# Electronic Supplementary Material (ESI) for RSC Advances.
# 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. 
# 
#######################################################################

data_I
_database_code_depnum_ccdc_archive 'CCDC 1852703'
_audit_update_record             
;
2018-07-01 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            'C24 H40 Cl2 Gd2 N2 O21'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H30 Gd2 N2 O16, 2(Cl), 5(H2 O)'
_chemical_formula_sum            'C24 H40 Cl2 Gd2 N2 O21'
_chemical_formula_weight         1077.98

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'
Cl Cl 0.1484 0.1585 '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      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.6682(6)
_cell_length_b                   10.0302(6)
_cell_length_c                   10.9110(7)
_cell_angle_alpha                104.893(2)
_cell_angle_beta                 93.675(2)
_cell_angle_gamma                110.003(2)
_cell_volume                     947.30(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9597
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.63

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_F_000             528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    3.692
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35673
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.241
_diffrn_reflns_theta_max         27.668
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8750
_reflns_number_gt                8280
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    0.992

_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0254P)²+0.3668P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3995 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.195(8)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         8750
_refine_ls_number_parameters     438
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0164
_refine_ls_wR_factor_ref         0.0436
_refine_ls_wR_factor_gt          0.0427
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.78236(2) 0.85920(2) 0.27339(2) 0.01776(11) Uani 1 1 d . . . . .
Gd2 Gd 0.44894(2) 1.00627(2) 0.19815(2) 0.01798(11) Uani 1 1 d . . . . .
Cl1 Cl 0.1281(4) 0.2033(4) 0.6740(4) 0.0475(7) Uani 1 1 d . . . . .
Cl2 Cl 0.0834(5) 0.6528(4) 0.8030(3) 0.0603(11) Uani 1 1 d . . . . .
O1 O 0.9326(8) 0.7412(8) 0.1466(8) 0.0265(18) Uani 1 1 d . . . . .
O2 O 0.7618(9) 0.6015(9) 0.2292(9) 0.037(2) Uani 1 1 d . . . . .
O3 O 0.6968(8) 0.0693(8) 0.1740(8) 0.0269(18) Uani 1 1 d . . . . .
O4 O 0.9055(8) 0.0298(8) 0.1603(8) 0.0276(19) Uani 1 1 d . . . . .
O5 O 1.6421(8) 0.7413(8) 0.0578(7) 0.0271(16) Uani 1 1 d . . . . .
O6 O 1.4246(9) 0.7780(8) 0.0414(8) 0.0295(18) Uani 1 1 d . . . . .
O7 O 1.0312(8) 0.9662(9) 0.3899(7) 0.0300(9) Uani 1 1 d D . . . .
O8 O 0.7779(11) 0.8009(10) 0.4800(9) 0.0484(11) Uani 1 1 d D . . . .
O9 O 0.3242(8) 0.8354(8) 0.3080(8) 0.0293(19) Uani 1 1 d . . . . .
O10 O 0.5334(9) 0.7943(9) 0.2934(8) 0.032(2) Uani 1 1 d . . . . .
O11 O 0.4723(10) 0.2622(9) 0.2430(10) 0.042(2) Uani 1 1 d . . . . .
O12 O 0.2970(8) 0.1252(8) 0.3257(8) 0.0270(18) Uani 1 1 d . . . . .
O13 O -0.1973(9) 0.0864(8) 0.4350(8) 0.0275(17) Uani 1 1 d . . . . .
O14 O -0.4153(9) 0.1126(8) 0.4131(8) 0.0301(17) Uani 1 1 d . . . . .
O15 O 0.1929(9) 0.9013(9) 0.0793(9) 0.036 Uani 1 1 d . . . . .
O16 O 0.4527(12) 1.0623(12) -0.0029(9) 0.056 Uani 1 1 d D . . . .
O17 O 1.3820(14) 1.0649(19) 0.6079(9) 0.148 Uani 1 1 d . . . . .
O18 O 1.0484(7) 0.8074(6) 0.5950(5) 0.068 Uani 1 1 d . . . . .
O19 O -0.1328(14) 0.8292(16) 0.8815(9) 0.122 Uani 1 1 d . . . . .
O20 O -0.1887(10) 0.9759(9) 0.7265(6) 0.109 Uani 1 1 d . . . . .
O21 O 0.5961(19) 1.0998(19) -0.2038(16) 0.229 Uani 1 1 d . U . . .
N1 N 1.2878(10) 0.4950(10) -0.0985(8) 0.025 Uani 1 1 d . . . . .
H1A H 1.244989 0.420344 -0.170449 0.030 Uiso 1 1 calc R U . . .
H1B H 1.240814 0.558118 -0.093591 0.030 Uiso 1 1 calc R U . . .
N2 N -0.0549(9) 0.3755(8) 0.5684(8) 0.0216(8) Uani 1 1 d . . . . .
H2A H -0.010823 0.451194 0.639413 0.026 Uiso 1 1 calc R U . . .
H2B H -0.010162 0.310668 0.564194 0.026 Uiso 1 1 calc R U . . .
C1 C 0.8663(11) 0.6197(9) 0.1677(10) 0.020(2) Uani 1 1 d . . . . .
C2 C 0.9178(11) 0.4899(11) 0.1264(10) 0.021(2) Uani 1 1 d . . . . .
C3 C 0.8427(12) 0.3579(11) 0.1410(11) 0.022(2) Uani 1 1 d . . . . .
H3 H 0.750904 0.340626 0.168612 0.027 Uiso 1 1 calc R U . . .
C4 C 0.8985(10) 0.2473(10) 0.1160(10) 0.020(2) Uani 1 1 d . . . . .
C5 C 0.8252(13) 0.1002(11) 0.1477(10) 0.021(2) Uani 1 1 d . . . . .
C6 C 1.0384(10) 0.2754(11) 0.0709(10) 0.025(2) Uani 1 1 d . . . . .
H6 H 1.077538 0.201011 0.055441 0.031 Uiso 1 1 calc R U . . .
C7 C 1.1137(11) 0.4018(11) 0.0502(10) 0.020(2) Uani 1 1 d . . . . .
C8 C 1.0567(12) 0.5167(11) 0.0833(11) 0.024(2) Uani 1 1 d . . . . .
H8 H 1.111019 0.610294 0.076543 0.028 Uiso 1 1 calc R U . . .
C9 C 1.2658(11) 0.4348(11) 0.0132(11) 0.024(2) Uani 1 1 d . . . . .
H9A H 1.338821 0.505726 0.086872 0.029 Uiso 1 1 calc R U . . .
H9B H 1.286121 0.344024 -0.006431 0.029 Uiso 1 1 calc R U . . .
C10 C 1.4462(12) 0.5727(12) -0.1083(12) 0.030(3) Uani 1 1 d . . . . .
H10 H 1.500514 0.507268 -0.103208 0.036 Uiso 1 1 calc R U . . .
C11 C 1.5106(11) 0.7090(11) 0.0050(11) 0.022(2) Uani 1 1 d . . . . .
C12 C 1.4555(7) 0.6043(8) -0.2358(6) 0.0520(16) Uani 1 1 d . . . . .
H12A H 1.392503 0.517287 -0.303154 0.078 Uiso 1 1 calc R U . . .
H12B H 1.556853 0.630635 -0.250799 0.078 Uiso 1 1 calc R U . . .
H12C H 1.423236 0.684949 -0.234801 0.078 Uiso 1 1 calc R U . . .
C13 C 0.4007(11) 0.7574(11) 0.3190(10) 0.020(2) Uani 1 1 d . . . . .
C14 C 0.3340(11) 0.6255(10) 0.3602(10) 0.021(2) Uani 1 1 d . . . . .
C15 C 0.3963(11) 0.5147(10) 0.3359(10) 0.019(2) Uani 1 1 d . . . . .
H15 H 0.489437 0.532827 0.310701 0.022 Uiso 1 1 calc R U . . .
C16 C 0.3103(12) 0.3721(10) 0.3514(10) 0.020(2) Uani 1 1 d . . . . .
C17 C 0.3622(12) 0.2489(11) 0.3050(11) 0.026(2) Uani 1 1 d . . . . .
C18 C 0.1769(12) 0.3490(11) 0.3944(11) 0.022(2) Uani 1 1 d . . . . .
H18 H 0.124485 0.257716 0.406438 0.026 Uiso 1 1 calc R U . . .
C19 C 0.1194(10) 0.4580(11) 0.4198(11) 0.023(2) Uani 1 1 d . . . . .
C20 C 0.2004(11) 0.6022(9) 0.4033(9) 0.020(2) Uani 1 1 d . . . . .
H20 H 0.162109 0.677156 0.421673 0.023 Uiso 1 1 calc R U . . .
C21 C -0.0365(12) 0.4315(12) 0.4529(11) 0.027(2) Uani 1 1 d . . . . .
H21A H -0.054107 0.523681 0.470186 0.032 Uiso 1 1 calc R U . . .
H21B H -0.109954 0.359489 0.379936 0.032 Uiso 1 1 calc R U . . .
C22 C -0.2177(10) 0.3015(11) 0.5762(11) 0.024(2) Uani 1 1 d . . . . .
H22 H -0.221719 0.274187 0.656298 0.029 Uiso 1 1 calc R U . . .
C23 C -0.2827(12) 0.1532(10) 0.4616(10) 0.022(2) Uani 1 1 d . . . . .
C24 C -0.3039(6) 0.4009(6) 0.5806(7) 0.0528(18) Uani 1 1 d . . . . .
H24A H -0.251149 0.494310 0.645154 0.079 Uiso 1 1 calc R U . . .
H24B H -0.400579 0.354855 0.601186 0.079 Uiso 1 1 calc R U . . .
H24C H -0.315430 0.417343 0.498311 0.079 Uiso 1 1 calc R U . . .
H15A H 0.099(12) 0.865(14) 0.110(12) 0.079 Uiso 1 1 d . U . . .
H7A H 1.098(13) 0.999(16) 0.372(14) 0.079 Uiso 1 1 d . U . . .
H7B H 1.038(11) 1.031(6) 0.461(4) 0.079 Uiso 1 1 d D U . . .
H15B H 0.173(12) 0.856(10) -0.006(9) 0.079 Uiso 1 1 d . U . . .
H8A H 0.845(5) 0.803(8) 0.537(5) 0.079 Uiso 1 1 d D U . . .
H16B H 0.438(10) 1.159(10) 0.011(8) 0.079 Uiso 1 1 d . U . . .
H8B H 0.708(4) 0.830(6) 0.506(7) 0.079 Uiso 1 1 d D U . . .
H16A H 0.435(10) 1.000(6) -0.078(3) 0.079 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O10 2.310(8) . ?
Gd1 O7 2.386(7) . ?
Gd1 O4 2.397(7) 1_565 ?
Gd1 O5 2.416(8) 1_455 ?
Gd1 O13 2.434(8) 1_665 ?
Gd1 O2 2.439(7) . ?
Gd1 O1 2.453(7) . ?
Gd1 O8 2.469(8) . ?
Gd1 C1 2.791(8) . ?
Gd1 O3 2.925(8) 1_565 ?
Gd1 C5 2.998(10) 1_565 ?
Gd2 O3 2.311(7) 1_565 ?
Gd2 O9 2.378(7) . ?
Gd2 O14 2.392(8) 1_665 ?
Gd2 O16 2.400(9) . ?
Gd2 O6 2.406(8) 1_455 ?
Gd2 O11 2.414(7) 1_565 ?
Gd2 O15 2.454(8) . ?
Gd2 O12 2.475(7) 1_565 ?
Gd2 C17 2.837(11) 1_565 ?
Gd2 O10 2.913(9) . ?
Gd2 C13 3.027(11) . ?
O1 C1 1.256(11) . ?
O2 C1 1.236(13) . ?
O3 C5 1.244(13) . ?
O4 C5 1.238(13) . ?
O5 C11 1.258(13) . ?
O6 C11 1.274(13) . ?
O7 H7A 0.69(11) . ?
O7 H7B 0.8600(15) . ?
O8 H8A 0.8600(15) . ?
O8 H8B 0.8600(15) . ?
O9 C13 1.268(12) . ?
O10 C13 1.278(13) . ?
O11 C17 1.285(13) . ?
O12 C17 1.271(11) . ?
O13 C23 1.234(13) . ?
O14 C23 1.239(14) . ?
O15 H15A 0.97(10) . ?
O15 H15B 0.90(10) . ?
O16 H16B 1.00(9) . ?
O16 H16A 0.8600(15) . ?
N1 C10 1.487(14) . ?
N1 C9 1.490(14) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C21 1.504(14) . ?
N2 C22 1.512(11) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
C1 C2 1.522(12) . ?
C2 C3 1.331(14) . ?
C2 C8 1.412(15) . ?
C3 C4 1.367(14) . ?
C3 H3 0.9300 . ?
C4 C6 1.431(13) . ?
C4 C5 1.542(13) . ?
C6 C7 1.313(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.418(13) . ?
C7 C9 1.499(14) . ?
C8 H8 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.494(16) . ?
C10 C12 1.506(14) . ?
C10 H10 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.459(14) . ?
C14 C20 1.368(14) . ?
C14 C15 1.412(13) . ?
C15 C16 1.448(12) . ?
C15 H15 0.9300 . ?
C16 C18 1.366(15) . ?
C16 C17 1.473(14) . ?
C18 C19 1.364(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.454(12) . ?
C19 C21 1.523(14) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C24 1.497(12) . ?
C22 C23 1.573(13) . ?
C22 H22 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 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
O10 Gd1 O7 144.3(3) . . ?
O10 Gd1 O4 123.9(3) . 1_565 ?
O7 Gd1 O4 78.3(3) . 1_565 ?
O10 Gd1 O5 73.6(3) . 1_455 ?
O7 Gd1 O5 142.0(3) . 1_455 ?
O4 Gd1 O5 77.3(3) 1_565 1_455 ?
O10 Gd1 O13 82.0(3) . 1_665 ?
O7 Gd1 O13 73.1(3) . 1_665 ?
O4 Gd1 O13 82.7(3) 1_565 1_665 ?
O5 Gd1 O13 131.2(3) 1_455 1_665 ?
O10 Gd1 O2 91.3(3) . . ?
O7 Gd1 O2 95.9(3) . . ?
O4 Gd1 O2 126.6(3) 1_565 . ?
O5 Gd1 O2 76.3(3) 1_455 . ?
O13 Gd1 O2 146.8(3) 1_665 . ?
O10 Gd1 O1 136.0(3) . . ?
O7 Gd1 O1 72.4(3) . . ?
O4 Gd1 O1 75.3(2) 1_565 . ?
O5 Gd1 O1 73.5(3) 1_455 . ?
O13 Gd1 O1 142.0(3) 1_665 . ?
O2 Gd1 O1 53.0(3) . . ?
O10 Gd1 O8 77.4(3) . . ?
O7 Gd1 O8 71.6(3) . . ?
O4 Gd1 O8 146.2(3) 1_565 . ?
O5 Gd1 O8 136.4(3) 1_455 . ?
O13 Gd1 O8 74.3(3) 1_665 . ?
O2 Gd1 O8 72.5(3) . . ?
O1 Gd1 O8 108.8(3) . . ?
O10 Gd1 C1 114.6(3) . . ?
O7 Gd1 C1 83.1(3) . . ?
O4 Gd1 C1 101.4(3) 1_565 . ?
O5 Gd1 C1 73.8(3) 1_455 . ?
O13 Gd1 C1 154.5(3) 1_665 . ?
O2 Gd1 C1 26.3(3) . . ?
O1 Gd1 C1 26.7(3) . . ?
O8 Gd1 C1 90.0(3) . . ?
O10 Gd1 O3 77.4(2) . 1_565 ?
O7 Gd1 O3 112.7(2) . 1_565 ?
O4 Gd1 O3 47.4(2) 1_565 1_565 ?
O5 Gd1 O3 68.8(2) 1_455 1_565 ?
O13 Gd1 O3 64.9(3) 1_665 1_565 ?
O2 Gd1 O3 145.1(3) . 1_565 ?
O1 Gd1 O3 115.9(2) . 1_565 ?
O8 Gd1 O3 134.3(3) . 1_565 ?
C1 Gd1 O3 135.3(3) . 1_565 ?
O10 Gd1 C5 101.4(3) . 1_565 ?
O7 Gd1 C5 94.2(3) . 1_565 ?
O4 Gd1 C5 23.3(3) 1_565 1_565 ?
O5 Gd1 C5 73.3(3) 1_455 1_565 ?
O13 Gd1 C5 71.1(3) 1_665 1_565 ?
O2 Gd1 C5 141.9(3) . 1_565 ?
O1 Gd1 C5 96.2(3) . 1_565 ?
O8 Gd1 C5 145.1(3) . 1_565 ?
C1 Gd1 C5 120.5(3) . 1_565 ?
O3 Gd1 C5 24.2(3) 1_565 1_565 ?
O3 Gd2 O9 124.8(3) 1_565 . ?
O3 Gd2 O14 75.4(3) 1_565 1_665 ?
O9 Gd2 O14 75.8(3) . 1_665 ?
O3 Gd2 O16 76.6(3) 1_565 . ?
O9 Gd2 O16 145.4(3) . . ?
O14 Gd2 O16 138.8(3) 1_665 . ?
O3 Gd2 O6 82.3(3) 1_565 1_455 ?
O9 Gd2 O6 80.8(3) . 1_455 ?
O14 Gd2 O6 129.0(3) 1_665 1_455 ?
O16 Gd2 O6 75.4(3) . 1_455 ?
O3 Gd2 O11 91.0(3) 1_565 1_565 ?
O9 Gd2 O11 126.9(3) . 1_565 ?
O14 Gd2 O11 78.1(3) 1_665 1_565 ?
O16 Gd2 O11 72.8(3) . 1_565 ?
O6 Gd2 O11 148.2(3) 1_455 1_565 ?
O3 Gd2 O15 143.5(3) 1_565 . ?
O9 Gd2 O15 78.2(3) . . ?
O14 Gd2 O15 141.1(3) 1_665 . ?
O16 Gd2 O15 71.2(4) . . ?
O6 Gd2 O15 73.6(3) 1_455 . ?
O11 Gd2 O15 95.4(3) 1_565 . ?
O3 Gd2 O12 136.9(2) 1_565 1_565 ?
O9 Gd2 O12 75.3(2) . 1_565 ?
O14 Gd2 O12 74.2(3) 1_665 1_565 ?
O16 Gd2 O12 108.7(3) . 1_565 ?
O6 Gd2 O12 140.8(3) 1_455 1_565 ?
O11 Gd2 O12 53.3(3) 1_565 1_565 ?
O15 Gd2 O12 71.5(3) . 1_565 ?
O3 Gd2 C17 115.4(3) 1_565 1_565 ?
O9 Gd2 C17 101.4(3) . 1_565 ?
O14 Gd2 C17 75.6(3) 1_665 1_565 ?
O16 Gd2 C17 90.1(3) . 1_565 ?
O6 Gd2 C17 154.2(3) 1_455 1_565 ?
O11 Gd2 C17 26.8(3) 1_565 1_565 ?
O15 Gd2 C17 81.7(3) . 1_565 ?
O12 Gd2 C17 26.6(2) 1_565 1_565 ?
O3 Gd2 O10 77.6(2) 1_565 . ?
O9 Gd2 O10 48.0(2) . . ?
O14 Gd2 O10 67.3(3) 1_665 . ?
O16 Gd2 O10 133.5(3) . . ?
O6 Gd2 O10 63.3(3) 1_455 . ?
O11 Gd2 O10 145.3(3) 1_565 . ?
O15 Gd2 O10 113.3(3) . . ?
O12 Gd2 O10 116.6(2) 1_565 . ?
C17 Gd2 O10 136.1(3) 1_565 . ?
O3 Gd2 C13 102.3(3) 1_565 . ?
O9 Gd2 C13 23.4(3) . . ?
O14 Gd2 C13 72.2(3) 1_665 . ?
O16 Gd2 C13 143.8(3) . . ?
O6 Gd2 C13 68.7(3) 1_455 . ?
O11 Gd2 C13 142.9(3) 1_565 . ?
O15 Gd2 C13 94.0(3) . . ?
O12 Gd2 C13 96.7(3) 1_565 . ?
C17 Gd2 C13 121.2(3) 1_565 . ?
O10 Gd2 C13 24.8(2) . . ?
C1 O1 Gd1 91.8(6) . . ?
C1 O2 Gd1 93.0(6) . . ?
C5 O3 Gd2 173.5(8) . 1_545 ?
C5 O3 Gd1 81.2(6) . 1_545 ?
Gd2 O3 Gd1 102.3(3) 1_545 1_545 ?
C5 O4 Gd1 106.7(7) . 1_545 ?
C11 O5 Gd1 136.0(7) . 1_655 ?
C11 O6 Gd2 136.2(7) . 1_655 ?
Gd1 O7 H7A 131(10) . . ?
Gd1 O7 H7B 111(6) . . ?
H7A O7 H7B 101(10) . . ?
Gd1 O8 H8A 134(4) . . ?
Gd1 O8 H8B 99(5) . . ?
H8A O8 H8B 118(7) . . ?
C13 O9 Gd2 108.4(7) . . ?
C13 O10 Gd1 172.6(9) . . ?
C13 O10 Gd2 82.6(7) . . ?
Gd1 O10 Gd2 102.7(3) . . ?
C17 O11 Gd2 95.3(6) . 1_545 ?
C17 O12 Gd2 92.8(6) . 1_545 ?
C23 O13 Gd1 134.1(7) . 1_445 ?
C23 O14 Gd2 134.6(7) . 1_445 ?
Gd2 O15 H15A 129(8) . . ?
Gd2 O15 H15B 121(7) . . ?
H15A O15 H15B 105(10) . . ?
Gd2 O16 H16B 108(5) . . ?
Gd2 O16 H16A 127(5) . . ?
H16B O16 H16A 122(7) . . ?
C10 N1 C9 114.9(9) . . ?
C10 N1 H1A 108.5 . . ?
C9 N1 H1A 108.5 . . ?
C10 N1 H1B 108.5 . . ?
C9 N1 H1B 108.5 . . ?
H1A N1 H1B 107.5 . . ?
C21 N2 C22 111.6(9) . . ?
C21 N2 H2A 109.3 . . ?
C22 N2 H2A 109.3 . . ?
C21 N2 H2B 109.3 . . ?
C22 N2 H2B 109.3 . . ?
H2A N2 H2B 108.0 . . ?
O2 C1 O1 122.2(8) . . ?
O2 C1 C2 116.3(9) . . ?
O1 C1 C2 121.3(9) . . ?
O2 C1 Gd1 60.8(5) . . ?
O1 C1 Gd1 61.5(5) . . ?
C2 C1 Gd1 173.2(7) . . ?
C3 C2 C8 119.9(9) . . ?
C3 C2 C1 121.7(9) . . ?
C8 C2 C1 118.0(9) . . ?
C2 C3 C4 121.0(10) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C6 118.5(9) . . ?
C3 C4 C5 122.6(9) . . ?
C6 C4 C5 118.6(9) . . ?
O4 C5 O3 124.1(10) . . ?
O4 C5 C4 116.9(10) . . ?
O3 C5 C4 118.4(9) . . ?
O4 C5 Gd1 50.0(5) . 1_545 ?
O3 C5 Gd1 74.6(6) . 1_545 ?
C4 C5 Gd1 160.1(7) . 1_545 ?
C7 C6 C4 122.7(9) . . ?
C7 C6 H6 118.6 . . ?
C4 C6 H6 118.6 . . ?
C6 C7 C8 117.4(9) . . ?
C6 C7 C9 122.3(9) . . ?
C8 C7 C9 119.6(9) . . ?
C2 C8 C7 120.3(10) . . ?
C2 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
N1 C9 C7 115.6(9) . . ?
N1 C9 H9A 108.4 . . ?
C7 C9 H9A 108.4 . . ?
N1 C9 H9B 108.4 . . ?
C7 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
N1 C10 C11 107.8(9) . . ?
N1 C10 C12 110.0(9) . . ?
C11 C10 C12 113.7(8) . . ?
N1 C10 H10 108.4 . . ?
C11 C10 H10 108.4 . . ?
C12 C10 H10 108.4 . . ?
O5 C11 O6 126.3(10) . . ?
O5 C11 C10 117.0(9) . . ?
O6 C11 C10 116.6(9) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O9 C13 O10 120.1(10) . . ?
O9 C13 C14 118.7(9) . . ?
O10 C13 C14 121.2(9) . . ?
O9 C13 Gd2 48.2(5) . . ?
O10 C13 Gd2 72.6(6) . . ?
C14 C13 Gd2 163.7(7) . . ?
C20 C14 C15 121.4(9) . . ?
C20 C14 C13 118.8(9) . . ?
C15 C14 C13 119.0(9) . . ?
C14 C15 C16 117.8(10) . . ?
C14 C15 H15 121.1 . . ?
C16 C15 H15 121.1 . . ?
C18 C16 C15 120.6(9) . . ?
C18 C16 C17 121.2(9) . . ?
C15 C16 C17 117.8(9) . . ?
O12 C17 O11 118.4(10) . . ?
O12 C17 C16 119.8(9) . . ?
O11 C17 C16 121.8(9) . . ?
O12 C17 Gd2 60.6(5) . 1_545 ?
O11 C17 Gd2 57.9(5) . 1_545 ?
C16 C17 Gd2 175.8(8) . 1_545 ?
C19 C18 C16 120.9(9) . . ?
C19 C18 H18 119.6 . . ?
C16 C18 H18 119.6 . . ?
C18 C19 C20 120.5(9) . . ?
C18 C19 C21 122.6(8) . . ?
C20 C19 C21 116.7(9) . . ?
C14 C20 C19 118.7(9) . . ?
C14 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
N2 C21 C19 111.3(9) . . ?
N2 C21 H21A 109.4 . . ?
C19 C21 H21A 109.4 . . ?
N2 C21 H21B 109.4 . . ?
C19 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C24 C22 N2 113.4(8) . . ?
C24 C22 C23 113.9(8) . . ?
N2 C22 C23 107.0(8) . . ?
C24 C22 H22 107.4 . . ?
N2 C22 H22 107.4 . . ?
C23 C22 H22 107.4 . . ?
O13 C23 O14 127.3(9) . . ?
O13 C23 C22 115.8(9) . . ?
O14 C23 C22 116.7(9) . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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
Gd1 O2 C1 O1 -2.9(11) . . . . ?
Gd1 O2 C1 C2 173.1(8) . . . . ?
Gd1 O1 C1 O2 2.8(11) . . . . ?
Gd1 O1 C1 C2 -172.9(8) . . . . ?
O2 C1 C2 C3 8.3(16) . . . . ?
O1 C1 C2 C3 -175.7(11) . . . . ?
O2 C1 C2 C8 -165.4(10) . . . . ?
O1 C1 C2 C8 10.5(15) . . . . ?
C8 C2 C3 C4 0.6(17) . . . . ?
C1 C2 C3 C4 -173.0(10) . . . . ?
C2 C3 C4 C6 -1.4(16) . . . . ?
C2 C3 C4 C5 172.2(10) . . . . ?
Gd1 O4 C5 O3 -9.1(13) 1_545 . . . ?
Gd1 O4 C5 C4 161.9(7) 1_545 . . . ?
Gd1 O3 C5 O4 7.2(11) 1_545 . . . ?
Gd1 O3 C5 C4 -163.6(9) 1_545 . . . ?
C3 C4 C5 O4 -157.7(11) . . . . ?
C6 C4 C5 O4 15.9(14) . . . . ?
C3 C4 C5 O3 13.8(16) . . . . ?
C6 C4 C5 O3 -172.6(11) . . . . ?
C3 C4 C5 Gd1 -113(2) . . . 1_545 ?
C6 C4 C5 Gd1 60(2) . . . 1_545 ?
C3 C4 C6 C7 -1.3(16) . . . . ?
C5 C4 C6 C7 -175.1(10) . . . . ?
C4 C6 C7 C8 4.4(16) . . . . ?
C4 C6 C7 C9 174.9(10) . . . . ?
C3 C2 C8 C7 2.7(17) . . . . ?
C1 C2 C8 C7 176.6(9) . . . . ?
C6 C7 C8 C2 -5.1(16) . . . . ?
C9 C7 C8 C2 -175.9(10) . . . . ?
C10 N1 C9 C7 160.8(9) . . . . ?
C6 C7 C9 N1 131.7(11) . . . . ?
C8 C7 C9 N1 -57.9(13) . . . . ?
C9 N1 C10 C11 -65.6(12) . . . . ?
C9 N1 C10 C12 170.0(8) . . . . ?
Gd1 O5 C11 O6 29.1(16) 1_655 . . . ?
Gd1 O5 C11 C10 -148.2(8) 1_655 . . . ?
Gd2 O6 C11 O5 8.4(17) 1_655 . . . ?
Gd2 O6 C11 C10 -174.4(7) 1_655 . . . ?
N1 C10 C11 O5 140.0(10) . . . . ?
C12 C10 C11 O5 -97.7(11) . . . . ?
N1 C10 C11 O6 -37.4(13) . . . . ?
C12 C10 C11 O6 84.8(11) . . . . ?
Gd2 O9 C13 O10 11.5(13) . . . . ?
Gd2 O9 C13 C14 -168.1(8) . . . . ?
Gd2 O10 C13 O9 -9.0(10) . . . . ?
Gd2 O10 C13 C14 170.6(10) . . . . ?
O9 C13 C14 C20 -9.3(15) . . . . ?
O10 C13 C14 C20 171.1(11) . . . . ?
Gd2 C13 C14 C20 -43(3) . . . . ?
O9 C13 C14 C15 160.9(10) . . . . ?
O10 C13 C14 C15 -18.7(16) . . . . ?
Gd2 C13 C14 C15 128(2) . . . . ?
C20 C14 C15 C16 3.3(15) . . . . ?
C13 C14 C15 C16 -166.7(9) . . . . ?
C14 C15 C16 C18 -3.2(16) . . . . ?
C14 C15 C16 C17 169.6(9) . . . . ?
Gd2 O12 C17 O11 -4.4(11) 1_545 . . . ?
Gd2 O12 C17 C16 175.2(9) 1_545 . . . ?
Gd2 O11 C17 O12 4.6(11) 1_545 . . . ?
Gd2 O11 C17 C16 -175.1(9) 1_545 . . . ?
C18 C16 C17 O12 -12.7(17) . . . . ?
C15 C16 C17 O12 174.5(10) . . . . ?
C18 C16 C17 O11 167.0(11) . . . . ?
C15 C16 C17 O11 -5.8(17) . . . . ?
C15 C16 C18 C19 2.0(17) . . . . ?
C17 C16 C18 C19 -170.6(11) . . . . ?
C16 C18 C19 C20 -0.8(17) . . . . ?
C16 C18 C19 C21 172.8(10) . . . . ?
C15 C14 C20 C19 -2.2(15) . . . . ?
C13 C14 C20 C19 167.8(9) . . . . ?
C18 C19 C20 C14 0.9(16) . . . . ?
C21 C19 C20 C14 -173.1(10) . . . . ?
C22 N2 C21 C19 -161.1(8) . . . . ?
C18 C19 C21 N2 57.2(14) . . . . ?
C20 C19 C21 N2 -129.0(10) . . . . ?
C21 N2 C22 C24 -57.6(10) . . . . ?
C21 N2 C22 C23 68.9(11) . . . . ?
Gd1 O13 C23 O14 5.3(18) 1_445 . . . ?
Gd1 O13 C23 C22 -179.0(7) 1_445 . . . ?
Gd2 O14 C23 O13 -44.8(17) 1_445 . . . ?
Gd2 O14 C23 C22 139.5(8) 1_445 . . . ?
C24 C22 C23 O13 162.7(9) . . . . ?
N2 C22 C23 O13 36.5(13) . . . . ?
C24 C22 C23 O14 -21.1(13) . . . . ?
N2 C22 C23 O14 -147.3(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2B Cl1 0.89 2.41 3.209(10) 148.9 . yes
N2 H2A Cl2 0.89 2.19 3.071(9) 172.6 . yes
O8 H8A O18 0.8600(15) 2.01(3) 2.800(11) 152(6) . yes
N1 H1A Cl1 0.89 2.25 3.129(9) 168.6 1_654 yes
N1 H1B Cl2 0.89 2.41 3.210(10) 149.6 1_654 yes
O7 H7B Cl1 0.8600(15) 2.40(3) 3.234(9) 162(8) 1_665 yes
O7 H7A O12 0.69(11) 2.08(12) 2.764(10) 172(15) 1_665 yes
O15 H15B Cl2 0.90(10) 2.37(10) 3.216(9) 157(8) 1_554 yes
O15 H15A O1 0.97(10) 1.81(11) 2.744(11) 162(11) 1_455 yes

_refine_diff_density_max         0.668
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.075


# start Validation Reply Form
_vrf_PLAT306_I                   
;
RESPONSE: The H atoms of lattice water molecules O17, O18, O19, 
O20 and O21 were not added owing to not suitable Fourier maps 
being picked up.
;
_vrf_PLAT430_I                   
;
RESPONSE: The H atoms of lattice water molecules O17, O19, O20 
and O21 were not added owing to not suitable Fourier maps being 
picked up. Thus hydrogen-bonding interactions between them 
could not be determined.
;
_vrf_PLAT987_I                   
;
RESPONSE: A BASF/TWIN Refinement does not well, but the 
measurement of CD spectrum as well as homochiral ligand 
further confirm the homochiral framework of I.
;


####################################################################### 
# 
# 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_II
_database_code_depnum_ccdc_archive 'CCDC 1852704'
_audit_update_record             
;
2018-07-01 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            'C24 H40 Cl2 Eu2 N2 O21'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H30 Eu2 N2 O16, 2(Cl), 5(H2 O)'
_chemical_formula_sum            'C24 H40 Cl2 Eu2 N2 O21'
_chemical_formula_weight         1067.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 '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'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.6686(6)
_cell_length_b                   10.0202(4)
_cell_length_c                   10.8727(4)
_cell_angle_alpha                104.824(3)
_cell_angle_beta                 93.710(5)
_cell_angle_gamma                109.569(5)
_cell_volume                     946.31(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5232
_cell_measurement_theta_min      3.9140
_cell_measurement_theta_max      27.5850

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_F_000             526
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    3.506
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14889
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.394
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7672
_reflns_number_gt                6514
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.988
_reflns_Friedel_fraction_max     0.986
_reflns_Friedel_fraction_full    0.990

_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0500P)²+6.3484P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2492 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.20(3)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         7672
_refine_ls_number_parameters     486
_refine_ls_number_restraints     194
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1427
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.041
_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
Eu1 Eu 0.69640(7) 0.39466(7) 0.47663(7) 0.0260(4) Uani 1 1 d D . . . .
Eu2 Eu 1.02998(7) 0.24809(7) 0.55522(7) 0.0266(4) Uani 1 1 d D . . . .
Cl1 Cl 0.3338(16) 0.0455(14) 0.0862(11) 0.064(4) Uani 1 1 d . . . . .
Cl2 Cl 0.3741(14) 0.5917(13) 0.9587(11) 0.055(3) Uani 1 1 d . . . . .
O1 O 0.548(2) 0.516(2) 0.605(2) 0.028(5) Uani 1 1 d . U . . .
O2 O 0.7281(17) 0.6596(17) 0.5345(16) 0.031(4) Uani 1 1 d . U . . .
O3 O 0.7750(17) 1.1880(17) 0.5654(16) 0.025(4) Uani 1 1 d . U . . .
O4 O 0.568(2) 1.224(2) 0.589(2) 0.031(5) Uani 1 1 d . . . . .
O5 O -0.164(2) 0.4997(19) 0.6939(17) 0.026(4) Uani 1 1 d . U . . .
O6 O 0.058(2) 0.481(2) 0.713(2) 0.033(6) Uani 1 1 d . . . . .
O7 O 0.444(3) 0.298(3) 0.349(2) 0.046(6) Uani 1 1 d D U . . .
O8 O 0.704(4) 0.454(3) 0.266(3) 0.078(10) Uani 1 1 d D . . . .
O9 O 0.183(2) 0.130(3) 0.430(3) 0.038(7) Uani 1 1 d . . . . .
O10 O 0.0248(18) -0.0002(18) 0.5316(16) 0.036(4) Uani 1 1 d . U . . .
O11 O -0.0601(18) -0.5427(19) 0.4402(16) 0.031(4) Uani 1 1 d . U . . .
O12 O 0.149(3) -0.590(3) 0.435(3) 0.043(6) Uani 1 1 d . U . . .
O13 O 0.889(2) 0.120(2) 0.339(2) 0.037(5) Uani 1 1 d . U . . .
O14 O 0.676(3) 0.166(3) 0.320(3) 0.039(6) Uani 1 1 d . U . . .
O15 O 1.027(3) 0.205(4) 0.764(2) 0.065(9) Uani 1 1 d D . . . .
O16 O 1.283(2) 0.359(2) 0.667(2) 0.029(5) Uani 1 1 d D U . . .
O17 O 0.434(3) 0.442(3) 0.145(3) 0.142(12) Uani 1 1 d . . . . .
O18 O 0.652(4) 0.283(3) 0.016(3) 0.151(12) Uani 1 1 d . . . . .
O19 O 1.009(6) -0.068(6) 0.168(5) 0.25(2) Uani 1 1 d . U . . .
O20 O 1.115(4) 0.233(4) 1.156(4) 0.143(12) Uani 1 1 d . U . . .
O21 O -0.353(3) 0.492(3) 0.895(3) 0.104(8) Uani 1 1 d . U . . .
N1 N 0.192(3) 0.767(3) 0.845(2) 0.031(6) Uani 1 1 d D U . . .
H1A H 0.237329 0.844035 0.917926 0.038 Uiso 1 1 calc R U . . .
H1B H 0.240733 0.702362 0.839979 0.038 Uiso 1 1 calc R U . . .
N2 N 0.534(3) -0.117(3) 0.179(2) 0.023(5) Uani 1 1 d D U . . .
H2A H 0.488542 -0.191135 0.103883 0.028 Uiso 1 1 calc R U . . .
H2B H 0.491632 -0.047739 0.185508 0.028 Uiso 1 1 calc R U . . .
C1 C 0.618(3) 0.640(3) 0.586(3) 0.024(7) Uani 1 1 d D U . . .
C2 C 0.558(3) 0.762(2) 0.627(2) 0.013(5) Uani 1 1 d D . . . .
C3 C 0.645(3) 0.902(2) 0.619(3) 0.018(6) Uani 1 1 d D U . . .
H3 H 0.740952 0.921397 0.596121 0.022 Uiso 1 1 calc R U . . .
C4 C 0.584(3) 1.013(3) 0.646(3) 0.028(7) Uani 1 1 d D U . . .
C5 C 0.643(4) 1.151(4) 0.601(4) 0.034(8) Uani 1 1 d . U . . .
C6 C 0.447(3) 0.987(3) 0.690(3) 0.030(8) Uani 1 1 d D . . . .
H6 H 0.407341 1.063939 0.709228 0.036 Uiso 1 1 calc R U . . .
C7 C 0.368(2) 0.850(3) 0.707(3) 0.023(6) Uani 1 1 d D . . . .
H7A H 0.392(18) 0.224(12) 0.37(2) 0.035 Uiso 1 1 d D U . . .
H15A H 1.04(2) 0.256(10) 0.841(7) 0.035 Uiso 1 1 d D U . . .
H8B H 0.69(3) 0.423(16) 0.185(4) 0.035 Uiso 1 1 d D U . . .
H15B H 0.97(2) 0.121(8) 0.767(4) 0.035 Uiso 1 1 d D U . . .
H16A H 1.364(13) 0.40(2) 0.64(2) 0.035 Uiso 1 1 d D U . . .
H7B H 0.398(6) 0.356(8) 0.371(11) 0.035 Uiso 1 1 d D U . . .
H16B H 1.29(2) 0.40(2) 0.746(5) 0.035 Uiso 1 1 d D U . . .
H8A H 0.69(2) 0.532(12) 0.274(6) 0.035 Uiso 1 1 d D U . . .
C8 C 0.429(4) 0.739(3) 0.679(3) 0.027(7) Uani 1 1 d D . . . .
H8 H 0.380474 0.647190 0.695460 0.033 Uiso 1 1 calc R U . . .
C9 C 0.210(3) 0.824(4) 0.732(3) 0.035(8) Uani 1 1 d D . . . .
H9A H 0.192297 0.918593 0.749303 0.042 Uiso 1 1 calc R U . . .
H9B H 0.138379 0.751856 0.655275 0.042 Uiso 1 1 calc R U . . .
C10 C 0.034(4) 0.690(3) 0.860(2) 0.024(7) Uani 1 1 d D U . . .
H10 H 0.033129 0.664845 0.942970 0.029 Uiso 1 1 calc R U . . .
C11 C -0.057(2) 0.792(2) 0.858(3) 0.060(7) Uani 1 1 d . . . . .
H11A H -0.017578 0.879567 0.934297 0.090 Uiso 1 1 calc R U . . .
H11B H -0.161759 0.737442 0.859820 0.090 Uiso 1 1 calc R U . . .
H11C H -0.049154 0.823612 0.779959 0.090 Uiso 1 1 calc R U . . .
C12 C -0.033(3) 0.545(3) 0.746(3) 0.021(6) Uani 1 1 d D U . . .
C13 C 0.124(3) 0.013(3) 0.457(3) 0.032(8) Uani 1 1 d D . . . .
C14 C 0.165(4) -0.124(3) 0.404(4) 0.051(10) Uani 1 1 d D U . . .
C15 C 0.090(3) -0.258(3) 0.425(3) 0.034(8) Uani 1 1 d D . . . .
H15 H 0.000291 -0.273383 0.459501 0.040 Uiso 1 1 calc R U . . .
C16 C 0.149(3) -0.370(3) 0.396(3) 0.025(7) Uani 1 1 d D . . . .
C17 C 0.072(3) -0.512(3) 0.425(3) 0.024(7) Uani 1 1 d D . . . .
C18 C 0.284(3) -0.345(3) 0.351(3) 0.027(7) Uani 1 1 d D U . . .
H18 H 0.321625 -0.422617 0.330490 0.033 Uiso 1 1 calc R U . . .
C19 C 0.363(3) -0.213(3) 0.336(3) 0.034(8) Uani 1 1 d D U . . .
C20 C 0.309(4) -0.096(3) 0.366(3) 0.024(6) Uani 1 1 d . U . . .
H20 H 0.366920 -0.000769 0.362023 0.029 Uiso 1 1 calc R U . . .
C21 C 0.511(3) -0.179(4) 0.290(3) 0.029(7) Uani 1 1 d D U . . .
H21A H 0.587218 -0.108585 0.364558 0.035 Uiso 1 1 calc R U . . .
H21B H 0.531222 -0.272169 0.268190 0.035 Uiso 1 1 calc R U . . .
C22 C 0.695(4) -0.049(3) 0.174(2) 0.047(12) Uani 1 1 d D . . . .
H22 H 0.747910 -0.118775 0.177948 0.057 Uiso 1 1 calc R U . . .
C23 C 0.699(3) -0.010(3) 0.044(2) 0.064(8) Uani 1 1 d D . . . .
H23A H 0.663199 -0.102027 -0.027717 0.096 Uiso 1 1 calc R U . . .
H23B H 0.801932 0.048255 0.040064 0.096 Uiso 1 1 calc R U . . .
H23C H 0.635918 0.047016 0.039078 0.096 Uiso 1 1 calc R U . . .
C24 C 0.755(4) 0.092(3) 0.291(3) 0.038(9) Uani 1 1 d 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 O11 2.313(17) 1_665 ?
Eu1 O4 2.41(2) 1_545 ?
Eu1 O14 2.41(3) . ?
Eu1 O5 2.425(18) 1_655 ?
Eu1 O1 2.46(2) . ?
Eu1 O7 2.47(2) . ?
Eu1 O2 2.472(15) . ?
Eu1 O8 2.51(3) . ?
Eu1 O3 2.789(16) 1_545 ?
Eu1 C1 2.81(2) . ?
Eu1 C5 3.00(3) 1_545 ?
Eu1 Eu2 4.0925(9) . ?
Eu2 O3 2.351(16) 1_545 ?
Eu2 O12 2.39(3) 1_665 ?
Eu2 O16 2.413(19) . ?
Eu2 O15 2.41(2) . ?
Eu2 O10 2.417(16) 1_655 ?
Eu2 O13 2.43(2) . ?
Eu2 O6 2.44(2) 1_655 ?
Eu2 O9 2.46(2) 1_655 ?
Eu2 C13 2.79(3) 1_655 ?
Eu2 C17 3.02(3) 1_665 ?
Eu2 O11 3.023(17) 1_665 ?
O1 C1 1.27(4) . ?
O2 C1 1.22(3) . ?
O3 C5 1.32(4) . ?
O4 C5 1.21(4) . ?
O5 C12 1.23(3) . ?
O6 C12 1.27(4) . ?
O7 H7A 0.841(15) . ?
O7 H7B 0.838(15) . ?
O8 H8B 0.843(15) . ?
O8 H8A 0.843(15) . ?
O9 C13 1.24(4) . ?
O10 C13 1.29(4) . ?
O11 C17 1.24(3) . ?
O12 C17 1.26(4) . ?
O13 C24 1.27(4) . ?
O14 C24 1.24(4) . ?
O15 H15A 0.843(15) . ?
O15 H15B 0.840(15) . ?
O16 H16A 0.842(15) . ?
O16 H16B 0.840(15) . ?
N1 C9 1.489(13) . ?
N1 C10 1.50(4) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 C22 1.48(4) . ?
N2 C21 1.497(13) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
C1 C2 1.503(13) . ?
C2 C8 1.38(4) . ?
C2 C3 1.401(14) . ?
C3 C4 1.399(13) . ?
C3 H3 0.9500 . ?
C4 C6 1.40(3) . ?
C4 C5 1.52(3) . ?
C6 C7 1.401(14) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(14) . ?
C7 C9 1.52(2) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C12 1.552(13) . ?
C10 C11 1.56(4) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 C14 1.534(14) . ?
C14 C15 1.37(3) . ?
C14 C20 1.44(5) . ?
C15 C16 1.395(13) . ?
C15 H15 0.9500 . ?
C16 C18 1.393(14) . ?
C16 C17 1.491(14) . ?
C18 C19 1.34(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.41(3) . ?
C19 C21 1.505(14) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C24 1.551(14) . ?
C22 C23 1.555(14) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Eu1 O4 128.3(7) 1_665 1_545 ?
O11 Eu1 O14 80.6(8) 1_665 . ?
O4 Eu1 O14 81.5(9) 1_545 . ?
O11 Eu1 O5 77.6(6) 1_665 1_655 ?
O4 Eu1 O5 76.1(7) 1_545 1_655 ?
O14 Eu1 O5 127.6(7) . 1_655 ?
O11 Eu1 O1 137.2(7) 1_665 . ?
O4 Eu1 O1 74.9(8) 1_545 . ?
O14 Eu1 O1 142.1(8) . . ?
O5 Eu1 O1 74.7(7) 1_655 . ?
O11 Eu1 O7 138.2(7) 1_665 . ?
O4 Eu1 O7 80.7(7) 1_545 . ?
O14 Eu1 O7 74.5(8) . . ?
O5 Eu1 O7 143.9(7) 1_655 . ?
O1 Eu1 O7 72.8(7) . . ?
O11 Eu1 O2 89.4(5) 1_665 . ?
O4 Eu1 O2 124.8(7) 1_545 . ?
O14 Eu1 O2 151.1(7) . . ?
O5 Eu1 O2 75.4(6) 1_655 . ?
O1 Eu1 O2 52.4(6) . . ?
O7 Eu1 O2 96.5(7) . . ?
O11 Eu1 O8 72.5(10) 1_665 . ?
O4 Eu1 O8 145.8(10) 1_545 . ?
O14 Eu1 O8 75.6(9) . . ?
O5 Eu1 O8 138.2(9) 1_655 . ?
O1 Eu1 O8 109.1(9) . . ?
O7 Eu1 O8 69.0(10) . . ?
O2 Eu1 O8 75.6(7) . . ?
O11 Eu1 O3 80.3(5) 1_665 1_545 ?
O4 Eu1 O3 48.6(6) 1_545 1_545 ?
O14 Eu1 O3 62.1(7) . 1_545 ?
O5 Eu1 O3 67.5(5) 1_655 1_545 ?
O1 Eu1 O3 117.0(6) . 1_545 ?
O7 Eu1 O3 115.0(6) . 1_545 ?
O2 Eu1 O3 142.8(5) . 1_545 ?
O8 Eu1 O3 132.7(8) . 1_545 ?
O11 Eu1 C1 113.9(8) 1_665 . ?
O4 Eu1 C1 101.2(9) 1_545 . ?
O14 Eu1 C1 156.3(8) . . ?
O5 Eu1 C1 75.4(8) 1_655 . ?
O1 Eu1 C1 26.9(8) . . ?
O7 Eu1 C1 82.6(9) . . ?
O2 Eu1 C1 25.6(7) . . ?
O8 Eu1 C1 90.6(10) . . ?
O3 Eu1 C1 136.2(7) 1_545 . ?
O11 Eu1 C5 106.1(8) 1_665 1_545 ?
O4 Eu1 C5 22.7(9) 1_545 1_545 ?
O14 Eu1 C5 69.7(10) . 1_545 ?
O5 Eu1 C5 71.6(8) 1_655 1_545 ?
O1 Eu1 C5 95.4(9) . 1_545 ?
O7 Eu1 C5 96.1(9) . 1_545 ?
O2 Eu1 C5 139.1(8) . 1_545 ?
O8 Eu1 C5 144.9(10) . 1_545 ?
O3 Eu1 C5 26.0(8) 1_545 1_545 ?
C1 Eu1 C5 119.9(10) . 1_545 ?
O11 Eu1 Eu2 46.8(4) 1_665 . ?
O4 Eu1 Eu2 81.6(5) 1_545 . ?
O14 Eu1 Eu2 67.0(6) . . ?
O5 Eu1 Eu2 63.3(4) 1_655 . ?
O1 Eu1 Eu2 135.7(5) . . ?
O7 Eu1 Eu2 139.4(6) . . ?
O2 Eu1 Eu2 123.5(4) . . ?
O8 Eu1 Eu2 111.3(9) . . ?
O3 Eu1 Eu2 33.7(3) 1_545 . ?
C1 Eu1 Eu2 136.7(6) . . ?
C5 Eu1 Eu2 59.3(7) 1_545 . ?
O3 Eu2 O12 120.4(8) 1_545 1_665 ?
O3 Eu2 O16 148.4(6) 1_545 . ?
O12 Eu2 O16 77.6(8) 1_665 . ?
O3 Eu2 O15 80.4(8) 1_545 . ?
O12 Eu2 O15 146.1(9) 1_665 . ?
O16 Eu2 O15 73.0(8) . . ?
O3 Eu2 O10 94.9(5) 1_545 1_655 ?
O12 Eu2 O10 127.1(8) 1_665 1_655 ?
O16 Eu2 O10 92.4(6) . 1_655 ?
O15 Eu2 O10 71.2(9) . 1_655 ?
O3 Eu2 O13 71.0(6) 1_545 . ?
O12 Eu2 O13 77.3(8) 1_665 . ?
O16 Eu2 O13 140.6(7) . . ?
O15 Eu2 O13 136.6(8) . . ?
O10 Eu2 O13 79.3(6) 1_655 . ?
O3 Eu2 O6 84.3(6) 1_545 1_655 ?
O12 Eu2 O6 82.4(9) 1_665 1_655 ?
O16 Eu2 O6 72.0(7) . 1_655 ?
O15 Eu2 O6 72.8(10) . 1_655 ?
O10 Eu2 O6 143.6(8) 1_655 1_655 ?
O13 Eu2 O6 133.2(8) . 1_655 ?
O3 Eu2 O9 136.1(7) 1_545 1_655 ?
O12 Eu2 O9 74.1(9) 1_665 1_655 ?
O16 Eu2 O9 71.0(7) . 1_655 ?
O15 Eu2 O9 110.8(10) . 1_655 ?
O10 Eu2 O9 53.9(7) 1_655 1_655 ?
O13 Eu2 O9 73.1(8) . 1_655 ?
O6 Eu2 O9 139.5(7) 1_655 1_655 ?
O3 Eu2 C13 117.0(8) 1_545 1_655 ?
O12 Eu2 C13 100.0(10) 1_665 1_655 ?
O16 Eu2 C13 81.0(8) . 1_655 ?
O15 Eu2 C13 91.8(11) . 1_655 ?
O10 Eu2 C13 27.5(8) 1_655 1_655 ?
O13 Eu2 C13 74.0(8) . 1_655 ?
O6 Eu2 C13 151.8(8) 1_655 1_655 ?
O9 Eu2 C13 26.3(9) 1_655 1_655 ?
O3 Eu2 C17 98.6(7) 1_545 1_665 ?
O12 Eu2 C17 23.5(9) 1_665 1_665 ?
O16 Eu2 C17 92.6(7) . 1_665 ?
O15 Eu2 C17 142.5(10) . 1_665 ?
O10 Eu2 C17 145.4(7) 1_655 1_665 ?
O13 Eu2 C17 75.2(7) . 1_665 ?
O6 Eu2 C17 69.8(9) 1_655 1_665 ?
O9 Eu2 C17 96.0(8) 1_655 1_665 ?
C13 Eu2 C17 120.6(10) 1_655 1_665 ?
O3 Eu2 O11 74.9(5) 1_545 1_665 ?
O12 Eu2 O11 46.7(7) 1_665 1_665 ?
O16 Eu2 O11 112.2(6) . 1_665 ?
O15 Eu2 O11 133.7(9) . 1_665 ?
O10 Eu2 O11 148.3(5) 1_655 1_665 ?
O13 Eu2 O11 69.0(6) . 1_665 ?
O6 Eu2 O11 66.4(7) 1_655 1_665 ?
O9 Eu2 O11 114.2(7) 1_655 1_665 ?
C13 Eu2 O11 134.3(8) 1_655 1_665 ?
C17 Eu2 O11 23.8(7) 1_665 1_665 ?
O3 Eu2 Eu1 41.1(4) 1_545 . ?
O12 Eu2 Eu1 80.4(7) 1_665 . ?
O16 Eu2 Eu1 136.4(5) . . ?
O15 Eu2 Eu1 110.1(8) . . ?
O10 Eu2 Eu1 130.6(4) 1_655 . ?
O13 Eu2 Eu1 67.1(5) . . ?
O6 Eu2 Eu1 68.1(5) 1_655 . ?
O9 Eu2 Eu1 136.5(6) 1_655 . ?
C13 Eu2 Eu1 140.1(6) 1_655 . ?
C17 Eu2 Eu1 57.7(6) 1_665 . ?
O11 Eu2 Eu1 33.9(3) 1_665 . ?
C1 O1 Eu1 92.2(17) . . ?
C1 O2 Eu1 93.0(14) . . ?
C5 O3 Eu2 165(2) . 1_565 ?
C5 O3 Eu1 86.1(17) . 1_565 ?
Eu2 O3 Eu1 105.2(6) 1_565 1_565 ?
C5 O4 Eu1 107(2) . 1_565 ?
C12 O5 Eu1 137.6(18) . 1_455 ?
C12 O6 Eu2 132.7(17) . 1_455 ?
Eu1 O7 H7A 108(10) . . ?
Eu1 O7 H7B 113(3) . . ?
H7A O7 H7B 102(2) . . ?
Eu1 O8 H8B 147(9) . . ?
Eu1 O8 H8A 109(3) . . ?
H8B O8 H8A 101(2) . . ?
C13 O9 Eu2 91.8(18) . 1_455 ?
C13 O10 Eu2 92.6(16) . 1_455 ?
C17 O11 Eu1 177.0(19) . 1_445 ?
C17 O11 Eu2 78.0(15) . 1_445 ?
Eu1 O11 Eu2 99.3(6) 1_445 1_445 ?
C17 O12 Eu2 108(2) . 1_445 ?
C24 O13 Eu2 133(2) . . ?
C24 O14 Eu1 137(2) . . ?
Eu2 O15 H15A 137(10) . . ?
Eu2 O15 H15B 118(3) . . ?
H15A O15 H15B 101(2) . . ?
Eu2 O16 H16A 132(10) . . ?
Eu2 O16 H16B 113(10) . . ?
H16A O16 H16B 108(10) . . ?
C9 N1 C10 115(2) . . ?
C9 N1 H1A 108.5 . . ?
C10 N1 H1A 108.5 . . ?
C9 N1 H1B 108.5 . . ?
C10 N1 H1B 108.5 . . ?
H1A N1 H1B 107.5 . . ?
C22 N2 C21 111(2) . . ?
C22 N2 H2A 109.4 . . ?
C21 N2 H2A 109.4 . . ?
C22 N2 H2B 109.4 . . ?
C21 N2 H2B 109.4 . . ?
H2A N2 H2B 108.0 . . ?
O2 C1 O1 122(2) . . ?
O2 C1 C2 120(2) . . ?
O1 C1 C2 118(3) . . ?
O2 C1 Eu1 61.4(12) . . ?
O1 C1 Eu1 60.9(13) . . ?
C2 C1 Eu1 172(2) . . ?
C8 C2 C3 122(2) . . ?
C8 C2 C1 121(2) . . ?
C3 C2 C1 117(2) . . ?
C4 C3 C2 118(2) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
C3 C4 C6 121(3) . . ?
C3 C4 C5 122(3) . . ?
C6 C4 C5 116(2) . . ?
O4 C5 O3 118(3) . . ?
O4 C5 C4 122(3) . . ?
O3 C5 C4 120(3) . . ?
O4 C5 Eu1 50.1(16) . 1_565 ?
O3 C5 Eu1 67.9(15) . 1_565 ?
C4 C5 Eu1 168(2) . 1_565 ?
C7 C6 C4 120(2) . . ?
C7 C6 H6 119.8 . . ?
C4 C6 H6 119.8 . . ?
C8 C7 C6 119(2) . . ?
C8 C7 C9 124(2) . . ?
C6 C7 C9 116(2) . . ?
C2 C8 C7 120(2) . . ?
C2 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
N1 C9 C7 108(2) . . ?
N1 C9 H9A 110.2 . . ?
C7 C9 H9A 110.2 . . ?
N1 C9 H9B 110.2 . . ?
C7 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
N1 C10 C12 108(2) . . ?
N1 C10 C11 110(2) . . ?
C12 C10 C11 111(2) . . ?
N1 C10 H10 109.4 . . ?
C12 C10 H10 109.4 . . ?
C11 C10 H10 109.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O5 C12 O6 125(2) . . ?
O5 C12 C10 121(3) . . ?
O6 C12 C10 114(3) . . ?
O9 C13 O10 122(2) . . ?
O9 C13 C14 122(3) . . ?
O10 C13 C14 116(3) . . ?
O9 C13 Eu2 61.9(15) . 1_455 ?
O10 C13 Eu2 59.8(12) . 1_455 ?
C14 C13 Eu2 176(2) . 1_455 ?
C15 C14 C20 120(3) . . ?
C15 C14 C13 122(3) . . ?
C20 C14 C13 116(3) . . ?
C14 C15 C16 119(3) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C18 C16 C15 120(3) . . ?
C18 C16 C17 120(2) . . ?
C15 C16 C17 119(2) . . ?
O11 C17 O12 125(3) . . ?
O11 C17 C16 118(2) . . ?
O12 C17 C16 117(2) . . ?
O11 C17 Eu2 78.3(15) . 1_445 ?
O12 C17 Eu2 48.9(15) . 1_445 ?
C16 C17 Eu2 158(2) . 1_445 ?
C19 C18 C16 121(3) . . ?
C19 C18 H18 119.3 . . ?
C16 C18 H18 119.3 . . ?
C18 C19 C20 120(3) . . ?
C18 C19 C21 124(2) . . ?
C20 C19 C21 116(3) . . ?
C19 C20 C14 119(3) . . ?
C19 C20 H20 120.6 . . ?
C14 C20 H20 120.6 . . ?
N2 C21 C19 120(2) . . ?
N2 C21 H21A 107.4 . . ?
C19 C21 H21A 107.4 . . ?
N2 C21 H21B 107.4 . . ?
C19 C21 H21B 107.4 . . ?
H21A C21 H21B 106.9 . . ?
N2 C22 C24 105(3) . . ?
N2 C22 C23 105(2) . . ?
C24 C22 C23 111(3) . . ?
N2 C22 H22 111.7 . . ?
C24 C22 H22 111.7 . . ?
C23 C22 H22 111.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O14 C24 O13 129(3) . . ?
O14 C24 C22 119(3) . . ?
O13 C24 C22 112(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O2 C1 O1 8(3) . . . . ?
Eu1 O2 C1 C2 -170(2) . . . . ?
Eu1 O1 C1 O2 -8(3) . . . . ?
Eu1 O1 C1 C2 170(2) . . . . ?
O2 C1 C2 C8 176(3) . . . . ?
O1 C1 C2 C8 -3(4) . . . . ?
O2 C1 C2 C3 -8(4) . . . . ?
O1 C1 C2 C3 173(3) . . . . ?
C8 C2 C3 C4 -10(4) . . . . ?
C1 C2 C3 C4 174(3) . . . . ?
C2 C3 C4 C6 5(4) . . . . ?
C2 C3 C4 C5 -161(3) . . . . ?
Eu1 O4 C5 O3 6(4) 1_565 . . . ?
Eu1 O4 C5 C4 -169(3) 1_565 . . . ?
Eu2 O3 C5 O4 133(6) 1_565 . . . ?
Eu1 O3 C5 O4 -5(3) 1_565 . . . ?
Eu2 O3 C5 C4 -52(9) 1_565 . . . ?
Eu1 O3 C5 C4 170(3) 1_565 . . . ?
Eu2 O3 C5 Eu1 138(7) 1_565 . . 1_565 ?
C3 C4 C5 O4 157(4) . . . . ?
C6 C4 C5 O4 -9(5) . . . . ?
C3 C4 C5 O3 -17(5) . . . . ?
C6 C4 C5 O3 176(3) . . . . ?
C3 C4 C5 Eu1 112(11) . . . 1_565 ?
C6 C4 C5 Eu1 -54(13) . . . 1_565 ?
C3 C4 C6 C7 -1(5) . . . . ?
C5 C4 C6 C7 166(3) . . . . ?
C4 C6 C7 C8 0(5) . . . . ?
C4 C6 C7 C9 -169(3) . . . . ?
C3 C2 C8 C7 10(4) . . . . ?
C1 C2 C8 C7 -175(3) . . . . ?
C6 C7 C8 C2 -5(4) . . . . ?
C9 C7 C8 C2 164(3) . . . . ?
C10 N1 C9 C7 -161(2) . . . . ?
C8 C7 C9 N1 60(4) . . . . ?
C6 C7 C9 N1 -131(3) . . . . ?
C9 N1 C10 C12 67(3) . . . . ?
C9 N1 C10 C11 -54(3) . . . . ?
Eu1 O5 C12 O6 -43(5) 1_455 . . . ?
Eu1 O5 C12 C10 137(2) 1_455 . . . ?
Eu2 O6 C12 O5 -4(5) 1_455 . . . ?
Eu2 O6 C12 C10 176.1(19) 1_455 . . . ?
N1 C10 C12 O5 -143(3) . . . . ?
C11 C10 C12 O5 -22(4) . . . . ?
N1 C10 C12 O6 36(3) . . . . ?
C11 C10 C12 O6 157(3) . . . . ?
Eu2 O9 C13 O10 -2(3) 1_455 . . . ?
Eu2 O9 C13 C14 178(3) 1_455 . . . ?
Eu2 O10 C13 O9 2(3) 1_455 . . . ?
Eu2 O10 C13 C14 -178(2) 1_455 . . . ?
O9 C13 C14 C15 -174(3) . . . . ?
O10 C13 C14 C15 6(5) . . . . ?
O9 C13 C14 C20 24(5) . . . . ?
O10 C13 C14 C20 -156(3) . . . . ?
C20 C14 C15 C16 -7(5) . . . . ?
C13 C14 C15 C16 -168(3) . . . . ?
C14 C15 C16 C18 3(5) . . . . ?
C14 C15 C16 C17 177(3) . . . . ?
Eu2 O11 C17 O12 15(3) 1_445 . . . ?
Eu2 O11 C17 C16 -164(3) 1_445 . . . ?
Eu2 O12 C17 O11 -20(4) 1_445 . . . ?
Eu2 O12 C17 C16 159(2) 1_445 . . . ?
C18 C16 C17 O11 -166(3) . . . . ?
C15 C16 C17 O11 20(4) . . . . ?
C18 C16 C17 O12 15(4) . . . . ?
C15 C16 C17 O12 -159(3) . . . . ?
C18 C16 C17 Eu2 60(6) . . . 1_445 ?
C15 C16 C17 Eu2 -114(5) . . . 1_445 ?
C15 C16 C18 C19 1(5) . . . . ?
C17 C16 C18 C19 -173(3) . . . . ?
C16 C18 C19 C20 0(5) . . . . ?
C16 C18 C19 C21 179(3) . . . . ?
C18 C19 C20 C14 -4(5) . . . . ?
C21 C19 C20 C14 177(3) . . . . ?
C15 C14 C20 C19 8(5) . . . . ?
C13 C14 C20 C19 170(3) . . . . ?
C22 N2 C21 C19 162(3) . . . . ?
C18 C19 C21 N2 127(4) . . . . ?
C20 C19 C21 N2 -54(4) . . . . ?
C21 N2 C22 C24 -70(3) . . . . ?
C21 N2 C22 C23 173(2) . . . . ?
Eu1 O14 C24 O13 -3(7) . . . . ?
Eu1 O14 C24 C22 -177(2) . . . . ?
Eu2 O13 C24 O14 33(6) . . . . ?
Eu2 O13 C24 C22 -152(2) . . . . ?
N2 C22 C24 O14 -38(4) . . . . ?
C23 C22 C24 O14 75(4) . . . . ?
N2 C22 C24 O13 147(3) . . . . ?
C23 C22 C24 O13 -100(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1B Cl2 0.91 2.46 3.25(3) 146.4 . yes
N2 H2B Cl1 0.91 2.37 3.18(3) 148.1 . yes
O7 H7A O9 0.841(15) 2.14(10) 2.86(3) 143(13) . yes
N1 H1A Cl1 0.91 2.22 3.12(3) 173.7 1_566 yes
N2 H2A Cl2 0.91 2.20 3.09(3) 164.2 1_544 yes
O16 H16B Cl2 0.840(15) 2.47(7) 3.28(2) 160(18) 1_655 yes
O16 H16A O1 0.842(15) 1.91(4) 2.75(3) 172(20) 1_655 yes

_refine_diff_density_max         3.370
_refine_diff_density_min         -2.031
_refine_diff_density_rms         0.193


# start Validation Reply Form
_vrf_PLAT306_II                  
;
RESPONSE: The H atoms of lattice water molecules O17, O18, O19, 
O20 and O21 were not added owing to not suitable Fourier maps 
being picked up.
;
_vrf_PLAT342_II                  
;
RESPONSE: The precision of the C-C bonds of II is slightly low, 
which perhaps results from the weak diffraction owing to the 
bad quality and small sizes of single crystal and/or from the 
effect of heavy Eu atom whose strong diffraction signals affect 
the accurate detection of lighter atom C. 
;
_vrf_PLAT420_II                  
;
RESPONSE: No suitable hydrogen-bonds for H7B of water O7 and 
H15A and H15B of water O15 were found. 
;
_vrf_PLAT430_II                  
;
RESPONSE: The H atoms of lattice water molecules O18 and O21 
were not added owing to not suitable Fourier maps being 
picked up. Thus hydrogen-bonding interactions between them 
could not be determined.
;
_vrf_PLAT987_II                  
;
RESPONSE: A BASF/TWIN Refinement does not well, but the 
measurement of CD spectrum as well as homochiral ligand 
further confirm the homochiral framework of II.
;
####################################################################### 
# 
# 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_III
_database_code_depnum_ccdc_archive 'CCDC 1852705'
_audit_update_record             
;
2018-07-01 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            'C24 H40 Cl2 N2 O21 Tb2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H30 N2 O16 Tb2, 2(Cl), 5(H2 O)'
_chemical_formula_sum            'C24 H40 Cl2 N2 O21 Tb2'
_chemical_formula_weight         1081.32

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.6763(4)
_cell_length_b                   10.0338(4)
_cell_length_c                   10.9853(5)
_cell_angle_alpha                105.072(3)
_cell_angle_beta                 93.691(3)
_cell_angle_gamma                110.107(4)
_cell_volume                     953.10(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8074
_cell_measurement_theta_min      3.8660
_cell_measurement_theta_max      28.8060

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_F_000             530
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    3.901
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15548
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.378
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7729
_reflns_number_gt                6732
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    0.992

_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0244P)²+2.0974P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2870 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.25(2)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         7729
_refine_ls_number_parameters     474
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0865
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.002

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 0.69419(5) 0.71488(5) 0.93849(5) 0.0206(3) Uani 1 1 d . . . . .
Tb2 Tb 1.02913(5) 0.56891(5) 1.01391(5) 0.0205(3) Uani 1 1 d . . . . .
Cl1 Cl 0.3300(13) 0.3629(11) 0.5451(9) 0.065(3) Uani 1 1 d . . . . .
Cl2 Cl 0.3768(12) -0.0826(9) 0.4133(9) 0.051(2) Uani 1 1 d . . . . .
O1 O 0.5688(16) 0.5380(15) 1.0378(13) 0.024(4) Uani 1 1 d . U . . .
O2 O 0.7862(18) 0.5060(18) 1.0439(16) 0.025(4) Uani 1 1 d . U . . .
O3 O 0.715(3) -0.031(2) 0.982(2) 0.043(7) Uani 1 1 d . . . . .
O4 O 0.5424(19) -0.165(2) 1.0664(19) 0.027(5) Uani 1 1 d . . . . .
O5 O 0.055(2) -0.198(2) 1.170(2) 0.027(5) Uani 1 1 d . . . . .
O6 O -0.169(2) -0.171(2) 1.1504(18) 0.027(5) Uani 1 1 d . . . . .
O7 O 0.440(2) 0.605(2) 0.821(2) 0.036(6) Uani 1 1 d . . . . .
O8 O 0.689(3) 0.767(3) 0.738(2) 0.048(6) Uani 1 1 d D . . . .
O9 O 0.1429(16) -0.2671(16) 0.8935(13) 0.025(4) Uani 1 1 d . U . . .
O10 O -0.0567(19) -0.2159(19) 0.9235(16) 0.030(5) Uani 1 1 d . U . . .
O11 O 0.005(2) 0.312(2) 0.968(2) 0.035(6) Uani 1 1 d . . . . .
O12 O 0.178(2) 0.453(2) 0.8886(18) 0.028(5) Uani 1 1 d . . . . .
O13 O 0.676(2) 0.492(2) 0.783(2) 0.029(5) Uani 1 1 d . . . . .
O14 O 0.890(2) 0.461(2) 0.800(2) 0.036(5) Uani 1 1 d . . . . .
O15 O 1.020(3) 0.512(2) 1.220(2) 0.052(6) Uani 1 1 d . . . . .
O16 O 1.278(2) 0.674(2) 1.131(2) 0.027(5) Uani 1 1 d D . . . .
O17 O -0.366(2) -0.212(2) 1.3457(17) 0.088(6) Uani 1 1 d . U . . .
O18 O 0.4299(13) 0.7670(11) 0.6162(10) 0.050(3) Uani 1 1 d . . . . .
O19 O 0.831(4) 0.778(4) 0.533(4) 0.283(16) Uani 1 1 d . U . . .
O20 O 1.052(2) 0.689(2) 0.4700(17) 0.123(6) Uani 1 1 d . . . . .
O21 O 1.1276(19) 0.5653(19) 0.6268(16) 0.079(5) Uani 1 1 d . U . . .
N1 N 0.190(2) 0.079(2) 1.3014(19) 0.025(5) Uani 1 1 d D . . . .
H1A H 0.233561 0.010921 1.295493 0.030 Uiso 1 1 calc R U . . .
H1B H 0.237716 0.156116 1.373538 0.030 Uiso 1 1 calc R U . . .
N2 N 0.531(2) 0.197(2) 0.6398(18) 0.023(5) Uani 1 1 d D . . . .
H2A H 0.481639 0.260227 0.643409 0.027 Uiso 1 1 calc R U . . .
H2B H 0.490358 0.120962 0.566075 0.027 Uiso 1 1 calc R U . . .
C1 C 0.652(3) 0.467(3) 1.060(3) 0.021(6) Uani 1 1 d . U . . .
C2 C 0.580(2) 0.331(2) 1.094(2) 0.025(7) Uani 1 1 d D . . . .
C3 C 0.643(2) 0.223(2) 1.078(2) 0.017(5) Uani 1 1 d D U . . .
H3 H 0.741311 0.242970 1.057901 0.020 Uiso 1 1 calc R U . . .
C4 C 0.558(3) 0.085(2) 1.092(3) 0.027(7) Uani 1 1 d D . . . .
C5 C 0.609(3) -0.046(2) 1.051(2) 0.022(5) Uani 1 1 d D U . . .
C6 C 0.417(3) 0.052(2) 1.128(3) 0.028(7) Uani 1 1 d D . . . .
H6 H 0.356610 -0.045115 1.127565 0.033 Uiso 1 1 calc R U . . .
C7 C 0.372(3) 0.173(2) 1.166(3) 0.023(6) Uani 1 1 d D . . . .
C8 C 0.445(2) 0.305(3) 1.139(2) 0.024(7) Uani 1 1 d D U . . .
H8 H 0.401636 0.378185 1.151164 0.028 Uiso 1 1 calc R U . . .
C9 C 0.208(2) 0.135(2) 1.1877(18) 0.023(5) Uani 1 1 d D U . . .
H9A H 0.182779 0.224817 1.202265 0.028 Uiso 1 1 calc R U . . .
H9B H 0.140102 0.057957 1.111071 0.028 Uiso 1 1 calc R U . . .
C10 C 0.030(2) 0.009(2) 1.312(2) 0.018(6) Uani 1 1 d D . . . .
H10 H 0.025843 -0.019620 1.392560 0.021 Uiso 1 1 calc R U . . .
C11 C -0.0588(17) 0.1103(17) 1.3153(18) 0.053(5) Uani 1 1 d . . . . .
H11A H -0.010000 0.202817 1.385613 0.079 Uiso 1 1 calc R U . . .
H11B H -0.160476 0.059189 1.328205 0.079 Uiso 1 1 calc R U . . .
H11C H -0.062756 0.133407 1.234042 0.079 Uiso 1 1 calc R U . . .
C12 C -0.036(3) -0.134(3) 1.198(2) 0.021(6) Uani 1 1 d . . . . .
C13 C 0.070(4) -0.189(3) 0.891(3) 0.024(7) Uani 1 1 d . U . . .
C14 C 0.142(2) -0.046(3) 0.853(2) 0.022(6) Uani 1 1 d D . . . .
C15 C 0.091(3) 0.069(2) 0.886(3) 0.027(6) Uani 1 1 d D . . . .
H15 H 0.001746 0.054483 0.922138 0.032 Uiso 1 1 calc R U . . .
C16 C 0.166(2) 0.206(2) 0.868(2) 0.016(6) Uani 1 1 d D . . . .
C17 C 0.113(3) 0.327(2) 0.917(2) 0.022(5) Uani 1 1 d . U . . .
C18 C 0.297(2) 0.222(3) 0.822(2) 0.020(6) Uani 1 1 d D U . . .
H18 H 0.346807 0.311667 0.802562 0.024 Uiso 1 1 calc R U . . .
C19 C 0.364(3) 0.117(2) 0.800(3) 0.020(5) Uani 1 1 d D U . . .
C20 C 0.279(2) -0.022(2) 0.811(3) 0.026(7) Uani 1 1 d D . . . .
H20 H 0.313761 -0.101303 0.788285 0.031 Uiso 1 1 calc R U . . .
C21 C 0.507(3) 0.136(2) 0.7501(18) 0.025(6) Uani 1 1 d D U . . .
H21A H 0.516634 0.037943 0.725103 0.030 Uiso 1 1 calc R U . . .
H21B H 0.589750 0.202212 0.821684 0.030 Uiso 1 1 calc R U . . .
C22 C 0.691(2) 0.280(3) 0.634(3) 0.036(8) Uani 1 1 d D . . . .
H22 H 0.748930 0.214483 0.637989 0.043 Uiso 1 1 calc R U . . .
C23 C 0.6997(19) 0.3144(18) 0.5088(14) 0.053(5) Uani 1 1 d . . . . .
H23A H 0.661324 0.393364 0.510628 0.079 Uiso 1 1 calc R U . . .
H23B H 0.639336 0.224954 0.438795 0.079 Uiso 1 1 calc R U . . .
H23C H 0.803733 0.347683 0.495381 0.079 Uiso 1 1 calc R U . . .
C24 C 0.758(3) 0.422(3) 0.747(2) 0.025(7) Uani 1 1 d D . . . .
H16A H 1.288(13) 0.729(12) 1.205(5) 0.037 Uiso 1 1 d D U . . .
H16B H 1.358(8) 0.719(12) 1.108(10) 0.037 Uiso 1 1 d D U . . .
H8B H 0.693(16) 0.730(11) 0.661(5) 0.037 Uiso 1 1 d D U . . .
H8A H 0.732(16) 0.858(4) 0.749(11) 0.037 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O10 2.297(18) 1_665 ?
Tb1 O1 2.348(14) . ?
Tb1 O13 2.38(2) . ?
Tb1 O6 2.380(19) 1_665 ?
Tb1 O8 2.392(19) . ?
Tb1 O3 2.403(19) 1_565 ?
Tb1 O7 2.43(2) . ?
Tb1 O4 2.485(19) 1_565 ?
Tb1 C5 2.817(19) 1_565 ?
Tb1 C1 3.04(3) . ?
Tb2 O2 2.285(17) . ?
Tb2 O16 2.387(18) . ?
Tb2 O9 2.397(14) 1_665 ?
Tb2 O14 2.41(2) . ?
Tb2 O11 2.42(2) 1_655 ?
Tb2 O12 2.430(18) 1_655 ?
Tb2 O5 2.44(2) 1_665 ?
Tb2 O15 2.47(2) . ?
Tb2 C17 2.79(2) 1_655 ?
Tb2 C13 3.00(3) 1_665 ?
O1 C1 1.29(3) . ?
O2 C1 1.26(3) . ?
O3 C5 1.31(3) . ?
O4 C5 1.21(3) . ?
O5 C12 1.26(3) . ?
O6 C12 1.24(3) . ?
O8 H8B 0.839(15) . ?
O8 H8A 0.838(15) . ?
O9 C13 1.23(3) . ?
O10 C13 1.26(4) . ?
O11 C17 1.20(3) . ?
O12 C17 1.33(3) . ?
O13 C24 1.25(3) . ?
O14 C24 1.26(3) . ?
O16 H16A 0.839(15) . ?
O16 H16B 0.839(15) . ?
N1 C10 1.488(12) . ?
N1 C9 1.494(12) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 C21 1.492(12) . ?
N2 C22 1.499(12) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
C1 C2 1.47(3) . ?
C2 C8 1.391(12) . ?
C2 C3 1.395(12) . ?
C3 C4 1.403(12) . ?
C3 H3 0.9500 . ?
C4 C6 1.400(12) . ?
C4 C5 1.524(14) . ?
C6 C7 1.401(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(12) . ?
C7 C9 1.54(3) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.53(3) . ?
C10 C12 1.540(19) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 C14 1.54(3) . ?
C14 C15 1.386(12) . ?
C14 C20 1.397(12) . ?
C15 C16 1.389(12) . ?
C15 H15 0.9500 . ?
C16 C18 1.378(12) . ?
C16 C17 1.46(2) . ?
C18 C19 1.395(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.391(12) . ?
C19 C21 1.49(3) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.50(3) . ?
C22 C24 1.532(14) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
O10 Tb1 O1 124.2(6) 1_665 . ?
O10 Tb1 O13 83.0(7) 1_665 . ?
O1 Tb1 O13 79.5(6) . . ?
O10 Tb1 O6 72.7(6) 1_665 1_665 ?
O1 Tb1 O6 79.5(6) . 1_665 ?
O13 Tb1 O6 130.2(7) . 1_665 ?
O10 Tb1 O8 80.0(7) 1_665 . ?
O1 Tb1 O8 141.8(7) . . ?
O13 Tb1 O8 74.5(8) . . ?
O6 Tb1 O8 138.6(8) 1_665 . ?
O10 Tb1 O3 90.3(7) 1_665 1_565 ?
O1 Tb1 O3 129.0(6) . 1_565 ?
O13 Tb1 O3 147.3(8) . 1_565 ?
O6 Tb1 O3 76.8(8) 1_665 1_565 ?
O8 Tb1 O3 72.8(9) . 1_565 ?
O10 Tb1 O7 145.8(6) 1_665 . ?
O1 Tb1 O7 76.2(6) . . ?
O13 Tb1 O7 73.7(7) . . ?
O6 Tb1 O7 141.4(7) 1_665 . ?
O8 Tb1 O7 70.0(8) . . ?
O3 Tb1 O7 96.0(8) 1_565 . ?
O10 Tb1 O4 134.7(6) 1_665 1_565 ?
O1 Tb1 O4 77.0(6) . 1_565 ?
O13 Tb1 O4 142.3(7) . 1_565 ?
O6 Tb1 O4 73.4(6) 1_665 1_565 ?
O8 Tb1 O4 107.9(7) . 1_565 ?
O3 Tb1 O4 53.1(7) 1_565 1_565 ?
O7 Tb1 O4 72.3(7) . 1_565 ?
O10 Tb1 C5 114.0(6) 1_665 1_565 ?
O1 Tb1 C5 101.9(6) . 1_565 ?
O13 Tb1 C5 156.1(7) . 1_565 ?
O6 Tb1 C5 72.8(6) 1_665 1_565 ?
O8 Tb1 C5 91.4(8) . 1_565 ?
O3 Tb1 C5 27.7(7) 1_565 1_565 ?
O7 Tb1 C5 83.4(7) . 1_565 ?
O4 Tb1 C5 25.4(6) 1_565 1_565 ?
O10 Tb1 C1 101.1(7) 1_665 . ?
O1 Tb1 C1 23.6(7) . . ?
O13 Tb1 C1 69.4(7) . . ?
O6 Tb1 C1 73.5(7) 1_665 . ?
O8 Tb1 C1 143.4(8) . . ?
O3 Tb1 C1 143.1(8) 1_565 . ?
O7 Tb1 C1 93.9(7) . . ?
O4 Tb1 C1 97.1(7) 1_565 . ?
C5 Tb1 C1 119.9(7) 1_565 . ?
O2 Tb2 O16 141.4(6) . . ?
O2 Tb2 O9 124.2(6) . 1_665 ?
O16 Tb2 O9 81.4(6) . 1_665 ?
O2 Tb2 O14 76.6(6) . . ?
O16 Tb2 O14 142.0(7) . . ?
O9 Tb2 O14 72.8(6) 1_665 . ?
O2 Tb2 O11 90.6(6) . 1_655 ?
O16 Tb2 O11 96.1(7) . 1_655 ?
O9 Tb2 O11 125.7(6) 1_665 1_655 ?
O14 Tb2 O11 78.0(8) . 1_655 ?
O2 Tb2 O12 137.6(6) . 1_655 ?
O16 Tb2 O12 72.1(7) . 1_655 ?
O9 Tb2 O12 74.8(5) 1_665 1_655 ?
O14 Tb2 O12 74.5(7) . 1_655 ?
O11 Tb2 O12 53.5(6) 1_655 1_655 ?
O2 Tb2 O5 81.9(7) . 1_665 ?
O16 Tb2 O5 73.0(7) . 1_665 ?
O9 Tb2 O5 82.2(6) 1_665 1_665 ?
O14 Tb2 O5 128.4(7) . 1_665 ?
O11 Tb2 O5 149.0(7) 1_655 1_665 ?
O12 Tb2 O5 140.5(7) 1_655 1_665 ?
O2 Tb2 O15 73.5(7) . . ?
O16 Tb2 O15 72.1(8) . . ?
O9 Tb2 O15 149.3(7) 1_665 . ?
O14 Tb2 O15 137.9(8) . . ?
O11 Tb2 O15 73.5(8) 1_655 . ?
O12 Tb2 O15 110.2(7) 1_655 . ?
O5 Tb2 O15 75.5(7) 1_665 . ?
O2 Tb2 C17 114.6(6) . 1_655 ?
O16 Tb2 C17 82.0(7) . 1_655 ?
O9 Tb2 C17 102.6(6) 1_665 1_655 ?
O14 Tb2 C17 77.2(7) . 1_655 ?
O11 Tb2 C17 25.3(6) 1_655 1_655 ?
O12 Tb2 C17 28.5(6) 1_655 1_655 ?
O5 Tb2 C17 153.5(7) 1_665 1_655 ?
O15 Tb2 C17 89.1(7) . 1_655 ?
O2 Tb2 C13 102.6(7) . 1_665 ?
O16 Tb2 C13 95.1(8) . 1_665 ?
O9 Tb2 C13 23.0(7) 1_665 1_665 ?
O14 Tb2 C13 71.1(7) . 1_665 ?
O11 Tb2 C13 142.1(7) 1_655 1_665 ?
O12 Tb2 C13 96.5(7) 1_655 1_665 ?
O5 Tb2 C13 68.8(7) 1_665 1_665 ?
O15 Tb2 C13 144.2(7) . 1_665 ?
C17 Tb2 C13 123.0(7) 1_655 1_665 ?
C1 O1 Tb1 109.7(16) . . ?
C1 O2 Tb2 178.3(18) . . ?
C5 O3 Tb1 94.0(13) . 1_545 ?
C5 O4 Tb1 92.8(14) . 1_545 ?
C12 O5 Tb2 132.4(17) . 1_445 ?
C12 O6 Tb1 133.9(17) . 1_445 ?
Tb1 O8 H8B 142(9) . . ?
Tb1 O8 H8A 111(8) . . ?
H8B O8 H8A 102(2) . . ?
C13 O9 Tb2 107.4(17) . 1_445 ?
C13 O10 Tb1 168.0(19) . 1_445 ?
C17 O11 Tb2 95.0(15) . 1_455 ?
C17 O12 Tb2 90.9(13) . 1_455 ?
C24 O13 Tb1 138.2(19) . . ?
C24 O14 Tb2 136.8(18) . . ?
Tb2 O16 H16A 115(9) . . ?
Tb2 O16 H16B 129(9) . . ?
H16A O16 H16B 101(2) . . ?
C10 N1 C9 112.2(19) . . ?
C10 N1 H1A 109.2 . . ?
C9 N1 H1A 109.2 . . ?
C10 N1 H1B 109.2 . . ?
C9 N1 H1B 109.2 . . ?
H1A N1 H1B 107.9 . . ?
C21 N2 C22 115(2) . . ?
C21 N2 H2A 108.5 . . ?
C22 N2 H2A 108.5 . . ?
C21 N2 H2B 108.5 . . ?
C22 N2 H2B 108.5 . . ?
H2A N2 H2B 107.5 . . ?
O2 C1 O1 122(3) . . ?
O2 C1 C2 121(2) . . ?
O1 C1 C2 117(2) . . ?
O2 C1 Tb1 75.9(16) . . ?
O1 C1 Tb1 46.7(12) . . ?
C2 C1 Tb1 160.3(19) . . ?
C8 C2 C3 119(2) . . ?
C8 C2 C1 120.3(19) . . ?
C3 C2 C1 120(2) . . ?
C2 C3 C4 118(2) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 121.2 . . ?
C6 C4 C3 123.7(19) . . ?
C6 C4 C5 115.9(18) . . ?
C3 C4 C5 120.1(18) . . ?
O4 C5 O3 120.1(19) . . ?
O4 C5 C4 122(2) . . ?
O3 C5 C4 116.6(19) . . ?
O4 C5 Tb1 61.8(12) . 1_545 ?
O3 C5 Tb1 58.3(11) . 1_545 ?
C4 C5 Tb1 171.1(16) . 1_545 ?
C4 C6 C7 115.7(19) . . ?
C4 C6 H6 122.2 . . ?
C7 C6 H6 122.2 . . ?
C8 C7 C6 121(2) . . ?
C8 C7 C9 118.8(18) . . ?
C6 C7 C9 116.1(18) . . ?
C7 C8 C2 121(2) . . ?
C7 C8 H8 119.5 . . ?
C2 C8 H8 119.5 . . ?
N1 C9 C7 108.8(17) . . ?
N1 C9 H9A 109.9 . . ?
C7 C9 H9A 109.9 . . ?
N1 C9 H9B 109.9 . . ?
C7 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N1 C10 C11 114.4(18) . . ?
N1 C10 C12 105.8(19) . . ?
C11 C10 C12 111.7(19) . . ?
N1 C10 H10 108.2 . . ?
C11 C10 H10 108.2 . . ?
C12 C10 H10 108.2 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O6 C12 O5 130(2) . . ?
O6 C12 C10 116(2) . . ?
O5 C12 C10 113(2) . . ?
O9 C13 O10 123(3) . . ?
O9 C13 C14 118(3) . . ?
O10 C13 C14 119(2) . . ?
O9 C13 Tb2 49.6(13) . 1_445 ?
O10 C13 Tb2 74.6(16) . 1_445 ?
C14 C13 Tb2 161.3(18) . 1_445 ?
C15 C14 C20 120(2) . . ?
C15 C14 C13 120.9(19) . . ?
C20 C14 C13 118.0(19) . . ?
C14 C15 C16 122(2) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C18 C16 C15 116(2) . . ?
C18 C16 C17 125.2(18) . . ?
C15 C16 C17 118.5(17) . . ?
O11 C17 O12 120(2) . . ?
O11 C17 C16 123(2) . . ?
O12 C17 C16 117.1(19) . . ?
O11 C17 Tb2 59.7(13) . 1_455 ?
O12 C17 Tb2 60.6(11) . 1_455 ?
C16 C17 Tb2 176.7(16) . 1_455 ?
C16 C18 C19 126(2) . . ?
C16 C18 H18 117.2 . . ?
C19 C18 H18 117.2 . . ?
C20 C19 C18 116(2) . . ?
C20 C19 C21 119.0(18) . . ?
C18 C19 C21 124.5(18) . . ?
C19 C20 C14 121(2) . . ?
C19 C20 H20 119.6 . . ?
C14 C20 H20 119.6 . . ?
C19 C21 N2 118.8(19) . . ?
C19 C21 H21A 107.6 . . ?
N2 C21 H21A 107.6 . . ?
C19 C21 H21B 107.6 . . ?
N2 C21 H21B 107.6 . . ?
H21A C21 H21B 107.1 . . ?
N2 C22 C23 109(2) . . ?
N2 C22 C24 109.8(19) . . ?
C23 C22 C24 111(2) . . ?
N2 C22 H22 108.9 . . ?
C23 C22 H22 108.9 . . ?
C24 C22 H22 108.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O13 C24 O14 124(2) . . ?
O13 C24 C22 118(3) . . ?
O14 C24 C22 118(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C1 O2 8(3) . . . . ?
Tb1 O1 C1 C2 -166.3(17) . . . . ?
O2 C1 C2 C8 166(3) . . . . ?
O1 C1 C2 C8 -19(4) . . . . ?
Tb1 C1 C2 C8 -50(6) . . . . ?
O2 C1 C2 C3 -16(4) . . . . ?
O1 C1 C2 C3 158(2) . . . . ?
Tb1 C1 C2 C3 128(5) . . . . ?
C8 C2 C3 C4 8(4) . . . . ?
C1 C2 C3 C4 -170(2) . . . . ?
C2 C3 C4 C6 -4(4) . . . . ?
C2 C3 C4 C5 169(2) . . . . ?
Tb1 O4 C5 O3 2(2) 1_545 . . . ?
Tb1 O4 C5 C4 171(2) 1_545 . . . ?
Tb1 O3 C5 O4 -2(3) 1_545 . . . ?
Tb1 O3 C5 C4 -171.6(18) 1_545 . . . ?
C6 C4 C5 O4 -10(4) . . . . ?
C3 C4 C5 O4 177(3) . . . . ?
C6 C4 C5 O3 160(3) . . . . ?
C3 C4 C5 O3 -13(4) . . . . ?
C3 C4 C6 C7 -7(4) . . . . ?
C5 C4 C6 C7 179(2) . . . . ?
C4 C6 C7 C8 15(4) . . . . ?
C4 C6 C7 C9 171(3) . . . . ?
C6 C7 C8 C2 -12(4) . . . . ?
C9 C7 C8 C2 -167(2) . . . . ?
C3 C2 C8 C7 -1(4) . . . . ?
C1 C2 C8 C7 177(2) . . . . ?
C10 N1 C9 C7 -167.6(18) . . . . ?
C8 C7 C9 N1 -136(2) . . . . ?
C6 C7 C9 N1 67(3) . . . . ?
C9 N1 C10 C11 -56(3) . . . . ?
C9 N1 C10 C12 68(3) . . . . ?
Tb1 O6 C12 O5 -38(5) 1_445 . . . ?
Tb1 O6 C12 C10 144.8(19) 1_445 . . . ?
Tb2 O5 C12 O6 -1(5) 1_445 . . . ?
Tb2 O5 C12 C10 176.1(17) 1_445 . . . ?
N1 C10 C12 O6 -146(2) . . . . ?
C11 C10 C12 O6 -21(3) . . . . ?
N1 C10 C12 O5 36(3) . . . . ?
C11 C10 C12 O5 161(2) . . . . ?
Tb2 O9 C13 O10 -13(3) 1_445 . . . ?
Tb2 O9 C13 C14 163.1(18) 1_445 . . . ?
Tb1 O10 C13 O9 -100(9) 1_445 . . . ?
Tb1 O10 C13 C14 84(9) 1_445 . . . ?
Tb1 O10 C13 Tb2 -110(9) 1_445 . . 1_445 ?
O9 C13 C14 C15 -159(2) . . . . ?
O10 C13 C14 C15 17(4) . . . . ?
Tb2 C13 C14 C15 -115(5) 1_445 . . . ?
O9 C13 C14 C20 7(4) . . . . ?
O10 C13 C14 C20 -177(3) . . . . ?
Tb2 C13 C14 C20 51(6) 1_445 . . . ?
C20 C14 C15 C16 5(4) . . . . ?
C13 C14 C15 C16 171(2) . . . . ?
C14 C15 C16 C18 -3(4) . . . . ?
C14 C15 C16 C17 -174(2) . . . . ?
Tb2 O11 C17 O12 -10(2) 1_455 . . . ?
Tb2 O11 C17 C16 178(2) 1_455 . . . ?
Tb2 O12 C17 O11 10(2) 1_455 . . . ?
Tb2 O12 C17 C16 -177.2(18) 1_455 . . . ?
C18 C16 C17 O11 -172(3) . . . . ?
C15 C16 C17 O11 -2(4) . . . . ?
C18 C16 C17 O12 15(4) . . . . ?
C15 C16 C17 O12 -174(2) . . . . ?
C15 C16 C18 C19 -5(4) . . . . ?
C17 C16 C18 C19 166(2) . . . . ?
C16 C18 C19 C20 9(4) . . . . ?
C16 C18 C19 C21 -180(3) . . . . ?
C18 C19 C20 C14 -7(4) . . . . ?
C21 C19 C20 C14 -178(3) . . . . ?
C15 C14 C20 C19 0(4) . . . . ?
C13 C14 C20 C19 -167(2) . . . . ?
C20 C19 C21 N2 126(3) . . . . ?
C18 C19 C21 N2 -45(4) . . . . ?
C22 N2 C21 C19 152(2) . . . . ?
C21 N2 C22 C23 171.7(19) . . . . ?
C21 N2 C22 C24 -66(3) . . . . ?
Tb1 O13 C24 O14 3(5) . . . . ?
Tb1 O13 C24 C22 -177(2) . . . . ?
Tb2 O14 C24 O13 38(4) . . . . ?
Tb2 O14 C24 C22 -142(2) . . . . ?
N2 C22 C24 O13 -37(4) . . . . ?
C23 C22 C24 O13 83(3) . . . . ?
N2 C22 C24 O14 142(3) . . . . ?
C23 C22 C24 O14 -97(3) . . . . ?

_refine_diff_density_max         0.994
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.142


# start Validation Reply Form
_vrf_PLAT043_III                 
;
RESPONSE: The H atoms of lattice water molecules O17, O18, O19, 
O20 and O21 as well as the H atoms of coordinated water molecules 
O7 and O15 were not added owing to not suitable Fourier maps 
being picked up, which results in the difference between the 
calculated and reported molecule weight.
;
_vrf_PLAT306_III                 
;
RESPONSE: The H atoms of lattice water molecules O17, O18, O19, 
O20 and O21 were not added owing to not suitable Fourier maps 
being picked up.
;
_vrf_PLAT342_III                 
;
RESPONSE: The precision of the C-C bonds of III is slightly low, 
which perhaps results from the weak diffraction owing to the 
bad quality and small sizes of single crystal and/or from the 
effect of heavy Tb atom whose strong diffraction signals affect 
the accurate detection of lighter atom C. 
;
_vrf_PLAT430_III                 
;
RESPONSE: The H atoms of water molecules O15, O17, O19, O20 
and O21 were not added owing to not suitable Fourier maps 
being picked up. Thus hydrogen-bonding interactions between them 
could not be determined.
;
_vrf_PLAT987_III                 
;
RESPONSE: A BASF/TWIN Refinement does not well, but the 
measurement of CD spectrum as well as homochiral ligand 
further confirm the homochiral framework of III.
;
####################################################################### 
# 
# 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_IV
_database_code_depnum_ccdc_archive 'CCDC 1852706'
_audit_update_record             
;
2018-07-01 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            'C24 H40 Cl2 Dy2 N2 O21'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H30 Dy2 N2 O16, 2(Cl), 5(H2 O)'
_chemical_formula_sum            'C24 H40 Cl2 Dy2 N2 O21'
_chemical_formula_weight         1088.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.6947(4)
_cell_length_b                   10.0533(5)
_cell_length_c                   11.0032(7)
_cell_angle_alpha                105.039(5)
_cell_angle_beta                 93.823(4)
_cell_angle_gamma                110.052(4)
_cell_volume                     958.48(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7731
_cell_measurement_theta_min      3.8620
_cell_measurement_theta_max      27.9020

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_F_000             532
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    4.088
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15523
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.370
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7775
_reflns_number_gt                6702
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_max     0.990
_reflns_Friedel_fraction_full    0.992

_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0206P)²+2.6248P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2752 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.22(2)
_chemical_absolute_configuration r
_refine_ls_number_reflns         7775
_refine_ls_number_parameters     486
_refine_ls_number_restraints     155
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.014
_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
Dy1 Dy 0.1684(2) 0.4273(2) 0.03850(18) 0.0209(3) Uani 1 1 d . . . . .
Dy2 Dy -0.1679(2) 0.5733(2) -0.03820(18) 0.0206(3) Uani 1 1 d . . . . .
Cl1 Cl 0.5168(14) -0.2248(12) -0.5633(11) 0.056(3) Uani 1 1 d . . . . .
Cl2 Cl 0.4704(14) 0.2220(13) -0.4317(11) 0.062(3) Uani 1 1 d . . . . .
O1 O 0.319(2) 0.313(2) -0.087(2) 0.028(5) Uani 1 1 d . . . . .
O2 O 0.1312(14) 0.1659(14) -0.0210(12) 0.025(3) Uani 1 1 d . U . . .
O3 O 0.0719(18) -0.3623(18) -0.0709(15) 0.022(4) Uani 1 1 d . U . . .
O4 O 0.286(2) -0.402(2) -0.075(2) 0.033(6) Uani 1 1 d . . . . .
O5 O 1.030(2) 0.312(2) -0.176(2) 0.031(5) Uani 1 1 d . . . . .
O6 O 0.814(2) 0.349(2) -0.1979(19) 0.033(5) Uani 1 1 d . U . . .
O7 O 0.415(2) 0.534(2) 0.1565(17) 0.026(5) Uani 1 1 d D U . . .
O8 O 0.162(2) 0.369(2) 0.2419(18) 0.049(7) Uani 1 1 d D . . . .
O9 O -0.284(2) 0.402(2) 0.0674(19) 0.024(5) Uani 1 1 d . U . . .
O10 O -0.080(2) 0.360(2) 0.0533(16) 0.031(5) Uani 1 1 d . U . . .
O11 O -0.1599(14) -0.1800(14) -0.0104(12) 0.026(3) Uani 1 1 d . U . . .
O12 O -0.318(2) -0.307(2) 0.0908(19) 0.025(5) Uani 1 1 d . U . . .
O13 O -0.810(2) -0.342(2) 0.1879(16) 0.018(4) Uani 1 1 d . U . . .
O14 O -1.031(2) -0.319(2) 0.171(2) 0.028(5) Uani 1 1 d . . . . .
O15 O -0.4209(19) 0.468(2) -0.1496(18) 0.038(6) Uani 1 1 d D . . . .
O16 O -0.173(2) 0.623(2) -0.2367(18) 0.048(7) Uani 1 1 d D . . . .
O17 O 0.980(5) 0.670(5) 0.562(4) 0.32(2) Uani 1 1 d . U . . .
O18 O 0.258(3) 0.404(4) 0.648(3) 0.088(8) Uani 1 1 d . . . . .
O19 O 0.4341(13) 0.3755(13) 0.3616(11) 0.048(3) Uani 1 1 d . . . . .
O20 O 0.191(2) 0.546(2) 0.4939(16) 0.113(6) Uani 1 1 d . . . . .
O21 O 0.765(4) 0.629(5) 0.370(4) 0.152(16) Uani 1 1 d . . . . .
N1 N 0.672(3) 0.063(3) -0.333(3) 0.025(6) Uani 1 1 d . . . . .
H1A H 0.626480 -0.012646 -0.406818 0.030 Uiso 1 1 calc R U . . .
H1B H 0.624226 0.127553 -0.325913 0.030 Uiso 1 1 calc R U . . .
N2 N -0.670(3) -0.055(3) 0.328(2) 0.020(5) Uani 1 1 d . U . . .
H2A H -0.626243 0.021850 0.400269 0.024 Uiso 1 1 calc R U . . .
H2B H -0.625178 -0.121946 0.325107 0.024 Uiso 1 1 calc R U . . .
C1 C 0.246(3) 0.187(3) -0.069(3) 0.030(8) Uani 1 1 d D . . . .
C2 C 0.306(3) 0.061(3) -0.114(3) 0.022(7) Uani 1 1 d D . . . .
C3 C 0.225(3) -0.074(3) -0.092(3) 0.027(7) Uani 1 1 d . U . . .
H3 H 0.134013 -0.088058 -0.060057 0.033 Uiso 1 1 calc R U . . .
C4 C 0.282(3) -0.190(3) -0.118(3) 0.020(6) Uani 1 1 d . . . . .
C5 C 0.208(3) -0.331(3) -0.078(3) 0.026(6) Uani 1 1 d . U . . .
C6 C 0.416(3) -0.160(3) -0.164(3) 0.025(7) Uani 1 1 d . . . . .
H6 H 0.453409 -0.237213 -0.184713 0.031 Uiso 1 1 calc R U . . .
C7 C 0.496(3) -0.031(3) -0.182(3) 0.017(6) Uani 1 1 d . U . . .
H7A H 0.449(14) 0.601(8) 0.230(4) 0.025 Uiso 1 1 d D U . . .
H8A H 0.129(4) 0.418(5) 0.302(4) 0.025 Uiso 1 1 d D U . . .
H15A H -0.413(5) 0.423(9) -0.225(3) 0.025 Uiso 1 1 d D U . . .
H16B H -0.129(9) 0.681(4) -0.280(4) 0.025 Uiso 1 1 d D U . . .
H16A H -0.220(9) 0.545(4) -0.299(4) 0.025 Uiso 1 1 d D U . . .
H8B H 0.236(4) 0.367(5) 0.288(5) 0.025 Uiso 1 1 d D U . . .
H7B H 0.474(8) 0.585(8) 0.115(5) 0.025 Uiso 1 1 d D U . . .
H15B H -0.515(3) 0.421(10) -0.154(5) 0.025 Uiso 1 1 d D U . . .
C8 C 0.434(3) 0.084(3) -0.160(3) 0.028(7) Uani 1 1 d . U . . .
H8 H 0.484386 0.174156 -0.177376 0.033 Uiso 1 1 calc R U . . .
C9 C 0.651(3) -0.001(4) -0.222(3) 0.031(8) Uani 1 1 d . . . . .
H9A H 0.728126 0.069509 -0.148144 0.038 Uiso 1 1 calc R U . . .
H9B H 0.668745 -0.094653 -0.245357 0.038 Uiso 1 1 calc R U . . .
C10 C 0.829(3) 0.141(3) -0.345(3) 0.025(6) Uani 1 1 d . . . . .
H10 H 0.883381 0.073077 -0.342724 0.030 Uiso 1 1 calc R U . . .
C11 C 0.895(3) 0.278(3) -0.224(3) 0.026(7) Uani 1 1 d . U . . .
C12 C 0.8382(19) 0.174(2) -0.4683(16) 0.053(5) Uani 1 1 d . . . . .
H12A H 0.813872 0.262395 -0.463051 0.079 Uiso 1 1 calc R U . . .
H12B H 0.767533 0.089663 -0.536814 0.079 Uiso 1 1 calc R U . . .
H12C H 0.939595 0.193459 -0.486559 0.079 Uiso 1 1 calc R U . . .
C13 C -0.207(3) 0.326(3) 0.090(2) 0.014(5) Uani 1 1 d . U . . .
C14 C -0.278(3) 0.187(2) 0.125(3) 0.025(7) Uani 1 1 d D . . . .
C15 C -0.220(2) 0.081(2) 0.102(2) 0.015(5) Uani 1 1 d D U . . .
H15 H -0.122509 0.102094 0.080615 0.018 Uiso 1 1 calc R U . . .
C16 C -0.301(3) -0.061(3) 0.109(3) 0.020(6) Uani 1 1 d . U . . .
C17 C -0.256(3) -0.189(3) 0.065(3) 0.020(6) Uani 1 1 d . U . . .
C18 C -0.445(3) -0.085(3) 0.150(2) 0.014(5) Uani 1 1 d . U . . .
H18 H -0.504181 -0.181481 0.151167 0.017 Uiso 1 1 calc R U . . .
C19 C -0.498(3) 0.025(3) 0.186(3) 0.022(7) Uani 1 1 d . . . . .
C20 C -0.418(3) 0.168(3) 0.165(3) 0.020(6) Uani 1 1 d . U . . .
H20 H -0.457311 0.243791 0.177832 0.024 Uiso 1 1 calc R U . . .
C21 C -0.647(3) 0.000(3) 0.215(3) 0.023(6) Uani 1 1 d . U . . .
H21A H -0.720744 -0.073291 0.139825 0.027 Uiso 1 1 calc R U . . .
H21B H -0.664333 0.094044 0.231500 0.027 Uiso 1 1 calc R U . . .
C22 C -0.835(3) -0.129(3) 0.332(2) 0.027(7) Uani 1 1 d D . . . .
H22 H -0.837316 -0.155770 0.414091 0.032 Uiso 1 1 calc R U . . .
C23 C -0.900(3) -0.280(2) 0.225(3) 0.025(7) Uani 1 1 d D . . . .
C24 C -0.9189(19) -0.0283(19) 0.342(2) 0.056(6) Uani 1 1 d . . . . .
H24A H -0.867337 0.062401 0.413088 0.084 Uiso 1 1 calc R U . . .
H24B H -1.019706 -0.078468 0.356341 0.084 Uiso 1 1 calc R U . . .
H24C H -0.924773 -0.002566 0.262094 0.084 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O10 2.298(18) . ?
Dy1 O7 2.381(18) . ?
Dy1 O4 2.40(2) 1_565 ?
Dy1 O13 2.399(18) 1_665 ?
Dy1 O5 2.41(2) 1_455 ?
Dy1 O2 2.428(12) . ?
Dy1 O1 2.44(2) . ?
Dy1 O8 2.455(19) . ?
Dy1 C5 2.96(3) 1_565 ?
Dy2 O3 2.270(17) 1_565 ?
Dy2 O9 2.34(2) . ?
Dy2 O14 2.36(2) 1_665 ?
Dy2 O16 2.37(2) . ?
Dy2 O11 2.392(12) 1_565 ?
Dy2 O15 2.406(18) . ?
Dy2 O6 2.41(2) 1_455 ?
Dy2 O12 2.48(2) 1_565 ?
Dy2 C17 2.80(2) 1_565 ?
O1 C1 1.30(3) . ?
O2 C1 1.24(3) . ?
O3 C5 1.26(3) . ?
O4 C5 1.21(3) . ?
O5 C11 1.27(4) . ?
O6 C11 1.24(4) . ?
O7 H7A 0.8600(16) . ?
O7 H7B 0.8600(15) . ?
O8 H8A 0.8600(15) . ?
O8 H8B 0.8600(15) . ?
O9 C13 1.29(3) . ?
O10 C13 1.28(3) . ?
O11 C17 1.29(3) . ?
O12 C17 1.25(3) . ?
O13 C23 1.27(3) . ?
O14 C23 1.25(4) . ?
O15 H15A 0.8600(16) . ?
O15 H15B 0.8600(15) . ?
O16 H16B 0.8600(15) . ?
O16 H16A 0.8600(15) . ?
N1 C10 1.48(4) . ?
N1 C9 1.51(4) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 C21 1.49(4) . ?
N2 C22 1.52(4) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
C1 C2 1.5500(15) . ?
C2 C8 1.34(4) . ?
C2 C3 1.41(4) . ?
C3 C4 1.426(19) . ?
C3 H3 0.9500 . ?
C4 C6 1.39(4) . ?
C4 C5 1.55(4) . ?
C6 C7 1.33(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.45(4) . ?
C7 C9 1.55(4) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C12 1.48(3) . ?
C10 C11 1.56(2) . ?
C10 H10 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.49(3) . ?
C14 C15 1.3501(15) . ?
C14 C20 1.42(4) . ?
C15 C16 1.40(3) . ?
C15 H15 0.9500 . ?
C16 C18 1.45(3) . ?
C16 C17 1.469(19) . ?
C18 C19 1.35(4) . ?
C18 H18 0.9500 . ?
C19 C21 1.45(4) . ?
C19 C20 1.46(4) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C24 1.50(3) . ?
C22 C23 1.5500(15) . ?
C22 H22 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
O10 Dy1 O7 144.9(6) . . ?
O10 Dy1 O4 122.1(7) . 1_565 ?
O7 Dy1 O4 79.9(7) . 1_565 ?
O10 Dy1 O13 83.6(6) . 1_665 ?
O7 Dy1 O13 73.4(6) . 1_665 ?
O4 Dy1 O13 79.5(7) 1_565 1_665 ?
O10 Dy1 O5 72.8(7) . 1_455 ?
O7 Dy1 O5 142.3(7) . 1_455 ?
O4 Dy1 O5 75.8(8) 1_565 1_455 ?
O13 Dy1 O5 128.5(7) 1_665 1_455 ?
O10 Dy1 O2 88.1(5) . . ?
O7 Dy1 O2 100.5(5) . . ?
O4 Dy1 O2 125.8(6) 1_565 . ?
O13 Dy1 O2 153.2(5) 1_665 . ?
O5 Dy1 O2 72.2(6) 1_455 . ?
O10 Dy1 O1 135.6(7) . . ?
O7 Dy1 O1 72.6(7) . . ?
O4 Dy1 O1 75.5(7) 1_565 . ?
O13 Dy1 O1 140.6(6) 1_665 . ?
O5 Dy1 O1 73.5(7) 1_455 . ?
O2 Dy1 O1 54.2(5) . . ?
O10 Dy1 O8 77.9(7) . . ?
O7 Dy1 O8 71.5(7) . . ?
O4 Dy1 O8 147.3(7) 1_565 . ?
O13 Dy1 O8 77.4(6) 1_665 . ?
O5 Dy1 O8 136.8(7) 1_455 . ?
O2 Dy1 O8 76.0(6) . . ?
O1 Dy1 O8 109.6(7) . . ?
O10 Dy1 C5 100.4(7) . 1_565 ?
O7 Dy1 C5 94.5(7) . 1_565 ?
O4 Dy1 C5 23.1(8) 1_565 1_565 ?
O13 Dy1 C5 66.6(7) 1_665 1_565 ?
O5 Dy1 C5 73.4(8) 1_455 1_565 ?
O2 Dy1 C5 140.1(6) . 1_565 ?
O1 Dy1 C5 96.9(7) . 1_565 ?
O8 Dy1 C5 143.8(7) . 1_565 ?
O3 Dy2 O9 125.7(7) 1_565 . ?
O3 Dy2 O14 77.2(7) 1_565 1_665 ?
O9 Dy2 O14 76.5(7) . 1_665 ?
O3 Dy2 O16 75.3(7) 1_565 . ?
O9 Dy2 O16 143.9(7) . . ?
O14 Dy2 O16 139.6(7) 1_665 . ?
O3 Dy2 O11 92.0(5) 1_565 1_565 ?
O9 Dy2 O11 129.9(6) . 1_565 ?
O14 Dy2 O11 82.5(6) 1_665 1_565 ?
O16 Dy2 O11 69.5(6) . 1_565 ?
O3 Dy2 O15 142.3(6) 1_565 . ?
O9 Dy2 O15 77.9(7) . . ?
O14 Dy2 O15 140.4(7) 1_665 . ?
O16 Dy2 O15 70.8(7) . . ?
O11 Dy2 O15 91.4(6) 1_565 . ?
O3 Dy2 O6 80.1(7) 1_565 1_455 ?
O9 Dy2 O6 81.5(7) . 1_455 ?
O14 Dy2 O6 129.5(7) 1_665 1_455 ?
O16 Dy2 O6 73.5(7) . 1_455 ?
O11 Dy2 O6 142.9(5) 1_565 1_455 ?
O15 Dy2 O6 74.9(7) . 1_455 ?
O3 Dy2 O12 137.2(6) 1_565 1_565 ?
O9 Dy2 O12 76.8(7) . 1_565 ?
O14 Dy2 O12 73.9(7) 1_665 1_565 ?
O16 Dy2 O12 108.6(7) . 1_565 ?
O11 Dy2 O12 53.7(6) 1_565 1_565 ?
O15 Dy2 O12 71.2(7) . 1_565 ?
O6 Dy2 O12 142.7(7) 1_455 1_565 ?
O3 Dy2 C17 115.4(7) 1_565 1_565 ?
O9 Dy2 C17 102.9(8) . 1_565 ?
O14 Dy2 C17 76.0(8) 1_665 1_565 ?
O16 Dy2 C17 89.7(8) . 1_565 ?
O11 Dy2 C17 27.2(6) 1_565 1_565 ?
O15 Dy2 C17 80.9(7) . 1_565 ?
O6 Dy2 C17 153.9(7) 1_455 1_565 ?
O12 Dy2 C17 26.5(7) 1_565 1_565 ?
C1 O1 Dy1 90.4(14) . . ?
C1 O2 Dy1 92.6(12) . . ?
C5 O3 Dy2 173.6(17) . 1_545 ?
C5 O4 Dy1 105.4(19) . 1_545 ?
C11 O5 Dy1 133(2) . 1_655 ?
C11 O6 Dy2 135.6(18) . 1_655 ?
Dy1 O7 H7A 128(9) . . ?
Dy1 O7 H7B 109(5) . . ?
H7A O7 H7B 96(8) . . ?
Dy1 O8 H8A 119(5) . . ?
Dy1 O8 H8B 126(4) . . ?
H8A O8 H8B 98.2(2) . . ?
C13 O9 Dy2 113.3(17) . . ?
C13 O10 Dy1 166.0(16) . . ?
C17 O11 Dy2 94.6(12) . 1_545 ?
C17 O12 Dy2 91.4(15) . 1_545 ?
C23 O13 Dy1 135.4(15) . 1_445 ?
C23 O14 Dy2 137(2) . 1_445 ?
Dy2 O15 H15A 103(3) . . ?
Dy2 O15 H15B 151(5) . . ?
H15A O15 H15B 98.2(2) . . ?
Dy2 O16 H16B 146(4) . . ?
Dy2 O16 H16A 112(4) . . ?
H16B O16 H16A 98.2(2) . . ?
C10 N1 C9 116(2) . . ?
C10 N1 H1A 108.3 . . ?
C9 N1 H1A 108.3 . . ?
C10 N1 H1B 108.3 . . ?
C9 N1 H1B 108.3 . . ?
H1A N1 H1B 107.4 . . ?
C21 N2 C22 112(2) . . ?
C21 N2 H2A 109.2 . . ?
C22 N2 H2A 109.2 . . ?
C21 N2 H2B 109.2 . . ?
C22 N2 H2B 109.2 . . ?
H2A N2 H2B 107.9 . . ?
O2 C1 O1 121.7(19) . . ?
O2 C1 C2 121(2) . . ?
O1 C1 C2 117(2) . . ?
C8 C2 C3 122(2) . . ?
C8 C2 C1 122(3) . . ?
C3 C2 C1 115(2) . . ?
C2 C3 C4 119(2) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C6 C4 C3 117(3) . . ?
C6 C4 C5 123(2) . . ?
C3 C4 C5 120(2) . . ?
O4 C5 O3 131(3) . . ?
O4 C5 C4 114(2) . . ?
O3 C5 C4 115(2) . . ?
O4 C5 Dy1 51.4(15) . 1_545 ?
O3 C5 Dy1 82.2(15) . 1_545 ?
C4 C5 Dy1 160.9(18) . 1_545 ?
C7 C6 C4 125(3) . . ?
C7 C6 H6 117.3 . . ?
C4 C6 H6 117.3 . . ?
C6 C7 C8 118(3) . . ?
C6 C7 C9 123(3) . . ?
C8 C7 C9 120(3) . . ?
C2 C8 C7 119(3) . . ?
C2 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
N1 C9 C7 115(2) . . ?
N1 C9 H9A 108.5 . . ?
C7 C9 H9A 108.5 . . ?
N1 C9 H9B 108.5 . . ?
C7 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C12 C10 N1 112(2) . . ?
C12 C10 C11 115(2) . . ?
N1 C10 C11 106(2) . . ?
C12 C10 H10 107.9 . . ?
N1 C10 H10 107.9 . . ?
C11 C10 H10 107.9 . . ?
O6 C11 O5 129(2) . . ?
O6 C11 C10 114(2) . . ?
O5 C11 C10 116(3) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O10 C13 O9 115(2) . . ?
O10 C13 C14 123(2) . . ?
O9 C13 C14 121(2) . . ?
C15 C14 C20 123(2) . . ?
C15 C14 C13 121(2) . . ?
C20 C14 C13 116(2) . . ?
C14 C15 C16 121(2) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C18 117(2) . . ?
C15 C16 C17 123(2) . . ?
C18 C16 C17 119(2) . . ?
O12 C17 O11 120(2) . . ?
O12 C17 C16 122(3) . . ?
O11 C17 C16 118(2) . . ?
O12 C17 Dy2 62.1(13) . 1_545 ?
O11 C17 Dy2 58.2(10) . 1_545 ?
C16 C17 Dy2 175(2) . 1_545 ?
C19 C18 C16 123(2) . . ?
C19 C18 H18 118.6 . . ?
C16 C18 H18 118.6 . . ?
C18 C19 C21 123(3) . . ?
C18 C19 C20 118(3) . . ?
C21 C19 C20 117(3) . . ?
C14 C20 C19 117(3) . . ?
C14 C20 H20 121.6 . . ?
C19 C20 H20 121.6 . . ?
C19 C21 N2 112(2) . . ?
C19 C21 H21A 109.1 . . ?
N2 C21 H21A 109.1 . . ?
C19 C21 H21B 109.1 . . ?
N2 C21 H21B 109.1 . . ?
H21A C21 H21B 107.9 . . ?
C24 C22 N2 114(2) . . ?
C24 C22 C23 117(2) . . ?
N2 C22 C23 109(2) . . ?
C24 C22 H22 105.5 . . ?
N2 C22 H22 105.5 . . ?
C23 C22 H22 105.5 . . ?
O14 C23 O13 125(2) . . ?
O14 C23 C22 117(2) . . ?
O13 C23 C22 117(2) . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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
Dy1 O2 C1 O1 -11(3) . . . . ?
Dy1 O2 C1 C2 172(3) . . . . ?
Dy1 O1 C1 O2 10(3) . . . . ?
Dy1 O1 C1 C2 -172(2) . . . . ?
O2 C1 C2 C8 -176(3) . . . . ?
O1 C1 C2 C8 6(4) . . . . ?
O2 C1 C2 C3 -3(4) . . . . ?
O1 C1 C2 C3 180(2) . . . . ?
C8 C2 C3 C4 0(4) . . . . ?
C1 C2 C3 C4 -173(3) . . . . ?
C2 C3 C4 C6 0(4) . . . . ?
C2 C3 C4 C5 172(2) . . . . ?
Dy1 O4 C5 O3 -24(4) 1_545 . . . ?
Dy1 O4 C5 C4 165.9(18) 1_545 . . . ?
C6 C4 C5 O4 10(4) . . . . ?
C3 C4 C5 O4 -162(3) . . . . ?
C6 C4 C5 O3 -162(3) . . . . ?
C3 C4 C5 O3 26(4) . . . . ?
C6 C4 C5 Dy1 45(7) . . . 1_545 ?
C3 C4 C5 Dy1 -126(5) . . . 1_545 ?
C3 C4 C6 C7 2(4) . . . . ?
C5 C4 C6 C7 -169(3) . . . . ?
C4 C6 C7 C8 -5(5) . . . . ?
C4 C6 C7 C9 175(3) . . . . ?
C3 C2 C8 C7 -3(4) . . . . ?
C1 C2 C8 C7 170(3) . . . . ?
C6 C7 C8 C2 5(4) . . . . ?
C9 C7 C8 C2 -174(3) . . . . ?
C10 N1 C9 C7 160(2) . . . . ?
C6 C7 C9 N1 131(3) . . . . ?
C8 C7 C9 N1 -50(4) . . . . ?
C9 N1 C10 C12 170(2) . . . . ?
C9 N1 C10 C11 -64(3) . . . . ?
Dy2 O6 C11 O5 -7(5) 1_655 . . . ?
Dy2 O6 C11 C10 -177.0(17) 1_655 . . . ?
Dy1 O5 C11 O6 41(5) 1_655 . . . ?
Dy1 O5 C11 C10 -150(2) 1_655 . . . ?
C12 C10 C11 O6 78(3) . . . . ?
N1 C10 C11 O6 -46(3) . . . . ?
C12 C10 C11 O5 -93(3) . . . . ?
N1 C10 C11 O5 143(3) . . . . ?
Dy1 O10 C13 O9 126(6) . . . . ?
Dy1 O10 C13 C14 -69(8) . . . . ?
Dy2 O9 C13 O10 1(3) . . . . ?
Dy2 O9 C13 C14 -163.9(19) . . . . ?
O10 C13 C14 C15 -9(4) . . . . ?
O9 C13 C14 C15 155(3) . . . . ?
O10 C13 C14 C20 179(2) . . . . ?
O9 C13 C14 C20 -17(4) . . . . ?
C20 C14 C15 C16 4(4) . . . . ?
C13 C14 C15 C16 -167(2) . . . . ?
C14 C15 C16 C18 -4(4) . . . . ?
C14 C15 C16 C17 169(3) . . . . ?
Dy2 O12 C17 O11 3(2) 1_545 . . . ?
Dy2 O12 C17 C16 177(2) 1_545 . . . ?
Dy2 O11 C17 O12 -3(3) 1_545 . . . ?
Dy2 O11 C17 C16 -177(2) 1_545 . . . ?
C15 C16 C17 O12 169(2) . . . . ?
C18 C16 C17 O12 -18(4) . . . . ?
C15 C16 C17 O11 -17(4) . . . . ?
C18 C16 C17 O11 156(2) . . . . ?
C15 C16 C18 C19 -3(4) . . . . ?
C17 C16 C18 C19 -177(3) . . . . ?
C16 C18 C19 C21 174(3) . . . . ?
C16 C18 C19 C20 9(4) . . . . ?
C15 C14 C20 C19 2(4) . . . . ?
C13 C14 C20 C19 173(2) . . . . ?
C18 C19 C20 C14 -8(4) . . . . ?
C21 C19 C20 C14 -174(3) . . . . ?
C18 C19 C21 N2 64(4) . . . . ?
C20 C19 C21 N2 -131(3) . . . . ?
C22 N2 C21 C19 -161(2) . . . . ?
C21 N2 C22 C24 -61(3) . . . . ?
C21 N2 C22 C23 71(3) . . . . ?
Dy2 O14 C23 O13 -33(5) 1_445 . . . ?
Dy2 O14 C23 C22 138(2) 1_445 . . . ?
Dy1 O13 C23 O14 -13(5) 1_445 . . . ?
Dy1 O13 C23 C22 176.7(17) 1_445 . . . ?
C24 C22 C23 O14 -14(4) . . . . ?
N2 C22 C23 O14 -145(3) . . . . ?
C24 C22 C23 O13 157(2) . . . . ?
N2 C22 C23 O13 27(4) . . . . ?

_refine_diff_density_max         1.159
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.156


# start Validation Reply Form
_vrf_PLAT306_IV                  
;
RESPONSE: The H atoms of lattice water molecules O17, O18, O19, 
O20 and O21 were not added owing to not suitable Fourier maps 
being picked up.
;
_vrf_PLAT342_IV                  
;
RESPONSE: The precision of the C-C bonds of IV is slightly low, 
which perhaps results from the weak diffraction owing to the 
bad quality and small sizes of single crystal and/or from the 
effect of heavy Dy atom whose strong diffraction signals affect 
the accurate detection of lighter atom C. 
;
_vrf_PLAT420_IV                  
;
RESPONSE: No suitable hydrogen-bond for H16A of water O16 
were found. 
;
_vrf_PLAT430_IV                  
;
RESPONSE: The H atoms of lattice water molecules O17, O18, O20 
and O21 were not added owing to not suitable Fourier maps being 
picked up. Thus hydrogen-bonding interactions between them 
could not be determined.
;
_vrf_PLAT987_IV                  
;
RESPONSE: A BASF/TWIN Refinement does not well, but the 
measurement of CD spectrum as well as homochiral ligand 
further confirm the homochiral framework of IV.
;
