.0(6) . 3_456 ?
C13 O4B Lu1 88.3(8) . . ?
Lu1 O1W H1W 109.9 . . ?
Lu1 O1W H1WA 123.6 . . ?
H1W O1W H1WA 113.5 . . ?
C4 O2 C6 116.2(6) . . ?
Lu1 O2W H2W 129.7 . . ?
Lu1 O2W H2W 129.67(12) . 6_565 ?
H2W O2W H2W 81.2 . 6_565 ?
C13 O3 Lu1 92.0(5) . . ?
O1 C1 O1 124.6(10) . 2_657 ?
O1 C1 C2 117.7(5) . . ?
O1 C1 C2 117.7(5) 2_657 . ?
C3 C2 C3 122.6(9) . 2_657 ?
C3 C2 C1 118.7(5) . . ?
C3 C2 C1 118.7(5) 2_657 . ?
C4 C3 C2 118.0(7) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
O2 C4 C3 124.4(6) . . ?
O2 C4 C5 115.0(7) . . ?
C3 C4 C5 120.6(7) . . ?
C4 C5 C4 120.2(9) . 2_657 ?
C4 C5 H5 119.9 . . ?
C4 C5 H5 119.9 2_657 . ?
O2 C6 C7 105.6(6) . . ?
O2 C6 H6A 110.6 . . ?
C7 C6 H6A 110.6 . . ?
O2 C6 H6B 110.6 . . ?
C7 C6 H6B 110.6 . . ?
H6A C6 H6B 108.7 . . ?
C8 C7 C12 120.5(8) . . ?
C8 C7 C6 121.3(9) . . ?
C12 C7 C6 118.1(8) . . ?
C7 C8 C9 119.1(9) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 120.8(9) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.1(8) . . ?
C9 C10 C13 121.5(8) . . ?
C11 C10 C13 118.3(8) . . ?
C12 C11 C10 120.5(9) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C7 118.9(9) . . ?
C11 C12 H12 120.5 . . ?
C7 C12 H12 120.5 . . ?
O3 C13 O4B 121.7(9) . . ?
O3 C13 O4A 116.1(9) . . ?
O3 C13 C10 122.3(8) . . ?
O4B C13 C10 114.1(10) . . ?
O4A C13 C10 118.3(9) . . ?
O3 C13 Lu1 61.4(4) . . ?
O4B C13 Lu1 63.3(7) . . ?
O4A C13 Lu1 57.2(7) . . ?
C10 C13 Lu1 175.2(6) . . ?
O6W O6W O6W 90.00(2) 2_654 6_565 ?
O6W O6W O6W 54(4) 2_654 5_664 ?
O6W O6W O6W 36(4) 6_565 5_664 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Lu1 O1 C1 O1 -29.0(8) 3_456 . . 2_657 ?
Lu1 O1 C1 C2 151.0(8) 3_456 . . . ?
O1 C1 C2 C3 162.2(5) . . . . ?
O1 C1 C2 C3 -17.8(5) 2_657 . . . ?
O1 C1 C2 C3 -17.8(5) . . . 2_657 ?
O1 C1 C2 C3 162.2(5) 2_657 . . 2_657 ?
C3 C2 C3 C4 0.6(5) 2_657 . . . ?
C1 C2 C3 C4 -179.4(5) . . . . ?
C6 O2 C4 C3 -2.9(12) . . . . ?
C6 O2 C4 C5 176.2(7) . . . . ?
C2 C3 C4 O2 177.9(6) . . . . ?
C2 C3 C4 C5 -1.2(11) . . . . ?
O2 C4 C5 C4 -178.5(8) . . . 2_657 ?
C3 C4 C5 C4 0.6(6) . . . 2_657 ?
C4 O2 C6 C7 -176.6(7) . . . . ?
O2 C6 C7 C8 -89.8(10) . . . . ?
O2 C6 C7 C12 92.8(10) . . . . ?
C12 C7 C8 C9 -0.4(14) . . . . ?
C6 C7 C8 C9 -177.7(8) . . . . ?
C7 C8 C9 C10 -1.4(14) . . . . ?
C8 C9 C10 C11 1.9(14) . . . . ?
C8 C9 C10 C13 177.8(8) . . . . ?
C9 C10 C11 C12 -0.7(14) . . . . ?
C13 C10 C11 C12 -176.7(8) . . . . ?
C10 C11 C12 C7 -1.0(14) . . . . ?
C8 C7 C12 C11 1.5(14) . . . . ?
C6 C7 C12 C11 179.0(8) . . . . ?
Lu1 O3 C13 O4B 20.3(11) . . . . ?
Lu1 O3 C13 O4A -17.5(10) . . . . ?
Lu1 O3 C13 C10 -176.4(7) . . . . ?
Lu1 O4B C13 O3 -19.9(11) . . . . ?
Lu1 O4B C13 C10 175.5(6) . . . . ?
Lu1 O4A C13 O3 18.3(10) . . . . ?
Lu1 O4A C13 C10 178.0(6) . . . . ?
C9 C10 C13 O3 178.2(9) . . . . ?
C11 C10 C13 O3 -5.9(13) . . . . ?
C9 C10 C13 O4B -17.3(13) . . . . ?
C11 C10 C13 O4B 158.6(10) . . . . ?
C9 C10 C13 O4A 19.7(13) . . . . ?
C11 C10 C13 O4A -164.4(10) . . . . ?

_refine_diff_density_max         0.807
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.191

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1473239'
_audit_update_record             
;
2017-08-21 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form 
_vrf_PLAT430_4                   
; 
PROBLEM: Short Inter D...A Contact O6W .. O6W .. 1.97 Ang. 
RESPONSE: Short Inter D...A Contact is due to strong disorder of the solvent. 
We assign these water molecules with such short interaction as 
disordered ones. When the distance > 2.5 Ang, it is the H bond contact 
to the O atom from water molecule. 
;
_vrf_PLAT043_4                   
; 
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 14.11 Check 
RESPONSE: The difference results from the hydrogens of lattice water 
molecules which were not located and included to refinement, 
however, they were included to final formula to calculate 
actual cell metric values. 
;
_vrf_PLAT306_4                   
; 
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O3W Check 
RESPONSE: Due to disorder on lattice O-atom, H-atoms can not be fixed. 
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C23 H19 Er O10,3.5(H2O))'
_chemical_formula_sum            'C46 H52 Er2 O27'
_chemical_formula_weight         1371.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.538(5)
_cell_length_b                   23.892(5)
_cell_length_c                   8.482(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.265(5)
_cell_angle_gamma                90
_cell_volume                     2658.9(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       block
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_F_000             1322
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.222
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9969
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.705
_diffrn_reflns_theta_max         28.446
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3449
_reflns_number_gt                3021
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0411P)²+1.6142P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         3449
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0751
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
Er1 Er 0.37756(2) 0.000000 0.16650(2) 0.02318(8) Uani 1 2 d S T P A .
O3 O 0.2486(2) 0.06364(13) 0.2038(4) 0.0501(8) Uani 1 1 d . . . . .
O4A O 0.3998(5) 0.0739(3) 0.3684(8) 0.0389(12) Uani 0.5 1 d . . P A 2
O1 O 0.0688(2) 0.42642(11) 0.9541(4) 0.0451(7) Uani 1 1 d . . . . .
O4B O 0.3779(5) 0.0488(3) 0.4044(8) 0.0389(12) Uani 0.5 1 d . . P A 1
O1W O 0.5533(3) 0.000000 0.2912(5) 0.0445(10) Uani 1 2 d S T P A .
H1WA H 0.586126 -0.019810 0.238186 0.067 Uiso 0.5 1 d R U P B -1
H1W H 0.555146 -0.014450 0.384426 0.067 Uiso 0.5 1 d R U P . .
O2W O 0.2701(3) 0.000000 -0.0987(5) 0.0483(10) Uani 1 2 d S T P A .
H2WB H 0.220917 0.022780 -0.150616 0.072 Uiso 1 1 d R U . . .
O2 O 0.1022(2) 0.22024(10) 0.8158(3) 0.0360(6) Uani 1 1 d . . . . .
C1 C 0.000000 0.40194(19) 1.000000 0.0265(10) Uani 1 2 d S T P . .
C2 C 0.000000 0.33909(18) 1.000000 0.0220(9) Uani 1 2 d S T P . .
C3 C 0.0552(2) 0.31093(13) 0.9072(4) 0.0241(6) Uani 1 1 d . . . . .
H3 H 0.092564 0.330506 0.846769 0.029 Uiso 1 1 calc R U . . .
C4 C 0.0535(2) 0.25284(13) 0.9066(4) 0.0253(7) Uani 1 1 d . . . . .
C5 C 0.000000 0.22374(19) 1.000000 0.0272(10) Uani 1 2 d S T P . .
H5 H -0.000001 0.184820 0.999998 0.033 Uiso 1 2 calc R U P . .
C6 C 0.1541(3) 0.24839(15) 0.7107(5) 0.0363(8) Uani 1 1 d . . . . .
H6A H 0.210655 0.270010 0.774247 0.044 Uiso 1 1 calc R U . . .
H6B H 0.107859 0.273657 0.638614 0.044 Uiso 1 1 calc R U . . .
C7 C 0.1923(3) 0.20441(15) 0.6136(4) 0.0322(8) Uani 1 1 d . . . . .
C8 C 0.2878(3) 0.18142(17) 0.6705(5) 0.0410(9) Uani 1 1 d . . . . .
H8 H 0.328674 0.193238 0.769767 0.049 Uiso 1 1 calc R U . . .
C9 C 0.3236(3) 0.14098(17) 0.5819(5) 0.0396(9) Uani 1 1 d . . . . .
H9 H 0.388213 0.125784 0.621503 0.048 Uiso 1 1 calc R U . . .
C10 C 0.2631(3) 0.12316(15) 0.4341(4) 0.0298(7) Uani 1 1 d . . . . .
C11 C 0.1675(3) 0.14709(18) 0.3751(5) 0.0391(9) Uani 1 1 d . . . . .
H11 H 0.126753 0.135895 0.275117 0.047 Uiso 1 1 calc R U . . .
C12 C 0.1332(3) 0.18735(18) 0.4649(5) 0.0407(9) Uani 1 1 d . . . . .
H12 H 0.069208 0.203259 0.424680 0.049 Uiso 1 1 calc R U . . .
C13 C 0.3020(3) 0.08026(16) 0.3374(5) 0.0318(8) Uani 1 1 d . . . . .
O3W O 0.1242(4) 0.0835(3) 0.7980(8) 0.131(2) Uiso 1 1 d . . . . .
O4W O 0.000000 0.078(2) 0.000000 0.105(16) Uiso 0.2 2 d S . P . .
O5W O 0.0576(14) 0.000000 0.233(2) 0.104(6) Uiso 0.4 2 d S . P . .
O6W O 0.000000 0.0411(11) 0.500000 0.113(8) Uiso 0.3 2 d S . P . .
O7W O -0.0314(17) 0.0613(9) 0.959(3) 0.119(8) Uiso 0.3 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.243(3) 4_546 ?
Er1 O1 2.243(3) 7_556 ?
Er1 O4B 2.330(7) . ?
Er1 O4B 2.330(7) 6 ?
Er1 O1W 2.353(4) . ?
Er1 O2W 2.359(4) . ?
Er1 O3 2.394(3) 6 ?
Er1 O3 2.394(3) . ?
Er1 O4A 2.426(7) 6 ?
Er1 O4A 2.426(7) . ?
Er1 C13 2.748(3) 6 ?
Er1 C13 2.748(3) . ?
O3 C13 1.249(5) . ?
O4A C13 1.292(7) . ?
O1 C1 1.241(3) . ?
O4B C13 1.287(8) . ?
O1W H1WA 0.8501 . ?
O1W H1W 0.8573 . ?
O1W H1W 0.8573 6 ?
O2W H2WB 0.8881 . ?
O2W H2WB 0.8881 6 ?
O2 C4 1.373(4) . ?
O2 C6 1.432(4) . ?
C1 C2 1.502(6) . ?
C2 C3 1.386(4) 2_557 ?
C2 C3 1.386(4) . ?
C3 C4 1.388(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.503(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.378(5) . ?
C7 C12 1.378(6) . ?
C8 C9 1.383(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(5) . ?
C10 C13 1.488(5) . ?
C11 C12 1.377(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
O4W O7W 0.62(4) 1_554 ?
O4W O7W 0.62(4) 2_556 ?
O7W O7W 0.96(4) 2_557 ?

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 Er1 O1 103.24(14) 4_546 7_556 ?
O1 Er1 O4B 148.8(2) 4_546 . ?
O1 Er1 O4B 94.07(18) 7_556 . ?
O1 Er1 O4B 94.06(18) 4_546 6 ?
O1 Er1 O4B 148.8(2) 7_556 6 ?
O4B Er1 O4B 60.1(3) . 6 ?
O1 Er1 O1W 78.47(10) 4_546 . ?
O1 Er1 O1W 78.47(10) 7_556 . ?
O4B Er1 O1W 79.89(18) . . ?
O4B Er1 O1W 79.89(18) 6 . ?
O1 Er1 O2W 76.00(11) 4_546 . ?
O1 Er1 O2W 76.00(11) 7_556 . ?
O4B Er1 O2W 134.04(19) . . ?
O4B Er1 O2W 134.04(19) 6 . ?
O1W Er1 O2W 138.29(15) . . ?
O1 Er1 O3 83.74(11) 4_546 6 ?
O1 Er1 O3 152.44(11) 7_556 6 ?
O4B Er1 O3 92.82(17) . 6 ?
O4B Er1 O3 54.10(18) 6 6 ?
O1W Er1 O3 129.04(10) . 6 ?
O2W Er1 O3 80.06(12) . 6 ?
O1 Er1 O3 152.44(11) 4_546 . ?
O1 Er1 O3 83.74(11) 7_556 . ?
O4B Er1 O3 54.10(18) . . ?
O4B Er1 O3 92.83(17) 6 . ?
O1W Er1 O3 129.04(10) . . ?
O2W Er1 O3 80.06(12) . . ?
O3 Er1 O3 78.84(17) 6 . ?
O1 Er1 O4A 75.74(18) 4_546 6 ?
O1 Er1 O4A 153.47(18) 7_556 6 ?
O4B Er1 O4A 77.3(2) . 6 ?
O4B Er1 O4A 18.36(18) 6 6 ?
O1W Er1 O4A 75.35(17) . 6 ?
O2W Er1 O4A 127.81(17) . 6 ?
O3 Er1 O4A 53.99(17) 6 6 ?
O3 Er1 O4A 109.65(17) . 6 ?
O1 Er1 O4A 153.47(18) 4_546 . ?
O1 Er1 O4A 75.74(18) 7_556 . ?
O1W Er1 O4A 75.35(17) . . ?
O2W Er1 O4A 127.81(17) . . ?
O3 Er1 O4A 109.65(17) 6 . ?
O3 Er1 O4A 53.99(17) . . ?
O4A Er1 O4A 93.4(3) 6 . ?
O1 Er1 C13 84.14(11) 4_546 6 ?
O1 Er1 C13 172.63(10) 7_556 6 ?
O4B Er1 C13 79.28(18) . 6 ?
O4B Er1 C13 27.82(19) 6 6 ?
O1W Er1 C13 103.24(11) . 6 ?
O2W Er1 C13 106.30(12) . 6 ?
O3 Er1 C13 27.01(10) 6 6 ?
O3 Er1 C13 89.72(12) . 6 ?
O1 Er1 C13 172.63(10) 4_546 . ?
O1 Er1 C13 84.14(11) 7_556 . ?
O4B Er1 C13 27.82(19) . . ?
O4B Er1 C13 79.29(18) 6 . ?
O1W Er1 C13 103.24(11) . . ?
O2W Er1 C13 106.30(12) . . ?
O3 Er1 C13 89.72(12) 6 . ?
O3 Er1 C13 27.01(10) . . ?
O4A Er1 C13 97.64(17) 6 . ?
O4A Er1 C13 28.05(17) . . ?
C13 Er1 C13 88.49(16) 6 . ?
C13 O3 Er1 92.5(2) . . ?
C13 O4A Er1 90.0(4) . . ?
C1 O1 Er1 149.8(3) . 7_556 ?
C13 O4B Er1 94.5(4) . . ?
Er1 O1W H1WA 111.4 . . ?
Er1 O1W H1W 102.2 . . ?
H1WA O1W H1W 111.3 . . ?
Er1 O1W H1W 102.20(9) . 6 ?
H1WA O1W H1W 144.3 . 6 ?
H1W O1W H1W 47.5 . 6 ?
Er1 O2W H2WB 133.2 . . ?
Er1 O2W H2WB 133.15(6) . 6 ?
H2WB O2W H2WB 75.6 . 6 ?
C4 O2 C6 117.4(3) . . ?
O1 C1 O1 123.8(5) 2_557 . ?
O1 C1 C2 118.1(2) 2_557 . ?
O1 C1 C2 118.1(2) . . ?
C3 C2 C3 121.9(4) 2_557 . ?
C3 C2 C1 119.0(2) 2_557 . ?
C3 C2 C1 119.0(2) . . ?
C2 C3 C4 118.5(3) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
O2 C4 C5 115.3(3) . . ?
O2 C4 C3 124.0(3) . . ?
C5 C4 C3 120.7(3) . . ?
C4 C5 C4 119.8(4) 2_557 . ?
C4 C5 H5 120.1 2_557 . ?
C4 C5 H5 120.1 . . ?
O2 C6 C7 107.5(3) . . ?
O2 C6 H6A 110.2 . . ?
C7 C6 H6A 110.2 . . ?
O2 C6 H6B 110.2 . . ?
C7 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
C8 C7 C12 119.1(3) . . ?
C8 C7 C6 120.4(4) . . ?
C12 C7 C6 120.5(4) . . ?
C7 C8 C9 120.8(4) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C10 119.9(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C11 119.3(3) . . ?
C9 C10 C13 120.0(3) . . ?
C11 C10 C13 120.7(3) . . ?
C12 C11 C10 120.0(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C7 120.9(4) . . ?
C11 C12 H12 119.6 . . ?
C7 C12 H12 119.6 . . ?
O3 C13 O4B 115.8(4) . . ?
O3 C13 O4A 118.8(4) . . ?
O3 C13 C10 120.9(3) . . ?
O4B C13 C10 120.8(4) . . ?
O4A C13 C10 116.9(4) . . ?
O3 C13 Er1 60.50(19) . . ?
O4B C13 Er1 57.7(3) . . ?
O4A C13 Er1 62.0(3) . . ?
C10 C13 Er1 178.4(3) . . ?
O7W O4W O7W 102(10) 1_554 2_556 ?
O4W O7W O7W 39(5) 1_556 2_557 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Er1 O1 C1 O1 -31.8(4) 7_556 . . 2_557 ?
Er1 O1 C1 C2 148.2(4) 7_556 . . . ?
O1 C1 C2 C3 -18.9(2) 2_557 . . 2_557 ?
O1 C1 C2 C3 161.1(2) . . . 2_557 ?
O1 C1 C2 C3 161.1(2) 2_557 . . . ?
O1 C1 C2 C3 -18.9(2) . . . . ?
C3 C2 C3 C4 0.8(2) 2_557 . . . ?
C1 C2 C3 C4 -179.2(2) . . . . ?
C6 O2 C4 C5 176.8(3) . . . . ?
C6 O2 C4 C3 -2.7(5) . . . . ?
C2 C3 C4 O2 177.8(3) . . . . ?
C2 C3 C4 C5 -1.7(5) . . . . ?
O2 C4 C5 C4 -178.7(3) . . . 2_557 ?
C3 C4 C5 C4 0.9(2) . . . 2_557 ?
C4 O2 C6 C7 -174.7(3) . . . . ?
O2 C6 C7 C8 -90.3(4) . . . . ?
O2 C6 C7 C12 91.0(4) . . . . ?
C12 C7 C8 C9 -1.2(6) . . . . ?
C6 C7 C8 C9 -179.9(4) . . . . ?
C7 C8 C9 C10 0.0(7) . . . . ?
C8 C9 C10 C11 1.2(6) . . . . ?
C8 C9 C10 C13 179.1(4) . . . . ?
C9 C10 C11 C12 -1.1(6) . . . . ?
C13 C10 C11 C12 -179.0(4) . . . . ?
C10 C11 C12 C7 -0.2(6) . . . . ?
C8 C7 C12 C11 1.3(6) . . . . ?
C6 C7 C12 C11 -180.0(4) . . . . ?
Er1 O3 C13 O4B -16.9(5) . . . . ?
Er1 O3 C13 O4A 22.0(5) . . . . ?
Er1 O3 C13 C10 -179.3(3) . . . . ?
Er1 O4B C13 O3 17.4(5) . . . . ?
Er1 O4B C13 C10 179.8(3) . . . . ?
Er1 O4A C13 O3 -21.6(5) . . . . ?
Er1 O4A C13 C10 178.8(3) . . . . ?
C9 C10 C13 O3 180.0(4) . . . . ?
C11 C10 C13 O3 -2.2(6) . . . . ?
C9 C10 C13 O4B 18.4(6) . . . . ?
C11 C10 C13 O4B -163.7(5) . . . . ?
C9 C10 C13 O4A -20.9(6) . . . . ?
C11 C10 C13 O4A 157.0(5) . . . . ?

_refine_diff_density_max         0.967
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.125

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1544752'
_audit_update_record             
;
2017-08-21 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form 
_vrf_CHEMW03_2                   
; 
PROBLEM: ALERT: The ratio of given/expected molecular weight as 
RESPONSE:  The difference results from the lattice water 
molecules which were removed by squeeze, 
however, they were included to final formula to calculate 
actual cell metric values. 
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H15 Ce O8 , 4.5(H2O)'
_chemical_formula_sum            'C23 H24 Ce O12.50'
_chemical_formula_weight         640.54

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'
Ce Ce -0.2486 2.6331 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   22.702(5)
_cell_length_b                   7.530(5)
_cell_length_c                   29.233(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4997(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       slice
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_F_000             2200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.863
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30644
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_av_R_equivalents  0.1366
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.393
_diffrn_reflns_theta_max         26.542
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5213
_reflns_number_gt                3023
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0530P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5213
_refine_ls_number_parameters     323
_refine_ls_number_restraints     315
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1177
_refine_ls_wR_factor_gt          0.0890
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.960
_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
Ce1 Ce -0.23060(2) -0.92647(4) 0.41733(2) 0.02067(11) Uani 1 1 d . . . . .
O5 O -0.18077(19) -0.6163(6) 0.41739(17) 0.0330(11) Uani 1 1 d . . . . .
O7 O 0.2134(2) 0.7848(6) 0.12996(15) 0.0322(12) Uani 1 1 d . . . . .
O1 O 0.2034(2) 0.1904(6) 0.53810(15) 0.0247(11) Uani 1 1 d . . . . .
O4 O -0.1258(2) -0.8474(6) 0.43299(18) 0.0381(13) Uani 1 1 d . . . . .
O8 O 0.1867(3) 1.0348(7) 0.16138(18) 0.0571(18) Uani 1 1 d . . . . .
O2 O 0.2525(3) 0.3853(8) 0.49915(18) 0.064(2) Uani 1 1 d . . . . .
O3 O 0.0733(3) -0.0987(8) 0.41361(18) 0.0617(19) Uani 1 1 d . . . . .
O6 O 0.1612(3) 0.3888(9) 0.3423(2) 0.072(2) Uani 1 1 d . . . . .
C2 C 0.1799(3) 0.2225(9) 0.4588(2) 0.0263(15) Uani 1 1 d . . . . .
C4 C 0.1115(3) 0.0414(10) 0.4184(3) 0.0369(18) Uani 1 1 d . . . . .
C3 C 0.1421(3) 0.0816(10) 0.4583(2) 0.0309(16) Uani 1 1 d . . . . .
H3 H 0.136949 0.012911 0.484448 0.037 Uiso 1 1 calc R U . . .
C15 C -0.1302(3) -0.6828(9) 0.4266(2) 0.0256(16) Uani 1 1 d . . . . .
C7 C 0.1878(3) 0.3281(10) 0.4195(2) 0.0363(17) Uani 1 1 d . . . . .
H7 H 0.214065 0.422761 0.419619 0.044 Uiso 1 1 calc R U . . .
C9 C 0.0197(3) -0.3476(11) 0.4397(3) 0.043(2) Uani 1 1 d . . . . .
C13 C -0.0835(3) -0.3855(9) 0.4246(3) 0.044(2) Uani 1 1 d . . . . .
H13 H -0.120096 -0.337344 0.417598 0.053 Uiso 1 1 calc R U . . .
C10 C 0.0255(3) -0.5283(10) 0.4426(3) 0.0392(19) Uani 1 1 d . . . . .
H10 H 0.062463 -0.577145 0.447996 0.047 Uiso 1 1 calc R U . . .
C1 C 0.2135(3) 0.2686(9) 0.5004(2) 0.0285(16) Uani 1 1 d . . . . .
C12 C -0.0773(3) -0.5683(10) 0.4296(2) 0.0310(16) Uani 1 1 d . . . . .
C5 C 0.1183(4) 0.1447(11) 0.3799(3) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.097606 0.117582 0.353323 0.052 Uiso 1 1 calc R U . . .
C6 C 0.1558(4) 0.2882(11) 0.3809(3) 0.042(2) Uani 1 1 d . . . . .
C14 C -0.0353(3) -0.2752(12) 0.4300(3) 0.051(2) Uani 1 1 d . . . . .
H14 H -0.039590 -0.152878 0.427207 0.061 Uiso 1 1 calc R U . . .
C11 C -0.0223(3) -0.6392(10) 0.4377(3) 0.0362(18) Uani 1 1 d . . . . .
H11 H -0.017450 -0.761610 0.439793 0.043 Uiso 1 1 calc R U . . .
C8 C 0.0704(4) -0.2243(12) 0.4489(3) 0.053(2) Uani 1 1 d . . . . .
H8A H 0.064836 -0.164949 0.478013 0.063 Uiso 1 1 calc R U . . .
H8B H 0.106926 -0.291074 0.450251 0.063 Uiso 1 1 calc R U . . .
C16 C 0.1828(12) 0.551(2) 0.3423(5) 0.108(9) Uani 0.593(9) 1 d . . P A 1
H16A H 0.223213 0.547001 0.353108 0.108 Uiso 0.593(9) 1 calc R U P A 1
H16B H 0.160321 0.623608 0.363280 0.108 Uiso 0.593(9) 1 calc R U P A 1
C17 C 0.1814(6) 0.6329(13) 0.2958(2) 0.074(7) Uani 0.593(9) 1 d G . P A 1
C18 C 0.1859(6) 0.8165(12) 0.2923(3) 0.081(7) Uani 0.593(9) 1 d G . P A 1
H18 H 0.186384 0.886141 0.318550 0.081 Uiso 0.593(9) 1 calc R U P A 1
C19 C 0.1896(6) 0.8960(9) 0.2495(3) 0.065(5) Uani 0.593(9) 1 d G . P A 1
H19 H 0.192634 1.018849 0.247092 0.065 Uiso 0.593(9) 1 calc R U P A 1
C20 C 0.1889(5) 0.7919(12) 0.2102(2) 0.032(3) Uani 0.593(9) 1 d G . P A 1
C21 C 0.1844(5) 0.6084(11) 0.2137(2) 0.044(4) Uani 0.593(9) 1 d G . P A 1
H21 H 0.183952 0.538727 0.187471 0.044 Uiso 0.593(9) 1 calc R U P A 1
C22 C 0.1807(6) 0.5288(9) 0.2566(3) 0.065(6) Uani 0.593(9) 1 d G . P A 1
H22 H 0.177702 0.406015 0.258929 0.065 Uiso 0.593(9) 1 calc R U P A 1
C16A C 0.1190(12) 0.394(4) 0.3103(8) 0.099(11) Uani 0.407(9) 1 d . . P A 2
H16C H 0.081919 0.430818 0.323880 0.099 Uiso 0.407(9) 1 calc R U P A 2
H16D H 0.113670 0.277277 0.296928 0.099 Uiso 0.407(9) 1 calc R U P A 2
C17A C 0.1381(8) 0.528(2) 0.2733(5) 0.067(7) Uani 0.407(9) 1 d G . P A 2
C18A C 0.1441(9) 0.709(2) 0.2806(4) 0.106(13) Uani 0.407(9) 1 d G . P A 2
H18A H 0.138070 0.756318 0.309689 0.106 Uiso 0.407(9) 1 calc R U P A 2
C19A C 0.1590(9) 0.8206(18) 0.2445(5) 0.073(9) Uani 0.407(9) 1 d G . P A 2
H19A H 0.163060 0.942065 0.249419 0.073 Uiso 0.407(9) 1 calc R U P A 2
C20A C 0.1680(8) 0.7504(19) 0.2011(4) 0.032(3) Uani 0.407(9) 1 d G . P A 2
C21A C 0.1620(8) 0.5689(19) 0.1938(4) 0.056(7) Uani 0.407(9) 1 d G . P A 2
H21A H 0.168022 0.521940 0.164749 0.056 Uiso 0.407(9) 1 calc R U P A 2
C22A C 0.1470(8) 0.4576(17) 0.2299(6) 0.076(8) Uani 0.407(9) 1 d G . P A 2
H22A H 0.143031 0.336190 0.225019 0.076 Uiso 0.407(9) 1 calc R U P A 2
C23 C 0.1944(3) 0.8704(10) 0.1644(2) 0.0333(17) 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
Ce1 O1 2.456(4) 5_546 ?
Ce1 O7 2.461(5) 6_546 ?
Ce1 O5 2.468(4) 7 ?
Ce1 O2 2.491(5) 3_446 ?
Ce1 O4 2.494(5) . ?
Ce1 O8 2.524(5) 4_535 ?
Ce1 O5 2.595(5) . ?
Ce1 O7 2.606(5) 4_535 ?
Ce1 O1 2.665(4) 3_446 ?
Ce1 C15 2.939(7) . ?
Ce1 C23 2.952(7) 4_535 ?
Ce1 C1 2.969(7) 3_446 ?
O5 C15 1.282(7) . ?
O7 C23 1.270(8) . ?
O1 C1 1.271(7) . ?
O4 C15 1.257(8) . ?
O8 C23 1.253(9) . ?
O2 C1 1.248(8) . ?
O3 C4 1.373(8) . ?
O3 C8 1.401(9) . ?
O6 C16 1.313(17) . ?
O6 C16A 1.34(2) . ?
O6 C6 1.364(9) . ?
C2 C3 1.364(9) . ?
C2 C7 1.409(9) . ?
C2 C1 1.477(9) . ?
C4 C5 1.378(10) . ?
C4 C3 1.391(9) . ?
C3 H3 0.9300 . ?
C15 C12 1.481(9) . ?
C7 C6 1.375(9) . ?
C7 H7 0.9300 . ?
C9 C10 1.369(11) . ?
C9 C14 1.392(11) . ?
C9 C8 1.503(10) . ?
C13 C14 1.383(10) . ?
C13 C12 1.392(10) . ?
C13 H13 0.9300 . ?
C10 C11 1.376(10) . ?
C10 H10 0.9300 . ?
C12 C11 1.379(10) . ?
C5 C6 1.376(10) . ?
C5 H5 0.9300 . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C16 C17 1.493(15) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.3900 . ?
C17 C22 1.3900 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 C23 1.470(9) . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C16A C17A 1.54(2) . ?
C16A H16C 0.9700 . ?
C16A H16D 0.9700 . ?
C17A C18A 1.3900 . ?
C17A C22A 1.3900 . ?
C18A C19A 1.3900 . ?
C18A H18A 0.9300 . ?
C19A C20A 1.3900 . ?
C19A H19A 0.9300 . ?
C20A C21A 1.3900 . ?
C20A C23 1.526(12) . ?
C21A C22A 1.3900 . ?
C21A H21A 0.9300 . ?
C22A H22A 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 Ce1 O7 162.01(15) 5_546 6_546 ?
O1 Ce1 O5 74.68(15) 5_546 7 ?
O7 Ce1 O5 87.35(16) 6_546 7 ?
O1 Ce1 O2 67.63(17) 5_546 3_446 ?
O7 Ce1 O2 112.99(16) 6_546 3_446 ?
O5 Ce1 O2 86.9(2) 7 3_446 ?
O1 Ce1 O4 81.72(15) 5_546 . ?
O7 Ce1 O4 116.19(16) 6_546 . ?
O5 Ce1 O4 156.28(15) 7 . ?
O2 Ce1 O4 86.4(2) 3_446 . ?
O1 Ce1 O8 106.91(16) 5_546 4_535 ?
O7 Ce1 O8 76.50(18) 6_546 4_535 ?
O5 Ce1 O8 104.79(18) 7 4_535 ?
O2 Ce1 O8 165.6(2) 3_446 4_535 ?
O4 Ce1 O8 79.6(2) . 4_535 ?
O1 Ce1 O5 128.20(15) 5_546 . ?
O7 Ce1 O5 69.14(15) 6_546 . ?
O5 Ce1 O5 151.24(13) 7 . ?
O2 Ce1 O5 87.4(2) 3_446 . ?
O4 Ce1 O5 50.89(15) . . ?
O8 Ce1 O5 86.14(16) 4_535 . ?
O1 Ce1 O7 64.43(14) 5_546 4_535 ?
O7 Ce1 O7 108.59(17) 6_546 4_535 ?
O5 Ce1 O7 68.86(15) 7 4_535 ?
O2 Ce1 O7 130.31(17) 3_446 4_535 ?
O4 Ce1 O7 98.84(16) . 4_535 ?
O8 Ce1 O7 50.27(15) 4_535 4_535 ?
O5 Ce1 O7 133.31(15) . 4_535 ?
O1 Ce1 O1 114.95(17) 5_546 3_446 ?
O7 Ce1 O1 63.45(14) 6_546 3_446 ?
O5 Ce1 O1 85.85(15) 7 3_446 ?
O2 Ce1 O1 49.55(15) 3_446 3_446 ?
O4 Ce1 O1 106.69(16) . 3_446 ?
O8 Ce1 O1 138.13(16) 4_535 3_446 ?
O5 Ce1 O1 69.18(14) . 3_446 ?
O7 Ce1 O1 154.17(14) 4_535 3_446 ?
O1 Ce1 C15 105.14(17) 5_546 . ?
O7 Ce1 C15 92.81(17) 6_546 . ?
O5 Ce1 C15 173.66(17) 7 . ?
O2 Ce1 C15 87.2(2) 3_446 . ?
O4 Ce1 C15 25.08(16) . . ?
O8 Ce1 C15 81.38(19) 4_535 . ?
O5 Ce1 C15 25.83(15) . . ?
O7 Ce1 C15 116.97(16) 4_535 . ?
O1 Ce1 C15 88.55(17) 3_446 . ?
O1 Ce1 C23 86.54(18) 5_546 4_535 ?
O7 Ce1 C23 91.40(19) 6_546 4_535 ?
O5 Ce1 C23 85.84(19) 7 4_535 ?
O2 Ce1 C23 154.17(19) 3_446 4_535 ?
O4 Ce1 C23 90.4(2) . 4_535 ?
O8 Ce1 C23 24.91(18) 4_535 4_535 ?
O5 Ce1 C23 110.21(18) . 4_535 ?
O7 Ce1 C23 25.44(16) 4_535 4_535 ?
O1 Ce1 C23 153.83(18) 3_446 4_535 ?
C15 Ce1 C23 100.5(2) . 4_535 ?
O1 Ce1 C1 90.10(18) 5_546 3_446 ?
O7 Ce1 C1 88.60(17) 6_546 3_446 ?
O5 Ce1 C1 83.27(18) 7 3_446 ?
O2 Ce1 C1 24.48(17) 3_446 3_446 ?
O4 Ce1 C1 99.39(18) . 3_446 ?
O8 Ce1 C1 162.51(18) 4_535 3_446 ?
O5 Ce1 C1 79.94(18) . 3_446 ?
O7 Ce1 C1 145.91(17) 4_535 3_446 ?
O1 Ce1 C1 25.35(15) 3_446 3_446 ?
C15 Ce1 C1 90.39(19) . 3_446 ?
C23 Ce1 C1 169.1(2) 4_535 3_446 ?
C15 O5 Ce1 163.1(4) . 7_565 ?
C15 O5 Ce1 92.2(4) . . ?
Ce1 O5 Ce1 99.55(15) 7_565 . ?
C23 O7 Ce1 161.5(5) . 6_676 ?
C23 O7 Ce1 92.7(4) . 4_575 ?
Ce1 O7 Ce1 99.44(15) 6_676 4_575 ?
C1 O1 Ce1 142.2(4) . 5_546 ?
C1 O1 Ce1 90.8(4) . 3_546 ?
Ce1 O1 Ce1 97.99(15) 5_546 3_546 ?
C15 O4 Ce1 97.7(4) . . ?
C23 O8 Ce1 97.0(4) . 4_575 ?
C1 O2 Ce1 99.7(4) . 3_546 ?
C4 O3 C8 118.2(6) . . ?
C16 O6 C6 123.3(9) . . ?
C16A O6 C6 121.9(11) . . ?
C3 C2 C7 120.7(6) . . ?
C3 C2 C1 121.1(6) . . ?
C7 C2 C1 118.2(6) . . ?
O3 C4 C5 114.9(7) . . ?
O3 C4 C3 124.7(7) . . ?
C5 C4 C3 120.4(7) . . ?
C2 C3 C4 119.5(6) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
O4 C15 O5 119.1(6) . . ?
O4 C15 C12 120.1(6) . . ?
O5 C15 C12 120.8(6) . . ?
O4 C15 Ce1 57.3(4) . . ?
O5 C15 Ce1 61.9(3) . . ?
C12 C15 Ce1 176.3(5) . . ?
C6 C7 C2 118.6(7) . . ?
C6 C7 H7 120.7 . . ?
C2 C7 H7 120.7 . . ?
C10 C9 C14 119.2(8) . . ?
C10 C9 C8 122.0(8) . . ?
C14 C9 C8 118.8(8) . . ?
C14 C13 C12 120.2(7) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C9 C10 C11 121.5(8) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
O2 C1 O1 118.6(6) . . ?
O2 C1 C2 120.6(6) . . ?
O1 C1 C2 120.8(6) . . ?
O2 C1 Ce1 55.8(4) . 3_546 ?
O1 C1 Ce1 63.8(3) . 3_546 ?
C2 C1 Ce1 169.2(5) . 3_546 ?
C11 C12 C13 119.5(7) . . ?
C11 C12 C15 121.3(7) . . ?
C13 C12 C15 119.2(7) . . ?
C6 C5 C4 119.7(7) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
O6 C6 C7 120.6(7) . . ?
O6 C6 C5 118.3(7) . . ?
C7 C6 C5 121.0(7) . . ?
C13 C14 C9 119.9(8) . . ?
C13 C14 H14 120.1 . . ?
C9 C14 H14 120.1 . . ?
C10 C11 C12 119.8(7) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
O3 C8 C9 108.7(7) . . ?
O3 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O6 C16 C17 112.2(13) . . ?
O6 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
O6 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C18 C17 C22 120.0 . . ?
C18 C17 C16 118.6(9) . . ?
C22 C17 C16 121.1(10) . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 C23 121.7(7) . . ?
C21 C20 C23 118.3(7) . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C17 120.0 . . ?
C21 C22 H22 120.0 . . ?
C17 C22 H22 120.0 . . ?
O6 C16A C17A 107.9(17) . . ?
O6 C16A H16C 110.1 . . ?
C17A C16A H16C 110.1 . . ?
O6 C16A H16D 110.1 . . ?
C17A C16A H16D 110.1 . . ?
H16C C16A H16D 108.4 . . ?
C18A C17A C22A 120.0 . . ?
C18A C17A C16A 124.2(17) . . ?
C22A C17A C16A 115.7(17) . . ?
C19A C18A C17A 120.0 . . ?
C19A C18A H18A 120.0 . . ?
C17A C18A H18A 120.0 . . ?
C18A C19A C20A 120.0 . . ?
C18A C19A H19A 120.0 . . ?
C20A C19A H19A 120.0 . . ?
C19A C20A C21A 120.0 . . ?
C19A C20A C23 118.4(10) . . ?
C21A C20A C23 120.8(10) . . ?
C20A C21A C22A 120.0 . . ?
C20A C21A H21A 120.0 . . ?
C22A C21A H21A 120.0 . . ?
C21A C22A C17A 120.0 . . ?
C21A C22A H22A 120.0 . . ?
C17A C22A H22A 120.0 . . ?
O8 C23 O7 119.6(7) . . ?
O8 C23 C20 116.7(7) . . ?
O7 C23 C20 123.1(7) . . ?
O8 C23 C20A 125.4(9) . . ?
O7 C23 C20A 113.0(8) . . ?
O8 C23 Ce1 58.0(4) . 4_575 ?
O7 C23 Ce1 61.8(4) . 4_575 ?
C20 C23 Ce1 165.7(6) . 4_575 ?

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
C8 O3 C4 C5 171.0(8) . . . . ?
C8 O3 C4 C3 -9.0(13) . . . . ?
C7 C2 C3 C4 0.4(11) . . . . ?
C1 C2 C3 C4 -179.6(7) . . . . ?
O3 C4 C3 C2 178.8(8) . . . . ?
C5 C4 C3 C2 -1.1(12) . . . . ?
Ce1 O4 C15 O5 2.8(7) . . . . ?
Ce1 O4 C15 C12 -177.0(5) . . . . ?
Ce1 O5 C15 O4 131.9(13) 7_565 . . . ?
Ce1 O5 C15 O4 -2.7(7) . . . . ?
Ce1 O5 C15 C12 -48.3(19) 7_565 . . . ?
Ce1 O5 C15 C12 177.1(6) . . . . ?
Ce1 O5 C15 Ce1 134.6(16) 7_565 . . . ?
C3 C2 C7 C6 1.3(12) . . . . ?
C1 C2 C7 C6 -178.8(7) . . . . ?
C14 C9 C10 C11 -2.3(13) . . . . ?
C8 C9 C10 C11 174.8(8) . . . . ?
Ce1 O2 C1 O1 -12.1(8) 3_546 . . . ?
Ce1 O2 C1 C2 167.9(6) 3_546 . . . ?
Ce1 O1 C1 O2 -93.0(9) 5_546 . . . ?
Ce1 O1 C1 O2 11.2(7) 3_546 . . . ?
Ce1 O1 C1 C2 87.0(9) 5_546 . . . ?
Ce1 O1 C1 C2 -168.9(6) 3_546 . . . ?
Ce1 O1 C1 Ce1 -104.2(6) 5_546 . . 3_546 ?
C3 C2 C1 O2 172.2(8) . . . . ?
C7 C2 C1 O2 -7.8(11) . . . . ?
C3 C2 C1 O1 -7.8(11) . . . . ?
C7 C2 C1 O1 172.3(7) . . . . ?
C3 C2 C1 Ce1 -121(2) . . . 3_546 ?
C7 C2 C1 Ce1 60(3) . . . 3_546 ?
C14 C13 C12 C11 -3.3(12) . . . . ?
C14 C13 C12 C15 176.1(7) . . . . ?
O4 C15 C12 C11 2.4(11) . . . . ?
O5 C15 C12 C11 -177.4(7) . . . . ?
O4 C15 C12 C13 -176.9(7) . . . . ?
O5 C15 C12 C13 3.3(10) . . . . ?
O3 C4 C5 C6 -179.7(8) . . . . ?
C3 C4 C5 C6 0.2(13) . . . . ?
C16 O6 C6 C7 -19.0(19) . . . . ?
C16A O6 C6 C7 -157.5(19) . . . . ?
C16 O6 C6 C5 161.9(16) . . . . ?
C16A O6 C6 C5 23(2) . . . . ?
C2 C7 C6 O6 178.7(7) . . . . ?
C2 C7 C6 C5 -2.2(13) . . . . ?
C4 C5 C6 O6 -179.4(8) . . . . ?
C4 C5 C6 C7 1.5(14) . . . . ?
C12 C13 C14 C9 1.1(13) . . . . ?
C10 C9 C14 C13 1.6(13) . . . . ?
C8 C9 C14 C13 -175.5(8) . . . . ?
C9 C10 C11 C12 0.1(12) . . . . ?
C13 C12 C11 C10 2.7(11) . . . . ?
C15 C12 C11 C10 -176.7(7) . . . . ?
C4 O3 C8 C9 171.3(7) . . . . ?
C10 C9 C8 O3 132.4(9) . . . . ?
C14 C9 C8 O3 -50.5(11) . . . . ?
C6 O6 C16 C17 -177.7(12) . . . . ?
O6 C16 C17 C18 161.0(13) . . . . ?
O6 C16 C17 C22 -24(2) . . . . ?
C22 C17 C18 C19 0.0 . . . . ?
C16 C17 C18 C19 174.7(16) . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C18 C19 C20 C23 -178.3(10) . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C23 C20 C21 C22 178.4(10) . . . . ?
C20 C21 C22 C17 0.0 . . . . ?
C18 C17 C22 C21 0.0 . . . . ?
C16 C17 C22 C21 -174.5(16) . . . . ?
C6 O6 C16A C17A 176.8(14) . . . . ?
O6 C16A C17A C18A -66(3) . . . . ?
O6 C16A C17A C22A 117(2) . . . . ?
C22A C17A C18A C19A 0.0 . . . . ?
C16A C17A C18A C19A -177.1(18) . . . . ?
C17A C18A C19A C20A 0.0 . . . . ?
C18A C19A C20A C21A 0.0 . . . . ?
C18A C19A C20A C23 -169.8(14) . . . . ?
C19A C20A C21A C22A 0.0 . . . . ?
C23 C20A C21A C22A 169.5(14) . . . . ?
C20A C21A C22A C17A 0.0 . . . . ?
C18A C17A C22A C21A 0.0 . . . . ?
C16A C17A C22A C21A 177.4(17) . . . . ?
Ce1 O8 C23 O7 -6.4(8) 4_575 . . . ?
Ce1 O8 C23 C20 164.8(7) 4_575 . . . ?
Ce1 O8 C23 C20A -168.9(10) 4_575 . . . ?
Ce1 O7 C23 O8 137.4(12) 6_676 . . . ?
Ce1 O7 C23 O8 6.1(8) 4_575 . . . ?
Ce1 O7 C23 C20 -33(2) 6_676 . . . ?
Ce1 O7 C23 C20 -164.4(8) 4_575 . . . ?
Ce1 O7 C23 C20A -58.0(18) 6_676 . . . ?
Ce1 O7 C23 C20A 170.8(8) 4_575 . . . ?
Ce1 O7 C23 Ce1 131.2(15) 6_676 . . 4_575 ?
C19 C20 C23 O8 -15.2(11) . . . . ?
C21 C20 C23 O8 166.4(7) . . . . ?
C19 C20 C23 O7 155.6(7) . . . . ?
C21 C20 C23 O7 -22.8(12) . . . . ?
C19 C20 C23 Ce1 49(3) . . . 4_575 ?
C21 C20 C23 Ce1 -129(2) . . . 4_575 ?
C19A C20A C23 O8 -32.0(15) . . . . ?
C21A C20A C23 O8 158.3(10) . . . . ?
C19A C20A C23 O7 164.4(9) . . . . ?
C21A C20A C23 O7 -5.3(14) . . . . ?

_refine_diff_density_max         0.737
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.193



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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1544751'
_audit_update_record             
;
2017-08-21 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form 
_vrf_CHEMW03_1                   
; 
PROBLEM: ALERT: The ratio of given/expected molecular weight as 
RESPONSE:  The difference results from the lattice water 
molecules which were removed by squeeze, 
however, they were included to final formula to calculate 
actual cell metric values. 
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H15 La O8 , 4.5(H2O)'
_chemical_formula_sum            'C23 H24 La O12.50'
_chemical_formula_weight         639.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   22.645(3)
_cell_length_b                   7.6075(10)
_cell_length_c                   29.260(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5040.7(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       slice
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             2192
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.735
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35353
_diffrn_reflns_av_unetI/netI     0.1187
_diffrn_reflns_av_R_equivalents  0.1616
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.392
_diffrn_reflns_theta_max         28.363
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6305
_reflns_number_gt                3290
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0640P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6305
_refine_ls_number_parameters     329
_refine_ls_number_restraints     315
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1452
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.948
_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
La1 La 0.27023(2) 0.42498(4) -0.08524(2) 0.02256(12) Uani 1 1 d . . . . .
O1 O 0.2528(3) 0.3830(9) -0.0009(2) 0.070(2) Uani 1 1 d . . . . .
C1 C 0.2139(3) 0.2675(9) -0.0026(2) 0.0301(17) Uani 1 1 d . . . . .
O2 O 0.2031(2) 0.1898(6) -0.04021(16) 0.0270(11) Uani 1 1 d . . . . .
C2 C 0.1794(3) 0.2213(9) 0.0391(2) 0.0276(16) Uani 1 1 d . . . . .
O3 O 0.1614(3) 0.3908(9) 0.1553(2) 0.073(2) Uani 1 1 d . . . . .
C3 C 0.1872(4) 0.3269(11) 0.0779(3) 0.040(2) Uani 1 1 d . . . . .
H3 H 0.213736 0.420167 0.077385 0.048 Uiso 1 1 calc R U . . .
O4 O 0.1844(4) 1.0320(7) 0.3355(2) 0.065(2) Uani 1 1 d . . . . .
C4 C 0.1550(4) 0.2911(12) 0.1172(3) 0.048(2) Uani 1 1 d . . . . .
O5 O 0.2134(2) 0.7867(6) 0.36696(17) 0.0354(13) Uani 1 1 d . . . . .
C5 C 0.1176(4) 0.1496(11) 0.1183(3) 0.044(2) Uani 1 1 d . . . . .
H5 H 0.096042 0.125676 0.144650 0.053 Uiso 1 1 calc R U . . .
O6 O 0.0740(3) -0.0974(8) 0.0850(2) 0.0630(19) Uani 1 1 d . . . . .
C6 C 0.1119(4) 0.0415(10) 0.0802(3) 0.041(2) Uani 1 1 d . . . . .
O7 O -0.1244(2) -0.8409(7) 0.0682(2) 0.0464(16) Uani 1 1 d . . . . .
C7 C 0.1424(3) 0.0817(10) 0.0400(2) 0.0327(16) Uani 1 1 d . . . . .
H7 H 0.137261 0.012900 0.014011 0.039 Uiso 1 1 calc R U . . .
O8 O -0.1794(2) -0.6138(6) 0.0849(2) 0.0354(12) Uani 1 1 d . . . . .
C8 C 0.1854(11) 0.553(2) 0.1555(5) 0.085(7) Uani 0.560(10) 1 d . . P A 1
H8A H 0.163451 0.628041 0.134854 0.085 Uiso 0.560(10) 1 calc R U P A 1
H8B H 0.225798 0.546073 0.144663 0.085 Uiso 0.560(10) 1 calc R U P A 1
C9 C 0.1845(7) 0.6280(13) 0.2014(3) 0.064(6) Uani 0.560(10) 1 d G . P A 1
C10 C 0.1841(7) 0.5263(9) 0.2409(3) 0.069(7) Uani 0.560(10) 1 d G . P A 1
H10 H 0.182248 0.404478 0.238790 0.069 Uiso 0.560(10) 1 calc R U P A 1
C11 C 0.1865(7) 0.6068(12) 0.2835(3) 0.048(5) Uani 0.560(10) 1 d G . P A 1
H11 H 0.186269 0.538825 0.309902 0.048 Uiso 0.560(10) 1 calc R U P A 1
C12 C 0.1893(7) 0.7890(13) 0.2866(3) 0.042(5) Uani 0.560(10) 1 d G . P A 1
C13 C 0.1897(8) 0.8906(10) 0.2471(4) 0.086(9) Uani 0.560(10) 1 d G . P A 1
H13 H 0.191572 1.012444 0.249239 0.086 Uiso 0.560(10) 1 calc R U P A 1
C14 C 0.1873(7) 0.8101(12) 0.2045(3) 0.083(8) Uani 0.560(10) 1 d G . P A 1
H14 H 0.187552 0.878101 0.178126 0.083 Uiso 0.560(10) 1 calc R U P A 1
C8A C 0.1187(13) 0.392(4) 0.1880(8) 0.100(11) Uani 0.440(10) 1 d . . P A 2
H8AA H 0.114920 0.275532 0.201385 0.100 Uiso 0.440(10) 1 calc R U P A 2
H8AB H 0.081037 0.423913 0.174623 0.100 Uiso 0.440(10) 1 calc R U P A 2
C9A C 0.1363(8) 0.525(2) 0.2247(5) 0.076(8) Uani 0.440(10) 1 d G . P A 2
C10A C 0.1442(9) 0.4567(17) 0.2683(6) 0.079(8) Uani 0.440(10) 1 d G . P A 2
H10A H 0.138464 0.337361 0.273592 0.079 Uiso 0.440(10) 1 calc R U P A 2
C11A C 0.1607(9) 0.567(2) 0.3040(4) 0.072(8) Uani 0.440(10) 1 d G . P A 2
H11A H 0.166014 0.521058 0.333182 0.072 Uiso 0.440(10) 1 calc R U P A 2
C12A C 0.1693(9) 0.745(2) 0.2961(5) 0.048(6) Uani 0.440(10) 1 d G . P A 2
C13A C 0.1613(10) 0.8134(19) 0.2524(6) 0.089(10) Uani 0.440(10) 1 d G . P A 2
H13A H 0.167060 0.932673 0.247121 0.089 Uiso 0.440(10) 1 calc R U P A 2
C14A C 0.1448(9) 0.703(2) 0.2167(4) 0.113(13) Uani 0.440(10) 1 d G . P A 2
H14A H 0.139510 0.748978 0.187529 0.113 Uiso 0.440(10) 1 calc R U P A 2
C15 C 0.1939(4) 0.8687(11) 0.3331(3) 0.045(2) Uani 1 1 d . . . . .
C16 C 0.0711(4) -0.2244(12) 0.0503(3) 0.061(3) Uani 1 1 d . . . . .
H16A H 0.107633 -0.291045 0.049337 0.073 Uiso 1 1 calc R U . . .
H16B H 0.065777 -0.167657 0.020852 0.073 Uiso 1 1 calc R U . . .
C17 C 0.0202(4) -0.3447(11) 0.0599(3) 0.045(2) Uani 1 1 d . . . . .
C18 C -0.0344(4) -0.2754(12) 0.0710(3) 0.058(3) Uani 1 1 d . . . . .
H18 H -0.038507 -0.154740 0.075028 0.070 Uiso 1 1 calc R U . . .
C19 C -0.0829(4) -0.3837(10) 0.0762(3) 0.049(2) Uani 1 1 d . . . . .
H19 H -0.119717 -0.335932 0.082908 0.059 Uiso 1 1 calc R U . . .
C20 C -0.0765(3) -0.5635(10) 0.0713(3) 0.0333(17) Uani 1 1 d . . . . .
C21 C -0.0211(3) -0.6353(10) 0.0622(3) 0.040(2) Uani 1 1 d . . . . .
H21 H -0.015922 -0.756284 0.060256 0.048 Uiso 1 1 calc R U . . .
C22 C 0.0257(4) -0.5221(11) 0.0563(3) 0.050(2) Uani 1 1 d . . . . .
H22 H 0.062677 -0.568981 0.049600 0.060 Uiso 1 1 calc R U . . .
C23 C -0.1295(3) -0.6790(9) 0.0750(3) 0.0332(19) 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
La1 O2 2.482(4) 7_665 ?
La1 O5 2.491(5) 8_565 ?
La1 O8 2.509(5) 5 ?
La1 O1 2.520(6) . ?
La1 O7 2.520(5) 3_545 ?
La1 O4 2.558(6) 2_564 ?
La1 O5 2.628(5) 2_564 ?
La1 O8 2.628(4) 3_545 ?
La1 O2 2.692(5) . ?
La1 C23 2.958(7) 3_545 ?
La1 C15 2.973(8) 2_564 ?
La1 C1 2.986(7) . ?
O1 C1 1.246(9) . ?
C1 O2 1.273(8) . ?
C1 C2 1.490(10) . ?
C2 C7 1.353(9) . ?
C2 C3 1.403(9) . ?
O3 C8 1.344(17) . ?
O3 C4 1.357(9) . ?
O3 C8A 1.36(2) . ?
C3 C4 1.387(10) . ?
C3 H3 0.9300 . ?
O4 C15 1.262(9) . ?
C4 C5 1.369(11) . ?
O5 C15 1.252(9) . ?
C5 C6 1.391(10) . ?
C5 H5 0.9300 . ?
O6 C6 1.369(8) . ?
O6 C16 1.403(10) . ?
C6 C7 1.399(10) . ?
O7 C23 1.253(8) . ?
C7 H7 0.9300 . ?
O8 C23 1.268(8) . ?
C8 C9 1.461(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 H10 0.9300 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 C15 1.491(10) . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C8A C9A 1.53(2) . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C9A C10A 1.3900 . ?
C9A C14A 1.3900 . ?
C10A C11A 1.3900 . ?
C10A H10A 0.9300 . ?
C11A C12A 1.3900 . ?
C11A H11A 0.9300 . ?
C12A C13A 1.3900 . ?
C12A C15 1.538(13) . ?
C13A C14A 1.3900 . ?
C13A H13A 0.9300 . ?
C14A H14A 0.9300 . ?
C16 C17 1.499(11) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C22 1.360(11) . ?
C17 C18 1.383(12) . ?
C18 C19 1.382(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.383(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.394(10) . ?
C20 C23 1.490(10) . ?
C21 C22 1.377(10) . ?
C21 H21 0.9300 . ?
C22 H22 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
O2 La1 O5 161.52(16) 7_665 8_565 ?
O2 La1 O8 74.49(16) 7_665 5 ?
O5 La1 O8 87.05(16) 8_565 5 ?
O2 La1 O1 67.72(18) 7_665 . ?
O5 La1 O1 112.77(17) 8_565 . ?
O8 La1 O1 86.6(2) 5 . ?
O2 La1 O7 82.59(16) 7_665 3_545 ?
O5 La1 O7 115.85(17) 8_565 3_545 ?
O8 La1 O7 157.06(16) 5 3_545 ?
O1 La1 O7 85.6(2) . 3_545 ?
O2 La1 O4 106.25(18) 7_665 2_564 ?
O5 La1 O4 77.4(2) 8_565 2_564 ?
O8 La1 O4 105.0(2) 5 2_564 ?
O1 La1 O4 165.3(2) . 2_564 ?
O7 La1 O4 80.3(2) 3_545 2_564 ?
O2 La1 O5 64.58(15) 7_665 2_564 ?
O5 La1 O5 108.28(18) 8_565 2_564 ?
O8 La1 O5 68.88(16) 5 2_564 ?
O1 La1 O5 130.48(19) . 2_564 ?
O7 La1 O5 100.58(17) 3_545 2_564 ?
O4 La1 O5 49.74(16) 2_564 2_564 ?
O2 La1 O8 128.61(16) 7_665 3_545 ?
O5 La1 O8 69.13(16) 8_565 3_545 ?
O8 La1 O8 150.65(13) 5 3_545 ?
O1 La1 O8 87.2(2) . 3_545 ?
O7 La1 O8 50.19(15) 3_545 3_545 ?
O4 La1 O8 86.80(18) 2_564 3_545 ?
O5 La1 O8 133.83(16) 2_564 3_545 ?
O2 La1 O2 114.64(18) 7_665 . ?
O5 La1 O2 63.48(15) 8_565 . ?
O8 La1 O2 85.18(15) 5 . ?
O1 La1 O2 49.30(16) . . ?
O7 La1 O2 105.60(17) 3_545 . ?
O4 La1 O2 139.09(17) 2_564 . ?
O5 La1 O2 153.50(16) 2_564 . ?
O8 La1 O2 69.18(15) 3_545 . ?
O2 La1 C23 105.86(18) 7_665 3_545 ?
O5 La1 C23 92.54(19) 8_565 3_545 ?
O8 La1 C23 172.46(18) 5 3_545 ?
O1 La1 C23 86.6(2) . 3_545 ?
O7 La1 C23 24.83(18) 3_545 3_545 ?
O4 La1 C23 82.2(2) 2_564 3_545 ?
O5 La1 C23 118.28(18) 2_564 3_545 ?
O8 La1 C23 25.37(16) 3_545 3_545 ?
O2 La1 C23 87.90(17) . 3_545 ?
O2 La1 C15 86.1(2) 7_665 2_564 ?
O5 La1 C15 91.8(2) 8_565 2_564 ?
O8 La1 C15 85.7(2) 5 2_564 ?
O1 La1 C15 153.8(2) . 2_564 ?
O7 La1 C15 92.0(2) 3_545 2_564 ?
O4 La1 C15 24.96(19) 2_564 2_564 ?
O5 La1 C15 24.87(18) 2_564 2_564 ?
O8 La1 C15 111.1(2) 3_545 2_564 ?
O2 La1 C15 154.0(2) . 2_564 ?
C23 La1 C15 101.9(2) 3_545 2_564 ?
O2 La1 C1 89.97(18) 7_665 . ?
O5 La1 C1 88.54(18) 8_565 . ?
O8 La1 C1 82.90(19) 5 . ?
O1 La1 C1 24.32(18) . . ?
O7 La1 C1 98.2(2) 3_545 . ?
O4 La1 C1 163.27(19) 2_564 . ?
O5 La1 C1 145.73(18) 2_564 . ?
O8 La1 C1 79.71(18) 3_545 . ?
O2 La1 C1 25.24(16) . . ?
C23 La1 C1 89.6(2) 3_545 . ?
C15 La1 C1 168.5(2) 2_564 . ?
C1 O1 La1 99.3(5) . . ?
O1 C1 O2 119.8(7) . . ?
O1 C1 C2 120.3(7) . . ?
O2 C1 C2 119.9(6) . . ?
O1 C1 La1 56.4(4) . . ?
O2 C1 La1 64.4(4) . . ?
C2 C1 La1 169.0(5) . . ?
C1 O2 La1 142.2(5) . 7_655 ?
C1 O2 La1 90.4(4) . . ?
La1 O2 La1 98.19(16) 7_655 . ?
C7 C2 C3 120.8(7) . . ?
C7 C2 C1 121.7(7) . . ?
C3 C2 C1 117.5(6) . . ?
C8 O3 C4 123.9(9) . . ?
C4 O3 C8A 120.2(12) . . ?
C4 C3 C2 119.5(7) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C15 O4 La1 96.3(5) . 2_565 ?
O3 C4 C5 119.0(7) . . ?
O3 C4 C3 120.9(8) . . ?
C5 C4 C3 120.0(7) . . ?
C15 O5 La1 161.6(6) . 8_566 ?
C15 O5 La1 93.2(5) . 2_565 ?
La1 O5 La1 99.67(16) 8_566 2_565 ?
C4 C5 C6 120.1(7) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C6 O6 C16 119.1(6) . . ?
O6 C6 C5 115.7(7) . . ?
O6 C6 C7 124.3(7) . . ?
C5 C6 C7 119.9(7) . . ?
C23 O7 La1 97.5(5) . 3_445 ?
C2 C7 C6 119.6(7) . . ?
C2 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C23 O8 La1 162.9(5) . 5 ?
C23 O8 La1 92.0(4) . 3_445 ?
La1 O8 La1 99.20(15) 5 3_445 ?
O3 C8 C9 111.0(13) . . ?
O3 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
O3 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 123.1(10) . . ?
C14 C9 C8 116.8(10) . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 C15 122.0(7) . . ?
C11 C12 C15 117.9(7) . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
O3 C8A C9A 108.1(18) . . ?
O3 C8A H8AA 110.1 . . ?
C9A C8A H8AA 110.1 . . ?
O3 C8A H8AB 110.1 . . ?
C9A C8A H8AB 110.1 . . ?
H8AA C8A H8AB 108.4 . . ?
C10A C9A C14A 120.0 . . ?
C10A C9A C8A 115.5(16) . . ?
C14A C9A C8A 124.5(16) . . ?
C9A C10A C11A 120.0 . . ?
C9A C10A H10A 120.0 . . ?
C11A C10A H10A 120.0 . . ?
C12A C11A C10A 120.0 . . ?
C12A C11A H11A 120.0 . . ?
C10A C11A H11A 120.0 . . ?
C11A C12A C13A 120.0 . . ?
C11A C12A C15 122.0(11) . . ?
C13A C12A C15 117.7(11) . . ?
C14A C13A C12A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C12A C13A H13A 120.0 . . ?
C13A C14A C9A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C9A C14A H14A 120.0 . . ?
O5 C15 O4 120.3(8) . . ?
O5 C15 C12 122.9(8) . . ?
O4 C15 C12 116.1(8) . . ?
O5 C15 C12A 112.4(9) . . ?
O4 C15 C12A 125.4(10) . . ?
O5 C15 La1 61.9(4) . 2_565 ?
O4 C15 La1 58.8(4) . 2_565 ?
C12 C15 La1 165.0(8) . 2_565 ?
O6 C16 C17 108.6(7) . . ?
O6 C16 H16A 110.0 . . ?
C17 C16 H16A 110.0 . . ?
O6 C16 H16B 110.0 . . ?
C17 C16 H16B 110.0 . . ?
H16A C16 H16B 108.3 . . ?
C22 C17 C18 118.6(8) . . ?
C22 C17 C16 121.4(9) . . ?
C18 C17 C16 120.0(8) . . ?
C19 C18 C17 120.6(8) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 119.7(8) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C19 C20 C21 120.1(7) . . ?
C19 C20 C23 119.4(7) . . ?
C21 C20 C23 120.5(7) . . ?
C22 C21 C20 118.2(7) . . ?
C22 C21 H21 120.9 . . ?
C20 C21 H21 120.9 . . ?
C17 C22 C21 122.7(8) . . ?
C17 C22 H22 118.7 . . ?
C21 C22 H22 118.7 . . ?
O7 C23 O8 120.2(7) . . ?
O7 C23 C20 119.6(7) . . ?
O8 C23 C20 120.2(6) . . ?
O7 C23 La1 57.6(4) . 3_445 ?
O8 C23 La1 62.6(4) . 3_445 ?
C20 C23 La1 176.4(5) . 3_445 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O1 C1 O2 11.7(9) . . . . ?
La1 O1 C1 C2 -167.6(6) . . . . ?
O1 C1 O2 La1 93.2(10) . . . 7_655 ?
C2 C1 O2 La1 -87.5(9) . . . 7_655 ?
La1 C1 O2 La1 104.0(7) . . . 7_655 ?
O1 C1 O2 La1 -10.8(8) . . . . ?
C2 C1 O2 La1 168.5(6) . . . . ?
O1 C1 C2 C7 -171.3(8) . . . . ?
O2 C1 C2 C7 9.4(11) . . . . ?
La1 C1 C2 C7 119(3) . . . . ?
O1 C1 C2 C3 7.9(12) . . . . ?
O2 C1 C2 C3 -171.4(7) . . . . ?
La1 C1 C2 C3 -61(3) . . . . ?
C7 C2 C3 C4 -2.3(13) . . . . ?
C1 C2 C3 C4 178.5(8) . . . . ?
C8 O3 C4 C5 -164.0(16) . . . . ?
C8A O3 C4 C5 -22(2) . . . . ?
C8 O3 C4 C3 18.4(19) . . . . ?
C8A O3 C4 C3 159.9(18) . . . . ?
C2 C3 C4 O3 -179.9(8) . . . . ?
C2 C3 C4 C5 2.5(14) . . . . ?
O3 C4 C5 C6 -177.6(9) . . . . ?
C3 C4 C5 C6 0.0(15) . . . . ?
C16 O6 C6 C5 -172.3(9) . . . . ?
C16 O6 C6 C7 9.9(14) . . . . ?
C4 C5 C6 O6 179.4(8) . . . . ?
C4 C5 C6 C7 -2.7(14) . . . . ?
C3 C2 C7 C6 -0.5(12) . . . . ?
C1 C2 C7 C6 178.7(7) . . . . ?
O6 C6 C7 C2 -179.3(8) . . . . ?
C5 C6 C7 C2 3.0(13) . . . . ?
C4 O3 C8 C9 178.3(12) . . . . ?
O3 C8 C9 C10 26(2) . . . . ?
O3 C8 C9 C14 -157.4(13) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C8 C9 C10 C11 176.5(17) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C15 -178.0(13) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C15 C12 C13 C14 177.9(13) . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
C8 C9 C14 C13 -176.7(16) . . . . ?
C4 O3 C8A C9A -176.0(14) . . . . ?
O3 C8A C9A C10A -119.2(19) . . . . ?
O3 C8A C9A C14A 60(3) . . . . ?
C14A C9A C10A C11A 0.0 . . . . ?
C8A C9A C10A C11A 179.4(19) . . . . ?
C9A C10A C11A C12A 0.0 . . . . ?
C10A C11A C12A C13A 0.0 . . . . ?
C10A C11A C12A C15 -173.4(16) . . . . ?
C11A C12A C13A C14A 0.0 . . . . ?
C15 C12A C13A C14A 173.6(16) . . . . ?
C12A C13A C14A C9A 0.0 . . . . ?
C10A C9A C14A C13A 0.0 . . . . ?
C8A C9A C14A C13A -179(2) . . . . ?
La1 O5 C15 O4 -141.4(13) 8_566 . . . ?
La1 O5 C15 O4 -6.9(10) 2_565 . . . ?
La1 O5 C15 C12 29(2) 8_566 . . . ?
La1 O5 C15 C12 163.5(10) 2_565 . . . ?
La1 O5 C15 C12A 53(2) 8_566 . . . ?
La1 O5 C15 C12A -172.2(10) 2_565 . . . ?
La1 O5 C15 La1 -134.6(17) 8_566 . . 2_565 ?
La1 O4 C15 O5 7.1(10) 2_565 . . . ?
La1 O4 C15 C12 -164.0(9) 2_565 . . . ?
La1 O4 C15 C12A 170.4(12) 2_565 . . . ?
C13 C12 C15 O5 -155.0(9) . . . . ?
C11 C12 C15 O5 23.0(15) . . . . ?
C13 C12 C15 O4 15.8(14) . . . . ?
C11 C12 C15 O4 -166.2(9) . . . . ?
C13 C12 C15 La1 -50(3) . . . 2_565 ?
C11 C12 C15 La1 128(2) . . . 2_565 ?
C11A C12A C15 O5 10.7(16) . . . . ?
C13A C12A C15 O5 -162.8(10) . . . . ?
C11A C12A C15 O4 -153.8(11) . . . . ?
C13A C12A C15 O4 32.7(18) . . . . ?
C6 O6 C16 C17 -171.0(8) . . . . ?
O6 C16 C17 C22 -134.6(10) . . . . ?
O6 C16 C17 C18 47.8(12) . . . . ?
C22 C17 C18 C19 -3.1(15) . . . . ?
C16 C17 C18 C19 174.5(9) . . . . ?
C17 C18 C19 C20 1.6(15) . . . . ?
C18 C19 C20 C21 1.6(13) . . . . ?
C18 C19 C20 C23 -177.6(8) . . . . ?
C19 C20 C21 C22 -3.0(13) . . . . ?
C23 C20 C21 C22 176.1(8) . . . . ?
C18 C17 C22 C21 1.6(15) . . . . ?
C16 C17 C22 C21 -176.0(9) . . . . ?
C20 C21 C22 C17 1.4(14) . . . . ?
La1 O7 C23 O8 -2.8(9) 3_445 . . . ?
La1 O7 C23 C20 177.3(6) 3_445 . . . ?
La1 O8 C23 O7 -128.4(14) 5 . . . ?
La1 O8 C23 O7 2.7(8) 3_445 . . . ?
La1 O8 C23 C20 51(2) 5 . . . ?
La1 O8 C23 C20 -177.5(7) 3_445 . . . ?
La1 O8 C23 La1 -131.1(17) 5 . . 3_445 ?
C19 C20 C23 O7 176.3(8) . . . . ?
C21 C20 C23 O7 -2.8(12) . . . . ?
C19 C20 C23 O8 -3.6(12) . . . . ?
C21 C20 C23 O8 177.3(8) . . . . ?

_refine_diff_density_max         0.753
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.188



####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1473241'
_audit_update_record             
;
2017-08-21 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form 
_vrf_PLAT043_5                   
; 
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      14.12 Check 
RESPONSE: The difference results from the hydrogens of lattice water 
molecules which were not located and included to refinement, 
however, they were included to final formula to calculate 
actual cell metric values.
;
_vrf_PLAT306_5                   
; 
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check 
RESPONSE: Due to disorder on lattice O-atom, H-atoms can not be fixed. 
;
_vrf_PLAT430_5                   
; 
PROBLEM: Short Inter D...A Contact  O3W    ..  O4W     ..       2.59 Ang. 
RESPONSE: This is H bond contact to the O atom from water molecule which may be slightly 
shortened due to disorder of the solvent. 
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C23 H26 O10 Tm,3.5(H20))'
_chemical_formula_sum            'C46 H52 O27 Tm2'
_chemical_formula_weight         1374.74

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'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.544(5)
_cell_length_b                   23.806(5)
_cell_length_c                   8.457(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.523(5)
_cell_angle_gamma                90
_cell_volume                     2639.7(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      7.5
_cell_measurement_theta_max      15

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.427
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8370
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.711
_diffrn_reflns_theta_max         26.180
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2711
_reflns_number_gt                2372
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0401P)²+11.8398P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         2711
_refine_ls_number_parameters     176
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_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
Tm1 Tm 0.37739(3) 0.500000 0.16495(4) 0.02464(12) Uani 1 2 d S T P . .
O4A O 0.1020(8) 0.0735(4) 0.6377(14) 0.040(2) Uani 0.5 1 d . . P A 2
O1 O 0.4311(4) 0.42664(16) 0.0448(6) 0.0492(12) Uani 1 1 d . . . . .
O4B O 0.1215(8) 0.0493(4) 0.5971(14) 0.040(2) Uani 0.5 1 d . . P A 1
O1W O 0.5524(5) 0.500000 0.2894(7) 0.0465(16) Uani 1 2 d S T P . .
H1WA H 0.579864 0.528910 0.259708 0.070 Uiso 0.5 1 d R U P B -1
H1W H 0.561354 0.500000 0.392588 0.070 Uiso 1 2 d R U P . .
O2 O 0.3976(3) 0.21971(16) 0.1818(5) 0.0384(10) Uani 1 1 d . . . . .
O2W O 0.2712(5) 0.500000 -0.1019(7) 0.0494(17) Uani 1 2 d S T P . .
H2W H 0.233095 0.474660 -0.167690 0.074 Uiso 1 1 d R U . . .
O3 O 0.2516(3) 0.0633(2) 0.7997(5) 0.0482(12) Uani 1 1 d . . . . .
C1 C 0.500000 0.4021(3) 0.000000 0.0248(15) Uani 1 2 d S T P . .
C2 C 0.500000 0.3391(3) 0.000000 0.0214(14) Uani 1 2 d S T P . .
C3 C 0.4441(4) 0.3108(2) 0.0940(6) 0.0265(11) Uani 1 1 d . . . . .
H3 H 0.406642 0.330576 0.153887 0.032 Uiso 1 1 calc R U . . .
C4 C 0.4461(4) 0.2523(2) 0.0955(6) 0.0278(12) Uani 1 1 d . . . . .
C5 C 0.500000 0.2237(3) 0.000000 0.0291(17) Uani 1 2 d S T P . .
H5 H 0.499999 0.184640 -0.000004 0.035 Uiso 1 2 calc R U P . .
C6 C 0.3465(5) 0.2480(2) 0.2889(7) 0.0385(14) Uani 1 1 d . . . . .
H6A H 0.289882 0.269842 0.225381 0.046 Uiso 1 1 calc R U . . .
H6B H 0.393377 0.273320 0.360465 0.046 Uiso 1 1 calc R U . . .
C7 C 0.3076(5) 0.2042(2) 0.3896(7) 0.0344(13) Uani 1 1 d . . . . .
C8 C 0.3684(5) 0.1869(3) 0.5321(8) 0.0420(15) Uani 1 1 d . . . . .
H8 H 0.433901 0.201437 0.567858 0.050 Uiso 1 1 calc R U . . .
C9 C 0.3332(5) 0.1466(3) 0.6279(8) 0.0416(15) Uani 1 1 d . . . . .
H9 H 0.374017 0.135968 0.729086 0.050 Uiso 1 1 calc R U . . .
C10 C 0.2374(4) 0.1230(2) 0.5698(6) 0.0314(12) Uani 1 1 d . . . . .
C11 C 0.1775(5) 0.1404(3) 0.4180(8) 0.0449(16) Uani 1 1 d . . . . .
H11 H 0.114118 0.123959 0.374921 0.054 Uiso 1 1 calc R U . . .
C12 C 0.2122(5) 0.1813(3) 0.3338(7) 0.0448(16) Uani 1 1 d . . . . .
H12 H 0.170333 0.194038 0.235898 0.054 Uiso 1 1 calc R U . . .
C13 C 0.1990(5) 0.0801(3) 0.6657(7) 0.0373(13) Uani 1 1 d . . . . .
O3W O 0.3784(7) 0.0823(5) 0.2032(12) 0.155(4) Uiso 1 1 d . . . . .
O4W O 0.5342(13) 0.0635(7) 0.031(2) 0.119(6) Uiso 0.45 1 d . . P . .
O5W O 0.557(2) 0.000000 0.228(4) 0.129(10) Uiso 0.4 2 d S . P . .
O6W O 0.500000 -0.027(2) 0.500000 0.13(2) Uiso 0.2 2 d S . P . .


_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
Tm1 O1 2.232(4) . ?
Tm1 O1 2.232(4) 6_565 ?
Tm1 O4B 2.326(11) 4_556 ?
Tm1 O4B 2.326(11) 7_556 ?
Tm1 O1W 2.339(6) . ?
Tm1 O2W 2.352(6) . ?
Tm1 O3 2.382(4) 7_556 ?
Tm1 O3 2.382(4) 4_556 ?
Tm1 O4A 2.386(11) 4_556 ?
Tm1 O4A 2.386(11) 7_556 ?
Tm1 C13 2.738(6) 4_556 ?
Tm1 C13 2.738(6) 7_556 ?
O4A C13 1.285(12) . ?
O1 C1 1.239(5) . ?
O4B C13 1.292(12) . ?
O1W H1WA 0.8501 . ?
O1W H1W 0.8500 . ?
O2 C4 1.344(6) . ?
O2 C6 1.438(7) . ?
O2W H2W 0.8921 . ?
O2W H2W 0.8921 6_565 ?
O3 C13 1.243(7) . ?
C1 C2 1.498(10) . ?
C2 C3 1.400(6) 2_655 ?
C2 C3 1.400(6) . ?
C3 C4 1.393(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.521(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.342(8) . ?
C7 C12 1.373(9) . ?
C8 C9 1.413(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.398(8) . ?
C10 C13 1.478(8) . ?
C11 C12 1.358(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
O4W O4W 0.95(3) 2_655 ?
O6W O6W 1.27(11) 5_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tm1 O1 103.0(2) . 6_565 ?
O1 Tm1 O4B 148.9(3) . 4_556 ?
O1 Tm1 O4B 93.8(3) 6_565 4_556 ?
O1 Tm1 O4B 93.8(3) . 7_556 ?
O1 Tm1 O4B 148.9(3) 6_565 7_556 ?
O4B Tm1 O4B 60.6(5) 4_556 7_556 ?
O1 Tm1 O1W 78.23(16) . . ?
O1 Tm1 O1W 78.23(16) 6_565 . ?
O4B Tm1 O1W 79.9(3) 4_556 . ?
O4B Tm1 O1W 79.9(3) 7_556 . ?
O1 Tm1 O2W 75.75(17) . . ?
O1 Tm1 O2W 75.75(17) 6_565 . ?
O4B Tm1 O2W 134.4(3) 4_556 . ?
O4B Tm1 O2W 134.4(3) 7_556 . ?
O1W Tm1 O2W 137.6(2) . . ?
O1 Tm1 O3 83.97(17) . 7_556 ?
O1 Tm1 O3 152.25(17) 6_565 7_556 ?
O4B Tm1 O3 93.2(3) 4_556 7_556 ?
O4B Tm1 O3 54.4(3) 7_556 7_556 ?
O1W Tm1 O3 129.46(14) . 7_556 ?
O2W Tm1 O3 80.16(17) . 7_556 ?
O1 Tm1 O3 152.25(17) . 4_556 ?
O1 Tm1 O3 83.97(17) 6_565 4_556 ?
O4B Tm1 O3 54.4(3) 4_556 4_556 ?
O4B Tm1 O3 93.2(3) 7_556 4_556 ?
O1W Tm1 O3 129.46(14) . 4_556 ?
O2W Tm1 O3 80.16(17) . 4_556 ?
O3 Tm1 O3 78.5(3) 7_556 4_556 ?
O1 Tm1 O4A 153.9(3) . 4_556 ?
O1 Tm1 O4A 75.5(3) 6_565 4_556 ?
O4B Tm1 O4A 18.3(3) 4_556 4_556 ?
O4B Tm1 O4A 77.9(4) 7_556 4_556 ?
O1W Tm1 O4A 76.0(3) . 4_556 ?
O2W Tm1 O4A 127.4(3) . 4_556 ?
O3 Tm1 O4A 109.7(3) 7_556 4_556 ?
O3 Tm1 O4A 53.8(3) 4_556 4_556 ?
O1 Tm1 O4A 75.5(3) . 7_556 ?
O1 Tm1 O4A 153.9(3) 6_565 7_556 ?
O4B Tm1 O4A 77.9(4) 4_556 7_556 ?
O4B Tm1 O4A 18.3(3) 7_556 7_556 ?
O1W Tm1 O4A 76.0(3) . 7_556 ?
O2W Tm1 O4A 127.4(3) . 7_556 ?
O3 Tm1 O4A 53.8(3) 7_556 7_556 ?
O3 Tm1 O4A 109.7(3) 4_556 7_556 ?
O1 Tm1 C13 172.62(18) . 4_556 ?
O1 Tm1 C13 84.40(18) 6_565 4_556 ?
O4B Tm1 C13 28.1(3) 4_556 4_556 ?
O4B Tm1 C13 79.6(3) 7_556 4_556 ?
O1W Tm1 C13 103.75(17) . 4_556 ?
O2W Tm1 C13 106.34(18) . 4_556 ?
O3 Tm1 C13 89.39(18) 7_556 4_556 ?
O3 Tm1 C13 26.97(16) 4_556 4_556 ?
O1 Tm1 C13 84.40(18) . 7_556 ?
O1 Tm1 C13 172.62(18) 6_565 7_556 ?
O4B Tm1 C13 79.6(3) 4_556 7_556 ?
O4B Tm1 C13 28.1(3) 7_556 7_556 ?
O1W Tm1 C13 103.75(17) . 7_556 ?
O2W Tm1 C13 106.34(18) . 7_556 ?
O3 Tm1 C13 26.97(16) 7_556 7_556 ?
O3 Tm1 C13 89.39(18) 4_556 7_556 ?
C13 Tm1 C13 88.2(3) 4_556 7_556 ?
C13 O4A Tm1 91.4(6) . 7_556 ?
C1 O1 Tm1 149.9(4) . . ?
C13 O4B Tm1 94.0(6) . 7_556 ?
Tm1 O1W H1WA 109.7 . . ?
Tm1 O1W H1W 109.3 . . ?
H1WA O1W H1W 110.0 . . ?
C4 O2 C6 116.7(4) . . ?
Tm1 O2W H2W 135.8 . . ?
Tm1 O2W H2W 135.84(4) . 6_565 ?
H2W O2W H2W 85.1 . 6_565 ?
C13 O3 Tm1 92.7(4) . 7_556 ?
O1 C1 O1 123.7(7) 2_655 . ?
O1 C1 C2 118.2(3) 2_655 . ?
O1 C1 C2 118.2(3) . . ?
C3 C2 C3 122.4(7) 2_655 . ?
C3 C2 C1 118.8(3) 2_655 . ?
C3 C2 C1 118.8(3) . . ?
C4 C3 C2 118.4(5) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
O2 C4 C3 124.9(5) . . ?
O2 C4 C5 115.5(5) . . ?
C3 C4 C5 119.7(5) . . ?
C4 C5 C4 121.5(7) . 2_655 ?
C4 C5 H5 119.2 . . ?
C4 C5 H5 119.2 2_655 . ?
O2 C6 C7 108.7(5) . . ?
O2 C6 H6A 109.9 . . ?
C7 C6 H6A 109.9 . . ?
O2 C6 H6B 109.9 . . ?
C7 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C8 C7 C12 119.9(5) . . ?
C8 C7 C6 119.5(6) . . ?
C12 C7 C6 120.6(6) . . ?
C7 C8 C9 120.3(6) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 119.5(6) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 118.9(5) . . ?
C9 C10 C13 120.8(5) . . ?
C11 C10 C13 120.3(5) . . ?
C12 C11 C10 119.7(6) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C7 121.7(6) . . ?
C11 C12 H12 119.2 . . ?
C7 C12 H12 119.2 . . ?
O3 C13 O4A 117.0(7) . . ?
O3 C13 O4B 116.2(7) . . ?
O3 C13 C10 121.5(5) . . ?
O4A C13 C10 117.8(7) . . ?
O4B C13 C10 120.2(7) . . ?
O3 C13 Tm1 60.3(3) . 7_556 ?
O4B C13 Tm1 57.9(5) . 7_556 ?
C10 C13 Tm1 178.2(4) . 7_556 ?

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
Tm1 O1 C1 O1 -32.2(6) . . . 2_655 ?
Tm1 O1 C1 C2 147.8(6) . . . . ?
O1 C1 C2 C3 -19.2(4) 2_655 . . 2_655 ?
O1 C1 C2 C3 160.8(4) . . . 2_655 ?
O1 C1 C2 C3 160.8(4) 2_655 . . . ?
O1 C1 C2 C3 -19.2(4) . . . . ?
C3 C2 C3 C4 1.2(4) 2_655 . . . ?
C1 C2 C3 C4 -178.8(4) . . . . ?
C6 O2 C4 C3 -4.8(8) . . . . ?
C6 O2 C4 C5 176.4(4) . . . . ?
C2 C3 C4 O2 178.9(4) . . . . ?
C2 C3 C4 C5 -2.3(7) . . . . ?
O2 C4 C5 C4 -179.9(5) . . . 2_655 ?
C3 C4 C5 C4 1.2(4) . . . 2_655 ?
C4 O2 C6 C7 -173.3(5) . . . . ?
O2 C6 C7 C8 88.6(7) . . . . ?
O2 C6 C7 C12 -89.6(7) . . . . ?
C12 C7 C8 C9 -2.3(10) . . . . ?
C6 C7 C8 C9 179.5(6) . . . . ?
C7 C8 C9 C10 3.2(10) . . . . ?
C8 C9 C10 C11 -0.7(10) . . . . ?
C8 C9 C10 C13 179.0(6) . . . . ?
C9 C10 C11 C12 -2.6(10) . . . . ?
C13 C10 C11 C12 177.7(6) . . . . ?
C10 C11 C12 C7 3.6(11) . . . . ?
C8 C7 C12 C11 -1.1(10) . . . . ?
C6 C7 C12 C11 177.1(6) . . . . ?
Tm1 O3 C13 O4A 22.3(8) 7_556 . . . ?
Tm1 O3 C13 O4B -15.8(7) 7_556 . . . ?
Tm1 O3 C13 C10 -179.7(5) 7_556 . . . ?
Tm1 O4A C13 O3 -22.2(7) 7_556 . . . ?
Tm1 O4A C13 C10 179.0(5) 7_556 . . . ?
Tm1 O4B C13 O3 16.2(8) 7_556 . . . ?
Tm1 O4B C13 C10 -179.7(5) 7_556 . . . ?
C9 C10 C13 O3 -0.9(10) . . . . ?
C11 C10 C13 O3 178.8(6) . . . . ?
C9 C10 C13 O4A 156.9(8) . . . . ?
C11 C10 C13 O4A -23.4(10) . . . . ?
C9 C10 C13 O4B -164.2(8) . . . . ?
C11 C10 C13 O4B 15.5(10) . . . . ?

_refine_diff_density_max         0.858
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.134

