# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

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

data_Compound_Tb-L
_database_code_depnum_ccdc_archive 'CCDC 1981571'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-k2O,O':k2O'',O''')diaquaditerbium(III)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 O20 Tb2, 4(H2 O)'
_chemical_formula_sum            'C12 H24 O24 Tb2'
_chemical_formula_weight         870.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   6.0149(3)
_cell_length_b                   7.3897(5)
_cell_length_c                   13.2793(7)
_cell_angle_alpha                102.177(6)
_cell_angle_beta                 101.709(5)
_cell_angle_gamma                90.413(5)
_cell_volume                     564.18(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2985
_cell_measurement_theta_min      2.8840
_cell_measurement_theta_max      27.3970

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6052 2936 572 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3948 2917 572 nmt -0.9997 -0.0001 0.0000 -0.0185 0.9601 -0.0795 0.0097
-0.9788 -0.9601


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.561
_exptl_crystal_F_000             418
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    6.334
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_T_max  2.439
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω
_diffrn_reflns_number            4840
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.824
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.626
_diffrn_reflns_point_group_measured_fraction_full 0.629
_reflns_number_total             4840
_reflns_number_gt                4732
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.263
_reflns_Friedel_fraction_max     0.261
_reflns_Friedel_fraction_full    0.264

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0823P)²+0.2908P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.025(14)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         4840
_refine_ls_number_parameters     324
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1015
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.006
_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 0.02162(6) 0.81663(6) 0.67891(4) 0.0087(2) Uani 1 1 d . . . . .
Tb2 Tb -0.02193(7) 0.18364(6) 0.32150(4) 0.0094(2) Uani 1 1 d . . . . .
C1A C 0.222(3) 0.930(3) 0.8959(14) 0.007(4) Uani 1 1 d . U . . .
C2A C 0.378(3) 1.028(2) 0.9993(11) 0.009(3) Uani 1 1 d . U . . .
H2A H 0.365154 0.959307 1.053688 0.011 Uiso 1 1 calc R U . . .
C3A C 0.623(3) 1.027(2) 0.9854(12) 0.011(3) Uani 1 1 d . U . . .
H3A H 0.655819 0.897745 0.958888 0.013 Uiso 1 1 calc R U . . .
C4A C 0.782(4) 1.096(3) 1.0938(17) 0.019(5) Uani 1 1 d . . . . .
C1B C 0.160(3) 0.391(2) 0.5684(12) 0.012(3) Uani 1 1 d . . . . .
C2B C 0.346(3) 0.245(3) 0.5632(13) 0.014(4) Uani 1 1 d . . . . .
H2B H 0.488058 0.307555 0.560442 0.017 Uiso 1 1 calc R U . . .
C3B C 0.381(2) 0.178(2) 0.6673(10) 0.007(3) Uani 1 1 d . U . . .
H3B H 0.465517 0.276166 0.724393 0.008 Uiso 1 1 calc R U . . .
C4B C 0.513(3) 0.001(2) 0.6621(11) 0.010(3) Uani 1 1 d . U . . .
C1C C -0.155(3) 0.835(2) 0.4333(12) 0.014(3) Uani 1 1 d . . . . .
C2C C -0.341(3) 0.697(2) 0.4350(13) 0.007(4) Uani 1 1 d . U . . .
H2C H -0.481429 0.762108 0.437949 0.008 Uiso 1 1 calc R U . . .
C3C C -0.378(3) 0.548(2) 0.3312(12) 0.013(3) Uani 1 1 d . . . . .
H3C H -0.465179 0.602024 0.275033 0.015 Uiso 1 1 calc R U . . .
C4C C -0.511(3) 0.378(2) 0.3360(11) 0.012(3) Uani 1 1 d . . . . .
O11A O 0.2648(19) 0.7764(16) 0.8490(8) 0.016(2) Uani 1 1 d . . . . .
O12A O 0.0480(19) 1.0124(16) 0.8573(8) 0.014(2) Uani 1 1 d . . . . .
O21A O 0.3251(18) 1.2141(15) 1.0344(8) 0.014(2) Uani 1 1 d . . . . .
O31A O 0.6504(18) 1.1276(16) 0.9096(8) 0.014(2) Uani 1 1 d . . . . .
O41A O 0.753(2) 1.0041(16) 1.1634(8) 0.015(2) Uani 1 1 d . . . . .
O42A O 0.9242(19) 1.2255(17) 1.1137(9) 0.018(3) Uani 1 1 d . . . . .
O12B O 0.1839(18) 0.5232(15) 0.6431(9) 0.011(2) Uani 1 1 d . . . . .
O11B O -0.0122(19) 0.3546(16) 0.4929(9) 0.014(2) Uani 1 1 d . . . . .
O21B O 0.2841(18) 0.1050(14) 0.4720(8) 0.010(2) Uani 1 1 d . . . . .
O31B O 0.1661(18) 0.1388(15) 0.6903(9) 0.010(2) Uani 1 1 d . . . . .
O41B O 0.408(2) -0.1426(17) 0.6673(8) 0.016(2) Uani 1 1 d . U . . .
O42B O 0.7174(18) 0.0126(15) 0.6555(8) 0.012(2) Uani 1 1 d . . . . .
O11C O 0.0250(19) 0.8551(15) 0.5070(8) 0.013(2) Uani 1 1 d . . . . .
O12C O -0.1795(19) 0.9150(16) 0.3594(9) 0.012(2) Uani 1 1 d . . . . .
O21C O -0.2804(18) 0.6199(15) 0.5272(8) 0.013(2) Uani 1 1 d . . . . .
O31C O -0.1688(18) 0.4942(15) 0.3032(8) 0.011(2) Uani 1 1 d . . . . .
O41C O -0.4100(18) 0.2266(16) 0.3332(8) 0.011(2) Uani 1 1 d . U . . .
O42C O -0.7212(18) 0.3933(15) 0.3361(8) 0.012(2) Uani 1 1 d . U . . .
O1W O -0.2485(19) 0.6525(17) 0.7430(8) 0.018(2) Uani 1 1 d . . . . .
O2W O 0.2337(19) -0.0276(16) 0.2496(9) 0.018(2) Uani 1 1 d . . . . .
O3W O 0.194(2) 0.4083(16) 0.8683(8) 0.017(2) Uiso 1 1 d . . . . .
O4W O -0.296(2) 0.6256(18) 0.1242(9) 0.025(3) Uiso 1 1 d . . . . .
O5W O 0.227(2) -0.3614(19) 0.1148(10) 0.029(3) Uiso 1 1 d . . . . .
O6W O -0.226(2) 0.4996(16) 0.9224(8) 0.018(2) Uiso 1 1 d . . . . .
H21A H 0.209945 1.229278 1.060705 0.027 Uiso 1 1 d . U . . .
H31A H 0.782554 1.089411 0.903780 0.027 Uiso 1 1 d . U . . .
H21B H 0.199808 0.009062 0.474984 0.027 Uiso 1 1 d . U . . .
H31B H 0.145772 0.223299 0.741331 0.027 Uiso 1 1 d . U . . .
H21C H -0.204220 0.524486 0.520618 0.027 Uiso 1 1 d . U . . .
H31C H -0.160249 0.523445 0.246945 0.027 Uiso 1 1 d . U . . .
H11W H -0.257868 0.617374 0.794977 0.027 Uiso 1 1 d . U . . .
H12W H -0.366874 0.707338 0.721958 0.027 Uiso 1 1 d . U . . .
H21W H 0.248681 -0.121038 0.205550 0.027 Uiso 1 1 d . U . . .
H22W H 0.363527 0.028031 0.277494 0.027 Uiso 1 1 d . U . . .
H31W H 0.250195 0.382133 0.926350 0.027 Uiso 1 1 d . U . . .
H32W H 0.239496 0.524734 0.875053 0.027 Uiso 1 1 d . U . . .
H41W H -0.286849 0.749031 0.138282 0.027 Uiso 1 1 d . U . . .
H42W H -0.267328 0.596812 0.064376 0.027 Uiso 1 1 d . U . . .
H51W H 0.366358 -0.373141 0.120997 0.027 Uiso 1 1 d . U . . .
H52W H 0.108970 -0.409198 0.067232 0.027 Uiso 1 1 d . U . . .
H61W H -0.290476 0.396657 0.919605 0.027 Uiso 1 1 d . U . . .
H62W H -0.093257 0.470815 0.909758 0.027 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O42B 2.353(11) 1_465 ?
Tb1 O11C 2.363(10) . ?
Tb1 O41B 2.378(12) 1_565 ?
Tb1 O12B 2.380(11) . ?
Tb1 O1W 2.409(11) . ?
Tb1 O12A 2.475(11) . ?
Tb1 O31B 2.492(11) 1_565 ?
Tb1 O11A 2.505(10) . ?
Tb1 O21C 2.591(10) . ?
Tb1 C1A 2.831(18) . ?
Tb2 O42C 2.324(11) 1_655 ?
Tb2 O11B 2.347(11) . ?
Tb2 O41A 2.377(10) 1_444 ?
Tb2 O12C 2.384(11) 1_545 ?
Tb2 O41C 2.390(11) . ?
Tb2 O2W 2.390(12) . ?
Tb2 O31C 2.507(10) . ?
Tb2 O21B 2.595(10) . ?
Tb2 O42A 2.796(11) 1_444 ?
Tb2 C4A 2.94(2) 1_444 ?
C1A O11A 1.23(2) . ?
C1A O12A 1.28(2) . ?
C1A C2A 1.53(2) . ?
C2A O21A 1.417(19) . ?
C2A C3A 1.520(18) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.41(2) . ?
C3A C4A 1.54(3) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.23(3) . ?
C4A O41A 1.29(2) . ?
C1B O12B 1.22(2) . ?
C1B O11B 1.269(19) . ?
C1B C2B 1.57(2) . ?
C2B O21B 1.40(2) . ?
C2B C3B 1.54(2) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.431(18) . ?
C3B C4B 1.53(2) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.25(2) . ?
C4B O42B 1.254(19) . ?
C1C O12C 1.23(2) . ?
C1C O11C 1.287(19) . ?
C1C C2C 1.51(2) . ?
C2C O21C 1.440(19) . ?
C2C C3C 1.55(2) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.420(19) . ?
C3C C4C 1.50(2) . ?
C3C H3C 0.9800 . ?
C4C O42C 1.27(2) . ?
C4C O41C 1.28(2) . ?
O21A H21A 0.8350 . ?
O31A H31A 0.8581 . ?
O21B H21B 0.8808 . ?
O31B H31B 0.8487 . ?
O21C H21C 0.8421 . ?
O31C H31C 0.8315 . ?
O1W H11W 0.7983 . ?
O1W H12W 0.8488 . ?
O2W H21W 0.8245 . ?
O2W H22W 0.8538 . ?
O3W H31W 0.8389 . ?
O3W H32W 0.8827 . ?
O4W H41W 0.8902 . ?
O4W H42W 0.8315 . ?
O5W H51W 0.8318 . ?
O5W H52W 0.8654 . ?
O6W H61W 0.8431 . ?
O6W H62W 0.8653 . ?

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
O42B Tb1 O11C 80.1(4) 1_465 . ?
O42B Tb1 O41B 130.4(4) 1_465 1_565 ?
O11C Tb1 O41B 72.3(4) . 1_565 ?
O42B Tb1 O12B 151.6(4) 1_465 . ?
O11C Tb1 O12B 90.8(4) . . ?
O41B Tb1 O12B 70.0(4) 1_565 . ?
O42B Tb1 O1W 81.6(4) 1_465 . ?
O11C Tb1 O1W 130.7(4) . . ?
O41B Tb1 O1W 146.7(4) 1_565 . ?
O12B Tb1 O1W 84.3(4) . . ?
O42B Tb1 O12A 76.6(4) 1_465 . ?
O11C Tb1 O12A 138.4(4) . . ?
O41B Tb1 O12A 97.8(4) 1_565 . ?
O12B Tb1 O12A 124.6(4) . . ?
O1W Tb1 O12A 79.2(4) . . ?
O42B Tb1 O31B 69.5(4) 1_465 1_565 ?
O11C Tb1 O31B 71.3(4) . 1_565 ?
O41B Tb1 O31B 63.0(4) 1_565 1_565 ?
O12B Tb1 O31B 132.8(4) . 1_565 ?
O1W Tb1 O31B 140.4(4) . 1_565 ?
O12A Tb1 O31B 68.4(4) . 1_565 ?
O42B Tb1 O11A 127.7(4) 1_465 . ?
O11C Tb1 O11A 144.6(4) . . ?
O41B Tb1 O11A 72.5(4) 1_565 . ?
O12B Tb1 O11A 73.2(4) . . ?
O1W Tb1 O11A 80.1(4) . . ?
O12A Tb1 O11A 52.0(4) . . ?
O31B Tb1 O11A 96.3(4) 1_565 . ?
O42B Tb1 O21C 75.7(4) 1_465 . ?
O11C Tb1 O21C 63.4(4) . . ?
O41B Tb1 O21C 122.9(4) 1_565 . ?
O12B Tb1 O21C 76.2(3) . . ?
O1W Tb1 O21C 67.8(4) . . ?
O12A Tb1 O21C 139.3(4) . . ?
O31B Tb1 O21C 126.4(3) 1_565 . ?
O11A Tb1 O21C 137.2(3) . . ?
O42B Tb1 C1A 103.5(5) 1_465 . ?
O11C Tb1 C1A 145.9(5) . . ?
O41B Tb1 C1A 80.5(5) 1_565 . ?
O12B Tb1 C1A 99.0(5) . . ?
O1W Tb1 C1A 83.0(5) . . ?
O12A Tb1 C1A 26.9(5) . . ?
O31B Tb1 C1A 78.2(5) 1_565 . ?
O11A Tb1 C1A 25.8(5) . . ?
O21C Tb1 C1A 150.7(5) . . ?
O42C Tb2 O11B 81.0(4) 1_655 . ?
O42C Tb2 O41A 126.9(4) 1_655 1_444 ?
O11B Tb2 O41A 146.9(4) . 1_444 ?
O42C Tb2 O12C 151.9(4) 1_655 1_545 ?
O11B Tb2 O12C 91.6(4) . 1_545 ?
O41A Tb2 O12C 71.2(4) 1_444 1_545 ?
O42C Tb2 O41C 131.9(4) 1_655 . ?
O11B Tb2 O41C 74.3(4) . . ?
O41A Tb2 O41C 73.3(4) 1_444 . ?
O12C Tb2 O41C 70.2(4) 1_545 . ?
O42C Tb2 O2W 81.2(4) 1_655 . ?
O11B Tb2 O2W 132.1(4) . . ?
O41A Tb2 O2W 75.5(4) 1_444 . ?
O12C Tb2 O2W 84.0(4) 1_545 . ?
O41C Tb2 O2W 144.5(4) . . ?
O42C Tb2 O31C 69.9(4) 1_655 . ?
O11B Tb2 O31C 73.4(4) . . ?
O41A Tb2 O31C 97.9(4) 1_444 . ?
O12C Tb2 O31C 133.8(4) 1_545 . ?
O41C Tb2 O31C 63.8(4) . . ?
O2W Tb2 O31C 138.1(4) . . ?
O42C Tb2 O21B 76.9(3) 1_655 . ?
O11B Tb2 O21B 62.9(3) . . ?
O41A Tb2 O21B 133.9(4) 1_444 . ?
O12C Tb2 O21B 75.6(3) 1_545 . ?
O41C Tb2 O21B 123.4(3) . . ?
O2W Tb2 O21B 69.9(4) . . ?
O31C Tb2 O21B 128.3(3) . . ?
O42C Tb2 O42A 78.7(3) 1_655 1_444 ?
O11B Tb2 O42A 141.5(4) . 1_444 ?
O41A Tb2 O42A 49.8(4) 1_444 1_444 ?
O12C Tb2 O42A 120.5(4) 1_545 1_444 ?
O41C Tb2 O42A 95.9(3) . 1_444 ?
O2W Tb2 O42A 76.2(4) . 1_444 ?
O31C Tb2 O42A 69.0(4) . 1_444 ?
O21B Tb2 O42A 140.6(3) . 1_444 ?
O42C Tb2 C4A 102.9(5) 1_655 1_444 ?
O11B Tb2 C4A 151.3(5) . 1_444 ?
O41A Tb2 C4A 25.4(5) 1_444 1_444 ?
O12C Tb2 C4A 96.5(5) 1_545 1_444 ?
O41C Tb2 C4A 82.7(5) . 1_444 ?
O2W Tb2 C4A 76.2(5) . 1_444 ?
O31C Tb2 C4A 81.2(5) . 1_444 ?
O21B Tb2 C4A 145.8(5) . 1_444 ?
O42A Tb2 C4A 24.5(5) 1_444 1_444 ?
O11A C1A O12A 120.4(16) . . ?
O11A C1A C2A 120.4(16) . . ?
O12A C1A C2A 119.2(15) . . ?
O11A C1A Tb1 62.2(9) . . ?
O12A C1A Tb1 60.9(8) . . ?
C2A C1A Tb1 162.0(13) . . ?
O21A C2A C3A 108.4(14) . . ?
O21A C2A C1A 113.2(13) . . ?
C3A C2A C1A 109.4(12) . . ?
O21A C2A H2A 108.6 . . ?
C3A C2A H2A 108.6 . . ?
C1A C2A H2A 108.6 . . ?
O31A C3A C2A 110.5(14) . . ?
O31A C3A C4A 114.1(15) . . ?
C2A C3A C4A 109.1(13) . . ?
O31A C3A H3A 107.6 . . ?
C2A C3A H3A 107.6 . . ?
C4A C3A H3A 107.6 . . ?
O42A C4A O41A 122.5(18) . . ?
O42A C4A C3A 124.0(18) . . ?
O41A C4A C3A 113.5(18) . . ?
O42A C4A Tb2 71.0(11) . 1_666 ?
O41A C4A Tb2 52.0(9) . 1_666 ?
C3A C4A Tb2 163.4(14) . 1_666 ?
O12B C1B O11B 125.7(15) . . ?
O12B C1B C2B 119.9(13) . . ?
O11B C1B C2B 114.4(13) . . ?
O21B C2B C3B 115.1(15) . . ?
O21B C2B C1B 110.6(13) . . ?
C3B C2B C1B 106.3(13) . . ?
O21B C2B H2B 108.2 . . ?
C3B C2B H2B 108.2 . . ?
C1B C2B H2B 108.2 . . ?
O31B C3B C4B 107.5(11) . . ?
O31B C3B C2B 110.0(12) . . ?
C4B C3B C2B 111.8(12) . . ?
O31B C3B H3B 109.2 . . ?
C4B C3B H3B 109.2 . . ?
C2B C3B H3B 109.2 . . ?
O41B C4B O42B 125.7(14) . . ?
O41B C4B C3B 116.8(13) . . ?
O42B C4B C3B 117.4(13) . . ?
O12C C1C O11C 123.9(16) . . ?
O12C C1C C2C 118.5(14) . . ?
O11C C1C C2C 117.5(14) . . ?
O21C C2C C1C 110.0(13) . . ?
O21C C2C C3C 112.8(14) . . ?
C1C C2C C3C 108.2(13) . . ?
O21C C2C H2C 108.6 . . ?
C1C C2C H2C 108.6 . . ?
C3C C2C H2C 108.6 . . ?
O31C C3C C4C 109.1(12) . . ?
O31C C3C C2C 111.6(13) . . ?
C4C C3C C2C 112.6(13) . . ?
O31C C3C H3C 107.8 . . ?
C4C C3C H3C 107.8 . . ?
C2C C3C H3C 107.8 . . ?
O42C C4C O41C 124.4(14) . . ?
O42C C4C C3C 117.4(14) . . ?
O41C C4C C3C 118.1(14) . . ?
C1A O11A Tb1 92.0(10) . . ?
C1A O12A Tb1 92.2(10) . . ?
C2A O21A H21A 116.1 . . ?
C3A O31A H31A 95.4 . . ?
C4A O41A Tb2 102.6(12) . 1_666 ?
C4A O42A Tb2 84.5(11) . 1_666 ?
C1B O12B Tb1 135.7(10) . . ?
C1B O11B Tb2 126.9(10) . . ?
C2B O21B Tb2 116.2(10) . . ?
C2B O21B H21B 117.8 . . ?
Tb2 O21B H21B 91.5 . . ?
C3B O31B Tb1 122.4(8) . 1_545 ?
C3B O31B H31B 108.0 . . ?
Tb1 O31B H31B 118.4 1_545 . ?
C4B O41B Tb1 129.0(10) . 1_545 ?
C4B O42B Tb1 133.5(10) . 1_645 ?
C1C O11C Tb1 123.2(10) . . ?
C1C O12C Tb2 137.6(11) . 1_565 ?
C2C O21C Tb1 114.8(9) . . ?
C2C O21C H21C 115.9 . . ?
Tb1 O21C H21C 95.1 . . ?
C3C O31C Tb2 120.4(9) . . ?
C3C O31C H31C 110.0 . . ?
Tb2 O31C H31C 114.8 . . ?
C4C O41C Tb2 126.2(10) . . ?
C4C O42C Tb2 134.2(10) . 1_455 ?
Tb1 O1W H11W 138.9 . . ?
Tb1 O1W H12W 98.8 . . ?
H11W O1W H12W 110.5 . . ?
Tb2 O2W H21W 147.0 . . ?
Tb2 O2W H22W 102.8 . . ?
H21W O2W H22W 109.6 . . ?
H31W O3W H32W 104.9 . . ?
H41W O4W H42W 103.3 . . ?
H51W O5W H52W 134.1 . . ?
H61W O6W H62W 103.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.84 1.99 2.815(17) 171.4 1_455 yes
O31A H31A O12A 0.86 1.88 2.717(17) 166.1 1_655 yes
O21B H21B O11C 0.88 1.72 2.582(15) 166.7 1_545 yes
O31B H31B O3W 0.85 1.90 2.726(15) 163.2 . yes
O21C H21C O11B 0.84 1.74 2.573(16) 167.2 . yes
O31C H31C O4W 0.83 1.97 2.725(17) 150.5 . yes
O1W H11W O6W 0.80 2.04 2.823(15) 168.5 . yes
O1W H12W O41B 0.85 1.89 2.725(17) 169.3 1_465 yes
O2W H21W O5W 0.82 1.91 2.720(17) 166.6 . yes
O2W H22W O41C 0.85 1.91 2.729(15) 159.4 1_655 yes
O3W H31W O21A 0.84 2.07 2.862(16) 156.3 1_545 yes
O3W H32W O11A 0.88 1.97 2.824(16) 161.6 . yes
O4W H41W O41A 0.89 1.85 2.737(18) 175.6 1_454 yes
O4W H42W O6W 0.83 1.94 2.765(17) 172.3 1_554 yes
O5W H51W O4W 0.83 2.02 2.848(19) 172.1 1_645 yes
O5W H52W O6W 0.87 2.46 3.321(17) 171.2 1_544 yes
O6W H61W O31A 0.84 1.99 2.805(16) 162.5 1_445 yes
O6W H62W O3W 0.87 1.95 2.808(18) 174.8 . yes

_refine_diff_density_max         2.786
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.181



# start Validation Reply Form
_vrf_PLAT342_Compound_Tb-L       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02333 Ang.  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but, despite of it, a substantial percentage of reflections cannot be successfully 
indexed.
;
# end Validation Reply Form

_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Compound_Ho-L
_database_code_depnum_ccdc_archive 'CCDC 1981578'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-k2O,O':k2O'',O''')diaquadiholmium(III)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Ho2 O20, 4(H2 O)'
_chemical_formula_sum            'C12 H24 Ho2 O24'
_chemical_formula_weight         882.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9870(4)
_cell_length_b                   7.3670(5)
_cell_length_c                   13.2590(9)
_cell_angle_alpha                102.346(2)
_cell_angle_beta                 101.822(2)
_cell_angle_gamma                90.365(2)
_cell_volume                     558.39(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5458
_cell_measurement_theta_min      2.834
_cell_measurement_theta_max      28.789


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.623
_exptl_crystal_F_000             422
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    7.151
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_process_details   
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_reflns_number            16950
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.834
_diffrn_reflns_theta_max         28.789
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             5458
_reflns_number_gt                5191
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_max     0.892
_reflns_Friedel_fraction_full    0.930

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+12.7832P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2304 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(7)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         5458
_refine_ls_number_parameters     344
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_restrained_S_all      1.222
_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
Ho1 Ho 0.02241(7) 0.81739(6) 0.67845(5) 0.0036(2) Uani 1 1 d . . . . .
Ho2 Ho -0.02326(8) 0.18352(7) 0.32249(5) 0.0041(2) Uani 1 1 d . . . . .
C1A C 0.221(3) 0.936(2) 0.8948(13) 0.002(3) Uani 1 1 d . U . . .
C2A C 0.377(3) 1.028(2) 0.9989(12) 0.004(3) Uani 1 1 d . U . . .
H2A H 0.361637 0.958752 1.052488 0.004 Uiso 1 1 calc R U . . .
C3A C 0.626(3) 1.027(2) 0.9858(12) 0.007(3) Uani 1 1 d . U . . .
H3A H 0.661049 0.898217 0.958797 0.008 Uiso 1 1 calc R U . . .
C4A C 0.785(3) 1.100(3) 1.0961(15) 0.008(4) Uani 1 1 d . U . . .
C1B C 0.158(3) 0.389(2) 0.5678(12) 0.008(3) Uani 1 1 d . . . . .
C2B C 0.346(3) 0.247(2) 0.5639(12) 0.004(3) Uani 1 1 d . U . . .
H2B H 0.488614 0.311509 0.561542 0.005 Uiso 1 1 calc R U . . .
C3B C 0.381(2) 0.1774(19) 0.6668(11) 0.005(3) Uani 1 1 d . . . . .
H3B H 0.465912 0.275349 0.724373 0.006 Uiso 1 1 calc R U . . .
C4B C 0.515(2) 0.0017(19) 0.6627(11) 0.005(3) Uani 1 1 d . U . . .
C1C C -0.151(2) 0.8328(19) 0.4342(11) 0.003(2) Uani 1 1 d . U . . .
C2C C -0.340(3) 0.695(2) 0.4351(12) 0.004(3) Uani 1 1 d . U . . .
H2C H -0.480175 0.761162 0.437757 0.005 Uiso 1 1 calc R U . . .
C3C C -0.379(2) 0.547(2) 0.3309(11) 0.005(3) Uani 1 1 d . . . . .
H3C H -0.464007 0.602652 0.274710 0.007 Uiso 1 1 calc R U . . .
C4C C -0.515(2) 0.374(2) 0.3338(11) 0.006(3) Uani 1 1 d . . . . .
O11A O 0.2656(19) 0.7769(15) 0.8470(8) 0.009(2) Uani 1 1 d . . . . .
O12A O 0.0455(18) 1.0133(15) 0.8551(8) 0.006(2) Uani 1 1 d . . . . .
O21A O 0.3231(18) 1.2182(15) 1.0341(8) 0.008(2) Uani 1 1 d . . . . .
O31A O 0.650(2) 1.1326(16) 0.9108(8) 0.009(2) Uani 1 1 d . . . . .
O41A O 0.754(2) 1.0077(16) 1.1646(9) 0.012(2) Uani 1 1 d . . . . .
O42A O 0.9253(18) 1.2290(16) 1.1148(9) 0.010(2) Uani 1 1 d . . . . .
O11B O -0.018(2) 0.3493(19) 0.4930(9) 0.016(3) Uani 1 1 d . . . . .
O12B O 0.1832(19) 0.5261(15) 0.6432(10) 0.008(2) Uani 1 1 d . . . . .
O21B O 0.2830(19) 0.1043(15) 0.4710(8) 0.007(2) Uani 1 1 d . . . . .
O31B O 0.1657(18) 0.1409(15) 0.6899(10) 0.006(2) Uani 1 1 d . . . . .
O41B O 0.409(2) -0.1443(17) 0.6682(9) 0.007(2) Uani 1 1 d . U . . .
O42B O 0.7190(18) 0.0135(14) 0.6553(8) 0.006(2) Uani 1 1 d . . . . .
O11C O 0.0226(18) 0.8513(14) 0.5073(8) 0.0054(19) Uani 1 1 d . U . . .
O12C O -0.1774(19) 0.9177(16) 0.3598(10) 0.007(2) Uani 1 1 d . . . . .
O21C O -0.2805(17) 0.6204(14) 0.5283(8) 0.0037(18) Uani 1 1 d . U . . .
O31C O -0.1646(19) 0.4907(14) 0.3038(9) 0.006(2) Uani 1 1 d . . . . .
O41C O -0.4098(19) 0.2273(18) 0.3328(9) 0.009(2) Uani 1 1 d . . . . .
O42C O -0.7219(19) 0.3882(15) 0.3360(9) 0.008(2) Uani 1 1 d . U . . .
O1W O -0.2426(19) 0.6553(16) 0.7425(9) 0.010(2) Uani 1 1 d . . . . .
O2W O 0.2276(19) -0.0243(15) 0.2504(9) 0.010(2) Uani 1 1 d . . . . .
O3W O 0.189(2) 0.4142(18) 0.8691(11) 0.014(3) Uani 1 1 d . . . . .
O4W O -0.294(3) 0.624(2) 0.1266(12) 0.025(3) Uani 1 1 d . . . . .
O5W O 0.220(3) -0.357(2) 0.1157(13) 0.035(4) Uani 1 1 d . . . . .
O6W O -0.225(2) 0.5056(16) 0.9243(10) 0.016(2) Uani 1 1 d . . . . .
H21A H 0.205044 1.230559 1.060734 0.025 Uiso 1 1 d . U . . .
H31A H 0.781856 1.108674 0.896993 0.025 Uiso 1 1 d . U . . .
H21B H 0.209316 0.015610 0.483677 0.025 Uiso 1 1 d . U . . .
H31B H 0.177068 0.179585 0.756820 0.025 Uiso 1 1 d . U . . .
H21C H -0.204220 0.524486 0.520618 0.025 Uiso 1 1 d . U . . .
H31C H -0.160249 0.523445 0.246945 0.025 Uiso 1 1 d . U . . .
H11W H -0.234431 0.640855 0.805056 0.025 Uiso 1 1 d . U . . .
H12W H -0.376469 0.690512 0.723975 0.025 Uiso 1 1 d . U . . .
H21W H 0.214447 -0.099326 0.190584 0.025 Uiso 1 1 d . U . . .
H22W H 0.361306 0.026318 0.262713 0.025 Uiso 1 1 d . U . . .
H31W H 0.257142 0.374469 0.923286 0.025 Uiso 1 1 d . U . . .
H32W H 0.236680 0.530140 0.878932 0.025 Uiso 1 1 d . U . . .
H41W H -0.220204 0.729794 0.146679 0.025 Uiso 1 1 d . U . . .
H42W H -0.307508 0.596028 0.060313 0.025 Uiso 1 1 d . U . . .
H51W H 0.355607 -0.374142 0.107352 0.025 Uiso 1 1 d . U . . .
H52W H 0.136132 -0.426220 0.060976 0.025 Uiso 1 1 d . U . . .
H61W H -0.335386 0.423821 0.909024 0.025 Uiso 1 1 d . U . . .
H62W H -0.107083 0.441502 0.921448 0.025 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O11C 2.335(10) . ?
Ho1 O42B 2.340(10) 1_465 ?
Ho1 O12B 2.352(11) . ?
Ho1 O41B 2.365(12) 1_565 ?
Ho1 O1W 2.372(11) . ?
Ho1 O12A 2.451(10) . ?
Ho1 O11A 2.482(11) . ?
Ho1 O31B 2.491(11) 1_565 ?
Ho1 O21C 2.571(10) . ?
Ho1 C1A 2.815(16) . ?
Ho2 O42C 2.297(11) 1_655 ?
Ho2 O11B 2.322(12) . ?
Ho2 O2W 2.346(11) . ?
Ho2 O41A 2.347(11) 1_444 ?
Ho2 O12C 2.348(11) 1_545 ?
Ho2 O41C 2.366(11) . ?
Ho2 O31C 2.465(11) . ?
Ho2 O21B 2.571(11) . ?
Ho2 O42A 2.800(12) 1_444 ?
Ho2 C4A 2.915(19) 1_444 ?
C1A O11A 1.268(19) . ?
C1A O12A 1.27(2) . ?
C1A C2A 1.52(2) . ?
C2A O21A 1.437(18) . ?
C2A C3A 1.532(18) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.42(2) . ?
C3A C4A 1.56(2) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.22(2) . ?
C4A O41A 1.28(2) . ?
C1B O12B 1.245(19) . ?
C1B O11B 1.274(18) . ?
C1B C2B 1.54(2) . ?
C2B O21B 1.421(19) . ?
C2B C3B 1.54(2) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.423(17) . ?
C3B C4B 1.52(2) . ?
C3B H3B 0.9800 . ?
C4B O42B 1.251(18) . ?
C4B O41B 1.267(19) . ?
C1C O11C 1.252(17) . ?
C1C O12C 1.260(18) . ?
C1C C2C 1.52(2) . ?
C2C O21C 1.437(18) . ?
C2C C3C 1.54(2) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.441(18) . ?
C3C C4C 1.52(2) . ?
C3C H3C 0.9800 . ?
C4C O42C 1.249(18) . ?
C4C O41C 1.25(2) . ?
O21A H21A 0.8496 . ?
O31A H31A 0.8554 . ?
O21B H21B 0.8504 . ?
O31B H31B 0.8601 . ?
O21C H21C 0.8429 . ?
O31C H31C 0.8440 . ?
O1W H11W 0.8506 . ?
O1W H12W 0.8481 . ?
O2W H21W 0.8525 . ?
O2W H22W 0.8503 . ?
O3W H31W 0.8607 . ?
O3W H32W 0.8739 . ?
O4W H41W 0.8532 . ?
O4W H42W 0.8455 . ?
O5W H51W 0.8496 . ?
O5W H52W 0.8532 . ?
O6W H61W 0.8547 . ?
O6W H62W 0.8536 . ?

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
O11C Ho1 O42B 80.2(4) . 1_465 ?
O11C Ho1 O12B 90.5(4) . . ?
O42B Ho1 O12B 151.8(4) 1_465 . ?
O11C Ho1 O41B 73.2(4) . 1_565 ?
O42B Ho1 O41B 130.8(4) 1_465 1_565 ?
O12B Ho1 O41B 69.7(4) . 1_565 ?
O11C Ho1 O1W 130.3(4) . . ?
O42B Ho1 O1W 82.0(4) 1_465 . ?
O12B Ho1 O1W 84.1(4) . . ?
O41B Ho1 O1W 145.8(4) 1_565 . ?
O11C Ho1 O12A 138.9(4) . . ?
O42B Ho1 O12A 76.0(4) 1_465 . ?
O12B Ho1 O12A 124.9(4) . . ?
O41B Ho1 O12A 98.1(4) 1_565 . ?
O1W Ho1 O12A 78.7(4) . . ?
O11C Ho1 O11A 144.7(4) . . ?
O42B Ho1 O11A 127.9(4) 1_465 . ?
O12B Ho1 O11A 72.9(4) . . ?
O41B Ho1 O11A 71.9(4) 1_565 . ?
O1W Ho1 O11A 79.7(4) . . ?
O12A Ho1 O11A 52.7(4) . . ?
O11C Ho1 O31B 72.0(4) . 1_565 ?
O42B Ho1 O31B 69.1(4) 1_465 1_565 ?
O12B Ho1 O31B 133.1(4) . 1_565 ?
O41B Ho1 O31B 63.7(4) 1_565 1_565 ?
O1W Ho1 O31B 140.2(4) . 1_565 ?
O12A Ho1 O31B 68.4(4) . 1_565 ?
O11A Ho1 O31B 96.6(4) . 1_565 ?
O11C Ho1 O21C 63.1(3) . . ?
O42B Ho1 O21C 75.8(3) 1_465 . ?
O12B Ho1 O21C 76.2(4) . . ?
O41B Ho1 O21C 123.3(4) 1_565 . ?
O1W Ho1 O21C 67.7(4) . . ?
O12A Ho1 O21C 138.5(3) . . ?
O11A Ho1 O21C 136.9(3) . . ?
O31B Ho1 O21C 126.6(3) 1_565 . ?
O11C Ho1 C1A 146.2(4) . . ?
O42B Ho1 C1A 102.8(4) 1_465 . ?
O12B Ho1 C1A 99.7(5) . . ?
O41B Ho1 C1A 80.3(4) 1_565 . ?
O1W Ho1 C1A 83.0(5) . . ?
O12A Ho1 C1A 26.8(4) . . ?
O11A Ho1 C1A 26.8(4) . . ?
O31B Ho1 C1A 77.7(5) 1_565 . ?
O21C Ho1 C1A 150.6(4) . . ?
O42C Ho2 O11B 82.7(4) 1_655 . ?
O42C Ho2 O2W 80.4(4) 1_655 . ?
O11B Ho2 O2W 132.6(4) . . ?
O42C Ho2 O41A 125.8(4) 1_655 1_444 ?
O11B Ho2 O41A 146.5(4) . 1_444 ?
O2W Ho2 O41A 75.1(4) . 1_444 ?
O42C Ho2 O12C 151.3(4) 1_655 1_545 ?
O11B Ho2 O12C 90.6(5) . 1_545 ?
O2W Ho2 O12C 84.0(4) . 1_545 ?
O41A Ho2 O12C 72.0(4) 1_444 1_545 ?
O42C Ho2 O41C 132.4(4) 1_655 . ?
O11B Ho2 O41C 73.9(4) . . ?
O2W Ho2 O41C 144.3(4) . . ?
O41A Ho2 O41C 73.4(4) 1_444 . ?
O12C Ho2 O41C 70.8(4) 1_545 . ?
O42C Ho2 O31C 70.0(4) 1_655 . ?
O11B Ho2 O31C 74.4(4) . . ?
O2W Ho2 O31C 137.1(4) . . ?
O41A Ho2 O31C 97.5(4) 1_444 . ?
O12C Ho2 O31C 134.8(4) 1_545 . ?
O41C Ho2 O31C 64.1(4) . . ?
O42C Ho2 O21B 76.7(4) 1_655 . ?
O11B Ho2 O21B 63.2(4) . . ?
O2W Ho2 O21B 70.0(4) . . ?
O41A Ho2 O21B 134.0(4) 1_444 . ?
O12C Ho2 O21B 75.4(4) 1_545 . ?
O41C Ho2 O21B 124.1(4) . . ?
O31C Ho2 O21B 128.4(4) . . ?
O42C Ho2 O42A 77.8(4) 1_655 1_444 ?
O11B Ho2 O42A 141.8(4) . 1_444 ?
O2W Ho2 O42A 75.9(4) . 1_444 ?
O41A Ho2 O42A 49.8(4) 1_444 1_444 ?
O12C Ho2 O42A 121.3(4) 1_545 1_444 ?
O41C Ho2 O42A 95.8(4) . 1_444 ?
O31C Ho2 O42A 68.2(4) . 1_444 ?
O21B Ho2 O42A 140.0(3) . 1_444 ?
O42C Ho2 C4A 101.9(5) 1_655 1_444 ?
O11B Ho2 C4A 151.3(5) . 1_444 ?
O2W Ho2 C4A 75.8(5) . 1_444 ?
O41A Ho2 C4A 25.4(5) 1_444 1_444 ?
O12C Ho2 C4A 97.4(5) 1_545 1_444 ?
O41C Ho2 C4A 82.7(5) . 1_444 ?
O31C Ho2 C4A 80.6(5) . 1_444 ?
O21B Ho2 C4A 145.5(4) . 1_444 ?
O42A Ho2 C4A 24.5(5) 1_444 1_444 ?
O11A C1A O12A 119.1(14) . . ?
O11A C1A C2A 119.0(15) . . ?
O12A C1A C2A 121.9(14) . . ?
O11A C1A Ho1 61.8(8) . . ?
O12A C1A Ho1 60.4(8) . . ?
C2A C1A Ho1 163.5(12) . . ?
O21A C2A C1A 111.6(13) . . ?
O21A C2A C3A 108.4(14) . . ?
C1A C2A C3A 109.6(12) . . ?
O21A C2A H2A 109.1 . . ?
C1A C2A H2A 109.1 . . ?
C3A C2A H2A 109.1 . . ?
O31A C3A C2A 109.1(15) . . ?
O31A C3A C4A 113.6(14) . . ?
C2A C3A C4A 108.7(13) . . ?
O31A C3A H3A 108.5 . . ?
C2A C3A H3A 108.5 . . ?
C4A C3A H3A 108.5 . . ?
O42A C4A O41A 123.7(17) . . ?
O42A C4A C3A 123.3(17) . . ?
O41A C4A C3A 113.0(16) . . ?
O42A C4A Ho2 72.5(10) . 1_666 ?
O41A C4A Ho2 51.7(8) . 1_666 ?
C3A C4A Ho2 163.1(13) . 1_666 ?
O12B C1B O11B 125.2(15) . . ?
O12B C1B C2B 119.4(13) . . ?
O11B C1B C2B 115.4(13) . . ?
O21B C2B C3B 113.9(13) . . ?
O21B C2B C1B 109.6(12) . . ?
C3B C2B C1B 107.0(12) . . ?
O21B C2B H2B 108.7 . . ?
C3B C2B H2B 108.7 . . ?
C1B C2B H2B 108.7 . . ?
O31B C3B C4B 108.6(11) . . ?
O31B C3B C2B 109.9(12) . . ?
C4B C3B C2B 113.0(12) . . ?
O31B C3B H3B 108.4 . . ?
C4B C3B H3B 108.4 . . ?
C2B C3B H3B 108.4 . . ?
O42B C4B O41B 125.5(13) . . ?
O42B C4B C3B 117.6(12) . . ?
O41B C4B C3B 116.9(13) . . ?
O11C C1C O12C 124.8(13) . . ?
O11C C1C C2C 116.8(12) . . ?
O12C C1C C2C 118.4(13) . . ?
O21C C2C C1C 109.4(12) . . ?
O21C C2C C3C 114.3(13) . . ?
C1C C2C C3C 108.1(12) . . ?
O21C C2C H2C 108.3 . . ?
C1C C2C H2C 108.3 . . ?
C3C C2C H2C 108.3 . . ?
O31C C3C C4C 108.3(12) . . ?
O31C C3C C2C 111.0(12) . . ?
C4C C3C C2C 113.1(12) . . ?
O31C C3C H3C 108.1 . . ?
C4C C3C H3C 108.1 . . ?
C2C C3C H3C 108.1 . . ?
O42C C4C O41C 125.4(13) . . ?
O42C C4C C3C 117.8(13) . . ?
O41C C4C C3C 116.7(13) . . ?
C1A O11A Ho1 91.5(9) . . ?
C1A O12A Ho1 92.8(9) . . ?
C2A O21A H21A 114.4 . . ?
C3A O31A H31A 105.1 . . ?
C4A O41A Ho2 102.8(11) . 1_666 ?
C4A O42A Ho2 83.1(11) . 1_666 ?
C1B O11B Ho2 125.8(10) . . ?
C1B O12B Ho1 136.4(11) . . ?
C2B O21B Ho2 115.8(9) . . ?
C2B O21B H21B 110.0 . . ?
Ho2 O21B H21B 98.4 . . ?
C3B O31B Ho1 121.3(9) . 1_545 ?
C3B O31B H31B 107.7 . . ?
Ho1 O31B H31B 96.7 1_545 . ?
C4B O41B Ho1 128.1(10) . 1_545 ?
C4B O42B Ho1 133.1(9) . 1_645 ?
C1C O11C Ho1 124.9(9) . . ?
C1C O12C Ho2 138.4(10) . 1_565 ?
C2C O21C Ho1 114.9(8) . . ?
C2C O21C H21C 113.9 . . ?
Ho1 O21C H21C 95.6 . . ?
C3C O31C Ho2 120.5(8) . . ?
C3C O31C H31C 106.9 . . ?
Ho2 O31C H31C 117.5 . . ?
C4C O41C Ho2 127.9(10) . . ?
C4C O42C Ho2 135.2(10) . 1_455 ?
Ho1 O1W H11W 128.1 . . ?
Ho1 O1W H12W 110.4 . . ?
H11W O1W H12W 104.8 . . ?
Ho2 O2W H21W 132.3 . . ?
Ho2 O2W H22W 111.0 . . ?
H21W O2W H22W 104.4 . . ?
H31W O3W H32W 106.7 . . ?
H41W O4W H42W 105.2 . . ?
H51W O5W H52W 104.5 . . ?
H61W O6W H62W 103.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.85 1.95 2.799(15) 173.5 1_455 yes
O31A H31A O12A 0.86 1.87 2.717(16) 169.6 1_655 yes
O21B H21B O11C 0.85 1.76 2.606(15) 171.8 1_545 yes
O31B H31B O3W 0.86 2.02 2.745(18) 141.9 . yes
O21C H21C O11B 0.84 1.74 2.575(17) 169.3 . yes
O31C H31C O4W 0.84 1.93 2.71(2) 152.8 . yes
O1W H11W O6W 0.85 2.03 2.841(17) 158.4 . yes
O1W H12W O41B 0.85 1.92 2.706(17) 153.1 1_465 yes
O2W H21W O5W 0.85 1.95 2.699(19) 146.4 . yes
O2W H22W O41C 0.85 1.95 2.730(15) 152.2 1_655 yes
O3W H31W O21A 0.86 2.03 2.857(18) 160.1 1_545 yes
O3W H32W O11A 0.87 1.97 2.796(17) 157.7 . yes
O4W H41W O41A 0.85 2.02 2.76(2) 145.2 1_454 yes
O4W H42W O6W 0.85 1.95 2.75(2) 158.8 1_554 yes
O5W H51W O4W 0.85 2.06 2.89(2) 165.1 1_645 yes
O5W H52W O6W 0.85 2.49 3.26(2) 151.2 1_544 yes
O6W H61W O31A 0.85 2.15 2.802(16) 132.6 1_445 yes
O6W H62W O3W 0.85 2.03 2.768(19) 145.0 . yes

_refine_diff_density_max         3.055
_refine_diff_density_min         -3.207
_refine_diff_density_rms         0.315


# start Validation Reply Form
_vrf_PLAT213_Compound_Ho-L       
;
PROBLEM: Atom O11B            has ADP max/min Ratio .....        4.8 prolat
RESPONSE: This compound, as well as most of the isostructural members with other 
lanthanide atoms, crystallizes as a twinned specimen. Despite the fact that twin 
law has been correctly determined and that specific absorption correction based 
on the faces of the crystal has been performed, somewhat large diffraction peaks
close to the lanthanide atoms could not be removed from the Fourier differences map. 
Nonetheless, the unaccounted positive residual density around the lanthanide 
heavy atoms is quite common for lanthanide-organic based crystal structures due to 
their large electronic shell.
;
_vrf_PLAT342_Compound_Ho-L       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02111 Ang.  
RESPONSE: The occurrence of a twinned specimen causes most of reflections to be
affected, which makes most of the molecular distances be somewhat out of the common
range.
;
# end Validation Reply Form


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

data_Compound_Dy-L
_database_code_depnum_ccdc_archive 'CCDC 1981576'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-k2O,O':k2O'',O''')diaquadidysprosium(III)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Dy2 O20, 4(H2 O)'
_chemical_formula_sum            'C12 H24 Dy2 O24'
_chemical_formula_weight         877.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9743(4)
_cell_length_b                   7.3542(5)
_cell_length_c                   13.1941(9)
_cell_angle_alpha                102.422(2)
_cell_angle_beta                 101.664(2)
_cell_angle_gamma                90.613(2)
_cell_volume                     553.55(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5601
_cell_measurement_theta_min      6.9310
_cell_measurement_theta_max      74.3650

loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -1.0001 -0.0001 0.0001 -0.0154 0.9623 -0.0751 0.0075 -0.9803 -0.9624

loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6000 8526 1023
2 0.4000 8452 1023

_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.632
_exptl_crystal_F_000             420
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    36.815
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.015
_exptl_absorpt_correction_T_max  0.156
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_reflns_number            18899
_diffrn_reflns_av_unetI/netI     0.1187
_diffrn_reflns_av_R_equivalents  0.2225
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.508
_diffrn_reflns_theta_max         74.244
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4449
_reflns_number_gt                4279
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.982
_reflns_Friedel_fraction_max     0.975
_reflns_Friedel_fraction_full    0.999

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1347P)²+9.6372P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1914 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(13)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         4449
_refine_ls_number_parameters     343
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0842
_refine_ls_wR_factor_ref         0.2110
_refine_ls_wR_factor_gt          0.2090
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.060
_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
Dy1 Dy 0.02208(12) 0.81691(11) 0.67835(8) 0.0151(4) Uani 1 1 d . . . . .
Dy2 Dy -0.02255(14) 0.18302(12) 0.32240(9) 0.0162(4) Uani 1 1 d . . . . .
C1A C 0.216(4) 0.934(3) 0.8950(18) 0.014(5) Uani 1 1 d . . . . .
C2A C 0.378(5) 1.030(3) 0.9991(18) 0.019(5) Uani 1 1 d . . . . .
H2A H 0.361873 0.962037 1.053749 0.023 Uiso 1 1 calc R U . . .
C3A C 0.627(4) 1.027(3) 0.9866(18) 0.015(4) Uani 1 1 d . . . . .
H3A H 0.659862 0.897542 0.959899 0.018 Uiso 1 1 calc R U . . .
C4A C 0.779(5) 1.096(4) 1.094(2) 0.020(5) Uani 1 1 d . . . . .
C1B C 0.159(4) 0.388(4) 0.5670(17) 0.020(5) Uani 1 1 d . . . . .
C2B C 0.347(5) 0.249(4) 0.5629(19) 0.021(5) Uani 1 1 d . . . . .
H2B H 0.489613 0.312762 0.559855 0.025 Uiso 1 1 calc R U . . .
C3B C 0.383(4) 0.177(3) 0.6667(16) 0.015(4) Uani 1 1 d . . . . .
H3B H 0.468262 0.275073 0.724850 0.018 Uiso 1 1 calc R U . . .
C4B C 0.510(4) 0.001(3) 0.6630(17) 0.017(4) Uani 1 1 d . . . . .
C1C C -0.151(4) 0.830(3) 0.4337(17) 0.015(4) Uani 1 1 d . . . . .
C2C C -0.338(4) 0.693(3) 0.4355(18) 0.016(5) Uani 1 1 d . . . . .
H2C H -0.477921 0.759325 0.438520 0.019 Uiso 1 1 calc R U . . .
C3C C -0.378(4) 0.547(3) 0.3313(17) 0.019(4) Uani 1 1 d . . . . .
H3C H -0.463163 0.603395 0.275137 0.022 Uiso 1 1 calc R U . . .
C4C C -0.516(4) 0.374(4) 0.3345(17) 0.021(5) Uani 1 1 d . . . . .
O11A O 0.266(3) 0.775(2) 0.8469(13) 0.023(3) Uani 1 1 d . . . . .
O12A O 0.048(3) 1.012(2) 0.8561(12) 0.020(3) Uani 1 1 d . . . . .
O21A O 0.328(3) 1.217(3) 1.0343(13) 0.024(4) Uani 1 1 d . . . . .
O31A O 0.653(3) 1.130(3) 0.9103(13) 0.021(3) Uani 1 1 d . . . . .
O41A O 0.757(3) 1.007(3) 1.1652(13) 0.025(4) Uani 1 1 d . . . . .
O42A O 0.925(3) 1.228(2) 1.1151(14) 0.023(4) Uani 1 1 d . . . . .
O12B O 0.182(3) 0.526(2) 0.6429(13) 0.019(3) Uani 1 1 d . . . . .
O11B O -0.013(3) 0.354(2) 0.4922(13) 0.021(3) Uani 1 1 d . . . . .
O21B O 0.283(2) 0.105(2) 0.4717(12) 0.014(3) Uani 1 1 d . . . . .
O31B O 0.169(3) 0.139(2) 0.6900(13) 0.017(3) Uani 1 1 d . . . . .
O41B O 0.410(3) -0.144(2) 0.6677(13) 0.020(3) Uani 1 1 d . . . . .
O42B O 0.718(3) 0.012(2) 0.6555(12) 0.020(3) Uani 1 1 d . . . . .
O11C O 0.022(3) 0.852(2) 0.5070(12) 0.019(3) Uani 1 1 d . . . . .
O12C O -0.179(3) 0.919(2) 0.3592(13) 0.017(3) Uani 1 1 d . U . . .
O21C O -0.279(3) 0.622(2) 0.5280(12) 0.016(3) Uani 1 1 d . . . . .
O31C O -0.166(3) 0.492(2) 0.3047(13) 0.018(3) Uani 1 1 d . . . . .
O41C O -0.408(3) 0.226(2) 0.3330(13) 0.018(3) Uani 1 1 d . . . . .
O42C O -0.720(3) 0.388(2) 0.3360(13) 0.021(3) Uani 1 1 d . . . . .
O1W O -0.246(3) 0.654(3) 0.7414(13) 0.025(4) Uani 1 1 d . . . . .
O2W O 0.230(3) -0.025(2) 0.2512(14) 0.022(3) Uani 1 1 d . . . . .
O3W O 0.195(3) 0.411(3) 0.8697(14) 0.025(4) Uani 1 1 d . . . . .
O4W O -0.298(5) 0.628(3) 0.1241(16) 0.039(5) Uani 1 1 d . . . . .
O5W O 0.223(4) -0.359(4) 0.1134(19) 0.050(6) Uani 1 1 d . . . . .
O6W O -0.219(4) 0.503(3) 0.9234(14) 0.028(4) Uani 1 1 d . . . . .
H21A H 0.209945 1.229278 1.060705 0.042 Uiso 1 1 d . U . . .
H31A H 0.782554 1.089411 0.903780 0.042 Uiso 1 1 d . U . . .
H21B H 0.199808 0.009062 0.474984 0.042 Uiso 1 1 d . U . . .
H31B H 0.145772 0.223299 0.741331 0.042 Uiso 1 1 d . U . . .
H21C H -0.204220 0.524486 0.520618 0.042 Uiso 1 1 d . U . . .
H31C H -0.160249 0.523445 0.246945 0.042 Uiso 1 1 d . U . . .
H11W H -0.257868 0.617374 0.794977 0.042 Uiso 1 1 d . U . . .
H12W H -0.366874 0.707338 0.721958 0.042 Uiso 1 1 d . U . . .
H21W H 0.248681 -0.121038 0.205550 0.042 Uiso 1 1 d . U . . .
H22W H 0.363527 0.028031 0.277494 0.042 Uiso 1 1 d . U . . .
H31W H 0.250195 0.382133 0.926350 0.042 Uiso 1 1 d . U . . .
H32W H 0.239496 0.524734 0.875053 0.042 Uiso 1 1 d . U . . .
H41W H -0.286849 0.749031 0.138282 0.042 Uiso 1 1 d . U . . .
H42W H -0.267328 0.596812 0.064376 0.042 Uiso 1 1 d . U . . .
H51W H 0.366358 -0.373141 0.120997 0.042 Uiso 1 1 d . U . . .
H52W H 0.108970 -0.409198 0.067232 0.042 Uiso 1 1 d . U . . .
H61W H -0.290476 0.396657 0.919605 0.042 Uiso 1 1 d . U . . .
H62W H -0.093257 0.470815 0.909758 0.042 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O11C 2.330(15) . ?
Dy1 O42B 2.339(17) 1_465 ?
Dy1 O12B 2.345(16) . ?
Dy1 O41B 2.370(18) 1_565 ?
Dy1 O1W 2.370(17) . ?
Dy1 O12A 2.445(16) . ?
Dy1 O31B 2.477(15) 1_565 ?
Dy1 O11A 2.483(18) . ?
Dy1 O21C 2.551(16) . ?
Dy1 C1A 2.80(2) . ?
Dy2 O42C 2.294(17) 1_655 ?
Dy2 O11B 2.310(16) . ?
Dy2 O41A 2.325(17) 1_444 ?
Dy2 O12C 2.328(15) 1_545 ?
Dy2 O2W 2.348(16) . ?
Dy2 O41C 2.356(16) . ?
Dy2 O31C 2.475(15) . ?
Dy2 O21B 2.568(15) . ?
Dy2 O42A 2.780(19) 1_444 ?
Dy2 C4A 2.94(3) 1_444 ?
C1A O12A 1.23(3) . ?
C1A O11A 1.28(3) . ?
C1A C2A 1.53(3) . ?
C2A O21A 1.41(3) . ?
C2A C3A 1.53(3) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.41(3) . ?
C3A C4A 1.50(4) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.24(4) . ?
C4A O41A 1.28(3) . ?
C1B O12B 1.25(3) . ?
C1B O11B 1.25(3) . ?
C1B C2B 1.54(3) . ?
C2B O21B 1.40(3) . ?
C2B C3B 1.55(3) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.41(3) . ?
C3B C4B 1.51(3) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.23(3) . ?
C4B O42B 1.27(3) . ?
C1C O11C 1.25(3) . ?
C1C O12C 1.28(3) . ?
C1C C2C 1.50(3) . ?
C2C O21C 1.41(3) . ?
C2C C3C 1.52(3) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.42(3) . ?
C3C C4C 1.52(3) . ?
C3C H3C 0.9800 . ?
C4C O42C 1.23(3) . ?
C4C O41C 1.27(3) . ?
O21A H21A 0.8462 . ?
O31A H31A 0.8477 . ?
O21B H21B 0.8698 . ?
O31B H31B 0.8508 . ?
O21C H21C 0.8480 . ?
O31C H31C 0.8515 . ?
O1W H11W 0.8236 . ?
O1W H12W 0.8497 . ?
O2W H21W 0.8466 . ?
O2W H22W 0.8556 . ?
O3W H31W 0.8273 . ?
O3W H32W 0.8556 . ?
O4W H41W 0.8704 . ?
O4W H42W 0.8301 . ?
O5W H51W 0.8531 . ?
O5W H52W 0.8371 . ?
O6W H61W 0.8717 . ?
O6W H62W 0.8351 . ?

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
O11C Dy1 O42B 80.0(6) . 1_465 ?
O11C Dy1 O12B 90.8(6) . . ?
O42B Dy1 O12B 151.6(6) 1_465 . ?
O11C Dy1 O41B 73.2(6) . 1_565 ?
O42B Dy1 O41B 130.9(6) 1_465 1_565 ?
O12B Dy1 O41B 69.8(6) . 1_565 ?
O11C Dy1 O1W 129.9(6) . . ?
O42B Dy1 O1W 81.7(6) 1_465 . ?
O12B Dy1 O1W 84.0(6) . . ?
O41B Dy1 O1W 146.1(6) 1_565 . ?
O11C Dy1 O12A 139.0(6) . . ?
O42B Dy1 O12A 76.5(6) 1_465 . ?
O12B Dy1 O12A 124.4(6) . . ?
O41B Dy1 O12A 97.8(6) 1_565 . ?
O1W Dy1 O12A 79.1(6) . . ?
O11C Dy1 O31B 71.8(6) . 1_565 ?
O42B Dy1 O31B 69.8(6) 1_465 1_565 ?
O12B Dy1 O31B 132.7(6) . 1_565 ?
O41B Dy1 O31B 63.1(5) 1_565 1_565 ?
O1W Dy1 O31B 140.8(6) . 1_565 ?
O12A Dy1 O31B 68.7(6) . 1_565 ?
O11C Dy1 O11A 144.7(6) . . ?
O42B Dy1 O11A 128.3(6) 1_465 . ?
O12B Dy1 O11A 72.5(6) . . ?
O41B Dy1 O11A 71.8(6) 1_565 . ?
O1W Dy1 O11A 80.1(6) . . ?
O12A Dy1 O11A 52.6(6) . . ?
O31B Dy1 O11A 96.6(6) 1_565 . ?
O11C Dy1 O21C 62.8(5) . . ?
O42B Dy1 O21C 75.5(6) 1_465 . ?
O12B Dy1 O21C 76.4(5) . . ?
O41B Dy1 O21C 123.2(5) 1_565 . ?
O1W Dy1 O21C 67.6(6) . . ?
O12A Dy1 O21C 138.9(5) . . ?
O31B Dy1 O21C 126.4(5) 1_565 . ?
O11A Dy1 O21C 136.9(5) . . ?
O11C Dy1 C1A 146.8(7) . . ?
O42B Dy1 C1A 102.7(7) 1_465 . ?
O12B Dy1 C1A 99.6(6) . . ?
O41B Dy1 C1A 80.9(7) 1_565 . ?
O1W Dy1 C1A 82.7(6) . . ?
O12A Dy1 C1A 26.1(7) . . ?
O31B Dy1 C1A 78.1(6) 1_565 . ?
O11A Dy1 C1A 27.2(7) . . ?
O21C Dy1 C1A 150.3(6) . . ?
O42C Dy2 O11B 81.5(7) 1_655 . ?
O42C Dy2 O41A 125.8(6) 1_655 1_444 ?
O11B Dy2 O41A 147.4(7) . 1_444 ?
O42C Dy2 O12C 151.6(6) 1_655 1_545 ?
O11B Dy2 O12C 91.8(6) . 1_545 ?
O41A Dy2 O12C 71.8(6) 1_444 1_545 ?
O42C Dy2 O2W 80.3(6) 1_655 . ?
O11B Dy2 O2W 132.2(6) . . ?
O41A Dy2 O2W 75.4(6) 1_444 . ?
O12C Dy2 O2W 84.1(6) 1_545 . ?
O42C Dy2 O41C 132.6(6) 1_655 . ?
O11B Dy2 O41C 74.5(6) . . ?
O41A Dy2 O41C 73.5(6) 1_444 . ?
O12C Dy2 O41C 70.4(6) 1_545 . ?
O2W Dy2 O41C 144.6(6) . . ?
O42C Dy2 O31C 70.5(6) 1_655 . ?
O11B Dy2 O31C 73.2(6) . . ?
O41A Dy2 O31C 97.7(6) 1_444 . ?
O12C Dy2 O31C 133.9(6) 1_545 . ?
O2W Dy2 O31C 137.9(6) . . ?
O41C Dy2 O31C 63.7(6) . . ?
O42C Dy2 O21B 76.6(6) 1_655 . ?
O11B Dy2 O21B 63.3(5) . . ?
O41A Dy2 O21B 133.9(6) 1_444 . ?
O12C Dy2 O21B 75.7(5) 1_545 . ?
O2W Dy2 O21B 69.6(6) . . ?
O41C Dy2 O21B 123.9(5) . . ?
O31C Dy2 O21B 128.3(5) . . ?
O42C Dy2 O42A 78.0(6) 1_655 1_444 ?
O11B Dy2 O42A 140.7(6) . 1_444 ?
O41A Dy2 O42A 49.6(6) 1_444 1_444 ?
O12C Dy2 O42A 121.1(5) 1_545 1_444 ?
O2W Dy2 O42A 76.6(6) . 1_444 ?
O41C Dy2 O42A 95.6(5) . 1_444 ?
O31C Dy2 O42A 68.4(5) . 1_444 ?
O21B Dy2 O42A 140.4(5) . 1_444 ?
O42C Dy2 C4A 102.6(7) 1_655 1_444 ?
O11B Dy2 C4A 150.7(6) . 1_444 ?
O41A Dy2 C4A 24.9(7) 1_444 1_444 ?
O12C Dy2 C4A 96.7(7) 1_545 1_444 ?
O2W Dy2 C4A 76.7(6) . 1_444 ?
O41C Dy2 C4A 82.1(6) . 1_444 ?
O31C Dy2 C4A 80.8(6) . 1_444 ?
O21B Dy2 C4A 146.0(6) . 1_444 ?
O42A Dy2 C4A 24.9(7) 1_444 1_444 ?
O12A C1A O11A 121(2) . . ?
O12A C1A C2A 121(2) . . ?
O11A C1A C2A 118(2) . . ?
O12A C1A Dy1 60.8(12) . . ?
O11A C1A Dy1 62.6(12) . . ?
C2A C1A Dy1 161.3(16) . . ?
O21A C2A C3A 108.0(19) . . ?
O21A C2A C1A 112(2) . . ?
C3A C2A C1A 110.9(18) . . ?
O21A C2A H2A 108.5 . . ?
C3A C2A H2A 108.5 . . ?
C1A C2A H2A 108.5 . . ?
O31A C3A C4A 115(2) . . ?
O31A C3A C2A 108.9(19) . . ?
C4A C3A C2A 108.7(18) . . ?
O31A C3A H3A 108.2 . . ?
C4A C3A H3A 108.2 . . ?
C2A C3A H3A 108.2 . . ?
O42A C4A O41A 120(3) . . ?
O42A C4A C3A 124(2) . . ?
O41A C4A C3A 116(2) . . ?
O42A C4A Dy2 70.5(15) . 1_666 ?
O41A C4A Dy2 49.9(13) . 1_666 ?
C3A C4A Dy2 164.3(18) . 1_666 ?
O12B C1B O11B 124(2) . . ?
O12B C1B C2B 120(2) . . ?
O11B C1B C2B 116(2) . . ?
O21B C2B C1B 109(2) . . ?
O21B C2B C3B 113(2) . . ?
C1B C2B C3B 107.1(18) . . ?
O21B C2B H2B 109.1 . . ?
C1B C2B H2B 109.1 . . ?
C3B C2B H2B 109.1 . . ?
O31B C3B C4B 106.6(18) . . ?
O31B C3B C2B 110.1(18) . . ?
C4B C3B C2B 114.0(18) . . ?
O31B C3B H3B 108.7 . . ?
C4B C3B H3B 108.7 . . ?
C2B C3B H3B 108.7 . . ?
O41B C4B O42B 124(2) . . ?
O41B C4B C3B 119(2) . . ?
O42B C4B C3B 117(2) . . ?
O11C C1C O12C 124(2) . . ?
O11C C1C C2C 117(2) . . ?
O12C C1C C2C 119(2) . . ?
O21C C2C C1C 109.4(19) . . ?
O21C C2C C3C 115.5(19) . . ?
C1C C2C C3C 107.9(18) . . ?
O21C C2C H2C 108.0 . . ?
C1C C2C H2C 108.0 . . ?
C3C C2C H2C 108.0 . . ?
O31C C3C C4C 108.4(18) . . ?
O31C C3C C2C 110.4(19) . . ?
C4C C3C C2C 112.8(18) . . ?
O31C C3C H3C 108.4 . . ?
C4C C3C H3C 108.4 . . ?
C2C C3C H3C 108.4 . . ?
O42C C4C O41C 126(2) . . ?
O42C C4C C3C 118(2) . . ?
O41C C4C C3C 116(2) . . ?
C1A O11A Dy1 90.3(14) . . ?
C1A O12A Dy1 93.1(14) . . ?
C2A O21A H21A 113.5 . . ?
C3A O31A H31A 94.2 . . ?
C4A O41A Dy2 105.2(18) . 1_666 ?
C4A O42A Dy2 84.6(15) . 1_666 ?
C1B O12B Dy1 136.7(15) . . ?
C1B O11B Dy2 126.3(15) . . ?
C2B O21B Dy2 115.5(13) . . ?
C2B O21B H21B 118.6 . . ?
Dy2 O21B H21B 92.2 . . ?
C3B O31B Dy1 122.4(13) . 1_545 ?
C3B O31B H31B 109.4 . . ?
Dy1 O31B H31B 117.5 1_545 . ?
C4B O41B Dy1 127.1(15) . 1_545 ?
C4B O42B Dy1 133.6(15) . 1_645 ?
C1C O11C Dy1 124.6(14) . . ?
C1C O12C Dy2 138.7(14) . 1_565 ?
C2C O21C Dy1 115.9(13) . . ?
C2C O21C H21C 114.1 . . ?
Dy1 O21C H21C 95.8 . . ?
C3C O31C Dy2 121.1(13) . . ?
C3C O31C H31C 107.3 . . ?
Dy2 O31C H31C 116.3 . . ?
C4C O41C Dy2 128.3(16) . . ?
C4C O42C Dy2 135.3(17) . 1_455 ?
Dy1 O1W H11W 139.8 . . ?
Dy1 O1W H12W 100.6 . . ?
H11W O1W H12W 107.4 . . ?
Dy2 O2W H21W 148.2 . . ?
Dy2 O2W H22W 105.1 . . ?
H21W O2W H22W 105.9 . . ?
H31W O3W H32W 107.9 . . ?
H41W O4W H42W 104.0 . . ?
H51W O5W H52W 133.3 . . ?
H61W O6W H62W 102.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.85 1.98 2.82(2) 173.8 1_455 yes
O31A H31A O12A 0.85 1.87 2.70(2) 166.0 1_655 yes
O21B H21B O11C 0.87 1.73 2.59(2) 167.0 1_545 yes
O31B H31B O3W 0.85 1.91 2.73(2) 162.0 . yes
O21C H21C O11B 0.85 1.74 2.57(2) 166.8 . yes
O31C H31C O4W 0.85 1.98 2.76(3) 151.6 . yes
O1W H11W O6W 0.82 2.02 2.83(2) 167.0 . yes
O1W H12W O41B 0.85 1.86 2.70(3) 167.2 1_465 yes
O2W H21W O5W 0.85 1.89 2.72(3) 165.1 . yes
O2W H22W O41C 0.86 1.90 2.71(2) 158.2 1_655 yes
O3W H31W O21A 0.83 2.05 2.84(3) 158.7 1_545 yes
O3W H32W O11A 0.86 1.96 2.79(3) 162.0 . yes
O4W H41W O41A 0.87 1.86 2.73(3) 175.9 1_454 yes
O4W H42W O6W 0.83 1.92 2.75(3) 173.7 1_554 yes
O5W H51W O4W 0.85 2.00 2.84(4) 170.0 1_645 yes
O5W H52W O6W 0.84 2.41 3.24(3) 168.8 1_544 yes
O6W H61W O31A 0.87 1.96 2.80(3) 160.9 1_445 yes
O6W H62W O3W 0.84 1.93 2.76(3) 175.0 . yes

_refine_diff_density_max         4.363
_refine_diff_density_min         -1.722
_refine_diff_density_rms         0.386


# start Validation Reply Form
_vrf_RINTA01_Compound_Dy-L       
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately. 
;
_vrf_PLAT971_Compound_Dy-L       
;
PROBLEM: Check Calcd Resid. Dens.  0.83A   From Dy2             4.61 eA-3  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. Despite the fact that specific absorption
correction based on the faces of the crystal has been performed, somewhat large
diffraction peaks close to the lanthanide atoms could not be removed. Nonetheless,
the unaccounted positive residual density is quite common for lanthanide-organic
based crystal structures. 
;
_vrf_PLAT020_Compound_Dy-L       
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.222 Report
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately.
;
_vrf_PLAT342_Compound_Dy-L       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03333 Ang.  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately. 
;
# end Validation Reply Form
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Compound_Tb-L'
_database_code_depnum_ccdc_archive 'CCDC 1981573'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-Î?3O,O',O'':Î?2O''',O'''')aquaditerbium(III)] hydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H14 O19 Tb2, (H2 O)'
_chemical_formula_sum            'C12 H16 O20 Tb2'
_chemical_formula_weight         798.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.83840(10)
_cell_length_b                   7.3898(2)
_cell_length_c                   11.9051(3)
_cell_angle_alpha                108.094(2)
_cell_angle_beta                 103.635(2)
_cell_angle_gamma                89.994(2)
_cell_volume                     472.99(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11484
_cell_measurement_theta_min      1.858
_cell_measurement_theta_max      28.141


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.802
_exptl_crystal_F_000             378
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    7.526
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_T_max  2.439
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
Single crystals of this compound crystallize as a twinned specimen, 
but no twin law has been applied for the data reduction because, ohterwise,
agreement factors got worse.  
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω
_diffrn_reflns_number            10195
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.858
_diffrn_reflns_theta_max         25.538
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3541
_reflns_number_gt                3511
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_max     0.999
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
The crystal is a twinned specimen but no twin law has been applied
during data reduction nor the refinement since it leads to better
agreement factors. Moreover, the structure possesses a strong
pseudosymmetry arising from the almost equivalent environment of the
two independent terbium atoms, which simulates a monoclinic unit cell.
However, all trials to finish the refinment with the monoclinic cell
led to unsatisfactory results, because it causes a disorder in the 
terbium environment that worsens the agreement factors.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0629P)²+8.3303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1712 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         3541
_refine_ls_number_parameters     307
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.007
_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 1.81966(8) 0.84565(7) 1.08441(6) 0.0089(2) Uani 1 1 d . . . . .
Tb2 Tb 1.47197(8) 1.13242(7) 0.65807(6) 0.0083(2) Uani 1 1 d . . . . .
C1A C 1.942(5) 1.239(5) 1.312(3) 0.092(12) Uani 1 1 d D U . . .
C1B C 1.543(3) 1.152(2) 0.9411(15) 0.012(3) Uani 1 1 d . U . . .
C1C C 1.749(3) 0.583(2) 0.8025(16) 0.016(3) Uani 1 1 d . . . . .
C2A C 2.176(5) 1.190(5) 1.2715(18) 0.071(9) Uani 1 1 d D U . . .
H2A H 2.254688 1.315583 1.286631 0.085 Uiso 1 1 calc R U . . .
C2B C 1.362(3) 1.300(3) 0.9449(17) 0.011(4) Uani 1 1 d . U . . .
H2B H 1.211090 1.240376 0.944049 0.014 Uiso 1 1 calc R U . . .
C2C C 1.928(3) 0.725(3) 0.7971(17) 0.010(4) Uani 1 1 d . U . . .
H2C H 2.078320 0.665069 0.796881 0.012 Uiso 1 1 calc R U . . .
C3A C 2.338(6) 1.110(4) 1.367(2) 0.088(11) Uani 1 1 d D U . . .
H3A H 2.449337 1.040390 1.322658 0.105 Uiso 1 1 calc R U . . .
C3B C 1.445(3) 1.463(2) 1.0671(15) 0.012(3) Uani 1 1 d . . . . .
H3B H 1.420449 1.418565 1.132909 0.014 Uiso 1 1 calc R U . . .
C3C C 1.844(3) 0.769(2) 0.6756(15) 0.012(3) Uani 1 1 d . . . . .
H3C H 1.867678 0.657851 0.609369 0.015 Uiso 1 1 calc R U . . .
C4A C 2.175(5) 0.944(4) 1.371(3) 0.052(7) Uani 1 1 d D U . . .
C4B C 1.312(3) 1.640(3) 1.0688(15) 0.014(3) Uani 1 1 d . . . . .
C4C C 1.980(3) 0.940(2) 0.6744(15) 0.011(3) Uani 1 1 d . . . . .
O11A O 1.917(5) 1.346(4) 1.417(2) 0.073(7) Uani 1 1 d D U . . .
O11B O 1.657(2) 1.1281(17) 0.8583(11) 0.012(2) Uani 1 1 d . . . . .
O11C O 1.633(2) 0.6396(17) 0.8836(10) 0.013(2) Uani 1 1 d . . . . .
O12A O 1.786(3) 1.118(2) 1.2565(16) 0.041(4) Uani 1 1 d D U . . .
O12B O 1.579(3) 1.070(2) 1.0179(14) 0.025(3) Uani 1 1 d . . . . .
O12C O 1.713(3) 0.4243(18) 0.7247(15) 0.027(3) Uani 1 1 d . . . . .
O21A O 2.126(2) 1.104(2) 1.1402(15) 0.028(3) Uani 1 1 d D . . . .
O21B O 1.328(2) 1.3580(16) 0.8404(10) 0.011(2) Uani 1 1 d . . . . .
O21C O 1.966(2) 0.8904(16) 0.9030(10) 0.011(2) Uani 1 1 d . . . . .
O31A O 2.494(3) 1.229(2) 1.4809(16) 0.043(4) Uani 1 1 d D . . . .
O31B O 1.693(2) 1.5217(16) 1.0918(11) 0.013(2) Uani 1 1 d . . . . .
O31C O 1.599(2) 0.8016(17) 0.6514(12) 0.014(2) Uani 1 1 d . . . . .
O41A O 2.247(2) 0.9239(18) 1.4681(12) 0.018(3) Uani 1 1 d . . . . .
O41B O 1.428(2) 1.7960(19) 1.0990(11) 0.015(2) Uani 1 1 d . . . . .
O41C O 1.860(2) 1.0692(19) 0.6440(11) 0.013(2) Uani 1 1 d . . . . .
O42A O 2.046(2) 0.8251(18) 1.2735(12) 0.018(3) Uani 1 1 d . . . . .
O42B O 1.091(2) 1.6150(16) 1.0407(11) 0.012(2) Uani 1 1 d . . . . .
O42C O 2.200(2) 0.9450(16) 0.7018(11) 0.012(2) Uani 1 1 d . . . . .
O1W O 1.167(2) 1.3351(19) 0.6058(16) 0.028(3) Uani 1 1 d . . . . .
O2W O 1.912(9) 0.671(8) 0.404(5) 0.168(18) Uani 1 1 d . U . . .
H21A H 2.219142 1.015474 1.114506 0.253 Uiso 1 1 d . U . . .
H31A H 2.615233 1.278940 1.470441 0.253 Uiso 1 1 d . U . . .
H21B H 1.429982 1.451174 0.861606 0.253 Uiso 1 1 d . U . . .
H31B H 1.661245 1.540974 1.022281 0.253 Uiso 1 1 d . U . . .
H21C H 1.883626 0.976128 0.882867 0.253 Uiso 1 1 d . U . . .
H31C H 1.634214 0.906428 0.709149 0.253 Uiso 1 1 d . U . . .
H11W H 1.105653 1.321466 0.530436 0.253 Uiso 1 1 d . U . . .
H12W H 1.069219 1.271914 0.624915 0.253 Uiso 1 1 d . U . . .
H21W H 1.911272 0.682092 0.324658 0.253 Uiso 1 1 d . U . . .
H22W H 1.882836 0.552885 0.391557 0.253 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O42B 2.351(11) 1_645 ?
Tb1 O41B 2.368(12) 1_545 ?
Tb1 O42A 2.376(12) . ?
Tb1 O12B 2.376(13) . ?
Tb1 O11C 2.394(12) . ?
Tb1 O12A 2.432(17) . ?
Tb1 O21A 2.437(13) . ?
Tb1 O31B 2.539(12) 1_545 ?
Tb1 O21C 2.612(11) . ?
Tb1 H21A 2.5437 . ?
Tb2 O41C 2.345(12) . ?
Tb2 O42C 2.357(11) 1_455 ?
Tb2 O41A 2.378(13) 1_454 ?
Tb2 O12C 2.381(13) 1_565 ?
Tb2 O11B 2.385(12) . ?
Tb2 O1W 2.419(13) . ?
Tb2 O31A 2.458(14) 1_454 ?
Tb2 O31C 2.538(11) . ?
Tb2 O21B 2.611(11) . ?
Tb2 H31C 2.1012 . ?
Tb2 H12W 2.5617 . ?
C1A O12A 1.189(15) . ?
C1A O11A 1.298(15) . ?
C1A C2A 1.553(15) . ?
C1B O12B 1.22(2) . ?
C1B O11B 1.28(2) . ?
C1B C2B 1.52(2) . ?
C1C O12C 1.23(2) . ?
C1C O11C 1.27(2) . ?
C1C C2C 1.51(2) . ?
C2A O21A 1.450(14) . ?
C2A C3A 1.571(15) . ?
C2A H2A 0.9800 . ?
C2B O21B 1.41(2) . ?
C2B C3B 1.54(2) . ?
C2B H2B 0.9800 . ?
C2C O21C 1.43(2) . ?
C2C C3C 1.55(2) . ?
C2C H2C 0.9800 . ?
C3A O31A 1.453(15) . ?
C3A C4A 1.569(15) . ?
C3A H3A 0.9800 . ?
C3B O31B 1.445(18) . ?
C3B C4B 1.51(2) . ?
C3B H3B 0.9800 . ?
C3C O31C 1.428(19) . ?
C3C C4C 1.50(2) . ?
C3C H3C 0.9800 . ?
C4A O41A 1.18(3) . ?
C4A O42A 1.29(4) . ?
C4B O41B 1.24(2) . ?
C4B O42B 1.25(2) . ?
C4C O42C 1.25(2) . ?
C4C O41C 1.28(2) . ?
O21A H21A 0.8753 . ?
O21B H21B 0.8459 . ?
O21C H21C 0.8554 . ?
O31A H31A 0.8503 . ?
O31B H31B 0.8609 . ?
O31C H31C 0.8472 . ?
O1W H11W 0.8584 . ?
O1W H12W 0.8520 . ?
O2W H21W 0.9708 . ?
O2W H22W 0.8488 . ?

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
O42B Tb1 O41B 127.6(4) 1_645 1_545 ?
O42B Tb1 O42A 72.6(4) 1_645 . ?
O41B Tb1 O42A 101.8(4) 1_545 . ?
O42B Tb1 O12B 146.7(4) 1_645 . ?
O41B Tb1 O12B 70.1(5) 1_545 . ?
O42A Tb1 O12B 136.5(5) . . ?
O42B Tb1 O11C 76.0(4) 1_645 . ?
O41B Tb1 O11C 77.8(4) 1_545 . ?
O42A Tb1 O11C 139.3(4) . . ?
O12B Tb1 O11C 82.3(5) . . ?
O42B Tb1 O12A 137.1(5) 1_645 . ?
O41B Tb1 O12A 76.9(5) 1_545 . ?
O42A Tb1 O12A 67.6(5) . . ?
O12B Tb1 O12A 69.0(6) . . ?
O11C Tb1 O12A 146.8(5) . . ?
O42B Tb1 O21A 91.3(4) 1_645 . ?
O41B Tb1 O21A 140.0(5) 1_545 . ?
O42A Tb1 O21A 78.9(5) . . ?
O12B Tb1 O21A 82.0(5) . . ?
O11C Tb1 O21A 127.3(5) . . ?
O12A Tb1 O21A 66.3(5) . . ?
O42B Tb1 O31B 66.3(4) 1_645 1_545 ?
O41B Tb1 O31B 62.3(4) 1_545 1_545 ?
O42A Tb1 O31B 74.4(4) . 1_545 ?
O12B Tb1 O31B 128.4(5) . 1_545 ?
O11C Tb1 O31B 69.7(4) . 1_545 ?
O12A Tb1 O31B 115.5(5) . 1_545 ?
O21A Tb1 O31B 149.1(4) . 1_545 ?
O42B Tb1 O21C 73.5(4) 1_645 . ?
O41B Tb1 O21C 129.3(4) 1_545 . ?
O42A Tb1 O21C 128.8(4) . . ?
O12B Tb1 O21C 74.1(4) . . ?
O11C Tb1 O21C 62.6(4) . . ?
O12A Tb1 O21C 121.3(5) . . ?
O21A Tb1 O21C 64.7(4) . . ?
O31B Tb1 O21C 123.1(4) 1_545 . ?
O42B Tb1 H21A 71.3 1_645 . ?
O41B Tb1 H21A 159.8 1_545 . ?
O42A Tb1 H21A 75.7 . . ?
O12B Tb1 H21A 97.6 . . ?
O11C Tb1 H21A 117.4 . . ?
O12A Tb1 H21A 83.8 . . ?
O21A Tb1 H21A 20.1 . . ?
O31B Tb1 H21A 133.6 1_545 . ?
O21C Tb1 H21A 57.6 . . ?
O41C Tb2 O42C 127.6(4) . 1_455 ?
O41C Tb2 O41A 101.7(4) . 1_454 ?
O42C Tb2 O41A 73.0(4) 1_455 1_454 ?
O41C Tb2 O12C 70.1(5) . 1_565 ?
O42C Tb2 O12C 146.7(4) 1_455 1_565 ?
O41A Tb2 O12C 136.1(5) 1_454 1_565 ?
O41C Tb2 O11B 77.8(4) . . ?
O42C Tb2 O11B 76.0(4) 1_455 . ?
O41A Tb2 O11B 139.8(4) 1_454 . ?
O12C Tb2 O11B 82.3(5) 1_565 . ?
O41C Tb2 O1W 140.4(5) . . ?
O42C Tb2 O1W 91.0(4) 1_455 . ?
O41A Tb2 O1W 79.5(5) 1_454 . ?
O12C Tb2 O1W 81.8(5) 1_565 . ?
O11B Tb2 O1W 126.3(5) . . ?
O41C Tb2 O31A 78.3(5) . 1_454 ?
O42C Tb2 O31A 135.4(5) 1_455 1_454 ?
O41A Tb2 O31A 65.7(5) 1_454 1_454 ?
O12C Tb2 O31A 70.4(6) 1_565 1_454 ?
O11B Tb2 O31A 148.5(5) . 1_454 ?
O1W Tb2 O31A 66.1(5) . 1_454 ?
O41C Tb2 O31C 62.3(4) . . ?
O42C Tb2 O31C 66.3(4) 1_455 . ?
O41A Tb2 O31C 74.7(4) 1_454 . ?
O12C Tb2 O31C 128.4(5) 1_565 . ?
O11B Tb2 O31C 69.7(4) . . ?
O1W Tb2 O31C 149.6(5) . . ?
O31A Tb2 O31C 115.7(5) 1_454 . ?
O41C Tb2 O21B 128.8(4) . . ?
O42C Tb2 O21B 73.6(4) 1_455 . ?
O41A Tb2 O21B 129.4(4) 1_454 . ?
O12C Tb2 O21B 74.1(4) 1_565 . ?
O11B Tb2 O21B 62.1(4) . . ?
O1W Tb2 O21B 64.3(5) . . ?
O31A Tb2 O21B 121.6(5) 1_454 . ?
O31C Tb2 O21B 122.7(4) . . ?
O41C Tb2 H31C 59.0 . . ?
O42C Tb2 H31C 69.1 1_455 . ?
O41A Tb2 H31C 92.7 1_454 . ?
O12C Tb2 H31C 115.6 1_565 . ?
O11B Tb2 H31C 52.0 . . ?
O1W Tb2 H31C 160.0 . . ?
O31A Tb2 H31C 127.4 1_454 . ?
O31C Tb2 H31C 18.1 . . ?
O21B Tb2 H31C 109.3 . . ?
O41C Tb2 H12W 159.4 . . ?
O42C Tb2 H12W 71.6 1_455 . ?
O41A Tb2 H12W 75.2 1_454 . ?
O12C Tb2 H12W 97.7 1_565 . ?
O11B Tb2 H12W 118.0 . . ?
O1W Tb2 H12W 19.4 . . ?
O31A Tb2 H12W 82.0 1_454 . ?
O31C Tb2 H12W 133.6 . . ?
O21B Tb2 H12W 58.7 . . ?
H31C Tb2 H12W 140.7 . . ?
O12A C1A O11A 114(2) . . ?
O12A C1A C2A 113(2) . . ?
O11A C1A C2A 128(2) . . ?
O12B C1B O11B 124.2(15) . . ?
O12B C1B C2B 119.5(15) . . ?
O11B C1B C2B 116.2(14) . . ?
O12C C1C O11C 123.9(16) . . ?
O12C C1C C2C 118.6(16) . . ?
O11C C1C C2C 117.4(16) . . ?
O21A C2A C1A 110.4(19) . . ?
O21A C2A C3A 125(2) . . ?
C1A C2A C3A 108(3) . . ?
O21A C2A H2A 103.8 . . ?
C1A C2A H2A 103.8 . . ?
C3A C2A H2A 103.8 . . ?
O21B C2B C1B 109.9(15) . . ?
O21B C2B C3B 114.6(15) . . ?
C1B C2B C3B 107.7(14) . . ?
O21B C2B H2B 108.2 . . ?
C1B C2B H2B 108.2 . . ?
C3B C2B H2B 108.2 . . ?
O21C C2C C1C 110.0(14) . . ?
O21C C2C C3C 113.8(15) . . ?
C1C C2C C3C 108.6(15) . . ?
O21C C2C H2C 108.1 . . ?
C1C C2C H2C 108.1 . . ?
C3C C2C H2C 108.1 . . ?
O31A C3A C4A 118(2) . . ?
O31A C3A C2A 124(2) . . ?
C4A C3A C2A 103(2) . . ?
O31A C3A H3A 102.8 . . ?
C4A C3A H3A 102.8 . . ?
C2A C3A H3A 102.8 . . ?
O31B C3B C4B 106.8(13) . . ?
O31B C3B C2B 111.6(13) . . ?
C4B C3B C2B 112.4(14) . . ?
O31B C3B H3B 108.7 . . ?
C4B C3B H3B 108.7 . . ?
C2B C3B H3B 108.7 . . ?
O31C C3C C4C 107.8(13) . . ?
O31C C3C C2C 111.8(13) . . ?
C4C C3C C2C 112.3(14) . . ?
O31C C3C H3C 108.3 . . ?
C4C C3C H3C 108.3 . . ?
C2C C3C H3C 108.3 . . ?
O41A C4A O42A 128(2) . . ?
O41A C4A C3A 107(2) . . ?
O42A C4A C3A 122(2) . . ?
O41B C4B O42B 125.5(17) . . ?
O41B C4B C3B 118.3(15) . . ?
O42B C4B C3B 116.2(15) . . ?
O42C C4C O41C 125.0(15) . . ?
O42C C4C C3C 117.8(14) . . ?
O41C C4C C3C 117.1(15) . . ?
C1B O11B Tb2 122.0(10) . . ?
C1C O11C Tb1 121.1(11) . . ?
C1A O12A Tb1 122.9(16) . . ?
C1B O12B Tb1 142.3(12) . . ?
C1C O12C Tb2 141.9(12) . 1_545 ?
C2A O21A Tb1 106.6(16) . . ?
C2A O21A H21A 115.2 . . ?
Tb1 O21A H21A 86.8 . . ?
C2B O21B Tb2 116.0(10) . . ?
C2B O21B H21B 103.7 . . ?
Tb2 O21B H21B 98.9 . . ?
C2C O21C Tb1 115.0(10) . . ?
C2C O21C H21C 107.4 . . ?
Tb1 O21C H21C 104.7 . . ?
C3A O31A Tb2 113.3(15) . 1_656 ?
C3A O31A H31A 112.9 . . ?
Tb2 O31A H31A 126.4 1_656 . ?
C3B O31B Tb1 120.2(9) . 1_565 ?
C3B O31B H31B 87.3 . . ?
Tb1 O31B H31B 61.7 1_565 . ?
C3C O31C Tb2 120.3(10) . . ?
C3C O31C H31C 88.1 . . ?
Tb2 O31C H31C 50.4 . . ?
C4A O41A Tb2 132.3(16) . 1_656 ?
C4B O41B Tb1 126.8(11) . 1_565 ?
C4C O41C Tb2 127.2(11) . . ?
C4A O42A Tb1 135.1(14) . . ?
C4B O42B Tb1 127.6(11) . 1_465 ?
C4C O42C Tb2 128.4(10) . 1_655 ?
Tb2 O1W H11W 119.3 . . ?
Tb2 O1W H12W 89.8 . . ?
H11W O1W H12W 103.9 . . ?
H21W O2W H22W 105.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O41B 0.88 2.02 2.870(19) 163.7 1_645 yes
O31A H31A O11A 0.85 2.12 2.96(3) 168.0 1_655 yes
O21B H21B O11C 0.85 1.74 2.584(16) 172.0 1_565 yes
O31B H31B O11C 0.86 1.98 2.821(17) 167.0 1_565 yes
O21C H21C O11B 0.86 1.76 2.598(16) 164.2 . yes
O31C H31C O11B 0.85 1.98 2.814(18) 166.4 . yes
O1W H11W O11A 0.86 1.59 2.41(3) 156.7 1_454 yes
O1W H12W O41C 0.85 2.03 2.870(19) 167.0 1_455 yes
O2W H21W O42A 0.97 1.65 2.45(5) 136.2 1_554 yes
O2W H22W O11A 0.85 1.65 2.45(6) 156.8 1_544 yes

_refine_diff_density_max         2.821
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.229


# start Validation Reply Form
_vrf_PLAT090_Compound_Tb-L-act1  
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.77 Note  
RESPONSE: The data has been acquired for a crystalline phase generated after
heating a single crystal up to 110 \^A?C. This fact has to be added to the facts 
that all specimens of this compound crystallize as twins and that the crystal
structre chiral and triclinic. All in all, these are best possible data according
to the previous facts. 
;
_vrf_PLAT220_Compound_Tb-L-act1  
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        9.2 Ratio 
RESPONSE: During the solid state transformation of the structure, it is observed
that one of the tartrate ligands undergoes a deep rearrangement (it changes its 
coordination mode). As a result, the ligand seems to be involved in some kind of
disorder. All our efforts to correctly handle that disorder have been unfruitful,
in such a way that ellipsoids of that ligand, as well as those in the surroundings,
are clearly affected. The refinement has been converged by using some soft restraints.
;
_vrf_PLAT342_Compound_Tb-L-act1  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03222 Ang.  
RESPONSE: During the solid state transformation of the structure, it is observed
that one of the tartrate ligands undergoes a deep rearrangement (it changes its 
coordination mode). As a result, the ligand seems to be involved in some kind of
disorder. All our efforts to correctly handle that disorder have been unfruitful,
in such a way that ellipsoids of that ligand, as well as those in the surroundings,
are clearly affected. The refinement has been converged by using some soft restraints.
;
_vrf_PLAT971_Compound_Tb-L-act1  
;
PROBLEM: Check Calcd Resid. Dens.  1.29A   From O11A            2.60 eA-3  
RESPONSE: The residual positive and non-accounted density is derived from the occurrence
of a minor twin (which could not be solved) as well as the presence of a disordered 
tartrate ligand. 
;
# end Validation Reply Form
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound_Tb-L''
_database_code_depnum_ccdc_archive 'CCDC 1981575'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-Î?3O,O',O'':Î?2O''',O'''')aquaditerbium(III)] hydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H14 O19 Tb2'
_chemical_formula_sum            'C12 H14 O19 Tb2'
_chemical_formula_weight         780.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.8375(4)
_cell_length_b                   7.3805(5)
_cell_length_c                   11.9157(10)
_cell_angle_alpha                72.000(7)
_cell_angle_beta                 76.266(6)
_cell_angle_gamma                90.024(6)
_cell_volume                     472.77(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11484
_cell_measurement_theta_min      1.858
_cell_measurement_theta_max      28.141


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.740
_exptl_crystal_F_000             368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    7.523
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_T_max  2.439
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
Single crystals of this compound crystallize as a twinned specimen, 
but no twin law has been applied for the data reduction because, ohterwise,
agreement factors got worse.  
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω
_diffrn_reflns_number            3028
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.856
_diffrn_reflns_theta_max         26.052
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.608
_diffrn_reflns_point_group_measured_fraction_full 0.624
_reflns_number_total             2262
_reflns_number_gt                2219
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.236
_reflns_Friedel_fraction_max     0.232
_reflns_Friedel_fraction_full    0.248

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
The crystal is a twinned specimen but no twin law has been applied
during data reduction nor the refinement since it leads to better
agreement factors. Moreover, the structure possesses a strong
pseudosymmetry arising from the almost equivalent environment of the
two independent terbium atoms, which simulates a monoclinic unit cell.
In this almost completely dehydrated structure, one of the independent
tartrate ligands is disordered into two equivalent dispositions, a fact
that has been well solved by assuming that some carboxylate oxygen 
atoms of one of the disordered parts correspond to hydroxyl or water 
molecules of the alternate fragment. This disorder is consistent with 
the O9 donor set around both terbium atoms. All trials to finish the 
refinment with the monoclinic cell led to unsatisfactory results, 
because it causes a disorder in the terbium environment that worsens 
the agreement factors.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0544P)²+7.9107P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.06(4)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         2262
_refine_ls_number_parameters     334
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.1058
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.60948(10) 0.45353(9) 0.72652(7) 0.0171(3) Uani 1 1 d . . . . .
Tb2 Tb 0.26104(9) -0.25931(8) 1.15281(7) 0.0168(3) Uani 1 1 d . . . . .
C1A C 0.930(6) 0.650(4) 0.439(3) 0.047(7) Uani 1 1 d . U . . .
C2A C 1.130(7) 0.463(6) 0.460(4) 0.024(8) Uani 0.5 1 d . U P A 1
H2A H 1.232096 0.483664 0.509826 0.029 Uiso 0.5 1 calc R U P A 1
C3A C 0.967(6) 0.288(5) 0.530(3) 0.011(6) Uani 0.5 1 d . U P A 1
H3A H 1.044415 0.177941 0.513204 0.013 Uiso 0.5 1 calc R U P A 1
C4A C 0.716(8) 0.298(7) 0.491(5) 0.035(10) Uani 0.5 1 d . U P A 1
O42A O 0.710(6) 0.288(4) 0.397(3) 0.031(7) Uani 0.5 1 d . . P A 1
C2A1 C 0.743(8) 0.489(6) 0.422(4) 0.028(9) Uani 0.5 1 d . U P A 2
H2A1 H 0.641607 0.559535 0.371011 0.034 Uiso 0.5 1 calc R U P A 2
C3A1 C 0.908(6) 0.373(5) 0.349(3) 0.015(7) Uani 0.5 1 d . U P A 2
H3A1 H 0.829919 0.246113 0.367081 0.018 Uiso 0.5 1 calc R U P A 2
C4A1 C 1.156(7) 0.352(6) 0.386(4) 0.024(8) Uani 0.5 1 d . U P A 2
O421 O 1.162(6) 0.247(4) 0.482(3) 0.030(7) Uani 0.5 1 d . . P A 2
O11A O 0.835(2) 0.660(2) 0.5375(14) 0.027(3) Uani 1 1 d . . . . .
O12A O 1.039(2) 0.759(2) 0.3421(15) 0.030(4) Uani 1 1 d . . . . .
O1A O 0.572(3) 0.352(3) 0.555(2) 0.058(6) Uani 1 1 d . . . . .
O2A O 1.291(4) 0.466(3) 0.328(2) 0.058(6) Uani 1 1 d . . . . .
O3A O 0.918(3) 0.256(2) 0.6723(19) 0.036(4) Uani 1 1 d . . . . .
O4A O 0.952(3) 0.490(2) 0.2056(17) 0.035(4) Uani 1 1 d . . . . .
C1B C 0.334(4) 0.001(3) 0.8706(18) 0.021(4) Uani 1 1 d . . . . .
C2B C 0.156(4) -0.141(3) 0.868(2) 0.019(5) Uani 1 1 d . U . . .
H2B H 0.007594 -0.079245 0.868015 0.023 Uiso 1 1 calc R U . . .
C3B C 0.240(3) -0.180(3) 0.7435(18) 0.020(4) Uani 1 1 d . . . . .
H3B H 0.214612 -0.068187 0.678498 0.024 Uiso 1 1 calc R U . . .
C4B C 0.103(3) -0.353(3) 0.7419(17) 0.020(4) Uani 1 1 d . . . . .
O11B O 0.450(2) -0.0550(19) 0.9527(12) 0.019(3) Uani 1 1 d . . . . .
O12B O 0.367(3) 0.163(2) 0.7943(17) 0.033(4) Uani 1 1 d . . . . .
O21B O 0.114(2) -0.3003(19) 0.9711(13) 0.020(3) Uani 1 1 d . . . . .
O31B O 0.485(2) -0.2120(18) 0.7188(14) 0.022(3) Uani 1 1 d . . . . .
O41B O 0.223(2) -0.481(2) 0.7109(14) 0.022(3) Uani 1 1 d . . . . .
O42B O -0.118(2) -0.3586(18) 0.7696(13) 0.019(3) Uani 1 1 d . . . . .
C1C C 0.535(3) 0.431(3) 1.0092(18) 0.020(4) Uani 1 1 d . . . . .
C2C C 0.722(4) 0.286(3) 1.011(2) 0.021(5) Uani 1 1 d . U . . .
H2C H 0.870602 0.347372 1.010592 0.025 Uiso 1 1 calc R U . . .
C3C C 0.632(3) 0.122(3) 1.1362(18) 0.020(4) Uani 1 1 d . . . . .
H3C H 0.655383 0.167810 1.201770 0.024 Uiso 1 1 calc R U . . .
C4C C 0.767(3) -0.053(3) 1.1372(18) 0.020(4) Uani 1 1 d . . . . .
O11C O 0.422(2) 0.4588(18) 0.9266(13) 0.021(3) Uani 1 1 d . . . . .
O12C O 0.502(3) 0.518(3) 1.0865(18) 0.039(4) Uani 1 1 d . . . . .
O21C O 0.758(2) 0.2283(18) 0.9101(13) 0.018(3) Uani 1 1 d . . . . .
O31C O 0.390(2) 0.0641(18) 1.1595(13) 0.020(3) Uani 1 1 d . . . . .
O41C O 0.649(2) -0.210(2) 1.1680(14) 0.020(3) Uani 1 1 d . . . . .
O42C O 0.989(2) -0.0266(19) 1.1090(14) 0.022(3) Uani 1 1 d . . . . .
H21B H 0.216289 -0.382304 0.965599 0.033 Uiso 1 1 d . U . . .
H31B H 0.447218 -0.303539 0.786784 0.033 Uiso 1 1 d . U . . .
H21C H 0.641920 0.144941 0.928083 0.033 Uiso 1 1 d . U . . .
H31C H 0.312287 0.154511 1.175882 0.033 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O41B 2.347(14) 1_565 ?
Tb1 O42B 2.355(12) 1_665 ?
Tb1 O11A 2.366(15) . ?
Tb1 O12B 2.376(14) . ?
Tb1 O11C 2.388(14) . ?
Tb1 O3A 2.410(15) . ?
Tb1 O1A 2.443(19) . ?
Tb1 O31B 2.554(13) 1_565 ?
Tb1 O21C 2.638(14) . ?
Tb2 O41C 2.351(13) . ?
Tb2 O42C 2.363(13) 1_455 ?
Tb2 O12C 2.363(15) 1_545 ?
Tb2 O12A 2.365(15) 1_446 ?
Tb2 O11B 2.389(14) . ?
Tb2 O4A 2.410(15) 1_446 ?
Tb2 O2A 2.460(19) 1_446 ?
Tb2 O31C 2.532(13) . ?
Tb2 O21B 2.610(14) . ?
C1A O11A 1.19(4) . ?
C1A O12A 1.21(4) . ?
C1A C2A1 1.70(5) . ?
C1A C2A 1.81(5) . ?
C2A C3A 1.49(5) . ?
C2A O2A 1.63(5) . ?
C2A H2A 0.9800 . ?
C3A O3A 1.60(4) . ?
C3A C4A 1.63(6) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.15(6) . ?
C4A O1A 1.15(5) . ?
C2A1 C3A1 1.57(5) . ?
C2A1 O1A 1.67(5) . ?
C2A1 H2A1 0.9800 . ?
C3A1 C4A1 1.60(5) . ?
C3A1 O4A 1.62(4) . ?
C3A1 H3A1 0.9800 . ?
C4A1 O2A 1.09(4) . ?
C4A1 O421 1.18(5) . ?
C1B O12B 1.24(2) . ?
C1B O11B 1.28(3) . ?
C1B C2B 1.49(3) . ?
C2B O21B 1.38(3) . ?
C2B C3B 1.57(3) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.43(2) . ?
C3B C4B 1.51(3) . ?
C3B H3B 0.9800 . ?
C4B O42B 1.25(2) . ?
C4B O41B 1.27(2) . ?
O21B H21B 0.8572 . ?
O31B H31B 0.8589 . ?
C1C O12C 1.26(2) . ?
C1C O11C 1.27(2) . ?
C1C C2C 1.53(3) . ?
C2C O21C 1.36(3) . ?
C2C C3C 1.58(3) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.41(2) . ?
C3C C4C 1.51(3) . ?
C3C H3C 0.9800 . ?
C4C O41C 1.26(2) . ?
C4C O42C 1.26(2) . ?
O21C H21C 0.8568 . ?
O31C H31C 0.8519 . ?

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
O41B Tb1 O42B 127.6(5) 1_565 1_665 ?
O41B Tb1 O11A 101.4(5) 1_565 . ?
O42B Tb1 O11A 72.9(5) 1_665 . ?
O41B Tb1 O12B 70.3(5) 1_565 . ?
O42B Tb1 O12B 146.6(5) 1_665 . ?
O11A Tb1 O12B 136.3(6) . . ?
O41B Tb1 O11C 78.0(5) 1_565 . ?
O42B Tb1 O11C 76.3(5) 1_665 . ?
O11A Tb1 O11C 140.0(5) . . ?
O12B Tb1 O11C 81.8(6) . . ?
O41B Tb1 O3A 140.9(5) 1_565 . ?
O42B Tb1 O3A 90.2(5) 1_665 . ?
O11A Tb1 O3A 78.2(6) . . ?
O12B Tb1 O3A 83.1(6) . . ?
O11C Tb1 O3A 127.0(6) . . ?
O41B Tb1 O1A 76.2(6) 1_565 . ?
O42B Tb1 O1A 137.5(7) 1_665 . ?
O11A Tb1 O1A 67.4(7) . . ?
O12B Tb1 O1A 69.0(7) . . ?
O11C Tb1 O1A 146.1(6) . . ?
O3A Tb1 O1A 67.6(6) . . ?
O41B Tb1 O31B 62.5(5) 1_565 1_565 ?
O42B Tb1 O31B 66.0(5) 1_665 1_565 ?
O11A Tb1 O31B 74.7(5) . 1_565 ?
O12B Tb1 O31B 128.5(5) . 1_565 ?
O11C Tb1 O31B 69.8(5) . 1_565 ?
O3A Tb1 O31B 148.1(5) . 1_565 ?
O1A Tb1 O31B 115.5(6) . 1_565 ?
O41B Tb1 O21C 129.7(5) 1_565 . ?
O42B Tb1 O21C 73.1(4) 1_665 . ?
O11A Tb1 O21C 128.7(5) . . ?
O12B Tb1 O21C 74.5(5) . . ?
O11C Tb1 O21C 62.3(4) . . ?
O3A Tb1 O21C 64.7(6) . . ?
O1A Tb1 O21C 122.1(6) . . ?
O31B Tb1 O21C 122.5(4) 1_565 . ?
O41C Tb2 O42C 127.4(5) . 1_455 ?
O41C Tb2 O12C 70.0(5) . 1_545 ?
O42C Tb2 O12C 146.9(5) 1_455 1_545 ?
O41C Tb2 O12A 101.0(5) . 1_446 ?
O42C Tb2 O12A 73.3(6) 1_455 1_446 ?
O12C Tb2 O12A 136.0(6) 1_545 1_446 ?
O41C Tb2 O11B 77.7(5) . . ?
O42C Tb2 O11B 76.3(5) 1_455 . ?
O12C Tb2 O11B 81.9(6) 1_545 . ?
O12A Tb2 O11B 140.0(5) 1_446 . ?
O41C Tb2 O4A 141.2(5) . 1_446 ?
O42C Tb2 O4A 90.2(5) 1_455 1_446 ?
O12C Tb2 O4A 83.2(6) 1_545 1_446 ?
O12A Tb2 O4A 79.0(6) 1_446 1_446 ?
O11B Tb2 O4A 126.7(5) . 1_446 ?
O41C Tb2 O2A 77.2(6) . 1_446 ?
O42C Tb2 O2A 136.6(7) 1_455 1_446 ?
O12C Tb2 O2A 69.5(8) 1_545 1_446 ?
O12A Tb2 O2A 66.5(7) 1_446 1_446 ?
O11B Tb2 O2A 146.9(6) . 1_446 ?
O4A Tb2 O2A 67.3(6) 1_446 1_446 ?
O41C Tb2 O31C 62.0(5) . . ?
O42C Tb2 O31C 66.3(5) 1_455 . ?
O12C Tb2 O31C 127.8(5) 1_545 . ?
O12A Tb2 O31C 74.7(5) 1_446 . ?
O11B Tb2 O31C 69.6(4) . . ?
O4A Tb2 O31C 148.7(5) 1_446 . ?
O2A Tb2 O31C 115.5(6) 1_446 . ?
O41C Tb2 O21B 129.6(5) . . ?
O42C Tb2 O21B 73.1(5) 1_455 . ?
O12C Tb2 O21B 74.9(5) 1_545 . ?
O12A Tb2 O21B 129.3(5) 1_446 . ?
O11B Tb2 O21B 62.4(4) . . ?
O4A Tb2 O21B 64.3(5) 1_446 . ?
O2A Tb2 O21B 122.0(5) 1_446 . ?
O31C Tb2 O21B 122.5(5) . . ?
O11A C1A O12A 137(2) . . ?
O11A C1A C2A1 102(3) . . ?
O12A C1A C2A1 112(3) . . ?
O11A C1A C2A 108(3) . . ?
O12A C1A C2A 100(2) . . ?
C3A C2A O2A 116(3) . . ?
C3A C2A C1A 103(3) . . ?
O2A C2A C1A 109(3) . . ?
C3A C2A H2A 109.5 . . ?
O2A C2A H2A 109.5 . . ?
C1A C2A H2A 109.5 . . ?
C2A C3A O3A 110(3) . . ?
C2A C3A C4A 112(3) . . ?
O3A C3A C4A 109(3) . . ?
C2A C3A H3A 108.3 . . ?
O3A C3A H3A 108.3 . . ?
C4A C3A H3A 108.3 . . ?
O42A C4A O1A 126(5) . . ?
O42A C4A C3A 120(4) . . ?
O1A C4A C3A 112(4) . . ?
C3A1 C2A1 O1A 113(3) . . ?
C3A1 C2A1 C1A 105(3) . . ?
O1A C2A1 C1A 112(3) . . ?
C3A1 C2A1 H2A1 108.6 . . ?
O1A C2A1 H2A1 108.6 . . ?
C1A C2A1 H2A1 108.6 . . ?
C2A1 C3A1 C4A1 110(3) . . ?
C2A1 C3A1 O4A 107(3) . . ?
C4A1 C3A1 O4A 110(3) . . ?
C2A1 C3A1 H3A1 109.8 . . ?
C4A1 C3A1 H3A1 109.8 . . ?
O4A C3A1 H3A1 109.8 . . ?
O2A C4A1 O421 126(4) . . ?
O2A C4A1 C3A1 114(4) . . ?
O421 C4A1 C3A1 119(4) . . ?
C1A O11A Tb1 137.9(16) . . ?
C1A O12A Tb2 137.6(15) . 1_664 ?
C4A O1A Tb1 128(3) . . ?
C2A1 O1A Tb1 112.9(18) . . ?
C2A O2A Tb2 116.1(18) . 1_664 ?
C3A O3A Tb1 108.5(15) . . ?
O12B C1B O11B 123.5(19) . . ?
O12B C1B C2B 119.8(19) . . ?
O11B C1B C2B 116.6(17) . . ?
O21B C2B C1B 112.0(18) . . ?
O21B C2B C3B 115.7(18) . . ?
C1B C2B C3B 107.3(17) . . ?
O21B C2B H2B 107.2 . . ?
C1B C2B H2B 107.2 . . ?
C3B C2B H2B 107.2 . . ?
O31B C3B C4B 108.0(15) . . ?
O31B C3B C2B 110.9(16) . . ?
C4B C3B C2B 111.8(16) . . ?
O31B C3B H3B 108.7 . . ?
C4B C3B H3B 108.7 . . ?
C2B C3B H3B 108.7 . . ?
O42B C4B O41B 124.9(18) . . ?
O42B C4B C3B 117.9(17) . . ?
O41B C4B C3B 117.1(17) . . ?
C1B O11B Tb2 120.9(12) . . ?
C1B O12B Tb1 142.2(14) . . ?
C2B O21B Tb2 115.1(12) . . ?
C2B O21B H21B 112.6 . . ?
Tb2 O21B H21B 88.1 . . ?
C3B O31B Tb1 119.5(10) . 1_545 ?
C3B O31B H31B 85.3 . . ?
Tb1 O31B H31B 60.5 1_545 . ?
C4B O41B Tb1 127.0(13) . 1_545 ?
C4B O42B Tb1 128.6(12) . 1_445 ?
O12C C1C O11C 123.4(19) . . ?
O12C C1C C2C 119.4(18) . . ?
O11C C1C C2C 117.2(18) . . ?
O21C C2C C1C 111.2(18) . . ?
O21C C2C C3C 115.1(18) . . ?
C1C C2C C3C 105.2(17) . . ?
O21C C2C H2C 108.4 . . ?
C1C C2C H2C 108.4 . . ?
C3C C2C H2C 108.4 . . ?
O31C C3C C4C 107.2(15) . . ?
O31C C3C C2C 112.1(16) . . ?
C4C C3C C2C 110.7(16) . . ?
O31C C3C H3C 108.9 . . ?
C4C C3C H3C 108.9 . . ?
C2C C3C H3C 108.9 . . ?
O41C C4C O42C 126.2(18) . . ?
O41C C4C C3C 117.3(17) . . ?
O42C C4C C3C 116.5(17) . . ?
C1C O11C Tb1 121.6(13) . . ?
C1C O12C Tb2 141.8(13) . 1_565 ?
C2C O21C Tb1 115.3(12) . . ?
C2C O21C H21C 103.1 . . ?
Tb1 O21C H21C 91.7 . . ?
C3C O31C Tb2 120.9(11) . . ?
C3C O31C H31C 106.6 . . ?
Tb2 O31C H31C 132.5 . . ?
C4C O41C Tb2 127.0(12) . . ?
C4C O42C Tb2 127.1(13) . 1_655 ?

_refine_diff_density_max         2.531
_refine_diff_density_min         -1.803
_refine_diff_density_rms         0.263



# start Validation Reply Form
_vrf_PLAT090_Compound_Tb-L''     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.77 Note  
RESPONSE: The data has been acquired for a crystalline phase generated after
heating a single crystal up to 210 \^A?C. This fact has to be added to the facts 
that all specimens of this compound crystallize as twins and that the crystal
structure is chiral and triclinic. All in all, these are best possible data 
according to the previous facts. 
;
_vrf_PLAT342_Compound_Tb-L''     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03222 Ang.  
RESPONSE: During the solid state transformation of the structure, it is observed
that one of the tartrate ligands undergoes a deep rearrangement (it changes its 
coordination mode). As a result, the ligand is disordered into two equivalent
dispositions, which has been solved using restraints for the occupation of some 
atoms, which distorts the bond distances.
;
_vrf_PLAT971_Compound_Tb-L''     
;
PROBLEM: Check Calcd Resid. Dens.  1.01A   From Tb1            2.56 eA-3  
RESPONSE: The residual positive and non-accounted density is derived from the 
occurrence of a minor twin (which could not be solved) as well as the presence
of a disordered tartrate ligand. 
;
_vrf_PLAT112_Compound_Tb-L''     
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         2        100 %Fit  
RESPONSE: As explained before in refinement details section, the structure 
possesses a strong pseudosymmetry arising from the disordered tartrate ligand
that simulates two perfectly equivalent terbium(III) environemtns, which
in turn simulates a monoclinic unit cell.
In this almost completely dehydrated structure, one of the independent
tartrate ligands is disordered into two equivalent dispositions, a fact
that has been well solved by assuming that some carboxylate oxygen 
atoms of one of the disordered parts correspond to hydroxyl or water 
molecules of the alternate fragment. This disorder is consistent with 
the O9 donor set around both terbium atoms. All trials to finish the 
refinment with the monoclinic cell led to unsatisfactory results, 
because it causes a disorder in the terbium environment that penalizes
the agreement factors.
;
_vrf_PLAT113_Compound_Tb-L''     
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group         I2 Check 
RESPONSE: As explained before in refinement details section, the structure 
possesses a strong pseudosymmetry arising from the disordered tartrate ligand
that simulates two perfectly equivalent terbium(III) environemtns, which
in turn simulates a monoclinic unit cell.
In this almost completely dehydrated structure, one of the independent
tartrate ligands is disordered into two equivalent dispositions, a fact
that has been well solved by assuming that some carboxylate oxygen 
atoms of one of the disordered parts correspond to hydroxyl or water 
molecules of the alternate fragment. This disorder is consistent with 
the O9 donor set around both terbium atoms. All trials to finish the 
refinment with the monoclinic cell led to unsatisfactory results, 
because it causes a disorder in the terbium environment that penalizes
the agreement factors.
;
_vrf_PLAT420_Compound_Tb-L''     
;
PROBLEM: D-H Without Acceptor       O31C     --H31C     .     Please Check 
RESPONSE: The fact that all water molecules crystallized as lattice molecules
have been lost during the thermal treatment applied to this single crystal
makes that hydroxyl groups have no adequate receptors with which establish
hydrogen bonding interactions. Although this group possesses some coordinated
oxygen atoms in the neighborhood, hydrogen atom acquires an incorrect disposition
around terbium atom. 
;
_vrf_PLAT430_Compound_Tb-L''     
;
PROBLEM: Short Inter D...A Contact  O2A      ..O12C     .       2.75 Ang.  
RESPONSE: A hydrogen bonding interaction exists between these two atoms although
no hydrogen atoms were refined in the surroundings of A ligand due to the disorder
existing, where some atoms, such as O2A correspond at the same time to carboxylate
and hydroxyl oxygen atoms.
;
_vrf_PLAT915_Compound_Tb-L''     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         23 %     
RESPONSE: Despite the fact that the Friedel Pair Coverage is low in this structure
as to clearly state its chirality, it must be taken into account that it comes from
a previously measured compound that has been heated at 210 \^A?C in order to be dehydrated.
Taking into account that chiral tartrate ligands have been employed in the syntheses,
crystal structure keeps its chiral nature upon dehydration.
;
# end Validation Reply Form
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound_Er-L
_database_code_depnum_ccdc_archive 'CCDC 1981580'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-k2O,O':k2O'',O''')diaquadierbium(III)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Er2 O20, 4(H2 O)'
_chemical_formula_sum            'C12 H24 Er2 O24'
_chemical_formula_weight         886.83

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

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9743(4)
_cell_length_b                   7.3542(5)
_cell_length_c                   13.1941(9)
_cell_angle_alpha                102.422(2)
_cell_angle_beta                 101.664(2)
_cell_angle_gamma                90.613(2)
_cell_volume                     553.55(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20350
_cell_measurement_theta_min      2.857
_cell_measurement_theta_max      28.831


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.660
_exptl_crystal_F_000             424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    7.648
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_process_details   
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_reflns_number            10693
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.234
_diffrn_reflns_theta_max         31.924
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.790
_diffrn_measured_fraction_theta_full 0.901
_diffrn_reflns_Laue_measured_fraction_max 0.790
_diffrn_reflns_Laue_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.648
_diffrn_reflns_point_group_measured_fraction_full 0.804
_reflns_number_total             4935
_reflns_number_gt                4464
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.641
_reflns_Friedel_fraction_max     0.506
_reflns_Friedel_fraction_full    0.707

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;


_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0790P)²+1.1119P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1650 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(19)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         4935
_refine_ls_number_parameters     344
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1115
_refine_ls_wR_factor_gt          0.1056
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.082
_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
Er1 Er 0.02237(6) 0.81754(5) 0.67817(4) 0.00702(19) Uani 1 1 d . . . . .
Er2 Er -0.02326(7) 0.18337(6) 0.32291(4) 0.0085(2) Uani 1 1 d . . . . .
C1A C 0.217(3) 0.935(2) 0.8937(13) 0.013(4) Uani 1 1 d . U . . .
C2A C 0.377(2) 1.030(2) 0.9986(11) 0.010(3) Uani 1 1 d . U . . .
H2A H 0.361117 0.960519 1.052600 0.012 Uiso 1 1 calc R U . . .
C3A C 0.625(2) 1.026(2) 0.9850(10) 0.009(2) Uani 1 1 d . U . . .
H3A H 0.657132 0.897156 0.956967 0.011 Uiso 1 1 calc R U . . .
C4A C 0.782(3) 1.095(2) 1.0968(13) 0.011(3) Uani 1 1 d . U . . .
C1B C 0.159(2) 0.3867(19) 0.5667(10) 0.010(2) Uani 1 1 d . U . . .
C2B C 0.344(2) 0.248(2) 0.5649(10) 0.005(2) Uani 1 1 d . U . . .
H2B H 0.486062 0.313271 0.562640 0.006 Uiso 1 1 calc R U . . .
C3B C 0.383(2) 0.1785(18) 0.6658(10) 0.007(2) Uani 1 1 d . U . . .
H3B H 0.468649 0.276784 0.723339 0.008 Uiso 1 1 calc R U . . .
C4B C 0.513(2) -0.0001(19) 0.6628(10) 0.010(2) Uani 1 1 d . U . . .
C1C C -0.151(2) 0.831(2) 0.4322(11) 0.013(3) Uani 1 1 d . . . . .
C2C C -0.339(2) 0.693(2) 0.4360(10) 0.004(2) Uani 1 1 d . U . . .
H2C H -0.479589 0.759729 0.438874 0.004 Uiso 1 1 calc R U . . .
C3C C -0.377(2) 0.5496(19) 0.3320(10) 0.010(2) Uani 1 1 d . U . . .
H3C H -0.459971 0.605856 0.275485 0.012 Uiso 1 1 calc R U . . .
C4C C -0.513(2) 0.374(2) 0.3336(10) 0.010(2) Uani 1 1 d . . . . .
O11A O 0.2628(18) 0.7729(14) 0.8468(8) 0.0121(19) Uani 1 1 d . . . . .
O12A O 0.0467(18) 1.0122(14) 0.8547(8) 0.0115(19) Uani 1 1 d . U . . .
O21A O 0.3252(17) 1.2204(14) 1.0352(8) 0.0106(18) Uani 1 1 d . . . . .
O31A O 0.6506(18) 1.1321(16) 0.9110(8) 0.014(2) Uani 1 1 d . . . . .
O41A O 0.7545(18) 1.0085(17) 1.1646(8) 0.017(2) Uani 1 1 d . . . . .
O42A O 0.9232(19) 1.2283(17) 1.1163(9) 0.020(2) Uani 1 1 d . . . . .
O11B O -0.018(2) 0.3506(16) 0.4911(8) 0.017(2) Uani 1 1 d . . . . .
O12B O 0.1795(18) 0.5253(13) 0.6436(8) 0.0091(18) Uani 1 1 d . . . . .
O21B O 0.2840(17) 0.1053(14) 0.4712(7) 0.0094(18) Uani 1 1 d . U . . .
O31B O 0.1644(17) 0.1402(15) 0.6911(8) 0.0102(19) Uani 1 1 d . U . . .
O41B O 0.4085(19) -0.1458(16) 0.6686(8) 0.013(2) Uani 1 1 d . U . . .
O42B O 0.7209(17) 0.0107(14) 0.6550(7) 0.0106(18) Uani 1 1 d . U . . .
O11C O 0.0245(17) 0.8502(13) 0.5085(7) 0.0078(17) Uani 1 1 d . U . . .
O12C O -0.1771(16) 0.9154(14) 0.3608(8) 0.0094(18) Uani 1 1 d . . . . .
O21C O -0.2804(17) 0.6212(14) 0.5278(7) 0.0092(18) Uani 1 1 d . U . . .
O31C O -0.1632(17) 0.4868(15) 0.3050(8) 0.0118(19) Uani 1 1 d . . . . .
O41C O -0.4089(18) 0.2250(16) 0.3329(8) 0.012(2) Uani 1 1 d . U . . .
O42C O -0.7239(18) 0.3864(14) 0.3350(8) 0.0116(19) Uani 1 1 d . U . . .
O1W O -0.2423(19) 0.6563(15) 0.7405(8) 0.013(2) Uani 1 1 d . U . . .
O2W O 0.2270(18) -0.0237(14) 0.2509(8) 0.0116(19) Uani 1 1 d . U . . .
O3W O 0.190(2) 0.413(2) 0.8700(11) 0.024(3) Uani 1 1 d . . . . .
O4W O -0.293(4) 0.621(3) 0.1275(14) 0.059(6) Uani 1 1 d . . . . .
O5W O 0.218(3) -0.359(2) 0.1161(13) 0.051(4) Uani 1 1 d . . . . .
O6W O -0.218(2) 0.5081(15) 0.9268(8) 0.015(2) Uani 1 1 d . U . . .
H21A H 0.205044 1.230559 1.060734 0.023 Uiso 1 1 d . U . . .
H31A H 0.781856 1.108674 0.896993 0.023 Uiso 1 1 d . U . . .
H21B H 0.209316 0.015610 0.483677 0.023 Uiso 1 1 d . U . . .
H31B H 0.177068 0.179585 0.756820 0.023 Uiso 1 1 d . U . . .
H21C H -0.204220 0.524486 0.520618 0.023 Uiso 1 1 d . U . . .
H31C H -0.160249 0.523445 0.246945 0.023 Uiso 1 1 d . U . . .
H11W H -0.234431 0.640855 0.805056 0.023 Uiso 1 1 d . U . . .
H12W H -0.376469 0.690512 0.723975 0.023 Uiso 1 1 d . U . . .
H21W H 0.214447 -0.099326 0.190584 0.023 Uiso 1 1 d . U . . .
H22W H 0.361306 0.026318 0.262713 0.023 Uiso 1 1 d . U . . .
H31W H 0.257142 0.374469 0.923286 0.023 Uiso 1 1 d . U . . .
H32W H 0.236680 0.530140 0.878932 0.023 Uiso 1 1 d . U . . .
H41W H -0.220204 0.729794 0.146679 0.023 Uiso 1 1 d . U . . .
H42W H -0.307508 0.596028 0.060313 0.023 Uiso 1 1 d . U . . .
H51W H 0.355607 -0.374142 0.107352 0.023 Uiso 1 1 d . U . . .
H52W H 0.136132 -0.426220 0.060976 0.023 Uiso 1 1 d . U . . .
H61W H -0.335386 0.423821 0.909024 0.023 Uiso 1 1 d . U . . .
H62W H -0.107083 0.441502 0.921448 0.023 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O11C 2.305(9) . ?
Er1 O42B 2.318(10) 1_465 ?
Er1 O1W 2.343(11) . ?
Er1 O12B 2.346(10) . ?
Er1 O41B 2.351(11) 1_565 ?
Er1 O12A 2.433(10) . ?
Er1 O31B 2.470(11) 1_565 ?
Er1 O11A 2.481(10) . ?
Er1 O21C 2.560(10) . ?
Er1 C1A 2.787(17) . ?
Er2 O42C 2.276(11) 1_655 ?
Er2 O11B 2.288(11) . ?
Er2 O2W 2.336(10) . ?
Er2 O41A 2.338(11) 1_444 ?
Er2 O41C 2.354(11) . ?
Er2 O12C 2.356(10) 1_545 ?
Er2 O31C 2.434(11) . ?
Er2 O21B 2.565(10) . ?
Er2 O42A 2.772(12) 1_444 ?
Er2 C4A 2.902(16) 1_444 ?
C1A O12A 1.24(2) . ?
C1A O11A 1.283(19) . ?
C1A C2A 1.53(2) . ?
C2A O21A 1.438(17) . ?
C2A C3A 1.526(18) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.403(18) . ?
C3A C4A 1.56(2) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.23(2) . ?
C4A O41A 1.24(2) . ?
C1B O12B 1.259(17) . ?
C1B O11B 1.278(17) . ?
C1B C2B 1.52(2) . ?
C2B O21B 1.418(16) . ?
C2B C3B 1.501(18) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.450(16) . ?
C3B C4B 1.531(18) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.260(18) . ?
C4B O42B 1.268(17) . ?
C1C O12C 1.219(18) . ?
C1C O11C 1.283(16) . ?
C1C C2C 1.52(2) . ?
C2C O21C 1.408(16) . ?
C2C C3C 1.515(18) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.448(17) . ?
C3C C4C 1.53(2) . ?
C3C H3C 0.9800 . ?
C4C O42C 1.265(17) . ?
C4C O41C 1.266(18) . ?
O21A H21A 0.8499 . ?
O31A H31A 0.8520 . ?
O21B H21B 0.8553 . ?
O31B H31B 0.8407 . ?
O21C H21C 0.8474 . ?
O31C H31C 0.8677 . ?
O1W H11W 0.8750 . ?
O1W H12W 0.8434 . ?
O2W H21W 0.8564 . ?
O2W H22W 0.8495 . ?
O3W H31W 0.8431 . ?
O3W H32W 0.8777 . ?
O4W H41W 0.8694 . ?
O4W H42W 0.8516 . ?
O5W H51W 0.8604 . ?
O5W H52W 0.8411 . ?
O6W H61W 0.8921 . ?
O6W H62W 0.8312 . ?

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
O11C Er1 O42B 80.4(3) . 1_465 ?
O11C Er1 O1W 130.0(3) . . ?
O42B Er1 O1W 81.7(4) 1_465 . ?
O11C Er1 O12B 90.7(3) . . ?
O42B Er1 O12B 151.3(3) 1_465 . ?
O1W Er1 O12B 83.4(4) . . ?
O11C Er1 O41B 73.4(4) . 1_565 ?
O42B Er1 O41B 131.5(4) 1_465 1_565 ?
O1W Er1 O41B 145.5(4) . 1_565 ?
O12B Er1 O41B 69.9(4) . 1_565 ?
O11C Er1 O12A 139.1(3) . . ?
O42B Er1 O12A 76.4(3) 1_465 . ?
O1W Er1 O12A 79.1(4) . . ?
O12B Er1 O12A 124.4(3) . . ?
O41B Er1 O12A 97.9(4) 1_565 . ?
O11C Er1 O31B 72.5(3) . 1_565 ?
O42B Er1 O31B 69.1(3) 1_465 1_565 ?
O1W Er1 O31B 139.9(4) . 1_565 ?
O12B Er1 O31B 134.0(4) . 1_565 ?
O41B Er1 O31B 64.4(4) 1_565 1_565 ?
O12A Er1 O31B 68.0(4) . 1_565 ?
O11C Er1 O11A 144.8(4) . . ?
O42B Er1 O11A 128.3(3) 1_465 . ?
O1W Er1 O11A 79.5(3) . . ?
O12B Er1 O11A 72.2(3) . . ?
O41B Er1 O11A 71.9(4) 1_565 . ?
O12A Er1 O11A 52.9(3) . . ?
O31B Er1 O11A 97.2(3) 1_565 . ?
O11C Er1 O21C 63.1(3) . . ?
O42B Er1 O21C 75.5(3) 1_465 . ?
O1W Er1 O21C 67.4(3) . . ?
O12B Er1 O21C 76.2(3) . . ?
O41B Er1 O21C 123.4(3) 1_565 . ?
O12A Er1 O21C 138.7(3) . . ?
O31B Er1 O21C 126.6(3) 1_565 . ?
O11A Er1 O21C 136.2(3) . . ?
O11C Er1 C1A 146.5(5) . . ?
O42B Er1 C1A 102.8(4) 1_465 . ?
O1W Er1 C1A 83.0(5) . . ?
O12B Er1 C1A 99.6(4) . . ?
O41B Er1 C1A 80.4(5) 1_565 . ?
O12A Er1 C1A 26.4(4) . . ?
O31B Er1 C1A 77.6(4) 1_565 . ?
O11A Er1 C1A 27.4(4) . . ?
O21C Er1 C1A 150.3(4) . . ?
O42C Er2 O11B 82.7(4) 1_655 . ?
O42C Er2 O2W 80.2(4) 1_655 . ?
O11B Er2 O2W 132.9(4) . . ?
O42C Er2 O41A 125.2(4) 1_655 1_444 ?
O11B Er2 O41A 146.6(4) . 1_444 ?
O2W Er2 O41A 75.3(4) . 1_444 ?
O42C Er2 O41C 132.8(4) 1_655 . ?
O11B Er2 O41C 74.1(4) . . ?
O2W Er2 O41C 144.1(4) . . ?
O41A Er2 O41C 73.1(4) 1_444 . ?
O42C Er2 O12C 151.2(3) 1_655 1_545 ?
O11B Er2 O12C 91.2(4) . 1_545 ?
O2W Er2 O12C 83.7(4) . 1_545 ?
O41A Er2 O12C 72.3(4) 1_444 1_545 ?
O41C Er2 O12C 70.9(4) . 1_545 ?
O42C Er2 O31C 70.1(4) 1_655 . ?
O11B Er2 O31C 73.5(4) . . ?
O2W Er2 O31C 137.4(4) . . ?
O41A Er2 O31C 97.3(4) 1_444 . ?
O41C Er2 O31C 64.1(4) . . ?
O12C Er2 O31C 134.9(3) 1_545 . ?
O42C Er2 O21B 76.7(3) 1_655 . ?
O11B Er2 O21B 63.8(3) . . ?
O2W Er2 O21B 69.6(3) . . ?
O41A Er2 O21B 134.2(4) 1_444 . ?
O41C Er2 O21B 124.5(3) . . ?
O12C Er2 O21B 75.4(3) 1_545 . ?
O31C Er2 O21B 128.4(3) . . ?
O42C Er2 O42A 77.7(3) 1_655 1_444 ?
O11B Er2 O42A 141.0(4) . 1_444 ?
O2W Er2 O42A 76.3(3) . 1_444 ?
O41A Er2 O42A 49.4(4) 1_444 1_444 ?
O41C Er2 O42A 95.3(3) . 1_444 ?
O12C Er2 O42A 121.3(3) 1_545 1_444 ?
O31C Er2 O42A 68.2(3) . 1_444 ?
O21B Er2 O42A 140.1(3) . 1_444 ?
O42C Er2 C4A 102.2(4) 1_655 1_444 ?
O11B Er2 C4A 150.8(4) . 1_444 ?
O2W Er2 C4A 76.0(4) . 1_444 ?
O41A Er2 C4A 24.5(4) 1_444 1_444 ?
O41C Er2 C4A 82.1(4) . 1_444 ?
O12C Er2 C4A 96.8(4) 1_545 1_444 ?
O31C Er2 C4A 81.1(4) . 1_444 ?
O21B Er2 C4A 145.4(4) . 1_444 ?
O42A Er2 C4A 25.0(4) 1_444 1_444 ?
O12A C1A O11A 120.4(15) . . ?
O12A C1A C2A 121.6(14) . . ?
O11A C1A C2A 117.9(14) . . ?
O12A C1A Er1 60.6(8) . . ?
O11A C1A Er1 62.9(8) . . ?
C2A C1A Er1 162.4(12) . . ?
O21A C2A C3A 108.6(13) . . ?
O21A C2A C1A 112.3(12) . . ?
C3A C2A C1A 109.9(11) . . ?
O21A C2A H2A 108.6 . . ?
C3A C2A H2A 108.6 . . ?
C1A C2A H2A 108.6 . . ?
O31A C3A C2A 108.9(13) . . ?
O31A C3A C4A 114.7(13) . . ?
C2A C3A C4A 107.8(11) . . ?
O31A C3A H3A 108.4 . . ?
C2A C3A H3A 108.4 . . ?
C4A C3A H3A 108.4 . . ?
O42A C4A O41A 122.5(16) . . ?
O42A C4A C3A 121.8(15) . . ?
O41A C4A C3A 115.7(15) . . ?
O42A C4A Er2 71.6(9) . 1_666 ?
O41A C4A Er2 51.4(8) . 1_666 ?
C3A C4A Er2 165.1(12) . 1_666 ?
O12B C1B O11B 123.3(13) . . ?
O12B C1B C2B 119.4(12) . . ?
O11B C1B C2B 117.2(12) . . ?
O21B C2B C3B 114.3(12) . . ?
O21B C2B C1B 109.2(11) . . ?
C3B C2B C1B 109.2(11) . . ?
O21B C2B H2B 108.0 . . ?
C3B C2B H2B 108.0 . . ?
C1B C2B H2B 108.0 . . ?
O31B C3B C2B 109.6(11) . . ?
O31B C3B C4B 107.0(10) . . ?
C2B C3B C4B 114.9(10) . . ?
O31B C3B H3B 108.4 . . ?
C2B C3B H3B 108.4 . . ?
C4B C3B H3B 108.4 . . ?
O41B C4B O42B 124.8(13) . . ?
O41B C4B C3B 118.2(12) . . ?
O42B C4B C3B 117.0(12) . . ?
O12C C1C O11C 125.3(15) . . ?
O12C C1C C2C 119.8(12) . . ?
O11C C1C C2C 114.8(12) . . ?
O21C C2C C3C 115.2(12) . . ?
O21C C2C C1C 110.4(10) . . ?
C3C C2C C1C 106.3(11) . . ?
O21C C2C H2C 108.2 . . ?
C3C C2C H2C 108.2 . . ?
C1C C2C H2C 108.2 . . ?
O31C C3C C2C 112.0(11) . . ?
O31C C3C C4C 105.8(11) . . ?
C2C C3C C4C 113.1(11) . . ?
O31C C3C H3C 108.6 . . ?
C2C C3C H3C 108.6 . . ?
C4C C3C H3C 108.6 . . ?
O42C C4C O41C 124.2(13) . . ?
O42C C4C C3C 117.9(13) . . ?
O41C C4C C3C 117.8(12) . . ?
C1A O11A Er1 89.7(9) . . ?
C1A O12A Er1 93.0(9) . . ?
C2A O21A H21A 113.2 . . ?
C3A O31A H31A 105.4 . . ?
C4A O41A Er2 104.2(11) . 1_666 ?
C4A O42A Er2 83.4(10) . 1_666 ?
C1B O11B Er2 125.3(9) . . ?
C1B O12B Er1 136.9(9) . . ?
C2B O21B Er2 115.6(8) . . ?
C2B O21B H21B 109.4 . . ?
Er2 O21B H21B 98.0 . . ?
C3B O31B Er1 121.2(8) . 1_545 ?
C3B O31B H31B 107.6 . . ?
Er1 O31B H31B 98.0 1_545 . ?
C4B O41B Er1 127.4(9) . 1_545 ?
C4B O42B Er1 133.7(9) . 1_645 ?
C1C O11C Er1 125.6(9) . . ?
C1C O12C Er2 139.1(10) . 1_565 ?
C2C O21C Er1 115.3(8) . . ?
C2C O21C H21C 114.6 . . ?
Er1 O21C H21C 95.3 . . ?
C3C O31C Er2 122.6(8) . . ?
C3C O31C H31C 104.3 . . ?
Er2 O31C H31C 118.9 . . ?
C4C O41C Er2 127.0(9) . . ?
C4C O42C Er2 135.9(9) . 1_455 ?
Er1 O1W H11W 128.0 . . ?
Er1 O1W H12W 112.2 . . ?
H11W O1W H12W 102.9 . . ?
Er2 O2W H21W 132.4 . . ?
Er2 O2W H22W 111.6 . . ?
H21W O2W H22W 103.5 . . ?
H31W O3W H32W 107.7 . . ?
H41W O4W H42W 102.6 . . ?
H51W O5W H52W 104.3 . . ?
H61W O6W H62W 102.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.85 1.97 2.816(15) 174.6 1_455 yes
O31A H31A O12A 0.85 1.88 2.721(15) 169.4 1_655 yes
O21B H21B O11C 0.86 1.76 2.609(14) 172.3 1_545 yes
O31B H31B O3W 0.84 2.01 2.726(18) 142.9 . yes
O21C H21C O11B 0.85 1.74 2.572(15) 168.0 . yes
O31C H31C O4W 0.87 1.90 2.71(3) 153.8 . yes
O1W H11W O6W 0.87 2.04 2.874(15) 159.4 . yes
O1W H12W O41B 0.84 1.91 2.689(15) 152.2 1_465 yes
O2W H21W O5W 0.86 1.95 2.705(19) 145.9 . yes
O2W H22W O41C 0.85 1.93 2.713(15) 151.9 1_655 yes
O3W H31W O21A 0.84 2.03 2.838(17) 160.6 1_545 yes
O3W H32W O11A 0.88 1.93 2.768(17) 158.3 . yes
O4W H41W O41A 0.87 2.02 2.79(3) 146.4 1_454 yes
O4W H42W O6W 0.85 1.93 2.728(19) 156.5 1_554 yes
O5W H51W O4W 0.86 2.07 2.91(3) 165.3 1_645 yes
O5W H52W O6W 0.84 2.43 3.20(2) 151.1 1_544 yes
O6W H61W O31A 0.89 2.15 2.819(16) 131.0 1_445 yes
O6W H62W O3W 0.83 2.02 2.744(17) 144.8 . yes

_refine_diff_density_max         2.999
_refine_diff_density_min         -2.444
_refine_diff_density_rms         0.291


# start Validation Reply Form
_vrf_PLAT029_Compound_Er-L       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.901 Why?  
RESPONSE: Single crystals of this compound, as the rest of isostructural members with
other lanthanide(III) atoms, crystallize as twinned specimens. Despite the fact that
an appropriate strategy was employed to measure large complitude in the data collection,
the small size of the obtained crystals did not allow obtaining high resolution data,
and some frames of the data collection had to be removed to avoid overlapping between 
spots. Therefore, the refinement shows some signs of low coverage, such this alert
as well as the occurrence of many non-positive anisotropic displacement parameters.
In any case, given that this structure is isomorphic to others published in the same 
paper, it can be perfectly trusted.
;
# end Validation Reply Form



_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Compound_Dy-D
_database_code_depnum_ccdc_archive 'CCDC 1981577'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-D-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-D-tartrate-k2O,O':k2O'',O''')diaquadidysprosium(III)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Dy2 O20, 4(H2 O)'
_chemical_formula_sum            'C12 H24 Dy2 O24'
_chemical_formula_weight         877.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9997(2)
_cell_length_b                   7.3674(3)
_cell_length_c                   13.2962(5)
_cell_angle_alpha                102.281(4)
_cell_angle_beta                 101.870(3)
_cell_angle_gamma                90.344(3)
_cell_volume                     561.23(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9372
_cell_measurement_theta_min      6.2060
_cell_measurement_theta_max      74.0930

loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -1.0001 -0.0004 0.0000 -0.0199 0.9617 -0.0760 0.0094 -0.9820 -0.9624

loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.5758 8900 889
2 0.4242 8849 889

_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.596
_exptl_crystal_F_000             420
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    36.311
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.011
_exptl_absorpt_correction_T_max  0.052
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_reflns_number            9372
_diffrn_reflns_av_unetI/netI     0.1113
_diffrn_reflns_av_R_equivalents  0.1918
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.481
_diffrn_reflns_theta_max         74.501
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_point_group_measured_fraction_full 0.922
_reflns_number_total             4072
_reflns_number_gt                3927
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_max     0.823
_reflns_Friedel_fraction_full    0.881

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1914 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(16)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         4072
_refine_ls_number_parameters     343
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.1017
_refine_ls_wR_factor_ref         0.2600
_refine_ls_wR_factor_gt          0.2579
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.166
_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
Dy1 Dy 0.97724(13) 0.18249(11) 0.32187(8) 0.0133(5) Uani 1 1 d . . . . .
Dy2 Dy 1.02282(14) 0.81694(12) 0.67755(8) 0.0130(5) Uani 1 1 d . . . . .
C1A C 0.775(5) 0.065(4) 0.1068(19) 0.015(5) Uani 1 1 d . U . . .
C2A C 0.629(4) -0.031(3) 0.0025(18) 0.015(5) Uani 1 1 d . . . . .
H2A H 0.647359 0.038596 -0.050537 0.019 Uiso 1 1 calc R U . . .
C3A C 0.374(4) -0.023(3) 0.0157(18) 0.013(5) Uani 1 1 d . . . . .
H3A H 0.339787 0.106172 0.042137 0.016 Uiso 1 1 calc R U . . .
C4A C 0.220(5) -0.099(4) -0.095(2) 0.017(5) Uani 1 1 d . . . . .
C1B C 0.844(4) 0.613(3) 0.4324(17) 0.013(4) Uani 1 1 d . U . . .
C2B C 0.650(4) 0.750(3) 0.4362(17) 0.011(4) Uani 1 1 d . U . . .
H2B H 0.509559 0.685477 0.439209 0.014 Uiso 1 1 calc R U . . .
C3B C 0.617(4) 0.823(4) 0.3332(17) 0.016(4) Uani 1 1 d . . . . .
H3B H 0.530395 0.726629 0.275494 0.019 Uiso 1 1 calc R U . . .
C4B C 0.490(4) 1.001(4) 0.3369(19) 0.015(5) Uani 1 1 d . . . . .
C1C C 1.150(5) 0.166(3) 0.5675(17) 0.016(5) Uani 1 1 d . . . . .
C2C C 1.340(4) 0.309(3) 0.5651(17) 0.013(4) Uani 1 1 d . . . . .
H2C H 1.480750 0.243409 0.562542 0.016 Uiso 1 1 calc R U . . .
C3C C 1.377(4) 0.452(4) 0.6685(17) 0.016(5) Uani 1 1 d . . . . .
H3C H 1.463935 0.395513 0.723979 0.019 Uiso 1 1 calc R U . . .
C4C C 1.515(5) 0.626(4) 0.6634(19) 0.016(5) Uani 1 1 d . . . . .
O11A O 0.727(3) 0.223(3) 0.1526(13) 0.020(4) Uani 1 1 d . . . . .
O12A O 0.952(4) -0.017(3) 0.1442(15) 0.018(4) Uani 1 1 d . U . . .
O21A O 0.669(3) -0.214(2) -0.0337(14) 0.019(4) Uani 1 1 d . . . . .
O31A O 0.348(4) -0.131(3) 0.0899(13) 0.022(4) Uani 1 1 d . . . . .
O41A O 0.250(4) -0.009(3) -0.1618(14) 0.025(5) Uani 1 1 d . . . . .
O42A O 0.073(4) -0.230(3) -0.1127(16) 0.024(4) Uani 1 1 d . . . . .
O12B O 0.820(3) 0.472(3) 0.3568(13) 0.019(4) Uani 1 1 d . . . . .
O11B O 1.018(4) 0.645(3) 0.5085(14) 0.018(4) Uani 1 1 d . . . . .
O21B O 0.719(3) 0.895(3) 0.5282(12) 0.012(3) Uani 1 1 d . . . . .
O31B O 0.834(3) 0.857(2) 0.3103(12) 0.015(3) Uani 1 1 d . . . . .
O41B O 0.589(3) 1.144(3) 0.3335(14) 0.020(4) Uani 1 1 d . . . . .
O42B O 0.277(3) 0.991(3) 0.3439(13) 0.020(4) Uani 1 1 d . . . . .
O11C O 0.975(4) 0.149(3) 0.4929(13) 0.021(4) Uani 1 1 d . . . . .
O12C O 1.181(3) 0.085(2) 0.6424(13) 0.015(3) Uani 1 1 d . . . . .
O21C O 1.279(3) 0.377(3) 0.4724(12) 0.012(3) Uani 1 1 d . . . . .
O31C O 1.166(3) 0.509(2) 0.6966(12) 0.016(3) Uani 1 1 d . . . . .
O41C O 1.409(3) 0.774(3) 0.6667(14) 0.022(4) Uani 1 1 d . . . . .
O42C O 1.719(3) 0.611(2) 0.6633(13) 0.018(3) Uani 1 1 d . U . . .
O1W O 1.246(3) 0.346(3) 0.2586(14) 0.024(4) Uani 1 1 d . . . . .
O2W O 0.771(3) 1.027(3) 0.7489(14) 0.020(4) Uani 1 1 d . U . . .
O3W O 0.803(4) 0.590(3) 0.1330(14) 0.026(4) Uani 1 1 d . . . . .
O4W O 1.301(4) 0.375(3) 0.8768(15) 0.027(4) Uani 1 1 d . . . . .
O5W O 0.776(4) 1.353(4) 0.8832(16) 0.037(5) Uani 1 1 d . . . . .
O6W O 1.226(3) 0.496(2) 0.0757(14) 0.019(4) Uani 1 1 d . . . . .
H21A H 0.790055 -0.229278 -0.060705 0.028 Uiso 1 1 d . U . . .
H31A H 0.217446 -0.089411 0.096220 0.028 Uiso 1 1 d . U . . .
H21B H 0.800192 0.990938 0.525016 0.028 Uiso 1 1 d . U . . .
H31B H 0.854228 0.776701 0.258669 0.028 Uiso 1 1 d . U . . .
H21C H 1.204220 0.475514 0.479382 0.028 Uiso 1 1 d . U . . .
H31C H 1.160249 0.476555 0.753055 0.028 Uiso 1 1 d . U . . .
H11W H 1.257868 0.382626 0.205023 0.028 Uiso 1 1 d . U . . .
H12W H 1.366874 0.292662 0.278042 0.028 Uiso 1 1 d . U . . .
H21W H 0.751319 1.121038 0.794450 0.028 Uiso 1 1 d . U . . .
H22W H 0.636473 0.971969 0.722506 0.028 Uiso 1 1 d . U . . .
H31W H 0.749805 0.617867 0.073650 0.028 Uiso 1 1 d . U . . .
H32W H 0.760504 0.475266 0.124947 0.028 Uiso 1 1 d . U . . .
H41W H 1.286849 0.250969 0.861718 0.028 Uiso 1 1 d . U . . .
H42W H 1.267328 0.403188 0.935624 0.028 Uiso 1 1 d . U . . .
H51W H 0.633642 1.373141 0.879003 0.028 Uiso 1 1 d . U . . .
H52W H 0.891030 1.409198 0.932768 0.028 Uiso 1 1 d . U . . .
H61W H 1.290476 0.603343 0.080395 0.028 Uiso 1 1 d . U . . .
H62W H 1.093257 0.529185 0.090242 0.028 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O42B 2.30(2) 1_645 ?
Dy1 O12B 2.33(2) . ?
Dy1 O11C 2.343(17) . ?
Dy1 O41B 2.39(2) 1_545 ?
Dy1 O1W 2.394(19) . ?
Dy1 O12A 2.476(19) . ?
Dy1 O31B 2.508(16) 1_545 ?
Dy1 O11A 2.512(19) . ?
Dy1 O21C 2.568(16) . ?
Dy1 C1A 2.81(2) . ?
Dy2 O42C 2.315(18) 1_455 ?
Dy2 O11B 2.329(17) . ?
Dy2 O12C 2.358(17) 1_565 ?
Dy2 O2W 2.360(19) . ?
Dy2 O41C 2.37(2) . ?
Dy2 O41A 2.38(2) 1_666 ?
Dy2 O31C 2.473(17) . ?
Dy2 O21B 2.568(17) . ?
Dy2 O42A 2.84(2) 1_666 ?
Dy2 C4A 2.94(3) 1_666 ?
C1A O11A 1.26(3) . ?
C1A O12A 1.29(4) . ?
C1A C2A 1.51(3) . ?
C2A O21A 1.37(3) . ?
C2A C3A 1.58(3) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.42(3) . ?
C3A C4A 1.56(3) . ?
C3A H3A 0.9800 . ?
C4A O41A 1.25(3) . ?
C4A O42A 1.26(3) . ?
C1B O12B 1.27(3) . ?
C1B O11B 1.28(3) . ?
C1B C2B 1.55(3) . ?
C2B O21B 1.43(3) . ?
C2B C3B 1.55(3) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.43(3) . ?
C3B C4B 1.52(4) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.22(3) . ?
C4B O42B 1.30(3) . ?
C1C O12C 1.25(3) . ?
C1C O11C 1.27(3) . ?
C1C C2C 1.56(3) . ?
C2C O21C 1.41(3) . ?
C2C C3C 1.52(3) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.44(3) . ?
C3C C4C 1.55(4) . ?
C3C H3C 0.9800 . ?
C4C O42C 1.23(4) . ?
C4C O41C 1.26(4) . ?
O21A H21A 0.8704 . ?
O31A H31A 0.8542 . ?
O21B H21B 0.8699 . ?
O31B H31B 0.8334 . ?
O21C H21C 0.8514 . ?
O31C H31C 0.8433 . ?
O1W H11W 0.8279 . ?
O1W H12W 0.8483 . ?
O2W H21W 0.8442 . ?
O2W H22W 0.8717 . ?
O3W H31W 0.8561 . ?
O3W H32W 0.8602 . ?
O4W H41W 0.8906 . ?
O4W H42W 0.8316 . ?
O5W H51W 0.8583 . ?
O5W H52W 0.8806 . ?
O6W H61W 0.8647 . ?
O6W H62W 0.8808 . ?

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
O42B Dy1 O12B 151.3(6) 1_645 . ?
O42B Dy1 O11C 80.9(7) 1_645 . ?
O12B Dy1 O11C 90.3(7) . . ?
O42B Dy1 O41B 131.2(7) 1_645 1_545 ?
O12B Dy1 O41B 70.0(7) . 1_545 ?
O11C Dy1 O41B 72.4(7) . 1_545 ?
O42B Dy1 O1W 81.3(7) 1_645 . ?
O12B Dy1 O1W 83.9(7) . . ?
O11C Dy1 O1W 130.2(6) . . ?
O41B Dy1 O1W 146.3(7) 1_545 . ?
O42B Dy1 O12A 75.9(6) 1_645 . ?
O12B Dy1 O12A 125.1(6) . . ?
O11C Dy1 O12A 138.7(7) . . ?
O41B Dy1 O12A 98.2(6) 1_545 . ?
O1W Dy1 O12A 79.4(7) . . ?
O42B Dy1 O31B 69.4(6) 1_645 1_545 ?
O12B Dy1 O31B 133.6(6) . 1_545 ?
O11C Dy1 O31B 72.0(6) . 1_545 ?
O41B Dy1 O31B 63.8(6) 1_545 1_545 ?
O1W Dy1 O31B 140.2(7) . 1_545 ?
O12A Dy1 O31B 68.0(6) . 1_545 ?
O42B Dy1 O11A 128.1(6) 1_645 . ?
O12B Dy1 O11A 72.9(6) . . ?
O11C Dy1 O11A 143.6(7) . . ?
O41B Dy1 O11A 71.6(6) 1_545 . ?
O1W Dy1 O11A 80.9(6) . . ?
O12A Dy1 O11A 53.0(7) . . ?
O31B Dy1 O11A 96.2(6) 1_545 . ?
O42B Dy1 O21C 75.5(6) 1_645 . ?
O12B Dy1 O21C 76.1(6) . . ?
O11C Dy1 O21C 62.9(6) . . ?
O41B Dy1 O21C 122.7(6) 1_545 . ?
O1W Dy1 O21C 67.7(6) . . ?
O12A Dy1 O21C 139.0(6) . . ?
O31B Dy1 O21C 126.1(5) 1_545 . ?
O11A Dy1 O21C 137.7(6) . . ?
O42B Dy1 C1A 103.1(7) 1_645 . ?
O12B Dy1 C1A 99.5(7) . . ?
O11C Dy1 C1A 145.7(7) . . ?
O41B Dy1 C1A 80.2(7) 1_545 . ?
O1W Dy1 C1A 83.7(7) . . ?
O12A Dy1 C1A 27.2(8) . . ?
O31B Dy1 C1A 77.6(6) 1_545 . ?
O11A Dy1 C1A 26.6(7) . . ?
O21C Dy1 C1A 151.4(7) . . ?
O42C Dy2 O11B 81.8(7) 1_455 . ?
O42C Dy2 O12C 151.7(6) 1_455 1_565 ?
O11B Dy2 O12C 92.3(6) . 1_565 ?
O42C Dy2 O2W 80.6(6) 1_455 . ?
O11B Dy2 O2W 133.2(7) . . ?
O12C Dy2 O2W 83.6(6) 1_565 . ?
O42C Dy2 O41C 132.7(7) 1_455 . ?
O11B Dy2 O41C 73.6(7) . . ?
O12C Dy2 O41C 70.2(7) 1_565 . ?
O2W Dy2 O41C 144.2(7) . . ?
O42C Dy2 O41A 125.6(7) 1_455 1_666 ?
O11B Dy2 O41A 146.4(8) . 1_666 ?
O12C Dy2 O41A 71.9(7) 1_565 1_666 ?
O2W Dy2 O41A 75.7(7) . 1_666 ?
O41C Dy2 O41A 73.2(7) . 1_666 ?
O42C Dy2 O31C 70.3(6) 1_455 . ?
O11B Dy2 O31C 73.1(6) . . ?
O12C Dy2 O31C 134.3(6) 1_565 . ?
O2W Dy2 O31C 137.6(6) . . ?
O41C Dy2 O31C 64.1(7) . . ?
O41A Dy2 O31C 96.5(6) 1_666 . ?
O42C Dy2 O21B 76.6(6) 1_455 . ?
O11B Dy2 O21B 63.6(6) . . ?
O12C Dy2 O21B 76.1(6) 1_565 . ?
O2W Dy2 O21B 70.2(6) . . ?
O41C Dy2 O21B 123.4(6) . . ?
O41A Dy2 O21B 135.2(6) 1_666 . ?
O31C Dy2 O21B 128.3(6) . . ?
O42C Dy2 O42A 77.7(6) 1_455 1_666 ?
O11B Dy2 O42A 140.3(7) . 1_666 ?
O12C Dy2 O42A 120.8(6) 1_565 1_666 ?
O2W Dy2 O42A 76.1(6) . 1_666 ?
O41C Dy2 O42A 96.3(6) . 1_666 ?
O41A Dy2 O42A 49.4(7) 1_666 1_666 ?
O31C Dy2 O42A 68.1(6) . 1_666 ?
O21B Dy2 O42A 140.3(6) . 1_666 ?
O42C Dy2 C4A 102.5(7) 1_455 1_666 ?
O11B Dy2 C4A 150.1(7) . 1_666 ?
O12C Dy2 C4A 96.3(7) 1_565 1_666 ?
O2W Dy2 C4A 76.4(7) . 1_666 ?
O41C Dy2 C4A 82.5(7) . 1_666 ?
O41A Dy2 C4A 24.5(7) 1_666 1_666 ?
O31C Dy2 C4A 80.4(6) . 1_666 ?
O21B Dy2 C4A 146.3(7) . 1_666 ?
O42A Dy2 C4A 25.1(7) 1_666 1_666 ?
O11A C1A O12A 122(2) . . ?
O11A C1A C2A 120(2) . . ?
O12A C1A C2A 118(2) . . ?
O11A C1A Dy1 63.3(13) . . ?
O12A C1A Dy1 61.7(13) . . ?
C2A C1A Dy1 164.8(17) . . ?
O21A C2A C1A 116(2) . . ?
O21A C2A C3A 107.6(19) . . ?
C1A C2A C3A 106.9(19) . . ?
O21A C2A H2A 108.6 . . ?
C1A C2A H2A 108.6 . . ?
C3A C2A H2A 108.6 . . ?
O31A C3A C4A 113(2) . . ?
O31A C3A C2A 108(2) . . ?
C4A C3A C2A 107.2(19) . . ?
O31A C3A H3A 109.5 . . ?
C4A C3A H3A 109.5 . . ?
C2A C3A H3A 109.5 . . ?
O41A C4A O42A 125(3) . . ?
O41A C4A C3A 113(2) . . ?
O42A C4A C3A 122(2) . . ?
O41A C4A Dy2 52.1(14) . 1_444 ?
O42A C4A Dy2 73.0(15) . 1_444 ?
C3A C4A Dy2 164.2(18) . 1_444 ?
O12B C1B O11B 123(2) . . ?
O12B C1B C2B 119(2) . . ?
O11B C1B C2B 118(2) . . ?
O21B C2B C1B 107.7(18) . . ?
O21B C2B C3B 112.7(18) . . ?
C1B C2B C3B 106.3(19) . . ?
O21B C2B H2B 110.0 . . ?
C1B C2B H2B 110.0 . . ?
C3B C2B H2B 110.0 . . ?
O31B C3B C4B 108(2) . . ?
O31B C3B C2B 109.6(19) . . ?
C4B C3B C2B 114(2) . . ?
O31B C3B H3B 108.4 . . ?
C4B C3B H3B 108.4 . . ?
C2B C3B H3B 108.4 . . ?
O41B C4B O42B 123(3) . . ?
O41B C4B C3B 120(2) . . ?
O42B C4B C3B 117(2) . . ?
O12C C1C O11C 127(2) . . ?
O12C C1C C2C 118(2) . . ?
O11C C1C C2C 115.1(19) . . ?
O21C C2C C3C 117(2) . . ?
O21C C2C C1C 109.1(18) . . ?
C3C C2C C1C 107(2) . . ?
O21C C2C H2C 107.9 . . ?
C3C C2C H2C 107.9 . . ?
C1C C2C H2C 107.9 . . ?
O31C C3C C2C 112(2) . . ?
O31C C3C C4C 108(2) . . ?
C2C C3C C4C 111(2) . . ?
O31C C3C H3C 108.4 . . ?
C2C C3C H3C 108.4 . . ?
C4C C3C H3C 108.4 . . ?
O42C C4C O41C 126(2) . . ?
O42C C4C C3C 117(2) . . ?
O41C C4C C3C 116(2) . . ?
C1A O11A Dy1 90.1(16) . . ?
C1A O12A Dy1 91.1(15) . . ?
C2A O21A H21A 113.9 . . ?
C3A O31A H31A 93.3 . . ?
C4A O41A Dy2 103.4(17) . 1_444 ?
C4A O42A Dy2 81.9(16) . 1_444 ?
C1B O12B Dy1 137.3(17) . . ?
C1B O11B Dy2 125.3(17) . . ?
C2B O21B Dy2 116.5(13) . . ?
C2B O21B H21B 119.1 . . ?
Dy2 O21B H21B 92.6 . . ?
C3B O31B Dy1 120.2(14) . 1_565 ?
C3B O31B H31B 110.3 . . ?
Dy1 O31B H31B 116.3 1_565 . ?
C4B O41B Dy1 126.8(19) . 1_565 ?
C4B O42B Dy1 134.4(16) . 1_465 ?
C1C O11C Dy1 125.1(16) . . ?
C1C O12C Dy2 136.0(16) . 1_545 ?
C2C O21C Dy1 116.9(13) . . ?
C2C O21C H21C 114.0 . . ?
Dy1 O21C H21C 95.9 . . ?
C3C O31C Dy2 120.8(14) . . ?
C3C O31C H31C 107.7 . . ?
Dy2 O31C H31C 117.2 . . ?
C4C O41C Dy2 128.2(16) . . ?
C4C O42C Dy2 134.8(17) . 1_655 ?
Dy1 O1W H11W 139.8 . . ?
Dy1 O1W H12W 100.7 . . ?
H11W O1W H12W 107.5 . . ?
Dy2 O2W H21W 148.9 . . ?
Dy2 O2W H22W 104.3 . . ?
H21W O2W H22W 105.6 . . ?
H31W O3W H32W 105.3 . . ?
H41W O4W H42W 103.0 . . ?
H51W O5W H52W 127.2 . . ?
H61W O6W H62W 100.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.87 1.96 2.82(3) 172.6 1_655 yes
O31A H31A O12A 0.85 1.87 2.71(3) 164.9 1_455 yes
O21B H21B O11C 0.87 1.73 2.59(3) 166.7 1_565 yes
O31B H31B O3W 0.83 1.89 2.70(2) 162.9 . yes
O21C H21C O11B 0.85 1.71 2.55(3) 166.3 . yes
O31C H31C O4W 0.84 1.99 2.76(3) 151.7 . yes
O1W H11W O6W 0.83 2.04 2.86(3) 168.4 . yes
O1W H12W O41B 0.85 1.86 2.69(3) 166.8 1_645 yes
O2W H21W O5W 0.84 1.85 2.67(3) 164.1 . yes
O2W H22W O41C 0.87 1.91 2.74(3) 158.8 1_455 yes
O3W H31W O21A 0.86 2.07 2.88(3) 157.4 1_565 yes
O3W H32W O11A 0.86 1.99 2.82(3) 161.3 . yes
O4W H41W O41A 0.89 1.88 2.77(3) 176.2 1_656 yes
O4W H42W O6W 0.83 1.91 2.74(3) 171.6 1_556 yes
O5W H51W O4W 0.86 1.99 2.84(3) 169.6 1_465 yes
O5W H52W O6W 0.88 2.44 3.30(3) 167.6 1_566 yes
O6W H61W O31A 0.86 1.96 2.80(3) 163.6 1_665 yes
O6W H62W O3W 0.88 1.96 2.84(3) 174.6 . yes

_refine_diff_density_max         4.235
_refine_diff_density_min         -2.382
_refine_diff_density_rms         0.550


# start Validation Reply Form
_vrf_RINTA01_Compound_Dy-D       
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately.
;
_vrf_PLAT971_Compound_Dy-D       
;
PROBLEM: Check Calcd Resid. Dens.  1.11A   From Dy2             4.32 eA-3  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. Despite the fact that specific absorption
correction based on the faces of the crystal has been performed, somewhat large
diffraction peaks close to the lanthanide atoms could not be removed. Nonetheless,
the unaccounted positive residual density is quite common for lanthanide-organic
based crystal structures. 
;
_vrf_PLAT975_Compound_Dy-D       
;
PROBLEM: Check Calcd Resid. Dens.  0.82A   From O11A            2.23 eA-3  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. Despite the fact that specific absorption
correction based on the faces of the crystal has been performed, somewhat large
diffraction peaks close to the lanthanide atoms could not be removed. Nonetheless,
the unaccounted positive residual density is quite common for lanthanide-organic
based crystal structures. 
;
_vrf_PLAT020_Compound_Dy-D       
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.192 Report
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately.
;
_vrf_PLAT342_Compound_Dy-D       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03444 Ang.  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately.
;
# end Validation Reply Form


_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Compound_Tb-L'-383K
_database_code_depnum_ccdc_archive 'CCDC 1981574'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-Î?3O,O',O'':Î?2O''',O'''')aquaditerbium(III)] hydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H14 O19 Tb2, 0.35(H2 O)'
_chemical_formula_sum            'C12 H14.70 O19.35 Tb2'
_chemical_formula_weight         786.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.8454(3)
_cell_length_b                   7.3765(3)
_cell_length_c                   11.9258(6)
_cell_angle_alpha                107.960(4)
_cell_angle_beta                 104.297(4)
_cell_angle_gamma                89.974(4)
_cell_volume                     472.42(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    383(2)
_cell_measurement_reflns_used    10072
_cell_measurement_theta_min      1.859
_cell_measurement_theta_max      28.434


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.805
_exptl_crystal_F_000             378
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    7.535
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_T_max  2.439
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
Single crystals of this compound crystallize as a twinned specimen, 
but no twin law has been applied for the data reduction because, ohterwise,
agreement factors got worse. These data correspond to a measurement performed
at 383 K in order to check the dehydration of the crystal.
;

_diffrn_ambient_temperature      383(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω
_diffrn_reflns_number            10072
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.859
_diffrn_reflns_theta_max         25.551
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3535
_reflns_number_gt                3453
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_max     0.999
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
The crystal is a twinned specimen but no twin law has been applied
during data reduction nor the refinement since it leads to better
agreement factors. Moreover, the structure possesses a strong
pseudosymmetry arising from the almost equivalent environment of the
two independent terbium atoms, which simulates a monoclinic unit cell.
However, all trials to finish the refinment with the monoclinic cell
led to unsatisfactory results, because it causes a disorder in the 
terbium environment that worsens the agreement factors.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²+3.1590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1664 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         3535
_refine_ls_number_parameters     303
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0815
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.013
_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 1.82410(7) 0.84528(6) 1.08336(5) 0.0193(2) Uani 1 1 d . . . . .
Tb2 Tb 1.46784(7) 1.13273(6) 0.65852(5) 0.0193(2) Uani 1 1 d . . . . .
C1A C 1.935(6) 1.235(7) 1.306(4) 0.114(12) Uani 1 1 d D U . . .
C1B C 1.548(3) 1.153(2) 0.9411(14) 0.023(3) Uani 1 1 d . . . . .
C1C C 1.748(3) 0.583(2) 0.8033(14) 0.026(3) Uani 1 1 d . . . . .
C2A C 2.178(6) 1.200(5) 1.2673(19) 0.102(10) Uani 1 1 d D U . . .
H2A H 2.257134 1.325612 1.282357 0.123 Uiso 1 1 calc R U . . .
C2B C 1.363(4) 1.303(2) 0.9448(19) 0.020(4) Uani 1 1 d . U . . .
H2B H 1.213390 1.243614 0.944286 0.024 Uiso 1 1 calc R U . . .
C2C C 1.924(3) 0.726(2) 0.7946(17) 0.016(3) Uani 1 1 d . . . . .
H2C H 2.073271 0.666182 0.794059 0.020 Uiso 1 1 calc R U . . .
C3A C 2.356(6) 1.090(5) 1.356(3) 0.098(10) Uani 1 1 d . U . . .
H3A H 2.467017 1.018463 1.313528 0.118 Uiso 1 1 calc R U . . .
C3B C 1.452(2) 1.465(2) 1.0665(13) 0.023(3) Uani 1 1 d . . . . .
H3B H 1.426132 1.418760 1.131572 0.028 Uiso 1 1 calc R U . . .
C3C C 1.839(2) 0.769(2) 0.6746(13) 0.023(3) Uani 1 1 d . . . . .
H3C H 1.862890 0.658697 0.608970 0.027 Uiso 1 1 calc R U . . .
C4A C 2.156(5) 0.935(3) 1.370(2) 0.064(6) Uani 1 1 d . U . . .
C4B C 1.320(2) 1.640(2) 1.0697(13) 0.022(3) Uani 1 1 d . . . . .
C4C C 1.973(2) 0.9403(19) 0.6729(13) 0.021(3) Uani 1 1 d . . . . .
O11A O 1.953(7) 1.343(5) 1.418(3) 0.157(12) Uani 1 1 d . U . . .
O11B O 1.6523(19) 1.1265(15) 0.8581(10) 0.027(2) Uani 1 1 d . . . . .
O11C O 1.6390(19) 0.6387(15) 0.8840(9) 0.028(2) Uani 1 1 d . . . . .
O12A O 1.793(3) 1.117(2) 1.2572(16) 0.062(4) Uani 1 1 d . . . . .
O12B O 1.583(3) 1.073(2) 1.0194(14) 0.045(3) Uani 1 1 d . . . . .
O12C O 1.712(3) 0.4257(16) 0.7239(14) 0.048(4) Uani 1 1 d . . . . .
O21A O 2.132(2) 1.0984(17) 1.1392(13) 0.042(3) Uani 1 1 d D . . . .
O21B O 1.3278(18) 1.3597(13) 0.8418(9) 0.023(2) Uani 1 1 d . . . . .
O21C O 1.9659(17) 0.8892(14) 0.9006(9) 0.025(2) Uani 1 1 d . . . . .
O31A O 2.495(3) 1.233(3) 1.4836(15) 0.062(4) Uani 1 1 d . . . . .
O31B O 1.6986(17) 1.5189(15) 1.0930(11) 0.028(2) Uani 1 1 d . . . . .
O31C O 1.5953(18) 0.7971(15) 0.6494(11) 0.028(2) Uani 1 1 d . . . . .
O41A O 2.246(2) 0.9226(17) 1.4671(11) 0.038(3) Uani 1 1 d . . . . .
O41B O 1.4373(19) 1.7949(16) 1.0993(11) 0.031(2) Uani 1 1 d . . . . .
O41C O 1.8516(18) 1.0688(18) 0.6433(11) 0.030(2) Uani 1 1 d . . . . .
O42A O 2.044(2) 0.8223(17) 1.2731(11) 0.041(3) Uani 1 1 d . . . . .
O42B O 1.1008(17) 1.6175(15) 1.0427(11) 0.028(2) Uani 1 1 d . . . . .
O42C O 2.1927(18) 0.9450(16) 0.6997(11) 0.030(2) Uani 1 1 d . . . . .
O1W O 1.158(2) 1.3295(18) 0.6051(14) 0.044(3) Uani 1 1 d . . . . .
O2W O 1.924(7) 0.668(5) 1.408(3) 0.043(13) Uiso 0.35(5) 1 d . . P . .
H21A H 2.213548 1.004866 1.109230 0.065 Uiso 1 1 d . U . . .
H31A H 2.617525 1.254705 1.459596 0.065 Uiso 1 1 d . U . . .
H21B H 1.432952 1.454361 0.864292 0.065 Uiso 1 1 d . U . . .
H31B H 1.654895 1.555634 1.029187 0.065 Uiso 1 1 d . U . . .
H21C H 1.879823 0.981274 0.892710 0.065 Uiso 1 1 d . U . . .
H31C H 1.593504 0.905060 0.703177 0.065 Uiso 1 1 d . U . . .
H11W H 1.100993 1.313154 0.528002 0.065 Uiso 1 1 d . U . . .
H12W H 1.057609 1.260917 0.620056 0.065 Uiso 1 1 d . U . . .
H21W H 2.047316 0.733339 1.370657 0.065 Uiso 0.3521 1 d . U P . .
H22W H 1.955963 0.578402 1.416699 0.065 Uiso 0.3521 1 d . U 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
Tb1 O41B 2.355(11) 1_545 ?
Tb1 O42B 2.357(10) 1_645 ?
Tb1 O42A 2.367(12) . ?
Tb1 O12B 2.375(12) . ?
Tb1 O11C 2.375(11) . ?
Tb1 O21A 2.411(12) . ?
Tb1 O12A 2.443(14) . ?
Tb1 O31B 2.561(10) 1_545 ?
Tb1 O21C 2.621(10) . ?
Tb1 H21A 2.4688 . ?
Tb2 O41C 2.331(10) . ?
Tb2 O42C 2.358(10) 1_455 ?
Tb2 O11B 2.373(10) . ?
Tb2 O41A 2.377(12) 1_454 ?
Tb2 O12C 2.392(12) 1_565 ?
Tb2 O1W 2.408(12) . ?
Tb2 O31A 2.457(14) 1_454 ?
Tb2 O31C 2.563(10) . ?
Tb2 O21B 2.622(10) . ?
Tb2 H31C 2.0002 . ?
Tb2 H12W 2.5646 . ?
C1A O12A 1.11(4) . ?
C1A O11A 1.30(5) . ?
C1A C2A 1.596(15) . ?
C1B O12B 1.231(18) . ?
C1B O11B 1.251(18) . ?
C1B C2B 1.55(2) . ?
C1C O12C 1.231(19) . ?
C1C O11C 1.248(18) . ?
C1C C2C 1.51(2) . ?
C2A O21A 1.435(15) . ?
C2A C3A 1.69(5) . ?
C2A H2A 0.9800 . ?
C2B O21B 1.38(2) . ?
C2B C3B 1.54(2) . ?
C2B H2B 0.9800 . ?
C2C O21C 1.42(2) . ?
C2C C3C 1.53(2) . ?
C2C H2C 0.9800 . ?
C3A O31A 1.58(4) . ?
C3A C4A 1.71(4) . ?
C3A H3A 0.9800 . ?
C3B O31B 1.428(16) . ?
C3B C4B 1.500(19) . ?
C3B H3B 0.9800 . ?
C3B H31B 1.5820 . ?
C3C O31C 1.408(16) . ?
C3C C4C 1.493(19) . ?
C3C H3C 0.9800 . ?
C4A O41A 1.17(3) . ?
C4A O42A 1.22(3) . ?
C4B O41B 1.234(18) . ?
C4B O42B 1.242(17) . ?
C4C O42C 1.244(17) . ?
C4C O41C 1.267(17) . ?
O21A H21A 0.8736 . ?
O21B H21B 0.8609 . ?
O21C H21C 0.8593 . ?
O31A H31A 0.8653 . ?
O31B H31B 0.8656 . ?
O31C H31C 0.8565 . ?
O1W H11W 0.8665 . ?
O1W H12W 0.8585 . ?
O2W H21W 1.1104 . ?
O2W H22W 0.7171 . ?

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
O41B Tb1 O42B 128.1(4) 1_545 1_645 ?
O41B Tb1 O42A 99.7(5) 1_545 . ?
O42B Tb1 O42A 72.7(4) 1_645 . ?
O41B Tb1 O12B 70.5(4) 1_545 . ?
O42B Tb1 O12B 147.7(4) 1_645 . ?
O42A Tb1 O12B 135.4(5) . . ?
O41B Tb1 O11C 78.6(4) 1_545 . ?
O42B Tb1 O11C 76.3(4) 1_645 . ?
O42A Tb1 O11C 138.6(4) . . ?
O12B Tb1 O11C 83.7(5) . . ?
O41B Tb1 O21A 140.6(4) 1_545 . ?
O42B Tb1 O21A 89.8(4) 1_645 . ?
O42A Tb1 O21A 79.7(5) . . ?
O12B Tb1 O21A 82.4(5) . . ?
O11C Tb1 O21A 127.2(4) . . ?
O41B Tb1 O12A 76.5(4) 1_545 . ?
O42B Tb1 O12A 136.0(5) 1_645 . ?
O42A Tb1 O12A 66.8(5) . . ?
O12B Tb1 O12A 68.6(6) . . ?
O11C Tb1 O12A 147.5(5) . . ?
O21A Tb1 O12A 67.0(5) . . ?
O41B Tb1 O31B 62.0(4) 1_545 1_545 ?
O42B Tb1 O31B 66.9(3) 1_645 1_545 ?
O42A Tb1 O31B 72.9(4) . 1_545 ?
O12B Tb1 O31B 128.9(4) . 1_545 ?
O11C Tb1 O31B 70.0(4) . 1_545 ?
O21A Tb1 O31B 148.1(4) . 1_545 ?
O12A Tb1 O31B 114.6(5) . 1_545 ?
O41B Tb1 O21C 129.6(4) 1_545 . ?
O42B Tb1 O21C 73.6(4) 1_645 . ?
O42A Tb1 O21C 130.6(4) . . ?
O12B Tb1 O21C 74.7(4) . . ?
O11C Tb1 O21C 62.1(3) . . ?
O21A Tb1 O21C 65.1(4) . . ?
O12A Tb1 O21C 122.1(5) . . ?
O31B Tb1 O21C 123.3(3) 1_545 . ?
O41B Tb1 H21A 161.0 1_545 . ?
O42B Tb1 H21A 69.5 1_645 . ?
O42A Tb1 H21A 77.7 . . ?
O12B Tb1 H21A 98.0 . . ?
O11C Tb1 H21A 115.9 . . ?
O21A Tb1 H21A 20.6 . . ?
O12A Tb1 H21A 85.3 . . ?
O31B Tb1 H21A 132.8 1_545 . ?
O21C Tb1 H21A 57.1 . . ?
O41C Tb2 O42C 128.2(4) . 1_455 ?
O41C Tb2 O11B 78.7(4) . . ?
O42C Tb2 O11B 76.2(4) 1_455 . ?
O41C Tb2 O41A 100.1(4) . 1_454 ?
O42C Tb2 O41A 73.2(4) 1_455 1_454 ?
O11B Tb2 O41A 139.5(4) . 1_454 ?
O41C Tb2 O12C 70.0(5) . 1_565 ?
O42C Tb2 O12C 147.6(4) 1_455 1_565 ?
O11B Tb2 O12C 83.2(5) . 1_565 ?
O41A Tb2 O12C 135.1(5) 1_454 1_565 ?
O41C Tb2 O1W 141.2(4) . . ?
O42C Tb2 O1W 89.3(4) 1_455 . ?
O11B Tb2 O1W 126.2(4) . . ?
O41A Tb2 O1W 79.5(5) 1_454 . ?
O12C Tb2 O1W 83.0(5) 1_565 . ?
O41C Tb2 O31A 77.0(4) . 1_454 ?
O42C Tb2 O31A 135.9(5) 1_455 1_454 ?
O11B Tb2 O31A 147.9(5) . 1_454 ?
O41A Tb2 O31A 66.2(5) 1_454 1_454 ?
O12C Tb2 O31A 68.9(6) 1_565 1_454 ?
O1W Tb2 O31A 67.3(5) . 1_454 ?
O41C Tb2 O31C 62.1(4) . . ?
O42C Tb2 O31C 66.9(4) 1_455 . ?
O11B Tb2 O31C 70.2(4) . . ?
O41A Tb2 O31C 73.7(4) 1_454 . ?
O12C Tb2 O31C 128.4(4) 1_565 . ?
O1W Tb2 O31C 148.1(4) . . ?
O31A Tb2 O31C 115.0(5) 1_454 . ?
O41C Tb2 O21B 129.1(4) . . ?
O42C Tb2 O21B 73.8(4) 1_455 . ?
O11B Tb2 O21B 61.7(3) . . ?
O41A Tb2 O21B 130.7(4) 1_454 . ?
O12C Tb2 O21B 74.4(4) 1_565 . ?
O1W Tb2 O21B 64.5(4) . . ?
O31A Tb2 O21B 121.7(4) 1_454 . ?
O31C Tb2 O21B 123.3(3) . . ?
O41C Tb2 H31C 63.7 . . ?
O42C Tb2 H31C 64.8 1_455 . ?
O11B Tb2 H31C 53.8 . . ?
O41A Tb2 H31C 88.9 1_454 . ?
O12C Tb2 H31C 120.8 1_565 . ?
O1W Tb2 H31C 153.8 . . ?
O31A Tb2 H31C 128.8 1_454 . ?
O31C Tb2 H31C 16.4 . . ?
O21B Tb2 H31C 108.7 . . ?
O41C Tb2 H12W 159.7 . . ?
O42C Tb2 H12W 69.7 1_455 . ?
O11B Tb2 H12W 118.3 . . ?
O41A Tb2 H12W 74.4 1_454 . ?
O12C Tb2 H12W 99.7 1_565 . ?
O1W Tb2 H12W 19.6 . . ?
O31A Tb2 H12W 83.0 1_454 . ?
O31C Tb2 H12W 131.7 . . ?
O21B Tb2 H12W 60.2 . . ?
H31C Tb2 H12W 134.3 . . ?
O12A C1A O11A 122(4) . . ?
O12A C1A C2A 115(3) . . ?
O11A C1A C2A 116(3) . . ?
O12B C1B O11B 125.7(13) . . ?
O12B C1B C2B 118.2(14) . . ?
O11B C1B C2B 116.1(13) . . ?
O12C C1C O11C 125.2(14) . . ?
O12C C1C C2C 116.7(14) . . ?
O11C C1C C2C 117.8(13) . . ?
O21A C2A C1A 110(3) . . ?
O21A C2A C3A 113(2) . . ?
C1A C2A C3A 110(3) . . ?
O21A C2A H2A 107.8 . . ?
C1A C2A H2A 107.8 . . ?
C3A C2A H2A 107.8 . . ?
O21B C2B C3B 115.1(13) . . ?
O21B C2B C1B 109.6(15) . . ?
C3B C2B C1B 107.0(14) . . ?
O21B C2B H2B 108.3 . . ?
C3B C2B H2B 108.3 . . ?
C1B C2B H2B 108.3 . . ?
O21C C2C C1C 109.1(14) . . ?
O21C C2C C3C 114.4(12) . . ?
C1C C2C C3C 110.2(14) . . ?
O21C C2C H2C 107.6 . . ?
C1C C2C H2C 107.6 . . ?
C3C C2C H2C 107.6 . . ?
O31A C3A C2A 113(2) . . ?
O31A C3A C4A 112(2) . . ?
C2A C3A C4A 102(2) . . ?
O31A C3A H3A 110.0 . . ?
C2A C3A H3A 110.0 . . ?
C4A C3A H3A 110.0 . . ?
O31B C3B C4B 108.1(11) . . ?
O31B C3B C2B 112.1(13) . . ?
C4B C3B C2B 112.4(12) . . ?
O31B C3B H3B 108.0 . . ?
C4B C3B H3B 108.0 . . ?
C2B C3B H3B 108.0 . . ?
O31B C3B H31B 32.9 . . ?
C4B C3B H31B 89.7 . . ?
C2B C3B H31B 96.1 . . ?
H3B C3B H31B 140.8 . . ?
O31C C3C C4C 108.9(11) . . ?
O31C C3C C2C 111.4(12) . . ?
C4C C3C C2C 112.6(12) . . ?
O31C C3C H3C 107.9 . . ?
C4C C3C H3C 107.9 . . ?
C2C C3C H3C 107.9 . . ?
O41A C4A O42A 134.6(19) . . ?
O41A C4A C3A 102(2) . . ?
O42A C4A C3A 114(2) . . ?
O41B C4B O42B 125.3(13) . . ?
O41B C4B C3B 118.0(13) . . ?
O42B C4B C3B 116.6(12) . . ?
O42C C4C O41C 125.3(13) . . ?
O42C C4C C3C 117.8(12) . . ?
O41C C4C C3C 116.9(12) . . ?
C1B O11B Tb2 123.9(9) . . ?
C1C O11C Tb1 122.4(9) . . ?
C1A O12A Tb1 123(2) . . ?
C1B O12B Tb1 140.5(10) . . ?
C1C O12C Tb2 140.4(11) . 1_545 ?
C2A O21A Tb1 109.3(16) . . ?
C2A O21A H21A 123.2 . . ?
Tb1 O21A H21A 83.4 . . ?
C2B O21B Tb2 116.2(9) . . ?
C2B O21B H21B 102.8 . . ?
Tb2 O21B H21B 99.3 . . ?
C2C O21C Tb1 115.5(9) . . ?
C2C O21C H21C 114.6 . . ?
Tb1 O21C H21C 95.7 . . ?
C3A O31A Tb2 113.8(15) . 1_656 ?
C3A O31A H31A 95.4 . . ?
Tb2 O31A H31A 130.5 1_656 . ?
C3B O31B Tb1 118.5(8) . 1_565 ?
C3B O31B H31B 83.3 . . ?
Tb1 O31B H31B 55.5 1_565 . ?
C3C O31C Tb2 118.8(8) . . ?
C3C O31C H31C 101.6 . . ?
Tb2 O31C H31C 41.2 . . ?
C4A O41A Tb2 136.5(14) . 1_656 ?
C4B O41B Tb1 127.4(9) . 1_565 ?
C4C O41C Tb2 127.6(9) . . ?
C4A O42A Tb1 135.8(12) . . ?
C4B O42B Tb1 129.2(9) . 1_465 ?
C4C O42C Tb2 129.3(9) . 1_655 ?
Tb2 O1W H11W 116.6 . . ?
Tb2 O1W H12W 90.6 . . ?
H11W O1W H12W 102.8 . . ?
H21W O2W H22W 115.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12A C1A C2A O21A 35(5) . . . . ?
O11A C1A C2A O21A -173(3) . . . . ?
O12A C1A C2A C3A -90(4) . . . . ?
O11A C1A C2A C3A 61(5) . . . . ?
O12B C1B C2B O21B -172.4(15) . . . . ?
O11B C1B C2B O21B 8(2) . . . . ?
O12B C1B C2B C3B 62(2) . . . . ?
O11B C1B C2B C3B -117.2(16) . . . . ?
O12C C1C C2C O21C -172.8(15) . . . . ?
O11C C1C C2C O21C 12(2) . . . . ?
O12C C1C C2C C3C 60.7(19) . . . . ?
O11C C1C C2C C3C -114.0(16) . . . . ?
O21A C2A C3A O31A 154(2) . . . . ?
C1A C2A C3A O31A -82(3) . . . . ?
O21A C2A C3A C4A -85(3) . . . . ?
C1A C2A C3A C4A 39(3) . . . . ?
O21B C2B C3B O31B -77.6(17) . . . . ?
C1B C2B C3B O31B 44.5(17) . . . . ?
O21B C2B C3B C4B 44(2) . . . . ?
C1B C2B C3B C4B 166.5(12) . . . . ?
O21C C2C C3C O31C -79.5(17) . . . . ?
C1C C2C C3C O31C 44.0(16) . . . . ?
O21C C2C C3C C4C 43.3(18) . . . . ?
C1C C2C C3C C4C 166.7(12) . . . . ?
O31A C3A C4A O41A -29(3) . . . . ?
C2A C3A C4A O41A -150(2) . . . . ?
O31A C3A C4A O42A 180(2) . . . . ?
C2A C3A C4A O42A 59(3) . . . . ?
O31B C3B C4B O41B -3.9(18) . . . . ?
C2B C3B C4B O41B -128.1(15) . . . . ?
O31B C3B C4B O42B 176.7(12) . . . . ?
C2B C3B C4B O42B 52.4(18) . . . . ?
O31C C3C C4C O42C 176.3(13) . . . . ?
C2C C3C C4C O42C 52.2(18) . . . . ?
O31C C3C C4C O41C -4.0(18) . . . . ?
C2C C3C C4C O41C -128.1(14) . . . . ?
O12B C1B O11B Tb2 144.2(14) . . . . ?
C2B C1B O11B Tb2 -36.5(18) . . . . ?
O12C C1C O11C Tb1 146.1(15) . . . . ?
C2C C1C O11C Tb1 -39.6(18) . . . . ?
O11A C1A O12A Tb1 -158(3) . . . . ?
C2A C1A O12A Tb1 -8(5) . . . . ?
O11B C1B O12B Tb1 1(3) . . . . ?
C2B C1B O12B Tb1 -177.8(15) . . . . ?
O11C C1C O12C Tb2 -2(3) . . . 1_545 ?
C2C C1C O12C Tb2 -175.9(15) . . . 1_545 ?
C1A C2A O21A Tb1 -43(3) . . . . ?
C3A C2A O21A Tb1 81(2) . . . . ?
C3B C2B O21B Tb2 138.6(11) . . . . ?
C1B C2B O21B Tb2 17.9(17) . . . . ?
C1C C2C O21C Tb1 15.0(15) . . . . ?
C3C C2C O21C Tb1 139.1(11) . . . . ?
C2A C3A O31A Tb2 130(2) . . . 1_656 ?
C4A C3A O31A Tb2 16(3) . . . 1_656 ?
C4B C3B O31B Tb1 -14.6(14) . . . 1_565 ?
C2B C3B O31B Tb1 109.9(11) . . . 1_565 ?
C4C C3C O31C Tb2 -13.6(14) . . . . ?
C2C C3C O31C Tb2 111.2(11) . . . . ?
O42A C4A O41A Tb2 179(2) . . . 1_656 ?
C3A C4A O41A Tb2 38(3) . . . 1_656 ?
O42B C4B O41B Tb1 -156.0(11) . . . 1_565 ?
C3B C4B O41B Tb1 24.6(19) . . . 1_565 ?
O42C C4C O41C Tb2 -156.3(11) . . . . ?
C3C C4C O41C Tb2 24.1(18) . . . . ?
O41A C4A O42A Tb1 172(2) . . . . ?
C3A C4A O42A Tb1 -50(4) . . . . ?
O41B C4B O42B Tb1 -18(2) . . . 1_465 ?
C3B C4B O42B Tb1 161.7(10) . . . 1_465 ?
O41C C4C O42C Tb2 -18(2) . . . 1_655 ?
C3C C4C O42C Tb2 161.2(10) . . . 1_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O41B 0.87 2.02 2.861(17) 160.8 1_645 yes
O31A H31A O11A 0.87 2.28 3.14(3) 173.1 1_655 yes
O21B H21B O11C 0.86 1.74 2.591(14) 170.5 1_565 yes
O31B H31B O11C 0.87 1.99 2.836(16) 165.8 1_565 yes
O21C H21C O11B 0.86 1.76 2.601(13) 166.8 . yes
O31C H31C O11B 0.86 2.01 2.841(16) 164.4 . yes
O1W H11W O11A 0.87 1.47 2.29(4) 158.3 1_454 yes
O1W H12W O41C 0.86 1.99 2.838(18) 171.3 1_455 yes
O2W H21W O41A 1.11 1.72 2.47(4) 119.6 . yes
O2W H22W O11A 0.72 1.74 2.44(5) 164.4 1_545 yes

_refine_diff_density_max         2.069
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.162


# start Validation Reply Form
_vrf_PLAT234_Compound_Tb-L'-383K 
;
PROBLEM: Large Hirshfeld Difference O12A     --C1A      .       0.31 Ang.  
RESPONSE: Despite the fact that it could not be properly solved, this ligand
is involved in a disorder coming from its rearrangement with the high 
temperature.
;
_vrf_PLAT430_Compound_Tb-L'-383K 
;
PROBLEM: Short Inter D...A Contact  O11A     ..O2W      .       2.44 Ang.  
RESPONSE: This water molecule has been refined with a partial occupation 
given big ellipsoid it presents. Apart from the fact that it could be 
involved in a disorder, its partial occupation agrees well with the 
fact it should be released from the crystal structure at that temperature.
;
_vrf_PLAT770_Compound_Tb-L'-383K 
;
PROBLEM: Suspect C-H Bond in CIF:  C3B      --H31B      .       1.58 Ang.  
RESPONSE: The hydrogen atom belongs to a hydroxyl group. The hydrogen atom,
ideally pointing out to other water molecule in the voids of the structure, has
lost the hydrogen bonding receptor at this temperature owing to the dehydration
of the MOF. 
;
_vrf_PLAT043_Compound_Tb-L'-383K 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      11.69 Check 
RESPONSE: The difference in the molecular weight reported corresponds to the
partial occupation of the lattice water molecule, which has been refined with
a partial occupation given big ellipsoid it presents. Apart from the fact that
it could be involved in a disorder, its partial occupation agrees well with the 
fact it should be released from the crystal structure at that temperature.
;
_vrf_PLAT090_Compound_Tb-L'-383K 
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.83 Note  
RESPONSE: The data has been acquired for a crystalline phase generated while
heating a single crystal up to 110 \^A?C. This fact has to be added to the facts 
that all specimens of this compound crystallize as twins and that the crystal
structre chiral and triclinic. All in all, these are best possible data 
according to the previous facts.
;
_vrf_PLAT220_Compound_Tb-L'-383K 
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        7.1 Ratio 
RESPONSE: The structure contains one lattice water molecule which has been 
refined with a partial occupation given big ellipsoid it presents. 
Apart from the fact that it could be involved in a disorder, 
its partial occupation agrees well with the fact it should be released 
from the crystal structure at that temperature.
;
_vrf_PLAT342_Compound_Tb-L'-383K 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03111 Ang.  
RESPONSE: During the solid state transformation of the structure, it is observed
that one of the tartrate ligands undergoes a deep rearrangement (it changes its 
coordination mode). As a result, the ligand seems to be involved in some kind of
disorder. All our efforts to correctly handle that disorder have been unfruitful,
in such a way that ellipsoids of that ligand, as well as those in the surroundings,
are clearly affected. The refinement has been converged by using some soft 
restraints.
;
# end Validation Reply Form

_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound_Tb-D
_database_code_depnum_ccdc_archive 'CCDC 1981572'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-D-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-D-tartrate-k2O,O':k2O'',O''')diaquaditerbium(III)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 O20 Tb2, 4(H2 O)'
_chemical_formula_sum            'C12 H24 O24 Tb2'
_chemical_formula_weight         870.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   6.0130(3)
_cell_length_b                   7.3878(3)
_cell_length_c                   13.2837(5)
_cell_angle_alpha                102.251(4)
_cell_angle_beta                 101.786(4)
_cell_angle_gamma                90.505(4)
_cell_volume                     563.66(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5692
_cell_measurement_theta_min      3.1980
_cell_measurement_theta_max      27.2150

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7338 9183 1830 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.2662 9203 1830 nmt -0.9998 0.0001 0.0000 -0.0153 0.9610 -0.0781 0.0077
-0.9799 -0.9602

_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_F_000             418
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    6.339
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.011
_exptl_absorpt_correction_T_max  0.052
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω
_diffrn_reflns_number            9724
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.650
_diffrn_reflns_theta_max         25.540
_diffrn_reflns_theta_full        26.003
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measured_fraction_theta_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_point_group_measured_fraction_full 0.937
_reflns_number_total             3938
_reflns_number_gt                3838
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_max     0.917
_reflns_Friedel_fraction_full    0.925

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0778P)²+4.2203P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1788 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         3938
_refine_ls_number_parameters     343
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.1094
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.005
_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 0.97849(7) 0.18296(6) 0.32126(5) 0.0090(2) Uani 1 1 d . . . . .
Tb2 Tb 1.02147(8) 0.81596(7) 0.67871(5) 0.0099(3) Uani 1 1 d . . . . .
C1A C 0.777(4) 0.066(3) 0.1039(16) 0.012(5) Uani 1 1 d . U . . .
C2A C 0.623(3) -0.031(3) 0.0005(13) 0.013(4) Uani 1 1 d . U . . .
H2A H 0.637965 0.038189 -0.053160 0.015 Uiso 1 1 calc R U . . .
C3A C 0.376(3) -0.027(3) 0.0139(13) 0.010(3) Uani 1 1 d . U . . .
H3A H 0.344575 0.102411 0.041340 0.012 Uiso 1 1 calc R U . . .
C4A C 0.216(4) -0.095(3) -0.0962(17) 0.015(5) Uani 1 1 d . U . . .
C1B C 0.839(3) 0.611(2) 0.4318(13) 0.014(3) Uani 1 1 d . U . . .
C2B C 0.654(3) 0.755(3) 0.4357(14) 0.013(4) Uani 1 1 d . U . . .
H2B H 0.511744 0.691194 0.437724 0.016 Uiso 1 1 calc R U . . .
C3B C 0.619(3) 0.823(2) 0.3325(12) 0.008(3) Uani 1 1 d . U . . .
H3B H 0.534602 0.724863 0.275305 0.009 Uiso 1 1 calc R U . . .
C4B C 0.487(3) 0.997(2) 0.3377(12) 0.009(3) Uani 1 1 d . U . . .
C1C C 1.156(3) 0.168(3) 0.5663(13) 0.014(3) Uani 1 1 d . . . . .
C2C C 1.339(3) 0.304(3) 0.5638(12) 0.008(3) Uani 1 1 d . U . . .
H2C H 1.479797 0.238869 0.560844 0.010 Uiso 1 1 calc R U . . .
C3C C 1.377(3) 0.450(2) 0.6702(12) 0.011(3) Uani 1 1 d . U . . .
H3C H 1.460838 0.394216 0.726381 0.013 Uiso 1 1 calc R U . . .
C4C C 1.511(3) 0.623(2) 0.6656(12) 0.011(3) Uani 1 1 d . U . . .
O11A O 0.737(2) 0.2236(18) 0.1517(9) 0.017(3) Uani 1 1 d . . . . .
O12A O 0.951(2) -0.0150(19) 0.1422(9) 0.016(3) Uani 1 1 d . . . . .
O21A O 0.6746(19) -0.2155(17) -0.0355(9) 0.015(3) Uani 1 1 d . . . . .
O31A O 0.349(2) -0.1309(18) 0.0886(9) 0.015(2) Uani 1 1 d . . . . .
O41A O 0.245(2) -0.0012(19) -0.1643(10) 0.018(3) Uani 1 1 d . . . . .
O42A O 0.076(2) -0.2235(18) -0.1153(10) 0.016(3) Uani 1 1 d . . . . .
O12B O 0.815(2) 0.4765(17) 0.3567(9) 0.010(2) Uani 1 1 d . . . . .
O11B O 1.012(2) 0.6462(19) 0.5079(10) 0.019(3) Uani 1 1 d . . . . .
O21B O 0.7154(19) 0.8939(16) 0.5280(8) 0.010(2) Uani 1 1 d . . . . .
O31B O 0.833(2) 0.8595(16) 0.3097(10) 0.011(3) Uani 1 1 d . . . . .
O41B O 0.592(2) 1.1414(19) 0.3325(9) 0.015(2) Uani 1 1 d . U . . .
O42B O 0.282(2) 0.9867(17) 0.3438(9) 0.015(2) Uani 1 1 d . . . . .
O11C O 0.976(2) 0.1451(16) 0.4925(9) 0.013(2) Uani 1 1 d . . . . .
O12C O 1.179(2) 0.0836(19) 0.6416(11) 0.017(3) Uani 1 1 d . . . . .
O21C O 1.281(2) 0.3796(16) 0.4729(9) 0.011(2) Uani 1 1 d . . . . .
O31C O 1.165(2) 0.5069(16) 0.6951(10) 0.010(2) Uani 1 1 d . . . . .
O41C O 1.409(2) 0.7705(18) 0.6673(9) 0.014(3) Uani 1 1 d . U . . .
O42C O 1.719(2) 0.6093(17) 0.6653(10) 0.014(2) Uani 1 1 d . . . . .
O1W O 1.248(2) 0.3469(18) 0.2570(9) 0.016(3) Uani 1 1 d . U . . .
O2W O 0.767(2) 1.0258(19) 0.7497(10) 0.019(3) Uani 1 1 d . U . . .
O3W O 0.805(3) 0.586(2) 0.1300(12) 0.024(4) Uani 1 1 d . . . . .
O4W O 1.293(4) 0.373(2) 0.8755(14) 0.039(5) Uani 1 1 d . . . . .
O5W O 0.775(3) 1.362(3) 0.8843(15) 0.054(5) Uani 1 1 d . . . . .
O6W O 1.219(2) 0.5020(18) 0.0762(11) 0.020(3) Uani 1 1 d . . . . .
H21A H 0.790055 -0.229278 -0.060705 0.031 Uiso 1 1 d . U . . .
H31A H 0.217446 -0.089411 0.096220 0.031 Uiso 1 1 d . U . . .
H21B H 0.800192 0.990938 0.525016 0.031 Uiso 1 1 d . U . . .
H31B H 0.854228 0.776701 0.258669 0.031 Uiso 1 1 d . U . . .
H21C H 1.204220 0.475514 0.479382 0.031 Uiso 1 1 d . U . . .
H31C H 1.160249 0.476555 0.753055 0.031 Uiso 1 1 d . U . . .
H11W H 1.257868 0.382626 0.205023 0.031 Uiso 1 1 d . U . . .
H12W H 1.366874 0.292662 0.278042 0.031 Uiso 1 1 d . U . . .
H21W H 0.751319 1.121038 0.794450 0.031 Uiso 1 1 d . U . . .
H22W H 0.636473 0.971969 0.722506 0.031 Uiso 1 1 d . U . . .
H31W H 0.749805 0.617867 0.073650 0.031 Uiso 1 1 d . U . . .
H32W H 0.760504 0.475266 0.124947 0.031 Uiso 1 1 d . U . . .
H41W H 1.286849 0.250969 0.861718 0.031 Uiso 1 1 d . U . . .
H42W H 1.267328 0.403188 0.935624 0.031 Uiso 1 1 d . U . . .
H51W H 0.633642 1.373141 0.879003 0.031 Uiso 1 1 d . U . . .
H52W H 0.891030 1.409198 0.932768 0.031 Uiso 1 1 d . U . . .
H61W H 1.290476 0.603343 0.080395 0.031 Uiso 1 1 d . U . . .
H62W H 1.093257 0.529185 0.090242 0.031 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O11C 2.353(11) . ?
Tb1 O42B 2.354(12) 1_645 ?
Tb1 O41B 2.378(12) 1_545 ?
Tb1 O12B 2.384(12) . ?
Tb1 O1W 2.409(12) . ?
Tb1 O12A 2.487(12) . ?
Tb1 O11A 2.496(12) . ?
Tb1 O31B 2.499(12) 1_545 ?
Tb1 O21C 2.586(11) . ?
Tb1 C1A 2.84(2) . ?
Tb2 O42C 2.320(12) 1_455 ?
Tb2 O11B 2.337(13) . ?
Tb2 O41A 2.369(12) 1_666 ?
Tb2 O12C 2.372(13) 1_565 ?
Tb2 O2W 2.375(13) . ?
Tb2 O41C 2.389(12) . ?
Tb2 O31C 2.485(12) . ?
Tb2 O21B 2.594(12) . ?
Tb2 O42A 2.767(13) 1_666 ?
Tb2 C4A 2.91(2) 1_666 ?
C1A O11A 1.25(2) . ?
C1A O12A 1.28(2) . ?
C1A C2A 1.52(3) . ?
C2A O21A 1.40(2) . ?
C2A C3A 1.53(2) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.41(2) . ?
C3A C4A 1.56(3) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.21(3) . ?
C4A O41A 1.29(3) . ?
C1B O12B 1.23(2) . ?
C1B O11B 1.27(2) . ?
C1B C2B 1.55(3) . ?
C2B O21B 1.40(2) . ?
C2B C3B 1.53(2) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.420(19) . ?
C3B C4B 1.52(2) . ?
C3B H3B 0.9800 . ?
C4B O42B 1.25(2) . ?
C4B O41B 1.26(2) . ?
C1C O12C 1.27(2) . ?
C1C O11C 1.29(2) . ?
C1C C2C 1.49(2) . ?
C2C O21C 1.42(2) . ?
C2C C3C 1.56(2) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.43(2) . ?
C3C C4C 1.53(2) . ?
C3C H3C 0.9800 . ?
C4C O41C 1.25(2) . ?
C4C O42C 1.26(2) . ?
O21A H21A 0.8283 . ?
O31A H31A 0.8687 . ?
O21B H21B 0.8888 . ?
O31B H31B 0.8421 . ?
O21C H21C 0.8469 . ?
O31C H31C 0.8518 . ?
O1W H11W 0.8012 . ?
O1W H12W 0.8469 . ?
O2W H21W 0.8392 . ?
O2W H22W 0.8512 . ?
O3W H31W 0.8355 . ?
O3W H32W 0.8468 . ?
O4W H41W 0.8765 . ?
O4W H42W 0.8289 . ?
O5W H51W 0.8450 . ?
O5W H52W 0.8611 . ?
O6W H61W 0.8447 . ?
O6W H62W 0.8338 . ?

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
O11C Tb1 O42B 80.3(4) . 1_645 ?
O11C Tb1 O41B 72.4(4) . 1_545 ?
O42B Tb1 O41B 130.4(4) 1_645 1_545 ?
O11C Tb1 O12B 90.9(4) . . ?
O42B Tb1 O12B 152.0(4) 1_645 . ?
O41B Tb1 O12B 70.0(4) 1_545 . ?
O11C Tb1 O1W 130.7(4) . . ?
O42B Tb1 O1W 81.5(4) 1_645 . ?
O41B Tb1 O1W 146.7(4) 1_545 . ?
O12B Tb1 O1W 84.5(4) . . ?
O11C Tb1 O12A 138.3(4) . . ?
O42B Tb1 O12A 76.3(4) 1_645 . ?
O41B Tb1 O12A 97.7(4) 1_545 . ?
O12B Tb1 O12A 124.6(4) . . ?
O1W Tb1 O12A 79.2(4) . . ?
O11C Tb1 O11A 144.8(4) . . ?
O42B Tb1 O11A 127.4(4) 1_645 . ?
O41B Tb1 O11A 72.7(4) 1_545 . ?
O12B Tb1 O11A 73.0(4) . . ?
O1W Tb1 O11A 79.8(4) . . ?
O12A Tb1 O11A 52.2(4) . . ?
O11C Tb1 O31B 71.4(4) . 1_545 ?
O42B Tb1 O31B 69.4(4) 1_645 1_545 ?
O41B Tb1 O31B 62.9(4) 1_545 1_545 ?
O12B Tb1 O31B 132.7(4) . 1_545 ?
O1W Tb1 O31B 140.3(4) . 1_545 ?
O12A Tb1 O31B 68.2(4) . 1_545 ?
O11A Tb1 O31B 96.5(4) . 1_545 ?
O11C Tb1 O21C 63.3(4) . . ?
O42B Tb1 O21C 75.9(4) 1_645 . ?
O41B Tb1 O21C 123.0(4) 1_545 . ?
O12B Tb1 O21C 76.4(4) . . ?
O1W Tb1 O21C 67.9(4) . . ?
O12A Tb1 O21C 139.3(4) . . ?
O11A Tb1 O21C 137.1(4) . . ?
O31B Tb1 O21C 126.4(4) 1_545 . ?
O11C Tb1 C1A 145.7(5) . . ?
O42B Tb1 C1A 103.1(5) 1_645 . ?
O41B Tb1 C1A 80.3(5) 1_545 . ?
O12B Tb1 C1A 99.1(5) . . ?
O1W Tb1 C1A 83.2(5) . . ?
O12A Tb1 C1A 26.9(5) . . ?
O11A Tb1 C1A 26.2(5) . . ?
O31B Tb1 C1A 77.9(5) 1_545 . ?
O21C Tb1 C1A 151.0(5) . . ?
O42C Tb2 O11B 81.8(5) 1_455 . ?
O42C Tb2 O41A 126.8(4) 1_455 1_666 ?
O11B Tb2 O41A 146.9(5) . 1_666 ?
O42C Tb2 O12C 151.8(4) 1_455 1_565 ?
O11B Tb2 O12C 91.6(5) . 1_565 ?
O41A Tb2 O12C 70.4(5) 1_666 1_565 ?
O42C Tb2 O2W 80.5(4) 1_455 . ?
O11B Tb2 O2W 132.0(4) . . ?
O41A Tb2 O2W 75.2(4) 1_666 . ?
O12C Tb2 O2W 84.0(5) 1_565 . ?
O42C Tb2 O41C 132.1(4) 1_455 . ?
O11B Tb2 O41C 74.1(4) . . ?
O41A Tb2 O41C 73.7(4) 1_666 . ?
O12C Tb2 O41C 70.7(5) 1_565 . ?
O2W Tb2 O41C 144.9(4) . . ?
O42C Tb2 O31C 70.2(4) 1_455 . ?
O11B Tb2 O31C 73.1(4) . . ?
O41A Tb2 O31C 99.1(4) 1_666 . ?
O12C Tb2 O31C 133.9(4) 1_565 . ?
O2W Tb2 O31C 138.3(4) . . ?
O41C Tb2 O31C 63.4(4) . . ?
O42C Tb2 O21B 76.8(4) 1_455 . ?
O11B Tb2 O21B 62.8(4) . . ?
O41A Tb2 O21B 133.2(4) 1_666 . ?
O12C Tb2 O21B 75.8(4) 1_565 . ?
O2W Tb2 O21B 69.8(4) . . ?
O41C Tb2 O21B 123.6(4) . . ?
O31C Tb2 O21B 127.7(4) . . ?
O42C Tb2 O42A 78.7(4) 1_455 1_666 ?
O11B Tb2 O42A 141.9(4) . 1_666 ?
O41A Tb2 O42A 50.0(4) 1_666 1_666 ?
O12C Tb2 O42A 120.1(4) 1_565 1_666 ?
O2W Tb2 O42A 76.2(4) . 1_666 ?
O41C Tb2 O42A 95.6(4) . 1_666 ?
O31C Tb2 O42A 69.6(4) . 1_666 ?
O21B Tb2 O42A 140.7(3) . 1_666 ?
O42C Tb2 C4A 102.8(5) 1_455 1_666 ?
O11B Tb2 C4A 151.5(6) . 1_666 ?
O41A Tb2 C4A 25.7(6) 1_666 1_666 ?
O12C Tb2 C4A 96.1(6) 1_565 1_666 ?
O2W Tb2 C4A 76.3(5) . 1_666 ?
O41C Tb2 C4A 82.6(5) . 1_666 ?
O31C Tb2 C4A 81.9(5) . 1_666 ?
O21B Tb2 C4A 145.8(5) . 1_666 ?
O42A Tb2 C4A 24.5(5) 1_666 1_666 ?
O11A C1A O12A 119.6(17) . . ?
O11A C1A C2A 121.4(18) . . ?
O12A C1A C2A 118.9(17) . . ?
O11A C1A Tb1 61.5(10) . . ?
O12A C1A Tb1 61.2(9) . . ?
C2A C1A Tb1 162.8(14) . . ?
O21A C2A C1A 114.0(15) . . ?
O21A C2A C3A 109.3(15) . . ?
C1A C2A C3A 108.8(14) . . ?
O21A C2A H2A 108.2 . . ?
C1A C2A H2A 108.2 . . ?
C3A C2A H2A 108.2 . . ?
O31A C3A C2A 109.1(16) . . ?
O31A C3A C4A 114.2(16) . . ?
C2A C3A C4A 108.7(14) . . ?
O31A C3A H3A 108.2 . . ?
C2A C3A H3A 108.2 . . ?
C4A C3A H3A 108.2 . . ?
O42A C4A O41A 123.4(19) . . ?
O42A C4A C3A 122.9(19) . . ?
O41A C4A C3A 113.7(18) . . ?
O42A C4A Tb2 71.1(11) . 1_444 ?
O41A C4A Tb2 53.0(10) . 1_444 ?
C3A C4A Tb2 164.3(15) . 1_444 ?
O12B C1B O11B 125.0(17) . . ?
O12B C1B C2B 119.7(15) . . ?
O11B C1B C2B 115.3(15) . . ?
O21B C2B C3B 115.2(16) . . ?
O21B C2B C1B 109.9(14) . . ?
C3B C2B C1B 107.1(14) . . ?
O21B C2B H2B 108.1 . . ?
C3B C2B H2B 108.1 . . ?
C1B C2B H2B 108.1 . . ?
O31B C3B C4B 108.9(13) . . ?
O31B C3B C2B 109.7(13) . . ?
C4B C3B C2B 112.0(13) . . ?
O31B C3B H3B 108.7 . . ?
C4B C3B H3B 108.7 . . ?
C2B C3B H3B 108.7 . . ?
O42B C4B O41B 125.0(15) . . ?
O42B C4B C3B 118.6(14) . . ?
O41B C4B C3B 116.4(14) . . ?
O12C C1C O11C 122.2(16) . . ?
O12C C1C C2C 119.8(15) . . ?
O11C C1C C2C 118.0(14) . . ?
O21C C2C C1C 110.4(13) . . ?
O21C C2C C3C 114.7(15) . . ?
C1C C2C C3C 106.4(13) . . ?
O21C C2C H2C 108.4 . . ?
C1C C2C H2C 108.4 . . ?
C3C C2C H2C 108.4 . . ?
O31C C3C C4C 107.2(13) . . ?
O31C C3C C2C 111.1(13) . . ?
C4C C3C C2C 111.2(13) . . ?
O31C C3C H3C 109.1 . . ?
C4C C3C H3C 109.1 . . ?
C2C C3C H3C 109.1 . . ?
O41C C4C O42C 124.7(15) . . ?
O41C C4C C3C 118.1(15) . . ?
O42C C4C C3C 117.2(15) . . ?
C1A O11A Tb1 92.3(11) . . ?
C1A O12A Tb1 92.0(11) . . ?
C2A O21A H21A 115.7 . . ?
C3A O31A H31A 94.8 . . ?
C4A O41A Tb2 101.3(12) . 1_444 ?
C4A O42A Tb2 84.4(12) . 1_444 ?
C1B O12B Tb1 136.0(12) . . ?
C1B O11B Tb2 126.8(12) . . ?
C2B O21B Tb2 116.6(11) . . ?
C2B O21B H21B 117.0 . . ?
Tb2 O21B H21B 91.6 . . ?
C3B O31B Tb1 121.6(9) . 1_565 ?
C3B O31B H31B 109.2 . . ?
Tb1 O31B H31B 117.6 1_565 . ?
C4B O41B Tb1 128.9(11) . 1_565 ?
C4B O42B Tb1 134.2(11) . 1_465 ?
C1C O11C Tb1 122.9(10) . . ?
C1C O12C Tb2 138.5(12) . 1_545 ?
C2C O21C Tb1 114.9(9) . . ?
C2C O21C H21C 115.8 . . ?
Tb1 O21C H21C 94.9 . . ?
C3C O31C Tb2 122.1(9) . . ?
C3C O31C H31C 106.4 . . ?
Tb2 O31C H31C 115.3 . . ?
C4C O41C Tb2 127.3(11) . . ?
C4C O42C Tb2 135.1(11) . 1_655 ?
Tb1 O1W H11W 139.2 . . ?
Tb1 O1W H12W 98.9 . . ?
H11W O1W H12W 110.5 . . ?
Tb2 O2W H21W 147.3 . . ?
Tb2 O2W H22W 103.9 . . ?
H21W O2W H22W 108.1 . . ?
H31W O3W H32W 108.6 . . ?
H41W O4W H42W 104.7 . . ?
H51W O5W H52W 132.4 . . ?
H61W O6W H62W 106.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.83 2.00 2.825(17) 171.9 1_655 yes
O31A H31A O12A 0.87 1.87 2.726(18) 167.0 1_455 yes
O21B H21B O11C 0.89 1.73 2.597(16) 166.4 1_565 yes
O31B H31B O3W 0.84 1.94 2.75(2) 163.1 . yes
O21C H21C O11B 0.85 1.75 2.586(18) 167.0 . yes
O31C H31C O4W 0.85 1.97 2.76(2) 152.6 . yes
O1W H11W O6W 0.80 2.06 2.847(17) 167.8 . yes
O1W H12W O41B 0.85 1.89 2.728(18) 169.0 1_645 yes
O2W H21W O5W 0.84 1.90 2.73(2) 165.9 . yes
O2W H22W O41C 0.85 1.93 2.735(18) 158.1 1_455 yes
O3W H31W O21A 0.84 2.08 2.876(19) 159.3 1_565 yes
O3W H32W O11A 0.85 1.98 2.79(2) 161.9 . yes
O4W H41W O41A 0.88 1.83 2.70(2) 174.3 1_656 yes
O4W H42W O6W 0.83 1.94 2.76(2) 173.7 1_556 yes
O5W H51W O4W 0.84 2.04 2.88(3) 172.5 1_465 yes
O5W H52W O6W 0.86 2.43 3.28(2) 172.0 1_566 yes
O6W H61W O31A 0.84 1.97 2.777(18) 160.1 1_665 yes
O6W H62W O3W 0.83 1.94 2.77(2) 176.7 . yes

_refine_diff_density_max         2.909
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.209






# start Validation Reply Form
_vrf_PLAT029_Compound_Tb-D       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.951 Why?  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately. Moreover, single crystals of this compound are particularly
small and do not diffract too much at high angles.
;
_vrf_PLAT090_Compound_Tb-D       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.83 Note  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately. Moreover, single crystals of this compound are particularly
small and do not diffract too much at high angles. Accordingly, the structure has
been refined employing some soft restraints to model the A.D.P.s of some atoms.
;
_vrf_PLAT920_Compound_Tb-D       
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       0.77 Degree
RESPONSE: ...
;
_vrf_PLAT342_Compound_Tb-D       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03444 Ang.  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. The twin has been successfully found
but there is a substantially high percentage of reflections which cannot be 
indexed appropriately.
;
# end Validation Reply Form


_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Compound_Tm-L
_database_code_depnum_ccdc_archive 'CCDC 1981582'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-L-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-L-tartrate-k2O,O':k2O'',O''')diaquadithulium(III)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 O20 Tm2, 4(H2 O)'
_chemical_formula_sum            'C12 H24 O24 Tm2'
_chemical_formula_weight         890.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9715(3)
_cell_length_b                   7.3102(4)
_cell_length_c                   13.3149(7)
_cell_angle_alpha                102.364(2)
_cell_angle_beta                 102.224(2)
_cell_angle_gamma                90.276(2)
_cell_volume                     554.11(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20350
_cell_measurement_theta_min      2.857
_cell_measurement_theta_max      28.831


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.668
_exptl_crystal_F_000             426
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    8.073
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_process_details   
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_reflns_number            20350
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.857
_diffrn_reflns_theta_max         28.831
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5641
_reflns_number_gt                5494
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_max     0.963
_reflns_Friedel_fraction_full    0.984

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;


_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+4.2586P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2620 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(4)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         5641
_refine_ls_number_parameters     344
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0614
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_restrained_S_all      1.230
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.02443(4) 0.82002(4) 0.67629(3) 0.00346(12) Uani 1 1 d . . . . .
Tm2 Tm -0.02471(4) 0.18192(4) 0.32428(3) 0.00386(12) Uani 1 1 d . . . . .
C1A C 0.2223(19) 0.9353(15) 0.8901(9) 0.004(2) Uani 1 1 d . U . . .
C2A C 0.3802(16) 1.0305(14) 0.9946(8) 0.0061(19) Uani 1 1 d . U . . .
H2A H 0.364174 0.960449 1.047997 0.007 Uiso 1 1 calc R U . . .
C3A C 0.6296(16) 1.0288(15) 0.9835(7) 0.0067(17) Uani 1 1 d . . . . .
H3A H 0.666899 0.898731 0.958859 0.008 Uiso 1 1 calc R U . . .
C4A C 0.7861(19) 1.1080(16) 1.0915(9) 0.010(2) Uani 1 1 d . . . . .
C1B C 0.1592(15) 0.3913(13) 0.5660(7) 0.0063(16) Uani 1 1 d . . . . .
C2B C 0.3474(17) 0.2489(16) 0.5635(8) 0.0055(19) Uani 1 1 d . U . . .
H2B H 0.490385 0.313015 0.561508 0.007 Uiso 1 1 calc R U . . .
C3B C 0.3814(14) 0.1806(12) 0.6664(7) 0.0039(15) Uani 1 1 d . U . . .
H3B H 0.466008 0.279150 0.724192 0.005 Uiso 1 1 calc R U . . .
C4B C 0.5149(15) 0.0012(12) 0.6612(7) 0.0050(15) Uani 1 1 d . U . . .
C1C C -0.1541(15) 0.8303(12) 0.4312(7) 0.0035(15) Uani 1 1 d . U . . .
C2C C -0.3427(17) 0.6950(15) 0.4330(8) 0.0040(18) Uani 1 1 d . U . . .
H2C H -0.482998 0.763555 0.434519 0.005 Uiso 1 1 calc R U . . .
C3C C -0.3838(15) 0.5431(12) 0.3287(7) 0.0049(15) Uani 1 1 d . . . . .
H3C H -0.472572 0.596733 0.272213 0.006 Uiso 1 1 calc R U . . .
C4C C -0.5157(16) 0.3700(13) 0.3346(7) 0.0067(16) Uani 1 1 d . U . . .
O11A O 0.2722(12) 0.7776(10) 0.8431(5) 0.0110(13) Uani 1 1 d . . . . .
O12A O 0.0506(12) 1.0152(10) 0.8514(5) 0.0088(13) Uani 1 1 d . . . . .
O21A O 0.3265(12) 1.2204(10) 1.0300(6) 0.0107(13) Uani 1 1 d . . . . .
O31A O 0.6521(12) 1.1318(10) 0.9062(6) 0.0112(13) Uani 1 1 d . . . . .
O41A O 0.7603(13) 1.0259(11) 1.1639(6) 0.0139(14) Uani 1 1 d . . . . .
O42A O 0.9319(13) 1.2406(11) 1.1064(7) 0.0178(16) Uani 1 1 d . . . . .
O11B O -0.0178(12) 0.3533(10) 0.4901(5) 0.0109(13) Uani 1 1 d . . . . .
O12B O 0.1810(12) 0.5291(9) 0.6407(6) 0.0083(13) Uani 1 1 d . . . . .
O21B O 0.2825(11) 0.1045(9) 0.4707(5) 0.0068(12) Uani 1 1 d . . . . .
O31B O 0.1650(11) 0.1413(9) 0.6876(5) 0.0050(12) Uani 1 1 d . U . . .
O41B O 0.4079(12) -0.1440(11) 0.6655(6) 0.0082(13) Uani 1 1 d . U . . .
O42B O 0.7211(11) 0.0123(9) 0.6550(5) 0.0072(12) Uani 1 1 d . . . . .
O11C O 0.0210(11) 0.8522(9) 0.5067(5) 0.0070(12) Uani 1 1 d . . . . .
O12C O -0.1754(12) 0.9145(10) 0.3568(6) 0.0073(13) Uani 1 1 d . U . . .
O21C O -0.2869(11) 0.6224(9) 0.5261(5) 0.0048(11) Uani 1 1 d . U . . .
O31C O -0.1709(11) 0.4864(9) 0.3015(6) 0.0069(12) Uani 1 1 d . . . . .
O41C O -0.4090(12) 0.2232(11) 0.3349(6) 0.0083(13) Uani 1 1 d . U . . .
O42C O -0.7261(11) 0.3852(9) 0.3366(6) 0.0083(13) Uani 1 1 d . . . . .
O1W O -0.2367(12) 0.6569(10) 0.7377(6) 0.0112(13) Uani 1 1 d . . . . .
O2W O 0.2248(11) -0.0233(10) 0.2537(6) 0.0123(14) Uani 1 1 d . . . . .
O3W O 0.1925(16) 0.4140(11) 0.8654(6) 0.0149(15) Uani 1 1 d . . . . .
O4W O -0.3028(17) 0.6352(12) 0.1242(7) 0.0198(17) Uani 1 1 d . . . . .
O5W O 0.2169(15) -0.3564(13) 0.1141(7) 0.027(2) Uani 1 1 d . . . . .
O6W O -0.2257(13) 0.5091(11) 0.9211(6) 0.0163(15) Uani 1 1 d . . . . .
H21A H 0.206053 1.242838 1.054038 0.024 Uiso 1 1 d . U . . .
H31A H 0.786415 1.111536 0.895063 0.024 Uiso 1 1 d . U . . .
H21B H 0.193216 0.026273 0.483663 0.024 Uiso 1 1 d . U . . .
H31B H 0.137529 0.213367 0.743598 0.024 Uiso 1 1 d . U . . .
H21C H -0.209541 0.526603 0.511787 0.024 Uiso 1 1 d . U . . .
H31C H -0.153169 0.515943 0.241088 0.024 Uiso 1 1 d . U . . .
H11W H -0.254244 0.619737 0.792122 0.024 Uiso 1 1 d . U . . .
H12W H -0.364215 0.703442 0.716055 0.024 Uiso 1 1 d . U . . .
H21W H 0.244977 -0.126251 0.214754 0.024 Uiso 1 1 d . U . . .
H22W H 0.359886 0.029958 0.279998 0.024 Uiso 1 1 d . U . . .
H31W H 0.246737 0.384483 0.924701 0.024 Uiso 1 1 d . U . . .
H32W H 0.242455 0.528023 0.873823 0.024 Uiso 1 1 d . U . . .
H41W H -0.269723 0.752215 0.138080 0.024 Uiso 1 1 d . U . . .
H42W H -0.298396 0.596001 0.060004 0.024 Uiso 1 1 d . U . . .
H51W H 0.351886 -0.362775 0.100740 0.024 Uiso 1 1 d . U . . .
H52W H 0.125257 -0.404075 0.055048 0.024 Uiso 1 1 d . U . . .
H61W H -0.311826 0.407285 0.914745 0.024 Uiso 1 1 d . U . . .
H62W H -0.104883 0.455310 0.905262 0.024 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O42B 2.306(6) 1_465 ?
Tm1 O11C 2.316(6) . ?
Tm1 O12B 2.323(7) . ?
Tm1 O1W 2.337(7) . ?
Tm1 O41B 2.341(7) 1_565 ?
Tm1 O12A 2.432(7) . ?
Tm1 O31B 2.453(6) 1_565 ?
Tm1 O11A 2.475(7) . ?
Tm1 O21C 2.589(6) . ?
Tm1 C1A 2.784(12) . ?
Tm2 O42C 2.271(7) 1_655 ?
Tm2 O11B 2.285(7) . ?
Tm2 O41A 2.301(7) 1_444 ?
Tm2 O12C 2.308(7) 1_545 ?
Tm2 O2W 2.316(7) . ?
Tm2 O41C 2.346(7) . ?
Tm2 O31C 2.450(7) . ?
Tm2 O21B 2.541(7) . ?
C1A O12A 1.252(13) . ?
C1A O11A 1.259(13) . ?
C1A C2A 1.527(15) . ?
C2A O21A 1.429(12) . ?
C2A C3A 1.527(12) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.426(12) . ?
C3A C4A 1.532(14) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.254(14) . ?
C4A O41A 1.274(14) . ?
C1B O12B 1.240(11) . ?
C1B O11B 1.281(11) . ?
C1B C2B 1.536(14) . ?
C2B O21B 1.423(12) . ?
C2B C3B 1.531(13) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.420(10) . ?
C3B C4B 1.535(12) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.254(12) . ?
C4B O42B 1.255(11) . ?
C1C O12C 1.259(11) . ?
C1C O11C 1.271(11) . ?
C1C C2C 1.503(13) . ?
C2C O21C 1.428(11) . ?
C2C C3C 1.554(13) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.433(10) . ?
C3C C4C 1.512(12) . ?
C3C H3C 0.9800 . ?
C4C O41C 1.251(12) . ?
C4C O42C 1.267(11) . ?
O21A H21A 0.8505 . ?
O31A H31A 0.8540 . ?
O21B H21B 0.8481 . ?
O31B H31B 0.8636 . ?
O21C H21C 0.8504 . ?
O31C H31C 0.9035 . ?
O1W H11W 0.8523 . ?
O1W H12W 0.8547 . ?
O2W H21W 0.8430 . ?
O2W H22W 0.8625 . ?
O3W H31W 0.8597 . ?
O3W H32W 0.8601 . ?
O4W H41W 0.8487 . ?
O4W H42W 0.8472 . ?
O5W H51W 0.8608 . ?
O5W H52W 0.8589 . ?
O6W H61W 0.8811 . ?
O6W H62W 0.8670 . ?

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
O42B Tm1 O11C 81.0(2) 1_465 . ?
O42B Tm1 O12B 151.0(2) 1_465 . ?
O11C Tm1 O12B 90.1(2) . . ?
O42B Tm1 O1W 81.3(2) 1_465 . ?
O11C Tm1 O1W 129.7(2) . . ?
O12B Tm1 O1W 83.5(3) . . ?
O42B Tm1 O41B 132.0(3) 1_465 1_565 ?
O11C Tm1 O41B 73.2(2) . 1_565 ?
O12B Tm1 O41B 69.7(3) . 1_565 ?
O1W Tm1 O41B 145.6(2) . 1_565 ?
O42B Tm1 O12A 75.9(2) 1_465 . ?
O11C Tm1 O12A 139.4(2) . . ?
O12B Tm1 O12A 124.9(2) . . ?
O1W Tm1 O12A 79.2(2) . . ?
O41B Tm1 O12A 98.4(2) 1_565 . ?
O42B Tm1 O31B 69.7(2) 1_465 1_565 ?
O11C Tm1 O31B 72.3(2) . 1_565 ?
O12B Tm1 O31B 133.5(2) . 1_565 ?
O1W Tm1 O31B 140.6(2) . 1_565 ?
O41B Tm1 O31B 64.1(2) 1_565 1_565 ?
O12A Tm1 O31B 68.5(2) . 1_565 ?
O42B Tm1 O11A 127.9(2) 1_465 . ?
O11C Tm1 O11A 144.5(2) . . ?
O12B Tm1 O11A 72.8(2) . . ?
O1W Tm1 O11A 80.2(2) . . ?
O41B Tm1 O11A 71.7(2) 1_565 . ?
O12A Tm1 O11A 52.9(2) . . ?
O31B Tm1 O11A 96.8(2) 1_565 . ?
O42B Tm1 O21C 75.1(2) 1_465 . ?
O11C Tm1 O21C 63.0(2) . . ?
O12B Tm1 O21C 76.3(2) . . ?
O1W Tm1 O21C 67.0(2) . . ?
O41B Tm1 O21C 123.6(2) 1_565 . ?
O12A Tm1 O21C 138.1(2) . . ?
O31B Tm1 O21C 126.3(2) 1_565 . ?
O11A Tm1 O21C 136.9(2) . . ?
O42B Tm1 C1A 102.6(3) 1_465 . ?
O11C Tm1 C1A 147.1(3) . . ?
O12B Tm1 C1A 99.7(3) . . ?
O1W Tm1 C1A 82.9(3) . . ?
O41B Tm1 C1A 80.9(3) 1_565 . ?
O12A Tm1 C1A 26.7(3) . . ?
O31B Tm1 C1A 78.3(3) 1_565 . ?
O11A Tm1 C1A 26.9(3) . . ?
O21C Tm1 C1A 149.8(3) . . ?
O42C Tm2 O11B 82.2(3) 1_655 . ?
O42C Tm2 O41A 121.7(3) 1_655 1_444 ?
O11B Tm2 O41A 148.0(3) . 1_444 ?
O42C Tm2 O12C 151.7(2) 1_655 1_545 ?
O11B Tm2 O12C 93.3(3) . 1_545 ?
O41A Tm2 O12C 75.1(3) 1_444 1_545 ?
O42C Tm2 O2W 79.8(2) 1_655 . ?
O11B Tm2 O2W 133.3(3) . . ?
O41A Tm2 O2W 75.8(3) 1_444 . ?
O12C Tm2 O2W 83.3(3) 1_545 . ?
O42C Tm2 O41C 133.0(3) 1_655 . ?
O11B Tm2 O41C 73.7(2) . . ?
O41A Tm2 O41C 74.3(3) 1_444 . ?
O12C Tm2 O41C 70.8(3) 1_545 . ?
O2W Tm2 O41C 144.4(3) . . ?
O42C Tm2 O31C 70.6(2) 1_655 . ?
O11B Tm2 O31C 74.1(3) . . ?
O41A Tm2 O31C 93.0(3) 1_444 . ?
O12C Tm2 O31C 135.1(2) 1_545 . ?
O2W Tm2 O31C 136.3(3) . . ?
O41C Tm2 O31C 64.3(2) . . ?
O42C Tm2 O21B 76.5(2) 1_655 . ?
O11B Tm2 O21B 64.2(2) . . ?
O41A Tm2 O21B 137.2(2) 1_444 . ?
O12C Tm2 O21B 76.3(2) 1_545 . ?
O2W Tm2 O21B 69.8(2) . . ?
O41C Tm2 O21B 124.0(2) . . ?
O31C Tm2 O21B 129.5(2) . . ?
O12A C1A O11A 121.1(10) . . ?
O12A C1A C2A 120.5(9) . . ?
O11A C1A C2A 118.4(9) . . ?
O12A C1A Tm1 60.8(5) . . ?
O11A C1A Tm1 62.8(6) . . ?
C2A C1A Tm1 162.8(8) . . ?
O21A C2A C3A 108.4(8) . . ?
O21A C2A C1A 112.4(8) . . ?
C3A C2A C1A 110.1(8) . . ?
O21A C2A H2A 108.7 . . ?
C3A C2A H2A 108.7 . . ?
C1A C2A H2A 108.7 . . ?
O31A C3A C2A 108.4(9) . . ?
O31A C3A C4A 113.3(9) . . ?
C2A C3A C4A 109.1(8) . . ?
O31A C3A H3A 108.7 . . ?
C2A C3A H3A 108.7 . . ?
C4A C3A H3A 108.7 . . ?
O42A C4A O41A 122.9(10) . . ?
O42A C4A C3A 122.3(11) . . ?
O41A C4A C3A 114.8(10) . . ?
O12B C1B O11B 124.1(8) . . ?
O12B C1B C2B 119.8(8) . . ?
O11B C1B C2B 116.0(8) . . ?
O21B C2B C3B 114.4(8) . . ?
O21B C2B C1B 109.1(8) . . ?
C3B C2B C1B 106.9(8) . . ?
O21B C2B H2B 108.7 . . ?
C3B C2B H2B 108.7 . . ?
C1B C2B H2B 108.7 . . ?
O31B C3B C2B 109.9(7) . . ?
O31B C3B C4B 107.9(7) . . ?
C2B C3B C4B 111.9(7) . . ?
O31B C3B H3B 109.0 . . ?
C2B C3B H3B 109.0 . . ?
C4B C3B H3B 109.0 . . ?
O41B C4B O42B 125.6(8) . . ?
O41B C4B C3B 116.6(8) . . ?
O42B C4B C3B 117.8(8) . . ?
O12C C1C O11C 123.6(8) . . ?
O12C C1C C2C 119.6(8) . . ?
O11C C1C C2C 116.7(8) . . ?
O21C C2C C1C 110.1(7) . . ?
O21C C2C C3C 114.3(8) . . ?
C1C C2C C3C 107.9(7) . . ?
O21C C2C H2C 108.1 . . ?
C1C C2C H2C 108.1 . . ?
C3C C2C H2C 108.1 . . ?
O31C C3C C4C 108.1(7) . . ?
O31C C3C C2C 111.1(7) . . ?
C4C C3C C2C 112.5(7) . . ?
O31C C3C H3C 108.3 . . ?
C4C C3C H3C 108.3 . . ?
C2C C3C H3C 108.3 . . ?
O41C C4C O42C 125.6(9) . . ?
O41C C4C C3C 117.2(8) . . ?
O42C C4C C3C 117.2(8) . . ?
C1A O11A Tm1 90.4(6) . . ?
C1A O12A Tm1 92.5(6) . . ?
C2A O21A H21A 119.3 . . ?
C3A O31A H31A 105.1 . . ?
C4A O41A Tm2 110.5(7) . 1_666 ?
C1B O11B Tm2 125.8(6) . . ?
C1B O12B Tm1 137.5(6) . . ?
C2B O21B Tm2 116.0(6) . . ?
C2B O21B H21B 107.1 . . ?
Tm2 O21B H21B 92.6 . . ?
C3B O31B Tm1 122.0(5) . 1_545 ?
C3B O31B H31B 114.1 . . ?
Tm1 O31B H31B 109.1 1_545 . ?
C4B O41B Tm1 128.3(6) . 1_545 ?
C4B O42B Tm1 134.5(6) . 1_645 ?
C1C O11C Tm1 125.9(6) . . ?
C1C O12C Tm2 138.1(6) . 1_565 ?
C2C O21C Tm1 114.8(5) . . ?
C2C O21C H21C 106.7 . . ?
Tm1 O21C H21C 97.7 . . ?
C3C O31C Tm2 120.4(5) . . ?
C3C O31C H31C 113.0 . . ?
Tm2 O31C H31C 113.6 . . ?
C4C O41C Tm2 127.4(6) . . ?
C4C O42C Tm2 135.2(6) . 1_455 ?
Tm1 O1W H11W 141.9 . . ?
Tm1 O1W H12W 103.0 . . ?
H11W O1W H12W 104.4 . . ?
Tm2 O2W H21W 148.9 . . ?
Tm2 O2W H22W 105.5 . . ?
H21W O2W H22W 105.6 . . ?
H31W O3W H32W 104.8 . . ?
H41W O4W H42W 105.8 . . ?
H51W O5W H52W 105.0 . . ?
H61W O6W H62W 98.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.85 1.91 2.751(10) 168.6 1_455 yes
O31A H31A O12A 0.85 1.88 2.722(10) 167.0 1_655 yes
O21B H21B O11C 0.85 1.75 2.595(9) 175.9 1_545 yes
O31B H31B O3W 0.86 1.91 2.724(11) 157.0 . yes
O21C H21C O11B 0.85 1.73 2.575(9) 171.8 . yes
O31C H31C O4W 0.90 2.00 2.775(11) 143.7 . yes
O1W H11W O6W 0.85 2.03 2.864(11) 167.2 . yes
O1W H12W O41B 0.85 1.87 2.704(10) 164.8 1_465 yes
O2W H21W O5W 0.84 1.90 2.722(11) 166.7 . yes
O2W H22W O41C 0.86 1.88 2.706(10) 159.1 1_655 yes
O3W H31W O21A 0.86 2.02 2.835(11) 158.4 1_545 yes
O3W H32W O11A 0.86 1.97 2.787(10) 158.5 . yes
O4W H41W O41A 0.85 1.96 2.800(11) 171.9 1_454 yes
O4W H42W O6W 0.85 1.96 2.799(11) 169.3 1_554 yes
O5W H51W O4W 0.86 2.02 2.844(13) 160.1 1_645 yes
O5W H52W O6W 0.86 2.43 3.251(12) 160.8 1_544 yes
O6W H61W O31A 0.88 2.00 2.804(10) 151.1 1_445 yes
O6W H62W O3W 0.87 1.97 2.802(12) 161.8 . yes

_refine_diff_density_max         2.088
_refine_diff_density_min         -2.079
_refine_diff_density_rms         0.213


# start Validation Reply Form
_vrf_PLAT987_Compound_Tm-L       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Single crystals of this compound are twinned as well as
the rest of isostructural compounds based on other lanthanide atoms.
Therefore, the structur has been refined with same twin law, indicated in
the article. Despite this aler Flack parameter is low and close to zero, which
indicates a pure enantiomer, so refinement has not been conducted.
;
# end Validation Reply Form 



_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound_Tm-D
_database_code_depnum_ccdc_archive 'CCDC 1981583'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-D-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-D-tartrate-k2O,O':k2O'',O''')diaquadithulium(III)] tetrahihydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Tm2 O20, 4(H2 O)'
_chemical_formula_sum            'C12 H24 O24 Tm2'
_chemical_formula_weight         890.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9678(4)
_cell_length_b                   7.3111(5)
_cell_length_c                   13.3197(9)
_cell_angle_alpha                102.352(2)
_cell_angle_beta                 102.260(2)
_cell_angle_gamma                90.173(2)
_cell_volume                     554.04(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15245
_cell_measurement_theta_min      2.856
_cell_measurement_theta_max      26.472


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.668
_exptl_crystal_F_000             426
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    8.074
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_process_details   
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_reflns_number            15245
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.856
_diffrn_reflns_theta_max         26.472
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4511
_reflns_number_gt                4344
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_max     0.974
_reflns_Friedel_fraction_full    0.986

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+6.1993P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2099 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(6)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         4511
_refine_ls_number_parameters     344
_refine_ls_number_restraints     123
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0678
_refine_ls_wR_factor_gt          0.0671
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.97528(5) 0.18011(5) 0.32335(4) 0.00375(17) Uani 1 1 d . . . . .
Tm2 Tm 1.02461(6) 0.81848(5) 0.67533(4) 0.00400(18) Uani 1 1 d . . . . .
C1A C 0.776(2) 0.0662(19) 0.1095(11) 0.004(3) Uani 1 1 d . U . . .
C2A C 0.619(2) -0.0304(18) 0.0049(10) 0.006(2) Uani 1 1 d . U . . .
H2A H 0.633596 0.039160 -0.048791 0.007 Uiso 1 1 calc R U . . .
C3A C 0.369(2) -0.0289(19) 0.0166(10) 0.007(2) Uani 1 1 d . U . . .
H3A H 0.331998 0.101121 0.041398 0.009 Uiso 1 1 calc R U . . .
C4A C 0.212(2) -0.108(2) -0.0923(12) 0.011(3) Uani 1 1 d . U . . .
C1B C 0.840(2) 0.6077(16) 0.4342(10) 0.006(2) Uani 1 1 d . . . . .
C2B C 0.651(2) 0.750(2) 0.4363(10) 0.006(3) Uani 1 1 d . U . . .
H2B H 0.507550 0.686560 0.438493 0.007 Uiso 1 1 calc R U . . .
C3B C 0.6174(19) 0.8188(16) 0.3333(9) 0.004(2) Uani 1 1 d . U . . .
H3B H 0.533250 0.720299 0.275469 0.005 Uiso 1 1 calc R U . . .
C4B C 0.4846(19) 0.9982(16) 0.3372(9) 0.004(2) Uani 1 1 d . U . . .
C1C C 1.154(2) 0.1711(15) 0.5685(9) 0.004(2) Uani 1 1 d . U . . .
C2C C 1.340(2) 0.306(2) 0.5663(11) 0.006(3) Uani 1 1 d . U . . .
H2C H 1.479741 0.236091 0.564587 0.007 Uiso 1 1 calc R U . . .
C3C C 1.3860(19) 0.4578(16) 0.6705(9) 0.004(2) Uani 1 1 d . U . . .
H3C H 1.475229 0.403271 0.726610 0.005 Uiso 1 1 calc R U . . .
C4C C 1.518(2) 0.6313(17) 0.6655(9) 0.007(2) Uani 1 1 d . . . . .
O11A O 0.7274(15) 0.2231(13) 0.1565(7) 0.0120(18) Uani 1 1 d . . . . .
O12A O 0.9478(15) -0.0144(12) 0.1481(7) 0.0107(18) Uani 1 1 d . U . . .
O21A O 0.6723(15) -0.2203(12) -0.0301(7) 0.0112(18) Uani 1 1 d . . . . .
O31A O 0.3481(16) -0.1314(13) 0.0936(7) 0.0126(18) Uani 1 1 d . . . . .
O41A O 0.2396(16) -0.0271(13) -0.1646(7) 0.0118(19) Uani 1 1 d . U . . .
O42A O 0.0680(16) -0.2407(13) -0.1059(8) 0.017(2) Uani 1 1 d . . . . .
O12B O 0.8185(15) 0.4710(12) 0.3588(7) 0.0076(17) Uani 1 1 d . U . . .
O11B O 1.0174(15) 0.6475(13) 0.5091(7) 0.0117(18) Uani 1 1 d . . . . .
O21B O 0.7177(14) 0.8944(11) 0.5289(7) 0.0069(17) Uani 1 1 d . . . . .
O31B O 0.8339(14) 0.8590(12) 0.3119(7) 0.0054(17) Uani 1 1 d . U . . .
O41B O 0.5922(16) 1.1433(14) 0.3343(7) 0.0091(19) Uani 1 1 d . U . . .
O42B O 0.2796(14) 0.9878(12) 0.3449(7) 0.0072(17) Uani 1 1 d . U . . .
O11C O 0.9782(15) 0.1487(11) 0.4919(7) 0.0073(17) Uani 1 1 d . . . . .
O12C O 1.1745(15) 0.0858(12) 0.6428(7) 0.0065(17) Uani 1 1 d . U . . .
O21C O 1.2876(14) 0.3789(11) 0.4734(7) 0.0062(16) Uani 1 1 d . U . . .
O31C O 1.1716(14) 0.5140(12) 0.6984(7) 0.0065(16) Uani 1 1 d . U . . .
O41C O 1.4104(16) 0.7779(14) 0.6644(7) 0.0103(19) Uani 1 1 d . U . . .
O42C O 1.7254(15) 0.6161(12) 0.6627(8) 0.0089(17) Uani 1 1 d . . . . .
O1W O 1.2376(15) 0.3423(13) 0.2613(8) 0.0124(19) Uani 1 1 d . . . . .
O2W O 0.7754(15) 1.0236(12) 0.7455(8) 0.0132(19) Uani 1 1 d . . . . .
O3W O 0.808(2) 0.5849(14) 0.1344(8) 0.014(2) Uani 1 1 d . . . . .
O4W O 1.302(2) 0.3641(14) 0.8743(8) 0.018(2) Uani 1 1 d . . . . .
O5W O 0.7818(19) 1.3548(16) 0.8858(9) 0.029(3) Uani 1 1 d . . . . .
O6W O 1.2264(16) 0.4921(14) 0.0789(8) 0.017(2) Uani 1 1 d . . . . .
H21A H 0.802225 -0.235770 -0.046433 0.025 Uiso 1 1 d . U . . .
H31A H 0.222204 -0.109756 0.114691 0.025 Uiso 1 1 d . U . . .
H21B H 0.799831 0.968825 0.509017 0.025 Uiso 1 1 d . U . . .
H31B H 0.856021 0.787764 0.253263 0.025 Uiso 1 1 d . U . . .
H21C H 1.188684 0.460892 0.481899 0.025 Uiso 1 1 d . U . . .
H31C H 1.160249 0.476555 0.753055 0.025 Uiso 1 1 d . U . . .
H11W H 1.271677 0.416375 0.225080 0.025 Uiso 1 1 d . U . . .
H12W H 1.365585 0.297710 0.284486 0.025 Uiso 1 1 d . U . . .
H21W H 0.763488 1.103312 0.800736 0.025 Uiso 1 1 d . U . . .
H22W H 0.641654 0.967812 0.723155 0.025 Uiso 1 1 d . U . . .
H31W H 0.743820 0.614784 0.075380 0.025 Uiso 1 1 d . U . . .
H32W H 0.749367 0.474026 0.129837 0.025 Uiso 1 1 d . U . . .
H41W H 1.288922 0.246366 0.869205 0.025 Uiso 1 1 d . U . . .
H42W H 1.293559 0.411264 0.937840 0.025 Uiso 1 1 d . U . . .
H51W H 0.645865 1.365508 0.899428 0.025 Uiso 1 1 d . U . . .
H52W H 0.874256 1.400532 0.945486 0.025 Uiso 1 1 d . U . . .
H61W H 1.293565 0.599074 0.084100 0.025 Uiso 1 1 d . U . . .
H62W H 1.112016 0.541579 0.102604 0.025 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O11C 2.302(8) . ?
Tm1 O42B 2.307(9) 1_645 ?
Tm1 O12B 2.322(9) . ?
Tm1 O41B 2.340(9) 1_545 ?
Tm1 O1W 2.345(9) . ?
Tm1 O12A 2.432(9) . ?
Tm1 O31B 2.455(8) 1_545 ?
Tm1 O11A 2.476(9) . ?
Tm1 O21C 2.596(8) . ?
Tm1 C1A 2.786(13) . ?
Tm2 O42C 2.271(9) 1_455 ?
Tm2 O11B 2.290(9) . ?
Tm2 O41A 2.294(9) 1_666 ?
Tm2 O12C 2.307(9) 1_565 ?
Tm2 O2W 2.311(9) . ?
Tm2 O41C 2.353(9) . ?
Tm2 O31C 2.451(8) . ?
Tm2 O21B 2.534(9) . ?
Tm2 C4A 2.989(15) 1_666 ?
C1A O12A 1.252(16) . ?
C1A O11A 1.252(16) . ?
C1A C2A 1.531(17) . ?
C2A O21A 1.427(15) . ?
C2A C3A 1.528(15) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.418(16) . ?
C3A C4A 1.543(19) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.252(18) . ?
C4A O41A 1.271(18) . ?
C1B O12B 1.241(15) . ?
C1B O11B 1.276(15) . ?
C1B C2B 1.537(18) . ?
C2B O21B 1.424(16) . ?
C2B C3B 1.534(17) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.424(14) . ?
C3B C4B 1.532(15) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.250(15) . ?
C4B O42B 1.253(14) . ?
C1C O12C 1.264(14) . ?
C1C O11C 1.282(14) . ?
C1C C2C 1.488(17) . ?
C2C O21C 1.427(16) . ?
C2C C3C 1.555(17) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.443(14) . ?
C3C C4C 1.510(15) . ?
C3C H3C 0.9800 . ?
C4C O41C 1.251(16) . ?
C4C O42C 1.253(15) . ?
O21A H21A 0.8500 . ?
O31A H31A 0.8601 . ?
O21B H21B 0.8495 . ?
O31B H31B 0.8769 . ?
O21C H21C 0.8501 . ?
O31C H31C 0.8465 . ?
O1W H11W 0.8485 . ?
O1W H12W 0.8541 . ?
O2W H21W 0.8511 . ?
O2W H22W 0.8586 . ?
O3W H31W 0.8703 . ?
O3W H32W 0.8663 . ?
O4W H41W 0.8506 . ?
O4W H42W 0.8552 . ?
O5W H51W 0.8688 . ?
O5W H52W 0.8646 . ?
O6W H61W 0.8602 . ?
O6W H62W 0.8608 . ?

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
O11C Tm1 O42B 81.1(3) . 1_645 ?
O11C Tm1 O12B 90.0(3) . . ?
O42B Tm1 O12B 151.0(3) 1_645 . ?
O11C Tm1 O41B 73.0(3) . 1_545 ?
O42B Tm1 O41B 131.8(3) 1_645 1_545 ?
O12B Tm1 O41B 69.9(3) . 1_545 ?
O11C Tm1 O1W 129.8(3) . . ?
O42B Tm1 O1W 81.1(3) 1_645 . ?
O12B Tm1 O1W 83.7(3) . . ?
O41B Tm1 O1W 145.9(3) 1_545 . ?
O11C Tm1 O12A 139.6(3) . . ?
O42B Tm1 O12A 76.2(3) 1_645 . ?
O12B Tm1 O12A 124.8(3) . . ?
O41B Tm1 O12A 98.2(3) 1_545 . ?
O1W Tm1 O12A 79.1(3) . . ?
O11C Tm1 O31B 72.4(3) . 1_545 ?
O42B Tm1 O31B 69.9(3) 1_645 1_545 ?
O12B Tm1 O31B 133.4(3) . 1_545 ?
O41B Tm1 O31B 63.8(3) 1_545 1_545 ?
O1W Tm1 O31B 140.4(3) . 1_545 ?
O12A Tm1 O31B 68.5(3) . 1_545 ?
O11C Tm1 O11A 144.4(3) . . ?
O42B Tm1 O11A 128.0(3) 1_645 . ?
O12B Tm1 O11A 72.8(3) . . ?
O41B Tm1 O11A 71.9(3) 1_545 . ?
O1W Tm1 O11A 80.1(3) . . ?
O12A Tm1 O11A 52.7(3) . . ?
O31B Tm1 O11A 96.7(3) 1_545 . ?
O11C Tm1 O21C 63.2(3) . . ?
O42B Tm1 O21C 75.1(3) 1_645 . ?
O12B Tm1 O21C 76.2(3) . . ?
O41B Tm1 O21C 123.6(3) 1_545 . ?
O1W Tm1 O21C 66.9(3) . . ?
O12A Tm1 O21C 138.1(3) . . ?
O31B Tm1 O21C 126.6(3) 1_545 . ?
O11A Tm1 O21C 136.6(3) . . ?
O11C Tm1 C1A 147.2(4) . . ?
O42B Tm1 C1A 102.9(3) 1_645 . ?
O12B Tm1 C1A 99.5(3) . . ?
O41B Tm1 C1A 80.9(4) 1_545 . ?
O1W Tm1 C1A 82.7(4) . . ?
O12A Tm1 C1A 26.7(3) . . ?
O31B Tm1 C1A 78.4(4) 1_545 . ?
O11A Tm1 C1A 26.7(3) . . ?
O21C Tm1 C1A 149.5(3) . . ?
O42C Tm2 O11B 82.2(3) 1_455 . ?
O42C Tm2 O41A 121.7(3) 1_455 1_666 ?
O11B Tm2 O41A 148.0(3) . 1_666 ?
O42C Tm2 O12C 151.4(3) 1_455 1_565 ?
O11B Tm2 O12C 93.2(3) . 1_565 ?
O41A Tm2 O12C 75.3(3) 1_666 1_565 ?
O42C Tm2 O2W 79.8(3) 1_455 . ?
O11B Tm2 O2W 133.1(3) . . ?
O41A Tm2 O2W 76.0(3) 1_666 . ?
O12C Tm2 O2W 83.2(3) 1_565 . ?
O42C Tm2 O41C 133.3(3) 1_455 . ?
O11B Tm2 O41C 73.8(3) . . ?
O41A Tm2 O41C 74.2(3) 1_666 . ?
O12C Tm2 O41C 70.6(3) 1_565 . ?
O2W Tm2 O41C 144.3(3) . . ?
O42C Tm2 O31C 70.8(3) 1_455 . ?
O11B Tm2 O31C 74.4(3) . . ?
O41A Tm2 O31C 92.7(3) 1_666 . ?
O12C Tm2 O31C 135.2(3) 1_565 . ?
O2W Tm2 O31C 136.4(3) . . ?
O41C Tm2 O31C 64.6(3) . . ?
O42C Tm2 O21B 76.2(3) 1_455 . ?
O11B Tm2 O21B 63.8(3) . . ?
O41A Tm2 O21B 137.7(3) 1_666 . ?
O12C Tm2 O21B 76.5(3) 1_565 . ?
O2W Tm2 O21B 70.0(3) . . ?
O41C Tm2 O21B 123.7(3) . . ?
O31C Tm2 O21B 129.3(3) . . ?
O42C Tm2 C4A 99.3(4) 1_455 1_666 ?
O11B Tm2 C4A 150.1(4) . 1_666 ?
O41A Tm2 C4A 23.4(4) 1_666 1_666 ?
O12C Tm2 C4A 98.5(4) 1_565 1_666 ?
O2W Tm2 C4A 75.8(4) . 1_666 ?
O41C Tm2 C4A 84.4(4) . 1_666 ?
O31C Tm2 C4A 78.0(4) . 1_666 ?
O21B Tm2 C4A 145.8(3) . 1_666 ?
O12A C1A O11A 121.0(12) . . ?
O12A C1A C2A 119.9(11) . . ?
O11A C1A C2A 119.1(11) . . ?
O12A C1A Tm1 60.7(7) . . ?
O11A C1A Tm1 62.7(7) . . ?
C2A C1A Tm1 162.6(10) . . ?
O21A C2A C3A 108.2(11) . . ?
O21A C2A C1A 112.7(10) . . ?
C3A C2A C1A 109.7(10) . . ?
O21A C2A H2A 108.7 . . ?
C3A C2A H2A 108.7 . . ?
C1A C2A H2A 108.7 . . ?
O31A C3A C2A 108.5(11) . . ?
O31A C3A C4A 113.7(11) . . ?
C2A C3A C4A 108.8(10) . . ?
O31A C3A H3A 108.6 . . ?
C2A C3A H3A 108.6 . . ?
C4A C3A H3A 108.6 . . ?
O42A C4A O41A 123.8(13) . . ?
O42A C4A C3A 121.2(14) . . ?
O41A C4A C3A 114.9(13) . . ?
O42A C4A Tm2 78.2(8) . 1_444 ?
O41A C4A Tm2 45.9(6) . 1_444 ?
C3A C4A Tm2 160.1(10) . 1_444 ?
O12B C1B O11B 124.4(11) . . ?
O12B C1B C2B 119.4(11) . . ?
O11B C1B C2B 116.0(11) . . ?
O21B C2B C3B 114.2(11) . . ?
O21B C2B C1B 108.5(10) . . ?
C3B C2B C1B 106.9(10) . . ?
O21B C2B H2B 109.0 . . ?
C3B C2B H2B 109.0 . . ?
C1B C2B H2B 109.0 . . ?
O31B C3B C4B 107.1(9) . . ?
O31B C3B C2B 110.4(9) . . ?
C4B C3B C2B 112.5(10) . . ?
O31B C3B H3B 108.9 . . ?
C4B C3B H3B 108.9 . . ?
C2B C3B H3B 108.9 . . ?
O41B C4B O42B 125.7(11) . . ?
O41B C4B C3B 116.9(10) . . ?
O42B C4B C3B 117.4(10) . . ?
O12C C1C O11C 123.4(10) . . ?
O12C C1C C2C 120.3(11) . . ?
O11C C1C C2C 116.3(10) . . ?
O21C C2C C1C 111.2(10) . . ?
O21C C2C C3C 114.1(11) . . ?
C1C C2C C3C 108.8(10) . . ?
O21C C2C H2C 107.5 . . ?
C1C C2C H2C 107.5 . . ?
C3C C2C H2C 107.5 . . ?
O31C C3C C4C 108.2(9) . . ?
O31C C3C C2C 110.0(9) . . ?
C4C C3C C2C 113.7(10) . . ?
O31C C3C H3C 108.3 . . ?
C4C C3C H3C 108.3 . . ?
C2C C3C H3C 108.3 . . ?
O41C C4C O42C 125.4(11) . . ?
O41C C4C C3C 117.4(11) . . ?
O42C C4C C3C 117.1(11) . . ?
C1A O11A Tm1 90.6(8) . . ?
C1A O12A Tm1 92.6(7) . . ?
C2A O21A H21A 115.7 . . ?
C3A O31A H31A 111.4 . . ?
C4A O41A Tm2 110.6(8) . 1_444 ?
C1B O12B Tm1 137.2(8) . . ?
C1B O11B Tm2 125.6(8) . . ?
C2B O21B Tm2 116.5(7) . . ?
C2B O21B H21B 102.0 . . ?
Tm2 O21B H21B 97.5 . . ?
C3B O31B Tm1 122.3(7) . 1_565 ?
C3B O31B H31B 112.7 . . ?
Tm1 O31B H31B 108.6 1_565 . ?
C4B O41B Tm1 128.6(8) . 1_565 ?
C4B O42B Tm1 134.3(8) . 1_465 ?
C1C O11C Tm1 126.1(8) . . ?
C1C O12C Tm2 138.6(8) . 1_545 ?
C2C O21C Tm1 113.9(7) . . ?
C2C O21C H21C 107.5 . . ?
Tm1 O21C H21C 87.7 . . ?
C3C O31C Tm2 120.0(7) . . ?
C3C O31C H31C 109.3 . . ?
Tm2 O31C H31C 119.1 . . ?
C4C O41C Tm2 127.1(8) . . ?
C4C O42C Tm2 135.4(8) . 1_655 ?
Tm1 O1W H11W 152.8 . . ?
Tm1 O1W H12W 102.9 . . ?
H11W O1W H12W 104.0 . . ?
Tm2 O2W H21W 142.7 . . ?
Tm2 O2W H22W 105.8 . . ?
H21W O2W H22W 104.1 . . ?
H31W O3W H32W 104.9 . . ?
H41W O4W H42W 104.0 . . ?
H51W O5W H52W 104.4 . . ?
H61W O6W H62W 93.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.85 1.91 2.751(13) 167.5 1_655 yes
O31A H31A O12A 0.86 1.88 2.729(13) 167.1 1_455 yes
O21B H21B O11C 0.85 1.77 2.610(12) 169.3 1_565 yes
O31B H31B O3W 0.88 1.89 2.729(14) 158.3 . yes
O21C H21C O11B 0.85 1.73 2.574(12) 172.4 . yes
O31C H31C O4W 0.85 2.00 2.763(14) 149.7 . yes
O1W H11W O6W 0.85 2.10 2.859(14) 148.7 . yes
O1W H12W O41B 0.85 1.87 2.700(13) 164.0 1_645 yes
O2W H21W O5W 0.85 1.93 2.718(14) 153.1 . yes
O2W H22W O41C 0.86 1.87 2.700(13) 160.8 1_455 yes
O3W H31W O21A 0.87 2.02 2.841(14) 156.7 1_565 yes
O3W H32W O11A 0.87 1.95 2.775(13) 158.4 . yes
O4W H41W O41A 0.85 1.96 2.804(14) 171.6 1_656 yes
O4W H42W O6W 0.86 1.97 2.818(15) 170.3 1_556 yes
O5W H51W O4W 0.87 2.01 2.835(17) 159.3 1_465 yes
O5W H52W O6W 0.86 2.43 3.263(14) 161.0 1_566 yes
O6W H61W O31A 0.86 1.97 2.800(13) 162.0 1_665 yes
O6W H62W O3W 0.86 1.96 2.798(15) 163.6 . yes

_refine_diff_density_max         1.560
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.205




# start Validation Reply Form
_vrf_PLAT987_Compound_Tm-D       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Single crystals of this compound are twinned as well as the rest of
isostructural compounds based on other lanthanide atoms. Therefore, the structure
has been refined with same twin law, indicated in the article. Despite this alert,
Flack parameter is low and close to zero, which indicates a pure enantiomer, so twin
refinement has not been conducted.
;
# end Validation Reply Form



_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Compound_Er-D
_database_code_depnum_ccdc_archive 'CCDC 1981581'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
"Poly{[bis(mu4-D-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')(mu-D-tartrate-k2O,O':k2O'',O''')diaquadierbium(III)] trihydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Er2 O20, 3(H2 O)'
_chemical_formula_sum            'C12 H22 Er2 O23'
_chemical_formula_weight         868.81

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

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9614(5)
_cell_length_b                   7.3515(6)
_cell_length_c                   13.1229(11)
_cell_angle_alpha                102.483(3)
_cell_angle_beta                 101.551(3)
_cell_angle_gamma                90.767(3)
_cell_volume                     549.18(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6474
_cell_measurement_theta_min      2.843
_cell_measurement_theta_max      24.739


_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.627
_exptl_crystal_F_000             414
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    7.702
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_process_details   
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_reflns_number            6474
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.843
_diffrn_reflns_theta_max         24.739
_diffrn_reflns_theta_full        24.739
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_point_group_measured_fraction_full 0.867
_reflns_number_total             3239
_reflns_number_gt                3151
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_max     0.743
_reflns_Friedel_fraction_full    0.743

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0076P)²+2.2405P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1310 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(9)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         3239
_refine_ls_number_parameters     335
_refine_ls_number_restraints     123
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0588
_refine_ls_wR_factor_gt          0.0582
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.076
_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
Er1 Er 0.97835(5) 0.18241(5) 0.32105(4) 0.00329(19) Uani 1 1 d . . . . .
Er2 Er 1.02011(5) 0.81590(5) 0.67914(4) 0.0041(2) Uani 1 1 d . . . . .
C1A C 0.784(3) 0.064(2) 0.1051(12) 0.006(4) Uani 1 1 d . U . . .
C2A C 0.629(2) -0.032(2) -0.0016(10) 0.007(3) Uani 1 1 d . U . . .
H2A H 0.645098 0.038141 -0.055672 0.008 Uiso 1 1 calc R U . . .
C3A C 0.380(2) -0.030(2) 0.0126(10) 0.009(3) Uani 1 1 d . U . . .
H3A H 0.349787 0.098691 0.042673 0.010 Uiso 1 1 calc R U . . .
C4A C 0.220(3) -0.093(2) -0.0958(13) 0.009(4) Uani 1 1 d . U . . .
C1B C 0.8415(19) 0.6111(18) 0.4309(9) 0.007(2) Uani 1 1 d . U . . .
C2B C 0.654(2) 0.750(2) 0.4341(10) 0.003(3) Uani 1 1 d . U . . .
H2B H 0.512074 0.683217 0.435957 0.004 Uiso 1 1 calc R U . . .
C3B C 0.6151(18) 0.8207(17) 0.3311(9) 0.005(2) Uani 1 1 d . U . . .
H3B H 0.529354 0.722993 0.272646 0.006 Uiso 1 1 calc R U . . .
C4B C 0.4876(19) 0.9984(17) 0.3363(9) 0.005(2) Uani 1 1 d . . . . .
C1C C 1.1502(18) 0.1659(16) 0.5668(8) 0.001(2) Uani 1 1 d . U . . .
C2C C 1.338(2) 0.307(2) 0.5650(10) 0.004(3) Uani 1 1 d . U . . .
H2C H 1.480908 0.243020 0.563249 0.005 Uiso 1 1 calc R U . . .
C3C C 1.3700(19) 0.4555(17) 0.6713(9) 0.006(2) Uani 1 1 d . U . . .
H3C H 1.449367 0.400643 0.729348 0.007 Uiso 1 1 calc R U . . .
C4C C 1.5080(18) 0.6268(17) 0.6695(8) 0.004(2) Uani 1 1 d . U . . .
O11A O 0.7424(14) 0.2223(12) 0.1510(6) 0.0094(18) Uani 1 1 d . . . . .
O12A O 0.9573(14) -0.0174(12) 0.1433(6) 0.0087(18) Uani 1 1 d . . . . .
O21A O 0.6769(13) -0.2205(12) -0.0379(7) 0.0108(19) Uani 1 1 d . . . . .
O31A O 0.3539(14) -0.1367(13) 0.0857(7) 0.0117(19) Uani 1 1 d . . . . .
O41A O 0.2481(14) 0.0058(14) -0.1636(7) 0.013(2) Uani 1 1 d . . . . .
O42A O 0.0776(14) -0.2225(13) -0.1201(7) 0.014(2) Uani 1 1 d . . . . .
O11B O 1.0179(14) 0.6520(12) 0.5073(6) 0.0083(18) Uani 1 1 d . . . . .
O12B O 0.8185(14) 0.4751(12) 0.3561(7) 0.0072(18) Uani 1 1 d . . . . .
O21B O 0.7142(13) 0.8934(12) 0.5304(6) 0.0065(17) Uani 1 1 d . U . . .
O31B O 0.8358(12) 0.8605(12) 0.3078(6) 0.0043(17) Uani 1 1 d . U . . .
O41B O 0.5911(14) 1.1437(14) 0.3306(7) 0.0075(18) Uani 1 1 d . U . . .
O42B O 0.2790(13) 0.9889(12) 0.3445(6) 0.0080(18) Uani 1 1 d . . . . .
O11C O 0.9718(13) 0.1466(12) 0.4911(6) 0.0076(18) Uani 1 1 d . . . . .
O12C O 1.1745(13) 0.0824(13) 0.6402(7) 0.0064(17) Uani 1 1 d . U . . .
O21C O 1.2803(13) 0.3796(12) 0.4728(6) 0.0052(17) Uani 1 1 d . . . . .
O31C O 1.1516(14) 0.5103(13) 0.6922(7) 0.0071(19) Uani 1 1 d . U . . .
O41C O 1.4060(15) 0.7749(14) 0.6717(7) 0.011(2) Uani 1 1 d . U . . .
O42C O 1.7168(13) 0.6103(12) 0.6661(7) 0.0083(17) Uani 1 1 d . U . . .
O1W O 1.2444(13) 0.3457(12) 0.2577(6) 0.0085(17) Uani 1 1 d . U . . .
O2W O 0.7686(13) 1.0256(12) 0.7533(6) 0.0090(18) Uani 1 1 d . . . . .
O3W O 0.7855(16) 0.5868(14) 0.1256(7) 0.0148(19) Uani 1 1 d . U . . .
O4W O 1.061(2) 0.3485(17) 0.8403(9) 0.036(3) Uani 1 1 d . . . . .
O5W O 1.2049(15) 0.4904(14) 0.0687(8) 0.018(2) Uani 1 1 d . . . . .
H21A H 0.789035 -0.217086 -0.068663 0.027 Uiso 1 1 d . U . . .
H31A H 0.228287 -0.115421 0.106847 0.027 Uiso 1 1 d . U . . .
H21B H 0.786315 0.987023 0.520384 0.027 Uiso 1 1 d . U . . .
H31B H 0.857289 0.781030 0.251663 0.027 Uiso 1 1 d . U . . .
H21C H 1.212582 0.480092 0.484941 0.027 Uiso 1 1 d . U . . .
H31C H 1.110981 0.466869 0.741207 0.027 Uiso 1 1 d . U . . .
H11W H 1.282286 0.361814 0.198589 0.027 Uiso 1 1 d . U . . .
H12W H 1.370351 0.295808 0.276791 0.027 Uiso 1 1 d . U . . .
H21W H 0.802009 1.134131 0.792871 0.027 Uiso 1 1 d . U . . .
H22W H 0.643609 0.962477 0.721203 0.027 Uiso 1 1 d . U . . .
H31W H 0.726096 0.647674 0.079216 0.027 Uiso 1 1 d . U . . .
H32W H 0.745934 0.477554 0.129775 0.027 Uiso 1 1 d . U . . .
H41W H 1.144266 0.253451 0.836213 0.027 Uiso 1 1 d . U . . .
H42W H 1.111422 0.408686 0.904846 0.027 Uiso 1 1 d . U . . .
H51W H 1.274307 0.597471 0.081575 0.027 Uiso 1 1 d . U . . .
H52W H 1.086184 0.511774 0.095532 0.027 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O11C 2.310(8) . ?
Er1 O42B 2.317(8) 1_645 ?
Er1 O41B 2.353(8) 1_545 ?
Er1 O1W 2.357(8) . ?
Er1 O12B 2.356(8) . ?
Er1 O12A 2.451(8) . ?
Er1 O31B 2.462(9) 1_545 ?
Er1 O11A 2.466(7) . ?
Er1 O21C 2.560(8) . ?
Er1 C1A 2.780(15) . ?
Er2 O42C 2.297(9) 1_455 ?
Er2 O11B 2.314(8) . ?
Er2 O41C 2.343(9) . ?
Er2 O12C 2.349(9) 1_565 ?
Er2 O2W 2.360(8) . ?
Er2 O41A 2.374(9) 1_666 ?
Er2 O31C 2.419(9) . ?
Er2 O21B 2.558(8) . ?
Er2 O42A 2.665(9) 1_666 ?
Er2 C4A 2.882(16) 1_666 ?
C1A O11A 1.244(18) . ?
C1A O12A 1.272(17) . ?
C1A C2A 1.531(19) . ?
C2A O21A 1.419(16) . ?
C2A C3A 1.529(13) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.393(17) . ?
C3A C4A 1.52(2) . ?
C3A H3A 0.9800 . ?
C4A O42A 1.21(2) . ?
C4A O41A 1.30(2) . ?
C1B O12B 1.225(15) . ?
C1B O11B 1.280(14) . ?
C1B C2B 1.525(17) . ?
C2B O21B 1.439(15) . ?
C2B C3B 1.527(17) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.449(14) . ?
C3B C4B 1.516(16) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.250(16) . ?
C4B O42B 1.272(14) . ?
C1C O12C 1.235(14) . ?
C1C O11C 1.285(13) . ?
C1C C2C 1.523(18) . ?
C2C O21C 1.409(16) . ?
C2C C3C 1.551(17) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.429(14) . ?
C3C C4C 1.502(17) . ?
C3C H3C 0.9800 . ?
C4C O41C 1.252(15) . ?
C4C O42C 1.261(14) . ?
O21A H21A 0.8503 . ?
O31A H31A 0.8539 . ?
O21B H21B 0.8544 . ?
O31B H31B 0.8688 . ?
O21C H21C 0.8469 . ?
O31C H31C 0.8501 . ?
O1W H11W 0.8808 . ?
O1W H12W 0.8562 . ?
O2W H21W 0.8494 . ?
O2W H22W 0.8533 . ?
O3W H31W 0.8559 . ?
O3W H32W 0.8497 . ?
O4W H41W 0.8606 . ?
O4W H42W 0.8573 . ?
O5W H51W 0.8519 . ?
O5W H52W 0.8531 . ?

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
O11C Er1 O42B 80.3(3) . 1_645 ?
O11C Er1 O41B 72.7(3) . 1_545 ?
O42B Er1 O41B 131.0(3) 1_645 1_545 ?
O11C Er1 O1W 130.9(3) . . ?
O42B Er1 O1W 82.2(3) 1_645 . ?
O41B Er1 O1W 145.5(3) 1_545 . ?
O11C Er1 O12B 90.9(3) . . ?
O42B Er1 O12B 151.7(3) 1_645 . ?
O41B Er1 O12B 69.8(3) 1_545 . ?
O1W Er1 O12B 83.6(3) . . ?
O11C Er1 O12A 137.9(3) . . ?
O42B Er1 O12A 75.7(3) 1_645 . ?
O41B Er1 O12A 98.1(3) 1_545 . ?
O1W Er1 O12A 79.3(3) . . ?
O12B Er1 O12A 125.2(3) . . ?
O11C Er1 O31B 71.8(3) . 1_545 ?
O42B Er1 O31B 68.9(3) 1_645 1_545 ?
O41B Er1 O31B 64.1(3) 1_545 1_545 ?
O1W Er1 O31B 140.0(3) . 1_545 ?
O12B Er1 O31B 133.7(3) . 1_545 ?
O12A Er1 O31B 67.4(3) . 1_545 ?
O11C Er1 O11A 144.9(3) . . ?
O42B Er1 O11A 127.5(3) 1_645 . ?
O41B Er1 O11A 72.5(3) 1_545 . ?
O1W Er1 O11A 79.1(3) . . ?
O12B Er1 O11A 73.0(3) . . ?
O12A Er1 O11A 52.9(3) . . ?
O31B Er1 O11A 96.7(3) 1_545 . ?
O11C Er1 O21C 63.7(3) . . ?
O42B Er1 O21C 75.7(3) 1_645 . ?
O41B Er1 O21C 123.3(3) 1_545 . ?
O1W Er1 O21C 67.7(3) . . ?
O12B Er1 O21C 76.3(3) . . ?
O12A Er1 O21C 138.6(3) . . ?
O31B Er1 O21C 126.6(3) 1_545 . ?
O11A Er1 O21C 136.7(3) . . ?
O11C Er1 C1A 145.6(4) . . ?
O42B Er1 C1A 102.9(4) 1_645 . ?
O41B Er1 C1A 80.2(4) 1_545 . ?
O1W Er1 C1A 83.1(4) . . ?
O12B Er1 C1A 99.5(4) . . ?
O12A Er1 C1A 27.2(4) . . ?
O31B Er1 C1A 77.4(4) 1_545 . ?
O11A Er1 C1A 26.6(4) . . ?
O21C Er1 C1A 150.7(4) . . ?
O42C Er2 O11B 83.5(3) 1_455 . ?
O42C Er2 O41C 132.7(3) 1_455 . ?
O11B Er2 O41C 74.4(3) . . ?
O42C Er2 O12C 151.0(3) 1_455 1_565 ?
O11B Er2 O12C 89.7(3) . 1_565 ?
O41C Er2 O12C 71.1(3) . 1_565 ?
O42C Er2 O2W 80.5(3) 1_455 . ?
O11B Er2 O2W 133.0(3) . . ?
O41C Er2 O2W 143.5(3) . . ?
O12C Er2 O2W 83.9(3) 1_565 . ?
O42C Er2 O41A 127.8(3) 1_455 1_666 ?
O11B Er2 O41A 144.9(3) . 1_666 ?
O41C Er2 O41A 72.1(3) . 1_666 ?
O12C Er2 O41A 69.9(3) 1_565 1_666 ?
O2W Er2 O41A 74.5(3) . 1_666 ?
O42C Er2 O31C 69.2(3) 1_455 . ?
O11B Er2 O31C 73.1(3) . . ?
O41C Er2 O31C 64.5(3) . . ?
O12C Er2 O31C 135.2(3) 1_565 . ?
O2W Er2 O31C 137.6(3) . . ?
O41A Er2 O31C 101.2(3) 1_666 . ?
O42C Er2 O21B 76.6(3) 1_455 . ?
O11B Er2 O21B 63.4(3) . . ?
O41C Er2 O21B 125.2(3) . . ?
O12C Er2 O21B 75.2(3) 1_565 . ?
O2W Er2 O21B 70.0(3) . . ?
O41A Er2 O21B 132.1(3) 1_666 . ?
O31C Er2 O21B 126.8(3) . . ?
O42C Er2 O42A 78.9(3) 1_455 1_666 ?
O11B Er2 O42A 142.5(3) . 1_666 ?
O41C Er2 O42A 93.8(3) . 1_666 ?
O12C Er2 O42A 120.6(3) 1_565 1_666 ?
O2W Er2 O42A 76.1(3) . 1_666 ?
O41A Er2 O42A 51.0(3) 1_666 1_666 ?
O31C Er2 O42A 69.7(3) . 1_666 ?
O21B Er2 O42A 140.8(2) . 1_666 ?
O42C Er2 C4A 103.4(4) 1_455 1_666 ?
O11B Er2 C4A 150.9(4) . 1_666 ?
O41C Er2 C4A 80.6(4) . 1_666 ?
O12C Er2 C4A 96.2(4) 1_565 1_666 ?
O2W Er2 C4A 76.0(4) . 1_666 ?
O41A Er2 C4A 26.4(4) 1_666 1_666 ?
O31C Er2 C4A 82.9(4) . 1_666 ?
O21B Er2 C4A 145.6(4) . 1_666 ?
O42A Er2 C4A 24.9(4) 1_666 1_666 ?
O11A C1A O12A 121.0(13) . . ?
O11A C1A C2A 119.5(13) . . ?
O12A C1A C2A 119.5(13) . . ?
O11A C1A Er1 62.5(7) . . ?
O12A C1A Er1 61.9(7) . . ?
C2A C1A Er1 163.7(11) . . ?
O21A C2A C3A 107.4(12) . . ?
O21A C2A C1A 113.4(11) . . ?
C3A C2A C1A 108.3(10) . . ?
O21A C2A H2A 109.2 . . ?
C3A C2A H2A 109.2 . . ?
C1A C2A H2A 109.2 . . ?
O31A C3A C4A 114.3(13) . . ?
O31A C3A C2A 109.5(12) . . ?
C4A C3A C2A 109.4(10) . . ?
O31A C3A H3A 107.8 . . ?
C4A C3A H3A 107.8 . . ?
C2A C3A H3A 107.8 . . ?
O42A C4A O41A 121.2(14) . . ?
O42A C4A C3A 125.0(15) . . ?
O41A C4A C3A 113.8(14) . . ?
O42A C4A Er2 67.5(8) . 1_444 ?
O41A C4A Er2 54.4(7) . 1_444 ?
C3A C4A Er2 164.9(11) . 1_444 ?
O12B C1B O11B 125.0(11) . . ?
O12B C1B C2B 119.3(10) . . ?
O11B C1B C2B 115.6(10) . . ?
O21B C2B C1B 109.4(9) . . ?
O21B C2B C3B 114.8(11) . . ?
C1B C2B C3B 108.5(9) . . ?
O21B C2B H2B 108.0 . . ?
C1B C2B H2B 108.0 . . ?
C3B C2B H2B 108.0 . . ?
O31B C3B C4B 107.0(10) . . ?
O31B C3B C2B 108.8(9) . . ?
C4B C3B C2B 114.1(9) . . ?
O31B C3B H3B 109.0 . . ?
C4B C3B H3B 109.0 . . ?
C2B C3B H3B 109.0 . . ?
O41B C4B O42B 124.0(10) . . ?
O41B C4B C3B 118.6(10) . . ?
O42B C4B C3B 117.4(11) . . ?
O12C C1C O11C 124.6(11) . . ?
O12C C1C C2C 119.4(10) . . ?
O11C C1C C2C 116.0(10) . . ?
O21C C2C C1C 110.1(10) . . ?
O21C C2C C3C 114.3(12) . . ?
C1C C2C C3C 106.6(10) . . ?
O21C C2C H2C 108.6 . . ?
C1C C2C H2C 108.6 . . ?
C3C C2C H2C 108.6 . . ?
O31C C3C C4C 108.4(9) . . ?
O31C C3C C2C 110.1(9) . . ?
C4C C3C C2C 112.2(10) . . ?
O31C C3C H3C 108.7 . . ?
C4C C3C H3C 108.7 . . ?
C2C C3C H3C 108.7 . . ?
O41C C4C O42C 125.3(12) . . ?
O41C C4C C3C 117.1(10) . . ?
O42C C4C C3C 117.6(10) . . ?
C1A O11A Er1 90.9(8) . . ?
C1A O12A Er1 90.9(8) . . ?
C2A O21A H21A 105.8 . . ?
C3A O31A H31A 110.8 . . ?
C4A O41A Er2 99.3(9) . 1_444 ?
C4A O42A Er2 87.6(9) . 1_444 ?
C1B O11B Er2 125.8(7) . . ?
C1B O12B Er1 136.7(8) . . ?
C2B O21B Er2 115.9(7) . . ?
C2B O21B H21B 111.3 . . ?
Er2 O21B H21B 98.0 . . ?
C3B O31B Er1 121.5(7) . 1_565 ?
C3B O31B H31B 110.6 . . ?
Er1 O31B H31B 114.3 1_565 . ?
C4B O41B Er1 127.4(7) . 1_565 ?
C4B O42B Er1 133.9(8) . 1_465 ?
C1C O11C Er1 124.1(7) . . ?
C1C O12C Er2 139.2(8) . 1_545 ?
C2C O21C Er1 115.2(8) . . ?
C2C O21C H21C 111.4 . . ?
Er1 O21C H21C 100.3 . . ?
C3C O31C Er2 121.4(7) . . ?
C3C O31C H31C 114.4 . . ?
Er2 O31C H31C 114.9 . . ?
C4C O41C Er2 127.0(9) . . ?
C4C O42C Er2 134.5(8) . 1_655 ?
Er1 O1W H11W 142.4 . . ?
Er1 O1W H12W 102.9 . . ?
H11W O1W H12W 92.3 . . ?
Er2 O2W H21W 127.7 . . ?
Er2 O2W H22W 97.3 . . ?
H21W O2W H22W 134.6 . . ?
H31W O3W H32W 128.0 . . ?
H41W O4W H42W 102.1 . . ?
H51W O5W H52W 103.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.85 1.97 2.810(12) 170.7 1_655 yes
O31A H31A O12A 0.85 1.88 2.723(11) 167.0 1_455 yes
O21B H21B O11C 0.85 1.75 2.598(12) 168.7 1_565 yes
O31B H31B O3W 0.87 1.91 2.734(12) 158.4 . yes
O21C H21C O11B 0.85 1.74 2.576(11) 166.6 . yes
O31C H31C O4W 0.85 1.78 2.624(15) 170.5 . yes
O1W H11W O5W 0.88 2.10 2.872(13) 146.1 . yes
O1W H12W O41B 0.86 1.87 2.702(12) 164.0 1_645 yes
O2W H21W O4W 0.85 2.09 2.811(16) 141.9 1_565 yes
O2W H22W O41C 0.85 1.88 2.707(13) 163.9 1_455 yes
O3W H31W O21A 0.86 1.96 2.795(13) 163.5 1_565 yes
O3W H32W O11A 0.85 1.96 2.785(13) 164.8 . yes
O4W H41W O41A 0.86 1.93 2.763(15) 162.2 1_656 yes
O4W H42W O5W 0.86 2.06 2.899(15) 165.2 1_556 yes
O5W H51W O31A 0.85 1.99 2.819(14) 163.6 1_665 yes
O5W H52W O3W 0.85 1.97 2.807(12) 165.7 . yes

_refine_diff_density_max         2.934
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.174


# start Validation Reply Form
_vrf_PLAT090_Compound_Er-D       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.52 Note  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. On the other hand, the structure
crystallizes in the P1 space group, which makes neccessary measuring the whole 
Ewald sphere. Despite the fact that data collection has been planned as such, 
the crystal promotes weak diffraction at relatively low angle (above 23 degrees
in 2theta), so acquired data is not enough as to get full Friedel coverage. 
In any case, the model is reliable owing to the fact that it consists of a 
isostructural counterpat of a big family of lanthanide-tartrate MOFs. 
;
_vrf_PLAT220_Compound_Er-D       
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        9.0 Ratio 
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. Despite the fact that specific absorption
correction based on the faces of the crystal has been performed, somewhat large
diffraction peaks close to the lanthanide atoms could not be removed. Nonetheless,
the unaccounted positive residual density around the lanthanide heavy atom is 
quite common for lanthanide-organic based crystal structures.
;
# end Validation Reply Form

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Compound_Ho-D
_database_code_depnum_ccdc_archive 'CCDC 1981579'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV EHU)
Spain
;
_audit_update_record             
;
2020-02-02 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        
;
Poly{[bis(mu4-D-tartrate-kO:k2O',O'':k2O''',O'''':kO''''')
(mu-D-tartrate-k2O,O':k2O'',O''')diaquadiholmium(III)] trihydrate}
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Ho2 O20, 3(H2 O)'
_chemical_formula_sum            'C12 H22 Ho2 O23'
_chemical_formula_weight         864.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   5.9693(2)
_cell_length_b                   7.3865(2)
_cell_length_c                   13.0842(5)
_cell_angle_alpha                102.540(3)
_cell_angle_beta                 101.363(3)
_cell_angle_gamma                90.912(2)
_cell_volume                     551.07(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6658
_cell_measurement_theta_min      7.0480
_cell_measurement_theta_max      74.3710

loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -1.0001 0.0002 -0.0002 0.0046 0.9612 -0.0776 -0.0011 -0.9846 -0.9608

loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6468 8253 639
2 0.3532 8179 639

_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.604
_exptl_crystal_F_000             412
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    14.061
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_reflns_number            8596
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.536
_diffrn_reflns_theta_max         74.424
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_point_group_measured_fraction_full 0.923
_reflns_number_total             3976
_reflns_number_gt                3921
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_max     0.827
_reflns_Friedel_fraction_full    0.883

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0902P)²+1.8552P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1793 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(10)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         3976
_refine_ls_number_parameters     334
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1243
_refine_ls_wR_factor_gt          0.1236
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.105
_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
Ho1 Ho 0.97991(8) 0.18299(7) 0.32023(5) 0.0083(2) Uani 1 1 d . . . . .
Ho2 Ho 1.01882(9) 0.81589(7) 0.67987(5) 0.0086(2) Uani 1 1 d . . . . .
C1A C 0.789(2) 0.0656(19) 0.1029(10) 0.012(3) Uani 1 1 d . . . . .
C2A C 0.631(2) -0.0336(17) -0.0026(9) 0.010(2) Uani 1 1 d . . . . .
H2A H 0.647431 0.034521 -0.057426 0.013 Uiso 1 1 calc R U . . .
C3A C 0.383(2) -0.0273(18) 0.0113(9) 0.011(2) Uani 1 1 d . . . . .
H3A H 0.356265 0.101403 0.043220 0.013 Uiso 1 1 calc R U . . .
C4A C 0.223(3) -0.0830(19) -0.0970(10) 0.012(3) Uani 1 1 d . U . . .
C1B C 0.840(2) 0.6121(15) 0.4301(8) 0.009(2) Uani 1 1 d . U . . .
C2B C 0.653(2) 0.7476(16) 0.4346(8) 0.007(2) Uani 1 1 d . U . . .
H2B H 0.511242 0.681329 0.436636 0.008 Uiso 1 1 calc R U . . .
C3B C 0.6175(19) 0.8222(15) 0.3309(8) 0.0084(19) Uani 1 1 d . . . . .
H3B H 0.532270 0.725392 0.271893 0.010 Uiso 1 1 calc R U . . .
C4B C 0.487(2) 1.0000(15) 0.3358(8) 0.010(2) Uani 1 1 d . . . . .
C1C C 1.1503(19) 0.1654(14) 0.5669(8) 0.0063(18) Uani 1 1 d . U . . .
C2C C 1.339(2) 0.3092(17) 0.5662(9) 0.011(2) Uani 1 1 d . . . . .
H2C H 1.482076 0.246818 0.564519 0.013 Uiso 1 1 calc R U . . .
C3C C 1.3682(19) 0.4549(14) 0.6724(8) 0.010(2) Uani 1 1 d . . . . .
H3C H 1.445069 0.400009 0.730808 0.012 Uiso 1 1 calc R U . . .
C4C C 1.509(2) 0.6276(15) 0.6712(8) 0.009(2) Uani 1 1 d . U . . .
O11A O 0.7459(14) 0.2204(12) 0.1496(6) 0.0136(16) Uani 1 1 d . . . . .
O12A O 0.9590(14) -0.0193(12) 0.1418(6) 0.0124(16) Uani 1 1 d . . . . .
O21A O 0.6775(14) -0.2208(11) -0.0399(6) 0.0127(16) Uani 1 1 d . . . . .
O31A O 0.3526(15) -0.1382(13) 0.0846(6) 0.0149(16) Uani 1 1 d . . . . .
O41A O 0.2493(15) 0.0097(13) -0.1641(6) 0.0151(17) Uani 1 1 d . . . . .
O42A O 0.0793(14) -0.2221(12) -0.1213(6) 0.0140(16) Uani 1 1 d . . . . .
O11B O 1.0161(15) 0.6514(12) 0.5071(7) 0.0125(16) Uani 1 1 d . . . . .
O12B O 0.8187(15) 0.4733(11) 0.3548(6) 0.0120(16) Uani 1 1 d . . . . .
O21B O 0.7138(14) 0.8941(11) 0.5293(6) 0.0105(15) Uani 1 1 d . . . . .
O31B O 0.8342(13) 0.8598(11) 0.3074(6) 0.0111(15) Uani 1 1 d . . . . .
O41B O 0.5935(15) 1.1427(12) 0.3303(6) 0.0125(16) Uani 1 1 d . . . . .
O42B O 0.2808(13) 0.9881(11) 0.3442(6) 0.0106(15) Uani 1 1 d . . . . .
O12C O 1.1732(14) 0.0790(12) 0.6402(7) 0.0126(16) Uani 1 1 d . . . . .
O11C O 0.9717(14) 0.1451(12) 0.4913(6) 0.0125(16) Uani 1 1 d . . . . .
O21C O 1.2805(14) 0.3797(11) 0.4736(6) 0.0092(15) Uani 1 1 d . . . . .
O31C O 1.1495(14) 0.5105(11) 0.6918(7) 0.0116(15) Uani 1 1 d . . . . .
O41C O 1.4044(15) 0.7740(12) 0.6736(7) 0.0140(17) Uani 1 1 d . . . . .
O42C O 1.7136(14) 0.6097(12) 0.6685(7) 0.0151(16) Uani 1 1 d . . . . .
O1W O 1.2492(15) 0.3452(12) 0.2561(6) 0.0163(17) Uani 1 1 d . U . . .
O2W O 0.7653(14) 1.0289(11) 0.7541(6) 0.0145(16) Uani 1 1 d . . . . .
O3W O 0.7913(17) 0.5854(12) 0.1243(7) 0.0173(17) Uani 1 1 d . . . . .
O4W O 1.060(2) 0.3480(14) 0.8409(7) 0.027(2) Uani 1 1 d . . . . .
O5W O 1.2049(17) 0.4918(13) 0.0675(7) 0.0231(19) Uani 1 1 d . . . . .
H21A H 0.787420 -0.232516 -0.074711 0.035 Uiso 1 1 d . U . . .
H31A H 0.242272 -0.085982 0.108167 0.035 Uiso 1 1 d . U . . .
H21B H 0.786874 0.978404 0.512100 0.035 Uiso 1 1 d . U . . .
H31B H 0.872648 0.767419 0.255903 0.035 Uiso 1 1 d . U . . .
H21C H 1.206883 0.477508 0.490144 0.035 Uiso 1 1 d . U . . .
H31C H 1.124459 0.469184 0.743972 0.035 Uiso 1 1 d . U . . .
H11W H 1.268275 0.377605 0.198688 0.035 Uiso 1 1 d . U . . .
H12W H 1.366874 0.292662 0.278042 0.035 Uiso 1 1 d . U . . .
H21W H 0.751319 1.121038 0.794450 0.035 Uiso 1 1 d . U . . .
H22W H 0.636473 0.971969 0.722506 0.035 Uiso 1 1 d . U . . .
H31W H 0.725221 0.615172 0.064874 0.035 Uiso 1 1 d . U . . .
H32W H 0.744876 0.472091 0.121328 0.035 Uiso 1 1 d . U . . .
H41W H 1.130987 0.247659 0.831806 0.035 Uiso 1 1 d . U . . .
H42W H 1.124238 0.403757 0.905980 0.035 Uiso 1 1 d . U . . .
H51W H 1.264143 0.597301 0.068321 0.035 Uiso 1 1 d . U . . .
H52W H 1.078189 0.512492 0.086592 0.035 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O11C 2.325(8) . ?
Ho1 O42B 2.335(8) 1_645 ?
Ho1 O41B 2.354(8) 1_545 ?
Ho1 O12B 2.355(8) . ?
Ho1 O1W 2.373(9) . ?
Ho1 O11A 2.462(8) . ?
Ho1 O12A 2.462(8) . ?
Ho1 O31B 2.487(8) 1_545 ?
Ho1 O21C 2.567(8) . ?
Ho1 C1A 2.785(12) . ?
Ho2 O42C 2.317(8) 1_455 ?
Ho2 O11B 2.320(8) . ?
Ho2 O12C 2.338(8) 1_565 ?
Ho2 O41C 2.342(9) . ?
Ho2 O41A 2.382(8) 1_666 ?
Ho2 O2W 2.387(8) . ?
Ho2 O31C 2.425(8) . ?
Ho2 O21B 2.578(8) . ?
Ho2 O42A 2.631(8) 1_666 ?
Ho2 C4A 2.862(13) 1_666 ?
C1A O11A 1.232(16) . ?
C1A O12A 1.279(17) . ?
C1A C2A 1.536(16) . ?
C2A O21A 1.414(14) . ?
C2A C3A 1.530(14) . ?
C2A H2A 0.9800 . ?
C3A O31A 1.424(14) . ?
C3A C4A 1.512(17) . ?
C3A H3A 0.9800 . ?
C4A O41A 1.256(16) . ?
C4A O42A 1.271(17) . ?
C1B O12B 1.243(14) . ?
C1B O11B 1.282(14) . ?
C1B C2B 1.514(16) . ?
C2B O21B 1.437(13) . ?
C2B C3B 1.551(14) . ?
C2B H2B 0.9800 . ?
C3B O31B 1.424(13) . ?
C3B C4B 1.534(15) . ?
C3B H3B 0.9800 . ?
C4B O41B 1.246(15) . ?
C4B O42B 1.259(15) . ?
C1C O12C 1.250(13) . ?
C1C O11C 1.285(13) . ?
C1C C2C 1.538(15) . ?
C2C O21C 1.404(13) . ?
C2C C3C 1.539(16) . ?
C2C H2C 0.9800 . ?
C3C O31C 1.428(14) . ?
C3C C4C 1.521(15) . ?
C3C H3C 0.9800 . ?
C4C O42C 1.237(15) . ?
C4C O41C 1.255(15) . ?
O21A H21A 0.8646 . ?
O31A H31A 0.8451 . ?
O21B H21B 0.8482 . ?
O31B H31B 0.9159 . ?
O21C H21C 0.8610 . ?
O31C H31C 0.8435 . ?
O1W H11W 0.8633 . ?
O1W H12W 0.8391 . ?
O2W H21W 0.7826 . ?
O2W H22W 0.8533 . ?
O3W H31W 0.8744 . ?
O3W H32W 0.8676 . ?
O4W H41W 0.8559 . ?
O4W H42W 0.8686 . ?
O5W H51W 0.8478 . ?
O5W H52W 0.8482 . ?

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
O11C Ho1 O42B 79.9(3) . 1_645 ?
O11C Ho1 O41B 72.4(3) . 1_545 ?
O42B Ho1 O41B 130.4(3) 1_645 1_545 ?
O11C Ho1 O12B 91.4(3) . . ?
O42B Ho1 O12B 152.2(3) 1_645 . ?
O41B Ho1 O12B 69.8(3) 1_545 . ?
O11C Ho1 O1W 131.2(3) . . ?
O42B Ho1 O1W 82.2(3) 1_645 . ?
O41B Ho1 O1W 146.1(3) 1_545 . ?
O12B Ho1 O1W 84.1(3) . . ?
O11C Ho1 O11A 145.0(3) . . ?
O42B Ho1 O11A 127.3(3) 1_645 . ?
O41B Ho1 O11A 72.8(3) 1_545 . ?
O12B Ho1 O11A 73.0(3) . . ?
O1W Ho1 O11A 79.3(3) . . ?
O11C Ho1 O12A 137.0(3) . . ?
O42B Ho1 O12A 75.5(3) 1_645 . ?
O41B Ho1 O12A 97.9(3) 1_545 . ?
O12B Ho1 O12A 125.4(3) . . ?
O1W Ho1 O12A 79.5(3) . . ?
O11A Ho1 O12A 52.9(3) . . ?
O11C Ho1 O31B 71.2(3) . 1_545 ?
O42B Ho1 O31B 68.9(3) 1_645 1_545 ?
O41B Ho1 O31B 63.6(3) 1_545 1_545 ?
O12B Ho1 O31B 133.2(3) . 1_545 ?
O1W Ho1 O31B 140.0(3) . 1_545 ?
O11A Ho1 O31B 96.5(3) . 1_545 ?
O12A Ho1 O31B 67.2(3) . 1_545 ?
O11C Ho1 O21C 63.6(3) . . ?
O42B Ho1 O21C 75.8(3) 1_645 . ?
O41B Ho1 O21C 123.0(3) 1_545 . ?
O12B Ho1 O21C 76.6(3) . . ?
O1W Ho1 O21C 68.1(3) . . ?
O11A Ho1 O21C 137.2(3) . . ?
O12A Ho1 O21C 139.0(3) . . ?
O31B Ho1 O21C 126.3(2) 1_545 . ?
O11C Ho1 C1A 145.7(3) . . ?
O42B Ho1 C1A 102.8(3) 1_645 . ?
O41B Ho1 C1A 80.8(3) 1_545 . ?
O12B Ho1 C1A 99.2(3) . . ?
O1W Ho1 C1A 82.6(3) . . ?
O11A Ho1 C1A 26.2(4) . . ?
O12A Ho1 C1A 27.3(4) . . ?
O31B Ho1 C1A 77.9(3) 1_545 . ?
O21C Ho1 C1A 150.6(3) . . ?
O42C Ho2 O11B 83.8(3) 1_455 . ?
O42C Ho2 O12C 151.3(3) 1_455 1_565 ?
O11B Ho2 O12C 89.6(3) . 1_565 ?
O42C Ho2 O41C 132.5(3) 1_455 . ?
O11B Ho2 O41C 74.8(3) . . ?
O12C Ho2 O41C 71.4(3) 1_565 . ?
O42C Ho2 O41A 128.3(3) 1_455 1_666 ?
O11B Ho2 O41A 144.4(3) . 1_666 ?
O12C Ho2 O41A 69.0(3) 1_565 1_666 ?
O41C Ho2 O41A 71.5(3) . 1_666 ?
O42C Ho2 O2W 80.6(3) 1_455 . ?
O11B Ho2 O2W 132.7(3) . . ?
O12C Ho2 O2W 83.6(3) 1_565 . ?
O41C Ho2 O2W 143.3(3) . . ?
O41A Ho2 O2W 74.7(3) 1_666 . ?
O42C Ho2 O31C 69.1(3) 1_455 . ?
O11B Ho2 O31C 72.7(3) . . ?
O12C Ho2 O31C 134.9(3) 1_565 . ?
O41C Ho2 O31C 64.1(3) . . ?
O41A Ho2 O31C 102.1(3) 1_666 . ?
O2W Ho2 O31C 138.5(3) . . ?
O42C Ho2 O21B 77.3(3) 1_455 . ?
O11B Ho2 O21B 63.2(3) . . ?
O12C Ho2 O21B 74.8(3) 1_565 . ?
O41C Ho2 O21B 125.4(3) . . ?
O41A Ho2 O21B 131.3(3) 1_666 . ?
O2W Ho2 O21B 69.8(3) . . ?
O31C Ho2 O21B 126.6(3) . . ?
O42C Ho2 O42A 78.8(3) 1_455 1_666 ?
O11B Ho2 O42A 142.2(3) . 1_666 ?
O12C Ho2 O42A 120.6(3) 1_565 1_666 ?
O41C Ho2 O42A 92.7(3) . 1_666 ?
O41A Ho2 O42A 51.9(3) 1_666 1_666 ?
O2W Ho2 O42A 77.1(3) . 1_666 ?
O31C Ho2 O42A 69.8(3) . 1_666 ?
O21B Ho2 O42A 141.8(3) . 1_666 ?
O42C Ho2 C4A 104.6(4) 1_455 1_666 ?
O11B Ho2 C4A 151.2(4) . 1_666 ?
O12C Ho2 C4A 94.6(3) 1_565 1_666 ?
O41C Ho2 C4A 79.5(4) . 1_666 ?
O41A Ho2 C4A 25.7(4) 1_666 1_666 ?
O2W Ho2 C4A 76.2(4) . 1_666 ?
O31C Ho2 C4A 84.4(3) . 1_666 ?
O21B Ho2 C4A 145.2(3) . 1_666 ?
O42A Ho2 C4A 26.3(3) 1_666 1_666 ?
O11A C1A O12A 121.7(11) . . ?
O11A C1A C2A 119.8(12) . . ?
O12A C1A C2A 118.4(11) . . ?
O11A C1A Ho1 62.1(6) . . ?
O12A C1A Ho1 62.1(6) . . ?
C2A C1A Ho1 161.6(9) . . ?
O21A C2A C3A 108.6(10) . . ?
O21A C2A C1A 114.5(10) . . ?
C3A C2A C1A 109.2(9) . . ?
O21A C2A H2A 108.1 . . ?
C3A C2A H2A 108.1 . . ?
C1A C2A H2A 108.1 . . ?
O31A C3A C4A 114.8(11) . . ?
O31A C3A C2A 108.5(11) . . ?
C4A C3A C2A 109.6(9) . . ?
O31A C3A H3A 107.9 . . ?
C4A C3A H3A 107.9 . . ?
C2A C3A H3A 107.9 . . ?
O41A C4A O42A 121.5(12) . . ?
O41A C4A C3A 116.1(12) . . ?
O42A C4A C3A 122.3(12) . . ?
O41A C4A Ho2 55.3(6) . 1_444 ?
O42A C4A Ho2 66.7(7) . 1_444 ?
C3A C4A Ho2 166.5(9) . 1_444 ?
O12B C1B O11B 124.1(11) . . ?
O12B C1B C2B 120.1(10) . . ?
O11B C1B C2B 115.8(9) . . ?
O21B C2B C1B 110.2(9) . . ?
O21B C2B C3B 112.2(9) . . ?
C1B C2B C3B 107.7(9) . . ?
O21B C2B H2B 108.9 . . ?
C1B C2B H2B 108.9 . . ?
C3B C2B H2B 108.9 . . ?
O31B C3B C4B 107.8(8) . . ?
O31B C3B C2B 109.4(9) . . ?
C4B C3B C2B 114.5(9) . . ?
O31B C3B H3B 108.3 . . ?
C4B C3B H3B 108.3 . . ?
C2B C3B H3B 108.3 . . ?
O41B C4B O42B 125.9(10) . . ?
O41B C4B C3B 117.1(10) . . ?
O42B C4B C3B 117.0(10) . . ?
O12C C1C O11C 123.5(10) . . ?
O12C C1C C2C 119.9(10) . . ?
O11C C1C C2C 116.6(9) . . ?
O21C C2C C1C 109.4(9) . . ?
O21C C2C C3C 115.1(9) . . ?
C1C C2C C3C 106.7(9) . . ?
O21C C2C H2C 108.5 . . ?
C1C C2C H2C 108.5 . . ?
C3C C2C H2C 108.5 . . ?
O31C C3C C4C 108.0(9) . . ?
O31C C3C C2C 110.0(9) . . ?
C4C C3C C2C 111.8(9) . . ?
O31C C3C H3C 109.0 . . ?
C4C C3C H3C 109.0 . . ?
C2C C3C H3C 109.0 . . ?
O42C C4C O41C 126.8(11) . . ?
O42C C4C C3C 117.0(10) . . ?
O41C C4C C3C 116.1(10) . . ?
C1A O11A Ho1 91.7(7) . . ?
C1A O12A Ho1 90.5(7) . . ?
C2A O21A H21A 113.2 . . ?
C3A O31A H31A 99.5 . . ?
C4A O41A Ho2 99.0(8) . 1_444 ?
C4A O42A Ho2 87.0(7) . 1_444 ?
C1B O11B Ho2 126.0(7) . . ?
C1B O12B Ho1 137.1(8) . . ?
C2B O21B Ho2 114.8(7) . . ?
C2B O21B H21B 106.0 . . ?
Ho2 O21B H21B 100.7 . . ?
C3B O31B Ho1 121.3(6) . 1_565 ?
C3B O31B H31B 112.9 . . ?
Ho1 O31B H31B 117.7 1_565 . ?
C4B O41B Ho1 128.7(7) . 1_565 ?
C4B O42B Ho1 132.8(7) . 1_465 ?
C1C O12C Ho2 140.2(7) . 1_545 ?
C1C O11C Ho1 123.5(7) . . ?
C2C O21C Ho1 116.1(6) . . ?
C2C O21C H21C 106.9 . . ?
Ho1 O21C H21C 100.4 . . ?
C3C O31C Ho2 122.2(6) . . ?
C3C O31C H31C 108.2 . . ?
Ho2 O31C H31C 116.8 . . ?
C4C O41C Ho2 128.2(7) . . ?
C4C O42C Ho2 133.9(8) . 1_655 ?
Ho1 O1W H11W 140.8 . . ?
Ho1 O1W H12W 98.6 . . ?
H11W O1W H12W 107.0 . . ?
Ho2 O2W H21W 147.7 . . ?
Ho2 O2W H22W 100.3 . . ?
H21W O2W H22W 112.0 . . ?
H31W O3W H32W 108.0 . . ?
H41W O4W H42W 102.3 . . ?
H51W O5W H52W 105.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O21A H21A O42A 0.86 1.96 2.809(12) 166.2 1_655 yes
O31A H31A O12A 0.85 1.88 2.706(12) 167.0 1_455 yes
O21B H21B O11C 0.85 1.74 2.582(11) 171.3 1_565 yes
O31B H31B O3W 0.92 1.91 2.748(11) 150.8 . yes
O21C H21C O11B 0.86 1.74 2.589(12) 169.5 . yes
O31C H31C O4W 0.84 1.80 2.635(13) 171.3 . yes
O1W H11W O5W 0.86 2.05 2.871(12) 159.8 . yes
O1W H12W O41B 0.84 1.88 2.710(12) 169.7 1_645 yes
O2W H21W O4W 0.78 2.37 2.804(14) 116.5 1_565 yes
O2W H22W O41C 0.85 1.91 2.722(12) 158.7 1_455 yes
O3W H31W O21A 0.87 2.00 2.814(11) 154.0 1_565 yes
O3W H32W O11A 0.87 1.97 2.802(12) 159.5 . yes
O4W H41W O41A 0.86 1.91 2.751(14) 166.2 1_656 yes
O4W H42W O5W 0.87 2.03 2.873(13) 164.1 1_556 yes
O5W H51W O31A 0.85 1.97 2.807(13) 168.6 1_665 yes
O5W H52W O3W 0.85 1.93 2.771(14) 173.5 . yes

_refine_diff_density_max         4.247
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.222


# start Validation Reply Form
_vrf_PLAT971_Compound_Ho-D       
;
PROBLEM: Check Calcd Resid. Dens.  0.96A   From Ho2             4.39 eA-3  
RESPONSE: This compound crystallizes as a twinned specimen as all isostructural
compounds with other trivalent metal ions. Despite the fact that specific absorption
correction based on the faces of the crystal has been performed, somewhat large
diffraction peaks close to the lanthanide atoms could not be removed. Nonetheless,
the unaccounted positive residual density around the lanthanide heavy atom is 
quite common for lanthanide-organic based crystal structures.
;
# end Validation Reply Form

