# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2024

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2117762'
loop_
_audit_author_name
_audit_author_address
'Carole Daiguebonne'
;INSA Rennes
France
;
_audit_update_record             
;
2024-10-28 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens. 0.21Ang From Nd1 6.18 eA-3
RESPONSE: Indeed there is a small residual density that is very near to a Nd ion.
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on Nd2 6.08 eA-3
RESPONSE: Indeed there is a small residual density that is very near to a Nd ion.
;
_vrf_PLAT975_shelx               
;
PROBLEM: Check Calcd Resid. Dens. 0.57Ang From O17 . 2.51 eA-3
RESPONSE: Indeed there is a small residual density that is very near to an O ion.
;
_vrf_PLAT043_shelx               
;
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 60.48 Check
RESPONSE: This is due to the fact that H atoms could not be placed.
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow4 Check
RESPONSE: This is due to the fact that H atoms could not be placed.
;
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Resid. Dens. 1.38Ang From O17 -2.57 eA-3
RESPONSE: Indeed there is a small residual density that is very near to an O ion.
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H60 Cl24 Nd4 O54'
_chemical_formula_weight         2928.72

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.8914(15)
_cell_length_b                   13.7161(17)
_cell_length_c                   16.245(2)
_cell_angle_alpha                74.024(6)
_cell_angle_beta                 86.691(6)
_cell_angle_gamma                72.279(5)
_cell_volume                     2221.5(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9607
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.47

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_F_000             1428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    3.125
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            10016
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.964
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             10016
_reflns_number_gt                9282
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0472P)²+2.6649P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10016
_refine_ls_number_parameters     586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1027
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_restrained_S_all      1.298
_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
Nd1 Nd 0.78981(2) 0.46113(2) 0.90080(2) 0.01063(7) Uani 1 1 d . . . . .
Nd2 Nd 0.67958(2) 0.50925(2) 0.45244(2) 0.01118(7) Uani 1 1 d . . . . .
Cl1 Cl 0.79253(10) 0.84029(8) 0.82260(6) 0.0247(2) Uani 1 1 d . . . . .
Cl2 Cl 0.74466(10) 1.05191(7) 0.87526(6) 0.0248(2) Uani 1 1 d . . . . .
Cl3 Cl 0.63472(9) 1.06562(7) 1.05525(6) 0.01982(18) Uani 1 1 d . . . . .
Cl4 Cl 0.57713(10) 0.87223(7) 1.18124(6) 0.0238(2) Uani 1 1 d . . . . .
Cl5 Cl 1.03410(9) 0.12162(7) 0.90676(5) 0.02058(18) Uani 1 1 d . . . . .
Cl6 Cl 1.08345(9) -0.09438(7) 0.86185(6) 0.02220(19) Uani 1 1 d . . . . .
Cl7 Cl 1.05463(10) -0.09570(7) 0.67209(6) 0.0242(2) Uani 1 1 d . . . . .
Cl8 Cl 0.97393(9) 0.11875(7) 0.52873(5) 0.02109(18) Uani 1 1 d . . . . .
Cl9 Cl 0.67040(9) 0.08879(7) 0.65147(5) 0.02011(18) Uani 1 1 d . . . . .
Cl10 Cl 0.73151(10) -0.12890(7) 0.60691(6) 0.0240(2) Uani 1 1 d . . . . .
Cl11 Cl 0.69248(9) -0.13268(7) 0.41968(6) 0.02115(18) Uani 1 1 d . . . . .
Cl12 Cl 0.59005(10) 0.07816(7) 0.27762(6) 0.02293(19) Uani 1 1 d . . . . .
O1 O 0.8452(3) 0.5935(2) 0.96649(18) 0.0203(5) Uani 1 1 d . . . . .
O2 O 0.6469(3) 0.6449(2) 0.91628(19) 0.0235(6) Uani 1 1 d . . . . .
O3 O 0.7142(3) 0.5885(3) 1.1432(3) 0.0428(9) Uani 1 1 d . . . . .
O4 O 0.5078(3) 0.6815(3) 1.1334(2) 0.0358(8) Uani 1 1 d . . . . .
O5 O 1.0481(3) 0.3667(2) 0.7364(2) 0.0288(7) Uani 1 1 d . . . . .
O6 O 0.8655(2) 0.3494(2) 0.80065(17) 0.0188(5) Uani 1 1 d . . . . .
O7 O 1.0309(3) 0.3443(2) 0.5416(2) 0.0308(7) Uani 1 1 d . . . . .
O8 O 0.8230(2) 0.3679(2) 0.56759(16) 0.0180(5) Uani 1 1 d . . . . .
O9 O 0.6503(2) 0.33970(19) 0.46403(17) 0.0170(5) Uani 1 1 d . . . . .
O10 O 0.4845(2) 0.31855(19) 0.54792(16) 0.0162(5) Uani 1 1 d . . . . .
O11 O 0.6007(3) 0.3086(2) 0.26947(17) 0.0211(6) Uani 1 1 d . . . . .
O12 O 0.4300(2) 0.3460(2) 0.35079(16) 0.0173(5) Uani 1 1 d . . . . .
O13 O 0.6475(3) 0.4555(2) 1.0280(2) 0.0303(7) Uani 1 1 d . . . . .
O14 O 0.9351(3) 0.3491(2) 1.02438(17) 0.0231(6) Uani 1 1 d . . . . .
O15 O 0.7386(3) 0.2874(2) 0.94915(19) 0.0261(6) Uani 1 1 d . . . . .
O16 O 1.0117(2) 0.4651(2) 0.86329(17) 0.0202(5) Uani 1 1 d . . . . .
O17 O 0.7805(3) 0.5928(2) 0.76279(17) 0.0210(6) Uani 1 1 d . . . . .
O18 O 0.5790(3) 0.4918(2) 0.83342(18) 0.0217(6) Uani 1 1 d . . . . .
O19 O 0.5585(2) 0.47917(19) 0.59159(16) 0.0141(5) Uani 1 1 d . . . . .
O20 O 0.7643(2) 0.6036(2) 0.53708(17) 0.0178(5) Uani 1 1 d . . . . .
O21 O 0.7080(3) 0.6656(2) 0.33938(18) 0.0258(6) Uani 1 1 d . . . . .
O22 O 0.6817(3) 0.4770(2) 0.30901(17) 0.0216(6) Uani 1 1 d . . . . .
O23 O 0.9065(2) 0.4775(2) 0.40613(17) 0.0192(5) Uani 1 1 d . . . . .
OW1 O 0.8360(3) 0.3457(3) 1.1834(2) 0.0334(7) Uani 1 1 d . . . . .
OW2 O 0.3929(3) 0.7321(2) 0.89561(18) 0.0231(6) Uani 1 1 d . . . . .
OW3 O 0.9798(3) 0.6706(2) 0.6913(2) 0.0330(7) Uani 1 1 d . . . . .
OW4 O 0.6514(3) 0.3090(2) 0.72228(18) 0.0228(6) Uani 1 1 d . . . . .
C1 C 0.7086(3) 0.7623(3) 0.9784(2) 0.0132(6) Uani 1 1 d . . . . .
C2 C 0.7336(3) 0.8498(3) 0.9220(2) 0.0156(7) Uani 1 1 d . . . . .
C3 C 0.7104(3) 0.9445(3) 0.9448(2) 0.0163(7) Uani 1 1 d . . . . .
C4 C 0.6616(3) 0.9507(3) 1.0251(2) 0.0151(7) Uani 1 1 d . . . . .
C5 C 0.6366(3) 0.8621(3) 1.0815(2) 0.0150(7) Uani 1 1 d . . . . .
C6 C 0.6581(3) 0.7676(3) 1.0590(2) 0.0135(6) Uani 1 1 d . . . . .
C7 C 0.7349(3) 0.6609(3) 0.9517(2) 0.0139(6) Uani 1 1 d . . . . .
C8 C 0.6272(4) 0.6709(3) 1.1177(2) 0.0164(7) Uani 1 1 d . . . . .
C9 C 0.9866(3) 0.2154(3) 0.7374(2) 0.0133(6) Uani 1 1 d . . . . .
C10 C 1.0201(3) 0.1196(3) 0.8018(2) 0.0142(6) Uani 1 1 d . . . . .
C11 C 1.0423(3) 0.0232(3) 0.7823(2) 0.0147(7) Uani 1 1 d . . . . .
C12 C 1.0286(3) 0.0227(3) 0.6973(2) 0.0159(7) Uani 1 1 d . . . . .
C13 C 0.9936(3) 0.1187(3) 0.6334(2) 0.0143(6) Uani 1 1 d . . . . .
C14 C 0.9740(3) 0.2148(3) 0.6528(2) 0.0122(6) Uani 1 1 d . . . . .
C15 C 0.9649(4) 0.3190(3) 0.7593(2) 0.0166(7) Uani 1 1 d . . . . .
C16 C 0.9390(3) 0.3181(3) 0.5816(2) 0.0138(6) Uani 1 1 d . . . . .
C17 C 0.6026(3) 0.1804(3) 0.4844(2) 0.0126(6) Uani 1 1 d . . . . .
C18 C 0.6475(3) 0.0857(3) 0.5483(2) 0.0139(6) Uani 1 1 d . . . . .
C19 C 0.6762(3) -0.0115(3) 0.5284(2) 0.0151(7) Uani 1 1 d . . . . .
C20 C 0.6585(3) -0.0133(3) 0.4446(2) 0.0148(7) Uani 1 1 d . . . . .
C21 C 0.6145(3) 0.0822(3) 0.3805(2) 0.0143(6) Uani 1 1 d . . . . .
C22 C 0.5868(3) 0.1787(3) 0.4002(2) 0.0139(6) Uani 1 1 d . . . . .
C23 C 0.5769(3) 0.2880(3) 0.5022(2) 0.0134(6) Uani 1 1 d . . . . .
C24 C 0.5356(3) 0.2851(3) 0.3337(2) 0.0139(7) 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
Nd1 O17 2.446(3) . ?
Nd1 O18 2.469(3) . ?
Nd1 O14 2.466(3) . ?
Nd1 O16 2.471(3) . ?
Nd1 O6 2.475(3) . ?
Nd1 O13 2.509(3) . ?
Nd1 O15 2.517(3) . ?
Nd1 O1 2.571(3) . ?
Nd1 O2 2.599(3) . ?
Nd1 C7 2.957(3) . ?
Nd2 O9 2.398(2) . ?
Nd2 O23 2.485(3) . ?
Nd2 O22 2.486(3) . ?
Nd2 O10 2.489(2) 2_666 ?
Nd2 O8 2.489(2) . ?
Nd2 O21 2.498(3) . ?
Nd2 O20 2.504(3) . ?
Nd2 O19 2.548(3) . ?
Nd2 O19 2.676(2) 2_666 ?
Cl1 C2 1.726(4) . ?
Cl2 C3 1.719(4) . ?
Cl3 C4 1.714(4) . ?
Cl4 C5 1.735(4) . ?
Cl5 C10 1.730(3) . ?
Cl6 C11 1.718(3) . ?
Cl7 C12 1.719(4) . ?
Cl8 C13 1.725(3) . ?
Cl9 C18 1.723(3) . ?
Cl10 C19 1.718(3) . ?
Cl11 C20 1.721(3) . ?
Cl12 C21 1.726(4) . ?
O1 C7 1.261(4) . ?
O2 C7 1.249(4) . ?
O3 C8 1.218(5) . ?
O4 C8 1.283(5) . ?
O5 C15 1.255(5) . ?
O6 C15 1.261(4) . ?
O7 C16 1.253(5) . ?
O8 C16 1.240(4) . ?
O9 C23 1.254(4) . ?
O10 C23 1.253(4) . ?
O11 C24 1.250(5) . ?
O12 C24 1.267(4) . ?
C1 C2 1.385(5) . ?
C1 C6 1.403(5) . ?
C1 C7 1.510(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.396(5) . ?
C4 C5 1.397(5) . ?
C5 C6 1.391(5) . ?
C6 C8 1.523(5) . ?
C9 C14 1.392(5) . ?
C9 C10 1.396(5) . ?
C9 C15 1.507(5) . ?
C10 C11 1.391(5) . ?
C11 C12 1.400(5) . ?
C12 C13 1.395(5) . ?
C13 C14 1.390(5) . ?
C14 C16 1.520(5) . ?
C17 C18 1.390(5) . ?
C17 C22 1.395(5) . ?
C17 C23 1.521(5) . ?
C18 C19 1.397(5) . ?
C19 C20 1.393(5) . ?
C20 C21 1.399(5) . ?
C21 C22 1.386(5) . ?
C22 C24 1.521(5) . ?

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
O17 Nd1 O18 73.93(9) . . ?
O17 Nd1 O14 142.56(9) . . ?
O18 Nd1 O14 143.11(9) . . ?
O17 Nd1 O16 71.68(9) . . ?
O18 Nd1 O16 141.07(9) . . ?
O14 Nd1 O16 71.60(9) . . ?
O17 Nd1 O6 77.25(9) . . ?
O18 Nd1 O6 81.92(9) . . ?
O14 Nd1 O6 98.87(9) . . ?
O16 Nd1 O6 73.24(9) . . ?
O17 Nd1 O13 133.20(10) . . ?
O18 Nd1 O13 78.78(11) . . ?
O14 Nd1 O13 75.06(10) . . ?
O16 Nd1 O13 139.37(10) . . ?
O6 Nd1 O13 135.28(10) . . ?
O17 Nd1 O15 134.46(10) . . ?
O18 Nd1 O15 73.62(9) . . ?
O14 Nd1 O15 72.87(10) . . ?
O16 Nd1 O15 120.71(10) . . ?
O6 Nd1 O15 67.30(9) . . ?
O13 Nd1 O15 68.65(10) . . ?
O17 Nd1 O1 86.11(9) . . ?
O18 Nd1 O1 124.40(9) . . ?
O14 Nd1 O1 75.22(9) . . ?
O16 Nd1 O1 70.78(9) . . ?
O6 Nd1 O1 143.55(9) . . ?
O13 Nd1 O1 78.86(10) . . ?
O15 Nd1 O1 139.04(9) . . ?
O17 Nd1 O2 71.83(10) . . ?
O18 Nd1 O2 74.35(9) . . ?
O14 Nd1 O2 115.51(9) . . ?
O16 Nd1 O2 110.78(9) . . ?
O6 Nd1 O2 145.08(9) . . ?
O13 Nd1 O2 64.51(10) . . ?
O15 Nd1 O2 127.03(10) . . ?
O1 Nd1 O2 50.07(8) . . ?
O17 Nd1 C7 77.75(9) . . ?
O18 Nd1 C7 99.26(9) . . ?
O14 Nd1 C7 95.73(9) . . ?
O16 Nd1 C7 90.83(9) . . ?
O6 Nd1 C7 153.56(9) . . ?
O13 Nd1 C7 69.96(10) . . ?
O15 Nd1 C7 138.60(10) . . ?
O1 Nd1 C7 25.15(9) . . ?
O2 Nd1 C7 24.92(9) . . ?
O9 Nd2 O23 100.89(9) . . ?
O9 Nd2 O22 69.14(9) . . ?
O23 Nd2 O22 74.00(9) . . ?
O9 Nd2 O10 129.32(9) . 2_666 ?
O23 Nd2 O10 128.35(9) . 2_666 ?
O22 Nd2 O10 109.73(9) . 2_666 ?
O9 Nd2 O8 69.07(9) . . ?
O23 Nd2 O8 71.06(8) . . ?
O22 Nd2 O8 117.73(9) . . ?
O10 Nd2 O8 132.42(8) 2_666 . ?
O9 Nd2 O21 139.22(9) . . ?
O23 Nd2 O21 68.38(9) . . ?
O22 Nd2 O21 70.09(9) . . ?
O10 Nd2 O21 65.58(9) 2_666 . ?
O8 Nd2 O21 134.04(9) . . ?
O9 Nd2 O20 140.78(8) . . ?
O23 Nd2 O20 78.33(9) . . ?
O22 Nd2 O20 143.30(9) . . ?
O10 Nd2 O20 70.24(8) 2_666 . ?
O8 Nd2 O20 73.88(9) . . ?
O21 Nd2 O20 77.60(9) . . ?
O9 Nd2 O19 78.15(8) . . ?
O23 Nd2 O19 138.22(8) . . ?
O22 Nd2 O19 138.84(8) . . ?
O10 Nd2 O19 72.74(8) 2_666 . ?
O8 Nd2 O19 69.77(8) . . ?
O21 Nd2 O19 136.57(9) . . ?
O20 Nd2 O19 77.45(8) . . ?
O9 Nd2 O19 66.16(8) . 2_666 ?
O23 Nd2 O19 144.50(8) . 2_666 ?
O22 Nd2 O19 70.50(8) . 2_666 ?
O10 Nd2 O19 66.35(8) 2_666 2_666 ?
O8 Nd2 O19 126.59(8) . 2_666 ?
O21 Nd2 O19 99.18(9) . 2_666 ?
O20 Nd2 O19 133.20(8) . 2_666 ?
O19 Nd2 O19 73.87(8) . 2_666 ?
C7 O1 Nd1 94.8(2) . . ?
C7 O2 Nd1 93.8(2) . . ?
C15 O6 Nd1 138.8(2) . . ?
C16 O8 Nd2 139.2(2) . . ?
C23 O9 Nd2 137.1(2) . . ?
C23 O10 Nd2 135.9(2) . 2_666 ?
Nd2 O19 Nd2 106.13(8) . 2_666 ?
C2 C1 C6 120.8(3) . . ?
C2 C1 C7 119.1(3) . . ?
C6 C1 C7 120.1(3) . . ?
C1 C2 C3 120.5(3) . . ?
C1 C2 Cl1 119.1(3) . . ?
C3 C2 Cl1 120.4(3) . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 Cl2 120.3(3) . . ?
C4 C3 Cl2 120.3(3) . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 Cl3 120.3(3) . . ?
C5 C4 Cl3 120.1(3) . . ?
C6 C5 C4 121.3(3) . . ?
C6 C5 Cl4 120.3(3) . . ?
C4 C5 Cl4 118.4(3) . . ?
C5 C6 C1 118.3(3) . . ?
C5 C6 C8 122.6(3) . . ?
C1 C6 C8 119.1(3) . . ?
O2 C7 O1 121.3(3) . . ?
O2 C7 C1 119.5(3) . . ?
O1 C7 C1 119.2(3) . . ?
O2 C7 Nd1 61.28(19) . . ?
O1 C7 Nd1 60.03(18) . . ?
C1 C7 Nd1 179.2(2) . . ?
O3 C8 O4 124.3(4) . . ?
O3 C8 C6 119.2(4) . . ?
O4 C8 C6 116.4(3) . . ?
C14 C9 C10 119.8(3) . . ?
C14 C9 C15 120.1(3) . . ?
C10 C9 C15 120.1(3) . . ?
C11 C10 C9 120.8(3) . . ?
C11 C10 Cl5 119.9(3) . . ?
C9 C10 Cl5 119.3(3) . . ?
C10 C11 C12 119.4(3) . . ?
C10 C11 Cl6 120.5(3) . . ?
C12 C11 Cl6 120.0(3) . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 Cl7 120.3(3) . . ?
C11 C12 Cl7 120.1(3) . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 Cl8 119.3(3) . . ?
C12 C13 Cl8 119.8(3) . . ?
C13 C14 C9 119.6(3) . . ?
C13 C14 C16 119.8(3) . . ?
C9 C14 C16 120.6(3) . . ?
O5 C15 O6 125.7(3) . . ?
O5 C15 C9 117.4(3) . . ?
O6 C15 C9 116.9(3) . . ?
O8 C16 O7 126.0(3) . . ?
O8 C16 C14 117.5(3) . . ?
O7 C16 C14 116.5(3) . . ?
C18 C17 C22 120.2(3) . . ?
C18 C17 C23 121.7(3) . . ?
C22 C17 C23 118.0(3) . . ?
C17 C18 C19 120.0(3) . . ?
C17 C18 Cl9 119.8(3) . . ?
C19 C18 Cl9 120.2(3) . . ?
C20 C19 C18 119.8(3) . . ?
C20 C19 Cl10 119.8(3) . . ?
C18 C19 Cl10 120.4(3) . . ?
C19 C20 C21 119.8(3) . . ?
C19 C20 Cl11 120.2(3) . . ?
C21 C20 Cl11 120.0(3) . . ?
C22 C21 C20 120.2(3) . . ?
C22 C21 Cl12 120.7(3) . . ?
C20 C21 Cl12 119.1(3) . . ?
C21 C22 C17 119.9(3) . . ?
C21 C22 C24 122.6(3) . . ?
C17 C22 C24 117.5(3) . . ?
O9 C23 O10 126.7(3) . . ?
O9 C23 C17 113.8(3) . . ?
O10 C23 C17 119.3(3) . . ?
O11 C24 O12 124.8(3) . . ?
O11 C24 C22 119.5(3) . . ?
O12 C24 C22 115.6(3) . . ?

_refine_diff_density_max         5.523
_refine_diff_density_min         -2.393
_refine_diff_density_rms         0.483



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2118210'
loop_
_audit_author_name
_audit_author_address
'Carole Daiguebonne'
;INSA Rennes
France
;
_audit_update_record             
;
2024-10-28 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H10 Cl4 O8 Y'
_chemical_formula_weight         464.87

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

_cell_length_a                   8.7595(6)
_cell_length_b                   6.7789(5)
_cell_length_c                   11.8297(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.615(3)
_cell_angle_gamma                90
_cell_volume                     699.07(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2620
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.29

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_F_000             458
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.969
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6274
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2741
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.768
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             1697
_reflns_number_gt                1491
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+2.9045P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1697
_refine_ls_number_parameters     136
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1208
_refine_ls_wR_factor_gt          0.1154
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.004
_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
Y1 Y 0.37470(6) 0.750000 0.95702(5) 0.01777(19) Uani 1 2 d S T P . .
Cl1 Cl 0.63919(19) 0.250000 0.6835(2) 0.0462(5) Uani 1 2 d S T P . .
Cl2 Cl 0.5217(2) 0.250000 0.42593(17) 0.0371(4) Uani 1 2 d S T P . .
Cl3 Cl 0.1680(2) 0.250000 0.35374(14) 0.0389(5) Uani 1 2 d S T P . .
Cl4 Cl -0.06071(18) 0.250000 0.53805(15) 0.0349(4) Uani 1 2 d S T P . .
O1 O 0.4281(6) 0.4087(6) 0.8968(3) 0.0591(14) Uani 1 1 d . . . . .
O2 O 0.0372(5) 0.4114(7) 0.8196(4) 0.0496(11) Uani 1 1 d . . . . .
H2 H -0.012173 0.473862 0.766630 0.059 Uiso 0.5 1 calc R U P . .
O3 O 0.6047(9) 0.750000 0.8607(6) 0.0570(18) Uani 1 2 d DS T P . .
H3B H 0.551(12) 0.750000 0.798(5) 0.068 Uiso 1 2 d DS U P . .
O4 O 0.2058(8) 0.750000 0.7908(6) 0.0559(19) Uani 1 2 d DS T P . .
H4A H 0.173(6) 0.863(5) 0.776(6) 0.067 Uiso 1 1 d D U . . .
H4B H 0.299(4) 0.750000 0.783(10) 0.067 Uiso 1 2 d DS U P . .
O5 O 0.1998(6) 0.5397(9) 1.0459(4) 0.0585(13) Uani 1 1 d D . . . .
H5A H 0.134(7) 0.574(12) 1.088(6) 0.070 Uiso 1 1 d D U . . .
C1 C 0.3430(7) 0.250000 0.7238(5) 0.0201(12) Uani 1 2 d S T P . .
C2 C 0.4456(7) 0.250000 0.6414(6) 0.0247(14) Uani 1 2 d S T P . .
C3 C 0.3923(7) 0.250000 0.5264(6) 0.0246(14) Uani 1 2 d S T P . .
C4 C 0.2354(8) 0.250000 0.4940(5) 0.0259(14) Uani 1 2 d S T P . .
C5 C 0.1342(7) 0.250000 0.5781(5) 0.0226(13) Uani 1 2 d S T P . .
C6 C 0.1869(7) 0.250000 0.6920(5) 0.0210(13) Uani 1 2 d S T P . .
C7 C 0.4050(8) 0.250000 0.8479(6) 0.0275(15) Uani 1 2 d S T P . .
C8 C 0.0762(8) 0.250000 0.7841(6) 0.0269(15) Uani 1 2 d S T P . .
H5B H 0.193(18) 0.415(3) 1.048(14) 0.29(11) Uiso 1 1 d D . . . .
H3A H 0.694(6) 0.750000 0.842(12) 0.6(4) Uiso 1 2 d DS . 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
Y1 O4 2.342(6) . ?
Y1 O5 2.408(5) 4_575 ?
Y1 O5 2.409(5) . ?
Y1 O3 2.410(8) . ?
Y1 O1 2.479(5) 4_575 ?
Y1 O1 2.479(5) . ?
Y1 O1 2.559(5) 2_657 ?
Y1 O1 2.559(4) 3_667 ?
Y1 C7 2.859(7) 3_667 ?
Y1 H3B 2.55(12) . ?
Y1 H4B 2.10(11) . ?
Cl1 C2 1.720(6) . ?
Cl2 C3 1.721(6) . ?
Cl3 C4 1.705(7) . ?
Cl4 C5 1.727(6) . ?
O1 C7 1.229(5) . ?
O2 C8 1.232(5) . ?
O2 H2 0.8400 . ?
O3 H3B 0.83(2) . ?
O3 H3A 0.84(2) . ?
O4 H4A 0.83(2) . ?
O4 H4B 0.83(2) . ?
O4 H4A 0.83(2) 4_575 ?
O5 H5A 0.83(2) . ?
O5 H5B 0.84(2) . ?
C1 C6 1.383(9) . ?
C1 C2 1.390(9) . ?
C1 C7 1.515(9) . ?
C2 C3 1.394(9) . ?
C3 C4 1.390(9) . ?
C4 C5 1.396(9) . ?
C5 C6 1.381(8) . ?
C6 C8 1.528(9) . ?

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
O4 Y1 O5 89.4(2) . 4_575 ?
O4 Y1 O5 89.4(2) . . ?
O5 Y1 O5 72.6(2) 4_575 . ?
O4 Y1 O3 95.3(3) . . ?
O5 Y1 O3 143.46(12) 4_575 . ?
O5 Y1 O3 143.46(12) . . ?
O4 Y1 O1 83.13(12) . 4_575 ?
O5 Y1 O1 73.66(18) 4_575 4_575 ?
O5 Y1 O1 145.48(18) . 4_575 ?
O3 Y1 O1 70.99(13) . 4_575 ?
O4 Y1 O1 83.13(12) . . ?
O5 Y1 O1 145.48(18) 4_575 . ?
O5 Y1 O1 73.66(18) . . ?
O3 Y1 O1 70.99(13) . . ?
O1 Y1 O1 137.9(2) 4_575 . ?
O4 Y1 O1 153.71(12) . 2_657 ?
O5 Y1 O1 82.68(18) 4_575 2_657 ?
O5 Y1 O1 111.74(18) . 2_657 ?
O3 Y1 O1 77.2(2) . 2_657 ?
O1 Y1 O1 70.60(14) 4_575 2_657 ?
O1 Y1 O1 116.91(11) . 2_657 ?
O4 Y1 O1 153.71(12) . 3_667 ?
O5 Y1 O1 111.74(18) 4_575 3_667 ?
O5 Y1 O1 82.68(18) . 3_667 ?
O3 Y1 O1 77.2(2) . 3_667 ?
O1 Y1 O1 116.92(11) 4_575 3_667 ?
O1 Y1 O1 70.60(14) . 3_667 ?
O1 Y1 O1 49.72(19) 2_657 3_667 ?
O4 Y1 C7 176.8(3) . 3_667 ?
O5 Y1 C7 93.20(18) 4_575 3_667 ?
O5 Y1 C7 93.20(18) . 3_667 ?
O3 Y1 C7 81.5(2) . 3_667 ?
O1 Y1 C7 95.76(11) 4_575 3_667 ?
O1 Y1 C7 95.76(11) . 3_667 ?
O1 Y1 C7 25.44(10) 2_657 3_667 ?
O1 Y1 C7 25.44(10) 3_667 3_667 ?
O4 Y1 H3B 76.2(10) . . ?
O5 Y1 H3B 141.3(4) 4_575 . ?
O5 Y1 H3B 141.3(4) . . ?
O3 Y1 H3B 19.1(10) . . ?
O1 Y1 H3B 69.08(13) 4_575 . ?
O1 Y1 H3B 69.08(12) . . ?
O1 Y1 H3B 94.5(9) 2_657 . ?
O1 Y1 H3B 94.5(9) 3_667 . ?
C7 Y1 H3B 100.6(10) 3_667 . ?
O4 Y1 H4B 20.7(7) . . ?
O5 Y1 H4B 105.9(6) 4_575 . ?
O5 Y1 H4B 105.9(6) . . ?
O3 Y1 H4B 74.6(7) . . ?
O1 Y1 H4B 76.6(2) 4_575 . ?
O1 Y1 H4B 76.6(2) . . ?
O1 Y1 H4B 142.2(5) 2_657 . ?
O1 Y1 H4B 142.2(5) 3_667 . ?
C7 Y1 H4B 156.1(7) 3_667 . ?
H3B Y1 H4B 55.5(12) . . ?
C7 O1 Y1 157.7(5) . . ?
C7 O1 Y1 91.1(4) . 3_667 ?
Y1 O1 Y1 109.40(14) . 3_667 ?
C8 O2 H2 109.5 . . ?
Y1 O3 H3B 90(9) . . ?
Y1 O3 H3A 167(10) . . ?
H3B O3 H3A 103(4) . . ?
Y1 O4 H4A 111(5) . . ?
Y1 O4 H4B 63(8) . . ?
H4A O4 H4B 108(4) . . ?
Y1 O4 H4A 111(5) . 4_575 ?
H4A O4 H4A 134(9) . 4_575 ?
H4B O4 H4A 108(4) . 4_575 ?
Y1 O5 H5A 127(6) . . ?
Y1 O5 H5B 131(7) . . ?
H5A O5 H5B 102(4) . . ?
C6 C1 C2 120.0(6) . . ?
C6 C1 C7 121.0(6) . . ?
C2 C1 C7 119.0(6) . . ?
C1 C2 C3 120.4(6) . . ?
C1 C2 Cl1 118.9(5) . . ?
C3 C2 Cl1 120.7(5) . . ?
C4 C3 C2 119.8(6) . . ?
C4 C3 Cl2 120.6(5) . . ?
C2 C3 Cl2 119.5(5) . . ?
C3 C4 C5 118.9(6) . . ?
C3 C4 Cl3 120.5(5) . . ?
C5 C4 Cl3 120.6(5) . . ?
C6 C5 C4 121.4(6) . . ?
C6 C5 Cl4 119.6(5) . . ?
C4 C5 Cl4 119.0(5) . . ?
C5 C6 C1 119.5(6) . . ?
C5 C6 C8 121.4(6) . . ?
C1 C6 C8 119.1(6) . . ?
O1 C7 O1 122.2(6) . 4_565 ?
O1 C7 C1 118.9(3) . . ?
O1 C7 C1 118.9(3) 4_565 . ?
O1 C7 Y1 63.5(3) . 3_667 ?
O1 C7 Y1 63.5(3) 4_565 3_667 ?
C1 C7 Y1 158.7(5) . 3_667 ?
O2 C8 O2 125.3(7) . 4_565 ?
O2 C8 C6 117.3(3) . . ?
O2 C8 C6 117.3(3) 4_565 . ?

_refine_diff_density_max         1.955
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.140



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2384464'
loop_
_audit_author_name
_audit_author_address
'Carole Daiguebonne'
;INSA Rennes
France
;
_audit_update_record             
;
2024-10-28 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Bond Without Acceptor O11 --H11B . Please Check
RESPONSE: Hydrogen atoms have been located based on residual
density peaks before refining with constraints.
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H14 Cl8 K O15 Tb'
_chemical_formula_weight         927.89

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.7604(5)
_cell_length_b                   11.5722(6)
_cell_length_c                   13.8453(7)
_cell_angle_alpha                90.302(2)
_cell_angle_beta                 97.300(2)
_cell_angle_gamma                102.131(2)
_cell_volume                     1360.39(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9851
_cell_measurement_theta_min      2.2955
_cell_measurement_theta_max      27.4870

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_F_000             900
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.610
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15418
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.371
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             6146
_reflns_number_gt                6020
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0085P)²+0.9140P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6146
_refine_ls_number_parameters     412
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0137
_refine_ls_R_factor_gt           0.0133
_refine_ls_wR_factor_ref         0.0313
_refine_ls_wR_factor_gt          0.0312
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.49390(2) 0.94013(2) 0.72645(2) 0.00932(3) Uani 1 1 d . . . . .
K1 K 0.91758(4) 1.16573(3) 0.84726(3) 0.01617(7) Uani 1 1 d . . . . .
Cl1 Cl 0.98163(5) 0.72128(3) 0.74743(3) 0.01663(8) Uani 1 1 d . . . . .
Cl2 Cl 0.94998(5) 0.45453(3) 0.79688(3) 0.01614(8) Uani 1 1 d . . . . .
Cl3 Cl 0.78523(5) 0.35797(3) 0.97570(3) 0.01661(8) Uani 1 1 d . . . . .
Cl4 Cl 0.64914(5) 0.52584(3) 1.10089(3) 0.01694(8) Uani 1 1 d . . . . .
Cl5 Cl 0.13980(5) 0.54522(3) 0.60783(3) 0.01712(8) Uani 1 1 d . . . . .
Cl6 Cl 0.24027(5) 0.34634(3) 0.49465(3) 0.01857(8) Uani 1 1 d . . . . .
Cl7 Cl 0.43520(5) 0.40960(3) 0.32201(3) 0.01752(8) Uani 1 1 d . . . . .
Cl8 Cl 0.51888(5) 0.67226(3) 0.26004(3) 0.01942(8) Uani 1 1 d . . . . .
O1 O 0.70691(14) 0.87812(10) 0.80191(8) 0.0180(2) Uani 1 1 d . . . . .
O2 O 0.92876(16) 0.94441(10) 0.89987(10) 0.0239(3) Uani 1 1 d . . . . .
O3 O 0.56112(14) 0.81092(10) 1.00537(8) 0.0171(2) Uani 1 1 d . . . . .
O4 O 0.76383(14) 0.81187(10) 1.12072(8) 0.0180(2) Uani 1 1 d . . . . .
O5 O 0.30012(14) 0.82207(10) 0.62228(8) 0.0160(2) Uani 1 1 d . . . . .
O6 O 0.12316(15) 0.83756(11) 0.49532(9) 0.0203(3) Uani 1 1 d . . . . .
O7 O 0.32846(14) 0.87517(10) 0.29374(8) 0.0162(2) Uani 1 1 d . . . . .
O8 O 0.52620(13) 0.91836(9) 0.41197(8) 0.0146(2) Uani 1 1 d . . . . .
O9 O 0.54283(15) 1.03499(10) 0.88362(8) 0.0171(2) Uani 1 1 d D . . . .
H9A H 0.621153 1.034664 0.923625 0.026 Uiso 1 1 d DG U . . .
H9B H 0.499411 1.084898 0.906451 0.026 Uiso 1 1 d DG U . . .
O10 O 0.27083(14) 1.01533(11) 0.75517(9) 0.0185(2) Uani 1 1 d D . . . .
H10A H 0.185535 0.998688 0.718880 0.028 Uiso 1 1 d DG U . . .
H10B H 0.266676 1.069437 0.795264 0.028 Uiso 1 1 d DG U . . .
O11 O 0.38804(16) 0.78440(11) 0.82998(9) 0.0210(3) Uani 1 1 d D . . . .
H11A H 0.442809 0.782233 0.883562 0.031 Uiso 1 1 d DG U . . .
H11B H 0.318968 0.726999 0.816094 0.031 Uiso 1 1 d DG U . . .
O12 O 0.63977(14) 0.88816(10) 0.60466(8) 0.0166(2) Uani 1 1 d D . . . .
H12A H 0.612458 0.898005 0.544126 0.025 Uiso 1 1 d DG U . . .
H12B H 0.739068 0.899597 0.618772 0.025 Uiso 1 1 d DG U . . .
O13 O 0.98361(16) 0.96225(11) 0.62321(9) 0.0215(3) Uani 1 1 d D . . . .
H13A H 1.023335 0.924920 0.585424 0.032 Uiso 1 1 d DG U . . .
H13B H 0.975791 1.026372 0.600441 0.032 Uiso 1 1 d DG U . . .
O14 O 1.04530(18) 1.24275(15) 0.68885(10) 0.0345(3) Uani 1 1 d D . . . .
H14A H 1.002392 1.230881 0.631257 0.052 Uiso 1 1 d DG U . . .
H14B H 1.135668 1.276892 0.687218 0.052 Uiso 1 1 d DG U . . .
O15 O 0.79059(15) 1.10305(11) 1.02636(9) 0.0193(2) Uani 1 1 d D . . . .
H15A H 0.873762 1.080644 1.046722 0.029 Uiso 1 1 d DG U . . .
H15B H 0.743805 1.111511 1.073871 0.029 Uiso 1 1 d DG U . . .
C1 C 0.81965(19) 0.86494(13) 0.86375(11) 0.0124(3) Uani 1 1 d . . . . .
C2 C 0.81662(18) 0.73891(13) 0.89576(11) 0.0111(3) Uani 1 1 d . . . . .
C3 C 0.88376(18) 0.66480(13) 0.84266(11) 0.0118(3) Uani 1 1 d . . . . .
C4 C 0.87314(18) 0.54687(13) 0.86605(11) 0.0122(3) Uani 1 1 d . . . . .
C5 C 0.79989(18) 0.50351(13) 0.94566(11) 0.0120(3) Uani 1 1 d . . . . .
C6 C 0.73961(18) 0.57931(13) 1.00196(11) 0.0125(3) Uani 1 1 d . . . . .
C7 C 0.74761(18) 0.69685(13) 0.97729(11) 0.0115(3) Uani 1 1 d . . . . .
C8 C 0.68542(19) 0.78040(13) 1.04015(11) 0.0120(3) Uani 1 1 d . . . . .
C9 C 0.23014(18) 0.79409(13) 0.53797(11) 0.0118(3) Uani 1 1 d . . . . .
C10 C 0.28137(18) 0.69690(13) 0.48329(11) 0.0115(3) Uani 1 1 d . . . . .
C11 C 0.24419(18) 0.57990(13) 0.51106(11) 0.0125(3) Uani 1 1 d . . . . .
C12 C 0.28896(19) 0.49030(13) 0.46072(11) 0.0128(3) Uani 1 1 d . . . . .
C13 C 0.37505(19) 0.51817(13) 0.38300(11) 0.0128(3) Uani 1 1 d . . . . .
C14 C 0.41168(19) 0.63499(14) 0.35536(11) 0.0130(3) Uani 1 1 d . . . . .
C15 C 0.36389(18) 0.72378(13) 0.40440(11) 0.0116(3) Uani 1 1 d . . . . .
C16 C 0.40781(18) 0.84781(13) 0.36867(11) 0.0119(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.2724(11) . ?
Tb1 O5 2.2828(11) . ?
Tb1 O10 2.3755(11) . ?
Tb1 O9 2.3799(11) . ?
Tb1 O12 2.3870(11) . ?
Tb1 O7 2.4057(12) 2_676 ?
Tb1 O11 2.4134(12) . ?
Tb1 O8 2.5405(11) 2_676 ?
Tb1 C16 2.8164(15) 2_676 ?
Tb1 K1 4.2063(4) . ?
K1 O14 2.6612(15) . ?
K1 O7 2.6783(12) 2_676 ?
K1 O2 2.6845(12) . ?
K1 O4 2.7264(13) 2_777 ?
K1 O15 2.8798(13) . ?
K1 Cl3 3.3198(5) 1_565 ?
K1 Cl2 3.3782(5) 1_565 ?
K1 O9 3.4147(14) . ?
K1 C1 3.4216(16) . ?
Cl1 C3 1.7210(16) . ?
Cl2 C4 1.7226(15) . ?
Cl3 C5 1.7193(15) . ?
Cl4 C6 1.7222(16) . ?
Cl5 C11 1.7190(16) . ?
Cl6 C12 1.7142(16) . ?
Cl7 C13 1.7173(15) . ?
Cl8 C14 1.7206(16) . ?
O1 C1 1.258(2) . ?
O2 C1 1.230(2) . ?
O3 C8 1.2540(19) . ?
O4 C8 1.243(2) . ?
O5 C9 1.2546(19) . ?
O6 C9 1.241(2) . ?
O7 C16 1.2539(19) . ?
O8 C16 1.2580(19) . ?
C1 C2 1.522(2) . ?
C2 C7 1.390(2) . ?
C2 C3 1.392(2) . ?
C3 C4 1.391(2) . ?
C4 C5 1.389(2) . ?
C5 C6 1.396(2) . ?
C6 C7 1.394(2) . ?
C7 C8 1.524(2) . ?
C9 C10 1.526(2) . ?
C10 C15 1.386(2) . ?
C10 C11 1.392(2) . ?
C11 C12 1.396(2) . ?
C12 C13 1.392(2) . ?
C13 C14 1.390(2) . ?
C14 C15 1.392(2) . ?
C15 C16 1.509(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O5 123.26(4) . . ?
O1 Tb1 O10 143.33(4) . . ?
O5 Tb1 O10 78.93(4) . . ?
O1 Tb1 O9 75.56(4) . . ?
O5 Tb1 O9 141.97(4) . . ?
O10 Tb1 O9 70.77(4) . . ?
O1 Tb1 O12 71.62(4) . . ?
O5 Tb1 O12 78.45(4) . . ?
O10 Tb1 O12 145.02(4) . . ?
O9 Tb1 O12 138.69(4) . . ?
O1 Tb1 O7 86.63(4) . 2_676 ?
O5 Tb1 O7 132.50(4) . 2_676 ?
O10 Tb1 O7 98.55(4) . 2_676 ?
O9 Tb1 O7 75.68(4) . 2_676 ?
O12 Tb1 O7 78.00(4) . 2_676 ?
O1 Tb1 O11 74.93(4) . . ?
O5 Tb1 O11 77.47(4) . . ?
O10 Tb1 O11 83.55(5) . . ?
O9 Tb1 O11 76.81(4) . . ?
O12 Tb1 O11 116.77(4) . . ?
O7 Tb1 O11 149.94(4) 2_676 . ?
O1 Tb1 O8 130.03(4) . 2_676 ?
O5 Tb1 O8 80.95(4) . 2_676 ?
O10 Tb1 O8 78.04(4) . 2_676 ?
O9 Tb1 O8 113.48(4) . 2_676 ?
O12 Tb1 O8 72.32(4) . 2_676 ?
O7 Tb1 O8 52.72(4) 2_676 2_676 ?
O11 Tb1 O8 153.91(4) . 2_676 ?
O1 Tb1 C16 109.94(5) . 2_676 ?
O5 Tb1 C16 107.28(4) . 2_676 ?
O10 Tb1 C16 86.49(4) . 2_676 ?
O9 Tb1 C16 93.50(4) . 2_676 ?
O12 Tb1 C16 75.26(4) . 2_676 ?
O7 Tb1 C16 26.31(4) 2_676 2_676 ?
O11 Tb1 C16 167.94(4) . 2_676 ?
O8 Tb1 C16 26.53(4) 2_676 2_676 ?
O1 Tb1 K1 55.32(3) . . ?
O5 Tb1 K1 163.58(3) . . ?
O10 Tb1 K1 111.78(3) . . ?
O9 Tb1 K1 54.25(3) . . ?
O12 Tb1 K1 86.16(3) . . ?
O7 Tb1 K1 36.32(3) 2_676 . ?
O11 Tb1 K1 115.17(3) . . ?
O8 Tb1 K1 88.99(3) 2_676 . ?
C16 Tb1 K1 62.62(3) 2_676 . ?
O14 K1 O7 76.67(4) . 2_676 ?
O14 K1 O2 117.48(5) . . ?
O7 K1 O2 101.00(4) 2_676 . ?
O14 K1 O4 69.73(4) . 2_777 ?
O7 K1 O4 142.48(4) 2_676 2_777 ?
O2 K1 O4 80.80(4) . 2_777 ?
O14 K1 O15 174.91(5) . . ?
O7 K1 O15 106.09(4) 2_676 . ?
O2 K1 O15 66.52(4) . . ?
O4 K1 O15 108.77(4) 2_777 . ?
O14 K1 Cl3 117.50(4) . 1_565 ?
O7 K1 Cl3 95.85(3) 2_676 1_565 ?
O2 K1 Cl3 124.79(3) . 1_565 ?
O4 K1 Cl3 114.03(3) 2_777 1_565 ?
O15 K1 Cl3 58.30(3) . 1_565 ?
O14 K1 Cl2 62.10(4) . 1_565 ?
O7 K1 Cl2 86.06(3) 2_676 1_565 ?
O2 K1 Cl2 172.71(3) . 1_565 ?
O4 K1 Cl2 92.50(3) 2_777 1_565 ?
O15 K1 Cl2 113.50(3) . 1_565 ?
Cl3 K1 Cl2 55.473(11) 1_565 1_565 ?
O14 K1 O9 132.69(4) . . ?
O7 K1 O9 56.05(3) 2_676 . ?
O2 K1 O9 74.21(4) . . ?
O4 K1 O9 152.47(4) 2_777 . ?
O15 K1 O9 50.38(3) . . ?
Cl3 K1 O9 72.94(2) 1_565 . ?
Cl2 K1 O9 111.71(2) 1_565 . ?
O14 K1 C1 115.34(5) . . ?
O7 K1 C1 82.45(4) 2_676 . ?
O2 K1 C1 18.71(4) . . ?
O4 K1 C1 96.97(4) 2_777 . ?
O15 K1 C1 69.51(4) . . ?
Cl3 K1 C1 125.11(3) 1_565 . ?
Cl2 K1 C1 168.50(3) 1_565 . ?
O9 K1 C1 60.89(3) . . ?
O14 K1 Tb1 101.97(4) . . ?
O7 K1 Tb1 32.14(2) 2_676 . ?
O2 K1 Tb1 71.88(3) . . ?
O4 K1 Tb1 143.62(3) 2_777 . ?
O15 K1 Tb1 82.13(3) . . ?
Cl3 K1 Tb1 101.332(12) 1_565 . ?
Cl2 K1 Tb1 115.414(12) 1_565 . ?
O9 K1 Tb1 34.447(19) . . ?
C1 K1 Tb1 53.30(3) . . ?
C4 Cl2 K1 121.19(6) . 1_545 ?
C5 Cl3 K1 122.99(5) . 1_545 ?
C1 O1 Tb1 162.50(10) . . ?
C1 O2 K1 116.89(10) . . ?
C8 O4 K1 122.45(10) . 2_777 ?
C9 O5 Tb1 150.81(11) . . ?
C16 O7 Tb1 95.45(9) . 2_676 ?
C16 O7 K1 152.99(10) . 2_676 ?
Tb1 O7 K1 111.55(4) 2_676 2_676 ?
C16 O8 Tb1 89.06(9) . 2_676 ?
Tb1 O9 K1 91.30(4) . . ?
O2 C1 O1 125.62(15) . . ?
O2 C1 C2 118.63(14) . . ?
O1 C1 C2 115.75(14) . . ?
O2 C1 K1 44.41(8) . . ?
O1 C1 K1 81.25(9) . . ?
C2 C1 K1 162.84(10) . . ?
C7 C2 C3 119.56(14) . . ?
C7 C2 C1 120.88(13) . . ?
C3 C2 C1 119.57(14) . . ?
C4 C3 C2 120.86(14) . . ?
C4 C3 Cl1 120.12(11) . . ?
C2 C3 Cl1 119.02(12) . . ?
C5 C4 C3 119.65(13) . . ?
C5 C4 Cl2 119.91(11) . . ?
C3 C4 Cl2 120.43(12) . . ?
C4 C5 C6 119.51(14) . . ?
C4 C5 Cl3 120.39(11) . . ?
C6 C5 Cl3 120.09(12) . . ?
C7 C6 C5 120.74(14) . . ?
C7 C6 Cl4 119.64(11) . . ?
C5 C6 Cl4 119.60(12) . . ?
C2 C7 C6 119.54(13) . . ?
C2 C7 C8 119.71(13) . . ?
C6 C7 C8 120.73(14) . . ?
O4 C8 O3 126.59(14) . . ?
O4 C8 C7 116.49(13) . . ?
O3 C8 C7 116.92(13) . . ?
O6 C9 O5 126.16(14) . . ?
O6 C9 C10 117.22(13) . . ?
O5 C9 C10 116.62(13) . . ?
C15 C10 C11 119.09(13) . . ?
C15 C10 C9 120.37(13) . . ?
C11 C10 C9 120.54(14) . . ?
C10 C11 C12 120.90(14) . . ?
C10 C11 Cl5 119.51(11) . . ?
C12 C11 Cl5 119.59(12) . . ?
C13 C12 C11 119.78(14) . . ?
C13 C12 Cl6 119.77(11) . . ?
C11 C12 Cl6 120.45(12) . . ?
C14 C13 C12 119.15(13) . . ?
C14 C13 Cl7 120.40(12) . . ?
C12 C13 Cl7 120.45(12) . . ?
C13 C14 C15 120.91(14) . . ?
C13 C14 Cl8 120.21(12) . . ?
C15 C14 Cl8 118.87(12) . . ?
C10 C15 C14 120.14(14) . . ?
C10 C15 C16 122.69(13) . . ?
C14 C15 C16 117.17(14) . . ?
O7 C16 O8 122.22(14) . . ?
O7 C16 C15 118.40(13) . . ?
O8 C16 C15 119.30(13) . . ?
O7 C16 Tb1 58.24(8) . 2_676 ?
O8 C16 Tb1 64.41(8) . 2_676 ?
C15 C16 Tb1 169.76(10) . 2_676 ?

_refine_diff_density_max         0.405
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.063



####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2117764'
loop_
_audit_author_name
_audit_author_address
'Carole Daiguebonne'
;INSA Rennes
France
;
_audit_update_record             
;
2024-10-28 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_shelx               
;
PROBLEM: Short Inter D-H..H-D Hw2A ..H9A . 2.08 Ang.
RESPONSE: Hydrogen atoms have been located based on residual
density peaks before refining with constraints.
;
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Bond Without Acceptor O13 --H13B . Please Check
RESPONSE: Hydrogen atoms have been located based on residual
density peaks before refining with constraints.
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H14 Cl8 K La O15'
_chemical_formula_weight         907.88

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'
Cl Cl 0.1484 0.1585 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.1777(11)
_cell_length_b                   12.7369(19)
_cell_length_c                   13.969(2)
_cell_angle_alpha                85.230(6)
_cell_angle_beta                 77.920(6)
_cell_angle_gamma                87.757(6)
_cell_volume                     1417.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9795
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.48

_exptl_crystal_description       stick
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_F_000             884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    2.477
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            6492
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.108
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6492
_reflns_number_gt                5984
_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 APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0262P)²+2.0868P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6492
_refine_ls_number_parameters     412
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0739
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.077
_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 0.48750(2) 0.25323(2) 0.47287(2) 0.01289(6) Uani 1 1 d . . . . .
K1 K 0.00347(8) 0.15628(6) 0.42899(5) 0.02535(15) Uani 1 1 d . . . . .
Cl1 Cl 0.02491(11) 0.25313(6) 0.76349(6) 0.02943(18) Uani 1 1 d . . . . .
Cl2 Cl 0.06802(10) 0.19967(6) 0.97936(5) 0.02418(16) Uani 1 1 d . . . . .
Cl3 Cl 0.26096(10) -0.00635(6) 1.03250(5) 0.02375(16) Uani 1 1 d . . . . .
Cl4 Cl 0.40590(10) -0.15690(6) 0.87045(5) 0.02347(15) Uani 1 1 d . . . . .
Cl5 Cl 0.88708(10) 0.35157(6) 0.16220(5) 0.02337(15) Uani 1 1 d . . . . .
Cl6 Cl 0.83955(9) 0.42857(6) -0.04928(5) 0.02228(15) Uani 1 1 d . . . . .
Cl7 Cl 0.63574(9) 0.63446(6) -0.08157(5) 0.02242(15) Uani 1 1 d . . . . .
Cl8 Cl 0.46385(9) 0.75715(6) 0.09726(5) 0.02213(15) Uani 1 1 d . . . . .
O1 O 0.2589(3) 0.13753(17) 0.55353(15) 0.0237(5) Uani 1 1 d . . . . .
O2 O 0.0199(3) 0.05556(18) 0.60920(15) 0.0251(5) Uani 1 1 d . . . . .
O3 O 0.4940(3) -0.08011(16) 0.61649(15) 0.0200(4) Uani 1 1 d . . . . .
O4 O 0.2662(3) -0.17419(16) 0.66029(14) 0.0193(4) Uani 1 1 d . . . . .
O5 O 0.5628(2) 0.42175(16) 0.37374(14) 0.0196(4) Uani 1 1 d . . . . .
O6 O 0.8225(2) 0.47817(16) 0.35763(14) 0.0178(4) Uani 1 1 d . . . . .
O7 O 0.5607(2) 0.68084(16) 0.36061(14) 0.0188(4) Uani 1 1 d . . . . .
O8 O 0.3247(2) 0.65628(17) 0.30976(15) 0.0217(4) Uani 1 1 d . . . . .
O9 O 0.6348(3) 0.10963(17) 0.56450(16) 0.0245(5) Uani 1 1 d D . . . .
H9A H 0.664(4) 0.115(3) 0.6170(18) 0.029 Uiso 1 1 d D U . . .
H9B H 0.588(4) 0.0497(19) 0.576(3) 0.029 Uiso 1 1 d D U . . .
O10 O 0.7783(3) 0.31276(17) 0.49821(15) 0.0191(4) Uani 1 1 d D . . . .
H10A H 0.764(4) 0.326(3) 0.5570(15) 0.023 Uiso 1 1 d D U . . .
H10B H 0.688(3) 0.303(3) 0.490(2) 0.023 Uiso 1 1 d D U . . .
O11 O 0.2217(3) 0.37047(17) 0.50269(16) 0.0229(4) Uani 1 1 d D . . . .
H11A H 0.204(5) 0.409(2) 0.5492(18) 0.027 Uiso 1 1 d D U . . .
H11B H 0.187(4) 0.406(2) 0.4588(19) 0.027 Uiso 1 1 d D U . . .
O12 O 0.3280(3) 0.26859(18) 0.32990(16) 0.0261(5) Uani 1 1 d D . . . .
H12B H 0.285(5) 0.3256(17) 0.313(3) 0.031 Uiso 1 1 d D U . . .
H12A H 0.314(5) 0.225(2) 0.295(2) 0.031 Uiso 1 1 d D U . . .
O13 O 0.1841(4) 0.1291(2) 0.2334(2) 0.0441(7) Uani 1 1 d D . . . .
H13A H 0.204(5) 0.0649(17) 0.243(4) 0.053 Uiso 1 1 d D U . . .
H13B H 0.095(4) 0.133(3) 0.213(3) 0.053 Uiso 1 1 d D U . . .
OW1 O 0.1688(3) 0.46257(18) 0.32393(17) 0.0245(5) Uani 1 1 d D . . . .
HW1A H 0.069(2) 0.469(3) 0.319(3) 0.029 Uiso 1 1 d D U . . .
HW1B H 0.207(4) 0.5213(19) 0.307(3) 0.029 Uiso 1 1 d D U . . .
OW2 O 0.7351(4) 0.0869(2) 0.7401(2) 0.0439(7) Uani 1 1 d D . . . .
HW2A H 0.843(3) 0.088(3) 0.703(3) 0.053 Uiso 1 1 d D U . . .
HW2B H 0.749(5) 0.149(2) 0.766(3) 0.053 Uiso 1 1 d D U . . .
C1 C 0.1937(4) 0.0710(2) 0.7214(2) 0.0168(5) Uani 1 1 d . . . . .
C2 C 0.1315(4) 0.1401(2) 0.7939(2) 0.0180(6) Uani 1 1 d . . . . .
C3 C 0.1517(4) 0.1166(2) 0.8901(2) 0.0174(6) Uani 1 1 d . . . . .
C4 C 0.2367(3) 0.0245(2) 0.9139(2) 0.0163(5) Uani 1 1 d . . . . .
C5 C 0.3008(4) -0.0434(2) 0.8414(2) 0.0168(5) Uani 1 1 d . . . . .
C6 C 0.2799(3) -0.0205(2) 0.74534(19) 0.0157(5) Uani 1 1 d . . . . .
C7 C 0.1547(4) 0.0907(2) 0.6203(2) 0.0167(5) Uani 1 1 d . . . . .
C8 C 0.3502(3) -0.0968(2) 0.66882(19) 0.0158(5) Uani 1 1 d . . . . .
C9 C 0.6820(3) 0.5134(2) 0.22439(19) 0.0145(5) Uani 1 1 d . . . . .
C10 C 0.7657(3) 0.4622(2) 0.1436(2) 0.0160(5) Uani 1 1 d . . . . .
C11 C 0.7478(3) 0.4979(2) 0.0489(2) 0.0162(5) Uani 1 1 d . . . . .
C12 C 0.6532(3) 0.5885(2) 0.03535(19) 0.0158(5) Uani 1 1 d . . . . .
C13 C 0.5718(3) 0.6407(2) 0.1165(2) 0.0154(5) Uani 1 1 d . . . . .
C14 C 0.5808(3) 0.6016(2) 0.21139(19) 0.0147(5) Uani 1 1 d . . . . .
C15 C 0.6914(3) 0.4676(2) 0.3269(2) 0.0155(5) Uani 1 1 d . . . . .
C16 C 0.4798(3) 0.6514(2) 0.30088(19) 0.0151(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O1 2.448(2) . ?
La1 O5 2.481(2) . ?
La1 O9 2.553(2) . ?
La1 O11 2.569(2) . ?
La1 O12 2.595(2) . ?
La1 O3 2.607(2) 2_656 ?
La1 O10 2.626(2) . ?
La1 O4 2.667(2) 2_656 ?
La1 C8 2.999(3) 2_656 ?
La1 K1 4.2825(9) 1_655 ?
La1 K1 4.3695(9) . ?
La1 H10B 1.847(19) . ?
K1 O4 2.745(2) 2_556 ?
K1 O10 2.754(2) 1_455 ?
K1 O2 2.755(2) . ?
K1 O2 2.815(2) 2_556 ?
K1 O13 2.862(3) . ?
K1 O1 2.977(2) . ?
K1 O12 3.072(3) . ?
K1 C7 3.210(3) . ?
K1 O9 3.255(2) 1_455 ?
K1 K1 4.2948(15) 2_556 ?
K1 H12A 2.94(4) . ?
K1 H13A 3.06(5) . ?
K1 H13B 2.99(5) . ?
Cl1 C2 1.723(3) . ?
Cl2 C3 1.716(3) . ?
Cl3 C4 1.721(3) . ?
Cl4 C5 1.716(3) . ?
Cl5 C10 1.725(3) . ?
Cl6 C11 1.715(3) . ?
Cl7 C12 1.721(3) . ?
Cl8 C13 1.727(3) . ?
O1 C7 1.252(3) . ?
O2 C7 1.250(4) . ?
O3 C8 1.264(3) . ?
O4 C8 1.250(4) . ?
O5 C15 1.254(3) . ?
O6 C15 1.251(3) . ?
O7 C16 1.256(3) . ?
O7 C14 2.363(3) . ?
O8 C16 1.248(3) . ?
O9 H9A 0.827(18) . ?
O9 H9B 0.854(18) . ?
O10 H10A 0.837(17) . ?
O10 H10B 0.788(18) . ?
O11 H11A 0.829(18) . ?
O11 H11B 0.820(18) . ?
O12 H12B 0.834(18) . ?
O12 H12A 0.792(18) . ?
O13 H13A 0.832(18) . ?
O13 H13B 0.834(18) . ?
OW1 HW1A 0.832(18) . ?
OW1 HW1B 0.820(18) . ?
OW2 HW2A 0.925(19) . ?
OW2 HW2B 0.912(19) . ?
C1 C6 1.392(4) . ?
C1 C2 1.398(4) . ?
C1 C7 1.510(4) . ?
C2 C3 1.396(4) . ?
C3 C4 1.393(4) . ?
C4 C5 1.392(4) . ?
C5 C6 1.393(4) . ?
C6 C8 1.514(4) . ?
C9 C10 1.390(4) . ?
C9 C14 1.391(4) . ?
C9 C15 1.517(4) . ?
C10 C11 1.397(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.395(4) . ?
C13 C14 1.392(4) . ?
C14 C16 1.518(4) . ?

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 La1 O5 145.56(7) . . ?
O1 La1 O9 76.99(7) . . ?
O5 La1 O9 137.16(7) . . ?
O1 La1 O11 73.74(7) . . ?
O5 La1 O11 74.26(7) . . ?
O9 La1 O11 139.30(7) . . ?
O1 La1 O12 83.70(8) . . ?
O5 La1 O12 71.73(7) . . ?
O9 La1 O12 137.84(7) . . ?
O11 La1 O12 65.57(7) . . ?
O1 La1 O3 70.00(7) . 2_656 ?
O5 La1 O3 118.90(7) . 2_656 ?
O9 La1 O3 70.84(7) . 2_656 ?
O11 La1 O3 122.48(7) . 2_656 ?
O12 La1 O3 67.39(7) . 2_656 ?
O1 La1 O10 139.75(7) . . ?
O5 La1 O10 70.71(7) . . ?
O9 La1 O10 67.65(7) . . ?
O11 La1 O10 123.25(7) . . ?
O12 La1 O10 135.89(7) . . ?
O3 La1 O10 113.31(7) 2_656 . ?
O1 La1 O4 118.18(7) . 2_656 ?
O5 La1 O4 83.40(6) . 2_656 ?
O9 La1 O4 73.44(7) . 2_656 ?
O11 La1 O4 146.25(6) . 2_656 ?
O12 La1 O4 83.70(7) . 2_656 ?
O3 La1 O4 49.38(6) 2_656 2_656 ?
O10 La1 O4 69.86(6) . 2_656 ?
O1 La1 C8 94.40(8) . 2_656 ?
O5 La1 C8 100.98(7) . 2_656 ?
O9 La1 C8 71.22(7) . 2_656 ?
O11 La1 C8 138.11(7) . 2_656 ?
O12 La1 C8 73.37(7) . 2_656 ?
O3 La1 C8 24.80(7) 2_656 2_656 ?
O10 La1 C8 91.97(7) . 2_656 ?
O4 La1 C8 24.61(7) 2_656 2_656 ?
O1 La1 K1 123.04(5) . 1_655 ?
O5 La1 K1 90.80(5) . 1_655 ?
O9 La1 K1 49.28(5) . 1_655 ?
O11 La1 K1 160.84(5) . 1_655 ?
O12 La1 K1 121.63(5) . 1_655 ?
O3 La1 K1 75.08(5) 2_656 1_655 ?
O10 La1 K1 38.30(5) . 1_655 ?
O4 La1 K1 38.33(4) 2_656 1_655 ?
C8 La1 K1 55.54(5) 2_656 1_655 ?
O1 La1 K1 40.68(5) . . ?
O5 La1 K1 108.84(5) . . ?
O9 La1 K1 112.79(5) . . ?
O11 La1 K1 56.51(5) . . ?
O12 La1 K1 43.71(6) . . ?
O3 La1 K1 66.85(5) 2_656 . ?
O10 La1 K1 179.55(5) . . ?
O4 La1 K1 110.11(4) 2_656 . ?
C8 La1 K1 88.09(6) 2_656 . ?
K1 La1 K1 141.88(2) 1_655 . ?
O1 La1 H10B 141.4(11) . . ?
O5 La1 H10B 68.2(11) . . ?
O9 La1 H10B 70.5(11) . . ?
O11 La1 H10B 120.2(11) . . ?
O12 La1 H10B 134.8(11) . . ?
O3 La1 H10B 116.1(11) 2_656 . ?
O10 La1 H10B 3.2(11) . . ?
O4 La1 H10B 71.8(10) 2_656 . ?
C8 La1 H10B 94.3(10) 2_656 . ?
K1 La1 H10B 41.2(11) 1_655 . ?
K1 La1 H10B 176.5(11) . . ?
O4 K1 O10 66.90(6) 2_556 1_455 ?
O4 K1 O2 127.78(7) 2_556 . ?
O10 K1 O2 96.78(7) 1_455 . ?
O4 K1 O2 80.55(6) 2_556 2_556 ?
O10 K1 O2 135.19(7) 1_455 2_556 ?
O2 K1 O2 79.12(7) . 2_556 ?
O4 K1 O13 82.89(8) 2_556 . ?
O10 K1 O13 129.74(8) 1_455 . ?
O2 K1 O13 133.12(9) . . ?
O2 K1 O13 71.73(8) 2_556 . ?
O4 K1 O1 171.54(6) 2_556 . ?
O10 K1 O1 107.30(6) 1_455 . ?
O2 K1 O1 45.25(6) . . ?
O2 K1 O1 100.90(6) 2_556 . ?
O13 K1 O1 105.51(8) . . ?
O4 K1 O12 119.31(6) 2_556 . ?
O10 K1 O12 105.87(6) 1_455 . ?
O2 K1 O12 112.82(6) . . ?
O2 K1 O12 116.91(6) 2_556 . ?
O13 K1 O12 55.15(7) . . ?
O1 K1 O12 67.62(6) . . ?
O4 K1 C7 149.45(7) 2_556 . ?
O10 K1 C7 100.46(7) 1_455 . ?
O2 K1 C7 22.57(7) . . ?
O2 K1 C7 92.16(7) 2_556 . ?
O13 K1 C7 123.10(8) . . ?
O1 K1 C7 22.95(7) . . ?
O12 K1 C7 90.52(7) . . ?
O4 K1 O9 62.04(6) 2_556 1_455 ?
O10 K1 O9 56.62(6) 1_455 1_455 ?
O2 K1 O9 67.66(6) . 1_455 ?
O2 K1 O9 81.49(6) 2_556 1_455 ?
O13 K1 O9 138.94(7) . 1_455 ?
O1 K1 O9 109.78(6) . 1_455 ?
O12 K1 O9 161.57(6) . 1_455 ?
C7 K1 O9 87.61(7) . 1_455 ?
O4 K1 La1 37.07(4) 2_556 1_455 ?
O10 K1 La1 36.22(4) 1_455 1_455 ?
O2 K1 La1 101.75(5) . 1_455 ?
O2 K1 La1 100.33(5) 2_556 1_455 ?
O13 K1 La1 118.79(6) . 1_455 ?
O1 K1 La1 134.94(5) . 1_455 ?
O12 K1 La1 132.54(5) . 1_455 ?
C7 K1 La1 117.68(5) . 1_455 ?
O9 K1 La1 36.48(4) 1_455 1_455 ?
O4 K1 K1 106.59(5) 2_556 2_556 ?
O10 K1 K1 122.74(5) 1_455 2_556 ?
O2 K1 K1 40.06(5) . 2_556 ?
O2 K1 K1 39.05(4) 2_556 2_556 ?
O13 K1 K1 103.47(7) . 2_556 ?
O1 K1 K1 70.87(5) . 2_556 ?
O12 K1 K1 123.06(5) . 2_556 ?
C7 K1 K1 55.41(5) . 2_556 ?
O9 K1 K1 70.07(4) 1_455 2_556 ?
La1 K1 K1 104.37(2) 1_455 2_556 ?
O4 K1 La1 153.30(5) 2_556 . ?
O10 K1 La1 105.66(5) 1_455 . ?
O2 K1 La1 77.55(5) . . ?
O2 K1 La1 116.57(5) 2_556 . ?
O13 K1 La1 83.61(6) . . ?
O1 K1 La1 32.41(4) . . ?
O12 K1 La1 35.72(4) . . ?
C7 K1 La1 55.03(5) . . ?
O9 K1 La1 137.00(4) 1_455 . ?
La1 K1 La1 141.88(2) 1_455 . ?
K1 K1 La1 98.91(2) 2_556 . ?
O4 K1 H12A 112.1(6) 2_556 . ?
O10 K1 H12A 116.4(5) 1_455 . ?
O2 K1 H12A 119.3(7) . . ?
O2 K1 H12A 103.7(4) 2_556 . ?
O13 K1 H12A 40.4(4) . . ?
O1 K1 H12A 75.8(6) . . ?
O12 K1 H12A 14.9(3) . . ?
C7 K1 H12A 98.4(7) . . ?
O9 K1 H12A 171.8(7) 1_455 . ?
La1 K1 H12A 135.4(7) 1_455 . ?
K1 K1 H12A 118.0(6) 2_556 . ?
La1 K1 H12A 46.3(6) . . ?
O4 K1 H13A 87.8(7) 2_556 . ?
O10 K1 H13A 144.1(5) 1_455 . ?
O2 K1 H13A 119.1(5) . . ?
O2 K1 H13A 57.7(6) 2_556 . ?
O13 K1 H13A 15.7(5) . . ?
O1 K1 H13A 100.1(7) . . ?
O12 K1 H13A 63.7(7) . . ?
C7 K1 H13A 113.4(6) . . ?
O9 K1 H13A 133.3(8) 1_455 . ?
La1 K1 H13A 124.8(7) 1_455 . ?
K1 K1 H13A 87.8(5) 2_556 . ?
La1 K1 H13A 85.4(8) . . ?
H12A K1 H13A 48.9(8) . . ?
O4 K1 H13B 66.7(4) 2_556 . ?
O10 K1 H13B 119.3(6) 1_455 . ?
O2 K1 H13B 143.0(7) . . ?
O2 K1 H13B 69.7(8) 2_556 . ?
O13 K1 H13B 16.2(4) . . ?
O1 K1 H13B 121.6(4) . . ?
O12 K1 H13B 67.3(6) . . ?
C7 K1 H13B 138.1(5) . . ?
O9 K1 H13B 124.3(5) 1_455 . ?
La1 K1 H13B 102.9(4) 1_455 . ?
K1 K1 H13B 106.6(8) 2_556 . ?
La1 K1 H13B 98.7(5) . . ?
H12A K1 H13B 53.5(8) . . ?
H13A K1 H13B 25.2(6) . . ?
C7 O1 La1 160.03(19) . . ?
C7 O1 K1 89.02(17) . . ?
La1 O1 K1 106.90(7) . . ?
C7 O2 K1 99.59(17) . . ?
C7 O2 K1 120.87(18) . 2_556 ?
K1 O2 K1 100.88(7) . 2_556 ?
C8 O3 La1 95.26(17) . 2_656 ?
C8 O4 La1 92.72(16) . 2_656 ?
C8 O4 K1 122.66(17) . 2_556 ?
La1 O4 K1 104.60(7) 2_656 2_556 ?
C15 O5 La1 138.70(18) . . ?
C16 O7 C14 35.10(15) . . ?
La1 O9 K1 94.25(7) . 1_655 ?
La1 O9 H9A 126(3) . . ?
K1 O9 H9A 95(3) 1_655 . ?
La1 O9 H9B 116(2) . . ?
K1 O9 H9B 125(3) 1_655 . ?
H9A O9 H9B 101(3) . . ?
La1 O10 K1 105.48(7) . 1_655 ?
La1 O10 H10A 106(2) . . ?
K1 O10 H10A 120(2) 1_655 . ?
La1 O10 H10B 7(3) . . ?
K1 O10 H10B 112(3) 1_655 . ?
H10A O10 H10B 104(3) . . ?
La1 O11 H11A 119(2) . . ?
La1 O11 H11B 124(3) . . ?
H11A O11 H11B 104(3) . . ?
La1 O12 K1 100.57(8) . . ?
La1 O12 H12B 121(2) . . ?
K1 O12 H12B 98(3) . . ?
La1 O12 H12A 130(3) . . ?
K1 O12 H12A 73(3) . . ?
H12B O12 H12A 109(3) . . ?
K1 O13 H13A 96(4) . . ?
K1 O13 H13B 91(3) . . ?
H13A O13 H13B 105(3) . . ?
HW1A OW1 HW1B 105(3) . . ?
HW2A OW2 HW2B 92(3) . . ?
C6 C1 C2 119.5(3) . . ?
C6 C1 C7 120.1(2) . . ?
C2 C1 C7 120.2(2) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 Cl1 120.3(2) . . ?
C1 C2 Cl1 119.1(2) . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 Cl2 120.2(2) . . ?
C2 C3 Cl2 120.1(2) . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 Cl3 120.0(2) . . ?
C3 C4 Cl3 120.4(2) . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 Cl4 119.7(2) . . ?
C6 C5 Cl4 119.6(2) . . ?
C1 C6 C5 119.9(2) . . ?
C1 C6 C8 121.1(2) . . ?
C5 C6 C8 119.0(2) . . ?
O2 C7 O1 124.6(3) . . ?
O2 C7 C1 116.4(2) . . ?
O1 C7 C1 119.0(3) . . ?
O2 C7 K1 57.83(14) . . ?
O1 C7 K1 68.03(15) . . ?
C1 C7 K1 168.13(18) . . ?
O4 C8 O3 122.5(3) . . ?
O4 C8 C6 119.5(2) . . ?
O3 C8 C6 118.0(2) . . ?
O4 C8 La1 62.67(14) . 2_656 ?
O3 C8 La1 59.94(14) . 2_656 ?
C6 C8 La1 175.03(18) . 2_656 ?
C10 C9 C14 120.1(2) . . ?
C10 C9 C15 119.5(2) . . ?
C14 C9 C15 120.3(2) . . ?
C9 C10 C11 120.5(3) . . ?
C9 C10 Cl5 119.0(2) . . ?
C11 C10 Cl5 120.4(2) . . ?
C12 C11 C10 119.5(2) . . ?
C12 C11 Cl6 120.4(2) . . ?
C10 C11 Cl6 120.1(2) . . ?
C11 C12 C13 119.7(2) . . ?
C11 C12 Cl7 119.5(2) . . ?
C13 C12 Cl7 120.8(2) . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 Cl8 120.3(2) . . ?
C12 C13 Cl8 118.8(2) . . ?
O7 C14 C9 101.87(19) . . ?
O7 C14 C13 133.5(2) . . ?
C9 C14 C13 119.1(2) . . ?
O7 C14 C16 28.40(13) . . ?
C9 C14 C16 119.3(2) . . ?
C13 C14 C16 121.6(2) . . ?
O6 C15 O5 125.8(3) . . ?
O6 C15 C9 118.9(2) . . ?
O5 C15 C9 115.3(2) . . ?
O7 C16 O8 126.2(3) . . ?
O7 C16 C14 116.5(2) . . ?
O8 C16 C14 117.3(2) . . ?

_refine_diff_density_max         1.591
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.198



####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2384468'
loop_
_audit_author_name
_audit_author_address
'Carole Daiguebonne'
;INSA Rennes
France
;
_audit_update_record             
;
2024-10-28 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H11 Cl8 O13 Y'
_chemical_formula_weight         783.76

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

_cell_length_a                   11.5640(6)
_cell_length_b                   18.5537(9)
_cell_length_c                   12.1650(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2610.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8549
_cell_measurement_theta_min      2.6666
_cell_measurement_theta_max      27.3864

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.117
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29504
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.075
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5978
_reflns_number_gt                5414
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0199P)²+0.8998P] 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_abs_structure_details 
;
 Flack x determined using 2293 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5978
_refine_ls_number_parameters     374
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0529
_refine_ls_wR_factor_gt          0.0506
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      1.014
_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
Y1 Y 0.38679(3) 0.56790(2) 0.47148(3) 0.01030(8) Uani 1 1 d . . . . .
Cl1 Cl 0.54122(11) 0.79408(6) 0.42293(10) 0.0317(3) Uani 1 1 d . . . . .
Cl2 Cl 0.55809(12) 0.95809(6) 0.47194(13) 0.0443(3) Uani 1 1 d . . . . .
Cl3 Cl 0.41356(14) 1.02493(6) 0.66159(11) 0.0432(4) Uani 1 1 d . . . . .
Cl4 Cl 0.25068(11) 0.92963(6) 0.80078(10) 0.0301(3) Uani 1 1 d . . . . .
Cl5 Cl 0.54262(8) 0.30737(5) 0.53247(8) 0.0182(2) Uani 1 1 d . . . . .
Cl6 Cl 0.49422(8) 0.14891(5) 0.46683(11) 0.0236(2) Uani 1 1 d . . . . .
Cl7 Cl 0.33115(11) 0.11461(6) 0.27140(11) 0.0308(3) Uani 1 1 d . . . . .
Cl8 Cl 0.21337(12) 0.23922(7) 0.14251(11) 0.0377(3) Uani 1 1 d . . . . .
O1 O 0.4334(2) 0.66182(15) 0.6282(2) 0.0179(6) Uani 1 1 d . . . . .
O2 O 0.3336(2) 0.69004(13) 0.4806(2) 0.0150(5) Uani 1 1 d . . . . .
O3 O 0.2035(2) 0.71915(16) 0.7145(2) 0.0193(6) Uani 1 1 d . . . . .
O4 O 0.2808(3) 0.77635(16) 0.8586(2) 0.0237(7) Uani 1 1 d . . . . .
H4 H 0.244157 0.745222 0.894617 0.028 Uiso 1 1 calc R U . . .
O5 O 0.3149(2) 0.44906(14) 0.4466(2) 0.0159(6) Uani 1 1 d . . . . .
O6 O 0.4944(2) 0.45980(14) 0.3905(2) 0.0162(6) Uani 1 1 d . . . . .
O7 O 0.1550(3) 0.39835(17) 0.2316(2) 0.0236(7) Uani 1 1 d . . . . .
O8 O 0.3288(2) 0.43576(15) 0.1792(2) 0.0156(6) Uani 1 1 d . . . . .
O9 O 0.4539(2) 0.50487(15) 0.6255(2) 0.0157(6) Uani 1 1 d D . . . .
H9A H 0.496969 0.528382 0.667052 0.019 Uiso 1 1 d DG U . . .
H9B H 0.419996 0.470229 0.655630 0.019 Uiso 1 1 d DG U . . .
O10 O 0.2267(3) 0.56081(16) 0.5910(3) 0.0163(7) Uani 1 1 d D . . . .
H10A H 0.169240 0.586235 0.585668 0.020 Uiso 1 1 d DG U . . .
H10B H 0.219002 0.519305 0.621724 0.020 Uiso 1 1 d DG U . . .
O11 O 0.2211(3) 0.57800(18) 0.3504(2) 0.0171(7) Uani 1 1 d D . . . .
H11A H 0.153476 0.571389 0.360211 0.021 Uiso 1 1 d DG U . . .
H11B H 0.215315 0.586817 0.286329 0.021 Uiso 1 1 d DG U . . .
O12 O 0.4370(2) 0.61446(15) 0.2980(2) 0.0147(6) Uani 1 1 d D . . . .
H12A H 0.510329 0.620148 0.282395 0.018 Uiso 1 1 d DG U . . .
H12B H 0.395040 0.650727 0.273568 0.018 Uiso 1 1 d DG U . . .
O13 O 0.5832(2) 0.60006(14) 0.4778(3) 0.0155(5) Uani 1 1 d D . . . .
H13A H 0.600743 0.605461 0.549856 0.019 Uiso 1 1 d DG U . . .
H13B H 0.632919 0.586662 0.426055 0.019 Uiso 1 1 d DG U . . .
C1 C 0.3868(3) 0.7074(2) 0.5693(3) 0.0123(8) Uani 1 1 d . . . . .
C2 C 0.3942(3) 0.7866(2) 0.5948(3) 0.0141(8) Uani 1 1 d . . . . .
C3 C 0.4622(4) 0.8311(2) 0.5296(3) 0.0196(9) Uani 1 1 d . . . . .
C4 C 0.4705(4) 0.9044(2) 0.5502(4) 0.0232(10) Uani 1 1 d . . . . .
C5 C 0.4063(4) 0.9341(2) 0.6359(4) 0.0245(10) Uani 1 1 d . . . . .
C6 C 0.3362(4) 0.8901(2) 0.7012(3) 0.0182(9) Uani 1 1 d . . . . .
C7 C 0.3331(3) 0.8162(2) 0.6830(3) 0.0134(8) Uani 1 1 d . . . . .
C8 C 0.2642(3) 0.7659(2) 0.7538(3) 0.0132(8) Uani 1 1 d . . . . .
C9 C 0.4048(3) 0.4224(2) 0.4047(3) 0.0116(8) Uani 1 1 d . . . . .
C10 C 0.3969(3) 0.3447(2) 0.3687(3) 0.0125(8) Uani 1 1 d . . . . .
C11 C 0.4524(3) 0.2897(2) 0.4229(3) 0.0133(8) Uani 1 1 d . . . . .
C12 C 0.4313(4) 0.2178(2) 0.3940(3) 0.0146(8) Uani 1 1 d . . . . .
C13 C 0.3577(4) 0.2025(2) 0.3076(3) 0.0163(8) Uani 1 1 d . . . . .
C14 C 0.3023(4) 0.2587(2) 0.2519(3) 0.0171(9) Uani 1 1 d . . . . .
C15 C 0.3205(3) 0.3293(2) 0.2830(3) 0.0123(8) Uani 1 1 d . . . . .
C16 C 0.2616(4) 0.3922(2) 0.2262(4) 0.0143(8) 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
Y1 O9 2.341(3) . ?
Y1 O13 2.349(2) . ?
Y1 O2 2.351(2) . ?
Y1 O12 2.353(3) . ?
Y1 O10 2.358(3) . ?
Y1 O5 2.376(3) . ?
Y1 O11 2.424(3) . ?
Y1 O6 2.558(3) . ?
Y1 O1 2.639(3) . ?
Y1 C9 2.827(4) . ?
Y1 C1 2.849(4) . ?
Cl1 C3 1.729(4) . ?
Cl2 C4 1.711(4) . ?
Cl3 C5 1.716(4) . ?
Cl4 C6 1.727(4) . ?
Cl5 C11 1.724(4) . ?
Cl6 C12 1.716(4) . ?
Cl7 C13 1.717(4) . ?
Cl8 C14 1.720(4) . ?
O1 C1 1.232(5) . ?
O2 C1 1.284(5) . ?
O3 C8 1.214(5) . ?
O4 C8 1.303(4) . ?
O5 C9 1.260(4) . ?
O6 C9 1.259(5) . ?
O7 C16 1.240(5) . ?
O8 C16 1.258(5) . ?
C1 C2 1.505(5) . ?
C2 C3 1.389(6) . ?
C2 C7 1.396(5) . ?
C3 C4 1.386(6) . ?
C4 C5 1.393(6) . ?
C5 C6 1.399(6) . ?
C6 C7 1.389(6) . ?
C7 C8 1.500(5) . ?
C9 C10 1.509(5) . ?
C10 C11 1.374(5) . ?
C10 C15 1.396(5) . ?
C11 C12 1.402(5) . ?
C12 C13 1.382(6) . ?
C13 C14 1.398(6) . ?
C14 C15 1.381(6) . ?
C15 C16 1.517(5) . ?

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
O9 Y1 O13 77.30(10) . . ?
O9 Y1 O2 122.06(10) . . ?
O13 Y1 O2 90.38(9) . . ?
O9 Y1 O12 145.04(10) . . ?
O13 Y1 O12 72.42(10) . . ?
O2 Y1 O12 75.69(10) . . ?
O9 Y1 O10 74.85(10) . . ?
O13 Y1 O10 138.83(11) . . ?
O2 Y1 O10 79.59(10) . . ?
O12 Y1 O10 140.11(10) . . ?
O9 Y1 O5 75.79(10) . . ?
O13 Y1 O5 125.33(9) . . ?
O2 Y1 O5 143.99(9) . . ?
O12 Y1 O5 108.21(10) . . ?
O10 Y1 O5 75.64(10) . . ?
O9 Y1 O11 141.90(10) . . ?
O13 Y1 O11 139.86(10) . . ?
O2 Y1 O11 75.35(10) . . ?
O12 Y1 O11 67.76(10) . . ?
O10 Y1 O11 76.02(9) . . ?
O5 Y1 O11 73.59(10) . . ?
O9 Y1 O6 75.83(10) . . ?
O13 Y1 O6 75.02(9) . . ?
O2 Y1 O6 154.34(9) . . ?
O12 Y1 O6 79.78(9) . . ?
O10 Y1 O6 125.15(10) . . ?
O5 Y1 O6 52.66(9) . . ?
O11 Y1 O6 102.20(10) . . ?
O9 Y1 O1 71.57(9) . . ?
O13 Y1 O1 67.11(10) . . ?
O2 Y1 O1 51.90(9) . . ?
O12 Y1 O1 110.81(10) . . ?
O10 Y1 O1 75.61(10) . . ?
O5 Y1 O1 140.95(9) . . ?
O11 Y1 O1 123.33(10) . . ?
O6 Y1 O1 134.16(9) . . ?
O9 Y1 C9 74.25(10) . . ?
O13 Y1 C9 100.41(10) . . ?
O2 Y1 C9 162.43(10) . . ?
O12 Y1 C9 94.27(10) . . ?
O10 Y1 C9 100.49(11) . . ?
O5 Y1 C9 26.24(10) . . ?
O11 Y1 C9 87.56(11) . . ?
O6 Y1 C9 26.43(10) . . ?
O1 Y1 C9 145.42(9) . . ?
O9 Y1 C1 96.86(11) . . ?
O13 Y1 C1 75.85(10) . . ?
O2 Y1 C1 26.44(10) . . ?
O12 Y1 C1 92.36(10) . . ?
O10 Y1 C1 78.05(11) . . ?
O5 Y1 C1 153.69(10) . . ?
O11 Y1 C1 100.58(11) . . ?
O6 Y1 C1 150.85(10) . . ?
O1 Y1 C1 25.59(10) . . ?
C9 Y1 C1 171.01(11) . . ?
C1 O1 Y1 86.8(2) . . ?
C1 O2 Y1 99.0(2) . . ?
C9 O5 Y1 97.3(2) . . ?
C9 O6 Y1 88.8(2) . . ?
O1 C1 O2 121.8(4) . . ?
O1 C1 C2 121.7(3) . . ?
O2 C1 C2 116.4(3) . . ?
O1 C1 Y1 67.6(2) . . ?
O2 C1 Y1 54.60(19) . . ?
C2 C1 Y1 166.8(3) . . ?
C3 C2 C7 119.5(4) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 120.8(3) . . ?
C2 C3 C4 121.2(4) . . ?
C2 C3 Cl1 119.5(3) . . ?
C4 C3 Cl1 119.3(3) . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 Cl2 120.8(3) . . ?
C5 C4 Cl2 120.1(3) . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 Cl3 119.9(3) . . ?
C6 C5 Cl3 119.9(3) . . ?
C7 C6 C5 120.0(4) . . ?
C7 C6 Cl4 121.1(3) . . ?
C5 C6 Cl4 118.8(3) . . ?
C6 C7 C2 119.8(4) . . ?
C6 C7 C8 122.4(4) . . ?
C2 C7 C8 117.8(4) . . ?
O3 C8 O4 125.3(4) . . ?
O3 C8 C7 121.7(3) . . ?
O4 C8 C7 113.0(3) . . ?
O6 C9 O5 121.2(3) . . ?
O6 C9 C10 122.5(3) . . ?
O5 C9 C10 116.2(3) . . ?
O6 C9 Y1 64.8(2) . . ?
O5 C9 Y1 56.47(19) . . ?
C10 C9 Y1 172.3(3) . . ?
C11 C10 C15 120.2(4) . . ?
C11 C10 C9 122.8(4) . . ?
C15 C10 C9 116.8(3) . . ?
C10 C11 C12 120.4(4) . . ?
C10 C11 Cl5 120.8(3) . . ?
C12 C11 Cl5 118.7(3) . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 Cl6 120.1(3) . . ?
C11 C12 Cl6 120.4(3) . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 Cl7 119.9(3) . . ?
C14 C13 Cl7 120.1(3) . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 Cl8 120.2(3) . . ?
C13 C14 Cl8 119.5(3) . . ?
C14 C15 C10 119.7(4) . . ?
C14 C15 C16 122.5(4) . . ?
C10 C15 C16 117.8(3) . . ?
O7 C16 O8 125.4(4) . . ?
O7 C16 C15 119.5(4) . . ?
O8 C16 C15 115.1(4) . . ?

_refine_diff_density_max         0.281
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.066



####################################################################### 
# 
# 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_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2118211'
loop_
_audit_author_name
_audit_author_address
'Carole Daiguebonne'
;INSA Rennes
France
;
_audit_update_record             
;
2024-10-28 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.53Ang From K1             -2.52 eA-3  
RESPONSE: Indeed there is a small residual density that is very near to a K ion.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H22 Cl8 K La O19'
_chemical_formula_weight         979.94

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.2758(3)
_cell_length_b                   13.9934(7)
_cell_length_c                   14.3376(6)
_cell_angle_alpha                85.9932(14)
_cell_angle_beta                 77.9272(12)
_cell_angle_gamma                75.6109(13)
_cell_volume                     1572.45(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7821
_cell_measurement_theta_min      2.6667
_cell_measurement_theta_max      27.4553

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.070
_exptl_crystal_F_000             964
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.250
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7136
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.110
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7136
_reflns_number_gt                6287
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0639P)²+3.1438P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7136
_refine_ls_number_parameters     472
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1196
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.022
_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 0.92265(3) 0.07300(2) 0.35521(2) 0.00951(9) Uani 1 1 d . . . . .
Cl1 Cl 1.01724(15) 0.29914(9) 0.55701(9) 0.0211(3) Uani 1 1 d . . . . .
Cl2 Cl 0.79186(19) 0.51439(9) 0.55778(10) 0.0282(3) Uani 1 1 d . . . . .
Cl3 Cl 0.40197(18) 0.55377(9) 0.63200(9) 0.0273(3) Uani 1 1 d . . . . .
Cl4 Cl 0.23450(15) 0.37978(10) 0.69747(10) 0.0275(3) Uani 1 1 d . . . . .
Cl5 Cl 0.92881(14) 0.34117(9) 0.08880(10) 0.0264(3) Uani 1 1 d . . . . .
Cl6 Cl 0.75962(16) 0.56106(9) 0.05278(9) 0.0231(3) Uani 1 1 d . . . . .
Cl7 Cl 0.36551(16) 0.63910(9) 0.11950(9) 0.0234(3) Uani 1 1 d . . . . .
Cl8 Cl 0.14294(14) 0.49019(9) 0.20428(9) 0.0217(3) Uani 1 1 d . . . . .
K1 K 0.6306(2) 0.07978(14) 0.00424(13) 0.0603(5) Uani 1 1 d . . . . .
O1 O 0.3445(4) 0.2430(3) 0.3088(2) 0.0203(7) Uani 1 1 d . . . . .
O2 O 0.2473(4) 0.2531(2) 0.1734(2) 0.0193(7) Uani 1 1 d . . . . .
O3 O 0.7761(4) 0.2006(2) 0.2487(2) 0.0156(7) Uani 1 1 d . . . . .
O4 O 0.6862(5) 0.1460(2) 0.1306(2) 0.0217(8) Uani 1 1 d . . . . .
O5 O 0.3814(4) 0.1644(3) 0.7587(2) 0.0206(7) Uani 1 1 d . . . . .
O6 O 0.5109(4) 0.1050(2) 0.6150(2) 0.0163(7) Uani 1 1 d . . . . .
O7 O 0.8603(4) 0.0926(2) 0.6872(2) 0.0149(7) Uani 1 1 d . . . . .
O8 O 0.8974(4) 0.0989(2) 0.5302(2) 0.0140(6) Uani 1 1 d . . . . .
O9 O 0.9593(4) 0.2532(3) 0.3555(2) 0.0183(7) Uani 1 1 d D . . . .
H9A H 0.932(6) 0.290(3) 0.310(3) 0.022 Uiso 1 1 d D U . . .
H9B H 1.044(5) 0.274(4) 0.361(4) 0.022 Uiso 1 1 d D U . . .
O10 O 0.6133(4) 0.1601(3) 0.4246(3) 0.0268(9) Uani 1 1 d D . . . .
H10A H 0.538(5) 0.194(4) 0.397(3) 0.032 Uiso 1 1 d D U . . .
H10B H 0.568(6) 0.153(4) 0.4809(17) 0.032 Uiso 1 1 d D U . . .
O11 O 0.7655(4) -0.0537(3) 0.4307(2) 0.0174(7) Uani 1 1 d D . . . .
H11A H 0.683(5) -0.069(4) 0.414(3) 0.021 Uiso 1 1 d D U . . .
H11B H 0.759(6) -0.074(4) 0.4872(18) 0.021 Uiso 1 1 d D U . . .
O12 O 1.2347(4) 0.0803(2) 0.3760(2) 0.0134(6) Uani 1 1 d D . . . .
H12A H 1.313(5) 0.031(2) 0.364(4) 0.016 Uiso 1 1 d D U . . .
H12B H 1.277(6) 0.127(2) 0.354(4) 0.016 Uiso 1 1 d D U . . .
O13 O 0.8130(4) -0.0099(3) 0.2364(2) 0.0184(7) Uani 1 1 d D . . . .
H13A H 0.750(6) 0.032(3) 0.209(4) 0.022 Uiso 1 1 d D U . . .
H13B H 0.762(6) -0.051(3) 0.264(4) 0.022 Uiso 1 1 d D U . . .
O14 O 1.1248(4) 0.0917(2) 0.1938(2) 0.0150(7) Uani 1 1 d D . . . .
H14A H 1.167(6) 0.141(3) 0.188(3) 0.018 Uiso 1 1 d D U . . .
H14B H 1.109(7) 0.087(4) 0.139(2) 0.018 Uiso 1 1 d D U . . .
OW1 O 0.8659(5) -0.0695(3) 0.0004(3) 0.0258(8) Uani 1 1 d D . . . .
H1A H 0.830(7) -0.120(3) 0.019(4) 0.031 Uiso 1 1 d D U . . .
H1B H 0.955(5) -0.081(4) 0.020(4) 0.031 Uiso 1 1 d D U . . .
OW2 O 0.5376(4) 0.0113(3) -0.1194(2) 0.0191(7) Uani 1 1 d D . . . .
H2A H 0.624(4) -0.017(3) -0.156(3) 0.023 Uiso 1 1 d D U . . .
H2B H 0.496(6) 0.057(3) -0.152(3) 0.023 Uiso 1 1 d D U . . .
OW3 O 0.8293(6) 0.1395(3) -0.1138(3) 0.0353(10) Uani 1 1 d D . . . .
H3A H 0.787(8) 0.196(2) -0.093(4) 0.042 Uiso 1 1 d D U . . .
H3B H 0.802(8) 0.138(4) -0.166(3) 0.042 Uiso 1 1 d D U . . .
OW4 O 1.0628(7) 0.2512(4) -0.1296(4) 0.0548(13) Uani 1 1 d D . . . .
H4A H 1.168(4) 0.232(5) -0.163(5) 0.066 Uiso 1 1 d D U . . .
H4B H 1.048(9) 0.312(2) -0.153(5) 0.066 Uiso 1 1 d D U . . .
OW5 O 0.3688(5) 0.1955(3) -0.0112(3) 0.0270(8) Uani 1 1 d D . . . .
H5A H 0.397(8) 0.238(3) -0.052(3) 0.032 Uiso 1 1 d D U . . .
H5B H 0.345(8) 0.223(4) 0.041(2) 0.032 Uiso 1 1 d D U . . .
C1 C 0.4381(6) 0.3505(3) 0.1847(3) 0.0127(9) Uani 1 1 d . . . . .
C2 C 0.6140(6) 0.3174(3) 0.1595(3) 0.0121(9) Uani 1 1 d . . . . .
C3 C 0.7116(6) 0.3837(4) 0.1192(3) 0.0153(9) Uani 1 1 d . . . . .
C4 C 0.6343(6) 0.4824(3) 0.1051(3) 0.0155(9) Uani 1 1 d . . . . .
C5 C 0.4589(6) 0.5163(3) 0.1321(3) 0.0141(9) Uani 1 1 d . . . . .
C6 C 0.3613(6) 0.4492(3) 0.1716(3) 0.0136(9) Uani 1 1 d . . . . .
C7 C 0.3347(6) 0.2761(3) 0.2269(3) 0.0148(9) Uani 1 1 d . . . . .
C8 C 0.6990(5) 0.2123(3) 0.1805(3) 0.0122(9) Uani 1 1 d . . . . .
C9 C 0.5495(6) 0.2580(3) 0.6525(3) 0.0134(9) Uani 1 1 d . . . . .
C10 C 0.7240(6) 0.2418(3) 0.6167(3) 0.0116(8) Uani 1 1 d . . . . .
C11 C 0.7989(6) 0.3209(4) 0.5912(3) 0.0159(9) Uani 1 1 d . . . . .
C12 C 0.7004(6) 0.4172(3) 0.5952(3) 0.0175(10) Uani 1 1 d . . . . .
C13 C 0.5260(6) 0.4346(3) 0.6287(3) 0.0176(10) Uani 1 1 d . . . . .
C14 C 0.4520(6) 0.3556(3) 0.6586(3) 0.0158(9) Uani 1 1 d . . . . .
C15 C 0.4720(6) 0.1700(3) 0.6800(3) 0.0148(9) Uani 1 1 d . . . . .
C16 C 0.8358(5) 0.1372(3) 0.6102(3) 0.0112(8) 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 O11 2.509(3) . ?
La1 O3 2.511(3) . ?
La1 O8 2.517(3) . ?
La1 O13 2.553(3) . ?
La1 O10 2.566(3) . ?
La1 O7 2.576(3) 2_756 ?
La1 O14 2.596(3) . ?
La1 O9 2.614(3) . ?
La1 O12 2.688(3) . ?
Cl1 C11 1.725(5) . ?
Cl2 C12 1.718(5) . ?
Cl3 C13 1.725(5) . ?
Cl4 C14 1.723(5) . ?
Cl5 C3 1.718(5) . ?
Cl6 C4 1.726(5) . ?
Cl7 C5 1.714(4) . ?
Cl8 C6 1.727(5) . ?
K1 O4 2.268(4) . ?
K1 OW3 2.364(5) . ?
K1 OW5 2.402(4) . ?
K1 OW2 2.414(4) . ?
K1 OW2 2.433(4) 2_655 ?
K1 OW1 2.471(4) . ?
K1 C8 3.452(5) . ?
K1 K1 3.496(4) 2_655 ?
K1 H1A 2.89(5) . ?
K1 H1B 3.08(4) . ?
K1 H2A 2.76(5) . ?
K1 H2B 2.77(5) . ?
K1 H3A 2.49(7) . ?
K1 H3B 2.73(6) . ?
K1 H5A 2.75(5) . ?
K1 H5B 2.67(6) . ?
O1 C7 1.243(6) . ?
O2 C7 1.264(6) . ?
O3 C8 1.256(5) . ?
O4 C8 1.248(5) . ?
O5 C15 1.226(6) . ?
O6 C15 1.284(6) . ?
O7 C16 1.259(5) . ?
O8 C16 1.252(5) . ?
O9 H9A 0.840(19) . ?
O9 H9B 0.839(19) . ?
O10 H10A 0.832(19) . ?
O10 H10B 0.826(19) . ?
O11 H11A 0.843(19) . ?
O11 H11B 0.835(19) . ?
O12 H12A 0.820(19) . ?
O12 H12B 0.827(19) . ?
O13 H13A 0.811(19) . ?
O13 H13B 0.826(19) . ?
O14 H14A 0.840(19) . ?
O14 H14B 0.838(19) . ?
OW1 H1A 0.843(19) . ?
OW1 H1B 0.819(19) . ?
OW2 H2A 0.823(19) . ?
OW2 H2B 0.818(19) . ?
OW3 H3A 0.828(19) . ?
OW3 H3B 0.823(19) . ?
OW4 H4A 0.89(2) . ?
OW4 H4B 0.88(2) . ?
OW5 H5A 0.839(19) . ?
OW5 H5B 0.825(19) . ?
C1 C6 1.387(6) . ?
C1 C2 1.390(6) . ?
C1 C7 1.523(6) . ?
C2 C3 1.395(6) . ?
C2 C8 1.505(6) . ?
C3 C4 1.391(6) . ?
C4 C5 1.389(6) . ?
C5 C6 1.403(6) . ?
C9 C10 1.394(6) . ?
C9 C14 1.401(6) . ?
C9 C15 1.518(6) . ?
C10 C11 1.391(6) . ?
C10 C16 1.522(6) . ?
C11 C12 1.388(7) . ?
C12 C13 1.387(7) . ?
C13 C14 1.394(7) . ?

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
O11 La1 O3 116.58(10) . . ?
O11 La1 O8 78.05(11) . . ?
O3 La1 O8 122.83(10) . . ?
O11 La1 O13 66.55(11) . . ?
O3 La1 O13 69.83(10) . . ?
O8 La1 O13 143.60(11) . . ?
O11 La1 O10 70.96(12) . . ?
O3 La1 O10 64.09(11) . . ?
O8 La1 O10 71.67(11) . . ?
O13 La1 O10 88.47(12) . . ?
O11 La1 O7 76.19(11) . 2_756 ?
O3 La1 O7 129.77(10) . 2_756 ?
O8 La1 O7 107.14(10) . 2_756 ?
O13 La1 O7 73.21(10) . 2_756 ?
O10 La1 O7 146.67(12) . 2_756 ?
O11 La1 O14 135.61(11) . . ?
O3 La1 O14 68.64(10) . . ?
O8 La1 O14 139.34(10) . . ?
O13 La1 O14 76.22(11) . . ?
O10 La1 O14 132.72(11) . . ?
O7 La1 O14 70.44(10) 2_756 . ?
O11 La1 O9 147.82(11) . . ?
O3 La1 O9 61.47(10) . . ?
O8 La1 O9 78.08(10) . . ?
O13 La1 O9 129.83(10) . . ?
O10 La1 O9 81.22(12) . . ?
O7 La1 O9 131.87(11) 2_756 . ?
O14 La1 O9 75.71(11) . . ?
O11 La1 O12 125.46(10) . . ?
O3 La1 O12 117.95(10) . . ?
O8 La1 O12 74.23(10) . . ?
O13 La1 O12 133.80(11) . . ?
O10 La1 O12 137.23(12) . . ?
O7 La1 O12 68.75(10) 2_756 . ?
O14 La1 O12 67.14(10) . . ?
O9 La1 O12 67.03(10) . . ?
O4 K1 OW3 96.48(16) . . ?
O4 K1 OW5 99.11(14) . . ?
OW3 K1 OW5 101.57(16) . . ?
O4 K1 OW2 173.22(16) . . ?
OW3 K1 OW2 89.43(15) . . ?
OW5 K1 OW2 76.36(13) . . ?
O4 K1 OW2 87.07(14) . 2_655 ?
OW3 K1 OW2 169.38(16) . 2_655 ?
OW5 K1 OW2 87.69(14) . 2_655 ?
OW2 K1 OW2 87.69(13) . 2_655 ?
O4 K1 OW1 94.75(14) . . ?
OW3 K1 OW1 83.74(15) . . ?
OW5 K1 OW1 164.45(16) . . ?
OW2 K1 OW1 89.18(13) . . ?
OW2 K1 OW1 86.00(14) 2_655 . ?
O4 K1 C8 8.09(11) . . ?
OW3 K1 C8 92.29(14) . . ?
OW5 K1 C8 93.23(13) . . ?
OW2 K1 C8 169.59(13) . . ?
OW2 K1 C8 92.38(12) 2_655 . ?
OW1 K1 C8 101.22(12) . . ?
O4 K1 K1 130.57(14) . 2_655 ?
OW3 K1 K1 132.62(14) . 2_655 ?
OW5 K1 K1 78.99(12) . 2_655 ?
OW2 K1 K1 44.05(9) . 2_655 ?
OW2 K1 K1 43.64(9) 2_655 2_655 ?
OW1 K1 K1 86.65(12) . 2_655 ?
C8 K1 K1 135.09(11) . 2_655 ?
O4 K1 H1A 99.6(11) . . ?
OW3 K1 H1A 98.0(9) . . ?
OW5 K1 H1A 151.1(7) . . ?
OW2 K1 H1A 82.8(11) . . ?
OW2 K1 H1A 71.5(9) 2_655 . ?
OW1 K1 H1A 15.7(7) . . ?
C8 K1 H1A 107.1(11) . . ?
K1 K1 H1A 72.1(7) 2_655 . ?
O4 K1 H1B 84.2(10) . . ?
OW3 K1 H1B 80.6(10) . . ?
OW5 K1 H1B 175.8(8) . . ?
OW2 K1 H1B 100.1(9) . . ?
OW2 K1 H1B 89.9(10) 2_655 . ?
OW1 K1 H1B 11.4(9) . . ?
C8 K1 H1B 90.3(9) . . ?
K1 K1 H1B 96.9(8) 2_655 . ?
H1A K1 H1B 24.8(6) . . ?
O4 K1 H2A 169.7(7) . . ?
OW3 K1 H2A 78.0(10) . . ?
OW5 K1 H2A 90.5(7) . . ?
OW2 K1 H2A 16.6(7) . . ?
OW2 K1 H2A 96.9(10) 2_655 . ?
OW1 K1 H2A 76.2(8) . . ?
C8 K1 H2A 170.1(9) . . ?
K1 K1 H2A 54.7(10) 2_655 . ?
H1A K1 H2A 72.9(14) . . ?
H1B K1 H2A 86.4(12) . . ?
O4 K1 H2B 162.0(7) . . ?
OW3 K1 H2B 82.3(11) . . ?
OW5 K1 H2B 63.8(8) . . ?
OW2 K1 H2B 16.4(7) . . ?
OW2 K1 H2B 97.4(10) 2_655 . ?
OW1 K1 H2B 102.9(7) . . ?
C8 K1 H2B 154.5(7) . . ?
K1 K1 H2B 55.0(10) 2_655 . ?
H1A K1 H2B 98.3(13) . . ?
H1B K1 H2B 113.2(13) . . ?
H2A K1 H2B 26.8(7) . . ?
O4 K1 H3A 84.6(10) . . ?
OW3 K1 H3A 19.4(6) . . ?
OW5 K1 H3A 88.4(11) . . ?
OW2 K1 H3A 100.2(11) . . ?
OW2 K1 H3A 170.1(7) 2_655 . ?
OW1 K1 H3A 100.0(10) . . ?
C8 K1 H3A 78.8(10) . . ?
K1 K1 H3A 143.8(12) 2_655 . ?
H1A K1 H3A 115.1(12) . . ?
H1B K1 H3A 94.6(14) . . ?
H2A K1 H3A 92.2(14) . . ?
H2B K1 H3A 89.0(15) . . ?
O4 K1 H3B 112.1(9) . . ?
OW3 K1 H3B 16.7(9) . . ?
OW5 K1 H3B 92.8(12) . . ?
OW2 K1 H3B 73.5(9) . . ?
OW2 K1 H3B 160.4(10) 2_655 . ?
OW1 K1 H3B 88.4(12) . . ?
C8 K1 H3B 107.1(9) . . ?
K1 K1 H3B 117.3(9) 2_655 . ?
H1A K1 H3B 100.2(16) . . ?
H1B K1 H3B 88.3(16) . . ?
H2A K1 H3B 63.5(14) . . ?
H2B K1 H3B 65.7(14) . . ?
H3A K1 H3B 29.0(9) . . ?
O4 K1 H5A 99.9(11) . . ?
OW3 K1 H5A 84.5(8) . . ?
OW5 K1 H5A 17.1(8) . . ?
OW2 K1 H5A 77.3(11) . . ?
OW2 K1 H5A 104.8(8) 2_655 . ?
OW1 K1 H5A 162.1(10) . . ?
C8 K1 H5A 92.6(11) . . ?
K1 K1 H5A 91.5(10) 2_655 . ?
H1A K1 H5A 159.9(15) . . ?
H1B K1 H5A 164.9(13) . . ?
H2A K1 H5A 88.3(14) . . ?
H2B K1 H5A 62.1(13) . . ?
H3A K1 H5A 71.5(14) . . ?
H3B K1 H5A 76.6(14) . . ?
O4 K1 H5B 82.0(8) . . ?
OW3 K1 H5B 108.1(11) . . ?
OW5 K1 H5B 17.7(7) . . ?
OW2 K1 H5B 93.0(8) . . ?
OW2 K1 H5B 82.2(11) 2_655 . ?
OW1 K1 H5B 167.9(10) . . ?
C8 K1 H5B 76.7(9) . . ?
K1 K1 H5B 86.7(12) 2_655 . ?
H1A K1 H5B 153.6(14) . . ?
H1B K1 H5B 164.4(13) . . ?
H2A K1 H5B 107.8(11) . . ?
H2B K1 H5B 81.3(11) . . ?
H3A K1 H5B 91.3(15) . . ?
H3B K1 H5B 103.6(15) . . ?
H5A K1 H5B 28.3(8) . . ?
C8 O3 La1 143.6(3) . . ?
C8 O4 K1 157.1(3) . . ?
C16 O7 La1 107.6(3) . 2_756 ?
C16 O8 La1 157.4(3) . . ?
La1 O9 H9A 116(4) . . ?
La1 O9 H9B 130(4) . . ?
H9A O9 H9B 98(3) . . ?
La1 O10 H10A 130(4) . . ?
La1 O10 H10B 123(4) . . ?
H10A O10 H10B 107(4) . . ?
La1 O11 H11A 128(3) . . ?
La1 O11 H11B 125(3) . . ?
H11A O11 H11B 103(3) . . ?
La1 O12 H12A 119(4) . . ?
La1 O12 H12B 122(3) . . ?
H12A O12 H12B 105(3) . . ?
La1 O13 H13A 110(4) . . ?
La1 O13 H13B 111(4) . . ?
H13A O13 H13B 110(4) . . ?
La1 O14 H14A 116(3) . . ?
La1 O14 H14B 128(3) . . ?
H14A O14 H14B 102(3) . . ?
K1 OW1 H1A 112(4) . . ?
K1 OW1 H1B 132(4) . . ?
H1A OW1 H1B 102(3) . . ?
K1 OW2 K1 92.31(13) . 2_655 ?
K1 OW2 H2A 107(4) . . ?
K1 OW2 H2A 121(4) 2_655 . ?
K1 OW2 H2B 107(4) . . ?
K1 OW2 H2B 124(4) 2_655 . ?
H2A OW2 H2B 103(3) . . ?
K1 OW3 H3A 89(5) . . ?
K1 OW3 H3B 108(5) . . ?
H3A OW3 H3B 107(4) . . ?
H4A OW4 H4B 94(3) . . ?
K1 OW5 H5A 105(4) . . ?
K1 OW5 H5B 100(4) . . ?
H5A OW5 H5B 106(4) . . ?
C6 C1 C2 119.9(4) . . ?
C6 C1 C7 121.8(4) . . ?
C2 C1 C7 118.3(4) . . ?
C1 C2 C3 119.5(4) . . ?
C1 C2 C8 120.1(4) . . ?
C3 C2 C8 120.3(4) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 Cl5 120.8(4) . . ?
C2 C3 Cl5 118.7(4) . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 Cl6 120.9(4) . . ?
C3 C4 Cl6 118.8(4) . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 Cl7 120.0(4) . . ?
C6 C5 Cl7 121.0(3) . . ?
C1 C6 C5 120.8(4) . . ?
C1 C6 Cl8 119.8(4) . . ?
C5 C6 Cl8 119.5(3) . . ?
O1 C7 O2 126.1(4) . . ?
O1 C7 C1 118.2(4) . . ?
O2 C7 C1 115.7(4) . . ?
O4 C8 O3 126.4(4) . . ?
O4 C8 C2 118.4(4) . . ?
O3 C8 C2 115.1(4) . . ?
O4 C8 K1 14.8(2) . . ?
O3 C8 K1 140.6(3) . . ?
C2 C8 K1 104.1(3) . . ?
C10 C9 C14 118.2(4) . . ?
C10 C9 C15 119.1(4) . . ?
C14 C9 C15 122.7(4) . . ?
C11 C10 C9 120.5(4) . . ?
C11 C10 C16 119.3(4) . . ?
C9 C10 C16 120.1(4) . . ?
C10 C11 C12 120.8(4) . . ?
C10 C11 Cl1 119.5(4) . . ?
C12 C11 Cl1 119.7(4) . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 Cl2 119.8(4) . . ?
C11 C12 Cl2 120.7(4) . . ?
C12 C13 C14 119.7(4) . . ?
C12 C13 Cl3 119.8(4) . . ?
C14 C13 Cl3 120.4(4) . . ?
C13 C14 C9 121.3(4) . . ?
C13 C14 Cl4 118.5(3) . . ?
C9 C14 Cl4 120.2(4) . . ?
O5 C15 O6 125.1(4) . . ?
O5 C15 C9 120.7(4) . . ?
O6 C15 C9 114.2(4) . . ?
O8 C16 O7 122.9(4) . . ?
O8 C16 C10 119.7(4) . . ?
O7 C16 C10 117.4(4) . . ?

_refine_diff_density_max         0.894
_refine_diff_density_min         -2.520
_refine_diff_density_rms         0.173



