# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_1R-La-RT2
_database_code_depnum_ccdc_archive 'CCDC 1574643'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT043_1R-La-RT2           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      12.19 Check
RESPONSE:12 H atoms should be attached to severely disordered O atoms 
of water or formic acid, for which the disorder could not eliminated 
although we have applied several restaints to limit it. Thus,these H atoms 
were omitted due to refinement instability and disordered solvent
;
_vrf_PLAT220_1R-La-RT2           
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         6.3 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF and water). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the La centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_1R-La-RT2           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[La2(C16H9O7)2(C3H7ON)2(H2O)0.7(CHOOH)1.3]??4.7H2O'
_chemical_formula_sum            'C39.30 H45.40 La2 N2 O24'
_chemical_formula_weight         1207.59

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'
N N 0.0061 0.0033 '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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.529(3)
_cell_length_b                   14.5251(15)
_cell_length_c                   13.6581(14)
_cell_angle_alpha                90
_cell_angle_beta                 100.636(3)
_cell_angle_gamma                90
_cell_volume                     5562.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9392
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      26.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_F_000             2405
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.589
_shelx_estimated_absorpt_T_min   0.683
_shelx_estimated_absorpt_T_max   0.692
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55510
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.591
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6988
_reflns_number_gt                5657
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0737P)²+37.2319P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6988
_refine_ls_number_parameters     305
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1422
_refine_ls_wR_factor_gt          0.1326
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.17935(2) 0.28823(2) 0.94776(2) 0.02058(10) Uani 1 1 d . . . . .
O1 O 0.23552(13) 0.3389(3) 0.8384(3) 0.0418(10) Uani 1 1 d . . . . .
O2 O 0.30762(14) 0.2773(3) 0.8805(3) 0.0350(8) Uani 1 1 d . . . . .
O3 O 0.20382(12) 0.5699(3) 0.5612(3) 0.0384(9) Uani 1 1 d . . . . .
O4 O 0.26543(12) 0.6551(2) 0.5485(3) 0.0281(7) Uani 1 1 d . . . . .
O5 O 0.42042(15) 0.3555(3) 0.6397(4) 0.0605(14) Uani 1 1 d . . . . .
O6 O 0.61081(13) 0.3258(3) 0.4629(3) 0.0419(9) Uani 1 1 d . . . . .
O7 O 0.59770(14) 0.1803(3) 0.4920(4) 0.0462(10) Uani 1 1 d . . . . .
C1 C 0.29571(16) 0.3923(3) 0.7567(4) 0.0267(10) Uani 1 1 d . . . . .
C2 C 0.26423(16) 0.4531(3) 0.6997(4) 0.0270(10) Uani 1 1 d . . . . .
H2 H 0.232155 0.452664 0.704627 0.032 Uiso 1 1 calc R U . . .
C3 C 0.28047(16) 0.5145(3) 0.6352(3) 0.0244(9) Uani 1 1 d . . . . .
C4 C 0.32813(17) 0.5115(3) 0.6256(4) 0.0268(10) Uani 1 1 d . . . . .
H4 H 0.339040 0.551707 0.581801 0.032 Uiso 1 1 calc R U . . .
C5 C 0.35956(17) 0.4501(3) 0.6800(4) 0.0283(10) Uani 1 1 d . . . . .
C6 C 0.34334(17) 0.3908(3) 0.7464(4) 0.0287(10) Uani 1 1 d . . . . .
H6 H 0.364412 0.349929 0.784156 0.034 Uiso 1 1 calc R U . . .
C7 C 0.27831(17) 0.3307(4) 0.8316(4) 0.0284(10) Uani 1 1 d . . . . .
C8 C 0.24787(16) 0.5834(3) 0.5786(3) 0.0246(9) Uani 1 1 d . . . . .
C9 C 0.41043(18) 0.4477(4) 0.6661(5) 0.0367(12) Uani 1 1 d . . . . .
H9A H 0.415091 0.489936 0.613691 0.044 Uiso 1 1 calc R U . . .
H9B H 0.431529 0.465529 0.727174 0.044 Uiso 1 1 calc R U . . .
C10 C 0.4620(2) 0.3393(4) 0.6064(5) 0.0458(15) Uani 1 1 d . . . . .
C11 C 0.4695(3) 0.2493(5) 0.5849(7) 0.069(2) Uani 1 1 d . U . . .
H11 H 0.447508 0.204564 0.594442 0.082 Uiso 1 1 calc R U . . .
C12 C 0.5100(3) 0.2249(5) 0.5488(7) 0.060(2) Uani 1 1 d . U . . .
H12 H 0.514999 0.163554 0.534192 0.072 Uiso 1 1 calc R U . . .
C13 C 0.54321(19) 0.2907(4) 0.5340(4) 0.0352(12) Uani 1 1 d . . . . .
C14 C 0.53503(18) 0.3802(4) 0.5577(4) 0.0371(12) Uani 1 1 d . . . . .
H14 H 0.556864 0.425320 0.548084 0.045 Uiso 1 1 calc R U . . .
C15 C 0.49497(19) 0.4052(4) 0.5956(5) 0.0404(13) Uani 1 1 d . . . . .
H15 H 0.490569 0.465944 0.613357 0.048 Uiso 1 1 calc R U . . .
C16 C 0.58653(18) 0.2650(4) 0.4935(4) 0.0340(11) Uani 1 1 d . . . . .
O8 O 0.15176(18) 0.2217(3) 0.7743(3) 0.0550(12) Uani 1 1 d . . . . .
C17 C 0.1627(4) 0.2463(8) 0.6962(6) 0.082(3) Uani 1 1 d . U . . .
H17 H 0.170694 0.308018 0.691233 0.099 Uiso 1 1 calc R U . . .
N1 N 0.1643(3) 0.1939(7) 0.6184(5) 0.088(2) Uani 1 1 d . U . . .
C18 C 0.1797(6) 0.2301(13) 0.5294(10) 0.153(6) Uani 1 1 d . U . . .
H18A H 0.182761 0.295775 0.534441 0.229 Uiso 1 1 calc R U . . .
H18B H 0.156494 0.214499 0.471443 0.229 Uiso 1 1 calc R U . . .
H18C H 0.209918 0.203542 0.523816 0.229 Uiso 1 1 calc R U . . .
C19 C 0.1486(6) 0.1031(9) 0.6153(9) 0.140(5) Uani 1 1 d . U . . .
H19A H 0.173141 0.063346 0.599964 0.209 Uiso 1 1 calc R U . . .
H19B H 0.120483 0.096846 0.564880 0.209 Uiso 1 1 calc R U . . .
H19C H 0.141327 0.086409 0.678841 0.209 Uiso 1 1 calc R U . . .
O9 O 0.1441(2) 0.4236(4) 0.8506(4) 0.0729(16) Uani 0.65 1 d D . P A 1
C20 C 0.1245(5) 0.4909(7) 0.8091(11) 0.095(5) Uani 0.65 1 d D U P A 1
H20 H 0.091751 0.481513 0.791431 0.114 Uiso 0.65 1 calc R U P A 1
O10 O 0.1354(4) 0.5680(5) 0.7837(7) 0.085(3) Uani 0.65 1 d D U P A 1
O9A O 0.1441(2) 0.4236(4) 0.8506(4) 0.0729(16) Uani 0.35 1 d . . P A 2
O11 O 0.1283(9) 0.6446(18) 0.7507(19) 0.122(8) Uiso 0.35 1 d . . P B 2
O12 O 0.5443(4) 0.0075(7) 0.4541(8) 0.147(3) Uiso 1 1 d . . . . .
O13 O 0.500000 0.2498(13) 0.250000 0.170(6) Uiso 1 2 d S . P . .
O14 O 0.1332(6) 0.4282(12) 0.5662(12) 0.115(5) Uiso 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O9A 2.479(4) . ?
La1 O9 2.479(4) . ?
La1 O4 2.489(3) 4_546 ?
La1 O2 2.495(4) 7_557 ?
La1 O1 2.495(3) . ?
La1 O8 2.545(4) . ?
La1 O7 2.554(4) 8_456 ?
La1 O3 2.596(4) 6_566 ?
La1 O6 2.600(4) 8_456 ?
La1 O4 2.712(3) 6_566 ?
La1 C16 2.934(5) 8_456 ?
La1 C8 3.033(5) 6_566 ?
O1 C7 1.247(6) . ?
O2 C7 1.242(6) . ?
O3 C8 1.251(6) . ?
O4 C8 1.257(5) . ?
O5 C10 1.366(6) . ?
O5 C9 1.429(7) . ?
O6 C16 1.242(7) . ?
O7 C16 1.271(7) . ?
C1 C2 1.391(6) . ?
C1 C6 1.392(6) . ?
C1 C7 1.510(6) . ?
C2 C3 1.392(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(6) . ?
C3 C8 1.483(6) . ?
C4 C5 1.380(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(6) . ?
C5 C9 1.499(6) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.365(10) . ?
C10 C15 1.370(8) . ?
C11 C12 1.383(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(7) . ?
C13 C16 1.492(7) . ?
C14 C15 1.387(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O8 C17 1.219(10) . ?
C17 N1 1.315(12) . ?
C17 H17 0.9300 . ?
N1 C19 1.392(15) . ?
N1 C18 1.465(14) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O9 C20 1.214(8) . ?
C20 O10 1.229(9) . ?
C20 H20 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 La1 O4 145.10(15) . 4_546 ?
O9 La1 O2 141.36(16) . 7_557 ?
O4 La1 O2 72.55(12) 4_546 7_557 ?
O9A La1 O1 71.81(16) . . ?
O9 La1 O1 71.81(16) . . ?
O4 La1 O1 76.56(12) 4_546 . ?
O2 La1 O1 132.43(12) 7_557 . ?
O9A La1 O8 77.14(19) . . ?
O9 La1 O8 77.14(19) . . ?
O4 La1 O8 79.06(14) 4_546 . ?
O2 La1 O8 134.20(15) 7_557 . ?
O1 La1 O8 71.17(15) . . ?
O9 La1 O7 71.74(16) . 8_456 ?
O4 La1 O7 137.38(12) 4_546 8_456 ?
O2 La1 O7 80.20(14) 7_557 8_456 ?
O1 La1 O7 143.49(14) . 8_456 ?
O8 La1 O7 98.60(16) . 8_456 ?
O9 La1 O3 74.20(19) . 6_566 ?
O4 La1 O3 120.34(11) 4_546 6_566 ?
O2 La1 O3 76.40(13) 7_557 6_566 ?
O1 La1 O3 89.50(14) . 6_566 ?
O8 La1 O3 149.32(15) . 6_566 ?
O7 La1 O3 82.71(13) 8_456 6_566 ?
O9 La1 O6 108.10(18) . 8_456 ?
O4 La1 O6 89.19(12) 4_546 8_456 ?
O2 La1 O6 70.49(14) 7_557 8_456 ?
O1 La1 O6 144.21(14) . 8_456 ?
O8 La1 O6 73.98(14) . 8_456 ?
O7 La1 O6 50.43(13) 8_456 8_456 ?
O3 La1 O6 125.59(12) 6_566 8_456 ?
O9 La1 O4 105.73(17) . 6_566 ?
O4 La1 O4 73.42(11) 4_546 6_566 ?
O2 La1 O4 71.04(12) 7_557 6_566 ?
O1 La1 O4 65.95(12) . 6_566 ?
O8 La1 O4 133.08(14) . 6_566 ?
O7 La1 O4 127.29(13) 8_456 6_566 ?
O3 La1 O4 48.51(10) 6_566 6_566 ?
O6 La1 O4 141.00(13) 8_456 6_566 ?
O9A La1 C16 91.68(18) . 8_456 ?
O9 La1 C16 91.68(18) . 8_456 ?
O4 La1 C16 112.57(14) 4_546 8_456 ?
O2 La1 C16 71.53(14) 7_557 8_456 ?
O1 La1 C16 155.47(14) . 8_456 ?
O8 La1 C16 87.82(16) . 8_456 ?
O7 La1 C16 25.60(15) 8_456 8_456 ?
O3 La1 C16 103.65(14) 6_566 8_456 ?
O6 La1 C16 25.02(14) 8_456 8_456 ?
O4 La1 C16 137.76(13) 6_566 8_456 ?
O9 La1 C8 88.95(18) . 6_566 ?
O4 La1 C8 97.39(12) 4_546 6_566 ?
O2 La1 C8 73.31(13) 7_557 6_566 ?
O1 La1 C8 75.87(13) . 6_566 ?
O8 La1 C8 146.78(13) . 6_566 ?
O7 La1 C8 105.50(13) 8_456 6_566 ?
O3 La1 C8 24.10(11) 6_566 6_566 ?
O6 La1 C8 139.23(12) 8_456 6_566 ?
O4 La1 C8 24.47(11) 6_566 6_566 ?
C16 La1 C8 123.05(14) 8_456 6_566 ?
C7 O1 La1 139.7(3) . . ?
C7 O2 La1 135.5(3) . 7_557 ?
C8 O3 La1 98.0(3) . 6_565 ?
C8 O4 La1 157.8(3) . 4_556 ?
C8 O4 La1 92.2(3) . 6_565 ?
La1 O4 La1 106.57(11) 4_556 6_565 ?
C10 O5 C9 118.1(4) . . ?
C16 O6 La1 92.7(3) . 8 ?
C16 O7 La1 94.2(3) . 8 ?
C2 C1 C6 119.7(4) . . ?
C2 C1 C7 119.8(4) . . ?
C6 C1 C7 120.5(4) . . ?
C1 C2 C3 120.3(4) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 119.0(4) . . ?
C4 C3 C8 120.2(4) . . ?
C2 C3 C8 120.8(4) . . ?
C5 C4 C3 121.3(4) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 119.3(4) . . ?
C4 C5 C9 119.7(4) . . ?
C6 C5 C9 121.0(4) . . ?
C5 C6 C1 120.3(4) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
O2 C7 O1 126.2(4) . . ?
O2 C7 C1 117.5(4) . . ?
O1 C7 C1 116.3(4) . . ?
O3 C8 O4 121.0(4) . . ?
O3 C8 C3 120.3(4) . . ?
O4 C8 C3 118.7(4) . . ?
O3 C8 La1 57.9(2) . 6_565 ?
O4 C8 La1 63.3(2) . 6_565 ?
C3 C8 La1 174.8(3) . 6_565 ?
O5 C9 C5 107.3(4) . . ?
O5 C9 H9A 110.3 . . ?
C5 C9 H9A 110.3 . . ?
O5 C9 H9B 110.3 . . ?
C5 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
C11 C10 O5 114.7(5) . . ?
C11 C10 C15 120.4(5) . . ?
O5 C10 C15 124.9(5) . . ?
C10 C11 C12 119.9(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C13 120.9(6) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 118.0(5) . . ?
C14 C13 C16 121.0(5) . . ?
C12 C13 C16 121.1(5) . . ?
C13 C14 C15 121.6(5) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C10 C15 C14 119.2(5) . . ?
C10 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
O6 C16 O7 121.8(5) . . ?
O6 C16 C13 119.9(5) . . ?
O7 C16 C13 118.4(5) . . ?
O6 C16 La1 62.3(3) . 8 ?
O7 C16 La1 60.2(2) . 8 ?
C13 C16 La1 170.7(4) . 8 ?
C17 O8 La1 128.2(5) . . ?
O8 C17 N1 126.2(10) . . ?
O8 C17 H17 116.9 . . ?
N1 C17 H17 116.9 . . ?
C17 N1 C19 121.0(9) . . ?
C17 N1 C18 121.6(11) . . ?
C19 N1 C18 117.3(11) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 La1 174.5(8) . . ?
O9 C20 O10 138.3(14) . . ?
O9 C20 H20 110.9 . . ?
O10 C20 H20 110.9 . . ?

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
C6 C1 C2 C3 -2.4(8) . . . . ?
C7 C1 C2 C3 175.7(5) . . . . ?
C1 C2 C3 C4 2.6(7) . . . . ?
C1 C2 C3 C8 -176.2(5) . . . . ?
C2 C3 C4 C5 -1.1(8) . . . . ?
C8 C3 C4 C5 177.8(5) . . . . ?
C3 C4 C5 C6 -0.8(8) . . . . ?
C3 C4 C5 C9 178.7(5) . . . . ?
C4 C5 C6 C1 1.1(8) . . . . ?
C9 C5 C6 C1 -178.4(5) . . . . ?
C2 C1 C6 C5 0.5(8) . . . . ?
C7 C1 C6 C5 -177.6(5) . . . . ?
La1 O2 C7 O1 -32.5(9) 7_557 . . . ?
La1 O2 C7 C1 147.3(4) 7_557 . . . ?
La1 O1 C7 O2 10.3(10) . . . . ?
La1 O1 C7 C1 -169.5(4) . . . . ?
C2 C1 C7 O2 179.7(5) . . . . ?
C6 C1 C7 O2 -2.3(8) . . . . ?
C2 C1 C7 O1 -0.5(7) . . . . ?
C6 C1 C7 O1 177.5(5) . . . . ?
La1 O3 C8 O4 5.5(5) 6_565 . . . ?
La1 O3 C8 C3 -174.3(4) 6_565 . . . ?
La1 O4 C8 O3 143.1(6) 4_556 . . . ?
La1 O4 C8 O3 -5.2(5) 6_565 . . . ?
La1 O4 C8 C3 -37.1(10) 4_556 . . . ?
La1 O4 C8 C3 174.6(4) 6_565 . . . ?
La1 O4 C8 La1 148.3(8) 4_556 . . 6_565 ?
C4 C3 C8 O3 157.5(5) . . . . ?
C2 C3 C8 O3 -23.6(7) . . . . ?
C4 C3 C8 O4 -22.3(7) . . . . ?
C2 C3 C8 O4 156.6(5) . . . . ?
C10 O5 C9 C5 168.9(5) . . . . ?
C4 C5 C9 O5 -123.9(5) . . . . ?
C6 C5 C9 O5 55.6(7) . . . . ?
C9 O5 C10 C11 178.6(7) . . . . ?
C9 O5 C10 C15 -0.5(10) . . . . ?
O5 C10 C11 C12 178.8(8) . . . . ?
C15 C10 C11 C12 -2.1(13) . . . . ?
C10 C11 C12 C13 0.0(14) . . . . ?
C11 C12 C13 C14 0.9(12) . . . . ?
C11 C12 C13 C16 -178.9(8) . . . . ?
C12 C13 C14 C15 0.2(10) . . . . ?
C16 C13 C14 C15 -179.9(6) . . . . ?
C11 C10 C15 C14 3.2(11) . . . . ?
O5 C10 C15 C14 -177.8(6) . . . . ?
C13 C14 C15 C10 -2.3(10) . . . . ?
La1 O6 C16 O7 -9.8(6) 8 . . . ?
La1 O6 C16 C13 169.6(5) 8 . . . ?
La1 O7 C16 O6 10.0(6) 8 . . . ?
La1 O7 C16 C13 -169.4(5) 8 . . . ?
C14 C13 C16 O6 -13.8(9) . . . . ?
C12 C13 C16 O6 166.1(7) . . . . ?
C14 C13 C16 O7 165.7(6) . . . . ?
C12 C13 C16 O7 -14.4(9) . . . . ?
La1 O8 C17 N1 151.3(8) . . . . ?
O8 C17 N1 C19 6.2(19) . . . . ?
O8 C17 N1 C18 -177.7(12) . . . . ?

_refine_diff_density_max         2.431
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.173

####################################################################### 
# 
# 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_5R-Eu-RT
_database_code_depnum_ccdc_archive 'CCDC 1574649'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_5R-Eu-RT            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O11 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Eu2(C16H9O7)2(C3H7ON)2(H2O)(CHOOH)]??3H2O'
_chemical_formula_sum            'C39 H41 Eu2 N2 O22'
_chemical_formula_weight         1193.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.4907(17)
_cell_length_b                   14.4061(9)
_cell_length_c                   13.6706(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.059(2)
_cell_angle_gamma                90
_cell_volume                     5541.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9908
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      28.36

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_F_000             2364
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    2.312
_shelx_estimated_absorpt_T_min   0.596
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26798
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.822
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6939
_reflns_number_gt                5818
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²+33.8916P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6939
_refine_ls_number_parameters     317
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.002
_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
Eu1 Eu 0.18172(2) 0.28994(2) 0.45615(2) 0.02062(7) Uani 1 1 d . . . . .
O1 O 0.23458(10) 0.3487(2) 0.3495(2) 0.0354(7) Uani 1 1 d . . . . .
O2 O 0.30546(11) 0.2783(2) 0.3822(2) 0.0330(7) Uani 1 1 d . . . . .
O3 O 0.20543(10) 0.5734(2) 0.0627(3) 0.0380(7) Uani 1 1 d . . . . .
O4 O 0.26708(10) 0.66115(19) 0.0519(2) 0.0285(6) Uani 1 1 d . . . . .
O5 O 0.42241(12) 0.3551(3) 0.1471(3) 0.0571(11) Uani 1 1 d . U . . .
O6 O 0.61564(11) 0.3218(2) -0.0305(3) 0.0446(9) Uani 1 1 d . . . . .
O7 O 0.60610(11) 0.1776(2) 0.0141(3) 0.0431(8) Uani 1 1 d . . . . .
C1 C 0.29486(13) 0.3969(3) 0.2611(3) 0.0260(8) Uani 1 1 d . . . . .
C2 C 0.26425(13) 0.4590(3) 0.2051(3) 0.0273(8) Uani 1 1 d . . . . .
H2 H 0.232318 0.460761 0.212130 0.033 Uiso 1 1 calc R U . . .
C3 C 0.28135(14) 0.5184(3) 0.1387(3) 0.0263(8) Uani 1 1 d . . . . .
C4 C 0.32884(14) 0.5144(3) 0.1267(3) 0.0285(8) Uani 1 1 d . . . . .
H4 H 0.340214 0.554288 0.082327 0.034 Uiso 1 1 calc R U . . .
C5 C 0.35948(14) 0.4511(3) 0.1807(3) 0.0308(9) Uani 1 1 d . . . . .
C6 C 0.34240(14) 0.3932(3) 0.2490(3) 0.0289(8) Uani 1 1 d . . . . .
H6 H 0.362911 0.351947 0.286597 0.035 Uiso 1 1 calc R U . . .
C7 C 0.27684(14) 0.3359(3) 0.3374(3) 0.0274(8) Uani 1 1 d . . . . .
C8 C 0.24910(14) 0.5885(3) 0.0816(3) 0.0262(8) Uani 1 1 d . . . . .
C9 C 0.41084(15) 0.4480(3) 0.1653(4) 0.0376(10) Uani 1 1 d . . . . .
H9A H 0.415317 0.486744 0.109423 0.045 Uiso 1 1 calc R U . . .
H9B H 0.431261 0.471051 0.223744 0.045 Uiso 1 1 calc R U . . .
C10 C 0.46502(16) 0.3380(4) 0.1156(5) 0.0467(13) Uani 1 1 d . . . . .
C11 C 0.4754(2) 0.2464(4) 0.1039(6) 0.0686(19) Uani 1 1 d . U . . .
H11 H 0.454506 0.200966 0.119350 0.082 Uiso 1 1 calc R U . . .
C12 C 0.5167(2) 0.2204(4) 0.0691(6) 0.0631(18) Uani 1 1 d . U . . .
H12 H 0.523248 0.157872 0.060935 0.076 Uiso 1 1 calc R U . . .
C13 C 0.54855(15) 0.2882(3) 0.0463(4) 0.0378(10) Uani 1 1 d . . . . .
C14 C 0.53806(15) 0.3796(3) 0.0610(4) 0.0393(11) Uani 1 1 d . . . . .
H14 H 0.559023 0.425346 0.046817 0.047 Uiso 1 1 calc R U . . .
C15 C 0.49669(16) 0.4056(3) 0.0967(4) 0.0423(11) Uani 1 1 d . . . . .
H15 H 0.490528 0.467879 0.107543 0.051 Uiso 1 1 calc R U . . .
C16 C 0.59277(14) 0.2610(3) 0.0075(4) 0.0334(9) Uani 1 1 d . . . . .
O8 O 0.14347(15) 0.4204(3) 0.3636(4) 0.0671(13) Uani 0.5 1 d . . P A 1
C17 C 0.1550(4) 0.4958(6) 0.3529(7) 0.092(3) Uani 0.5 1 d . U P A 1
H17 H 0.181164 0.515230 0.397737 0.111 Uiso 0.5 1 calc R U P A 1
N1 N 0.1371(4) 0.5600(6) 0.2869(7) 0.135(3) Uani 0.5 1 d . U P A 1
C18 C 0.1524(7) 0.6471(8) 0.2777(10) 0.084(5) Uani 0.5 1 d . U P A 1
H18A H 0.130573 0.689842 0.300134 0.127 Uiso 0.5 1 calc R U P A 1
H18B H 0.154480 0.659310 0.209520 0.127 Uiso 0.5 1 calc R U P A 1
H18C H 0.183247 0.654361 0.317031 0.127 Uiso 0.5 1 calc R U P A 1
C19 C 0.0997(9) 0.5358(18) 0.2155(18) 0.155(10) Uani 0.5 1 d . U P A 1
H19A H 0.091100 0.587730 0.172417 0.232 Uiso 0.5 1 calc R U P A 1
H19B H 0.073050 0.518169 0.246476 0.232 Uiso 0.5 1 calc R U P A 1
H19C H 0.108809 0.484553 0.177717 0.232 Uiso 0.5 1 calc R U P A 1
O9 O 0.15351(17) 0.2290(3) 0.2882(3) 0.0628(12) Uani 0.5 1 d . . P A 1
C20 C 0.1613(4) 0.2577(10) 0.2100(7) 0.055(3) Uani 0.5 1 d . U P A 1
H20 H 0.170709 0.319397 0.208446 0.066 Uiso 0.5 1 calc R U P A 1
N2 N 0.1580(5) 0.2115(10) 0.1260(7) 0.071(3) Uani 0.5 1 d . U P A 1
C21 C 0.1432(9) 0.1244(14) 0.1196(11) 0.113(6) Uani 0.5 1 d . U P A 1
H21A H 0.156422 0.091567 0.178605 0.169 Uiso 0.5 1 calc R U P A 1
H21B H 0.153300 0.095471 0.063159 0.169 Uiso 0.5 1 calc R U P A 1
H21C H 0.109138 0.123020 0.112280 0.169 Uiso 0.5 1 calc R U P A 1
C22 C 0.1632(10) 0.265(2) 0.0310(14) 0.142(8) Uani 0.5 1 d . U P A 1
H22A H 0.137923 0.248394 -0.020879 0.212 Uiso 0.5 1 calc R U P A 1
H22B H 0.193211 0.250620 0.011297 0.212 Uiso 0.5 1 calc R U P A 1
H22C H 0.161742 0.330867 0.043450 0.212 Uiso 0.5 1 calc R U P A 1
O8A O 0.14347(15) 0.4204(3) 0.3636(4) 0.0671(13) Uani 0.5 1 d . . P A 2
C17A C 0.1550(4) 0.4958(6) 0.3529(7) 0.092(3) Uani 0.5 1 d . . P A 2
H17A H 0.181164 0.515230 0.397737 0.111 Uiso 0.5 1 calc R U P A 2
O10 O 0.1371(4) 0.5600(6) 0.2869(7) 0.135(3) Uani 0.5 1 d . . P A 2
O9A O 0.15351(17) 0.2290(3) 0.2882(3) 0.0628(12) Uani 0.5 1 d . . P A 2
O11 O 0.000000 0.2682(19) 0.250000 0.333(10) Uiso 1 2 d S . P . .
O12 O 0.0534(6) 0.5023(11) 0.4654(11) 0.270(7) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O4 2.373(3) 4_545 ?
Eu1 O2 2.394(3) 7_556 ?
Eu1 O1 2.408(3) . ?
Eu1 O8 2.426(4) . ?
Eu1 O8A 2.426(4) . ?
Eu1 O7 2.455(3) 8_456 ?
Eu1 O9 2.472(4) . ?
Eu1 O9A 2.472(4) . ?
Eu1 O3 2.479(3) 6_566 ?
Eu1 O6 2.505(3) 8_456 ?
Eu1 O4 2.668(3) 6_566 ?
Eu1 C16 2.831(4) 8_456 ?
O1 C7 1.255(5) . ?
O2 C7 1.254(5) . ?
O3 C8 1.249(5) . ?
O4 C8 1.260(5) . ?
O5 C10 1.372(5) . ?
O5 C9 1.410(6) . ?
O6 C16 1.251(6) . ?
O7 C16 1.259(6) . ?
C1 C6 1.391(5) . ?
C1 C2 1.392(5) . ?
C1 C7 1.513(5) . ?
C2 C3 1.391(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(5) . ?
C3 C8 1.499(5) . ?
C4 C5 1.392(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(5) . ?
C5 C9 1.512(5) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.367(8) . ?
C10 C15 1.380(7) . ?
C11 C12 1.389(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.401(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.373(6) . ?
C13 C16 1.494(6) . ?
C14 C15 1.396(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O8 C17 1.150(9) . ?
C17 N1 1.337(11) . ?
C17 H17 0.9300 . ?
N1 C18 1.340(15) . ?
N1 C19 1.37(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O9 C20 1.198(10) . ?
C20 N2 1.317(15) . ?
C20 H20 0.9300 . ?
N2 C21 1.32(2) . ?
N2 C22 1.54(2) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
O8A C17A 1.150(9) . ?
C17A O10 1.337(11) . ?
C17A H17A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Eu1 O2 73.50(10) 4_545 7_556 ?
O4 Eu1 O1 78.43(10) 4_545 . ?
O2 Eu1 O1 133.16(10) 7_556 . ?
O4 Eu1 O8 144.12(13) 4_545 . ?
O2 Eu1 O8 142.23(13) 7_556 . ?
O1 Eu1 O8 71.60(12) . . ?
O4 Eu1 O8A 144.12(13) 4_545 . ?
O2 Eu1 O8A 142.23(13) 7_556 . ?
O1 Eu1 O8A 71.60(12) . . ?
O4 Eu1 O7 137.80(11) 4_545 8_456 ?
O2 Eu1 O7 78.13(12) 7_556 8_456 ?
O1 Eu1 O7 142.44(11) . 8_456 ?
O8 Eu1 O7 71.10(13) . 8_456 ?
O4 Eu1 O9 77.98(14) 4_545 . ?
O2 Eu1 O9 133.78(14) 7_556 . ?
O1 Eu1 O9 72.87(13) . . ?
O8 Eu1 O9 74.74(17) . . ?
O7 Eu1 O9 101.18(15) 8_456 . ?
O4 Eu1 O9A 77.98(14) 4_545 . ?
O2 Eu1 O9A 133.78(14) 7_556 . ?
O1 Eu1 O9A 72.87(13) . . ?
O8A Eu1 O9A 74.74(17) . . ?
O7 Eu1 O9A 101.18(15) 8_456 . ?
O4 Eu1 O3 122.36(10) 4_545 6_566 ?
O2 Eu1 O3 78.21(12) 7_556 6_566 ?
O1 Eu1 O3 86.44(11) . 6_566 ?
O8 Eu1 O3 75.52(16) . 6_566 ?
O7 Eu1 O3 80.28(11) 8_456 6_566 ?
O9 Eu1 O3 147.87(14) . 6_566 ?
O4 Eu1 O6 88.61(11) 4_545 8_456 ?
O2 Eu1 O6 71.09(12) 7_556 8_456 ?
O1 Eu1 O6 144.97(12) . 8_456 ?
O8 Eu1 O6 104.75(15) . 8_456 ?
O7 Eu1 O6 52.46(11) 8_456 8_456 ?
O9 Eu1 O6 72.64(14) . 8_456 ?
O3 Eu1 O6 127.27(11) 6_566 8_456 ?
O4 Eu1 O4 73.12(10) 4_545 6_566 ?
O2 Eu1 O4 70.18(10) 7_556 6_566 ?
O1 Eu1 O4 66.13(10) . 6_566 ?
O8 Eu1 O4 110.55(14) . 6_566 ?
O7 Eu1 O4 124.75(11) 8_456 6_566 ?
O9 Eu1 O4 133.41(13) . 6_566 ?
O3 Eu1 O4 50.14(9) 6_566 6_566 ?
O6 Eu1 O4 140.46(12) 8_456 6_566 ?
O4 Eu1 C16 112.93(12) 4_545 8_456 ?
O2 Eu1 C16 71.15(12) 7_556 8_456 ?
O1 Eu1 C16 155.60(12) . 8_456 ?
O8 Eu1 C16 89.09(14) . 8_456 ?
O8A Eu1 C16 89.09(14) . 8_456 ?
O7 Eu1 C16 26.33(12) 8_456 8_456 ?
O9 Eu1 C16 88.02(15) . 8_456 ?
O9A Eu1 C16 88.02(15) . 8_456 ?
O3 Eu1 C16 103.41(12) 6_566 8_456 ?
O6 Eu1 C16 26.22(12) 8_456 8_456 ?
O4 Eu1 C16 136.82(11) 6_566 8_456 ?
C7 O1 Eu1 137.2(3) . . ?
C7 O2 Eu1 135.7(3) . 7_556 ?
C8 O3 Eu1 98.8(2) . 6_565 ?
C8 O4 Eu1 161.4(3) . 4 ?
C8 O4 Eu1 89.5(2) . 6_565 ?
Eu1 O4 Eu1 106.88(10) 4 6_565 ?
C10 O5 C9 118.0(4) . . ?
C16 O6 Eu1 91.6(3) . 8 ?
C16 O7 Eu1 93.8(3) . 8 ?
C6 C1 C2 119.7(3) . . ?
C6 C1 C7 120.2(3) . . ?
C2 C1 C7 120.1(3) . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 C8 119.7(3) . . ?
C2 C3 C8 120.4(3) . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 119.4(3) . . ?
C4 C5 C9 119.0(4) . . ?
C6 C5 C9 121.6(4) . . ?
C1 C6 C5 120.4(4) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O2 C7 O1 126.6(4) . . ?
O2 C7 C1 117.1(3) . . ?
O1 C7 C1 116.3(3) . . ?
O3 C8 O4 121.3(4) . . ?
O3 C8 C3 120.0(3) . . ?
O4 C8 C3 118.7(4) . . ?
O3 C8 Eu1 56.4(2) . 6_565 ?
O4 C8 Eu1 65.1(2) . 6_565 ?
C3 C8 Eu1 174.0(3) . 6_565 ?
O5 C9 C5 108.1(4) . . ?
O5 C9 H9A 110.1 . . ?
C5 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C5 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
C11 C10 O5 115.4(4) . . ?
C11 C10 C15 120.0(4) . . ?
O5 C10 C15 124.6(5) . . ?
C10 C11 C12 120.7(5) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C13 120.1(5) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 118.2(4) . . ?
C14 C13 C16 121.2(4) . . ?
C12 C13 C16 120.6(4) . . ?
C13 C14 C15 121.6(4) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C10 C15 C14 119.2(4) . . ?
C10 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
O6 C16 O7 121.7(4) . . ?
O6 C16 C13 119.2(4) . . ?
O7 C16 C13 119.1(4) . . ?
O6 C16 Eu1 62.2(2) . 8 ?
O7 C16 Eu1 59.9(2) . 8 ?
C13 C16 Eu1 173.6(4) . 8 ?
C17 O8 Eu1 133.1(6) . . ?
O8 C17 N1 130.7(11) . . ?
O8 C17 H17 114.6 . . ?
N1 C17 H17 114.6 . . ?
C17 N1 C18 128.0(13) . . ?
C17 N1 C19 118.4(13) . . ?
C18 N1 C19 113.6(14) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Eu1 128.9(6) . . ?
O9 C20 N2 127.2(12) . . ?
O9 C20 H20 116.4 . . ?
N2 C20 H20 116.4 . . ?
C20 N2 C21 121.0(12) . . ?
C20 N2 C22 118.5(15) . . ?
C21 N2 C22 119.6(14) . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17A O8A Eu1 133.1(6) . . ?
O8A C17A O10 130.7(11) . . ?
O8A C17A H17A 114.6 . . ?
O10 C17A H17A 114.6 . . ?

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
C6 C1 C2 C3 -1.3(6) . . . . ?
C7 C1 C2 C3 176.7(4) . . . . ?
C1 C2 C3 C4 1.4(6) . . . . ?
C1 C2 C3 C8 -177.1(4) . . . . ?
C2 C3 C4 C5 0.1(7) . . . . ?
C8 C3 C4 C5 178.6(4) . . . . ?
C3 C4 C5 C6 -1.7(7) . . . . ?
C3 C4 C5 C9 179.5(4) . . . . ?
C2 C1 C6 C5 -0.3(7) . . . . ?
C7 C1 C6 C5 -178.3(4) . . . . ?
C4 C5 C6 C1 1.8(7) . . . . ?
C9 C5 C6 C1 -179.5(4) . . . . ?
Eu1 O2 C7 O1 -31.2(7) 7_556 . . . ?
Eu1 O2 C7 C1 148.4(3) 7_556 . . . ?
Eu1 O1 C7 O2 3.2(8) . . . . ?
Eu1 O1 C7 C1 -176.4(3) . . . . ?
C6 C1 C7 O2 -5.3(6) . . . . ?
C2 C1 C7 O2 176.7(4) . . . . ?
C6 C1 C7 O1 174.3(4) . . . . ?
C2 C1 C7 O1 -3.6(6) . . . . ?
Eu1 O3 C8 O4 4.1(4) 6_565 . . . ?
Eu1 O3 C8 C3 -174.5(3) 6_565 . . . ?
Eu1 O4 C8 O3 149.0(6) 4 . . . ?
Eu1 O4 C8 O3 -3.8(4) 6_565 . . . ?
Eu1 O4 C8 C3 -32.4(10) 4 . . . ?
Eu1 O4 C8 C3 174.9(3) 6_565 . . . ?
Eu1 O4 C8 Eu1 152.7(8) 4 . . 6_565 ?
C4 C3 C8 O3 154.2(4) . . . . ?
C2 C3 C8 O3 -27.3(6) . . . . ?
C4 C3 C8 O4 -24.4(6) . . . . ?
C2 C3 C8 O4 154.1(4) . . . . ?
C10 O5 C9 C5 170.0(5) . . . . ?
C4 C5 C9 O5 -129.0(5) . . . . ?
C6 C5 C9 O5 52.3(6) . . . . ?
C9 O5 C10 C11 176.9(6) . . . . ?
C9 O5 C10 C15 -2.7(9) . . . . ?
O5 C10 C11 C12 177.7(7) . . . . ?
C15 C10 C11 C12 -2.6(11) . . . . ?
C10 C11 C12 C13 0.5(12) . . . . ?
C11 C12 C13 C14 1.1(11) . . . . ?
C11 C12 C13 C16 -179.1(6) . . . . ?
C12 C13 C14 C15 -0.6(9) . . . . ?
C16 C13 C14 C15 179.6(5) . . . . ?
C11 C10 C15 C14 3.0(9) . . . . ?
O5 C10 C15 C14 -177.3(5) . . . . ?
C13 C14 C15 C10 -1.4(9) . . . . ?
Eu1 O6 C16 O7 -6.9(5) 8 . . . ?
Eu1 O6 C16 C13 172.9(4) 8 . . . ?
Eu1 O7 C16 O6 7.1(5) 8 . . . ?
Eu1 O7 C16 C13 -172.7(4) 8 . . . ?
C14 C13 C16 O6 -14.3(8) . . . . ?
C12 C13 C16 O6 166.0(6) . . . . ?
C14 C13 C16 O7 165.5(5) . . . . ?
C12 C13 C16 O7 -14.2(8) . . . . ?
Eu1 O8 C17 N1 165.3(7) . . . . ?
O8 C17 N1 C18 -179.5(11) . . . . ?
O8 C17 N1 C19 -3(2) . . . . ?
Eu1 O9 C20 N2 158.7(10) . . . . ?
O9 C20 N2 C21 3(3) . . . . ?
O9 C20 N2 C22 172.0(16) . . . . ?
Eu1 O8A C17A O10 165.3(7) . . . . ?

_refine_diff_density_max         1.435
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.134

####################################################################### 
# 
# 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_4R-Sm-RT2
_database_code_depnum_ccdc_archive 'CCDC 1574651'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT601_4R-Sm-RT2           
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        236 Ang**3
RESPONSE: The existance of large voids containing loosely bound water
solvent is typical for MOF structures.

# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.250  0.250  0.000       235         8 ' '
   2  0.750  0.750  0.000       235         8 ' '
   3  0.250  0.750  0.500       235         8 ' '
   4  0.750  0.250  0.500       235         8 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT220_4R-Sm-RT2           
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         10.0 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the Sm centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT242_4R-Sm-RT2           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         N1 Check
RESPONSE: This may be due to disorder of DMF molecules. 
Application of ISOR restrain doesn't solve this problem completely. 
However, this issue does not undermine the structure.
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[Sm(C16H9O7)(C3H7ON)(H2O)0.5(CHOOH)0.5]??1.25H2O'
_chemical_formula_sum            'C19.50 H20.50 N O10.75 Sm'
_chemical_formula_weight         591.22

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'
N N 0.0061 0.0033 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.754(4)
_cell_length_b                   14.412(2)
_cell_length_c                   13.787(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.044(4)
_cell_angle_gamma                90
_cell_volume                     5670.3(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      26.25

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             2340
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.117
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6208
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44139
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.566
_diffrn_reflns_theta_max         26.427
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5767
_reflns_number_gt                4449
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0498P)²+96.9690P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5767
_refine_ls_number_parameters     299
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1425
_refine_ls_wR_factor_gt          0.1316
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.130
_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
Sm1 Sm 0.31727(2) 0.20916(2) 0.53667(3) 0.02338(13) Uani 1 1 d . . . . .
O1 O 0.30328(18) 0.2784(4) 0.3776(4) 0.0337(12) Uani 1 1 d . . . . .
O2 O 0.23412(18) 0.3502(4) 0.3513(4) 0.0401(14) Uani 1 1 d . . . . .
O3 O 0.20688(18) 0.5739(4) 0.0691(4) 0.0382(13) Uani 1 1 d . . . . .
O4 O 0.26778(18) 0.6607(3) 0.0515(4) 0.0301(12) Uani 1 1 d . . . . .
O5 O 0.4227(2) 0.3591(4) 0.1512(5) 0.0593(19) Uani 1 1 d . U . . .
O6 O 0.6082(2) 0.1797(4) 0.0288(5) 0.0481(16) Uani 1 1 d . . . . .
O7 O 0.6177(2) 0.3224(4) -0.0181(5) 0.0492(17) Uani 1 1 d . . . . .
C1 C 0.2939(3) 0.3991(5) 0.2604(5) 0.0281(16) Uani 1 1 d . . . . .
C2 C 0.2647(3) 0.4611(5) 0.2073(6) 0.0288(16) Uani 1 1 d . . . . .
H2 H 0.233197 0.463250 0.215952 0.035 Uiso 1 1 calc R U . . .
C3 C 0.2818(3) 0.5207(5) 0.1406(6) 0.0293(16) Uani 1 1 d . . . . .
C4 C 0.3283(3) 0.5169(5) 0.1274(6) 0.0317(17) Uani 1 1 d . . . . .
H4 H 0.339797 0.556813 0.082951 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3587(3) 0.4536(5) 0.1798(6) 0.0327(18) Uani 1 1 d . . . . .
C6 C 0.3410(3) 0.3959(5) 0.2461(6) 0.0328(18) Uani 1 1 d . . . . .
H6 H 0.360807 0.354081 0.281948 0.039 Uiso 1 1 calc R U . . .
C7 C 0.2758(3) 0.3369(5) 0.3360(5) 0.0296(16) Uani 1 1 d . . . . .
C8 C 0.2499(3) 0.5894(5) 0.0848(5) 0.0289(17) Uani 1 1 d . . . . .
C9 C 0.4095(3) 0.4520(6) 0.1636(7) 0.043(2) Uani 1 1 d . . . . .
H9A H 0.413987 0.487846 0.105931 0.051 Uiso 1 1 calc R U . . .
H9B H 0.428641 0.478967 0.219292 0.051 Uiso 1 1 calc R U . . .
C10 C 0.4659(3) 0.3422(6) 0.1229(7) 0.048(2) Uani 1 1 d . U . . .
C11 C 0.4776(4) 0.2496(8) 0.1193(9) 0.067(3) Uani 1 1 d . U . . .
H11 H 0.457744 0.204328 0.139112 0.080 Uiso 1 1 calc R U . . .
C12 C 0.5200(4) 0.2249(8) 0.0852(9) 0.064(3) Uani 1 1 d . U . . .
H12 H 0.527388 0.162435 0.080045 0.077 Uiso 1 1 calc R U . . .
C13 C 0.5506(3) 0.2905(6) 0.0595(7) 0.0397(19) Uani 1 1 d . . . . .
C14 C 0.5384(3) 0.3828(6) 0.0677(7) 0.044(2) Uani 1 1 d . . . . .
H14 H 0.558652 0.428444 0.050136 0.053 Uiso 1 1 calc R U . . .
C15 C 0.4973(3) 0.4087(6) 0.1012(7) 0.048(2) Uani 1 1 d . . . . .
H15 H 0.490632 0.471170 0.109256 0.057 Uiso 1 1 calc R U . . .
C16 C 0.5949(3) 0.2635(6) 0.0202(6) 0.0350(18) Uani 1 1 d . . . . .
O8 O 0.3554(3) 0.0770(5) 0.6232(6) 0.073(2) Uani 1 1 d D U . . .
C17 C 0.3413(6) -0.0028(8) 0.6317(12) 0.102(5) Uani 1 1 d D U . . .
H17 H 0.316385 -0.022421 0.587042 0.122 Uiso 1 1 calc R U . . .
N1 N 0.3584(6) -0.0622(10) 0.6979(12) 0.126(5) Uani 1 1 d D U . . .
C18 C 0.3399(8) -0.1538(12) 0.7040(16) 0.178(9) Uani 1 1 d D U . . .
H18A H 0.357257 -0.186299 0.757499 0.268 Uiso 1 1 calc R U . . .
H18B H 0.307534 -0.150234 0.714526 0.268 Uiso 1 1 calc R U . . .
H18C H 0.342432 -0.186461 0.644221 0.268 Uiso 1 1 calc R U . . .
C19 C 0.3989(12) -0.047(3) 0.775(3) 0.36(2) Uani 1 1 d D U . . .
H19A H 0.404211 -0.101569 0.814301 0.536 Uiso 1 1 calc R U . . .
H19B H 0.426454 -0.032898 0.744780 0.536 Uiso 1 1 calc R U . . .
H19C H 0.392132 0.004456 0.815735 0.536 Uiso 1 1 calc R U . . .
O9 O 0.3473(3) 0.2664(6) 0.7009(5) 0.078(3) Uani 0.5 1 d D . P A 1
C20 C 0.3387(9) 0.2426(18) 0.7836(10) 0.083(7) Uani 0.5 1 d D U P A 1
H20 H 0.327998 0.182148 0.788793 0.099 Uiso 0.5 1 calc R U P A 1
O10 O 0.3426(10) 0.2896(18) 0.8609(16) 0.135(8) Uani 0.5 1 d D U P A 1
O9A O 0.3473(3) 0.2664(6) 0.7009(5) 0.078(3) Uani 0.5 1 d . . P A 2
O11 O 0.3631(12) 0.372(3) 0.874(2) 0.189(13) Uiso 0.5 1 d . . P B 2
O12 O 0.5488(12) 0.001(2) 0.973(2) 0.187(12) Uiso 0.5 1 d . . P . .
O13 O 0.500000 0.235(4) 0.750000 0.24(3) Uiso 0.5 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O4 2.378(5) 6_566 ?
Sm1 O1 2.398(5) . ?
Sm1 O2 2.421(5) 7_556 ?
Sm1 O8 2.435(7) . ?
Sm1 O6 2.463(5) 2_655 ?
Sm1 O9A 2.465(7) . ?
Sm1 O9 2.465(7) . ?
Sm1 O3 2.482(5) 4_545 ?
Sm1 O7 2.518(5) 2_655 ?
Sm1 O4 2.687(5) 4_545 ?
Sm1 C16 2.846(7) 2_655 ?
Sm1 C8 2.954(8) 4_545 ?
O1 C7 1.247(9) . ?
O2 C7 1.255(9) . ?
O3 C8 1.250(9) . ?
O4 C8 1.261(8) . ?
O5 C10 1.368(9) . ?
O5 C9 1.407(10) . ?
O6 C16 1.268(10) . ?
O7 C16 1.232(10) . ?
C1 C2 1.373(10) . ?
C1 C6 1.392(10) . ?
C1 C7 1.516(9) . ?
C2 C3 1.391(10) . ?
C3 C4 1.372(10) . ?
C3 C8 1.496(10) . ?
C4 C5 1.401(10) . ?
C5 C6 1.379(10) . ?
C5 C9 1.505(10) . ?
C10 C15 1.373(12) . ?
C10 C11 1.378(14) . ?
C11 C12 1.405(14) . ?
C12 C13 1.368(13) . ?
C13 C14 1.383(12) . ?
C13 C16 1.495(10) . ?
C14 C15 1.375(11) . ?
O8 C17 1.229(9) . ?
C17 N1 1.302(18) . ?
N1 C18 1.431(9) . ?
N1 C19 1.496(18) . ?
O9 C20 1.243(10) . ?
C20 O10 1.257(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Sm1 O1 73.47(17) 6_566 . ?
O4 Sm1 O2 78.78(18) 6_566 7_556 ?
O1 Sm1 O2 133.12(18) . 7_556 ?
O4 Sm1 O8 144.4(2) 6_566 . ?
O1 Sm1 O8 142.0(2) . . ?
O2 Sm1 O8 71.6(2) 7_556 . ?
O4 Sm1 O6 136.41(18) 6_566 2_655 ?
O1 Sm1 O6 78.0(2) . 2_655 ?
O2 Sm1 O6 143.1(2) 7_556 2_655 ?
O8 Sm1 O6 71.6(2) . 2_655 ?
O4 Sm1 O9A 78.6(3) 6_566 . ?
O1 Sm1 O9A 134.6(2) . . ?
O2 Sm1 O9A 72.8(2) 7_556 . ?
O8 Sm1 O9A 74.1(3) . . ?
O6 Sm1 O9A 99.9(3) 2_655 . ?
O4 Sm1 O9 78.6(3) 6_566 . ?
O1 Sm1 O9 134.6(2) . . ?
O2 Sm1 O9 72.8(2) 7_556 . ?
O8 Sm1 O9 74.1(3) . . ?
O6 Sm1 O9 99.9(3) 2_655 . ?
O4 Sm1 O3 122.86(18) 6_566 4_545 ?
O1 Sm1 O3 77.63(19) . 4_545 ?
O2 Sm1 O3 87.1(2) 7_556 4_545 ?
O8 Sm1 O3 75.5(3) . 4_545 ?
O6 Sm1 O3 80.94(19) 2_655 4_545 ?
O9 Sm1 O3 147.6(2) . 4_545 ?
O4 Sm1 O7 87.52(19) 6_566 2_655 ?
O1 Sm1 O7 71.4(2) . 2_655 ?
O2 Sm1 O7 144.3(2) 7_556 2_655 ?
O8 Sm1 O7 105.2(3) . 2_655 ?
O6 Sm1 O7 52.00(19) 2_655 2_655 ?
O9 Sm1 O7 72.3(2) . 2_655 ?
O3 Sm1 O7 127.39(18) 4_545 2_655 ?
O4 Sm1 O4 73.91(17) 6_566 4_545 ?
O1 Sm1 O4 69.69(17) . 4_545 ?
O2 Sm1 O4 66.67(17) 7_556 4_545 ?
O8 Sm1 O4 110.4(2) . 4_545 ?
O6 Sm1 O4 125.05(19) 2_655 4_545 ?
O9 Sm1 O4 134.4(2) . 4_545 ?
O3 Sm1 O4 49.94(16) 4_545 4_545 ?
O7 Sm1 O4 140.2(2) 2_655 4_545 ?
O4 Sm1 C16 111.5(2) 6_566 2_655 ?
O1 Sm1 C16 71.8(2) . 2_655 ?
O2 Sm1 C16 154.8(2) 7_556 2_655 ?
O8 Sm1 C16 89.4(2) . 2_655 ?
O6 Sm1 C16 26.4(2) 2_655 2_655 ?
O9A Sm1 C16 86.5(3) . 2_655 ?
O9 Sm1 C16 86.5(3) . 2_655 ?
O3 Sm1 C16 104.4(2) 4_545 2_655 ?
O7 Sm1 C16 25.6(2) 2_655 2_655 ?
O4 Sm1 C16 137.4(2) 4_545 2_655 ?
O4 Sm1 C8 98.81(19) 6_566 4_545 ?
O1 Sm1 C8 72.5(2) . 4_545 ?
O2 Sm1 C8 75.4(2) 7_556 4_545 ?
O8 Sm1 C8 92.5(3) . 4_545 ?
O6 Sm1 C8 103.3(2) 2_655 4_545 ?
O9 Sm1 C8 148.0(2) . 4_545 ?
O3 Sm1 C8 24.68(18) 4_545 4_545 ?
O7 Sm1 C8 139.8(2) 2_655 4_545 ?
O4 Sm1 C8 25.27(17) 4_545 4_545 ?
C16 Sm1 C8 123.1(2) 2_655 4_545 ?
C7 O1 Sm1 136.7(5) . . ?
C7 O2 Sm1 136.2(5) . 7_556 ?
C8 O3 Sm1 99.3(4) . 4 ?
C8 O4 Sm1 161.6(5) . 6_565 ?
C8 O4 Sm1 89.3(5) . 4 ?
Sm1 O4 Sm1 106.09(17) 6_565 4 ?
C10 O5 C9 118.2(7) . . ?
C16 O6 Sm1 93.9(4) . 2_655 ?
C16 O7 Sm1 92.2(5) . 2_655 ?
C2 C1 C6 119.1(6) . . ?
C2 C1 C7 120.9(6) . . ?
C6 C1 C7 120.0(7) . . ?
C1 C2 C3 120.8(7) . . ?
C4 C3 C2 119.5(7) . . ?
C4 C3 C8 120.3(6) . . ?
C2 C3 C8 120.3(6) . . ?
C3 C4 C5 120.9(7) . . ?
C6 C5 C4 118.5(7) . . ?
C6 C5 C9 122.3(7) . . ?
C4 C5 C9 119.3(7) . . ?
C5 C6 C1 121.3(7) . . ?
O1 C7 O2 126.2(7) . . ?
O1 C7 C1 117.7(6) . . ?
O2 C7 C1 116.1(7) . . ?
O3 C8 O4 121.4(7) . . ?
O3 C8 C3 120.2(6) . . ?
O4 C8 C3 118.4(7) . . ?
O3 C8 Sm1 56.0(4) . 4 ?
O4 C8 Sm1 65.4(4) . 4 ?
C3 C8 Sm1 174.3(5) . 4 ?
O5 C9 C5 108.4(7) . . ?
O5 C10 C15 125.5(8) . . ?
O5 C10 C11 114.6(8) . . ?
C15 C10 C11 119.9(8) . . ?
C10 C11 C12 118.9(10) . . ?
C13 C12 C11 121.6(10) . . ?
C12 C13 C14 117.8(8) . . ?
C12 C13 C16 121.2(8) . . ?
C14 C13 C16 121.0(7) . . ?
C15 C14 C13 121.7(8) . . ?
C10 C15 C14 119.9(8) . . ?
O7 C16 O6 121.7(7) . . ?
O7 C16 C13 120.0(7) . . ?
O6 C16 C13 118.3(7) . . ?
O7 C16 Sm1 62.2(4) . 2_655 ?
O6 C16 Sm1 59.7(4) . 2_655 ?
C13 C16 Sm1 174.8(6) . 2_655 ?
C17 O8 Sm1 130.2(10) . . ?
O8 C17 N1 125.6(16) . . ?
C17 N1 C18 122.5(17) . . ?
C17 N1 C19 126(2) . . ?
C18 N1 C19 111(2) . . ?
C20 O9 Sm1 131.5(12) . . ?
O9 C20 O10 128(2) . . ?

_refine_diff_density_max         1.237
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.165

####################################################################### 
# 
# 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_2R-Ce-RT2
_database_code_depnum_ccdc_archive 'CCDC 1574645'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT043_2R-Ce-RT2           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      6.10 Check
RESPONSE:6 H atoms should be attached to severely disordered O atoms 
of water or formic acid, for which the disorder could not eliminated 
although we have applied several restaints to limit it. Thus,these H atoms 
were omitted due to refinement instability and disordered solvent.
;
_vrf_PLAT220_2R-Ce-RT2           
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         7.4 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the Ce centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_2R-Ce-RT2           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O14 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;
_vrf_PLAT601_2R-Ce-RT2           
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        101 Ang**3
RESPONSE: The existance of the voids containing loosely bound water
solvent is typical for MOF structures.

# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.548  0.250       101         8 ' '
   2  0.043  0.880  0.142        14         1 ' '
   3  0.500  0.048  0.250       101         8 ' '
   4  0.543  0.380  0.142        14         1 ' '
   5  0.261  0.860  0.193        14         1 ' '
   6  0.761  0.360  0.193        14         1 ' '
   7  0.239  0.360  0.307        14         1 ' '
   8  0.739  0.860  0.307        14         1 ' '
   9  0.457  0.380  0.357        14         0 ' '
  10  0.957  0.880  0.357        14         0 ' '
  11  0.043  0.121  0.642        14         0 ' '
  12  0.000  0.452  0.750       100         8 ' '
  13  0.543  0.621  0.642        14         0 ' '
  14  0.500  0.952  0.750       100         8 ' '
  15  0.261  0.140  0.693        14         1 ' '
  16  0.761  0.640  0.693        14         1 ' '
  17  0.239  0.640  0.807        14         1 ' '
  18  0.739  0.140  0.807        14         1 ' '
  19  0.457  0.620  0.857        14         0 ' '
  20  0.957  0.120  0.857        14         0 ' ' 
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[Ce(C16H9O7)(C3H7ON)(H2O)0.35(CHOOH)0.65]??2.35H2O'
_chemical_formula_sum            'C19.65 H22.70 Ce N O12'
_chemical_formula_weight         605.01

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'
N N 0.0061 0.0033 '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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.477(4)
_cell_length_b                   14.5281(18)
_cell_length_c                   13.6564(17)
_cell_angle_alpha                90
_cell_angle_beta                 100.456(3)
_cell_angle_gamma                90
_cell_volume                     5556.1(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      26.41

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             2413
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.692
_shelx_estimated_absorpt_T_min   0.667
_shelx_estimated_absorpt_T_max   0.687
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35177
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.798
_diffrn_reflns_theta_max         26.456
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5699
_reflns_number_gt                4629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0756P)²+52.8629P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5699
_refine_ls_number_parameters     305
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1437
_refine_ls_wR_factor_gt          0.1344
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.17976(2) 0.28841(2) 0.94916(2) 0.02017(13) Uani 1 1 d . . . . .
O1 O 0.23512(15) 0.3418(3) 0.8415(3) 0.0395(12) Uani 1 1 d . . . . .
O2 O 0.30710(16) 0.2784(3) 0.8816(3) 0.0343(10) Uani 1 1 d . . . . .
O3 O 0.20395(15) 0.5714(3) 0.5625(4) 0.0383(11) Uani 1 1 d . . . . .
O4 O 0.26569(14) 0.6568(3) 0.5499(3) 0.0268(9) Uani 1 1 d . . . . .
O5 O 0.42097(17) 0.3558(3) 0.6421(5) 0.0587(16) Uani 1 1 d . . . . .
O6 O 0.61172(16) 0.3252(3) 0.4638(4) 0.0414(12) Uani 1 1 d . . . . .
O7 O 0.59954(16) 0.1801(3) 0.4969(4) 0.0443(12) Uani 1 1 d . . . . .
C1 C 0.2952(2) 0.3939(4) 0.7578(4) 0.0266(12) Uani 1 1 d . . . . .
C2 C 0.2640(2) 0.4551(4) 0.7004(4) 0.0271(12) Uani 1 1 d . . . . .
H2 H 0.231839 0.455086 0.705286 0.033 Uiso 1 1 calc R U . . .
C3 C 0.2805(2) 0.5161(4) 0.6361(4) 0.0247(12) Uani 1 1 d . . . . .
C4 C 0.3285(2) 0.5129(4) 0.6270(4) 0.0260(12) Uani 1 1 d . . . . .
H4 H 0.339840 0.553787 0.584383 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3593(2) 0.4505(4) 0.6798(5) 0.0281(13) Uani 1 1 d . . . . .
C6 C 0.3432(2) 0.3924(4) 0.7471(5) 0.0276(13) Uani 1 1 d . . . . .
H6 H 0.364396 0.352153 0.785467 0.033 Uiso 1 1 calc R U . . .
C7 C 0.2780(2) 0.3325(4) 0.8339(4) 0.0284(13) Uani 1 1 d . . . . .
C8 C 0.2478(2) 0.5853(4) 0.5801(4) 0.0242(12) Uani 1 1 d . . . . .
C9 C 0.4106(2) 0.4483(5) 0.6669(5) 0.0366(15) Uani 1 1 d . . . . .
H9A H 0.415429 0.489951 0.614069 0.044 Uiso 1 1 calc R U . . .
H9B H 0.431357 0.467030 0.727974 0.044 Uiso 1 1 calc R U . . .
C10 C 0.4626(3) 0.3394(5) 0.6086(6) 0.0469(19) Uani 1 1 d . . . . .
C11 C 0.4714(3) 0.2500(6) 0.5890(9) 0.069(3) Uani 1 1 d . U . . .
H11 H 0.449831 0.204958 0.600688 0.083 Uiso 1 1 calc R U . . .
C12 C 0.5117(3) 0.2244(6) 0.5521(8) 0.060(2) Uani 1 1 d . U . . .
H12 H 0.516711 0.162894 0.538057 0.073 Uiso 1 1 calc R U . . .
C13 C 0.5443(2) 0.2905(4) 0.5363(5) 0.0349(15) Uani 1 1 d . . . . .
C14 C 0.5358(2) 0.3800(5) 0.5580(5) 0.0366(15) Uani 1 1 d . . . . .
H14 H 0.557656 0.425130 0.548103 0.044 Uiso 1 1 calc R U . . .
C15 C 0.4952(2) 0.4049(5) 0.5948(6) 0.0404(16) Uani 1 1 d . . . . .
H15 H 0.490265 0.466109 0.609899 0.048 Uiso 1 1 calc R U . . .
C16 C 0.5877(2) 0.2640(5) 0.4961(5) 0.0328(14) Uani 1 1 d . . . . .
O8 O 0.1523(2) 0.2227(4) 0.7773(4) 0.0552(15) Uani 1 1 d . . . . .
C17 C 0.1637(4) 0.2473(9) 0.6988(8) 0.088(3) Uani 1 1 d . U . . .
H17 H 0.172831 0.308425 0.694818 0.105 Uiso 1 1 calc R U . . .
N1 N 0.1642(4) 0.1955(8) 0.6195(6) 0.094(3) Uani 1 1 d . U . . .
C18 C 0.1787(8) 0.2341(16) 0.5323(13) 0.177(8) Uani 1 1 d . U . . .
H18A H 0.173647 0.299429 0.531130 0.266 Uiso 1 1 calc R U . . .
H18B H 0.160203 0.207000 0.473611 0.266 Uiso 1 1 calc R U . . .
H18C H 0.211968 0.221522 0.534080 0.266 Uiso 1 1 calc R U . . .
C19 C 0.1458(7) 0.1060(12) 0.6131(11) 0.149(6) Uani 1 1 d . U . . .
H19A H 0.168103 0.065135 0.590384 0.224 Uiso 1 1 calc R U . . .
H19B H 0.116085 0.104850 0.566951 0.224 Uiso 1 1 calc R U . . .
H19C H 0.140721 0.086597 0.677508 0.224 Uiso 1 1 calc R U . . .
O9 O 0.1425(2) 0.4210(4) 0.8515(5) 0.0687(18) Uani 0.65 1 d D . P A 1
C20 C 0.1527(5) 0.5024(7) 0.8398(10) 0.075(4) Uani 0.65 1 d D U P A 1
H20 H 0.180384 0.522541 0.880981 0.089 Uiso 0.65 1 calc R U P A 1
O10 O 0.1317(4) 0.5627(7) 0.7812(7) 0.081(3) Uani 0.65 1 d D U P A 1
O9A O 0.1425(2) 0.4210(4) 0.8515(5) 0.0687(18) Uani 0.35 1 d . . P A 2
O11 O 0.1393(8) 0.6453(17) 0.7628(17) 0.095(7) Uiso 0.35 1 d . . P B 2
O12 O 0.5445(5) 0.0066(9) 0.4561(9) 0.163(4) Uiso 1 1 d . . . . .
O13 O 0.1358(8) 0.4286(15) 0.5685(16) 0.133(7) Uiso 0.5 1 d . . P . .
O14 O 0.500000 0.2486(15) 0.250000 0.182(7) Uiso 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O4 2.462(4) 4_546 ?
Ce1 O1 2.468(4) . ?
Ce1 O9A 2.471(5) . ?
Ce1 O9 2.471(5) . ?
Ce1 O2 2.472(4) 7_557 ?
Ce1 O8 2.522(5) . ?
Ce1 O7 2.529(4) 8_456 ?
Ce1 O3 2.575(4) 6_566 ?
Ce1 O6 2.581(4) 8_456 ?
Ce1 O4 2.700(4) 6_566 ?
Ce1 C16 2.912(6) 8_456 ?
Ce1 C8 3.011(6) 6_566 ?
O1 C7 1.251(7) . ?
O2 C7 1.239(8) . ?
O3 C8 1.246(7) . ?
O4 C8 1.259(7) . ?
O5 C10 1.367(7) . ?
O5 C9 1.430(8) . ?
O6 C16 1.251(8) . ?
O7 C16 1.264(8) . ?
C1 C2 1.393(8) . ?
C1 C6 1.402(8) . ?
C1 C7 1.516(8) . ?
C2 C3 1.388(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.397(8) . ?
C3 C8 1.483(8) . ?
C4 C5 1.371(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(8) . ?
C5 C9 1.502(8) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.358(12) . ?
C10 C15 1.367(10) . ?
C11 C12 1.386(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.381(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.365(9) . ?
C13 C16 1.490(8) . ?
C14 C15 1.389(8) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O8 C17 1.228(12) . ?
C17 N1 1.322(14) . ?
C17 H17 0.9300 . ?
N1 C19 1.398(18) . ?
N1 C18 1.443(18) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O9 C20 1.234(9) . ?
C20 O10 1.261(9) . ?
C20 H20 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ce1 O1 77.10(15) 4_546 . ?
O4 Ce1 O9A 144.83(17) 4_546 . ?
O1 Ce1 O9A 72.03(18) . . ?
O4 Ce1 O9 144.83(17) 4_546 . ?
O1 Ce1 O9 72.03(18) . . ?
O4 Ce1 O2 72.65(14) 4_546 7_557 ?
O1 Ce1 O2 132.52(15) . 7_557 ?
O9 Ce1 O2 142.02(18) . 7_557 ?
O4 Ce1 O8 78.47(17) 4_546 . ?
O1 Ce1 O8 71.84(17) . . ?
O9A Ce1 O8 76.3(2) . . ?
O9 Ce1 O8 76.3(2) . . ?
O2 Ce1 O8 133.65(17) 7_557 . ?
O4 Ce1 O7 137.55(14) 4_546 8_456 ?
O1 Ce1 O7 143.27(16) . 8_456 ?
O9 Ce1 O7 71.24(18) . 8_456 ?
O2 Ce1 O7 79.65(16) 7_557 8_456 ?
O8 Ce1 O7 99.58(19) . 8_456 ?
O4 Ce1 O3 120.74(13) 4_546 6_566 ?
O1 Ce1 O3 88.81(16) . 6_566 ?
O9 Ce1 O3 75.5(2) . 6_566 ?
O2 Ce1 O3 76.69(16) 7_557 6_566 ?
O8 Ce1 O3 149.57(17) . 6_566 ?
O7 Ce1 O3 81.80(15) 8_456 6_566 ?
O4 Ce1 O6 89.13(14) 4_546 8_456 ?
O1 Ce1 O6 144.78(16) . 8_456 ?
O9 Ce1 O6 106.6(2) . 8_456 ?
O2 Ce1 O6 70.43(16) 7_557 8_456 ?
O8 Ce1 O6 73.72(17) . 8_456 ?
O7 Ce1 O6 50.93(15) 8_456 8_456 ?
O3 Ce1 O6 125.60(14) 6_566 8_456 ?
O4 Ce1 O4 73.34(14) 4_546 6_566 ?
O1 Ce1 O4 65.98(14) . 6_566 ?
O9 Ce1 O4 107.83(19) . 6_566 ?
O2 Ce1 O4 70.73(14) 7_557 6_566 ?
O8 Ce1 O4 133.20(16) . 6_566 ?
O7 Ce1 O4 126.36(15) 8_456 6_566 ?
O3 Ce1 O4 48.86(12) 6_566 6_566 ?
O6 Ce1 O4 140.62(15) 8_456 6_566 ?
O4 Ce1 C16 112.86(16) 4_546 8_456 ?
O1 Ce1 C16 155.73(17) . 8_456 ?
O9A Ce1 C16 90.4(2) . 8_456 ?
O9 Ce1 C16 90.4(2) . 8_456 ?
O2 Ce1 C16 71.40(17) 7_557 8_456 ?
O8 Ce1 C16 88.07(19) . 8_456 ?
O7 Ce1 C16 25.66(17) 8_456 8_456 ?
O3 Ce1 C16 103.17(16) 6_566 8_456 ?
O6 Ce1 C16 25.43(17) 8_456 8_456 ?
O4 Ce1 C16 137.24(16) 6_566 8_456 ?
O4 Ce1 C8 97.61(14) 4_546 6_566 ?
O1 Ce1 C8 75.52(16) . 6_566 ?
O9 Ce1 C8 90.7(2) . 6_566 ?
O2 Ce1 C8 73.27(16) 7_557 6_566 ?
O8 Ce1 C8 147.19(16) . 6_566 ?
O7 Ce1 C8 104.53(16) 8_456 6_566 ?
O3 Ce1 C8 24.19(14) 6_566 6_566 ?
O6 Ce1 C8 139.08(15) 8_456 6_566 ?
O4 Ce1 C8 24.72(13) 6_566 6_566 ?
C16 Ce1 C8 122.50(17) 8_456 6_566 ?
C7 O1 Ce1 138.9(4) . . ?
C7 O2 Ce1 135.6(4) . 7_557 ?
C8 O3 Ce1 97.9(3) . 6_565 ?
C8 O4 Ce1 158.6(4) . 4_556 ?
C8 O4 Ce1 91.6(3) . 6_565 ?
Ce1 O4 Ce1 106.66(13) 4_556 6_565 ?
C10 O5 C9 118.2(5) . . ?
C16 O6 Ce1 92.2(4) . 8 ?
C16 O7 Ce1 94.3(4) . 8 ?
C2 C1 C6 119.1(5) . . ?
C2 C1 C7 120.6(5) . . ?
C6 C1 C7 120.3(5) . . ?
C3 C2 C1 120.6(5) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 C8 120.5(5) . . ?
C4 C3 C8 120.6(5) . . ?
C5 C4 C3 121.3(5) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 119.6(5) . . ?
C4 C5 C9 119.6(5) . . ?
C6 C5 C9 120.7(5) . . ?
C5 C6 C1 120.4(5) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O2 C7 O1 126.5(5) . . ?
O2 C7 C1 117.7(5) . . ?
O1 C7 C1 115.8(5) . . ?
O3 C8 O4 121.4(5) . . ?
O3 C8 C3 120.2(5) . . ?
O4 C8 C3 118.4(5) . . ?
O3 C8 Ce1 57.9(3) . 6_565 ?
O4 C8 Ce1 63.7(3) . 6_565 ?
C3 C8 Ce1 174.1(4) . 6_565 ?
O5 C9 C5 107.2(5) . . ?
O5 C9 H9A 110.3 . . ?
C5 C9 H9A 110.3 . . ?
O5 C9 H9B 110.3 . . ?
C5 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
C11 C10 O5 115.8(7) . . ?
C11 C10 C15 119.0(6) . . ?
O5 C10 C15 125.3(6) . . ?
C10 C11 C12 121.5(8) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C13 C12 C11 119.7(8) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 118.5(6) . . ?
C14 C13 C16 121.2(6) . . ?
C12 C13 C16 120.3(6) . . ?
C13 C14 C15 121.2(6) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C10 C15 C14 120.0(6) . . ?
C10 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
O6 C16 O7 121.7(6) . . ?
O6 C16 C13 119.3(6) . . ?
O7 C16 C13 118.9(6) . . ?
O6 C16 Ce1 62.3(3) . 8 ?
O7 C16 Ce1 60.0(3) . 8 ?
C13 C16 Ce1 171.2(5) . 8 ?
C17 O8 Ce1 128.0(6) . . ?
O8 C17 N1 126.5(12) . . ?
O8 C17 H17 116.8 . . ?
N1 C17 H17 116.8 . . ?
C17 N1 C19 121.4(12) . . ?
C17 N1 C18 120.2(14) . . ?
C19 N1 C18 118.0(13) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Ce1 136.8(8) . . ?
O9 C20 O10 130.7(13) . . ?
O9 C20 H20 114.6 . . ?
O10 C20 H20 114.6 . . ?

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
C6 C1 C2 C3 -2.2(9) . . . . ?
C7 C1 C2 C3 175.1(6) . . . . ?
C1 C2 C3 C4 2.3(9) . . . . ?
C1 C2 C3 C8 -176.0(6) . . . . ?
C2 C3 C4 C5 0.4(9) . . . . ?
C8 C3 C4 C5 178.7(6) . . . . ?
C3 C4 C5 C6 -3.1(10) . . . . ?
C3 C4 C5 C9 179.1(6) . . . . ?
C4 C5 C6 C1 3.2(10) . . . . ?
C9 C5 C6 C1 -179.1(6) . . . . ?
C2 C1 C6 C5 -0.6(9) . . . . ?
C7 C1 C6 C5 -177.9(6) . . . . ?
Ce1 O2 C7 O1 -32.3(10) 7_557 . . . ?
Ce1 O2 C7 C1 148.2(4) 7_557 . . . ?
Ce1 O1 C7 O2 8.3(11) . . . . ?
Ce1 O1 C7 C1 -172.2(4) . . . . ?
C2 C1 C7 O2 178.9(6) . . . . ?
C6 C1 C7 O2 -3.8(9) . . . . ?
C2 C1 C7 O1 -0.7(9) . . . . ?
C6 C1 C7 O1 176.6(6) . . . . ?
Ce1 O3 C8 O4 5.4(6) 6_565 . . . ?
Ce1 O3 C8 C3 -173.5(5) 6_565 . . . ?
Ce1 O4 C8 O3 144.0(8) 4_556 . . . ?
Ce1 O4 C8 O3 -5.1(6) 6_565 . . . ?
Ce1 O4 C8 C3 -37.1(13) 4_556 . . . ?
Ce1 O4 C8 C3 173.8(5) 6_565 . . . ?
Ce1 O4 C8 Ce1 149.0(10) 4_556 . . 6_565 ?
C2 C3 C8 O3 -24.4(9) . . . . ?
C4 C3 C8 O3 157.3(6) . . . . ?
C2 C3 C8 O4 156.7(6) . . . . ?
C4 C3 C8 O4 -21.7(8) . . . . ?
C10 O5 C9 C5 168.1(7) . . . . ?
C4 C5 C9 O5 -126.2(6) . . . . ?
C6 C5 C9 O5 56.0(8) . . . . ?
C9 O5 C10 C11 178.1(8) . . . . ?
C9 O5 C10 C15 -1.3(12) . . . . ?
O5 C10 C11 C12 178.2(10) . . . . ?
C15 C10 C11 C12 -2.3(15) . . . . ?
C10 C11 C12 C13 1.2(16) . . . . ?
C11 C12 C13 C14 0.2(14) . . . . ?
C11 C12 C13 C16 -179.6(9) . . . . ?
C12 C13 C14 C15 -0.4(12) . . . . ?
C16 C13 C14 C15 179.4(7) . . . . ?
C11 C10 C15 C14 2.1(13) . . . . ?
O5 C10 C15 C14 -178.5(8) . . . . ?
C13 C14 C15 C10 -0.8(12) . . . . ?
Ce1 O6 C16 O7 -8.7(7) 8 . . . ?
Ce1 O6 C16 C13 170.2(6) 8 . . . ?
Ce1 O7 C16 O6 8.9(7) 8 . . . ?
Ce1 O7 C16 C13 -170.0(5) 8 . . . ?
C14 C13 C16 O6 -13.9(11) . . . . ?
C12 C13 C16 O6 165.9(8) . . . . ?
C14 C13 C16 O7 165.0(7) . . . . ?
C12 C13 C16 O7 -15.1(11) . . . . ?
Ce1 O8 C17 N1 152.9(10) . . . . ?
O8 C17 N1 C19 8(2) . . . . ?
O8 C17 N1 C18 -179.7(15) . . . . ?
Ce1 O9 C20 O10 174.2(10) . . . . ?

_refine_diff_density_max         1.711
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.170

####################################################################### 
# 
# 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_6-B-A6-Tb-15
_database_code_depnum_ccdc_archive 'CCDC 1574648'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_6-B-A6-Tb-15        
;
PROBLEM: Check Calcd Resid. Dens.  0.88A   From Tb1            -3.98 eA-3  
PROBLEM: Check Calcd Resid. Dens.  1.00A   From Tb1            -2.86 eA-3
RESPONSE: The deep residual density hole is very close to the heavy Tb
atom, which might be resulted from the disorder of the heavy Tb atom 
and could not be modelled properly.
;

_vrf_PLAT973_6-B-A6-Tb-15        
;
PROBLEM: Check Calcd Positive Resid. Density on       Tb1       2.51 eA-3  
RESPONSE: The deep residual density hole is very close to the heavy Tb1
atom, which might be resulted from the disorder of the heavy Tb1 atom 
and could not be modelled properly.
;
_vrf_PLAT029_6-B-A6-Tb-15        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.948 Why?
RESPONSE: This is caused by the limited data collection strategy on the 
synchrotron radiation facility
;

_vrf_PLAT306_6-B-A6-Tb-15        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Tb(C16H9O7)(C3H7ON)(CHOOH)]??H2O'
_chemical_formula_sum            'C20 H20 N O11 Tb'
_chemical_formula_weight         609.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1140 4.1650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.214(6)
_cell_length_b                   14.429(3)
_cell_length_c                   13.411(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.77(3)
_cell_angle_gamma                90
_cell_volume                     5363.5(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27014
_cell_measurement_theta_min      1.58
_cell_measurement_theta_max      30.95

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_F_000             2400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.660
_shelx_estimated_absorpt_T_min   0.691
_shelx_estimated_absorpt_T_max   0.777
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.710
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5268
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.615
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_full        25.214
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_point_group_measured_fraction_full 0.948
_reflns_number_total             5268
_reflns_number_gt                5109
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1892P)²+18.2264P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0195(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5268
_refine_ls_number_parameters     320
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.2259
_refine_ls_wR_factor_gt          0.2235
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.002
_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 0.31877(2) 0.71218(2) 0.04889(2) 0.0344(3) Uani 1 1 d . . . . .
O1 O 0.26643(16) 0.6552(3) 0.1534(3) 0.0413(9) Uani 1 1 d . . . . .
O2 O 0.1943(2) 0.7254(3) 0.1164(4) 0.0416(11) Uani 1 1 d . . . . .
O3 O 0.29631(16) 0.4255(3) 0.4450(4) 0.0438(10) Uani 1 1 d . . . . .
O4 O 0.23334(15) 0.3382(3) 0.4496(3) 0.0366(9) Uani 1 1 d . . . . .
O5 O 0.07761(19) 0.6490(3) 0.3544(5) 0.0573(13) Uani 1 1 d . U . . .
O6 O -0.10581(16) 0.8226(3) 0.4937(4) 0.0441(10) Uani 1 1 d . . . . .
O7 O -0.11492(17) 0.6767(3) 0.5367(4) 0.0473(11) Uani 1 1 d . . . . .
C1 C 0.2057(2) 0.6063(4) 0.2406(5) 0.0374(11) Uani 1 1 d . . . . .
C2 C 0.2367(2) 0.5431(4) 0.2975(5) 0.0395(12) Uani 1 1 d . . . . .
H2 H 0.269687 0.540819 0.291247 0.047 Uiso 1 1 calc R U . . .
C3 C 0.2194(2) 0.4829(4) 0.3637(4) 0.0373(11) Uani 1 1 d . . . . .
C4 C 0.1709(2) 0.4872(4) 0.3750(5) 0.0386(12) Uani 1 1 d . . . . .
H4 H 0.159144 0.445530 0.419497 0.046 Uiso 1 1 calc R U . . .
C5 C 0.1406(2) 0.5518(4) 0.3215(5) 0.0399(13) Uani 1 1 d . . . . .
C6 C 0.1574(2) 0.6107(4) 0.2525(4) 0.0389(12) Uani 1 1 d . . . . .
H6 H 0.136025 0.653620 0.213687 0.047 Uiso 1 1 calc R U . . .
C7 C 0.2237(2) 0.6678(4) 0.1641(4) 0.0371(11) Uani 1 1 d . . . . .
C8 C 0.2522(2) 0.4115(4) 0.4222(5) 0.0390(12) Uani 1 1 d . . . . .
C9 C 0.0884(2) 0.5548(4) 0.3336(5) 0.0433(13) Uani 1 1 d . . . . .
H9A H 0.067175 0.533237 0.270666 0.052 Uiso 1 1 calc R U . . .
H9B H 0.083448 0.514145 0.390249 0.052 Uiso 1 1 calc R U . . .
C10 C 0.0350(3) 0.6647(5) 0.3861(6) 0.0495(16) Uani 1 1 d . U . . .
C11 C 0.0249(3) 0.7577(7) 0.4010(10) 0.071(3) Uani 1 1 d . U . . .
H11 H 0.045714 0.804904 0.384828 0.085 Uiso 1 1 calc R U . . .
C12 C -0.0161(4) 0.7807(5) 0.4399(9) 0.065(2) Uani 1 1 d . U . . .
H12 H -0.022210 0.843865 0.452927 0.078 Uiso 1 1 calc R U . . .
C13 C -0.0482(3) 0.7130(4) 0.4601(6) 0.0440(16) Uani 1 1 d . . . . .
C14 C -0.0379(2) 0.6220(4) 0.4410(5) 0.0426(13) Uani 1 1 d . . . . .
H14 H -0.059925 0.575128 0.452480 0.051 Uiso 1 1 calc R U . . .
C15 C 0.0032(2) 0.5962(4) 0.4058(5) 0.0451(13) Uani 1 1 d . . . . .
H15 H 0.009664 0.532719 0.395222 0.054 Uiso 1 1 calc R U . . .
C16 C -0.0919(2) 0.7388(5) 0.5002(5) 0.0402(12) Uani 1 1 d . . . . .
O8 O 0.3453(3) 0.7782(4) 0.2148(6) 0.0608(17) Uani 0.5 1 d . U P A 1
C17 C 0.3355(4) 0.7505(9) 0.2964(8) 0.081(3) Uani 0.5 1 d . U P A 1
H17 H 0.324375 0.688432 0.297858 0.097 Uiso 0.5 1 calc R U P A 1
N1 N 0.3391(5) 0.7985(9) 0.3811(10) 0.118(4) Uani 0.5 1 d . U P A 1
C18 C 0.3575(7) 0.8929(10) 0.3910(10) 0.062(4) Uani 0.5 1 d . U P A 1
H18A H 0.392831 0.891559 0.407191 0.094 Uiso 0.5 1 calc R U P A 1
H18B H 0.345101 0.924554 0.445424 0.094 Uiso 0.5 1 calc R U P A 1
H18C H 0.346966 0.926058 0.326900 0.094 Uiso 0.5 1 calc R U P A 1
C19 C 0.3288(9) 0.760(2) 0.4817(17) 0.081(5) Uani 0.5 1 d . U P A 1
H19A H 0.299289 0.787578 0.496479 0.122 Uiso 0.5 1 calc R U P A 1
H19B H 0.355937 0.773961 0.536587 0.122 Uiso 0.5 1 calc R U P A 1
H19C H 0.324746 0.692147 0.475998 0.122 Uiso 0.5 1 calc R U P A 1
O9 O 0.3586(2) 0.5920(4) 0.1534(6) 0.0695(16) Uani 0.5 1 d . U P A 1
N2 N 0.3703(4) 0.4544(7) 0.2352(8) 0.102(3) Uani 0.5 1 d . U P A 1
C20 C 0.3491(4) 0.5116(6) 0.1585(7) 0.067(2) Uani 0.5 1 d . U P A 1
H20 H 0.325464 0.485921 0.106078 0.080 Uiso 0.5 1 calc R U P A 1
C21 C 0.3975(7) 0.4980(13) 0.3308(15) 0.073(4) Uani 0.5 1 d . U P A 1
H21A H 0.431692 0.481673 0.339464 0.109 Uiso 0.5 1 calc R U P A 1
H21B H 0.384436 0.475239 0.389102 0.109 Uiso 0.5 1 calc R U P A 1
H21C H 0.393910 0.565527 0.326344 0.109 Uiso 0.5 1 calc R U P A 1
C22 C 0.3574(7) 0.3592(8) 0.2365(9) 0.053(3) Uani 0.5 1 d . U P A 1
H22A H 0.322977 0.352102 0.208104 0.079 Uiso 0.5 1 calc R U P A 1
H22B H 0.363926 0.336421 0.306617 0.079 Uiso 0.5 1 calc R U P A 1
H22C H 0.376376 0.323403 0.195834 0.079 Uiso 0.5 1 calc R U P A 1
O8A O 0.3453(3) 0.7782(4) 0.2148(6) 0.0608(17) Uani 0.5 1 d . . P A 2
C17A C 0.3355(4) 0.7505(9) 0.2964(8) 0.081(3) Uani 0.5 1 d . U P A 2
H17A H 0.324375 0.688432 0.297858 0.097 Uiso 0.5 1 calc R U P A 2
O10A O 0.3391(5) 0.7985(9) 0.3811(10) 0.118(4) Uani 0.5 1 d . . P A 2
O9A O 0.3586(2) 0.5920(4) 0.1534(6) 0.0695(16) Uani 0.5 1 d . . P A 2
C20A C 0.3491(4) 0.5116(6) 0.1585(7) 0.067(2) Uani 0.5 1 d . . P A 2
H20A H 0.325464 0.485921 0.106078 0.080 Uiso 0.5 1 calc R U P A 2
O11A O 0.3703(4) 0.4544(7) 0.2352(8) 0.102(3) Uani 0.5 1 d . U P A 2
O12 O 0.0475(10) 0.008(2) 0.433(2) 0.160(9) Uiso 0.5 1 d . . P . .
O13 O 1.000000 0.7462(12) 0.750000 0.109(4) Uiso 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O4 2.341(4) 4 ?
Tb1 O2 2.357(6) 7_565 ?
Tb1 O1 2.365(4) . ?
Tb1 O9 2.376(6) . ?
Tb1 O9A 2.376(6) . ?
Tb1 O8A 2.408(7) . ?
Tb1 O8 2.408(7) . ?
Tb1 O6 2.432(4) 8_565 ?
Tb1 O3 2.442(4) 6_565 ?
Tb1 O7 2.493(4) 8_565 ?
Tb1 O4 2.629(4) 6_565 ?
Tb1 C16 2.808(6) 8_565 ?
O1 C7 1.255(7) . ?
O2 C7 1.260(8) . ?
O3 C8 1.242(8) . ?
O4 C8 1.269(7) . ?
O5 C10 1.365(7) . ?
O5 C9 1.432(7) . ?
O6 C16 1.269(9) . ?
O7 C16 1.258(8) . ?
C1 C2 1.389(9) . ?
C1 C6 1.403(8) . ?
C1 C7 1.513(7) . ?
C2 C3 1.393(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.407(8) . ?
C3 C8 1.503(8) . ?
C4 C5 1.373(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(8) . ?
C5 C9 1.512(8) . ?
C6 H6 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.393(9) . ?
C10 C11 1.395(13) . ?
C11 C12 1.395(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(8) . ?
C13 C16 1.482(9) . ?
C14 C15 1.382(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O8 C17 1.244(13) . ?
C17 N1 1.318(17) . ?
C17 H17 0.9500 . ?
N1 C18 1.455(19) . ?
N1 C19 1.54(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O9 C20 1.195(11) . ?
N2 C20 1.366(13) . ?
N2 C22 1.423(17) . ?
N2 C21 1.50(2) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
O8A C17A 1.244(13) . ?
C17A O10A 1.318(17) . ?
C17A H17A 0.9500 . ?
O9A C20A 1.195(11) . ?
C20A O11A 1.366(13) . ?
C20A H20A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb1 O2 73.92(16) 4 7_565 ?
O4 Tb1 O1 78.62(14) 4 . ?
O2 Tb1 O1 133.21(18) 7_565 . ?
O4 Tb1 O9 142.25(19) 4 . ?
O2 Tb1 O9 143.8(2) 7_565 . ?
O1 Tb1 O9 71.07(18) . . ?
O4 Tb1 O9A 142.25(19) 4 . ?
O2 Tb1 O9A 143.8(2) 7_565 . ?
O1 Tb1 O9A 71.07(18) . . ?
O4 Tb1 O8A 76.8(2) 4 . ?
O2 Tb1 O8A 133.2(2) 7_565 . ?
O1 Tb1 O8A 73.2(2) . . ?
O9A Tb1 O8A 73.3(2) . . ?
O4 Tb1 O8 76.8(2) 4 . ?
O2 Tb1 O8 133.2(2) 7_565 . ?
O1 Tb1 O8 73.2(2) . . ?
O9 Tb1 O8 73.3(2) . . ?
O4 Tb1 O6 138.54(15) 4 8_565 ?
O2 Tb1 O6 77.58(18) 7_565 8_565 ?
O1 Tb1 O6 141.90(16) . 8_565 ?
O9 Tb1 O6 71.61(19) . 8_565 ?
O8 Tb1 O6 102.9(2) . 8_565 ?
O4 Tb1 O3 122.72(15) 4 6_565 ?
O2 Tb1 O3 78.21(17) 7_565 6_565 ?
O1 Tb1 O3 86.04(15) . 6_565 ?
O9 Tb1 O3 77.7(2) . 6_565 ?
O8 Tb1 O3 148.46(18) . 6_565 ?
O6 Tb1 O3 78.87(15) 8_565 6_565 ?
O4 Tb1 O7 88.91(14) 4 8_565 ?
O2 Tb1 O7 71.33(19) 7_565 8_565 ?
O1 Tb1 O7 145.30(16) . 8_565 ?
O9 Tb1 O7 103.3(2) . 8_565 ?
O8 Tb1 O7 72.5(2) . 8_565 ?
O6 Tb1 O7 53.32(15) 8_565 8_565 ?
O3 Tb1 O7 127.15(15) 6_565 8_565 ?
O4 Tb1 O4 72.63(15) 4 6_565 ?
O2 Tb1 O4 70.25(16) 7_565 6_565 ?
O1 Tb1 O4 65.72(14) . 6_565 ?
O9 Tb1 O4 112.6(2) . 6_565 ?
O8 Tb1 O4 132.4(2) . 6_565 ?
O6 Tb1 O4 124.09(15) 8_565 6_565 ?
O3 Tb1 O4 50.97(14) 6_565 6_565 ?
O7 Tb1 O4 140.63(16) 8_565 6_565 ?
O4 Tb1 C16 113.48(17) 4 8_565 ?
O2 Tb1 C16 71.0(2) 7_565 8_565 ?
O1 Tb1 C16 155.75(18) . 8_565 ?
O9 Tb1 C16 88.6(2) . 8_565 ?
O9A Tb1 C16 88.6(2) . 8_565 ?
O8A Tb1 C16 88.7(2) . 8_565 ?
O8 Tb1 C16 88.7(2) . 8_565 ?
O6 Tb1 C16 26.81(19) 8_565 8_565 ?
O3 Tb1 C16 102.74(17) 6_565 8_565 ?
O7 Tb1 C16 26.60(18) 8_565 8_565 ?
O4 Tb1 C16 136.84(16) 6_565 8_565 ?
C7 O1 Tb1 137.5(4) . . ?
C7 O2 Tb1 134.6(4) . 7_565 ?
C8 O3 Tb1 98.6(4) . 6_566 ?
C8 O4 Tb1 161.4(4) . 4_545 ?
C8 O4 Tb1 89.0(4) . 6_566 ?
Tb1 O4 Tb1 107.37(15) 4_545 6_566 ?
C10 O5 C9 116.7(5) . . ?
C16 O6 Tb1 93.4(4) . 8_466 ?
C16 O7 Tb1 90.9(4) . 8_466 ?
C2 C1 C6 119.4(5) . . ?
C2 C1 C7 120.1(5) . . ?
C6 C1 C7 120.4(5) . . ?
C1 C2 C3 120.0(5) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 C8 120.4(5) . . ?
C4 C3 C8 119.3(5) . . ?
C5 C4 C3 119.8(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 C9 119.1(5) . . ?
C6 C5 C9 120.7(6) . . ?
C5 C6 C1 120.2(5) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
O1 C7 O2 126.4(5) . . ?
O1 C7 C1 116.3(5) . . ?
O2 C7 C1 117.3(5) . . ?
O3 C8 O4 121.3(6) . . ?
O3 C8 C3 120.5(5) . . ?
O4 C8 C3 118.2(5) . . ?
O3 C8 Tb1 56.4(3) . 6_566 ?
O4 C8 Tb1 65.0(3) . 6_566 ?
C3 C8 Tb1 174.5(4) . 6_566 ?
O5 C9 C5 107.2(5) . . ?
O5 C9 H9A 110.3 . . ?
C5 C9 H9A 110.3 . . ?
O5 C9 H9B 110.3 . . ?
C5 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
O5 C10 C15 125.3(6) . . ?
O5 C10 C11 114.8(6) . . ?
C15 C10 C11 119.9(6) . . ?
C10 C11 C12 119.3(8) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C13 C12 C11 121.4(7) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C12 117.6(6) . . ?
C14 C13 C16 121.7(6) . . ?
C12 C13 C16 120.7(6) . . ?
C13 C14 C15 122.6(6) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C10 119.1(6) . . ?
C14 C15 H15 120.5 . . ?
C10 C15 H15 120.5 . . ?
O7 C16 O6 122.1(6) . . ?
O7 C16 C13 119.1(6) . . ?
O6 C16 C13 118.8(5) . . ?
O7 C16 Tb1 62.5(3) . 8_466 ?
O6 C16 Tb1 59.8(3) . 8_466 ?
C13 C16 Tb1 172.3(5) . 8_466 ?
C17 O8 Tb1 127.1(6) . . ?
O8 C17 N1 126.5(11) . . ?
O8 C17 H17 116.7 . . ?
N1 C17 H17 116.7 . . ?
C17 N1 C18 122.6(13) . . ?
C17 N1 C19 124.6(14) . . ?
C18 N1 C19 112.6(14) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Tb1 131.0(7) . . ?
C20 N2 C22 121.1(11) . . ?
C20 N2 C21 118.1(11) . . ?
C22 N2 C21 118.9(11) . . ?
O9 C20 N2 124.0(10) . . ?
O9 C20 H20 118.0 . . ?
N2 C20 H20 118.0 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17A O8A Tb1 127.1(6) . . ?
O8A C17A O10A 126.5(11) . . ?
O8A C17A H17A 116.7 . . ?
O10A C17A H17A 116.7 . . ?
C20A O9A Tb1 131.0(7) . . ?
O9A C20A O11A 124.0(10) . . ?
O9A C20A H20A 118.0 . . ?
O11A C20A H20A 118.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.7(9) . . . . ?
C7 C1 C2 C3 -176.3(5) . . . . ?
C1 C2 C3 C4 -1.4(9) . . . . ?
C1 C2 C3 C8 177.5(5) . . . . ?
C2 C3 C4 C5 -0.8(9) . . . . ?
C8 C3 C4 C5 -179.7(6) . . . . ?
C3 C4 C5 C6 2.7(9) . . . . ?
C3 C4 C5 C9 179.3(6) . . . . ?
C4 C5 C6 C1 -2.5(9) . . . . ?
C9 C5 C6 C1 -179.0(6) . . . . ?
C2 C1 C6 C5 0.2(9) . . . . ?
C7 C1 C6 C5 178.2(5) . . . . ?
Tb1 O1 C7 O2 -3.0(11) . . . . ?
Tb1 O1 C7 C1 175.8(4) . . . . ?
Tb1 O2 C7 O1 32.6(10) 7_565 . . . ?
Tb1 O2 C7 C1 -146.2(5) 7_565 . . . ?
C2 C1 C7 O1 2.7(9) . . . . ?
C6 C1 C7 O1 -175.3(5) . . . . ?
C2 C1 C7 O2 -178.4(6) . . . . ?
C6 C1 C7 O2 3.6(9) . . . . ?
Tb1 O3 C8 O4 -3.5(6) 6_566 . . . ?
Tb1 O3 C8 C3 174.7(4) 6_566 . . . ?
Tb1 O4 C8 O3 -149.3(9) 4_545 . . . ?
Tb1 O4 C8 O3 3.2(6) 6_566 . . . ?
Tb1 O4 C8 C3 32.4(14) 4_545 . . . ?
Tb1 O4 C8 C3 -175.0(5) 6_566 . . . ?
Tb1 O4 C8 Tb1 -152.5(12) 4_545 . . 6_566 ?
C2 C3 C8 O3 28.2(9) . . . . ?
C4 C3 C8 O3 -152.9(6) . . . . ?
C2 C3 C8 O4 -153.6(6) . . . . ?
C4 C3 C8 O4 25.3(8) . . . . ?
C10 O5 C9 C5 -168.5(6) . . . . ?
C4 C5 C9 O5 129.8(6) . . . . ?
C6 C5 C9 O5 -53.7(8) . . . . ?
C9 O5 C10 C15 4.3(12) . . . . ?
C9 O5 C10 C11 -177.2(8) . . . . ?
O5 C10 C11 C12 -175.7(10) . . . . ?
C15 C10 C11 C12 2.8(15) . . . . ?
C10 C11 C12 C13 -2.8(18) . . . . ?
C11 C12 C13 C14 0.5(16) . . . . ?
C11 C12 C13 C16 -179.2(10) . . . . ?
C12 C13 C14 C15 1.8(13) . . . . ?
C16 C13 C14 C15 -178.5(7) . . . . ?
C13 C14 C15 C10 -1.7(11) . . . . ?
O5 C10 C15 C14 177.7(7) . . . . ?
C11 C10 C15 C14 -0.6(12) . . . . ?
Tb1 O7 C16 O6 6.3(7) 8_466 . . . ?
Tb1 O7 C16 C13 -171.4(6) 8_466 . . . ?
Tb1 O6 C16 O7 -6.5(7) 8_466 . . . ?
Tb1 O6 C16 C13 171.3(6) 8_466 . . . ?
C14 C13 C16 O7 14.4(12) . . . . ?
C12 C13 C16 O7 -165.9(9) . . . . ?
C14 C13 C16 O6 -163.4(7) . . . . ?
C12 C13 C16 O6 16.3(12) . . . . ?
Tb1 O8 C17 N1 -160.9(11) . . . . ?
O8 C17 N1 C18 -3(2) . . . . ?
O8 C17 N1 C19 -176.9(17) . . . . ?
Tb1 O9 C20 N2 -167.3(7) . . . . ?
C22 N2 C20 O9 -179.9(10) . . . . ?
C21 N2 C20 O9 15.9(16) . . . . ?
Tb1 O8A C17A O10A -160.9(11) . . . . ?
Tb1 O9A C20A O11A -167.3(7) . . . . ?

_refine_diff_density_max         2.458
_refine_diff_density_min         -3.774
_refine_diff_density_rms         0.235

####################################################################### 
# 
# 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_12-14R-B-AYY21-Laeutb
_database_code_depnum_ccdc_archive 'CCDC 1574656'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_12-14R-B-AYY21-Laeutb 
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      17.13 Check
RESPONSE:17 H atoms should be attached to severely disordered O atoms 
of water or formic acid, for which the disorder could not eliminated 
although we have applied several restaints to limit it. Thus,these H atoms 
were omitted due to refinement instability and disordered solvent
;
_vrf_PLAT220_12-14R-B-AYY21-Laeutb 
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         7.7 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the La(Eu & Tb) centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_12-14R-B-AYY21-Laeutb 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O14 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O15 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;
_vrf_PLAT430_12-14R-B-AYY21-Laeutb 
;
PROBLEM: SShort Inter D...A Contact O14      ..O15       .       2.80 Ang.
RESPONSE: there should be bond between the two water molecules.
;
_vrf_PLAT975_12-14R-B-AYY21-Laeutb 
;
PROBLEM: Check Calcd Resid. Dens.  0.57A   From O13             2.29 eA-3   
RESPONSE: Most probably this is due to the relatively poor quality of crystal.
The peak cannot has any chemical meaning.
;
_vrf_PLAT971_12-14R-B-AYY21-Laeutb 
;
PROBLEM: Check Calcd Resid. Dens.  1.50A   From O12             2.67 eA-3  
RESPONSE: This is due to the severe disorder of O12 atom and the relatively 
poor quality of crystal,which could not be modelled properly.
;
_vrf_PLAT973_12-14R-B-AYY21-Laeutb 
;
PROBLEM: Check Calcd Positive Resid. Density on       Tb1       1.78 eA-3  
RESPONSE: The residual density peak is close to the heavy Tb1 atom, 
which might be resulted from the disorder of the Tb1 core and could 
not be modelled properly.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[(Eu0.10La0.44Tb0.46)2(C16H9O7)2(C3H7ON)2(H2O)(CHOOH)]??7H2O'
_chemical_formula_sum            'C39 H50 Eu0.20 La0.88 N2 O26 Tb0.92'
_chemical_formula_weight         1261.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2440 2.4630 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1050 3.6800 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1140 4.1650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.445(6)
_cell_length_b                   14.543(3)
_cell_length_c                   13.394(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.85(3)
_cell_angle_gamma                90
_cell_volume                     5423(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    59274
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      31.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_F_000             2514
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.158
_shelx_estimated_absorpt_T_min   0.672
_shelx_estimated_absorpt_T_max   0.752
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.710
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8758
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.789
_diffrn_reflns_theta_max         31.237
_diffrn_reflns_theta_full        25.214
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8758
_reflns_number_gt                7639
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1169P)²+26.1517P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8758
_refine_ls_number_parameters     308
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1782
_refine_ls_wR_factor_gt          0.1735
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.31987(2) 0.78694(2) 0.05546(2) 0.02633(11) Uani 0.44 1 d . . P . .
Eu1 Eu 0.31987(2) 0.78694(2) 0.05546(2) 0.02633(11) Uani 0.1 1 d . . P . .
Tb1 Tb 0.31987(2) 0.78694(2) 0.05546(2) 0.02633(11) Uani 0.46 1 d . . P . .
O1 O 0.73441(10) 0.3435(2) -0.0458(2) 0.0292(6) Uani 1 1 d . . . . .
O2 O 0.79731(11) 0.4293(2) -0.0525(3) 0.0347(6) Uani 1 1 d . . . . .
O3 O 0.76584(12) 0.6651(3) -0.3348(3) 0.0439(9) Uani 1 1 d . . . . .
O4 O 0.69256(12) 0.7281(2) -0.3814(3) 0.0325(6) Uani 1 1 d . . . . .
O5 O 0.58018(15) 0.6480(3) -0.1334(5) 0.0618(12) Uani 1 1 d . U . . .
O6 O 0.39929(14) 0.8218(3) 0.0092(3) 0.0422(8) Uani 1 1 d . . . . .
O7 O 0.38748(13) 0.6751(2) 0.0417(3) 0.0375(7) Uani 1 1 d . . . . .
C1 C 0.71986(14) 0.4869(3) -0.1321(3) 0.0274(7) Uani 1 1 d . . . . .
C2 C 0.73646(14) 0.5493(3) -0.1960(3) 0.0292(7) Uani 1 1 d . . . . .
H2 H 0.769387 0.549103 -0.200279 0.035 Uiso 1 1 calc R U . . .
C3 C 0.70482(14) 0.6121(3) -0.2541(3) 0.0301(8) Uani 1 1 d . . . . .
C4 C 0.65650(15) 0.6132(3) -0.2455(4) 0.0339(8) Uani 1 1 d . . . . .
H4 H 0.634743 0.654820 -0.285711 0.041 Uiso 1 1 calc R U . . .
C5 C 0.64018(15) 0.5539(3) -0.1786(4) 0.0344(9) Uani 1 1 d . . . . .
C6 C 0.67138(14) 0.4894(3) -0.1236(3) 0.0294(7) Uani 1 1 d . . . . .
H6 H 0.659888 0.446967 -0.080182 0.035 Uiso 1 1 calc R U . . .
C7 C 0.75291(14) 0.4160(3) -0.0738(3) 0.0272(7) Uani 1 1 d . . . . .
C8 C 0.72254(15) 0.6742(3) -0.3297(3) 0.0322(8) Uani 1 1 d . . . . .
C9 C 0.58884(16) 0.5560(4) -0.1652(4) 0.0396(10) Uani 1 1 d . . . . .
H9A H 0.566630 0.540939 -0.230212 0.048 Uiso 1 1 calc R U . . .
H9B H 0.584001 0.510925 -0.112853 0.048 Uiso 1 1 calc R U . . .
C10 C 0.5380(2) 0.6639(4) -0.0995(6) 0.0543(16) Uani 1 1 d . . . . .
C11 C 0.5297(3) 0.7552(5) -0.0789(8) 0.0673(18) Uani 1 1 d . U . . .
H11 H 0.551437 0.801318 -0.091295 0.081 Uiso 1 1 calc R U . . .
C12 C 0.4895(3) 0.7794(4) -0.0400(7) 0.0586(16) Uani 1 1 d . U . . .
H12 H 0.484952 0.841449 -0.021792 0.070 Uiso 1 1 calc R U . . .
C13 C 0.45577(17) 0.7118(3) -0.0279(4) 0.0349(9) Uani 1 1 d . . . . .
C14 C 0.46391(15) 0.6219(3) -0.0540(3) 0.0331(8) Uani 1 1 d . . . . .
H14 H 0.441403 0.575650 -0.045778 0.040 Uiso 1 1 calc R U . . .
C15 C 0.50440(15) 0.5973(3) -0.0922(4) 0.0357(9) Uani 1 1 d . . . . .
H15 H 0.508653 0.535841 -0.112688 0.043 Uiso 1 1 calc R U . . .
C16 C 0.41151(17) 0.7372(3) 0.0100(3) 0.0324(8) Uani 1 1 d . . . . .
O8 O 0.3482(2) 0.7184(3) 0.2271(4) 0.0662(16) Uani 1 1 d . . . . .
C17 C 0.3384(4) 0.7490(8) 0.3074(6) 0.081(2) Uani 1 1 d . U . . .
H17 H 0.333422 0.813359 0.311188 0.097 Uiso 1 1 calc R U . . .
N1 N 0.3345(3) 0.6995(7) 0.3868(5) 0.087(2) Uani 1 1 d . U . . .
C18 C 0.3223(5) 0.7341(11) 0.4769(8) 0.107(4) Uani 1 1 d . U . . .
H18A H 0.325581 0.801149 0.478495 0.160 Uiso 1 1 calc R U . . .
H18B H 0.343826 0.707513 0.536465 0.160 Uiso 1 1 calc R U . . .
H18C H 0.289032 0.717424 0.478073 0.160 Uiso 1 1 calc R U . . .
C19 C 0.3495(6) 0.5957(10) 0.3911(10) 0.120(4) Uani 1 1 d . U . . .
H19A H 0.353623 0.575786 0.323574 0.181 Uiso 1 1 calc R U . . .
H19B H 0.324387 0.558538 0.411979 0.181 Uiso 1 1 calc R U . . .
H19C H 0.379774 0.587720 0.440591 0.181 Uiso 1 1 calc R U . . .
O9 O 0.35815(19) 0.9125(4) 0.1630(4) 0.0691(14) Uani 0.5 1 d D . P A 1
C20 C 0.3531(5) 0.9926(5) 0.1715(8) 0.055(3) Uani 0.5 1 d D U P A 1
H20 H 0.325764 1.014167 0.124058 0.066 Uiso 0.5 1 calc R U P A 1
O10 O 0.3736(4) 1.0569(7) 0.2254(8) 0.077(3) Uani 0.5 1 d D U P A 1
O12 O 0.500000 0.7382(7) 0.250000 0.078(2) Uiso 1 2 d S . P B 1
O9A O 0.35815(19) 0.9125(4) 0.1630(4) 0.0691(14) Uani 0.5 1 d . . P A 2
O11 O 0.3650(8) 1.1340(16) 0.2420(18) 0.146(7) Uiso 0.5 1 d . . P C 2
O13 O 0.500000 0.867(2) 0.250000 0.302(15) Uiso 1 2 d S . P D 2
O14 O 0.4569(5) 0.9910(10) 0.0531(11) 0.180(5) Uiso 1 1 d . . . . .
O15 O 0.8705(8) 0.5611(16) 0.9400(17) 0.282(10) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O1 2.432(3) 5_665 ?
La1 O3 2.436(3) 8_466 ?
La1 O9A 2.440(5) . ?
La1 O9 2.440(5) . ?
La1 O4 2.441(3) 2_654 ?
La1 O8 2.484(5) . ?
La1 O6 2.514(4) . ?
La1 O2 2.531(3) 3_455 ?
La1 O7 2.554(3) . ?
La1 O1 2.659(3) 3_455 ?
La1 C16 2.888(5) . ?
La1 C7 2.966(4) 3_455 ?
O1 C7 1.269(5) . ?
O2 C7 1.251(5) . ?
O3 C8 1.255(5) . ?
O4 C8 1.256(5) . ?
O5 C10 1.387(6) . ?
O5 C9 1.439(7) . ?
O6 C16 1.278(6) . ?
O7 C16 1.258(6) . ?
C1 C2 1.395(5) . ?
C1 C6 1.408(5) . ?
C1 C7 1.501(6) . ?
C2 C3 1.401(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.403(5) . ?
C3 C8 1.518(6) . ?
C4 C5 1.391(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(6) . ?
C5 C9 1.508(6) . ?
C6 H6 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.378(7) . ?
C10 C11 1.386(10) . ?
C11 C12 1.396(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.407(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(6) . ?
C13 C16 1.497(7) . ?
C14 C15 1.399(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O8 C17 1.247(9) . ?
C17 N1 1.307(11) . ?
C17 H17 0.9500 . ?
N1 C18 1.414(12) . ?
N1 C19 1.568(16) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O9 C20 1.183(8) . ?
C20 O10 1.250(8) . ?
C20 H20 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 O3 77.46(12) 5_665 8_466 ?
O1 La1 O9A 144.74(14) 5_665 . ?
O3 La1 O9A 71.94(15) 8_466 . ?
O1 La1 O9 144.74(14) 5_665 . ?
O3 La1 O9 71.94(15) 8_466 . ?
O1 La1 O4 73.14(11) 5_665 2_654 ?
O3 La1 O4 133.72(12) 8_466 2_654 ?
O9 La1 O4 141.84(15) . 2_654 ?
O1 La1 O8 79.52(17) 5_665 . ?
O3 La1 O8 71.44(15) 8_466 . ?
O9A La1 O8 74.5(2) . . ?
O9 La1 O8 74.5(2) . . ?
O4 La1 O8 134.38(15) 2_654 . ?
O1 La1 O6 137.48(11) 5_665 . ?
O3 La1 O6 143.25(13) 8_466 . ?
O9A La1 O6 71.33(15) . . ?
O9 La1 O6 71.33(15) . . ?
O4 La1 O6 78.25(13) 2_654 . ?
O8 La1 O6 99.90(18) . . ?
O1 La1 O2 121.58(10) 5_665 3_455 ?
O3 La1 O2 89.61(13) 8_466 3_455 ?
O9 La1 O2 75.83(17) . 3_455 ?
O4 La1 O2 76.77(12) 2_654 3_455 ?
O8 La1 O2 148.55(15) . 3_455 ?
O6 La1 O2 80.18(11) . 3_455 ?
O1 La1 O7 88.80(11) 5_665 . ?
O3 La1 O7 143.45(13) 8_466 . ?
O9A La1 O7 105.53(16) . . ?
O9 La1 O7 105.53(16) . . ?
O4 La1 O7 70.81(12) 2_654 . ?
O8 La1 O7 72.84(13) . . ?
O6 La1 O7 51.87(12) . . ?
O2 La1 O7 125.87(11) 3_455 . ?
O1 La1 O1 73.15(11) 5_665 3_455 ?
O3 La1 O1 66.13(11) 8_466 3_455 ?
O9 La1 O1 108.68(16) . 3_455 ?
O4 La1 O1 71.53(11) 2_654 3_455 ?
O8 La1 O1 133.27(15) . 3_455 ?
O6 La1 O1 125.83(11) . 3_455 ?
O2 La1 O1 50.04(10) 3_455 3_455 ?
O7 La1 O1 141.55(11) . 3_455 ?
O1 La1 C16 112.60(12) 5_665 . ?
O3 La1 C16 155.16(13) 8_466 . ?
O9A La1 C16 89.95(16) . . ?
O9 La1 C16 89.95(16) . . ?
O4 La1 C16 70.76(12) 2_654 . ?
O8 La1 C16 87.67(16) . . ?
O6 La1 C16 26.20(13) . . ?
O2 La1 C16 102.60(12) 3_455 . ?
O7 La1 C16 25.81(12) . . ?
O1 La1 C16 137.72(11) 3_455 . ?
O1 La1 C7 97.93(11) 5_665 3_455 ?
O3 La1 C7 76.23(13) 8_466 3_455 ?
O9A La1 C7 91.51(17) . 3_455 ?
O9 La1 C7 91.51(17) . 3_455 ?
O4 La1 C7 73.42(11) 2_654 3_455 ?
O8 La1 C7 147.35(13) . 3_455 ?
O6 La1 C7 103.31(12) . 3_455 ?
O2 La1 C7 24.73(10) 3_455 3_455 ?
O7 La1 C7 139.80(11) . 3_455 ?
O1 La1 C7 25.34(10) 3_455 3_455 ?
C16 La1 C7 122.31(11) . 3_455 ?
C7 O1 La1 158.4(3) . 5_665 ?
C7 O1 La1 91.0(2) . 3_545 ?
La1 O1 La1 106.85(11) 5_665 3_545 ?
C7 O2 La1 97.5(3) . 3_545 ?
C8 O3 La1 138.7(3) . 8_565 ?
C8 O4 La1 133.9(3) . 2_654 ?
C10 O5 C9 117.6(4) . . ?
C16 O6 La1 93.5(3) . . ?
C16 O7 La1 92.1(3) . . ?
C2 C1 C6 119.6(4) . . ?
C2 C1 C7 120.7(3) . . ?
C6 C1 C7 119.7(3) . . ?
C1 C2 C3 120.4(4) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 C8 119.7(3) . . ?
C4 C3 C8 120.9(4) . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 C9 121.6(4) . . ?
C6 C5 C9 118.6(4) . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
O2 C7 O1 121.4(4) . . ?
O2 C7 C1 120.5(4) . . ?
O1 C7 C1 118.1(3) . . ?
O2 C7 La1 57.8(2) . 3_545 ?
O1 C7 La1 63.7(2) . 3_545 ?
C1 C7 La1 175.3(3) . 3_545 ?
O3 C8 O4 126.8(4) . . ?
O3 C8 C3 116.0(4) . . ?
O4 C8 C3 117.2(4) . . ?
O5 C9 C5 106.5(4) . . ?
O5 C9 H9A 110.4 . . ?
C5 C9 H9A 110.4 . . ?
O5 C9 H9B 110.4 . . ?
C5 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
C15 C10 C11 120.7(5) . . ?
C15 C10 O5 124.4(5) . . ?
C11 C10 O5 114.8(5) . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 119.8(6) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 118.5(5) . . ?
C14 C13 C16 121.0(4) . . ?
C12 C13 C16 120.5(5) . . ?
C13 C14 C15 121.7(4) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C10 C15 C14 118.8(5) . . ?
C10 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
O7 C16 O6 121.9(4) . . ?
O7 C16 C13 119.4(4) . . ?
O6 C16 C13 118.8(4) . . ?
O7 C16 La1 62.1(2) . . ?
O6 C16 La1 60.3(2) . . ?
C13 C16 La1 172.5(3) . . ?
C17 O8 La1 124.6(5) . . ?
O8 C17 N1 125.2(10) . . ?
O8 C17 H17 117.4 . . ?
N1 C17 H17 117.4 . . ?
C17 N1 C18 125.2(11) . . ?
C17 N1 C19 119.5(8) . . ?
C18 N1 C19 115.0(9) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 La1 138.2(7) . . ?
O9 C20 O10 137.8(14) . . ?
O9 C20 H20 111.1 . . ?
O10 C20 H20 111.1 . . ?

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
C6 C1 C2 C3 -2.1(6) . . . . ?
C7 C1 C2 C3 176.8(4) . . . . ?
C1 C2 C3 C4 1.5(7) . . . . ?
C1 C2 C3 C8 -175.0(4) . . . . ?
C2 C3 C4 C5 1.3(7) . . . . ?
C8 C3 C4 C5 177.7(5) . . . . ?
C3 C4 C5 C6 -3.5(8) . . . . ?
C3 C4 C5 C9 177.8(5) . . . . ?
C4 C5 C6 C1 2.8(7) . . . . ?
C9 C5 C6 C1 -178.3(4) . . . . ?
C2 C1 C6 C5 -0.1(7) . . . . ?
C7 C1 C6 C5 -179.0(4) . . . . ?
La1 O2 C7 O1 -4.1(4) 3_545 . . . ?
La1 O2 C7 C1 174.8(3) 3_545 . . . ?
La1 O1 C7 O2 -142.0(6) 5_665 . . . ?
La1 O1 C7 O2 3.9(4) 3_545 . . . ?
La1 O1 C7 C1 39.0(9) 5_665 . . . ?
La1 O1 C7 C1 -175.1(3) 3_545 . . . ?
La1 O1 C7 La1 -145.9(7) 5_665 . . 3_545 ?
C2 C1 C7 O2 24.7(6) . . . . ?
C6 C1 C7 O2 -156.4(4) . . . . ?
C2 C1 C7 O1 -156.3(4) . . . . ?
C6 C1 C7 O1 22.6(6) . . . . ?
La1 O3 C8 O4 -10.9(9) 8_565 . . . ?
La1 O3 C8 C3 168.0(4) 8_565 . . . ?
La1 O4 C8 O3 33.7(8) 2_654 . . . ?
La1 O4 C8 C3 -145.2(3) 2_654 . . . ?
C2 C3 C8 O3 -0.4(7) . . . . ?
C4 C3 C8 O3 -176.9(5) . . . . ?
C2 C3 C8 O4 178.6(4) . . . . ?
C4 C3 C8 O4 2.2(7) . . . . ?
C10 O5 C9 C5 -169.5(5) . . . . ?
C4 C5 C9 O5 -57.9(7) . . . . ?
C6 C5 C9 O5 123.3(5) . . . . ?
C9 O5 C10 C15 1.4(10) . . . . ?
C9 O5 C10 C11 -174.4(7) . . . . ?
C15 C10 C11 C12 6.8(12) . . . . ?
O5 C10 C11 C12 -177.2(8) . . . . ?
C10 C11 C12 C13 -4.1(13) . . . . ?
C11 C12 C13 C14 0.9(11) . . . . ?
C11 C12 C13 C16 -177.7(7) . . . . ?
C12 C13 C14 C15 -0.3(8) . . . . ?
C16 C13 C14 C15 178.2(4) . . . . ?
C11 C10 C15 C14 -6.2(10) . . . . ?
O5 C10 C15 C14 178.2(6) . . . . ?
C13 C14 C15 C10 3.0(8) . . . . ?
La1 O7 C16 O6 8.5(5) . . . . ?
La1 O7 C16 C13 -171.7(4) . . . . ?
La1 O6 C16 O7 -8.6(5) . . . . ?
La1 O6 C16 C13 171.5(4) . . . . ?
C14 C13 C16 O7 17.2(7) . . . . ?
C12 C13 C16 O7 -164.3(6) . . . . ?
C14 C13 C16 O6 -162.9(5) . . . . ?
C12 C13 C16 O6 15.6(8) . . . . ?
La1 O8 C17 N1 149.7(8) . . . . ?
O8 C17 N1 C18 -178.5(11) . . . . ?
O8 C17 N1 C19 8.7(17) . . . . ?
La1 O9 C20 O10 -177.9(11) . . . . ?

_refine_diff_density_max         2.710
_refine_diff_density_min         -2.081
_refine_diff_density_rms         0.204

####################################################################### 
# 
# 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_9R-Nd-RT2
_database_code_depnum_ccdc_archive 'CCDC 1574657'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_9R-Nd-RT2           
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         6.8 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the Nd centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_9R-Nd-RT2           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;
_vrf_PLAT601_2R-Ce-RT2           
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        115 Ang**3
RESPONSE: The existance of the voids containing loosely bound water
solvent is typical for MOF structures.

# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.242  0.856  0.085        43         0 ' '
   2  0.258  0.638 -0.090        41         0 ' '
   3  0.742  0.356  0.085        43         0 ' '
   4  0.758  0.138 -0.090        41         0 ' '
   5  0.000  0.565  0.250       120         2 ' '
   6  0.500  0.065  0.250       120         2 ' '
   7  0.000  0.931  0.250         7         2 ' '
   8  0.500  0.431  0.250         7         2 ' '
   9  0.258  0.356  0.415        43         0 ' '
  10  0.758  0.856  0.415        43         0 ' '
  11  0.242  0.138  0.590        41         0 ' '
  12  0.742  0.638  0.590        41         0 ' '
  13  0.000  0.435  0.750       121         2 ' '
  14  0.500  0.935  0.750       121         2 ' '
  15  0.000  0.069  0.750         7         2 ' '
  16  0.500  0.569  0.750         7         2 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;
_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[Nd2(C16H9O7)2(C3H7ON)1.2(H2O)1.4(CHOOH)1.4]??3.6H2O'
_chemical_formula_sum            'C37 H39.20 N1.20 Nd2 O23'
_chemical_formula_weight         1157.17

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'
N N 0.0061 0.0033 '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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.560(2)
_cell_length_b                   14.3583(11)
_cell_length_c                   13.7162(11)
_cell_angle_alpha                90
_cell_angle_beta                 97.985(2)
_cell_angle_gamma                90
_cell_volume                     5570.2(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9759
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.04

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_F_000             2294
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.912
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56284
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.584
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5711
_reflns_number_gt                4440
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²+50.4587P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5711
_refine_ls_number_parameters     299
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1138
_refine_ls_wR_factor_gt          0.1057
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.68253(2) 0.20905(2) 0.46010(2) 0.01972(10) Uani 1 1 d . . . . .
O1 O 0.73180(14) 0.3369(3) 0.4467(3) 0.0356(10) Uani 1 1 d . . . . .
O2 O 0.79369(15) 0.4244(3) 0.4341(4) 0.0436(11) Uani 1 1 d . . . . .
O3 O 0.76559(14) 0.6492(3) 0.1462(3) 0.0414(11) Uani 1 1 d . . . . .
O4 O 0.69560(15) 0.7218(3) 0.1183(3) 0.0385(10) Uani 1 1 d . . . . .
O5 O 0.57735(17) 0.6441(4) 0.3509(4) 0.0629(15) Uani 1 1 d . U . . .
O6 O 0.39170(16) 0.8231(3) 0.4779(4) 0.0494(12) Uani 1 1 d . . . . .
O7 O 0.38260(16) 0.6793(4) 0.5255(4) 0.0530(13) Uani 1 1 d . . . . .
C1 C 0.7179(2) 0.4794(4) 0.3591(5) 0.0327(13) Uani 1 1 d . . . . .
C2 C 0.6711(2) 0.4841(4) 0.3725(5) 0.0376(15) Uani 1 1 d . . . . .
H2 H 0.659523 0.444577 0.417273 0.045 Uiso 1 1 calc R U . . .
C3 C 0.6409(2) 0.5481(4) 0.3191(5) 0.0375(15) Uani 1 1 d . . . . .
C4 C 0.6580(2) 0.6053(4) 0.2505(5) 0.0360(14) Uani 1 1 d . . . . .
H4 H 0.637733 0.646515 0.213183 0.043 Uiso 1 1 calc R U . . .
C5 C 0.7054(2) 0.6010(4) 0.2373(4) 0.0311(13) Uani 1 1 d . . . . .
C6 C 0.7353(2) 0.5392(4) 0.2924(4) 0.0342(14) Uani 1 1 d . . . . .
H6 H 0.767185 0.537520 0.285025 0.041 Uiso 1 1 calc R U . . .
C7 C 0.7499(2) 0.4095(4) 0.4162(5) 0.0333(14) Uani 1 1 d . . . . .
C8 C 0.7237(2) 0.6626(4) 0.1607(4) 0.0315(13) Uani 1 1 d . . . . .
C9 C 0.5895(2) 0.5509(5) 0.3342(6) 0.0458(17) Uani 1 1 d . U . . .
H9A H 0.569743 0.526893 0.276435 0.055 Uiso 1 1 calc R U . . .
H9B H 0.584594 0.512698 0.390281 0.055 Uiso 1 1 calc R U . . .
C10 C 0.5342(2) 0.6616(5) 0.3813(6) 0.053(2) Uani 1 1 d . . . . .
C11 C 0.5230(3) 0.7524(6) 0.3891(7) 0.072(2) Uani 1 1 d . U . . .
H11 H 0.543453 0.797847 0.371245 0.086 Uiso 1 1 calc R U . . .
C12 C 0.4812(3) 0.7792(6) 0.4237(7) 0.070(2) Uani 1 1 d . U . . .
H12 H 0.474349 0.842045 0.430226 0.084 Uiso 1 1 calc R U . . .
C13 C 0.4501(2) 0.7125(5) 0.4481(5) 0.0450(17) Uani 1 1 d . . . . .
C14 C 0.4611(2) 0.6206(5) 0.4361(6) 0.0491(18) Uani 1 1 d . . . . .
H14 H 0.440179 0.574922 0.451392 0.059 Uiso 1 1 calc R U . . .
C15 C 0.5027(2) 0.5941(5) 0.4018(6) 0.0477(18) Uani 1 1 d . . . . .
H15 H 0.509187 0.531469 0.392737 0.057 Uiso 1 1 calc R U . . .
C16 C 0.4056(2) 0.7402(5) 0.4855(5) 0.0395(15) Uani 1 1 d . . . . .
O8 O 0.6537(2) 0.2667(5) 0.2949(4) 0.0756(18) Uani 0.6 1 d . . P A 1
N1 N 0.6557(6) 0.2843(12) 0.1312(11) 0.107(5) Uani 0.6 1 d D U P A 1
C17 C 0.6609(6) 0.2390(13) 0.2165(11) 0.078(4) Uani 0.6 1 d . U P A 1
H17 H 0.671507 0.177921 0.214750 0.093 Uiso 0.6 1 calc R U P A 1
C18 C 0.6547(13) 0.222(2) 0.037(2) 0.213(15) Uani 0.6 1 d D U P A 1
H18A H 0.638900 0.164399 0.046589 0.320 Uiso 0.6 1 d R U P A 1
H18B H 0.686509 0.209325 0.025548 0.320 Uiso 0.6 1 d R U P A 1
H18C H 0.638146 0.254108 -0.018759 0.320 Uiso 0.6 1 d R U P A 1
C19 C 0.6345(8) 0.3764(14) 0.1212(17) 0.137(8) Uani 0.6 1 d D U P A 1
H19A H 0.604127 0.373563 0.143349 0.205 Uiso 0.6 1 d R U P A 1
H19B H 0.630752 0.395106 0.053376 0.205 Uiso 0.6 1 d R U P A 1
H19C H 0.654067 0.420867 0.160241 0.205 Uiso 0.6 1 d R U P A 1
O9 O 0.6449(2) 0.0779(4) 0.3717(4) 0.0731(17) Uani 0.7 1 d D U P A 1
C20 C 0.6583(4) -0.0008(6) 0.3590(8) 0.060(3) Uani 0.7 1 d D U P A 1
H20 H 0.685038 -0.020921 0.399974 0.072 Uiso 0.7 1 calc R U P A 1
O10 O 0.6390(4) -0.0595(8) 0.2942(8) 0.111(4) Uani 0.7 1 d D U P A 1
O8A O 0.6537(2) 0.2667(5) 0.2949(4) 0.0756(18) Uani 0.4 1 d . . P A 2
O9A O 0.6449(2) 0.0779(4) 0.3717(4) 0.0731(17) Uani 0.3 1 d . . P A 2
O11 O 0.6569(7) -0.1500(14) 0.2883(14) 0.069(5) Uiso 0.3 1 d . . P B 2
O12 O 0.4426(6) 0.0040(13) 0.5223(13) 0.282(8) Uiso 1 1 d . . . . .
O13 O 0.500000 0.767(2) 0.750000 0.351(16) Uiso 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O1 2.335(4) . ?
Nd1 O4 2.369(4) 6_566 ?
Nd1 O3 2.379(4) 4_645 ?
Nd1 O9 2.410(5) . ?
Nd1 O9A 2.410(5) . ?
Nd1 O6 2.435(4) 5_666 ?
Nd1 O2 2.443(4) 7_656 ?
Nd1 O8 2.446(6) . ?
Nd1 O8A 2.446(6) . ?
Nd1 O7 2.485(5) 5_666 ?
Nd1 O1 2.681(4) 7_656 ?
Nd1 C16 2.818(6) 5_666 ?
O1 C7 1.262(7) . ?
O2 C7 1.258(7) . ?
O3 C8 1.255(7) . ?
O4 C8 1.255(7) . ?
O5 C10 1.377(7) . ?
O5 C9 1.408(8) . ?
O6 C16 1.254(8) . ?
O7 C16 1.263(8) . ?
C1 C2 1.377(8) . ?
C1 C6 1.396(8) . ?
C1 C7 1.502(8) . ?
C2 C3 1.396(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(8) . ?
C3 C9 1.514(8) . ?
C4 C5 1.391(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(8) . ?
C5 C8 1.521(8) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.350(11) . ?
C10 C15 1.378(9) . ?
C11 C12 1.400(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.380(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(9) . ?
C13 C16 1.489(8) . ?
C14 C15 1.392(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O8 C17 1.190(16) . ?
N1 C17 1.33(2) . ?
N1 C19 1.453(16) . ?
N1 C18 1.569(18) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9599 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O9 C20 1.214(8) . ?
C20 O10 1.291(8) . ?
C20 H20 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nd1 O4 73.90(15) . 6_566 ?
O1 Nd1 O3 78.59(15) . 4_645 ?
O4 Nd1 O3 132.89(15) 6_566 4_645 ?
O1 Nd1 O9 143.70(18) . . ?
O4 Nd1 O9 142.27(17) 6_566 . ?
O3 Nd1 O9 71.45(17) 4_645 . ?
O1 Nd1 O9A 143.70(18) . . ?
O4 Nd1 O9A 142.27(17) 6_566 . ?
O3 Nd1 O9A 71.45(17) 4_645 . ?
O1 Nd1 O6 137.70(15) . 5_666 ?
O4 Nd1 O6 78.09(16) 6_566 5_666 ?
O3 Nd1 O6 142.38(16) 4_645 5_666 ?
O9 Nd1 O6 71.25(18) . 5_666 ?
O1 Nd1 O2 122.85(14) . 7_656 ?
O4 Nd1 O2 77.81(16) 6_566 7_656 ?
O3 Nd1 O2 86.30(16) 4_645 7_656 ?
O9 Nd1 O2 75.7(2) . 7_656 ?
O6 Nd1 O2 80.08(15) 5_666 7_656 ?
O1 Nd1 O8 77.9(2) . . ?
O4 Nd1 O8 134.21(18) 6_566 . ?
O3 Nd1 O8 73.30(18) 4_645 . ?
O9 Nd1 O8 74.3(2) . . ?
O6 Nd1 O8 100.9(2) 5_666 . ?
O2 Nd1 O8 147.80(19) 7_656 . ?
O1 Nd1 O8A 77.9(2) . . ?
O4 Nd1 O8A 134.21(18) 6_566 . ?
O3 Nd1 O8A 73.30(18) 4_645 . ?
O9A Nd1 O8A 74.3(2) . . ?
O6 Nd1 O8A 100.9(2) 5_666 . ?
O2 Nd1 O8A 147.80(19) 7_656 . ?
O1 Nd1 O7 88.00(15) . 5_666 ?
O4 Nd1 O7 71.39(17) 6_566 5_666 ?
O3 Nd1 O7 144.97(16) 4_645 5_666 ?
O9 Nd1 O7 104.94(19) . 5_666 ?
O6 Nd1 O7 52.90(15) 5_666 5_666 ?
O2 Nd1 O7 127.48(15) 7_656 5_666 ?
O8 Nd1 O7 72.29(18) . 5_666 ?
O1 Nd1 O1 73.18(15) . 7_656 ?
O4 Nd1 O1 69.44(14) 6_566 7_656 ?
O3 Nd1 O1 66.33(14) 4_645 7_656 ?
O9 Nd1 O1 111.20(18) . 7_656 ?
O6 Nd1 O1 124.63(15) 5_666 7_656 ?
O2 Nd1 O1 50.49(13) 7_656 7_656 ?
O8 Nd1 O1 133.85(18) . 7_656 ?
O7 Nd1 O1 139.86(16) 5_666 7_656 ?
O1 Nd1 C16 112.80(17) . 5_666 ?
O4 Nd1 C16 71.45(18) 6_566 5_666 ?
O3 Nd1 C16 155.61(18) 4_645 5_666 ?
O9 Nd1 C16 89.0(2) . 5_666 ?
O9A Nd1 C16 89.0(2) . 5_666 ?
O6 Nd1 C16 26.36(17) 5_666 5_666 ?
O2 Nd1 C16 103.32(17) 7_656 5_666 ?
O8 Nd1 C16 87.7(2) . 5_666 ?
O8A Nd1 C16 87.7(2) . 5_666 ?
O7 Nd1 C16 26.62(17) 5_666 5_666 ?
O1 Nd1 C16 136.62(16) 7_656 5_666 ?
C7 O1 Nd1 162.8(4) . . ?
C7 O1 Nd1 88.4(4) . 7_656 ?
Nd1 O1 Nd1 106.82(15) . 7_656 ?
C7 O2 Nd1 99.7(4) . 7_656 ?
C8 O3 Nd1 136.9(4) . 4_655 ?
C8 O4 Nd1 135.8(4) . 6_565 ?
C10 O5 C9 118.3(5) . . ?
C16 O6 Nd1 94.1(4) . 5_666 ?
C16 O7 Nd1 91.6(4) . 5_666 ?
C2 C1 C6 119.9(6) . . ?
C2 C1 C7 119.7(5) . . ?
C6 C1 C7 120.4(5) . . ?
C1 C2 C3 120.2(5) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 119.8(5) . . ?
C4 C3 C9 121.1(6) . . ?
C2 C3 C9 119.0(6) . . ?
C3 C4 C5 120.1(6) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 C8 120.3(5) . . ?
C4 C5 C8 119.9(5) . . ?
C5 C6 C1 120.3(5) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
O2 C7 O1 121.2(6) . . ?
O2 C7 C1 120.3(5) . . ?
O1 C7 C1 118.5(5) . . ?
O2 C7 Nd1 55.2(3) . 7_656 ?
O1 C7 Nd1 66.1(3) . 7_656 ?
C1 C7 Nd1 173.6(4) . 7_656 ?
O4 C8 O3 126.4(5) . . ?
O4 C8 C5 117.1(5) . . ?
O3 C8 C5 116.6(5) . . ?
O5 C9 C3 108.2(5) . . ?
O5 C9 H9A 110.1 . . ?
C3 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C3 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
C11 C10 O5 115.6(6) . . ?
C11 C10 C15 119.7(6) . . ?
O5 C10 C15 124.7(6) . . ?
C10 C11 C12 121.0(7) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 120.0(7) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C12 118.3(6) . . ?
C14 C13 C16 121.3(6) . . ?
C12 C13 C16 120.5(6) . . ?
C13 C14 C15 121.6(6) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C10 C15 C14 119.3(6) . . ?
C10 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
O6 C16 O7 121.1(6) . . ?
O6 C16 C13 120.0(6) . . ?
O7 C16 C13 118.9(6) . . ?
O6 C16 Nd1 59.5(3) . 5_666 ?
O7 C16 Nd1 61.8(3) . 5_666 ?
C13 C16 Nd1 175.1(5) . 5_666 ?
C17 O8 Nd1 130.2(9) . . ?
C17 N1 C19 121.5(17) . . ?
C17 N1 C18 115.7(19) . . ?
C19 N1 C18 118.8(19) . . ?
O8 C17 N1 128.3(16) . . ?
O8 C17 H17 115.9 . . ?
N1 C17 H17 115.8 . . ?
N1 C18 H18A 109.4 . . ?
N1 C18 H18B 109.6 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.4 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 108.2 . . ?
N1 C19 H19B 109.6 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 110.6 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Nd1 132.3(7) . . ?
O9 C20 O10 126.5(12) . . ?
O9 C20 H20 116.8 . . ?
O10 C20 H20 116.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.5(10) . . . . ?
C7 C1 C2 C3 -179.3(6) . . . . ?
C1 C2 C3 C4 1.7(10) . . . . ?
C1 C2 C3 C9 179.1(6) . . . . ?
C2 C3 C4 C5 -2.2(10) . . . . ?
C9 C3 C4 C5 -179.5(6) . . . . ?
C3 C4 C5 C6 0.4(10) . . . . ?
C3 C4 C5 C8 178.9(6) . . . . ?
C4 C5 C6 C1 1.8(9) . . . . ?
C8 C5 C6 C1 -176.7(6) . . . . ?
C2 C1 C6 C5 -2.2(10) . . . . ?
C7 C1 C6 C5 177.6(6) . . . . ?
Nd1 O2 C7 O1 -4.3(7) 7_656 . . . ?
Nd1 O2 C7 C1 174.5(5) 7_656 . . . ?
Nd1 O1 C7 O2 -148.9(10) . . . . ?
Nd1 O1 C7 O2 3.9(6) 7_656 . . . ?
Nd1 O1 C7 C1 32.2(16) . . . . ?
Nd1 O1 C7 C1 -175.0(5) 7_656 . . . ?
Nd1 O1 C7 Nd1 -152.8(13) . . . 7_656 ?
C2 C1 C7 O2 -153.7(6) . . . . ?
C6 C1 C7 O2 26.4(9) . . . . ?
C2 C1 C7 O1 25.2(9) . . . . ?
C6 C1 C7 O1 -154.7(6) . . . . ?
Nd1 O4 C8 O3 32.3(10) 6_565 . . . ?
Nd1 O4 C8 C5 -147.8(4) 6_565 . . . ?
Nd1 O3 C8 O4 -2.9(11) 4_655 . . . ?
Nd1 O3 C8 C5 177.2(4) 4_655 . . . ?
C6 C5 C8 O4 -175.0(6) . . . . ?
C4 C5 C8 O4 6.5(9) . . . . ?
C6 C5 C8 O3 4.9(9) . . . . ?
C4 C5 C8 O3 -173.6(6) . . . . ?
C10 O5 C9 C3 -170.4(6) . . . . ?
C4 C3 C9 O5 -52.4(9) . . . . ?
C2 C3 C9 O5 130.2(7) . . . . ?
C9 O5 C10 C11 -175.3(8) . . . . ?
C9 O5 C10 C15 3.6(12) . . . . ?
O5 C10 C11 C12 -177.0(9) . . . . ?
C15 C10 C11 C12 4.1(15) . . . . ?
C10 C11 C12 C13 -1.6(15) . . . . ?
C11 C12 C13 C14 -0.9(14) . . . . ?
C11 C12 C13 C16 179.6(8) . . . . ?
C12 C13 C14 C15 0.9(13) . . . . ?
C16 C13 C14 C15 -179.6(7) . . . . ?
C11 C10 C15 C14 -4.0(13) . . . . ?
O5 C10 C15 C14 177.2(8) . . . . ?
C13 C14 C15 C10 1.5(12) . . . . ?
Nd1 O6 C16 O7 -6.3(7) 5_666 . . . ?
Nd1 O6 C16 C13 174.4(6) 5_666 . . . ?
Nd1 O7 C16 O6 6.1(7) 5_666 . . . ?
Nd1 O7 C16 C13 -174.5(6) 5_666 . . . ?
C14 C13 C16 O6 -166.1(7) . . . . ?
C12 C13 C16 O6 13.4(12) . . . . ?
C14 C13 C16 O7 14.5(11) . . . . ?
C12 C13 C16 O7 -166.0(8) . . . . ?
Nd1 O8 C17 N1 -160.1(14) . . . . ?
C19 N1 C17 O8 -7(3) . . . . ?
C18 N1 C17 O8 -164(2) . . . . ?
Nd1 O9 C20 O10 -164.7(9) . . . . ?

_refine_diff_density_max         1.350
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.137

####################################################################### 
# 
# 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_7R-Dy-RT
_database_code_depnum_ccdc_archive 'CCDC 1574647'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_7R-Dy-RT            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O11 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Dy2(C16H9O7)2(C3H7ON)2(H2O)(CHOOH)]??3H2O'
_chemical_formula_sum            'C39 H42 Dy2 N2 O22'
_chemical_formula_weight         1215.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.4551(16)
_cell_length_b                   14.2978(8)
_cell_length_c                   13.6672(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.2430(10)
_cell_angle_gamma                90
_cell_volume                     5503.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9782
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      28.40

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_F_000             2392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.764
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26432
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.841
_diffrn_reflns_theta_max         28.408
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6846
_reflns_number_gt                6014
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0336P)²+53.8595P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6846
_refine_ls_number_parameters     313
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0911
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.135
_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
Dy1 Dy 0.31742(2) 0.20892(2) 0.54025(2) 0.01872(7) Uani 1 1 d . . . . .
O1 O 0.26839(11) 0.3368(2) 0.5530(2) 0.0275(6) Uani 1 1 d . . . . .
O2 O 0.20652(11) 0.4244(2) 0.5646(3) 0.0345(7) Uani 1 1 d . . . . .
O3 O 0.23446(10) 0.6488(2) 0.8540(2) 0.0323(7) Uani 1 1 d . . . . .
O4 O 0.30455(11) 0.7223(2) 0.8824(2) 0.0294(7) Uani 1 1 d . . . . .
O5 O 0.42311(13) 0.6456(3) 0.6497(4) 0.0540(11) Uani 1 1 d . . . . .
O6 O 0.60888(12) 0.8239(2) 0.5219(3) 0.0396(8) Uani 1 1 d . . . . .
O7 O 0.61764(12) 0.6798(3) 0.4734(3) 0.0444(9) Uani 1 1 d . . . . .
C1 C 0.28189(14) 0.4799(3) 0.6409(3) 0.0243(8) Uani 1 1 d . . . . .
C2 C 0.26448(14) 0.5390(3) 0.7077(3) 0.0255(8) Uani 1 1 d . . . . .
H2 H 0.232535 0.536823 0.715290 0.031 Uiso 1 1 calc R U . . .
C3 C 0.29476(14) 0.6016(3) 0.7634(3) 0.0243(8) Uani 1 1 d . . . . .
C4 C 0.34229(14) 0.6061(3) 0.7498(3) 0.0276(9) Uani 1 1 d . . . . .
H4 H 0.362570 0.647999 0.786921 0.033 Uiso 1 1 calc R U . . .
C5 C 0.35965(15) 0.5485(3) 0.6813(4) 0.0296(9) Uani 1 1 d . . . . .
C6 C 0.32918(15) 0.4848(3) 0.6272(3) 0.0282(9) Uani 1 1 d . . . . .
H6 H 0.340609 0.445408 0.581801 0.034 Uiso 1 1 calc R U . . .
C7 C 0.25006(15) 0.4096(3) 0.5832(3) 0.0242(8) Uani 1 1 d . . . . .
C8 C 0.27647(14) 0.6627(3) 0.8396(3) 0.0237(8) Uani 1 1 d . . . . .
C9 C 0.41101(16) 0.5517(3) 0.6655(4) 0.0369(11) Uani 1 1 d . . . . .
H9A H 0.431075 0.526931 0.723037 0.044 Uiso 1 1 calc R U . . .
H9B H 0.415607 0.513964 0.608630 0.044 Uiso 1 1 calc R U . . .
C10 C 0.46624(17) 0.6623(4) 0.6201(4) 0.0424(12) Uani 1 1 d . . . . .
C11 C 0.4774(2) 0.7556(4) 0.6113(7) 0.066(2) Uani 1 1 d . . . . .
H11 H 0.456789 0.801375 0.628308 0.080 Uiso 1 1 calc R U . . .
C12 C 0.5192(2) 0.7813(4) 0.5771(6) 0.061(2) Uani 1 1 d . . . . .
H12 H 0.526451 0.844244 0.571109 0.073 Uiso 1 1 calc R U . . .
C13 C 0.55035(16) 0.7133(3) 0.5517(4) 0.0360(11) Uani 1 1 d . . . . .
C14 C 0.53915(16) 0.6207(4) 0.5635(4) 0.0384(11) Uani 1 1 d . . . . .
H14 H 0.560002 0.574728 0.548114 0.046 Uiso 1 1 calc R U . . .
C15 C 0.49709(17) 0.5942(4) 0.5980(4) 0.0404(12) Uani 1 1 d . . . . .
H15 H 0.490150 0.531311 0.605917 0.048 Uiso 1 1 calc R U . . .
C16 C 0.59475(14) 0.7401(3) 0.5133(4) 0.0313(9) Uani 1 1 d . . . . .
O8 O 0.35582(16) 0.0795(3) 0.6297(4) 0.0605(12) Uani 0.5 1 d . . P A 1
C17 C 0.3430(3) 0.0042(7) 0.6388(7) 0.077(2) Uani 0.5 1 d . U P A 1
H17 H 0.317225 -0.014770 0.593469 0.093 Uiso 0.5 1 calc R U P A 1
N1 N 0.3605(4) -0.0606(7) 0.7070(7) 0.129(3) Uani 0.5 1 d . U P A 1
C18 C 0.3452(6) -0.1475(10) 0.7170(12) 0.068(4) Uani 0.5 1 d . U P A 1
H18A H 0.367319 -0.190728 0.695109 0.101 Uiso 0.5 1 d R U P A 1
H18B H 0.314627 -0.155387 0.677961 0.101 Uiso 0.5 1 d R U P A 1
H18C H 0.342749 -0.159188 0.785265 0.101 Uiso 0.5 1 d R U P A 1
C19 C 0.3961(10) -0.042(2) 0.776(2) 0.135(9) Uani 0.5 1 d . U P A 1
H19A H 0.402833 -0.094605 0.818946 0.202 Uiso 0.5 1 d R U P A 1
H19B H 0.387541 0.010821 0.813986 0.202 Uiso 0.5 1 d R U P A 1
H19C H 0.423787 -0.026068 0.746766 0.202 Uiso 0.5 1 d R U P A 1
O9 O 0.34626(18) 0.2666(4) 0.7052(3) 0.0627(13) Uani 0.5 1 d . . P A 1
C20 C 0.3394(5) 0.2391(10) 0.7843(9) 0.052(3) Uani 0.5 1 d . U P A 1
H20 H 0.328188 0.178165 0.786022 0.063 Uiso 0.5 1 calc R U P A 1
N2 N 0.3455(5) 0.2833(11) 0.8685(8) 0.076(4) Uani 0.5 1 d . U P A 1
C21 C 0.3604(9) 0.3674(17) 0.8782(18) 0.115(7) Uani 0.5 1 d . U P A 1
H21A H 0.393694 0.368838 0.873504 0.173 Uiso 0.5 1 d R U P A 1
H21B H 0.355168 0.391477 0.941340 0.173 Uiso 0.5 1 d R U P A 1
H21C H 0.343515 0.405228 0.826624 0.173 Uiso 0.5 1 d R U P A 1
C22 C 0.3442(11) 0.224(2) 0.964(2) 0.143(10) Uani 0.5 1 d . U P A 1
H22A H 0.341480 0.158997 0.944732 0.214 Uiso 0.5 1 d R U P A 1
H22B H 0.317019 0.241591 0.993560 0.214 Uiso 0.5 1 d R U P A 1
H22C H 0.372499 0.232582 1.010077 0.214 Uiso 0.5 1 d R U P A 1
O8A O 0.35582(16) 0.0795(3) 0.6297(4) 0.0605(12) Uani 0.5 1 d . . P A 2
C17A C 0.3430(3) 0.0042(7) 0.6388(7) 0.077(2) Uani 0.5 1 d . . P A 2
H17A H 0.317225 -0.014770 0.593469 0.093 Uiso 0.5 1 calc R U P A 2
O10 O 0.3605(4) -0.0606(7) 0.7070(7) 0.129(3) Uani 0.5 1 d . . P A 2
O9A O 0.34626(18) 0.2666(4) 0.7052(3) 0.0627(13) Uani 0.5 1 d . . P A 2
O11 O 0.500000 0.772(2) 0.250000 0.324(9) Uiso 1 2 d S . P . .
O12 O 0.5593(7) 0.0051(15) 0.4744(15) 0.312(9) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.321(3) . ?
Dy1 O4 2.351(3) 6_565 ?
Dy1 O3 2.371(3) 4_546 ?
Dy1 O8 2.394(4) . ?
Dy1 O8A 2.394(4) . ?
Dy1 O6 2.419(3) 5_666 ?
Dy1 O2 2.423(3) 7_556 ?
Dy1 O9A 2.430(4) . ?
Dy1 O9 2.430(4) . ?
Dy1 O7 2.466(3) 5_666 ?
Dy1 O1 2.669(3) 7_556 ?
Dy1 C16 2.799(4) 5_666 ?
O1 C7 1.260(5) . ?
O2 C7 1.247(5) . ?
O3 C8 1.254(5) . ?
O4 C8 1.254(5) . ?
O5 C10 1.367(5) . ?
O5 C9 1.411(6) . ?
O6 C16 1.263(6) . ?
O7 C16 1.252(6) . ?
C1 C6 1.387(5) . ?
C1 C2 1.387(5) . ?
C1 C7 1.499(5) . ?
C2 C3 1.390(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(5) . ?
C3 C8 1.508(5) . ?
C4 C5 1.390(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(6) . ?
C5 C9 1.508(5) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.374(7) . ?
C10 C11 1.379(8) . ?
C11 C12 1.390(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.392(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(7) . ?
C13 C16 1.487(6) . ?
C14 C15 1.401(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O8 C17 1.149(10) . ?
C17 N1 1.358(12) . ?
C17 H17 0.9300 . ?
N1 C19 1.31(3) . ?
N1 C18 1.331(16) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O9 C20 1.192(13) . ?
C20 N2 1.303(17) . ?
C20 H20 0.9300 . ?
N2 C21 1.28(2) . ?
N2 C22 1.56(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
O8A C17A 1.149(10) . ?
C17A O10 1.358(12) . ?
C17A H17A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O4 73.94(11) . 6_565 ?
O1 Dy1 O3 78.81(11) . 4_546 ?
O4 Dy1 O3 133.03(11) 6_565 4_546 ?
O1 Dy1 O8 143.66(14) . . ?
O4 Dy1 O8 142.34(14) 6_565 . ?
O3 Dy1 O8 71.76(13) 4_546 . ?
O1 Dy1 O8A 143.66(14) . . ?
O4 Dy1 O8A 142.34(14) 6_565 . ?
O3 Dy1 O8A 71.76(13) 4_546 . ?
O1 Dy1 O6 137.71(11) . 5_666 ?
O4 Dy1 O6 77.74(12) 6_565 5_666 ?
O3 Dy1 O6 142.29(12) 4_546 5_666 ?
O8 Dy1 O6 70.99(14) . 5_666 ?
O1 Dy1 O2 122.90(11) . 7_556 ?
O4 Dy1 O2 78.06(12) 6_565 7_556 ?
O3 Dy1 O2 85.91(12) 4_546 7_556 ?
O8 Dy1 O2 76.29(16) . 7_556 ?
O6 Dy1 O2 79.87(11) 5_666 7_556 ?
O1 Dy1 O9A 77.85(15) . . ?
O4 Dy1 O9A 134.14(14) 6_565 . ?
O3 Dy1 O9A 73.41(14) 4_546 . ?
O8A Dy1 O9A 73.73(18) . . ?
O6 Dy1 O9A 101.37(16) 5_666 . ?
O2 Dy1 O9A 147.62(15) 7_556 . ?
O1 Dy1 O9 77.85(15) . . ?
O4 Dy1 O9 134.14(14) 6_565 . ?
O3 Dy1 O9 73.41(14) 4_546 . ?
O8 Dy1 O9 73.73(18) . . ?
O6 Dy1 O9 101.37(16) 5_666 . ?
O2 Dy1 O9 147.62(15) 7_556 . ?
O1 Dy1 O7 87.87(11) . 5_666 ?
O4 Dy1 O7 71.36(13) 6_565 5_666 ?
O3 Dy1 O7 144.99(12) 4_546 5_666 ?
O8 Dy1 O7 104.18(16) . 5_666 ?
O6 Dy1 O7 53.23(11) 5_666 5_666 ?
O2 Dy1 O7 127.80(11) 7_556 5_666 ?
O9 Dy1 O7 72.19(14) . 5_666 ?
O1 Dy1 O1 73.16(11) . 7_556 ?
O4 Dy1 O1 69.67(10) 6_565 7_556 ?
O3 Dy1 O1 66.14(10) 4_546 7_556 ?
O8 Dy1 O1 111.98(14) . 7_556 ?
O6 Dy1 O1 124.38(11) 5_666 7_556 ?
O2 Dy1 O1 50.54(9) 7_556 7_556 ?
O9 Dy1 O1 133.67(14) . 7_556 ?
O7 Dy1 O1 140.01(13) 5_666 7_556 ?
O1 Dy1 C16 112.55(12) . 5_666 ?
O4 Dy1 C16 71.26(13) 6_565 5_666 ?
O3 Dy1 C16 155.66(13) 4_546 5_666 ?
O8 Dy1 C16 88.58(15) . 5_666 ?
O8A Dy1 C16 88.58(15) . 5_666 ?
O6 Dy1 C16 26.76(13) 5_666 5_666 ?
O2 Dy1 C16 103.64(12) 7_556 5_666 ?
O9A Dy1 C16 87.63(15) . 5_666 ?
O9 Dy1 C16 87.63(15) . 5_666 ?
O7 Dy1 C16 26.55(13) 5_666 5_666 ?
O1 Dy1 C16 136.78(12) 7_556 5_666 ?
C7 O1 Dy1 163.1(3) . . ?
C7 O1 Dy1 88.0(2) . 7_556 ?
Dy1 O1 Dy1 106.84(10) . 7_556 ?
C7 O2 Dy1 100.0(3) . 7_556 ?
C8 O3 Dy1 136.8(3) . 4_556 ?
C8 O4 Dy1 135.8(3) . 6_566 ?
C10 O5 C9 117.4(4) . . ?
C16 O6 Dy1 93.7(3) . 5_666 ?
C16 O7 Dy1 91.8(3) . 5_666 ?
C6 C1 C2 120.2(4) . . ?
C6 C1 C7 119.2(3) . . ?
C2 C1 C7 120.6(3) . . ?
C1 C2 C3 120.0(4) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 C8 120.2(3) . . ?
C4 C3 C8 120.2(4) . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 119.4(4) . . ?
C4 C5 C9 121.6(4) . . ?
C6 C5 C9 119.0(4) . . ?
C1 C6 C5 120.2(4) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
O2 C7 O1 121.3(4) . . ?
O2 C7 C1 120.1(4) . . ?
O1 C7 C1 118.6(4) . . ?
O2 C7 Dy1 55.0(2) . 7_556 ?
O1 C7 Dy1 66.4(2) . 7_556 ?
C1 C7 Dy1 173.5(3) . 7_556 ?
O4 C8 O3 126.3(4) . . ?
O4 C8 C3 117.1(3) . . ?
O3 C8 C3 116.6(4) . . ?
O5 C9 C5 108.3(4) . . ?
O5 C9 H9A 110.0 . . ?
C5 C9 H9A 110.0 . . ?
O5 C9 H9B 110.0 . . ?
C5 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O5 C10 C15 124.7(5) . . ?
O5 C10 C11 115.0(5) . . ?
C15 C10 C11 120.3(4) . . ?
C10 C11 C12 120.2(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 120.4(5) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 118.4(4) . . ?
C14 C13 C16 120.8(4) . . ?
C12 C13 C16 120.7(4) . . ?
C13 C14 C15 121.6(4) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C10 C15 C14 119.1(5) . . ?
C10 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
O7 C16 O6 121.0(4) . . ?
O7 C16 C13 119.8(4) . . ?
O6 C16 C13 119.1(4) . . ?
O7 C16 Dy1 61.7(2) . 5_666 ?
O6 C16 Dy1 59.6(2) . 5_666 ?
C13 C16 Dy1 174.5(4) . 5_666 ?
C17 O8 Dy1 130.6(6) . . ?
O8 C17 N1 128.5(10) . . ?
O8 C17 H17 115.7 . . ?
N1 C17 H17 115.7 . . ?
C19 N1 C18 110.5(16) . . ?
C19 N1 C17 121.5(16) . . ?
C18 N1 C17 128.0(13) . . ?
N1 C18 H18A 109.3 . . ?
N1 C18 H18B 109.7 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.9 . . ?
N1 C19 H19B 108.7 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.9 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Dy1 130.7(7) . . ?
O9 C20 N2 128.6(13) . . ?
O9 C20 H20 115.7 . . ?
N2 C20 H20 115.7 . . ?
C21 N2 C20 123.3(16) . . ?
C21 N2 C22 118.5(18) . . ?
C20 N2 C22 117.1(16) . . ?
N2 C21 H21A 109.1 . . ?
N2 C21 H21B 109.9 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.4 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 108.2 . . ?
N2 C22 H22B 109.1 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 111.1 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17A O8A Dy1 130.6(6) . . ?
O8A C17A O10 128.5(10) . . ?
O8A C17A H17A 115.7 . . ?
O10 C17A H17A 115.7 . . ?

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
C6 C1 C2 C3 -1.9(7) . . . . ?
C7 C1 C2 C3 177.7(4) . . . . ?
C1 C2 C3 C4 1.6(7) . . . . ?
C1 C2 C3 C8 -177.0(4) . . . . ?
C2 C3 C4 C5 -0.1(7) . . . . ?
C8 C3 C4 C5 178.5(4) . . . . ?
C3 C4 C5 C6 -1.1(7) . . . . ?
C3 C4 C5 C9 -179.7(5) . . . . ?
C2 C1 C6 C5 0.7(7) . . . . ?
C7 C1 C6 C5 -178.9(4) . . . . ?
C4 C5 C6 C1 0.8(7) . . . . ?
C9 C5 C6 C1 179.5(5) . . . . ?
Dy1 O2 C7 O1 -4.0(5) 7_556 . . . ?
Dy1 O2 C7 C1 174.9(3) 7_556 . . . ?
Dy1 O1 C7 O2 -148.5(7) . . . . ?
Dy1 O1 C7 O2 3.6(4) 7_556 . . . ?
Dy1 O1 C7 C1 32.6(12) . . . . ?
Dy1 O1 C7 C1 -175.3(3) 7_556 . . . ?
Dy1 O1 C7 Dy1 -152.1(10) . . . 7_556 ?
C6 C1 C7 O2 -153.3(4) . . . . ?
C2 C1 C7 O2 27.1(6) . . . . ?
C6 C1 C7 O1 25.6(6) . . . . ?
C2 C1 C7 O1 -153.9(4) . . . . ?
Dy1 O4 C8 O3 32.2(7) 6_566 . . . ?
Dy1 O4 C8 C3 -147.9(3) 6_566 . . . ?
Dy1 O3 C8 O4 -2.5(8) 4_556 . . . ?
Dy1 O3 C8 C3 177.5(3) 4_556 . . . ?
C2 C3 C8 O4 -175.0(4) . . . . ?
C4 C3 C8 O4 6.3(6) . . . . ?
C2 C3 C8 O3 4.9(6) . . . . ?
C4 C3 C8 O3 -173.8(4) . . . . ?
C10 O5 C9 C5 -171.0(5) . . . . ?
C4 C5 C9 O5 -51.2(7) . . . . ?
C6 C5 C9 O5 130.2(5) . . . . ?
C9 O5 C10 C15 4.8(9) . . . . ?
C9 O5 C10 C11 -176.5(6) . . . . ?
O5 C10 C11 C12 -176.8(7) . . . . ?
C15 C10 C11 C12 2.0(12) . . . . ?
C10 C11 C12 C13 -0.2(13) . . . . ?
C11 C12 C13 C14 -1.4(11) . . . . ?
C11 C12 C13 C16 178.8(7) . . . . ?
C12 C13 C14 C15 1.4(9) . . . . ?
C16 C13 C14 C15 -178.9(5) . . . . ?
O5 C10 C15 C14 176.7(6) . . . . ?
C11 C10 C15 C14 -2.1(10) . . . . ?
C13 C14 C15 C10 0.4(9) . . . . ?
Dy1 O7 C16 O6 5.7(5) 5_666 . . . ?
Dy1 O7 C16 C13 -174.0(4) 5_666 . . . ?
Dy1 O6 C16 O7 -5.9(5) 5_666 . . . ?
Dy1 O6 C16 C13 173.8(4) 5_666 . . . ?
C14 C13 C16 O7 13.9(8) . . . . ?
C12 C13 C16 O7 -166.4(6) . . . . ?
C14 C13 C16 O6 -165.8(5) . . . . ?
C12 C13 C16 O6 13.9(9) . . . . ?
Dy1 O8 C17 N1 -163.3(7) . . . . ?
O8 C17 N1 C19 2(2) . . . . ?
O8 C17 N1 C18 179.7(12) . . . . ?
Dy1 O9 C20 N2 -161.6(12) . . . . ?
O9 C20 N2 C21 1(3) . . . . ?
O9 C20 N2 C22 -167.1(17) . . . . ?
Dy1 O8A C17A O10 -163.3(7) . . . . ?

_refine_diff_density_max         1.493
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.143

####################################################################### 
# 
# 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_13R-B-AYY20-LAEUTB
_database_code_depnum_ccdc_archive 'CCDC 1574653'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_13R-B-AYY20-LAEUTB  
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      15.12 Check
RESPONSE:15 H atoms should be attached to severely disordered O atoms 
of water or formic acid, for which the disorder could not eliminated 
although we have applied several restaints to limit it. Thus,these H atoms 
were omitted due to refinement instability and disordered solvent
;
_vrf_PLAT306_13R-B-AYY20-LAEUTB  
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O14 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O15 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;
_vrf_PLAT430_13R-B-AYY20-LAEUTB  
;
PROBLEM: Short Inter D...A Contact O2      ..O15       .       2.84 Ang.
RESPONSE: there should be bond between the two water molecules.

PROBLEM: Short Inter D...A Contact O14      ..O15       .       2.74 Ang.
RESPONSE: there should be bond between the two water molecules.
;
_vrf_PLAT971_13R-B-AYY20-LAEUTB  
;
PROBLEM: Check Calcd Resid. Dens.  1.50A   From O12             2.67 eA-3  
PROBLEM: Check Calcd Resid. Dens.  0.77A   From C20             2.79 eA-3  
RESPONSE: They are due to the severe disorder of O12 and C20 atoms and 
the relatively poor quality of crystal,which could not be modelled properly.
;
_vrf_PLAT972_13R-B-AYY20-LAEUTB  
;
PROBLEM: Check Calcd Resid. Dens.  0.85A   From Tb1            -4.25 eA-3    
PROBLEM: Check Calcd Resid. Dens.  0.92A   From Tb1            -2.88 eA-3  
RESPONSE: The residual density peaks are close to the heavy Tb1 atom, 
which might be resulted from the disorder of the Tb1 core and could 
not be modelled properly.
;
_vrf_PLAT973_13R-B-AYY20-LAEUTB  
;
PROBLEM: Check Calcd Positive Resid. Density on       Tb1       2.57 eA-3  
PROBLEM: Check Calcd Positive Resid. Density on       Eu1       2.57 eA-3   
PROBLEM: Check Calcd Positive Resid. Density on       La1       2.57 eA-3   
RESPONSE: Three heavy atoms locate at a same position with different occupies. 
The residual density peak is close to these heavy atoms, which might be resulted 
from the disorder of these heavy core and could not be modelled properly.
;
_vrf_PLAT975_13R-B-AYY20-LAEUTB  
;
PROBLEM: Check Calcd Resid. Dens.  0.57A   From O13             2.29 eA-3   
RESPONSE: Most probably this is due to the relatively poor quality of crystal.
The peak cannot has any chemical meaning.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[(Eu0.11La0.66Tb0.23)2(C16H9O7)2(C3H7ON)2(H2O)(CHOOH)]??7H2O'
_chemical_formula_sum            'C39 H48 Eu0.22 La1.32 N2 O26 Tb0.46'
_chemical_formula_weight         1250.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2440 2.4630 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1050 3.6800 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1140 4.1650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.533(6)
_cell_length_b                   14.512(3)
_cell_length_c                   13.441(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.87(3)
_cell_angle_gamma                90
_cell_volume                     5446(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    60868
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      31.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             2492
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.920
_shelx_estimated_absorpt_T_min   0.700
_shelx_estimated_absorpt_T_max   0.775
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.710
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8606
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.915
_diffrn_reflns_theta_max         31.252
_diffrn_reflns_theta_full        25.214
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             8606
_reflns_number_gt                7479
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1453P)²+32.6113P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0080(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8606
_refine_ls_number_parameters     308
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0745
_refine_ls_wR_factor_ref         0.2208
_refine_ls_wR_factor_gt          0.2150
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.32004(2) 0.78683(2) 0.05643(2) 0.03090(14) Uani 0.66 1 d . . P . .
Eu1 Eu 0.32004(2) 0.78683(2) 0.05643(2) 0.03090(14) Uani 0.11 1 d . . P . .
Tb1 Tb 0.32004(2) 0.78683(2) 0.05643(2) 0.03090(14) Uani 0.23 1 d . . P . .
O1 O 0.73476(12) 0.3454(2) -0.0438(3) 0.0343(7) Uani 1 1 d . . . . .
O2 O 0.79727(13) 0.4307(3) -0.0520(3) 0.0403(8) Uani 1 1 d . . . . .
O3 O 0.76550(14) 0.6689(4) -0.3321(4) 0.0501(11) Uani 1 1 d . . . . .
O4 O 0.69210(15) 0.7295(3) -0.3805(3) 0.0381(8) Uani 1 1 d . . . . .
O5 O 0.58088(18) 0.6480(4) -0.1286(5) 0.0654(13) Uani 1 1 d . U . . .
O6 O 0.40062(16) 0.8214(3) 0.0132(4) 0.0465(9) Uani 1 1 d . . . . .
O7 O 0.38786(15) 0.6736(3) 0.0418(3) 0.0419(8) Uani 1 1 d . . . . .
C1 C 0.71987(17) 0.4887(3) -0.1306(4) 0.0329(8) Uani 1 1 d . . . . .
C2 C 0.73633(17) 0.5515(4) -0.1947(4) 0.0344(9) Uani 1 1 d . . . . .
H2 H 0.769199 0.551917 -0.198600 0.041 Uiso 1 1 calc R U . . .
C3 C 0.70460(17) 0.6135(4) -0.2529(4) 0.0355(9) Uani 1 1 d . . . . .
C4 C 0.65634(18) 0.6144(4) -0.2446(4) 0.0387(10) Uani 1 1 d . . . . .
H4 H 0.634647 0.656168 -0.284526 0.046 Uiso 1 1 calc R U . . .
C5 C 0.63992(18) 0.5540(4) -0.1777(4) 0.0407(11) Uani 1 1 d . . . . .
C6 C 0.67192(17) 0.4902(4) -0.1225(4) 0.0347(9) Uani 1 1 d . . . . .
H6 H 0.660829 0.447415 -0.079100 0.042 Uiso 1 1 calc R U . . .
C7 C 0.75293(16) 0.4175(3) -0.0726(3) 0.0317(8) Uani 1 1 d . . . . .
C8 C 0.72216(18) 0.6762(4) -0.3279(4) 0.0378(10) Uani 1 1 d . . . . .
C9 C 0.58902(18) 0.5567(4) -0.1641(5) 0.0439(12) Uani 1 1 d . . . . .
H9A H 0.566745 0.543872 -0.229453 0.053 Uiso 1 1 calc R U . . .
H9B H 0.583893 0.509856 -0.113842 0.053 Uiso 1 1 calc R U . . .
C10 C 0.5390(2) 0.6637(5) -0.0964(7) 0.0584(18) Uani 1 1 d . . . . .
C11 C 0.5313(3) 0.7543(7) -0.0707(9) 0.073(2) Uani 1 1 d . U . . .
H11 H 0.554088 0.800329 -0.077696 0.087 Uiso 1 1 calc R U . . .
C12 C 0.4906(3) 0.7783(5) -0.0346(8) 0.0629(19) Uani 1 1 d . U . . .
H12 H 0.485944 0.840236 -0.016018 0.076 Uiso 1 1 calc R U . . .
C13 C 0.4563(2) 0.7109(3) -0.0256(5) 0.0381(11) Uani 1 1 d . . . . .
C14 C 0.46435(18) 0.6216(4) -0.0534(4) 0.0383(10) Uani 1 1 d . . . . .
H14 H 0.441690 0.575327 -0.046483 0.046 Uiso 1 1 calc R U . . .
C15 C 0.50469(19) 0.5970(4) -0.0915(4) 0.0406(10) Uani 1 1 d . . . . .
H15 H 0.508535 0.535737 -0.113486 0.049 Uiso 1 1 calc R U . . .
C16 C 0.4123(2) 0.7363(4) 0.0120(4) 0.0367(9) Uani 1 1 d . . . . .
O8 O 0.3495(3) 0.7190(4) 0.2299(5) 0.073(2) Uani 1 1 d . . . . .
C17 C 0.3402(4) 0.7500(9) 0.3088(6) 0.082(3) Uani 1 1 d . U . . .
H17 H 0.337197 0.815032 0.313018 0.098 Uiso 1 1 calc R U . . .
N1 N 0.3340(3) 0.7029(7) 0.3860(6) 0.086(3) Uani 1 1 d . U . . .
C18 C 0.3209(5) 0.7414(13) 0.4746(9) 0.106(4) Uani 1 1 d . U . . .
H18A H 0.327113 0.807844 0.476857 0.158 Uiso 1 1 calc R U . . .
H18B H 0.339872 0.712243 0.535528 0.158 Uiso 1 1 calc R U . . .
H18C H 0.286793 0.730353 0.471907 0.158 Uiso 1 1 calc R U . . .
C19 C 0.3466(6) 0.5957(11) 0.3886(11) 0.120(4) Uani 1 1 d . U . . .
H19A H 0.354213 0.577513 0.323483 0.179 Uiso 1 1 calc R U . . .
H19B H 0.319006 0.560075 0.400151 0.179 Uiso 1 1 calc R U . . .
H19C H 0.374226 0.583567 0.443602 0.179 Uiso 1 1 calc R U . . .
O9 O 0.3563(2) 0.9170(5) 0.1641(4) 0.0746(18) Uani 0.5 1 d D . P A 1
C20 C 0.3795(5) 0.9881(7) 0.1857(12) 0.064(4) Uani 0.5 1 d D U P A 1
H20 H 0.410060 0.985091 0.168178 0.077 Uiso 0.5 1 calc R U P A 1
O10 O 0.3726(5) 1.0622(7) 0.2247(8) 0.076(3) Uani 0.5 1 d D U P A 1
O12 O 0.500000 0.7382(8) 0.250000 0.082(2) Uiso 1 2 d S . P B 1
O9A O 0.3563(2) 0.9170(5) 0.1641(4) 0.0746(18) Uani 0.5 1 d . . P A 2
O11 O 0.4085(12) 1.135(2) 0.253(3) 0.186(12) Uiso 0.5 1 d . . P C 2
O13 O 0.500000 0.8982(17) 0.250000 0.202(9) Uiso 1 2 d S . P D 2
O14 O 0.4561(6) 0.9898(13) 0.0593(14) 0.212(7) Uiso 1 1 d . . . . .
O15 O 0.8734(8) 0.5540(17) 0.9386(19) 0.273(10) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O3 2.458(4) 8_466 ?
La1 O1 2.460(4) 5_665 ?
La1 O4 2.463(4) 2_654 ?
La1 O9A 2.473(6) . ?
La1 O9 2.473(6) . ?
La1 O8 2.511(6) . ?
La1 O6 2.535(4) . ?
La1 O2 2.552(4) 3_455 ?
La1 O7 2.577(4) . ?
La1 O1 2.667(3) 3_455 ?
La1 C16 2.910(5) . ?
La1 C7 2.984(5) 3_455 ?
O1 C7 1.263(6) . ?
O2 C7 1.253(6) . ?
O3 C8 1.254(6) . ?
O4 C8 1.259(7) . ?
O5 C10 1.370(8) . ?
O5 C9 1.444(8) . ?
O6 C16 1.280(7) . ?
O7 C16 1.261(7) . ?
C1 C6 1.395(6) . ?
C1 C2 1.400(6) . ?
C1 C7 1.504(7) . ?
C2 C3 1.396(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(7) . ?
C3 C8 1.517(7) . ?
C4 C5 1.403(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(7) . ?
C5 C9 1.501(7) . ?
C6 H6 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.388(12) . ?
C10 C15 1.390(8) . ?
C11 C12 1.393(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.405(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(7) . ?
C13 C16 1.494(8) . ?
C14 C15 1.399(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O8 C17 1.231(10) . ?
C17 N1 1.284(12) . ?
C17 H17 0.9500 . ?
N1 C18 1.432(14) . ?
N1 C19 1.596(18) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O9 C20 1.228(9) . ?
C20 O10 1.229(9) . ?
C20 H20 0.9500 . ?

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
O3 La1 O1 76.87(14) 8_466 5_665 ?
O3 La1 O4 133.80(14) 8_466 2_654 ?
O1 La1 O4 73.05(13) 5_665 2_654 ?
O3 La1 O9A 71.59(17) 8_466 . ?
O1 La1 O9A 145.06(16) 5_665 . ?
O4 La1 O9A 141.18(17) 2_654 . ?
O3 La1 O9 71.59(17) 8_466 . ?
O1 La1 O9 145.06(16) 5_665 . ?
O4 La1 O9 141.18(17) 2_654 . ?
O3 La1 O8 70.69(18) 8_466 . ?
O1 La1 O8 81.1(2) 5_665 . ?
O4 La1 O8 135.49(18) 2_654 . ?
O9A La1 O8 74.7(2) . . ?
O9 La1 O8 74.7(2) . . ?
O3 La1 O6 143.70(15) 8_466 . ?
O1 La1 O6 137.10(13) 5_665 . ?
O4 La1 O6 78.57(15) 2_654 . ?
O9A La1 O6 72.13(17) . . ?
O9 La1 O6 72.13(17) . . ?
O8 La1 O6 98.3(2) . . ?
O3 La1 O2 90.88(16) 8_466 3_455 ?
O1 La1 O2 121.03(12) 5_665 3_455 ?
O4 La1 O2 76.07(14) 2_654 3_455 ?
O9 La1 O2 74.7(2) . 3_455 ?
O8 La1 O2 147.99(17) . 3_455 ?
O6 La1 O2 81.00(14) . 3_455 ?
O3 La1 O7 142.45(15) 8_466 . ?
O1 La1 O7 88.49(12) 5_665 . ?
O4 La1 O7 70.79(14) 2_654 . ?
O9A La1 O7 107.57(19) . . ?
O9 La1 O7 107.57(19) . . ?
O8 La1 O7 72.99(15) . . ?
O6 La1 O7 51.55(14) . . ?
O2 La1 O7 125.82(13) 3_455 . ?
O3 La1 O1 66.31(14) 8_466 3_455 ?
O1 La1 O1 73.32(13) 5_665 3_455 ?
O4 La1 O1 71.89(13) 2_654 3_455 ?
O9 La1 O1 106.27(19) . 3_455 ?
O8 La1 O1 133.68(17) . 3_455 ?
O6 La1 O1 126.69(13) . 3_455 ?
O2 La1 O1 49.61(11) 3_455 3_455 ?
O7 La1 O1 141.85(13) . 3_455 ?
O3 La1 C16 154.67(15) 8_466 . ?
O1 La1 C16 112.23(14) 5_665 . ?
O4 La1 C16 70.88(15) 2_654 . ?
O9A La1 C16 91.47(19) . . ?
O9 La1 C16 91.47(19) . . ?
O8 La1 C16 86.99(18) . . ?
O6 La1 C16 26.05(15) . . ?
O2 La1 C16 102.93(14) 3_455 . ?
O7 La1 C16 25.66(14) . . ?
O1 La1 C16 138.30(13) 3_455 . ?
O3 La1 C7 77.11(15) 8_466 3_455 ?
O1 La1 C7 97.65(13) 5_665 3_455 ?
O4 La1 C7 73.15(13) 2_654 3_455 ?
O9A La1 C7 89.7(2) . 3_455 ?
O9 La1 C7 89.7(2) . 3_455 ?
O8 La1 C7 147.24(15) . 3_455 ?
O6 La1 C7 104.17(14) . 3_455 ?
O2 La1 C7 24.61(12) 3_455 3_455 ?
O7 La1 C7 139.76(12) . 3_455 ?
O1 La1 C7 25.02(12) 3_455 3_455 ?
C16 La1 C7 122.71(14) . 3_455 ?
C7 O1 La1 157.0(3) . 5_665 ?
C7 O1 La1 91.7(3) . 3_545 ?
La1 O1 La1 106.68(13) 5_665 3_545 ?
C7 O2 La1 97.4(3) . 3_545 ?
C8 O3 La1 139.4(4) . 8_565 ?
C8 O4 La1 133.8(4) . 2_654 ?
C10 O5 C9 117.9(5) . . ?
C16 O6 La1 93.5(3) . . ?
C16 O7 La1 92.1(3) . . ?
C6 C1 C2 119.7(4) . . ?
C6 C1 C7 119.4(4) . . ?
C2 C1 C7 120.8(4) . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 C8 119.6(4) . . ?
C4 C3 C8 120.7(4) . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 119.0(5) . . ?
C6 C5 C9 119.6(5) . . ?
C4 C5 C9 121.4(5) . . ?
C1 C6 C5 120.8(4) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
O2 C7 O1 121.2(4) . . ?
O2 C7 C1 120.5(4) . . ?
O1 C7 C1 118.3(4) . . ?
O2 C7 La1 58.0(3) . 3_545 ?
O1 C7 La1 63.3(2) . 3_545 ?
C1 C7 La1 175.4(3) . 3_545 ?
O3 C8 O4 126.2(5) . . ?
O3 C8 C3 116.3(5) . . ?
O4 C8 C3 117.5(4) . . ?
O5 C9 C5 106.8(5) . . ?
O5 C9 H9A 110.4 . . ?
C5 C9 H9A 110.4 . . ?
O5 C9 H9B 110.4 . . ?
C5 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
O5 C10 C11 115.4(6) . . ?
O5 C10 C15 124.6(6) . . ?
C11 C10 C15 119.9(6) . . ?
C10 C11 C12 120.7(8) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C13 120.1(7) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 118.2(6) . . ?
C14 C13 C16 121.4(5) . . ?
C12 C13 C16 120.4(6) . . ?
C13 C14 C15 122.3(5) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C10 C15 C14 118.8(6) . . ?
C10 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
O7 C16 O6 122.1(5) . . ?
O7 C16 C13 119.2(5) . . ?
O6 C16 C13 118.8(5) . . ?
O7 C16 La1 62.3(3) . . ?
O6 C16 La1 60.4(3) . . ?
C13 C16 La1 172.2(4) . . ?
C17 O8 La1 124.5(5) . . ?
O8 C17 N1 126.3(11) . . ?
O8 C17 H17 116.9 . . ?
N1 C17 H17 116.9 . . ?
C17 N1 C18 124.5(12) . . ?
C17 N1 C19 118.0(9) . . ?
C18 N1 C19 117.3(11) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 La1 157.0(9) . . ?
O9 C20 O10 135.2(15) . . ?
O9 C20 H20 112.4 . . ?
O10 C20 H20 112.4 . . ?

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
C6 C1 C2 C3 -2.0(8) . . . . ?
C7 C1 C2 C3 176.0(5) . . . . ?
C1 C2 C3 C4 1.9(8) . . . . ?
C1 C2 C3 C8 -175.4(5) . . . . ?
C2 C3 C4 C5 0.5(9) . . . . ?
C8 C3 C4 C5 177.8(5) . . . . ?
C3 C4 C5 C6 -2.6(9) . . . . ?
C3 C4 C5 C9 177.2(6) . . . . ?
C2 C1 C6 C5 -0.2(8) . . . . ?
C7 C1 C6 C5 -178.2(5) . . . . ?
C4 C5 C6 C1 2.5(9) . . . . ?
C9 C5 C6 C1 -177.4(5) . . . . ?
La1 O2 C7 O1 -3.7(5) 3_545 . . . ?
La1 O2 C7 C1 174.9(4) 3_545 . . . ?
La1 O1 C7 O2 -140.0(7) 5_665 . . . ?
La1 O1 C7 O2 3.5(5) 3_545 . . . ?
La1 O1 C7 C1 41.3(10) 5_665 . . . ?
La1 O1 C7 C1 -175.2(4) 3_545 . . . ?
La1 O1 C7 La1 -143.6(8) 5_665 . . 3_545 ?
C6 C1 C7 O2 -157.5(5) . . . . ?
C2 C1 C7 O2 24.4(7) . . . . ?
C6 C1 C7 O1 21.2(7) . . . . ?
C2 C1 C7 O1 -156.9(5) . . . . ?
La1 O3 C8 O4 -14.5(11) 8_565 . . . ?
La1 O3 C8 C3 164.7(5) 8_565 . . . ?
La1 O4 C8 O3 34.9(10) 2_654 . . . ?
La1 O4 C8 C3 -144.3(4) 2_654 . . . ?
C2 C3 C8 O3 -0.8(8) . . . . ?
C4 C3 C8 O3 -178.1(6) . . . . ?
C2 C3 C8 O4 178.4(5) . . . . ?
C4 C3 C8 O4 1.1(8) . . . . ?
C10 O5 C9 C5 -170.7(6) . . . . ?
C6 C5 C9 O5 120.3(6) . . . . ?
C4 C5 C9 O5 -59.5(8) . . . . ?
C9 O5 C10 C11 -175.2(8) . . . . ?
C9 O5 C10 C15 2.9(12) . . . . ?
O5 C10 C11 C12 -178.5(10) . . . . ?
C15 C10 C11 C12 3.4(15) . . . . ?
C10 C11 C12 C13 -1.1(16) . . . . ?
C11 C12 C13 C14 0.0(13) . . . . ?
C11 C12 C13 C16 -179.4(8) . . . . ?
C12 C13 C14 C15 -1.1(9) . . . . ?
C16 C13 C14 C15 178.2(5) . . . . ?
O5 C10 C15 C14 177.6(7) . . . . ?
C11 C10 C15 C14 -4.5(11) . . . . ?
C13 C14 C15 C10 3.4(9) . . . . ?
La1 O7 C16 O6 8.9(5) . . . . ?
La1 O7 C16 C13 -171.3(4) . . . . ?
La1 O6 C16 O7 -9.0(5) . . . . ?
La1 O6 C16 C13 171.2(4) . . . . ?
C14 C13 C16 O7 17.0(8) . . . . ?
C12 C13 C16 O7 -163.7(7) . . . . ?
C14 C13 C16 O6 -163.2(5) . . . . ?
C12 C13 C16 O6 16.2(9) . . . . ?
La1 O8 C17 N1 145.6(9) . . . . ?
O8 C17 N1 C18 -176.9(12) . . . . ?
O8 C17 N1 C19 9.2(19) . . . . ?
La1 O9 C20 O10 131(2) . . . . ?

_refine_diff_density_max         2.619
_refine_diff_density_min         -4.353
_refine_diff_density_rms         0.223

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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data_8R-Er-RT
_database_code_depnum_ccdc_archive 'CCDC 1574650'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_8R-Er-RT            
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         9.0 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the Er centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_8R-Er-RT            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Er2(C16H9O7)2(C3H7ON)3(CHOOH)]??3H2O'
_chemical_formula_sum            'C42 H47 Er2 N3 O22'
_chemical_formula_weight         1280.34

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'
N N 0.0061 0.0033 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.4713(18)
_cell_length_b                   14.2708(9)
_cell_length_c                   13.6430(9)
_cell_angle_alpha                90
_cell_angle_beta                 97.961(2)
_cell_angle_gamma                90
_cell_volume                     5489.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9445
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_F_000             2528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    3.110
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26350
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.846
_diffrn_reflns_theta_max         28.317
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6790
_reflns_number_gt                5994
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0275P)²+42.5969P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6790
_refine_ls_number_parameters     316
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.165
_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 0.81706(2) 0.70819(2) 0.53896(2) 0.01815(6) Uani 1 1 d . . . . .
O1 O 0.76563(9) 0.6478(2) 0.6440(2) 0.0307(6) Uani 1 1 d . . . . .
O2 O 0.69582(10) 0.7229(2) 0.6174(2) 0.0281(6) Uani 1 1 d . . . . .
O3 O 0.73055(10) 0.66483(19) 0.4457(2) 0.0280(6) Uani 1 1 d . . . . .
O4 O 0.79279(10) 0.5771(2) 0.4348(2) 0.0328(6) Uani 1 1 d . . . . .
O5 O 0.57666(11) 0.6462(2) 0.8497(3) 0.0520(10) Uani 1 1 d . U . . .
O6 O 0.38983(10) 0.8247(2) 0.9750(3) 0.0387(7) Uani 1 1 d . . . . .
O7 O 0.38152(11) 0.6811(2) 1.0257(3) 0.0439(8) Uani 1 1 d . . . . .
C1 C 0.70530(13) 0.6012(3) 0.7353(3) 0.0232(7) Uani 1 1 d . . . . .
C2 C 0.73536(12) 0.5382(3) 0.7911(3) 0.0247(7) Uani 1 1 d . . . . .
H2 H 0.767298 0.535682 0.783429 0.030 Uiso 1 1 calc R U . . .
C3 C 0.71766(13) 0.4790(3) 0.8581(3) 0.0245(7) Uani 1 1 d . . . . .
C4 C 0.67025(13) 0.4843(3) 0.8717(3) 0.0280(8) Uani 1 1 d . . . . .
H4 H 0.658558 0.444636 0.916720 0.034 Uiso 1 1 calc R U . . .
C5 C 0.64027(13) 0.5486(3) 0.8184(3) 0.0287(8) Uani 1 1 d . . . . .
C6 C 0.65774(13) 0.6062(3) 0.7495(3) 0.0282(8) Uani 1 1 d . . . . .
H6 H 0.637577 0.648331 0.712529 0.034 Uiso 1 1 calc R U . . .
C7 C 0.72361(12) 0.6625(3) 0.6593(3) 0.0230(7) Uani 1 1 d . . . . .
C8 C 0.74906(13) 0.5918(3) 0.4158(3) 0.0233(7) Uani 1 1 d . . . . .
C9 C 0.58885(14) 0.5517(3) 0.8345(4) 0.0370(10) Uani 1 1 d . . . . .
H9A H 0.568885 0.526533 0.777219 0.044 Uiso 1 1 calc R U . . .
H9B H 0.584249 0.514356 0.891803 0.044 Uiso 1 1 calc R U . . .
C10 C 0.53330(15) 0.6630(4) 0.8790(4) 0.0417(11) Uani 1 1 d . . . . .
C11 C 0.52184(19) 0.7568(4) 0.8862(5) 0.0609(16) Uani 1 1 d . U . . .
H11 H 0.542244 0.802680 0.868325 0.073 Uiso 1 1 calc R U . . .
C12 C 0.47990(18) 0.7822(4) 0.9200(5) 0.0539(14) Uani 1 1 d . U . . .
H12 H 0.472477 0.845343 0.925353 0.065 Uiso 1 1 calc R U . . .
C13 C 0.44883(14) 0.7143(3) 0.9461(4) 0.0346(9) Uani 1 1 d . . . . .
C14 C 0.46033(15) 0.6215(3) 0.9361(4) 0.0382(10) Uani 1 1 d . . . . .
H14 H 0.439639 0.575425 0.952352 0.046 Uiso 1 1 calc R U . . .
C15 C 0.50244(15) 0.5951(3) 0.9021(4) 0.0394(10) Uani 1 1 d . . . . .
H15 H 0.509530 0.532085 0.895033 0.047 Uiso 1 1 calc R U . . .
C16 C 0.40422(13) 0.7416(3) 0.9846(3) 0.0320(9) Uani 1 1 d . . . . .
O8 O 0.85513(14) 0.5793(3) 0.6260(3) 0.0607(11) Uani 0.75 1 d D . P A 1
C17 C 0.8409(3) 0.5012(5) 0.6342(6) 0.078(2) Uani 0.75 1 d D U P A 1
H17 H 0.815237 0.481549 0.589259 0.094 Uiso 0.75 1 calc R U P A 1
N1 N 0.8591(4) 0.4404(6) 0.7031(7) 0.124(3) Uani 0.75 1 d . U P A 1
C18 C 0.8435(5) 0.3522(10) 0.7125(10) 0.108(4) Uani 0.75 1 d . U P A 1
H18A H 0.862331 0.322285 0.767542 0.161 Uiso 0.75 1 calc R U P A 1
H18B H 0.810947 0.353640 0.723545 0.161 Uiso 0.75 1 calc R U P A 1
H18C H 0.846119 0.317711 0.653047 0.161 Uiso 0.75 1 calc R U P A 1
C19 C 0.8935(8) 0.4646(16) 0.7806(15) 0.208(10) Uani 0.75 1 d . U P A 1
H19A H 0.882975 0.517778 0.814765 0.312 Uiso 0.75 1 calc R U P A 1
H19B H 0.922373 0.480097 0.755302 0.312 Uiso 0.75 1 calc R U P A 1
H19C H 0.899081 0.412802 0.825582 0.312 Uiso 0.75 1 calc R U P A 1
O9 O 0.84645(16) 0.7640(3) 0.7017(3) 0.0645(12) Uani 0.75 1 d . . P A 1
C20 C 0.8394(4) 0.7380(10) 0.7791(8) 0.127(4) Uani 0.75 1 d . U P A 1
H20 H 0.827980 0.677107 0.781601 0.152 Uiso 0.75 1 calc R U P A 1
N2 N 0.8459(4) 0.7856(9) 0.8673(7) 0.167(4) Uani 0.75 1 d . U P A 1
C21 C 0.8700(7) 0.8710(15) 0.8775(15) 0.173(8) Uani 0.75 1 d . U P A 1
H21A H 0.899369 0.865516 0.850873 0.260 Uiso 0.75 1 calc R U P A 1
H21B H 0.876334 0.887400 0.946260 0.260 Uiso 0.75 1 calc R U P A 1
H21C H 0.850815 0.918783 0.842220 0.260 Uiso 0.75 1 calc R U P A 1
C22 C 0.8445(9) 0.7184(17) 0.9628(13) 0.204(10) Uani 0.75 1 d . U P A 1
H22A H 0.848097 0.654278 0.943928 0.305 Uiso 0.75 1 calc R U P A 1
H22B H 0.814756 0.726093 0.987324 0.305 Uiso 0.75 1 calc R U P A 1
H22C H 0.869940 0.735132 1.013587 0.305 Uiso 0.75 1 calc R U P A 1
O8A O 0.85513(14) 0.5793(3) 0.6260(3) 0.0607(11) Uani 0.25 1 d . . P A 2
C17A C 0.8409(3) 0.5012(5) 0.6342(6) 0.078(2) Uani 0.25 1 d . . P A 2
H17A H 0.815237 0.481549 0.589259 0.094 Uiso 0.25 1 calc R U P A 2
O10 O 0.8591(4) 0.4404(6) 0.7031(7) 0.124(3) Uani 0.25 1 d . . P A 2
O9A O 0.84645(16) 0.7640(3) 0.7017(3) 0.0645(12) Uani 0.25 1 d . . P A 2
C20A C 0.8394(4) 0.7380(10) 0.7791(8) 0.127(4) Uani 0.25 1 d . . P A 2
H20A H 0.827980 0.677107 0.781601 0.152 Uiso 0.25 1 calc R U P A 2
O11 O 0.8459(4) 0.7856(9) 0.8673(7) 0.167(4) Uani 0.25 1 d . . P A 2
O12 O 0.500000 0.7756(19) 0.250000 0.328(11) Uiso 1 2 d S . P . .
O13 O 0.4369(7) 0.0107(15) 0.0176(14) 0.337(9) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O3 2.290(3) 7_666 ?
Er1 O2 2.331(3) 7_666 ?
Er1 O1 2.350(3) . ?
Er1 O8A 2.368(4) . ?
Er1 O8 2.368(4) . ?
Er1 O4 2.392(3) . ?
Er1 O9 2.398(4) . ?
Er1 O9A 2.398(4) . ?
Er1 O6 2.403(3) 8_565 ?
Er1 O7 2.447(3) 8_565 ?
Er1 O3 2.683(3) . ?
Er1 C16 2.781(4) 8_565 ?
O1 C7 1.260(4) . ?
O2 C7 1.253(4) . ?
O3 C8 1.262(4) . ?
O4 C8 1.254(5) . ?
O5 C10 1.371(5) . ?
O5 C9 1.414(6) . ?
O6 C16 1.256(5) . ?
O7 C16 1.256(5) . ?
C1 C2 1.393(5) . ?
C1 C6 1.396(5) . ?
C1 C7 1.504(5) . ?
C2 C3 1.390(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(5) . ?
C3 C8 1.498(5) 6_566 ?
C4 C5 1.389(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(5) . ?
C5 C9 1.511(5) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.373(6) . ?
C10 C11 1.384(8) . ?
C11 C12 1.387(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.391(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(6) . ?
C13 C16 1.491(5) . ?
C14 C15 1.396(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O8 C17 1.197(7) . ?
C17 N1 1.331(10) . ?
C17 H17 0.9300 . ?
N1 C18 1.348(15) . ?
N1 C19 1.38(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O9 C20 1.163(11) . ?
C20 N2 1.372(14) . ?
C20 H20 0.9300 . ?
N2 C21 1.40(2) . ?
N2 C22 1.62(2) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
O8A C17A 1.197(7) . ?
C17A O10 1.331(10) . ?
C17A H17A 0.9300 . ?
O9A C20A 1.163(11) . ?
C20A O11 1.372(14) . ?
C20A H20A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Er1 O2 74.29(10) 7_666 7_666 ?
O3 Er1 O1 78.92(10) 7_666 . ?
O2 Er1 O1 132.86(10) 7_666 . ?
O3 Er1 O8A 143.55(13) 7_666 . ?
O2 Er1 O8A 142.13(13) 7_666 . ?
O1 Er1 O8A 71.95(11) . . ?
O3 Er1 O8 143.55(13) 7_666 . ?
O2 Er1 O8 142.13(13) 7_666 . ?
O1 Er1 O8 71.95(11) . . ?
O3 Er1 O4 123.16(10) 7_666 . ?
O2 Er1 O4 77.93(11) 7_666 . ?
O1 Er1 O4 85.53(11) . . ?
O8A Er1 O4 76.41(15) . . ?
O8 Er1 O4 76.41(15) . . ?
O3 Er1 O9 77.74(15) 7_666 . ?
O2 Er1 O9 134.21(13) 7_666 . ?
O1 Er1 O9 74.00(13) . . ?
O8 Er1 O9 73.56(17) . . ?
O4 Er1 O9 147.64(14) . . ?
O3 Er1 O9A 77.74(15) 7_666 . ?
O2 Er1 O9A 134.21(13) 7_666 . ?
O1 Er1 O9A 74.00(13) . . ?
O8A Er1 O9A 73.56(17) . . ?
O4 Er1 O9A 147.64(14) . . ?
O3 Er1 O6 137.62(10) 7_666 8_565 ?
O2 Er1 O6 77.55(11) 7_666 8_565 ?
O1 Er1 O6 142.31(11) . 8_565 ?
O8 Er1 O6 70.90(12) . 8_565 ?
O4 Er1 O6 79.88(10) . 8_565 ?
O9 Er1 O6 101.15(15) . 8_565 ?
O3 Er1 O7 87.44(11) 7_666 8_565 ?
O2 Er1 O7 71.61(12) 7_666 8_565 ?
O1 Er1 O7 144.98(11) . 8_565 ?
O8 Er1 O7 104.03(14) . 8_565 ?
O4 Er1 O7 128.24(10) . 8_565 ?
O9 Er1 O7 71.63(13) . 8_565 ?
O6 Er1 O7 53.57(11) 8_565 8_565 ?
O3 Er1 O3 73.11(10) 7_666 . ?
O2 Er1 O3 69.26(9) 7_666 . ?
O1 Er1 O3 66.15(9) . . ?
O8A Er1 O3 112.63(13) . . ?
O8 Er1 O3 112.63(13) . . ?
O4 Er1 O3 50.76(9) . . ?
O9 Er1 O3 134.04(13) . . ?
O9A Er1 O3 134.04(13) . . ?
O6 Er1 O3 124.32(10) 8_565 . ?
O7 Er1 O3 139.69(11) 8_565 . ?
O3 Er1 C16 112.45(12) 7_666 8_565 ?
O2 Er1 C16 71.35(11) 7_666 8_565 ?
O1 Er1 C16 155.76(11) . 8_565 ?
O8A Er1 C16 88.31(13) . 8_565 ?
O8 Er1 C16 88.31(13) . 8_565 ?
O4 Er1 C16 103.78(12) . 8_565 ?
O9 Er1 C16 87.23(14) . 8_565 ?
O9A Er1 C16 87.23(14) . 8_565 ?
O6 Er1 C16 26.79(12) 8_565 8_565 ?
O7 Er1 C16 26.85(12) 8_565 8_565 ?
O3 Er1 C16 136.68(11) . 8_565 ?
C7 O1 Er1 136.6(2) . . ?
C7 O2 Er1 135.8(2) . 7_666 ?
C8 O3 Er1 164.3(3) . 7_666 ?
C8 O3 Er1 87.0(2) . . ?
Er1 O3 Er1 106.89(10) 7_666 . ?
C8 O4 Er1 100.9(2) . . ?
C10 O5 C9 117.4(4) . . ?
C16 O6 Er1 93.6(2) . 8_466 ?
C16 O7 Er1 91.6(3) . 8_466 ?
C2 C1 C6 119.5(3) . . ?
C2 C1 C7 120.4(3) . . ?
C6 C1 C7 120.1(3) . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 C8 120.7(3) . 6_566 ?
C4 C3 C8 119.1(3) . 6_566 ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 C9 118.7(3) . . ?
C6 C5 C9 121.7(3) . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O2 C7 O1 126.4(3) . . ?
O2 C7 C1 117.2(3) . . ?
O1 C7 C1 116.4(3) . . ?
O4 C8 O3 121.2(3) . . ?
O4 C8 C3 120.0(3) . 6_565 ?
O3 C8 C3 118.8(3) . 6_565 ?
O4 C8 Er1 53.98(19) . . ?
O3 C8 Er1 67.3(2) . . ?
C3 C8 Er1 172.5(3) 6_565 . ?
O5 C9 C5 108.2(4) . . ?
O5 C9 H9A 110.1 . . ?
C5 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C5 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O5 C10 C15 125.0(4) . . ?
O5 C10 C11 114.9(4) . . ?
C15 C10 C11 120.1(4) . . ?
C10 C11 C12 119.9(5) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.7(5) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 118.5(4) . . ?
C14 C13 C16 120.8(4) . . ?
C12 C13 C16 120.7(4) . . ?
C13 C14 C15 121.3(4) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C10 C15 C14 119.5(4) . . ?
C10 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
O6 C16 O7 121.0(4) . . ?
O6 C16 C13 119.4(4) . . ?
O7 C16 C13 119.6(4) . . ?
O6 C16 Er1 59.6(2) . 8_466 ?
O7 C16 Er1 61.6(2) . 8_466 ?
C13 C16 Er1 174.9(3) . 8_466 ?
C17 O8 Er1 129.3(5) . . ?
O8 C17 N1 124.7(9) . . ?
O8 C17 H17 117.6 . . ?
N1 C17 H17 117.6 . . ?
C17 N1 C18 125.1(12) . . ?
C17 N1 C19 122.9(12) . . ?
C18 N1 C19 111.7(12) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Er1 130.8(6) . . ?
O9 C20 N2 128.2(12) . . ?
O9 C20 H20 115.9 . . ?
N2 C20 H20 115.9 . . ?
C20 N2 C21 121.6(14) . . ?
C20 N2 C22 113.3(14) . . ?
C21 N2 C22 120.2(14) . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17A O8A Er1 129.3(5) . . ?
O8A C17A O10 124.7(9) . . ?
O8A C17A H17A 117.6 . . ?
O10 C17A H17A 117.6 . . ?
C20A O9A Er1 130.8(6) . . ?
O9A C20A O11 128.2(12) . . ?
O9A C20A H20A 115.9 . . ?
O11 C20A H20A 115.9 . . ?

_refine_diff_density_max         1.250
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_3R-Pr-RT2
_database_code_depnum_ccdc_archive 'CCDC 1574654'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT043_3R-Pr-RT2           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      13.11 Check
RESPONSE:13 H atoms should be attached to severely disordered O atoms 
of water or formic acid, for which the disorder could not eliminated 
although we have applied several restaints to limit it. Thus,these H atoms 
were omitted due to refinement instability and disordered solvent
;
_vrf_PLAT220_3R-Pr-RT2           
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         8.0 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the Pr centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_3R-Pr-RT2           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Pr2(C16H9O7)2(C3H7ON)2(H2O)(CHOOH)]??5H2O'
_chemical_formula_sum            'C39 H46 N2 O24 Pr2'
_chemical_formula_weight         1208.60

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'
N N 0.0061 0.0033 '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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.480(4)
_cell_length_b                   14.4960(15)
_cell_length_c                   13.6564(14)
_cell_angle_alpha                90
_cell_angle_beta                 100.308(5)
_cell_angle_gamma                90
_cell_volume                     5547.0(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9210
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      26.42

_exptl_crystal_description       block
_exptl_crystal_colour            aqua
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             2416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.810
_shelx_estimated_absorpt_T_min   0.641
_shelx_estimated_absorpt_T_max   0.660
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65301
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.801
_diffrn_reflns_theta_max         26.836
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5824
_reflns_number_gt                4777
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0677P)²+46.4163P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5824
_refine_ls_number_parameters     305
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1294
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.111
_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
Pr1 Pr 0.31981(2) 0.78879(2) 0.55002(2) 0.02093(11) Uani 1 1 d . . . . .
O1 O 0.30707(14) 0.7219(3) 0.3823(3) 0.0338(9) Uani 1 1 d . . . . .
O2 O 0.23502(13) 0.6567(3) 0.3428(3) 0.0395(10) Uani 1 1 d . . . . .
O3 O 0.20396(13) 0.4289(3) 0.0610(3) 0.0387(10) Uani 1 1 d . . . . .
O4 O 0.26593(13) 0.3424(2) 0.0498(3) 0.0283(8) Uani 1 1 d . . . . .
O5 O 0.42132(16) 0.6451(3) 0.1421(4) 0.0609(15) Uani 1 1 d . . . . .
O6 O 0.60106(14) 0.8213(3) -0.0006(4) 0.0445(11) Uani 1 1 d . . . . .
O7 O 0.61261(14) 0.6760(3) -0.0362(3) 0.0430(10) Uani 1 1 d . . . . .
C1 C 0.29537(18) 0.6059(4) 0.2585(4) 0.0278(11) Uani 1 1 d . . . . .
C2 C 0.26419(18) 0.5444(4) 0.2013(4) 0.0275(11) Uani 1 1 d . . . . .
H2 H 0.232089 0.543953 0.206652 0.033 Uiso 1 1 calc R U . . .
C3 C 0.28076(18) 0.4841(3) 0.1366(4) 0.0247(10) Uani 1 1 d . . . . .
C4 C 0.32865(18) 0.4878(4) 0.1263(4) 0.0280(11) Uani 1 1 d . . . . .
H4 H 0.339823 0.447681 0.082453 0.034 Uiso 1 1 calc R U . . .
C5 C 0.35948(18) 0.5499(4) 0.1800(4) 0.0303(12) Uani 1 1 d . . . . .
C6 C 0.34321(18) 0.6081(4) 0.2473(4) 0.0294(12) Uani 1 1 d . . . . .
H6 H 0.364242 0.648899 0.285195 0.035 Uiso 1 1 calc R U . . .
C7 C 0.27769(19) 0.6668(4) 0.3345(4) 0.0286(11) Uani 1 1 d . . . . .
C8 C 0.24809(18) 0.4148(3) 0.0792(4) 0.0248(11) Uani 1 1 d . . . . .
C9 C 0.4107(2) 0.5525(4) 0.1663(5) 0.0382(14) Uani 1 1 d . . . . .
H9A H 0.431537 0.533338 0.227059 0.046 Uiso 1 1 calc R U . . .
H9B H 0.415422 0.511109 0.113164 0.046 Uiso 1 1 calc R U . . .
C10 C 0.4629(2) 0.6619(5) 0.1083(6) 0.0478(17) Uani 1 1 d . . . . .
C11 C 0.4714(3) 0.7518(6) 0.0890(8) 0.072(2) Uani 1 1 d . U . . .
H11 H 0.449712 0.796729 0.100303 0.087 Uiso 1 1 calc R U . . .
C12 C 0.5121(3) 0.7775(5) 0.0525(7) 0.065(2) Uani 1 1 d . U . . .
H12 H 0.517216 0.839102 0.038359 0.078 Uiso 1 1 calc R U . . .
C13 C 0.5453(2) 0.7103(4) 0.0373(5) 0.0359(13) Uani 1 1 d . . . . .
C14 C 0.5361(2) 0.6207(4) 0.0581(5) 0.0381(14) Uani 1 1 d . . . . .
H14 H 0.557692 0.575261 0.047316 0.046 Uiso 1 1 calc R U . . .
C15 C 0.4958(2) 0.5956(4) 0.0945(5) 0.0424(15) Uani 1 1 d . . . . .
H15 H 0.490874 0.534215 0.109635 0.051 Uiso 1 1 calc R U . . .
C16 C 0.58868(19) 0.7368(4) -0.0022(4) 0.0334(13) Uani 1 1 d . . . . .
O8 O 0.3473(2) 0.7240(4) 0.7215(4) 0.0578(14) Uani 1 1 d . . . . .
C17 C 0.3369(4) 0.7510(9) 0.7985(8) 0.095(3) Uani 1 1 d . U . . .
H17 H 0.328451 0.812767 0.801012 0.114 Uiso 1 1 calc R U . . .
N1 N 0.3363(4) 0.7011(8) 0.8801(6) 0.105(3) Uani 1 1 d . U . . .
C18 C 0.3261(8) 0.7456(16) 0.9719(12) 0.195(8) Uani 1 1 d . U . . .
H18A H 0.331215 0.810878 0.968579 0.293 Uiso 1 1 calc R U . . .
H18B H 0.346846 0.720578 1.028831 0.293 Uiso 1 1 calc R U . . .
H18C H 0.293469 0.734092 0.977650 0.293 Uiso 1 1 calc R U . . .
C19 C 0.3540(8) 0.6115(12) 0.8873(12) 0.171(7) Uani 1 1 d . U . . .
H19A H 0.356174 0.589120 0.822134 0.256 Uiso 1 1 calc R U . . .
H19B H 0.332957 0.572607 0.916433 0.256 Uiso 1 1 calc R U . . .
H19C H 0.385128 0.611018 0.928375 0.256 Uiso 1 1 calc R U . . .
O9 O 0.3573(2) 0.9205(4) 0.6487(4) 0.0727(17) Uani 0.5 1 d D . P A 1
C20 C 0.3466(5) 1.0015(6) 0.6584(9) 0.050(3) Uani 0.5 1 d D U P A 1
H20A H 0.319364 1.022987 0.616607 0.061 Uiso 0.5 1 calc R U P A 1
O10 O 0.3691(4) 1.0592(7) 0.7203(7) 0.061(3) Uani 0.5 1 d D U P A 1
O9A O 0.3573(2) 0.9205(4) 0.6487(4) 0.0727(17) Uani 0.5 1 d . . P A 2
O11 O 0.3564(8) 1.1423(15) 0.7328(15) 0.145(7) Uiso 0.5 1 d . . P B 2
O12 O 0.500000 0.7511(15) 0.750000 0.197(7) Uiso 1 2 d S . P . .
O13 O 0.5450(5) 0.9956(9) 0.9583(9) 0.185(5) Uiso 1 1 d . . . . .
O14 O 0.3621(10) 0.924(2) 0.933(2) 0.196(10) Uiso 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O4 2.443(3) 6_566 ?
Pr1 O1 2.453(4) . ?
Pr1 O2 2.455(3) 7_566 ?
Pr1 O9 2.468(5) . ?
Pr1 O9A 2.468(5) . ?
Pr1 O6 2.510(4) 2_655 ?
Pr1 O8 2.514(5) . ?
Pr1 O3 2.552(4) 4 ?
Pr1 O7 2.558(4) 2_655 ?
Pr1 O4 2.690(4) 4 ?
Pr1 C16 2.897(5) 2_655 ?
Pr1 C8 2.995(5) 4 ?
O1 C7 1.252(7) . ?
O2 C7 1.249(6) . ?
O3 C8 1.253(6) . ?
O4 C8 1.263(6) . ?
O5 C10 1.369(7) . ?
O5 C9 1.427(7) . ?
O6 C16 1.273(7) . ?
O7 C16 1.253(7) . ?
C1 C2 1.394(7) . ?
C1 C6 1.398(7) . ?
C1 C7 1.516(7) . ?
C2 C3 1.385(7) . ?
C3 C4 1.397(7) . ?
C3 C8 1.492(7) . ?
C4 C5 1.375(7) . ?
C5 C6 1.387(7) . ?
C5 C9 1.504(7) . ?
C10 C11 1.359(11) . ?
C10 C15 1.379(9) . ?
C11 C12 1.392(10) . ?
C12 C13 1.400(9) . ?
C13 C14 1.364(8) . ?
C13 C16 1.483(7) . ?
C14 C15 1.379(8) . ?
O8 C17 1.206(11) . ?
C17 N1 1.331(14) . ?
N1 C19 1.390(18) . ?
N1 C18 1.484(17) . ?
O9 C20 1.226(8) . ?
C20 O10 1.278(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Pr1 O1 72.75(13) 6_566 . ?
O4 Pr1 O2 77.56(13) 6_566 7_566 ?
O1 Pr1 O2 132.87(13) . 7_566 ?
O4 Pr1 O9 144.42(16) 6_566 . ?
O1 Pr1 O9 142.46(17) . . ?
O2 Pr1 O9 71.62(16) 7_566 . ?
O4 Pr1 O9A 144.42(16) 6_566 . ?
O1 Pr1 O9A 142.46(17) . . ?
O2 Pr1 O9A 71.62(16) 7_566 . ?
O4 Pr1 O6 137.71(13) 6_566 2_655 ?
O1 Pr1 O6 79.22(14) . 2_655 ?
O2 Pr1 O6 142.92(14) 7_566 2_655 ?
O9 Pr1 O6 71.33(16) . 2_655 ?
O4 Pr1 O8 78.52(16) 6_566 . ?
O1 Pr1 O8 133.73(16) . . ?
O2 Pr1 O8 71.92(16) 7_566 . ?
O9 Pr1 O8 75.4(2) . . ?
O9A Pr1 O8 75.4(2) . . ?
O6 Pr1 O8 100.14(17) 2_655 . ?
O4 Pr1 O3 121.25(12) 6_566 4 ?
O1 Pr1 O3 77.32(14) . 4 ?
O2 Pr1 O3 88.22(14) 7_566 4 ?
O9 Pr1 O3 75.64(19) . 4 ?
O6 Pr1 O3 81.16(13) 2_655 4 ?
O8 Pr1 O3 148.84(16) . 4 ?
O4 Pr1 O7 89.04(13) 6_566 2_655 ?
O1 Pr1 O7 70.50(15) . 2_655 ?
O2 Pr1 O7 144.80(15) 7_566 2_655 ?
O9 Pr1 O7 106.07(18) . 2_655 ?
O6 Pr1 O7 51.43(13) 2_655 2_655 ?
O8 Pr1 O7 73.57(15) . 2_655 ?
O3 Pr1 O7 126.01(13) 4 2_655 ?
O4 Pr1 O4 73.21(12) 6_566 4 ?
O1 Pr1 O4 70.83(13) . 4 ?
O2 Pr1 O4 65.97(13) 7_566 4 ?
O9 Pr1 O4 108.59(17) . 4 ?
O6 Pr1 O4 125.92(13) 2_655 4 ?
O8 Pr1 O4 133.07(15) . 4 ?
O3 Pr1 O4 49.36(11) 4 4 ?
O7 Pr1 O4 140.72(14) 2_655 4 ?
O4 Pr1 C16 112.80(15) 6_566 2_655 ?
O1 Pr1 C16 71.07(15) . 2_655 ?
O2 Pr1 C16 155.79(15) 7_566 2_655 ?
O9 Pr1 C16 90.30(18) . 2_655 ?
O9A Pr1 C16 90.30(18) . 2_655 ?
O6 Pr1 C16 25.99(16) 2_655 2_655 ?
O8 Pr1 C16 88.30(17) . 2_655 ?
O3 Pr1 C16 103.10(15) 4 2_655 ?
O7 Pr1 C16 25.60(15) 2_655 2_655 ?
O4 Pr1 C16 137.09(14) 4 2_655 ?
O4 Pr1 C8 97.75(13) 6_566 4 ?
O1 Pr1 C8 73.68(14) . 4 ?
O2 Pr1 C8 75.08(14) 7_566 4 ?
O9 Pr1 C8 91.19(18) . 4 ?
O6 Pr1 C8 104.07(14) 2_655 4 ?
O8 Pr1 C8 146.83(15) . 4 ?
O3 Pr1 C8 24.48(13) 4 4 ?
O7 Pr1 C8 139.59(14) 2_655 4 ?
O4 Pr1 C8 24.93(12) 4 4 ?
C16 Pr1 C8 122.53(15) 2_655 4 ?
C7 O1 Pr1 135.4(3) . . ?
C7 O2 Pr1 138.5(4) . 7_566 ?
C8 O3 Pr1 98.0(3) . 4_545 ?
C8 O4 Pr1 159.3(3) . 6_565 ?
C8 O4 Pr1 91.2(3) . 4_545 ?
Pr1 O4 Pr1 106.79(12) 6_565 4_545 ?
C10 O5 C9 118.5(5) . . ?
C16 O6 Pr1 94.2(3) . 2_655 ?
C16 O7 Pr1 92.5(3) . 2_655 ?
C2 C1 C6 119.3(5) . . ?
C2 C1 C7 120.0(4) . . ?
C6 C1 C7 120.7(5) . . ?
C3 C2 C1 120.4(5) . . ?
C2 C3 C4 119.4(5) . . ?
C2 C3 C8 120.6(4) . . ?
C4 C3 C8 120.1(4) . . ?
C5 C4 C3 120.8(5) . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 C9 119.4(5) . . ?
C6 C5 C9 120.9(5) . . ?
C5 C6 C1 120.4(5) . . ?
O2 C7 O1 126.7(5) . . ?
O2 C7 C1 116.2(5) . . ?
O1 C7 C1 117.1(4) . . ?
O3 C8 O4 121.2(5) . . ?
O3 C8 C3 120.3(4) . . ?
O4 C8 C3 118.5(4) . . ?
O3 C8 Pr1 57.6(3) . 4_545 ?
O4 C8 Pr1 63.9(3) . 4_545 ?
C3 C8 Pr1 174.9(4) . 4_545 ?
O5 C9 C5 107.6(5) . . ?
C11 C10 O5 115.5(6) . . ?
C11 C10 C15 119.5(6) . . ?
O5 C10 C15 124.9(6) . . ?
C10 C11 C12 121.0(7) . . ?
C11 C12 C13 119.7(7) . . ?
C14 C13 C12 118.1(5) . . ?
C14 C13 C16 121.7(5) . . ?
C12 C13 C16 120.1(6) . . ?
C13 C14 C15 122.0(5) . . ?
C10 C15 C14 119.7(6) . . ?
O7 C16 O6 121.0(5) . . ?
O7 C16 C13 119.7(5) . . ?
O6 C16 C13 119.2(5) . . ?
O7 C16 Pr1 61.9(3) . 2_655 ?
O6 C16 Pr1 59.8(3) . 2_655 ?
C13 C16 Pr1 171.8(4) . 2_655 ?
C17 O8 Pr1 127.4(6) . . ?
O8 C17 N1 126.6(12) . . ?
C17 N1 C19 120.5(11) . . ?
C17 N1 C18 120.3(13) . . ?
C19 N1 C18 118.0(13) . . ?
C20 O9 Pr1 135.0(7) . . ?
O9 C20 O10 126.3(12) . . ?

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
C6 C1 C2 C3 2.2(8) . . . . ?
C7 C1 C2 C3 -175.6(5) . . . . ?
C1 C2 C3 C4 -2.5(8) . . . . ?
C1 C2 C3 C8 176.8(5) . . . . ?
C2 C3 C4 C5 0.6(8) . . . . ?
C8 C3 C4 C5 -178.7(5) . . . . ?
C3 C4 C5 C6 1.7(9) . . . . ?
C3 C4 C5 C9 -179.5(5) . . . . ?
C4 C5 C6 C1 -1.9(9) . . . . ?
C9 C5 C6 C1 179.2(6) . . . . ?
C2 C1 C6 C5 0.0(9) . . . . ?
C7 C1 C6 C5 177.8(5) . . . . ?
Pr1 O2 C7 O1 -6.9(10) 7_566 . . . ?
Pr1 O2 C7 C1 173.1(4) 7_566 . . . ?
Pr1 O1 C7 O2 31.5(9) . . . . ?
Pr1 O1 C7 C1 -148.5(4) . . . . ?
C2 C1 C7 O2 1.3(8) . . . . ?
C6 C1 C7 O2 -176.5(5) . . . . ?
C2 C1 C7 O1 -178.7(5) . . . . ?
C6 C1 C7 O1 3.6(8) . . . . ?
Pr1 O3 C8 O4 -5.5(5) 4_545 . . . ?
Pr1 O3 C8 C3 174.6(4) 4_545 . . . ?
Pr1 O4 C8 O3 -145.4(7) 6_565 . . . ?
Pr1 O4 C8 O3 5.2(5) 4_545 . . . ?
Pr1 O4 C8 C3 34.5(12) 6_565 . . . ?
Pr1 O4 C8 C3 -174.9(4) 4_545 . . . ?
Pr1 O4 C8 Pr1 -150.5(9) 6_565 . . 4_545 ?
C2 C3 C8 O3 24.6(8) . . . . ?
C4 C3 C8 O3 -156.1(5) . . . . ?
C2 C3 C8 O4 -155.3(5) . . . . ?
C4 C3 C8 O4 23.9(7) . . . . ?
C10 O5 C9 C5 -168.2(6) . . . . ?
C4 C5 C9 O5 125.7(6) . . . . ?
C6 C5 C9 O5 -55.4(8) . . . . ?
C9 O5 C10 C11 -178.4(7) . . . . ?
C9 O5 C10 C15 0.7(11) . . . . ?
O5 C10 C11 C12 -178.8(9) . . . . ?
C15 C10 C11 C12 2.0(14) . . . . ?
C10 C11 C12 C13 -1.3(15) . . . . ?
C11 C12 C13 C14 0.7(13) . . . . ?
C11 C12 C13 C16 179.6(8) . . . . ?
C12 C13 C14 C15 -1.0(11) . . . . ?
C16 C13 C14 C15 -179.8(6) . . . . ?
C11 C10 C15 C14 -2.2(12) . . . . ?
O5 C10 C15 C14 178.7(7) . . . . ?
C13 C14 C15 C10 1.7(11) . . . . ?
Pr1 O7 C16 O6 8.9(6) 2_655 . . . ?
Pr1 O7 C16 C13 -170.8(5) 2_655 . . . ?
Pr1 O6 C16 O7 -9.1(6) 2_655 . . . ?
Pr1 O6 C16 C13 170.7(5) 2_655 . . . ?
C14 C13 C16 O7 14.5(10) . . . . ?
C12 C13 C16 O7 -164.3(7) . . . . ?
C14 C13 C16 O6 -165.2(6) . . . . ?
C12 C13 C16 O6 16.0(10) . . . . ?
Pr1 O8 C17 N1 153.8(9) . . . . ?
O8 C17 N1 C19 8(2) . . . . ?
O8 C17 N1 C18 175.7(14) . . . . ?
Pr1 O9 C20 O10 173.9(8) . . . . ?

_refine_diff_density_max         1.496
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.157

####################################################################### 
# 
# 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_10R-Gd-RT2
_database_code_depnum_ccdc_archive 'CCDC 1574655'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT601_10R-Gd-RT2          
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        605 Ang**3
RESPONSE: The existance of large voids containing loosely bound water
solvent is typical for MOF structures.

# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.001  0.499  0.000       603        59 ' '
   2 -0.006  0.494  0.500       595        58 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT220_10R-Gd-RT2          
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         10.0 Ratio
PROBLEM: Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range        6.3 Ratio 
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the Gd centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_10R-Gd-RT2          
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O13 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;
_vrf_PLAT971_10R-Gd-RT2          
;
PROBLEM: Check Calcd Resid. Dens.  0.75A   From Gd1             2.97 eA-3  
RESPONSE: The deep residual density hole is very close to the heavy Gd1
atom, which might be resulted from the disorder of the heavy Gd1 atom 
and could not be modelled properly.
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Gd2(C16H9O7)2(C3H7ON)2(H2O)(CHOOH)]??3H2O'
_chemical_formula_sum            'C39 H42 Gd2 N2 O22'
_chemical_formula_weight         1205.24

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'
N N 0.0061 0.0033 '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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.7055(13)
_cell_length_b                   14.4824(7)
_cell_length_c                   13.5829(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.5250(10)
_cell_angle_gamma                90
_cell_volume                     5598.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9918
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_F_000             2376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    2.417
_shelx_estimated_absorpt_T_min   0.551
_shelx_estimated_absorpt_T_max   0.595
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26062
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.833
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6956
_reflns_number_gt                6032
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0594P)²+91.8173P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6956
_refine_ls_number_parameters     299
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1283
_refine_ls_wR_factor_gt          0.1214
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.080
_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
Gd1 Gd 0.68273(2) 0.78861(2) 0.46284(2) 0.01489(9) Uani 1 1 d . . . . .
O1 O 0.73239(13) 0.6605(2) 0.4515(3) 0.0222(7) Uani 1 1 d . . . . .
O2 O 0.79387(13) 0.5746(3) 0.4357(3) 0.0265(8) Uani 1 1 d . . . . .
O3 O 0.76775(13) 0.3460(3) 0.1530(3) 0.0292(9) Uani 1 1 d . . . . .
O4 O 0.69815(13) 0.2745(3) 0.1256(3) 0.0233(7) Uani 1 1 d . . . . .
O5 O 0.57781(15) 0.3562(3) 0.3506(4) 0.0426(12) Uani 1 1 d . . . . .
O6 O 0.39084(14) 0.1814(3) 0.4716(4) 0.0337(9) Uani 1 1 d . . . . .
O7 O 0.38022(14) 0.3259(3) 0.5142(3) 0.0326(9) Uani 1 1 d . . . . .
C1 C 0.71925(17) 0.5188(3) 0.3628(4) 0.0197(9) Uani 1 1 d . . . . .
C2 C 0.73701(17) 0.4582(3) 0.2972(4) 0.0207(9) Uani 1 1 d . . . . .
H2 H 0.769426 0.459898 0.289508 0.025 Uiso 1 1 calc R U . . .
C3 C 0.70745(17) 0.3956(3) 0.2431(4) 0.0199(9) Uani 1 1 d . . . . .
C4 C 0.65995(17) 0.3923(4) 0.2560(4) 0.0224(10) Uani 1 1 d . . . . .
H4 H 0.639630 0.349436 0.218879 0.027 Uiso 1 1 calc R U . . .
C5 C 0.64232(17) 0.4514(4) 0.3228(4) 0.0228(10) Uani 1 1 d . . . . .
C6 C 0.67206(17) 0.5152(4) 0.3758(4) 0.0224(10) Uani 1 1 d . . . . .
H6 H 0.660080 0.556278 0.420957 0.027 Uiso 1 1 calc R U . . .
C7 C 0.75063(18) 0.5887(3) 0.4197(4) 0.0207(9) Uani 1 1 d . . . . .
C8 C 0.72589(17) 0.3331(4) 0.1682(4) 0.0211(9) Uani 1 1 d . . . . .
C9 C 0.59084(18) 0.4499(4) 0.3375(4) 0.0271(11) Uani 1 1 d . . . . .
H9A H 0.585943 0.486784 0.396721 0.033 Uiso 1 1 calc R U . . .
H9B H 0.571397 0.476760 0.278919 0.033 Uiso 1 1 calc R U . . .
C10 C 0.5337(2) 0.3404(4) 0.3763(5) 0.0347(14) Uani 1 1 d . . . . .
C11 C 0.5222(3) 0.2480(5) 0.3840(7) 0.056(2) Uani 1 1 d . U . . .
H11 H 0.543290 0.201503 0.368013 0.067 Uiso 1 1 calc R U . . .
C12 C 0.4797(3) 0.2238(5) 0.4150(7) 0.052(2) Uani 1 1 d . U . . .
H12 H 0.471773 0.160386 0.419643 0.062 Uiso 1 1 calc R U . . .
C13 C 0.44856(19) 0.2910(4) 0.4396(5) 0.0285(12) Uani 1 1 d . . . . .
C14 C 0.46054(19) 0.3826(4) 0.4292(5) 0.0302(12) Uani 1 1 d . . . . .
H14 H 0.439277 0.429247 0.444149 0.036 Uiso 1 1 calc R U . . .
C15 C 0.50288(19) 0.4086(4) 0.3974(5) 0.0304(12) Uani 1 1 d . . . . .
H15 H 0.510406 0.471900 0.390439 0.036 Uiso 1 1 calc R U . . .
C16 C 0.40382(18) 0.2650(4) 0.4763(4) 0.0261(11) Uani 1 1 d . . . . .
O8 O 0.64287(18) 0.9164(4) 0.3701(4) 0.0480(13) Uani 1 1 d . . . . .
C17 C 0.6577(4) 0.9934(7) 0.3639(9) 0.076(3) Uani 1 1 d . U . . .
H17 H 0.684344 1.011135 0.409025 0.092 Uiso 1 1 calc R U . . .
N1 N 0.6388(5) 1.0567(8) 0.2962(9) 0.106(3) Uani 1 1 d . U . . .
C18 C 0.6580(7) 1.1472(9) 0.2928(12) 0.132(6) Uani 1 1 d . U . . .
H18A H 0.637235 1.191531 0.319824 0.197 Uiso 1 1 calc R U . . .
H18B H 0.660904 1.163384 0.223799 0.197 Uiso 1 1 calc R U . . .
H18C H 0.689083 1.148779 0.332361 0.197 Uiso 1 1 calc R U . . .
C19 C 0.6035(8) 1.0218(18) 0.2233(17) 0.204(10) Uani 1 1 d . U . . .
H19A H 0.606271 1.051160 0.159312 0.306 Uiso 1 1 calc R U . . .
H19B H 0.572525 1.035202 0.242672 0.306 Uiso 1 1 calc R U . . .
H19C H 0.607378 0.954897 0.217424 0.306 Uiso 1 1 calc R U . . .
O9 O 0.6517(2) 0.7265(4) 0.2998(4) 0.0478(13) Uani 0.5 1 d . . P A 1
C20 C 0.6551(7) 0.7635(13) 0.2197(11) 0.057(4) Uani 0.5 1 d D U P A 1
O10 O 0.6480(10) 0.7137(17) 0.1390(16) 0.140(8) Uani 0.5 1 d D U P A 1
O12 O 0.500000 0.236(2) 0.750000 0.226(12) Uiso 1 2 d S . P B 1
O9A O 0.6517(2) 0.7265(4) 0.2998(4) 0.0478(13) Uani 0.5 1 d . . P A 2
O11 O 0.6306(9) 0.6262(19) 0.1333(19) 0.142(8) Uiso 0.5 1 d . . P C 2
O13 O 0.500000 0.389(2) 0.750000 0.268(14) Uiso 1 2 d S . P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.357(4) . ?
Gd1 O4 2.380(4) 6_566 ?
Gd1 O3 2.403(4) 4_655 ?
Gd1 O6 2.436(4) 5_666 ?
Gd1 O8 2.438(5) . ?
Gd1 O9A 2.448(5) . ?
Gd1 O9 2.448(5) . ?
Gd1 O2 2.456(4) 7_666 ?
Gd1 O7 2.502(4) 5_666 ?
Gd1 O1 2.663(4) 7_666 ?
Gd1 C16 2.828(5) 5_666 ?
Gd1 C7 2.926(5) 7_666 ?
O1 C7 1.265(6) . ?
O2 C7 1.249(6) . ?
O3 C8 1.259(6) . ?
O4 C8 1.252(6) . ?
O5 C10 1.377(6) . ?
O5 C9 1.425(7) . ?
O6 C16 1.265(7) . ?
O7 C16 1.262(7) . ?
C1 C6 1.390(6) . ?
C1 C2 1.395(6) . ?
C1 C7 1.500(7) . ?
C2 C3 1.385(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.398(6) . ?
C3 C8 1.509(6) . ?
C4 C5 1.390(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(7) . ?
C5 C9 1.517(7) . ?
C6 H6 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.379(8) . ?
C10 C11 1.385(10) . ?
C11 C12 1.386(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.391(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(8) . ?
C13 C16 1.486(7) . ?
C14 C15 1.394(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O8 C17 1.200(12) . ?
C17 N1 1.362(14) . ?
C17 H17 0.9500 . ?
N1 C19 1.41(2) . ?
N1 C18 1.425(17) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O9 C20 1.228(17) . ?
C20 O10 1.305(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O4 73.60(13) . 6_566 ?
O1 Gd1 O3 79.31(13) . 4_655 ?
O4 Gd1 O3 133.41(13) 6_566 4_655 ?
O1 Gd1 O6 136.45(13) . 5_666 ?
O4 Gd1 O6 78.09(14) 6_566 5_666 ?
O3 Gd1 O6 142.51(14) 4_655 5_666 ?
O1 Gd1 O8 144.18(16) . . ?
O4 Gd1 O8 142.11(16) 6_566 . ?
O3 Gd1 O8 71.17(15) 4_655 . ?
O6 Gd1 O8 71.50(16) 5_666 . ?
O1 Gd1 O9A 78.66(17) . . ?
O4 Gd1 O9A 134.48(16) 6_566 . ?
O3 Gd1 O9A 73.22(17) 4_655 . ?
O6 Gd1 O9A 99.52(18) 5_666 . ?
O8 Gd1 O9A 73.80(19) . . ?
O1 Gd1 O9 78.66(17) . . ?
O4 Gd1 O9 134.48(16) 6_566 . ?
O3 Gd1 O9 73.22(17) 4_655 . ?
O6 Gd1 O9 99.52(18) 5_666 . ?
O8 Gd1 O9 73.80(19) . . ?
O1 Gd1 O2 123.26(12) . 7_666 ?
O4 Gd1 O2 77.57(14) 6_566 7_666 ?
O3 Gd1 O2 86.96(14) 4_655 7_666 ?
O6 Gd1 O2 80.66(13) 5_666 7_666 ?
O8 Gd1 O2 75.69(18) . 7_666 ?
O9 Gd1 O2 147.62(16) . 7_666 ?
O1 Gd1 O7 86.52(13) . 5_666 ?
O4 Gd1 O7 71.27(15) 6_566 5_666 ?
O3 Gd1 O7 144.08(15) 4_655 5_666 ?
O6 Gd1 O7 52.95(13) 5_666 5_666 ?
O8 Gd1 O7 105.66(17) . 5_666 ?
O9 Gd1 O7 71.70(16) . 5_666 ?
O2 Gd1 O7 127.83(13) 7_666 5_666 ?
O1 Gd1 O1 73.74(13) . 7_666 ?
O4 Gd1 O1 69.65(12) 6_566 7_666 ?
O3 Gd1 O1 66.70(13) 4_655 7_666 ?
O6 Gd1 O1 125.35(13) 5_666 7_666 ?
O8 Gd1 O1 110.87(16) . 7_666 ?
O9 Gd1 O1 134.52(16) . 7_666 ?
O2 Gd1 O1 50.53(11) 7_666 7_666 ?
O7 Gd1 O1 139.75(14) 5_666 7_666 ?
O1 Gd1 C16 111.41(15) . 5_666 ?
O4 Gd1 C16 71.73(15) 6_566 5_666 ?
O3 Gd1 C16 154.72(15) 4_655 5_666 ?
O6 Gd1 C16 26.49(15) 5_666 5_666 ?
O8 Gd1 C16 89.34(17) . 5_666 ?
O9A Gd1 C16 86.20(18) . 5_666 ?
O9 Gd1 C16 86.20(18) . 5_666 ?
O2 Gd1 C16 104.08(15) 7_666 5_666 ?
O7 Gd1 C16 26.50(15) 5_666 5_666 ?
O1 Gd1 C16 137.46(14) 7_666 5_666 ?
O1 Gd1 C7 98.96(13) . 7_666 ?
O4 Gd1 C7 72.40(14) 6_566 7_666 ?
O3 Gd1 C7 75.33(14) 4_655 7_666 ?
O6 Gd1 C7 103.22(14) 5_666 7_666 ?
O8 Gd1 C7 92.87(18) . 7_666 ?
O9 Gd1 C7 148.36(16) . 7_666 ?
O2 Gd1 C7 24.92(13) 7_666 7_666 ?
O7 Gd1 C7 139.94(14) 5_666 7_666 ?
O1 Gd1 C7 25.61(12) 7_666 7_666 ?
C16 Gd1 C7 122.93(15) 5_666 7_666 ?
C7 O1 Gd1 161.8(3) . . ?
C7 O1 Gd1 88.9(3) . 7_666 ?
Gd1 O1 Gd1 106.26(12) . 7_666 ?
C7 O2 Gd1 99.1(3) . 7_666 ?
C8 O3 Gd1 135.7(3) . 4_645 ?
C8 O4 Gd1 136.0(3) . 6_565 ?
C10 O5 C9 117.1(5) . . ?
C16 O6 Gd1 94.3(3) . 5_666 ?
C16 O7 Gd1 91.3(3) . 5_666 ?
C6 C1 C2 120.1(4) . . ?
C6 C1 C7 119.3(4) . . ?
C2 C1 C7 120.6(4) . . ?
C3 C2 C1 120.1(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 C8 120.4(4) . . ?
C4 C3 C8 119.8(4) . . ?
C5 C4 C3 120.3(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 119.7(4) . . ?
C4 C5 C9 121.5(5) . . ?
C6 C5 C9 118.8(4) . . ?
C1 C6 C5 120.0(4) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
O2 C7 O1 121.5(5) . . ?
O2 C7 C1 119.7(4) . . ?
O1 C7 C1 118.9(4) . . ?
O2 C7 Gd1 56.0(3) . 7_666 ?
O1 C7 Gd1 65.5(3) . 7_666 ?
C1 C7 Gd1 174.9(4) . 7_666 ?
O4 C8 O3 126.0(5) . . ?
O4 C8 C3 117.4(4) . . ?
O3 C8 C3 116.6(4) . . ?
O5 C9 C5 107.8(4) . . ?
O5 C9 H9A 110.1 . . ?
C5 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C5 C9 H9B 110.1 . . ?
H9A C9 H9B 108.5 . . ?
O5 C10 C15 124.7(5) . . ?
O5 C10 C11 114.6(5) . . ?
C15 C10 C11 120.7(5) . . ?
C10 C11 C12 119.6(6) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 120.9(6) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 118.1(5) . . ?
C14 C13 C16 121.0(5) . . ?
C12 C13 C16 120.9(5) . . ?
C13 C14 C15 121.9(5) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
C10 C15 C14 118.6(5) . . ?
C10 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
O7 C16 O6 121.2(5) . . ?
O7 C16 C13 119.6(5) . . ?
O6 C16 C13 119.2(5) . . ?
O7 C16 Gd1 62.2(3) . 5_666 ?
O6 C16 Gd1 59.2(3) . 5_666 ?
C13 C16 Gd1 177.2(4) . 5_666 ?
C17 O8 Gd1 126.4(7) . . ?
O8 C17 N1 124.0(13) . . ?
O8 C17 H17 118.0 . . ?
N1 C17 H17 118.0 . . ?
C17 N1 C19 114.7(14) . . ?
C17 N1 C18 121.3(14) . . ?
C19 N1 C18 123.5(15) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Gd1 125.4(8) . . ?
O9 C20 O10 118.8(18) . . ?

_refine_diff_density_max         3.021
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.188

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

data_11R-Ho-RT
_database_code_depnum_ccdc_archive 'CCDC 1574646'
_audit_update_record             
;
2018-02-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_11R-Ho-RT           
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         7.7 Ratio
RESPONSE: The crystals of the complex are sensitive to the loss of 
crystallization solvent (DMF). The measurements were performed 
several times for different crystals from different batches leading in 
each case to severe disorder issues related to the crystallization solvent.
This disorder affects also the organic ligands coordinated to the Ho centers. 
Please note that the ADP ratios are larger for some peripheral atoms.
This confirms that the large ADP ratios are related to crystallization solvent 
disorder. Finally the larger ADP ratios for some atoms don't affect
the most important part of the structure.
;
_vrf_PLAT306_11R-Ho-RT           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O10 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.

PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O11 Check
RESPONSE: This is due to the severe disorder of this atom, which could not 
refine position of H atoms.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Ho2(C16H9O7)2(C3H7ON)2.4(H2O)1.6]??3H2O'
_chemical_formula_sum            'C39.20 H44 Ho2 N2.40 O21'
_chemical_formula_weight         1214.63

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'
N N 0.0061 0.0033 '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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.5245(17)
_cell_length_b                   14.3258(9)
_cell_length_c                   13.6361(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.979(2)
_cell_angle_gamma                90
_cell_volume                     5518.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9479
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      28.43

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             2392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    2.915
_shelx_estimated_absorpt_T_min   0.507
_shelx_estimated_absorpt_T_max   0.541
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26797
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.841
_diffrn_reflns_theta_max         28.456
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6920
_reflns_number_gt                6035
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²+46.8916P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6920
_refine_ls_number_parameters     317
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0898
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.002
_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 0.18273(2) 0.29081(2) 0.96055(2) 0.01834(6) Uani 1 1 d . . . . .
O1 O 0.23414(10) 0.3513(2) 0.8542(2) 0.0309(7) Uani 1 1 d . . . . .
O2 O 0.30404(11) 0.2773(2) 0.8816(2) 0.0284(6) Uani 1 1 d . . . . .
O3 O 0.20683(10) 0.5763(2) 0.5643(3) 0.0330(7) Uani 1 1 d . . . . .
O4 O 0.26875(11) 0.6639(2) 0.5534(2) 0.0277(6) Uani 1 1 d . . . . .
O5 O 0.42311(12) 0.3542(3) 0.6496(3) 0.0451(8) Uani 1 1 d . U . . .
O6 O 0.60986(11) 0.1768(2) 0.5247(3) 0.0380(8) Uani 1 1 d . . . . .
O7 O 0.61840(12) 0.3204(3) 0.4747(3) 0.0437(9) Uani 1 1 d . . . . .
C1 C 0.29428(13) 0.3982(3) 0.7629(3) 0.0231(7) Uani 1 1 d . . . . .
C2 C 0.26442(13) 0.4609(3) 0.7076(3) 0.0240(8) Uani 1 1 d . . . . .
H2 H 0.232569 0.463253 0.715415 0.029 Uiso 1 1 calc R U . . .
C3 C 0.28181(14) 0.5202(3) 0.6403(3) 0.0245(8) Uani 1 1 d . . . . .
C4 C 0.32925(14) 0.5153(3) 0.6267(3) 0.0271(8) Uani 1 1 d . . . . .
H4 H 0.340883 0.554926 0.581749 0.033 Uiso 1 1 calc R U . . .
C5 C 0.35926(14) 0.4513(3) 0.6803(3) 0.0281(9) Uani 1 1 d . . . . .
C6 C 0.34190(14) 0.3936(3) 0.7494(3) 0.0268(8) Uani 1 1 d . . . . .
H6 H 0.362085 0.351810 0.786503 0.032 Uiso 1 1 calc R U . . .
C7 C 0.27605(14) 0.3372(3) 0.8394(3) 0.0231(7) Uani 1 1 d . . . . .
C8 C 0.25042(14) 0.5908(3) 0.5827(3) 0.0235(7) Uani 1 1 d . . . . .
C9 C 0.41073(15) 0.4484(3) 0.6647(4) 0.0360(10) Uani 1 1 d . . . . .
H9A H 0.415437 0.485757 0.607572 0.043 Uiso 1 1 calc R U . . .
H9B H 0.430491 0.473592 0.722303 0.043 Uiso 1 1 calc R U . . .
C10 C 0.46615(17) 0.3372(4) 0.6201(4) 0.0407(12) Uani 1 1 d . . . . .
C11 C 0.4774(2) 0.2438(5) 0.6119(5) 0.0532(14) Uani 1 1 d . U . . .
H11 H 0.456799 0.198055 0.628509 0.064 Uiso 1 1 calc R U . . .
C12 C 0.5196(2) 0.2183(4) 0.5787(5) 0.0491(13) Uani 1 1 d . U . . .
H12 H 0.527047 0.155461 0.573286 0.059 Uiso 1 1 calc R U . . .
C13 C 0.55089(16) 0.2868(3) 0.5535(4) 0.0346(10) Uani 1 1 d . . . . .
C14 C 0.53963(16) 0.3792(3) 0.5644(4) 0.0373(11) Uani 1 1 d . . . . .
H14 H 0.560450 0.425159 0.548933 0.045 Uiso 1 1 calc R U . . .
C15 C 0.49730(16) 0.4056(4) 0.5985(4) 0.0396(11) Uani 1 1 d . . . . .
H15 H 0.490316 0.468359 0.606365 0.048 Uiso 1 1 calc R U . . .
C16 C 0.59566(14) 0.2594(3) 0.5154(3) 0.0309(9) Uani 1 1 d . . . . .
O8 O 0.14437(15) 0.4195(3) 0.8711(3) 0.0542(10) Uani 0.7 1 d . U P A 1
C17 C 0.1569(3) 0.4958(6) 0.8615(6) 0.0456(17) Uani 0.7 1 d . U P A 1
H17 H 0.182096 0.515610 0.907442 0.055 Uiso 0.7 1 calc R U P A 1
N1 N 0.1404(3) 0.5575(6) 0.7952(7) 0.067(2) Uani 0.7 1 d . U P A 1
C18 C 0.1564(5) 0.6458(10) 0.7871(10) 0.094(4) Uani 0.7 1 d . U P A 1
H18A H 0.135828 0.688525 0.814847 0.141 Uiso 0.7 1 calc R U P A 1
H18B H 0.156715 0.660542 0.718538 0.141 Uiso 0.7 1 calc R U P A 1
H18C H 0.187828 0.651011 0.822242 0.141 Uiso 0.7 1 calc R U P A 1
C19 C 0.1103(9) 0.5408(18) 0.7299(18) 0.179(9) Uani 0.7 1 d . U P A 1
H19A H 0.107688 0.591208 0.683046 0.269 Uiso 0.7 1 calc R U P A 1
H19B H 0.080805 0.533432 0.755436 0.269 Uiso 0.7 1 calc R U P A 1
H19C H 0.117752 0.484178 0.697745 0.269 Uiso 0.7 1 calc R U P A 1
O9 O 0.15386(17) 0.2331(3) 0.7961(3) 0.0597(12) Uani 0.5 1 d . . P A 1
C20 C 0.1603(4) 0.2628(9) 0.7168(9) 0.048(2) Uani 0.5 1 d . U P A 1
H20 H 0.170858 0.324032 0.714806 0.057 Uiso 0.5 1 calc R U P A 1
N2 N 0.1538(5) 0.2168(9) 0.6322(10) 0.068(3) Uani 0.5 1 d . U P A 1
C21 C 0.1539(10) 0.2797(19) 0.537(2) 0.136(9) Uani 0.5 1 d . U P A 1
H21A H 0.179108 0.260211 0.501947 0.204 Uiso 0.5 1 calc R U P A 1
H21B H 0.158576 0.343747 0.556859 0.204 Uiso 0.5 1 calc R U P A 1
H21C H 0.124192 0.273338 0.495186 0.204 Uiso 0.5 1 calc R U P A 1
C22 C 0.1356(8) 0.1325(16) 0.6248(16) 0.108(6) Uani 0.5 1 d . U P A 1
H22A H 0.151483 0.093811 0.676575 0.162 Uiso 0.5 1 calc R U P A 1
H22B H 0.139493 0.106379 0.561623 0.162 Uiso 0.5 1 calc R U P A 1
H22C H 0.102491 0.135583 0.630877 0.162 Uiso 0.5 1 calc R U P A 1
O8A O 0.14437(15) 0.4195(3) 0.8711(3) 0.0542(10) Uani 0.3 1 d . . P A 2
O9A O 0.15386(17) 0.2331(3) 0.7961(3) 0.0597(12) Uani 0.5 1 d . . P A 2
O10 O 0.500000 0.218(3) 0.250000 0.392(19) Uiso 1 2 d S . P . .
O11 O 0.5618(8) 0.9937(17) 0.4813(17) 0.356(11) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O4 2.309(3) 4_546 ?
Ho1 O2 2.346(3) 7_557 ?
Ho1 O1 2.365(3) . ?
Ho1 O8 2.391(4) . ?
Ho1 O8A 2.391(4) . ?
Ho1 O6 2.409(3) 8_456 ?
Ho1 O3 2.414(3) 6_566 ?
Ho1 O9A 2.424(4) . ?
Ho1 O9 2.424(4) . ?
Ho1 O7 2.458(3) 8_456 ?
Ho1 O4 2.680(3) 6_566 ?
Ho1 C16 2.786(4) 8_456 ?
O1 C7 1.256(5) . ?
O2 C7 1.256(5) . ?
O3 C8 1.251(5) . ?
O4 C8 1.260(5) . ?
O5 C10 1.366(5) . ?
O5 C9 1.417(6) . ?
O6 C16 1.252(6) . ?
O7 C16 1.261(6) . ?
C1 C2 1.387(5) . ?
C1 C6 1.398(5) . ?
C1 C7 1.507(5) . ?
C2 C3 1.392(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(5) . ?
C3 C8 1.498(5) . ?
C4 C5 1.391(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(5) . ?
C5 C9 1.513(5) . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.382(7) . ?
C10 C11 1.385(8) . ?
C11 C12 1.391(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.402(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.375(7) . ?
C13 C16 1.496(5) . ?
C14 C15 1.404(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O8 C17 1.163(9) . ?
C17 N1 1.304(11) . ?
C17 H17 0.9300 . ?
N1 C19 1.17(2) . ?
N1 C18 1.355(16) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O9 C20 1.199(12) . ?
C20 N2 1.319(17) . ?
C20 H20 0.9300 . ?
N2 C22 1.31(2) . ?
N2 C21 1.58(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ho1 O2 74.10(10) 4_546 7_557 ?
O4 Ho1 O1 78.96(11) 4_546 . ?
O2 Ho1 O1 132.89(10) 7_557 . ?
O4 Ho1 O8 143.40(13) 4_546 . ?
O2 Ho1 O8 142.45(13) 7_557 . ?
O1 Ho1 O8 71.55(12) . . ?
O4 Ho1 O8A 143.40(13) 4_546 . ?
O2 Ho1 O8A 142.45(13) 7_557 . ?
O1 Ho1 O8A 71.55(12) . . ?
O4 Ho1 O6 137.62(11) 4_546 8_456 ?
O2 Ho1 O6 77.54(12) 7_557 8_456 ?
O1 Ho1 O6 142.31(11) . 8_456 ?
O8 Ho1 O6 71.31(13) . 8_456 ?
O4 Ho1 O3 122.97(11) 4_546 6_566 ?
O2 Ho1 O3 78.11(12) 7_557 6_566 ?
O1 Ho1 O3 85.40(12) . 6_566 ?
O8 Ho1 O3 76.31(14) . 6_566 ?
O6 Ho1 O3 79.94(11) 8_456 6_566 ?
O4 Ho1 O9A 77.64(15) 4_546 . ?
O2 Ho1 O9A 134.24(14) 7_557 . ?
O1 Ho1 O9A 73.62(13) . . ?
O8A Ho1 O9A 73.65(17) . . ?
O6 Ho1 O9A 101.64(15) 8_456 . ?
O3 Ho1 O9A 147.50(14) 6_566 . ?
O4 Ho1 O9 77.64(15) 4_546 . ?
O2 Ho1 O9 134.24(14) 7_557 . ?
O1 Ho1 O9 73.62(13) . . ?
O8 Ho1 O9 73.65(17) . . ?
O6 Ho1 O9 101.64(15) 8_456 . ?
O3 Ho1 O9 147.50(14) 6_566 . ?
O4 Ho1 O7 87.62(11) 4_546 8_456 ?
O2 Ho1 O7 71.63(13) 7_557 8_456 ?
O1 Ho1 O7 144.98(12) . 8_456 ?
O8 Ho1 O7 104.26(15) . 8_456 ?
O6 Ho1 O7 53.50(11) 8_456 8_456 ?
O3 Ho1 O7 128.31(11) 6_566 8_456 ?
O9 Ho1 O7 71.96(14) . 8_456 ?
O4 Ho1 O4 73.13(11) 4_546 6_566 ?
O2 Ho1 O4 69.34(10) 7_557 6_566 ?
O1 Ho1 O4 66.16(10) . 6_566 ?
O8 Ho1 O4 112.23(13) . 6_566 ?
O6 Ho1 O4 124.15(11) 8_456 6_566 ?
O3 Ho1 O4 50.55(9) 6_566 6_566 ?
O9 Ho1 O4 133.70(13) . 6_566 ?
O7 Ho1 O4 139.86(12) 8_456 6_566 ?
O4 Ho1 C16 112.67(12) 4_546 8_456 ?
O2 Ho1 C16 71.46(12) 7_557 8_456 ?
O1 Ho1 C16 155.63(12) . 8_456 ?
O8 Ho1 C16 88.52(14) . 8_456 ?
O8A Ho1 C16 88.52(14) . 8_456 ?
O6 Ho1 C16 26.65(13) 8_456 8_456 ?
O3 Ho1 C16 103.79(12) 6_566 8_456 ?
O9A Ho1 C16 87.65(15) . 8_456 ?
O9 Ho1 C16 87.65(15) . 8_456 ?
O7 Ho1 C16 26.91(13) 8_456 8_456 ?
O4 Ho1 C16 136.69(11) 6_566 8_456 ?
C7 O1 Ho1 136.5(3) . . ?
C7 O2 Ho1 135.7(3) . 7_557 ?
C8 O3 Ho1 100.5(2) . 6_565 ?
C8 O4 Ho1 163.8(3) . 4_556 ?
C8 O4 Ho1 87.6(2) . 6_565 ?
Ho1 O4 Ho1 106.87(11) 4_556 6_565 ?
C10 O5 C9 117.7(4) . . ?
C16 O6 Ho1 93.7(3) . 8 ?
C16 O7 Ho1 91.2(3) . 8 ?
C2 C1 C6 119.5(3) . . ?
C2 C1 C7 120.5(3) . . ?
C6 C1 C7 119.9(3) . . ?
C1 C2 C3 120.4(3) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 C8 121.0(3) . . ?
C4 C3 C8 119.1(3) . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.7(4) . . ?
C4 C5 C9 118.9(4) . . ?
C6 C5 C9 121.4(4) . . ?
C5 C6 C1 120.3(4) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
O2 C7 O1 126.5(4) . . ?
O2 C7 C1 117.0(3) . . ?
O1 C7 C1 116.5(3) . . ?
O3 C8 O4 121.2(4) . . ?
O3 C8 C3 119.9(4) . . ?
O4 C8 C3 118.9(4) . . ?
O3 C8 Ho1 54.6(2) . 6_565 ?
O4 C8 Ho1 66.8(2) . 6_565 ?
C3 C8 Ho1 173.2(3) . 6_565 ?
O5 C9 C5 108.2(4) . . ?
O5 C9 H9A 110.1 . . ?
C5 C9 H9A 110.1 . . ?
O5 C9 H9B 110.1 . . ?
C5 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O5 C10 C15 124.6(5) . . ?
O5 C10 C11 115.2(5) . . ?
C15 C10 C11 120.3(4) . . ?
C10 C11 C12 120.1(6) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 120.3(5) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 118.8(4) . . ?
C14 C13 C16 120.9(4) . . ?
C12 C13 C16 120.3(4) . . ?
C13 C14 C15 121.3(4) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C10 C15 C14 119.2(5) . . ?
C10 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
O6 C16 O7 121.3(4) . . ?
O6 C16 C13 119.5(4) . . ?
O7 C16 C13 119.1(4) . . ?
O6 C16 Ho1 59.7(2) . 8 ?
O7 C16 Ho1 61.9(2) . 8 ?
C13 C16 Ho1 175.3(3) . 8 ?
C17 O8 Ho1 131.0(5) . . ?
O8 C17 N1 128.9(9) . . ?
O8 C17 H17 115.6 . . ?
N1 C17 H17 115.6 . . ?
C19 N1 C17 123.0(16) . . ?
C19 N1 C18 110.3(16) . . ?
C17 N1 C18 126.6(11) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O9 Ho1 129.7(7) . . ?
O9 C20 N2 126.3(12) . . ?
O9 C20 H20 116.9 . . ?
N2 C20 H20 116.9 . . ?
C22 N2 C20 122.2(15) . . ?
C22 N2 C21 120.6(17) . . ?
C20 N2 C21 114.6(14) . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

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
C6 C1 C2 C3 -1.3(6) . . . . ?
C7 C1 C2 C3 177.0(4) . . . . ?
C1 C2 C3 C4 1.5(7) . . . . ?
C1 C2 C3 C8 -177.6(4) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C8 C3 C4 C5 179.1(4) . . . . ?
C3 C4 C5 C6 -1.5(7) . . . . ?
C3 C4 C5 C9 -179.3(4) . . . . ?
C4 C5 C6 C1 1.7(7) . . . . ?
C9 C5 C6 C1 179.4(4) . . . . ?
C2 C1 C6 C5 -0.3(7) . . . . ?
C7 C1 C6 C5 -178.6(4) . . . . ?
Ho1 O2 C7 O1 -33.0(7) 7_557 . . . ?
Ho1 O2 C7 C1 147.3(3) 7_557 . . . ?
Ho1 O1 C7 O2 2.5(7) . . . . ?
Ho1 O1 C7 C1 -177.7(3) . . . . ?
C2 C1 C7 O2 174.9(4) . . . . ?
C6 C1 C7 O2 -6.8(6) . . . . ?
C2 C1 C7 O1 -4.9(6) . . . . ?
C6 C1 C7 O1 173.4(4) . . . . ?
Ho1 O3 C8 O4 4.5(4) 6_565 . . . ?
Ho1 O3 C8 C3 -175.2(3) 6_565 . . . ?
Ho1 O4 C8 O3 150.0(8) 4_556 . . . ?
Ho1 O4 C8 O3 -4.0(4) 6_565 . . . ?
Ho1 O4 C8 C3 -30.3(12) 4_556 . . . ?
Ho1 O4 C8 C3 175.7(3) 6_565 . . . ?
Ho1 O4 C8 Ho1 153.9(10) 4_556 . . 6_565 ?
C2 C3 C8 O3 -27.2(6) . . . . ?
C4 C3 C8 O3 153.7(4) . . . . ?
C2 C3 C8 O4 153.2(4) . . . . ?
C4 C3 C8 O4 -25.9(6) . . . . ?
C10 O5 C9 C5 170.9(4) . . . . ?
C4 C5 C9 O5 -131.2(5) . . . . ?
C6 C5 C9 O5 51.0(6) . . . . ?
C9 O5 C10 C15 -3.9(8) . . . . ?
C9 O5 C10 C11 176.6(5) . . . . ?
O5 C10 C11 C12 177.5(6) . . . . ?
C15 C10 C11 C12 -2.0(9) . . . . ?
C10 C11 C12 C13 0.0(10) . . . . ?
C11 C12 C13 C14 1.5(9) . . . . ?
C11 C12 C13 C16 -178.4(5) . . . . ?
C12 C13 C14 C15 -1.1(8) . . . . ?
C16 C13 C14 C15 178.9(5) . . . . ?
O5 C10 C15 C14 -177.1(5) . . . . ?
C11 C10 C15 C14 2.4(9) . . . . ?
C13 C14 C15 C10 -0.9(9) . . . . ?
Ho1 O6 C16 O7 5.2(5) 8 . . . ?
Ho1 O6 C16 C13 -174.6(4) 8 . . . ?
Ho1 O7 C16 O6 -5.1(5) 8 . . . ?
Ho1 O7 C16 C13 174.7(4) 8 . . . ?
C14 C13 C16 O6 165.7(5) . . . . ?
C12 C13 C16 O6 -14.3(8) . . . . ?
C14 C13 C16 O7 -14.1(8) . . . . ?
C12 C13 C16 O7 165.9(5) . . . . ?
Ho1 O8 C17 N1 162.3(7) . . . . ?
O8 C17 N1 C19 -4(2) . . . . ?
O8 C17 N1 C18 -179.9(11) . . . . ?
Ho1 O9 C20 N2 162.0(10) . . . . ?
O9 C20 N2 C22 5(2) . . . . ?
O9 C20 N2 C21 166.9(16) . . . . ?

_refine_diff_density_max         1.389
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.142

