# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1855008'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 Cl4 Eu F4 N4 Na O16'
_chemical_formula_weight         1369.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1580 3.6680 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0360 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0557(4)
_cell_length_b                   12.7534(5)
_cell_length_c                   22.0808(8)
_cell_angle_alpha                73.488(3)
_cell_angle_beta                 85.530(3)
_cell_angle_gamma                72.201(4)
_cell_volume                     2584.88(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18025
_cell_measurement_theta_min      3.7460
_cell_measurement_theta_max      28.5650

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7821
_exptl_absorpt_correction_T_max  0.8386
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22543
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9006
_reflns_number_gt                8010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0399P)²+1.8298P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9006
_refine_ls_number_parameters     745
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu2 Eu 0.123113(19) 0.489801(17) 0.258509(9) 0.02698(8) Uani 1 1 d . . .
Cl1 Cl -0.41387(11) 0.81342(11) 0.54051(6) 0.0525(3) Uani 1 1 d . . .
Cl2 Cl 0.23742(13) 1.03925(13) 0.39727(7) 0.0649(4) Uani 1 1 d . . .
Cl3 Cl -0.04084(12) 0.25220(12) -0.06485(6) 0.0551(4) Uani 1 1 d . . .
C15 C -0.1115(4) 0.7758(3) 0.2711(2) 0.0318(9) Uani 1 1 d . . .
C16 C 0.0365(4) 0.7548(3) 0.2740(2) 0.0312(9) Uani 1 1 d . . .
C19 C -0.1979(4) 0.8630(3) 0.2923(2) 0.0332(10) Uani 1 1 d . . .
H19 H -0.2935 0.8774 0.2878 0.040 Uiso 1 1 calc R . .
N2 N -0.1557(3) 0.9305(3) 0.31941(17) 0.0333(8) Uani 1 1 d . . .
C18 C -0.0135(4) 0.9132(3) 0.3260(2) 0.0313(9) Uani 1 1 d . . .
C17 C 0.0825(4) 0.8277(3) 0.3028(2) 0.0316(9) Uani 1 1 d . . .
C14 C -0.1786(4) 0.7049(3) 0.2467(2) 0.0346(10) Uani 1 1 d . . .
O1 O -0.0999(3) 0.6235(2) 0.22657(14) 0.0381(7) Uani 1 1 d . . .
O2 O -0.3080(3) 0.7292(3) 0.24882(18) 0.0551(10) Uani 1 1 d . . .
C23 C 0.2264(4) 0.8118(4) 0.3081(2) 0.0380(10) Uani 1 1 d . . .
H23 H 0.2913 0.7559 0.2929 0.046 Uiso 1 1 calc R . .
C24 C 0.2699(4) 0.8784(4) 0.3355(2) 0.0395(11) Uani 1 1 d . . .
C26 C 0.0348(4) 0.9788(4) 0.3553(2) 0.0397(11) Uani 1 1 d . . .
H26 H -0.0282 1.0351 0.3709 0.048 Uiso 1 1 calc R . .
C20 C -0.2572(4) 1.0278(4) 0.3361(2) 0.0347(10) Uani 1 1 d . . .
H20 H -0.2610 1.1035 0.3080 0.042 Uiso 1 1 calc R . .
C21 C -0.2829(4) 1.0219(4) 0.4045(2) 0.0478(13) Uani 1 1 d . . .
H21A H -0.2329 0.9525 0.4354 0.057 Uiso 1 1 calc R . .
H21B H -0.2995 1.0919 0.4169 0.057 Uiso 1 1 calc R . .
C22 C -0.3917(4) 1.0147(4) 0.3647(2) 0.0455(12) Uani 1 1 d . . .
H22A H -0.4078 0.9410 0.3717 0.055 Uiso 1 1 calc R . .
H22B H -0.4743 1.0802 0.3533 0.055 Uiso 1 1 calc R . .
C5 C -0.0379(4) 0.6635(3) 0.48062(19) 0.0293(9) Uani 1 1 d . . .
N1 N 0.1018(3) 0.6481(3) 0.49263(17) 0.0342(9) Uani 1 1 d . . .
C4 C -0.0709(4) 0.6201(3) 0.43428(18) 0.0276(9) Uani 1 1 d . . .
C13 C -0.1447(4) 0.7209(4) 0.5154(2) 0.0340(10) Uani 1 1 d . . .
H13 H -0.1226 0.7479 0.5471 0.041 Uiso 1 1 calc R . .
C12 C -0.2815(4) 0.7364(4) 0.5020(2) 0.0341(10) Uani 1 1 d . . .
C10 C -0.2116(4) 0.6343(4) 0.42283(19) 0.0322(10) Uani 1 1 d . . .
H10 H -0.2353 0.6049 0.3926 0.039 Uiso 1 1 calc R . .
C11 C -0.3133(4) 0.6916(4) 0.4564(2) 0.0369(10) Uani 1 1 d . . .
F1 F -0.4485(2) 0.7041(3) 0.44608(13) 0.0557(8) Uani 1 1 d . . .
C6 C 0.2024(4) 0.5924(4) 0.4591(2) 0.0348(10) Uani 1 1 d . . .
H6 H 0.2948 0.5824 0.4686 0.042 Uiso 1 1 calc R . .
C2 C 0.1783(4) 0.5497(3) 0.41227(19) 0.0281(9) Uani 1 1 d . . .
C3 C 0.0387(4) 0.5596(3) 0.39752(18) 0.0268(9) Uani 1 1 d . . .
C1 C 0.3056(4) 0.4911(4) 0.3799(2) 0.0340(10) Uani 1 1 d . . .
O6 O 0.0035(3) 0.5224(2) 0.35618(13) 0.0318(7) Uani 1 1 d . . .
O4 O 0.2873(3) 0.4466(3) 0.33774(14) 0.0417(8) Uani 1 1 d . . .
O5 O 0.4213(3) 0.4869(3) 0.39735(16) 0.0561(10) Uani 1 1 d . . .
C25 C 0.1756(4) 0.9595(4) 0.3608(2) 0.0407(11) Uani 1 1 d . . .
O3 O 0.1273(3) 0.6783(2) 0.25614(15) 0.0412(8) Uani 1 1 d . . .
C7 C 0.1404(4) 0.6778(4) 0.5471(2) 0.0470(12) Uani 1 1 d . . .
H7 H 0.1280 0.6276 0.5885 0.056 Uiso 1 1 calc R . .
C9 C 0.2622(5) 0.7211(5) 0.5421(3) 0.0565(15) Uani 1 1 d . . .
H9A H 0.3098 0.7327 0.5020 0.068 Uiso 1 1 calc R . .
H9B H 0.3218 0.6968 0.5791 0.068 Uiso 1 1 calc R . .
C8 C 0.1158(5) 0.7970(5) 0.5452(3) 0.0678(18) Uani 1 1 d . . .
H8A H 0.0874 0.8189 0.5839 0.081 Uiso 1 1 calc R . .
H8B H 0.0754 0.8548 0.5069 0.081 Uiso 1 1 calc R . .
C37 C -0.0642(4) 0.3419(4) 0.0341(2) 0.0380(11) Uani 1 1 d . . .
C36 C -0.0187(4) 0.3847(4) 0.0757(2) 0.0324(9) Uani 1 1 d . . .
H36 H -0.0784 0.4105 0.1063 0.039 Uiso 1 1 calc R . .
C30 C 0.1195(4) 0.3894(3) 0.07206(19) 0.0289(9) Uani 1 1 d . . .
C38 C 0.0230(4) 0.3046(4) -0.0128(2) 0.0345(10) Uani 1 1 d . . .
C39 C 0.1569(4) 0.3101(3) -0.0177(2) 0.0333(10) Uani 1 1 d . . .
H39 H 0.2145 0.2863 -0.0493 0.040 Uiso 1 1 calc R . .
C31 C 0.2071(4) 0.3515(3) 0.02507(19) 0.0282(9) Uani 1 1 d . . .
C29 C 0.1675(4) 0.4364(3) 0.11689(19) 0.0290(9) Uani 1 1 d . . .
O9 O 0.0839(3) 0.4691(3) 0.15780(13) 0.0344(7) Uani 1 1 d . . .
C28 C 0.3092(4) 0.4389(3) 0.10960(19) 0.0292(9) Uani 1 1 d . . .
C32 C 0.3884(4) 0.3986(3) 0.06356(19) 0.0310(9) Uani 1 1 d . . .
H32 H 0.4801 0.4015 0.0600 0.037 Uiso 1 1 calc R . .
N3 N 0.3450(3) 0.3552(3) 0.02280(16) 0.0320(8) Uani 1 1 d . . .
C33 C 0.4381(4) 0.3198(4) -0.0264(2) 0.0415(12) Uani 1 1 d . . .
H33 H 0.4217 0.3738 -0.0687 0.050 Uiso 1 1 calc R . .
F3 F -0.1966(2) 0.3360(3) 0.03790(14) 0.0620(9) Uani 1 1 d . . .
F2 F 0.4076(2) 0.8665(3) 0.33852(15) 0.0622(9) Uani 1 1 d . . .
C49 C 0.5076(4) 0.1638(4) 0.2005(2) 0.0348(10) Uani 1 1 d . . .
H49 H 0.5260 0.2172 0.2171 0.042 Uiso 1 1 calc R . .
C50 C 0.6113(4) 0.0977(4) 0.1722(2) 0.0407(11) Uani 1 1 d . . .
C52 C 0.4581(4) 0.0015(4) 0.1508(2) 0.0381(11) Uani 1 1 d . . .
H52 H 0.4426 -0.0542 0.1352 0.046 Uiso 1 1 calc R . .
C44 C 0.3488(4) 0.0709(4) 0.1784(2) 0.0321(10) Uani 1 1 d . . .
C43 C 0.3732(4) 0.1516(3) 0.20458(19) 0.0295(9) Uani 1 1 d . . .
O12 O 0.2860(3) 0.2985(2) 0.25513(14) 0.0342(7) Uani 1 1 d . . .
C42 C 0.2603(4) 0.2251(3) 0.23381(19) 0.0282(9) Uani 1 1 d . . .
C45 C 0.1121(4) 0.1261(4) 0.2084(2) 0.0355(10) Uani 1 1 d . . .
H45 H 0.0243 0.1155 0.2102 0.043 Uiso 1 1 calc R . .
N4 N 0.2135(3) 0.0611(3) 0.17977(17) 0.0319(8) Uani 1 1 d . . .
C41 C 0.1270(4) 0.2063(3) 0.2351(2) 0.0318(10) Uani 1 1 d . . .
C40 C -0.0014(4) 0.2700(4) 0.2643(2) 0.0420(12) Uani 1 1 d . . .
O10 O 0.0039(3) 0.3512(2) 0.28522(14) 0.0400(8) Uani 1 1 d . . .
O11 O -0.1073(3) 0.2380(3) 0.2668(2) 0.0815(15) Uani 1 1 d . . .
C51 C 0.5881(4) 0.0166(4) 0.1471(2) 0.0393(11) Uani 1 1 d . . .
O7 O 0.3059(3) 0.5303(2) 0.19077(14) 0.0366(7) Uani 1 1 d . . .
O8 O 0.5090(3) 0.4590(4) 0.14851(18) 0.0652(12) Uani 1 1 d . . .
C27 C 0.3806(4) 0.4793(4) 0.1528(2) 0.0363(10) Uani 1 1 d . . .
Cl4 Cl 0.72268(11) -0.06392(12) 0.11055(7) 0.0584(4) Uani 1 1 d . . .
F4 F 0.7402(2) 0.1108(3) 0.16823(16) 0.0644(9) Uani 1 1 d . . .
C46 C 0.1885(4) -0.0222(4) 0.1523(2) 0.0407(11) Uani 1 1 d . . .
H46 H 0.2282 -0.1027 0.1759 0.049 Uiso 1 1 calc R . .
C34 C 0.4853(4) 0.1960(5) -0.0243(3) 0.0544(14) Uani 1 1 d . . .
H34A H 0.4545 0.1432 0.0107 0.065 Uiso 1 1 calc R . .
H34B H 0.4949 0.1764 -0.0642 0.065 Uiso 1 1 calc R . .
C47 C 0.1839(4) 0.0010(5) 0.0825(3) 0.0525(14) Uani 1 1 d . . .
H47A H 0.2222 -0.0633 0.0648 0.063 Uiso 1 1 calc R . .
H47B H 0.1967 0.0728 0.0570 0.063 Uiso 1 1 calc R . .
C35 C 0.5849(5) 0.2518(5) -0.0104(3) 0.0578(15) Uani 1 1 d . . .
H35A H 0.6150 0.2326 0.0331 0.069 Uiso 1 1 calc R . .
H35B H 0.6553 0.2658 -0.0416 0.069 Uiso 1 1 calc R . .
O3W O 0.7481(4) 0.5321(5) 0.16725(19) 0.1054(19) Uani 1 1 d . . .
H3WA H 0.7199 0.5354 0.1313 0.158 Uiso 1 1 d R A 1
H3WB H 0.8368 0.5132 0.1678 0.158 Uiso 1 1 d R A 1
C48 C 0.0540(5) 0.0056(5) 0.1195(3) 0.0688(18) Uani 1 1 d . . .
H48A H -0.0126 0.0803 0.1164 0.083 Uiso 1 1 calc R . .
H48B H 0.0129 -0.0559 0.1242 0.083 Uiso 1 1 calc R . .
O2W O 0.6284(4) 0.5282(3) 0.3146(2) 0.0826(9) Uani 1 1 d . . .
H2WA H 0.6823 0.5703 0.3065 0.124 Uiso 1 1 d R B 1
H2WB H 0.6424 0.4859 0.3524 0.124 Uiso 1 1 d R B 1
O1W O 0.5478(3) 0.3085(3) 0.30977(19) 0.0698(12) Uani 1 1 d . . .
H1WA H 0.5917 0.2374 0.3208 0.105 Uiso 1 1 d R C 1
H1WB H 0.4708 0.3187 0.2922 0.105 Uiso 1 1 d R C 1
O4W O -0.5599(5) 0.7185(4) 0.1820(2) 0.0749(12) Uani 1 1 d G . .
H4WA H -0.4979 0.7147 0.2072 0.112 Uiso 1 1 d G . .
H4WB H -0.5986 0.6664 0.1983 0.112 Uiso 1 1 d G . .
Na1 Na 0.6793(4) 0.4038(3) 0.2403(2) 0.0826(9) Uani 0.70 1 d P D 1
Na' Na 0.7507(6) 0.3920(6) 0.2838(3) 0.0517(17) Uani 0.30 1 d P E 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu2 O4 2.332(3) . ?
Eu2 O10 2.345(3) . ?
Eu2 O7 2.365(3) . ?
Eu2 O1 2.379(3) . ?
Eu2 O9 2.388(3) . ?
Eu2 O3 2.402(3) . ?
Eu2 O6 2.464(2) . ?
Eu2 O12 2.506(3) . ?
Cl1 C12 1.720(4) . ?
Cl2 C25 1.731(4) . ?
Cl3 C38 1.730(4) . ?
C15 C19 1.361(5) . ?
C15 C16 1.432(5) . ?
C15 C14 1.507(5) . ?
C16 O3 1.250(4) . ?
C16 C17 1.458(5) . ?
C19 N2 1.354(5) . ?
C19 H19 0.9300 . ?
N2 C18 1.392(5) . ?
N2 C20 1.464(5) . ?
C18 C17 1.407(5) . ?
C18 C26 1.399(5) . ?
C17 C23 1.408(5) . ?
C14 O2 1.242(5) . ?
C14 O1 1.268(5) . ?
C23 C24 1.357(6) . ?
C23 H23 0.9300 . ?
C24 F2 1.350(4) . ?
C24 C25 1.388(6) . ?
C26 C25 1.370(6) . ?
C26 H26 0.9300 . ?
C20 C22 1.483(5) . ?
C20 C21 1.496(6) . ?
C20 H20 0.9800 . ?
C21 C22 1.494(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C5 N1 1.394(5) . ?
C5 C4 1.396(5) . ?
C5 C13 1.410(5) . ?
N1 C6 1.348(5) . ?
N1 C7 1.471(5) . ?
C4 C10 1.404(5) . ?
C4 C3 1.472(5) . ?
C13 C12 1.372(5) . ?
C13 H13 0.9300 . ?
C12 C11 1.391(6) . ?
C10 C11 1.363(5) . ?
C10 H10 0.9300 . ?
C11 F1 1.349(4) . ?
C6 C2 1.367(5) . ?
C6 H6 0.9300 . ?
C2 C3 1.425(5) . ?
C2 C1 1.511(5) . ?
C3 O6 1.258(4) . ?
C1 O5 1.235(5) . ?
C1 O4 1.269(5) . ?
C7 C8 1.451(7) . ?
C7 C9 1.474(6) . ?
C7 H7 0.9800 . ?
C9 C8 1.502(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C37 F3 1.351(4) . ?
C37 C36 1.363(5) . ?
C37 C38 1.397(6) . ?
C36 C30 1.404(5) . ?
C36 H36 0.9300 . ?
C30 C31 1.403(5) . ?
C30 C29 1.470(5) . ?
C38 C39 1.364(5) . ?
C39 C31 1.394(5) . ?
C39 H39 0.9300 . ?
C31 N3 1.399(5) . ?
C29 O9 1.256(4) . ?
C29 C28 1.431(5) . ?
C28 C32 1.361(5) . ?
C28 C27 1.517(5) . ?
C32 N3 1.342(5) . ?
C32 H32 0.9300 . ?
N3 C33 1.457(5) . ?
C33 C35 1.477(6) . ?
C33 C34 1.492(7) . ?
C33 H33 0.9800 . ?
C49 C50 1.359(5) . ?
C49 C43 1.400(5) . ?
C49 H49 0.9300 . ?
C50 F4 1.351(4) . ?
C50 C51 1.388(6) . ?
C52 C51 1.371(5) . ?
C52 C44 1.403(5) . ?
C52 H52 0.9300 . ?
C44 N4 1.401(5) . ?
C44 C43 1.404(5) . ?
C43 C42 1.471(5) . ?
O12 C42 1.258(4) . ?
C42 C41 1.429(5) . ?
C45 N4 1.345(5) . ?
C45 C41 1.366(5) . ?
C45 H45 0.9300 . ?
N4 C46 1.453(5) . ?
C41 C40 1.506(5) . ?
C40 O11 1.244(5) . ?
C40 O10 1.264(5) . ?
C51 Cl4 1.729(4) . ?
O7 C27 1.267(4) . ?
O8 C27 1.238(5) . ?
C46 C48 1.481(6) . ?
C46 C47 1.486(7) . ?
C46 H46 0.9800 . ?
C34 C35 1.488(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C47 C48 1.479(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
O3W H3WA 0.8499 . ?
O3W H3WB 0.8499 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
O2W Na' 2.056(7) . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8498 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Eu2 O10 108.37(11) . . ?
O4 Eu2 O7 83.40(10) . . ?
O10 Eu2 O7 137.92(9) . . ?
O4 Eu2 O1 137.27(9) . . ?
O10 Eu2 O1 85.41(10) . . ?
O7 Eu2 O1 113.57(10) . . ?
O4 Eu2 O9 145.43(9) . . ?
O10 Eu2 O9 77.63(10) . . ?
O7 Eu2 O9 71.76(9) . . ?
O1 Eu2 O9 76.13(9) . . ?
O4 Eu2 O3 79.06(11) . . ?
O10 Eu2 O3 148.35(9) . . ?
O7 Eu2 O3 72.47(9) . . ?
O1 Eu2 O3 70.41(9) . . ?
O9 Eu2 O3 114.17(11) . . ?
O4 Eu2 O6 70.13(9) . . ?
O10 Eu2 O6 77.96(9) . . ?
O7 Eu2 O6 141.95(8) . . ?
O1 Eu2 O6 73.90(9) . . ?
O9 Eu2 O6 142.48(8) . . ?
O3 Eu2 O6 75.94(9) . . ?
O4 Eu2 O12 75.92(9) . . ?
O10 Eu2 O12 69.85(9) . . ?
O7 Eu2 O12 74.59(9) . . ?
O1 Eu2 O12 144.92(9) . . ?
O9 Eu2 O12 74.57(9) . . ?
O3 Eu2 O12 140.42(9) . . ?
O6 Eu2 O12 121.90(9) . . ?
C19 C15 C16 119.1(4) . . ?
C19 C15 C14 117.2(3) . . ?
C16 C15 C14 123.6(3) . . ?
O3 C16 C15 125.8(4) . . ?
O3 C16 C17 118.3(3) . . ?
C15 C16 C17 115.9(3) . . ?
N2 C19 C15 125.2(4) . . ?
N2 C19 H19 117.4 . . ?
C15 C19 H19 117.4 . . ?
C19 N2 C18 119.3(3) . . ?
C19 N2 C20 120.7(3) . . ?
C18 N2 C20 119.7(3) . . ?
N2 C18 C17 118.9(3) . . ?
N2 C18 C26 121.2(3) . . ?
C17 C18 C26 119.9(4) . . ?
C18 C17 C23 119.0(4) . . ?
C18 C17 C16 121.6(3) . . ?
C23 C17 C16 119.4(3) . . ?
O2 C14 O1 124.4(4) . . ?
O2 C14 C15 117.4(3) . . ?
O1 C14 C15 118.2(3) . . ?
C14 O1 Eu2 133.6(3) . . ?
C24 C23 C17 119.6(4) . . ?
C24 C23 H23 120.2 . . ?
C17 C23 H23 120.2 . . ?
F2 C24 C23 119.8(4) . . ?
F2 C24 C25 118.7(4) . . ?
C23 C24 C25 121.4(4) . . ?
C25 C26 C18 119.6(4) . . ?
C25 C26 H26 120.2 . . ?
C18 C26 H26 120.2 . . ?
N2 C20 C22 119.3(3) . . ?
N2 C20 C21 118.6(4) . . ?
C22 C20 C21 60.2(3) . . ?
N2 C20 H20 115.8 . . ?
C22 C20 H20 115.8 . . ?
C21 C20 H20 115.8 . . ?
C22 C21 C20 59.4(3) . . ?
C22 C21 H21A 117.8 . . ?
C20 C21 H21A 117.8 . . ?
C22 C21 H21B 117.8 . . ?
C20 C21 H21B 117.8 . . ?
H21A C21 H21B 115.0 . . ?
C20 C22 C21 60.3(3) . . ?
C20 C22 H22A 117.7 . . ?
C21 C22 H22A 117.7 . . ?
C20 C22 H22B 117.7 . . ?
C21 C22 H22B 117.7 . . ?
H22A C22 H22B 114.9 . . ?
N1 C5 C4 119.2(3) . . ?
N1 C5 C13 120.4(3) . . ?
C4 C5 C13 120.4(3) . . ?
C6 N1 C5 119.5(3) . . ?
C6 N1 C7 119.7(3) . . ?
C5 N1 C7 120.2(3) . . ?
C5 C4 C10 119.2(3) . . ?
C5 C4 C3 121.3(3) . . ?
C10 C4 C3 119.5(3) . . ?
C12 C13 C5 119.3(4) . . ?
C12 C13 H13 120.4 . . ?
C5 C13 H13 120.4 . . ?
C13 C12 C11 119.9(3) . . ?
C13 C12 Cl1 120.2(3) . . ?
C11 C12 Cl1 119.9(3) . . ?
C11 C10 C4 119.5(4) . . ?
C11 C10 H10 120.2 . . ?
C4 C10 H10 120.2 . . ?
F1 C11 C10 119.7(4) . . ?
F1 C11 C12 118.6(3) . . ?
C10 C11 C12 121.7(4) . . ?
N1 C6 C2 124.6(4) . . ?
N1 C6 H6 117.7 . . ?
C2 C6 H6 117.7 . . ?
C6 C2 C3 119.7(3) . . ?
C6 C2 C1 116.4(3) . . ?
C3 C2 C1 123.8(3) . . ?
O6 C3 C2 125.6(3) . . ?
O6 C3 C4 118.8(3) . . ?
C2 C3 C4 115.6(3) . . ?
O5 C1 O4 124.1(4) . . ?
O5 C1 C2 117.8(4) . . ?
O4 C1 C2 118.1(3) . . ?
C3 O6 Eu2 129.8(2) . . ?
C1 O4 Eu2 136.7(3) . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 Cl2 120.3(3) . . ?
C24 C25 Cl2 119.4(3) . . ?
C16 O3 Eu2 129.0(2) . . ?
C8 C7 N1 120.1(5) . . ?
C8 C7 C9 61.8(3) . . ?
N1 C7 C9 118.9(4) . . ?
C8 C7 H7 115.2 . . ?
N1 C7 H7 115.2 . . ?
C9 C7 H7 115.2 . . ?
C7 C9 C8 58.4(3) . . ?
C7 C9 H9A 117.9 . . ?
C8 C9 H9A 117.9 . . ?
C7 C9 H9B 117.9 . . ?
C8 C9 H9B 117.9 . . ?
H9A C9 H9B 115.1 . . ?
C7 C8 C9 59.8(3) . . ?
C7 C8 H8A 117.8 . . ?
C9 C8 H8A 117.8 . . ?
C7 C8 H8B 117.8 . . ?
C9 C8 H8B 117.8 . . ?
H8A C8 H8B 114.9 . . ?
F3 C37 C36 119.5(4) . . ?
F3 C37 C38 119.2(3) . . ?
C36 C37 C38 121.4(3) . . ?
C37 C36 C30 119.2(4) . . ?
C37 C36 H36 120.4 . . ?
C30 C36 H36 120.4 . . ?
C36 C30 C31 119.3(3) . . ?
C36 C30 C29 118.9(3) . . ?
C31 C30 C29 121.8(3) . . ?
C39 C38 C37 120.2(3) . . ?
C39 C38 Cl3 120.5(3) . . ?
C37 C38 Cl3 119.4(3) . . ?
C38 C39 C31 119.7(4) . . ?
C38 C39 H39 120.2 . . ?
C31 C39 H39 120.2 . . ?
C39 C31 N3 121.3(3) . . ?
C39 C31 C30 120.2(3) . . ?
N3 C31 C30 118.5(3) . . ?
O9 C29 C28 126.0(3) . . ?
O9 C29 C30 118.7(3) . . ?
C28 C29 C30 115.3(3) . . ?
C29 O9 Eu2 131.4(2) . . ?
C32 C28 C29 119.5(3) . . ?
C32 C28 C27 116.9(3) . . ?
C29 C28 C27 123.5(3) . . ?
N3 C32 C28 125.3(3) . . ?
N3 C32 H32 117.3 . . ?
C28 C32 H32 117.3 . . ?
C32 N3 C31 119.6(3) . . ?
C32 N3 C33 120.1(3) . . ?
C31 N3 C33 120.2(3) . . ?
N3 C33 C35 119.5(4) . . ?
N3 C33 C34 118.4(4) . . ?
C35 C33 C34 60.2(3) . . ?
N3 C33 H33 115.8 . . ?
C35 C33 H33 115.8 . . ?
C34 C33 H33 115.8 . . ?
C50 C49 C43 120.2(4) . . ?
C50 C49 H49 119.9 . . ?
C43 C49 H49 119.9 . . ?
F4 C50 C49 119.5(4) . . ?
F4 C50 C51 118.9(3) . . ?
C49 C50 C51 121.6(4) . . ?
C51 C52 C44 119.5(4) . . ?
C51 C52 H52 120.3 . . ?
C44 C52 H52 120.3 . . ?
N4 C44 C52 120.5(3) . . ?
N4 C44 C43 119.1(3) . . ?
C52 C44 C43 120.5(3) . . ?
C49 C43 C44 118.4(3) . . ?
C49 C43 C42 120.2(3) . . ?
C44 C43 C42 121.4(3) . . ?
C42 O12 Eu2 127.2(2) . . ?
O12 C42 C41 125.1(3) . . ?
O12 C42 C43 119.3(3) . . ?
C41 C42 C43 115.6(3) . . ?
N4 C45 C41 125.7(3) . . ?
N4 C45 H45 117.2 . . ?
C41 C45 H45 117.2 . . ?
C45 N4 C44 119.0(3) . . ?
C45 N4 C46 122.1(3) . . ?
C44 N4 C46 118.9(3) . . ?
C45 C41 C42 119.2(3) . . ?
C45 C41 C40 116.6(3) . . ?
C42 C41 C40 124.2(3) . . ?
O11 C40 O10 123.7(4) . . ?
O11 C40 C41 117.2(4) . . ?
O10 C40 C41 119.1(3) . . ?
C40 O10 Eu2 135.9(3) . . ?
C52 C51 C50 119.8(4) . . ?
C52 C51 Cl4 120.3(3) . . ?
C50 C51 Cl4 119.8(3) . . ?
C27 O7 Eu2 131.9(2) . . ?
O8 C27 O7 124.6(4) . . ?
O8 C27 C28 117.1(3) . . ?
O7 C27 C28 118.3(3) . . ?
N4 C46 C48 119.2(4) . . ?
N4 C46 C47 119.7(4) . . ?
C48 C46 C47 59.8(3) . . ?
N4 C46 H46 115.6 . . ?
C48 C46 H46 115.6 . . ?
C47 C46 H46 115.6 . . ?
C35 C34 C33 59.4(3) . . ?
C35 C34 H34A 117.8 . . ?
C33 C34 H34A 117.8 . . ?
C35 C34 H34B 117.8 . . ?
C33 C34 H34B 117.8 . . ?
H34A C34 H34B 115.0 . . ?
C46 C47 C48 59.9(3) . . ?
C46 C47 H47A 117.8 . . ?
C48 C47 H47A 117.8 . . ?
C46 C47 H47B 117.8 . . ?
C48 C47 H47B 117.8 . . ?
H47A C47 H47B 114.9 . . ?
C33 C35 C34 60.4(3) . . ?
C33 C35 H35A 117.7 . . ?
C34 C35 H35A 117.7 . . ?
C33 C35 H35B 117.7 . . ?
C34 C35 H35B 117.7 . . ?
H35A C35 H35B 114.9 . . ?
H3WA O3W H3WB 109.5 . . ?
C46 C48 C47 60.3(3) . . ?
C46 C48 H48A 117.7 . . ?
C47 C48 H48A 117.7 . . ?
C46 C48 H48B 117.7 . . ?
C47 C48 H48B 117.7 . . ?
H48A C48 H48B 114.9 . . ?
Na' O2W H2WA 99.6 . . ?
Na' O2W H2WB 89.0 . . ?
H2WA O2W H2WB 109.5 . . ?
H1WA O1W H1WB 109.5 . . ?
H4WA O4W H4WB 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
C19 C15 C16 O3 -179.8(4) . . . . ?
C14 C15 C16 O3 1.4(7) . . . . ?
C19 C15 C16 C17 2.6(6) . . . . ?
C14 C15 C16 C17 -176.2(4) . . . . ?
C16 C15 C19 N2 -3.3(7) . . . . ?
C14 C15 C19 N2 175.6(4) . . . . ?
C15 C19 N2 C18 1.1(7) . . . . ?
C15 C19 N2 C20 175.2(4) . . . . ?
C19 N2 C18 C17 1.6(6) . . . . ?
C20 N2 C18 C17 -172.5(4) . . . . ?
C19 N2 C18 C26 -178.2(4) . . . . ?
C20 N2 C18 C26 7.6(6) . . . . ?
N2 C18 C17 C23 178.5(4) . . . . ?
C26 C18 C17 C23 -1.6(6) . . . . ?
N2 C18 C17 C16 -2.1(6) . . . . ?
C26 C18 C17 C16 177.8(4) . . . . ?
O3 C16 C17 C18 -177.8(4) . . . . ?
C15 C16 C17 C18 0.0(6) . . . . ?
O3 C16 C17 C23 1.5(6) . . . . ?
C15 C16 C17 C23 179.4(4) . . . . ?
C19 C15 C14 O2 -1.4(6) . . . . ?
C16 C15 C14 O2 177.4(4) . . . . ?
C19 C15 C14 O1 179.8(4) . . . . ?
C16 C15 C14 O1 -1.4(6) . . . . ?
O2 C14 O1 Eu2 -142.2(4) . . . . ?
C15 C14 O1 Eu2 36.5(6) . . . . ?
O4 Eu2 O1 C14 1.5(4) . . . . ?
O10 Eu2 O1 C14 113.8(4) . . . . ?
O7 Eu2 O1 C14 -105.2(4) . . . . ?
O9 Eu2 O1 C14 -167.8(4) . . . . ?
O3 Eu2 O1 C14 -45.4(4) . . . . ?
O6 Eu2 O1 C14 35.0(4) . . . . ?
O12 Eu2 O1 C14 158.1(3) . . . . ?
C18 C17 C23 C24 0.2(7) . . . . ?
C16 C17 C23 C24 -179.2(4) . . . . ?
C17 C23 C24 F2 -177.5(4) . . . . ?
C17 C23 C24 C25 2.5(7) . . . . ?
N2 C18 C26 C25 -179.8(4) . . . . ?
C17 C18 C26 C25 0.3(7) . . . . ?
C19 N2 C20 C22 41.2(6) . . . . ?
C18 N2 C20 C22 -144.8(4) . . . . ?
C19 N2 C20 C21 111.1(4) . . . . ?
C18 N2 C20 C21 -74.8(5) . . . . ?
N2 C20 C21 C22 -109.3(4) . . . . ?
N2 C20 C22 C21 108.2(5) . . . . ?
C4 C5 N1 C6 0.4(6) . . . . ?
C13 C5 N1 C6 179.6(4) . . . . ?
C4 C5 N1 C7 -171.1(4) . . . . ?
C13 C5 N1 C7 8.1(6) . . . . ?
N1 C5 C4 C10 179.2(4) . . . . ?
C13 C5 C4 C10 -0.1(6) . . . . ?
N1 C5 C4 C3 -0.6(6) . . . . ?
C13 C5 C4 C3 -179.8(4) . . . . ?
N1 C5 C13 C12 179.0(4) . . . . ?
C4 C5 C13 C12 -1.8(6) . . . . ?
C5 C13 C12 C11 2.7(7) . . . . ?
C5 C13 C12 Cl1 -176.2(3) . . . . ?
C5 C4 C10 C11 1.0(6) . . . . ?
C3 C4 C10 C11 -179.2(4) . . . . ?
C4 C10 C11 F1 -179.1(4) . . . . ?
C4 C10 C11 C12 -0.2(7) . . . . ?
C13 C12 C11 F1 177.3(4) . . . . ?
Cl1 C12 C11 F1 -3.9(6) . . . . ?
C13 C12 C11 C10 -1.7(7) . . . . ?
Cl1 C12 C11 C10 177.1(4) . . . . ?
C5 N1 C6 C2 1.0(7) . . . . ?
C7 N1 C6 C2 172.5(4) . . . . ?
N1 C6 C2 C3 -2.1(7) . . . . ?
N1 C6 C2 C1 179.3(4) . . . . ?
C6 C2 C3 O6 -179.0(4) . . . . ?
C1 C2 C3 O6 -0.4(7) . . . . ?
C6 C2 C3 C4 1.7(6) . . . . ?
C1 C2 C3 C4 -179.8(4) . . . . ?
C5 C4 C3 O6 -179.8(4) . . . . ?
C10 C4 C3 O6 0.4(6) . . . . ?
C5 C4 C3 C2 -0.4(6) . . . . ?
C10 C4 C3 C2 179.8(4) . . . . ?
C6 C2 C1 O5 -0.6(6) . . . . ?
C3 C2 C1 O5 -179.2(4) . . . . ?
C6 C2 C1 O4 177.4(4) . . . . ?
C3 C2 C1 O4 -1.2(6) . . . . ?
C2 C3 O6 Eu2 -27.0(6) . . . . ?
C4 C3 O6 Eu2 152.3(3) . . . . ?
O4 Eu2 O6 C3 35.7(3) . . . . ?
O10 Eu2 O6 C3 150.5(3) . . . . ?
O7 Eu2 O6 C3 -13.0(4) . . . . ?
O1 Eu2 O6 C3 -120.8(3) . . . . ?
O9 Eu2 O6 C3 -159.1(3) . . . . ?
O3 Eu2 O6 C3 -47.5(3) . . . . ?
O12 Eu2 O6 C3 93.7(3) . . . . ?
O5 C1 O4 Eu2 -145.6(4) . . . . ?
C2 C1 O4 Eu2 36.5(6) . . . . ?
O10 Eu2 O4 C1 -112.8(4) . . . . ?
O7 Eu2 O4 C1 108.7(4) . . . . ?
O1 Eu2 O4 C1 -9.2(5) . . . . ?
O9 Eu2 O4 C1 152.4(3) . . . . ?
O3 Eu2 O4 C1 35.4(4) . . . . ?
O6 Eu2 O4 C1 -43.5(4) . . . . ?
O12 Eu2 O4 C1 -175.5(4) . . . . ?
C18 C26 C25 C24 2.4(7) . . . . ?
C18 C26 C25 Cl2 -179.6(4) . . . . ?
F2 C24 C25 C26 176.1(4) . . . . ?
C23 C24 C25 C26 -3.9(7) . . . . ?
F2 C24 C25 Cl2 -1.9(6) . . . . ?
C23 C24 C25 Cl2 178.1(4) . . . . ?
C15 C16 O3 Eu2 -33.2(6) . . . . ?
C17 C16 O3 Eu2 144.3(3) . . . . ?
O4 Eu2 O3 C16 -108.5(4) . . . . ?
O10 Eu2 O3 C16 -1.2(5) . . . . ?
O7 Eu2 O3 C16 165.0(4) . . . . ?
O1 Eu2 O3 C16 41.2(4) . . . . ?
O9 Eu2 O3 C16 105.1(4) . . . . ?
O6 Eu2 O3 C16 -36.5(4) . . . . ?
O12 Eu2 O3 C16 -160.0(3) . . . . ?
C6 N1 C7 C8 113.5(5) . . . . ?
C5 N1 C7 C8 -75.0(6) . . . . ?
C6 N1 C7 C9 41.2(6) . . . . ?
C5 N1 C7 C9 -147.3(4) . . . . ?
N1 C7 C9 C8 110.8(5) . . . . ?
N1 C7 C8 C9 -108.8(5) . . . . ?
F3 C37 C36 C30 179.2(4) . . . . ?
C38 C37 C36 C30 -1.2(7) . . . . ?
C37 C36 C30 C31 0.9(6) . . . . ?
C37 C36 C30 C29 179.6(4) . . . . ?
F3 C37 C38 C39 179.9(4) . . . . ?
C36 C37 C38 C39 0.3(7) . . . . ?
F3 C37 C38 Cl3 0.1(6) . . . . ?
C36 C37 C38 Cl3 -179.5(4) . . . . ?
C37 C38 C39 C31 0.9(7) . . . . ?
Cl3 C38 C39 C31 -179.4(3) . . . . ?
C38 C39 C31 N3 178.0(4) . . . . ?
C38 C39 C31 C30 -1.2(6) . . . . ?
C36 C30 C31 C39 0.3(6) . . . . ?
C29 C30 C31 C39 -178.4(4) . . . . ?
C36 C30 C31 N3 -179.0(4) . . . . ?
C29 C30 C31 N3 2.4(6) . . . . ?
C36 C30 C29 O9 1.2(6) . . . . ?
C31 C30 C29 O9 179.9(4) . . . . ?
C36 C30 C29 C28 -179.6(4) . . . . ?
C31 C30 C29 C28 -0.9(6) . . . . ?
C28 C29 O9 Eu2 -23.0(6) . . . . ?
C30 C29 O9 Eu2 156.2(3) . . . . ?
O4 Eu2 O9 C29 -13.6(4) . . . . ?
O10 Eu2 O9 C29 -118.1(4) . . . . ?
O7 Eu2 O9 C29 32.7(3) . . . . ?
O1 Eu2 O9 C29 153.7(4) . . . . ?
O3 Eu2 O9 C29 93.0(3) . . . . ?
O6 Eu2 O9 C29 -168.6(3) . . . . ?
O12 Eu2 O9 C29 -45.8(3) . . . . ?
O9 C29 C28 C32 178.9(4) . . . . ?
C30 C29 C28 C32 -0.3(6) . . . . ?
O9 C29 C28 C27 1.9(7) . . . . ?
C30 C29 C28 C27 -177.3(4) . . . . ?
C29 C28 C32 N3 0.0(7) . . . . ?
C27 C28 C32 N3 177.2(4) . . . . ?
C28 C32 N3 C31 1.6(7) . . . . ?
C28 C32 N3 C33 177.1(4) . . . . ?
C39 C31 N3 C32 178.1(4) . . . . ?
C30 C31 N3 C32 -2.7(6) . . . . ?
C39 C31 N3 C33 2.6(6) . . . . ?
C30 C31 N3 C33 -178.2(4) . . . . ?
C32 N3 C33 C35 45.1(6) . . . . ?
C31 N3 C33 C35 -139.5(4) . . . . ?
C32 N3 C33 C34 114.9(5) . . . . ?
C31 N3 C33 C34 -69.6(5) . . . . ?
C43 C49 C50 F4 179.6(4) . . . . ?
C43 C49 C50 C51 -0.3(7) . . . . ?
C51 C52 C44 N4 176.7(4) . . . . ?
C51 C52 C44 C43 -2.9(7) . . . . ?
C50 C49 C43 C44 -0.6(7) . . . . ?
C50 C49 C43 C42 -178.5(4) . . . . ?
N4 C44 C43 C49 -177.4(4) . . . . ?
C52 C44 C43 C49 2.3(6) . . . . ?
N4 C44 C43 C42 0.5(6) . . . . ?
C52 C44 C43 C42 -179.9(4) . . . . ?
O4 Eu2 O12 C42 156.9(3) . . . . ?
O10 Eu2 O12 C42 40.9(3) . . . . ?
O7 Eu2 O12 C42 -116.2(3) . . . . ?
O1 Eu2 O12 C42 -7.0(4) . . . . ?
O9 Eu2 O12 C42 -41.3(3) . . . . ?
O3 Eu2 O12 C42 -150.7(3) . . . . ?
O6 Eu2 O12 C42 101.6(3) . . . . ?
Eu2 O12 C42 C41 -31.9(6) . . . . ?
Eu2 O12 C42 C43 147.8(3) . . . . ?
C49 C43 C42 O12 -0.2(6) . . . . ?
C44 C43 C42 O12 -178.0(4) . . . . ?
C49 C43 C42 C41 179.5(4) . . . . ?
C44 C43 C42 C41 1.7(6) . . . . ?
C41 C45 N4 C44 2.6(7) . . . . ?
C41 C45 N4 C46 -179.8(4) . . . . ?
C52 C44 N4 C45 177.8(4) . . . . ?
C43 C44 N4 C45 -2.6(6) . . . . ?
C52 C44 N4 C46 0.1(6) . . . . ?
C43 C44 N4 C46 179.7(4) . . . . ?
N4 C45 C41 C42 -0.3(7) . . . . ?
N4 C45 C41 C40 179.5(4) . . . . ?
O12 C42 C41 C45 177.9(4) . . . . ?
C43 C42 C41 C45 -1.8(6) . . . . ?
O12 C42 C41 C40 -1.9(7) . . . . ?
C43 C42 C41 C40 178.4(4) . . . . ?
C45 C41 C40 O11 6.2(7) . . . . ?
C42 C41 C40 O11 -174.0(5) . . . . ?
C45 C41 C40 O10 -174.6(4) . . . . ?
C42 C41 C40 O10 5.2(7) . . . . ?
O11 C40 O10 Eu2 -148.7(4) . . . . ?
C41 C40 O10 Eu2 32.2(7) . . . . ?
O4 Eu2 O10 C40 -110.6(4) . . . . ?
O7 Eu2 O10 C40 -9.8(5) . . . . ?
O1 Eu2 O10 C40 110.9(4) . . . . ?
O9 Eu2 O10 C40 34.1(4) . . . . ?
O3 Eu2 O10 C40 150.4(4) . . . . ?
O6 Eu2 O10 C40 -174.6(5) . . . . ?
O12 Eu2 O10 C40 -43.8(4) . . . . ?
C44 C52 C51 C50 1.9(7) . . . . ?
C44 C52 C51 Cl4 -177.4(4) . . . . ?
F4 C50 C51 C52 179.7(4) . . . . ?
C49 C50 C51 C52 -0.3(8) . . . . ?
F4 C50 C51 Cl4 -0.9(7) . . . . ?
C49 C50 C51 Cl4 179.1(4) . . . . ?
O4 Eu2 O7 C27 110.0(4) . . . . ?
O10 Eu2 O7 C27 -0.2(5) . . . . ?
O1 Eu2 O7 C27 -110.8(4) . . . . ?
O9 Eu2 O7 C27 -45.6(4) . . . . ?
O3 Eu2 O7 C27 -169.4(4) . . . . ?
O6 Eu2 O7 C27 155.4(3) . . . . ?
O12 Eu2 O7 C27 32.9(4) . . . . ?
Eu2 O7 C27 O8 -134.6(4) . . . . ?
Eu2 O7 C27 C28 44.8(6) . . . . ?
C32 C28 C27 O8 -9.3(6) . . . . ?
C29 C28 C27 O8 167.8(4) . . . . ?
C32 C28 C27 O7 171.3(4) . . . . ?
C29 C28 C27 O7 -11.6(6) . . . . ?
C45 N4 C46 C48 38.0(7) . . . . ?
C44 N4 C46 C48 -144.4(4) . . . . ?
C45 N4 C46 C47 107.9(5) . . . . ?
C44 N4 C46 C47 -74.5(5) . . . . ?
N3 C33 C34 C35 -109.6(5) . . . . ?
N4 C46 C47 C48 -108.6(5) . . . . ?
N3 C33 C35 C34 107.8(5) . . . . ?
N4 C46 C48 C47 109.3(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.914
_refine_diff_density_rms         0.082

# start Validation Reply Form 
_vrf_PLAT415_1a                  
;
PROBLEM:  
RESPONSE: Because the disorder of H3WA and H1WA. 
;
_vrf_PLAT420_1a                  
;
PROBLEM:  
RESPONSE: Because the disorder of H1WA. 
;
_vrf_PLAT910_1a                  
;
PROBLEM:
RESPONSE: Theta min = 2.965 deg. The theta value of the missing reflections 
are less than 3.7460 deg. and therefore reflections were excluded. 
;
_vrf_PLAT973_1a                  
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature. 
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2b
_database_code_depnum_ccdc_archive 'CCDC 1855012'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H38 Cl4 F4 K N4 O15 Pr'
_chemical_formula_weight         1356.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8210 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0279(3)
_cell_length_b                   12.7769(4)
_cell_length_c                   22.0478(7)
_cell_angle_alpha                73.703(3)
_cell_angle_beta                 86.366(2)
_cell_angle_gamma                72.703(3)
_cell_volume                     2588.14(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10836
_cell_measurement_theta_min      3.5450
_cell_measurement_theta_max      29.0170

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7973
_exptl_absorpt_correction_T_max  0.8579
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19267
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9069
_reflns_number_gt                8226
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0286P)²+2.5206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9069
_refine_ls_number_parameters     751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0819
_refine_ls_wR_factor_gt          0.0795
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.12001(2) 0.490604(15) 0.257554(10) 0.02965(7) Uani 1 1 d . . .
Cl2 Cl 0.72211(10) -0.05611(10) 0.10754(6) 0.0609(3) Uani 1 1 d . . .
Cl3 Cl -0.41043(10) 0.81254(9) 0.54181(6) 0.0545(3) Uani 1 1 d . . .
Cl1 Cl -0.04586(12) 0.25441(10) -0.07042(6) 0.0616(3) Uani 1 1 d . . .
F2 F 0.7395(2) 0.1179(2) 0.16562(15) 0.0681(8) Uani 1 1 d . . .
F1 F -0.1969(2) 0.3316(2) 0.03399(14) 0.0689(8) Uani 1 1 d . . .
F4 F 0.3992(2) 0.8640(2) 0.33676(14) 0.0659(8) Uani 1 1 d . . .
F3 F -0.4475(2) 0.7084(2) 0.44509(12) 0.0564(7) Uani 1 1 d . . .
O1 O 0.3086(3) 0.5282(2) 0.18866(12) 0.0393(6) Uani 1 1 d . . .
O3 O 0.0848(2) 0.4660(2) 0.15442(12) 0.0382(6) Uani 1 1 d . . .
O2 O 0.5095(3) 0.4643(3) 0.14413(16) 0.0592(9) Uani 1 1 d . . .
O10 O -0.1146(3) 0.6201(2) 0.22648(13) 0.0435(7) Uani 1 1 d . . .
O4 O 0.0036(3) 0.3454(2) 0.28400(14) 0.0434(7) Uani 1 1 d . . .
O11 O 0.1130(3) 0.6866(2) 0.24715(15) 0.0500(8) Uani 1 1 d . . .
O8 O 0.4208(3) 0.4842(3) 0.40392(16) 0.0625(9) Uani 1 1 d . . .
O12 O -0.3225(3) 0.7343(2) 0.24093(19) 0.0686(10) Uani 1 1 d . . .
O5 O -0.1016(3) 0.2263(3) 0.26753(19) 0.0730(11) Uani 1 1 d . . .
O9 O 0.0026(2) 0.5265(2) 0.35710(12) 0.0348(6) Uani 1 1 d . . .
O7 O 0.2869(3) 0.4552(2) 0.33867(14) 0.0486(7) Uani 1 1 d . . .
O6 O 0.2871(2) 0.29568(19) 0.25560(13) 0.0372(6) Uani 1 1 d . . .
N3 N 0.1040(3) 0.6481(2) 0.49612(15) 0.0320(7) Uani 1 1 d . . .
N1 N 0.3427(3) 0.3553(2) 0.01961(15) 0.0367(7) Uani 1 1 d . . .
N2 N 0.2173(3) 0.0585(2) 0.17849(15) 0.0329(7) Uani 1 1 d . . .
N4 N -0.1652(3) 0.9282(2) 0.31759(16) 0.0374(8) Uani 1 1 d . . .
C7 C 0.0198(4) 0.3040(3) -0.0172(2) 0.0412(10) Uani 1 1 d . . .
C3 C 0.1682(4) 0.4345(3) 0.11386(17) 0.0315(8) Uani 1 1 d . . .
C9 C 0.2055(4) 0.3510(3) 0.02208(17) 0.0312(8) Uani 1 1 d . . .
C10 C 0.4350(4) 0.3195(4) -0.0293(2) 0.0447(10) Uani 1 1 d . . .
H10 H 0.4192 0.3732 -0.0716 0.054 Uiso 1 1 calc R . .
C5 C -0.0179(4) 0.3798(3) 0.07265(19) 0.0393(9) Uani 1 1 d . . .
H5 H -0.0763 0.4029 0.1039 0.047 Uiso 1 1 calc R . .
C13 C 0.3875(4) 0.3982(3) 0.06110(18) 0.0361(9) Uani 1 1 d . . .
H13 H 0.4794 0.4009 0.0579 0.043 Uiso 1 1 calc R . .
C8 C 0.1536(4) 0.3108(3) -0.02201(19) 0.0389(9) Uani 1 1 d . . .
H8 H 0.2099 0.2891 -0.0541 0.047 Uiso 1 1 calc R . .
C6 C -0.0646(4) 0.3386(3) 0.0303(2) 0.0427(10) Uani 1 1 d . . .
C29 C 0.0380(3) 0.5633(3) 0.39897(16) 0.0274(7) Uani 1 1 d . . .
C20 C 0.5884(4) 0.0213(3) 0.1446(2) 0.0414(9) Uani 1 1 d . . .
C48 C -0.0233(4) 0.9108(3) 0.32413(19) 0.0341(8) Uani 1 1 d . . .
C28 C 0.1782(3) 0.5515(3) 0.41490(17) 0.0297(8) Uani 1 1 d . . .
C35 C -0.0359(3) 0.6644(3) 0.48335(17) 0.0285(8) Uani 1 1 d . . .
C19 C 0.6105(4) 0.1027(3) 0.1703(2) 0.0422(10) Uani 1 1 d . . .
C39 C 0.2031(4) 0.5931(3) 0.46307(18) 0.0337(8) Uani 1 1 d . . .
H39 H 0.2957 0.5821 0.4734 0.040 Uiso 1 1 calc R . .
C26 C 0.1164(4) 0.1208(3) 0.20754(19) 0.0356(9) Uani 1 1 d . . .
H26 H 0.0291 0.1086 0.2092 0.043 Uiso 1 1 calc R . .
C18 C 0.5079(4) 0.1666(3) 0.19880(19) 0.0384(9) Uani 1 1 d . . .
H18 H 0.5263 0.2202 0.2155 0.046 Uiso 1 1 calc R . .
C1 C 0.3810(4) 0.4800(3) 0.15010(18) 0.0345(8) Uani 1 1 d . . .
C23 C 0.1905(4) -0.0237(3) 0.1497(2) 0.0404(10) Uani 1 1 d . . .
H23 H 0.2312 -0.1042 0.1723 0.048 Uiso 1 1 calc R . .
C52 C -0.2093(4) 0.8628(3) 0.28981(19) 0.0379(9) Uani 1 1 d . . .
H52 H -0.3052 0.8768 0.2858 0.046 Uiso 1 1 calc R . .
C30 C -0.0702(3) 0.6227(3) 0.43555(16) 0.0268(7) Uani 1 1 d . . .
C4 C 0.1199(4) 0.3872(3) 0.06869(17) 0.0309(8) Uani 1 1 d . . .
C22 C 0.3504(3) 0.0713(3) 0.17664(18) 0.0320(8) Uani 1 1 d . . .
C17 C 0.3738(3) 0.1523(3) 0.20327(17) 0.0295(8) Uani 1 1 d . . .
C27 C 0.3049(4) 0.4935(3) 0.38357(19) 0.0363(9) Uani 1 1 d . . .
C14 C 0.0009(4) 0.2618(3) 0.2641(2) 0.0415(10) Uani 1 1 d . . .
C21 C 0.4596(4) 0.0044(3) 0.14845(19) 0.0386(9) Uani 1 1 d . . .
H21 H 0.4443 -0.0512 0.1325 0.046 Uiso 1 1 calc R . .
C2 C 0.3096(4) 0.4380(3) 0.10736(17) 0.0319(8) Uani 1 1 d . . .
C36 C 0.1439(4) 0.6773(3) 0.5507(2) 0.0436(10) Uani 1 1 d . . .
H36 H 0.1336 0.6268 0.5922 0.052 Uiso 1 1 calc R . .
C40 C -0.1928(4) 0.7057(3) 0.2424(2) 0.0414(9) Uani 1 1 d . . .
C43 C 0.0711(4) 0.8290(3) 0.29922(18) 0.0335(8) Uani 1 1 d . . .
C44 C 0.2147(4) 0.8129(3) 0.3043(2) 0.0414(10) Uani 1 1 d . . .
H44 H 0.2782 0.7590 0.2877 0.050 Uiso 1 1 calc R . .
C41 C -0.1243(4) 0.7771(3) 0.26684(19) 0.0358(9) Uani 1 1 d . . .
C51 C -0.3991(4) 1.0128(3) 0.3627(2) 0.0500(11) Uani 1 1 d . . .
H51A H -0.4169 0.9398 0.3693 0.060 Uiso 1 1 calc R . .
H51B H -0.4809 1.0786 0.3513 0.060 Uiso 1 1 calc R . .
C38 C 0.2631(4) 0.7241(4) 0.5450(2) 0.0553(12) Uani 1 1 d . . .
H38A H 0.3091 0.7362 0.5047 0.066 Uiso 1 1 calc R . .
H38B H 0.3242 0.7014 0.5817 0.066 Uiso 1 1 calc R . .
C45 C 0.2608(4) 0.8764(3) 0.3336(2) 0.0428(10) Uani 1 1 d . . .
C47 C 0.0270(4) 0.9736(3) 0.3553(2) 0.0412(9) Uani 1 1 d . . .
H47 H -0.0351 1.0272 0.3726 0.049 Uiso 1 1 calc R . .
C50 C -0.2886(4) 1.0182(3) 0.4030(2) 0.0499(11) Uani 1 1 d . . .
H50A H -0.3033 1.0874 0.4159 0.060 Uiso 1 1 calc R . .
H50B H -0.2392 0.9486 0.4339 0.060 Uiso 1 1 calc R . .
C46 C 0.1683(4) 0.9556(3) 0.3602(2) 0.0431(10) Uani 1 1 d . . .
C12 C 0.5818(4) 0.2508(4) -0.0121(3) 0.0630(13) Uani 1 1 d . . .
H12A H 0.6117 0.2318 0.0316 0.076 Uiso 1 1 calc R . .
H12B H 0.6528 0.2641 -0.0428 0.076 Uiso 1 1 calc R . .
C25 C 0.0552(5) 0.0043(4) 0.1170(3) 0.0712(16) Uani 1 1 d . . .
H25A H 0.0143 -0.0571 0.1207 0.085 Uiso 1 1 calc R . .
H25B H -0.0117 0.0779 0.1151 0.085 Uiso 1 1 calc R . .
C11 C 0.4812(4) 0.1955(4) -0.0269(2) 0.0583(13) Uani 1 1 d . . .
H11A H 0.4495 0.1433 0.0079 0.070 Uiso 1 1 calc R . .
H11B H 0.4907 0.1757 -0.0666 0.070 Uiso 1 1 calc R . .
C42 C 0.0228(4) 0.7587(3) 0.26887(19) 0.0371(9) Uani 1 1 d . . .
C33 C -0.2787(4) 0.7368(3) 0.50308(19) 0.0363(9) Uani 1 1 d . . .
C15 C 0.1306(4) 0.2009(3) 0.23501(18) 0.0322(8) Uani 1 1 d . . .
C16 C 0.2624(4) 0.2224(3) 0.23353(17) 0.0306(8) Uani 1 1 d . . .
C31 C -0.2114(3) 0.6381(3) 0.42318(17) 0.0316(8) Uani 1 1 d . . .
H31 H -0.2358 0.6102 0.3921 0.038 Uiso 1 1 calc R . .
C32 C -0.3128(4) 0.6938(3) 0.45666(19) 0.0360(9) Uani 1 1 d . . .
C34 C -0.1421(4) 0.7209(3) 0.51739(18) 0.0344(8) Uani 1 1 d . . .
H34 H -0.1198 0.7473 0.5495 0.041 Uiso 1 1 calc R . .
C24 C 0.1842(4) 0.0027(4) 0.0797(2) 0.0525(11) Uani 1 1 d . . .
H24A H 0.1960 0.0753 0.0552 0.063 Uiso 1 1 calc R . .
H24B H 0.2220 -0.0598 0.0608 0.063 Uiso 1 1 calc R . .
C49 C -0.2642(4) 1.0249(3) 0.3347(2) 0.0406(10) Uani 1 1 d . . .
H49 H -0.2670 1.1004 0.3070 0.049 Uiso 1 1 calc R . .
C37 C 0.1178(4) 0.7978(4) 0.5482(3) 0.0605(13) Uani 1 1 d . . .
H37A H 0.0907 0.8199 0.5869 0.073 Uiso 1 1 calc R . .
H37B H 0.0756 0.8547 0.5098 0.073 Uiso 1 1 calc R . .
O2W O 0.5429(3) 0.3104(3) 0.31255(16) 0.0661(9) Uani 1 1 d . . .
H2WA H 0.5871 0.2400 0.3197 0.099 Uiso 0.60 1 d PR A 1
H2WB H 0.4704 0.3188 0.2916 0.099 Uiso 0.60 1 d PR A 1
H2WC H 0.5668 0.2407 0.3128 0.099 Uiso 0.40 1 d PR A 2
H2WD H 0.4796 0.3431 0.2839 0.099 Uiso 0.40 1 d PR A 2
O1W O 0.6224(4) 0.5388(4) 0.3256(2) 0.1067(15) Uani 1 1 d . . .
H1WA H 0.6597 0.5927 0.3177 0.160 Uiso 0.60 1 d PR B 1
H1WB H 0.6507 0.4995 0.3629 0.160 Uiso 0.60 1 d PR B 1
H1WC H 0.6495 0.5953 0.3047 0.160 Uiso 0.40 1 d PR B 2
H1WD H 0.6405 0.5319 0.3639 0.160 Uiso 0.40 1 d PR B 2
Cl4 Cl 0.23288(12) 1.03192(11) 0.39834(7) 0.0674(4) Uani 1 1 d . . .
O3W O -0.5683(4) 0.7218(3) 0.18120(19) 0.0734(10) Uani 1 1 d G . .
H3WA H -0.4944 0.7106 0.2020 0.110 Uiso 1 1 d G C 4
H3WB H -0.5882 0.6591 0.1938 0.110 Uiso 1 1 d G D 4
K1 K 0.6986(2) 0.4380(2) 0.24017(11) 0.0820(7) Uani 0.60 1 d P E 1
K1' K 0.7367(8) 0.3886(6) 0.2761(4) 0.088(2) Uani 0.20 1 d P . 2
K1'' K 0.7491(7) 0.5231(10) 0.1665(4) 0.136(4) Uani 0.20 1 d P . 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O7 2.383(3) . ?
Pr1 O4 2.396(2) . ?
Pr1 O1 2.425(2) . ?
Pr1 O11 2.429(2) . ?
Pr1 O3 2.442(2) . ?
Pr1 O10 2.449(2) . ?
Pr1 O9 2.516(2) . ?
Pr1 O6 2.566(2) . ?
Cl2 C20 1.723(4) . ?
Cl3 C33 1.724(4) . ?
Cl1 C7 1.725(4) . ?
F2 C19 1.358(4) . ?
F1 C6 1.351(4) . ?
F4 C45 1.353(4) . ?
F3 C32 1.339(4) . ?
O1 C1 1.257(4) . ?
O3 C3 1.252(4) . ?
O2 C1 1.248(4) . ?
O10 C40 1.267(4) . ?
O10 K1'' 2.703(8) 1_455 ?
O4 C14 1.271(4) . ?
O4 K1' 2.574(8) 1_455 ?
O11 C42 1.262(4) . ?
O8 C27 1.233(4) . ?
O12 C40 1.241(5) . ?
O5 C14 1.230(4) . ?
O5 K1' 2.268(7) 1_455 ?
O9 C29 1.259(4) . ?
O7 C27 1.265(4) . ?
O6 C16 1.258(4) . ?
N3 C39 1.339(4) . ?
N3 C35 1.391(4) . ?
N3 C36 1.466(5) . ?
N1 C13 1.349(4) . ?
N1 C9 1.391(4) . ?
N1 C10 1.459(5) . ?
N2 C26 1.339(4) . ?
N2 C22 1.389(4) . ?
N2 C23 1.463(4) . ?
N4 C52 1.345(5) . ?
N4 C48 1.384(4) . ?
N4 C49 1.462(4) . ?
C7 C8 1.366(5) . ?
C7 C6 1.389(6) . ?
C3 C2 1.429(5) . ?
C3 C4 1.471(5) . ?
C9 C4 1.388(5) . ?
C9 C8 1.408(5) . ?
C10 C12 1.483(6) . ?
C10 C11 1.500(6) . ?
C5 C6 1.360(5) . ?
C5 C4 1.408(5) . ?
C13 C2 1.365(5) . ?
C29 C28 1.425(5) . ?
C29 C30 1.465(5) . ?
C20 C21 1.365(5) . ?
C20 C19 1.391(5) . ?
C48 C47 1.401(5) . ?
C48 C43 1.400(5) . ?
C28 C39 1.379(5) . ?
C28 C27 1.502(5) . ?
C35 C34 1.401(5) . ?
C35 C30 1.408(5) . ?
C19 C18 1.351(5) . ?
C26 C15 1.371(5) . ?
C18 C17 1.404(5) . ?
C1 C2 1.513(5) . ?
C23 C25 1.476(6) . ?
C23 C24 1.487(6) . ?
C52 C41 1.372(5) . ?
C30 C31 1.404(5) . ?
C22 C17 1.405(5) . ?
C22 C21 1.404(5) . ?
C17 C16 1.463(5) . ?
C14 C15 1.510(5) . ?
C36 C38 1.472(5) . ?
C36 C37 1.468(5) . ?
C40 C41 1.514(5) . ?
C43 C44 1.400(5) . ?
C43 C42 1.457(5) . ?
C44 C45 1.358(5) . ?
C41 C42 1.425(5) . ?
C51 C49 1.483(5) . ?
C51 C50 1.493(6) . ?
C38 C37 1.491(6) . ?
C45 C46 1.391(5) . ?
C47 C46 1.373(5) . ?
C50 C49 1.493(6) . ?
C46 Cl4 1.727(4) . ?
C12 C11 1.489(6) . ?
C25 C24 1.487(6) . ?
C33 C34 1.367(5) . ?
C33 C32 1.392(5) . ?
C15 C16 1.425(5) . ?
C31 C32 1.362(5) . ?
O2W K1' 2.434(8) . ?
O1W K1' 2.429(8) . ?
O1W K1 2.527(5) . ?
K1' O5 2.268(7) 1_655 ?
K1' O4 2.574(8) 1_655 ?
K1'' O10 2.703(8) 1_655 ?

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
O7 Pr1 O4 109.58(10) . . ?
O7 Pr1 O1 83.02(9) . . ?
O4 Pr1 O1 135.49(8) . . ?
O7 Pr1 O11 81.58(10) . . ?
O4 Pr1 O11 148.89(8) . . ?
O1 Pr1 O11 73.26(8) . . ?
O7 Pr1 O3 145.14(8) . . ?
O4 Pr1 O3 77.55(9) . . ?
O1 Pr1 O3 70.29(8) . . ?
O11 Pr1 O3 110.31(10) . . ?
O7 Pr1 O10 135.95(8) . . ?
O4 Pr1 O10 84.19(9) . . ?
O1 Pr1 O10 116.76(9) . . ?
O11 Pr1 O10 69.03(9) . . ?
O3 Pr1 O10 77.69(8) . . ?
O7 Pr1 O9 68.62(8) . . ?
O4 Pr1 O9 80.26(8) . . ?
O1 Pr1 O9 141.47(8) . . ?
O11 Pr1 O9 77.12(9) . . ?
O3 Pr1 O9 144.84(8) . . ?
O10 Pr1 O9 73.21(8) . . ?
O7 Pr1 O6 77.43(8) . . ?
O4 Pr1 O6 68.44(8) . . ?
O1 Pr1 O6 73.50(8) . . ?
O11 Pr1 O6 142.41(8) . . ?
O3 Pr1 O6 73.82(8) . . ?
O10 Pr1 O6 143.87(8) . . ?
O9 Pr1 O6 121.93(8) . . ?
C1 O1 Pr1 133.6(2) . . ?
C3 O3 Pr1 132.5(2) . . ?
C40 O10 Pr1 135.1(2) . . ?
C40 O10 K1'' 114.0(3) . 1_455 ?
Pr1 O10 K1'' 108.9(2) . 1_455 ?
C14 O4 Pr1 137.0(2) . . ?
C14 O4 K1' 81.8(3) . 1_455 ?
Pr1 O4 K1' 123.23(18) . 1_455 ?
C42 O11 Pr1 127.3(2) . . ?
C14 O5 K1' 96.7(3) . 1_455 ?
C29 O9 Pr1 131.5(2) . . ?
C27 O7 Pr1 140.2(2) . . ?
C16 O6 Pr1 127.2(2) . . ?
C39 N3 C35 119.6(3) . . ?
C39 N3 C36 119.7(3) . . ?
C35 N3 C36 120.2(3) . . ?
C13 N1 C9 119.2(3) . . ?
C13 N1 C10 120.3(3) . . ?
C9 N1 C10 120.5(3) . . ?
C26 N2 C22 119.0(3) . . ?
C26 N2 C23 121.3(3) . . ?
C22 N2 C23 119.6(3) . . ?
C52 N4 C48 119.3(3) . . ?
C52 N4 C49 121.0(3) . . ?
C48 N4 C49 119.4(3) . . ?
C8 C7 C6 120.0(3) . . ?
C8 C7 Cl1 120.3(3) . . ?
C6 C7 Cl1 119.7(3) . . ?
O3 C3 C2 126.1(3) . . ?
O3 C3 C4 118.4(3) . . ?
C2 C3 C4 115.5(3) . . ?
N1 C9 C4 119.0(3) . . ?
N1 C9 C8 120.7(3) . . ?
C4 C9 C8 120.3(3) . . ?
N1 C10 C12 119.1(4) . . ?
N1 C10 C11 118.4(3) . . ?
C12 C10 C11 59.9(3) . . ?
C6 C5 C4 119.3(4) . . ?
N1 C13 C2 125.6(3) . . ?
C7 C8 C9 119.4(4) . . ?
F1 C6 C5 119.3(4) . . ?
F1 C6 C7 119.0(3) . . ?
C5 C6 C7 121.7(3) . . ?
O9 C29 C28 125.1(3) . . ?
O9 C29 C30 119.3(3) . . ?
C28 C29 C30 115.6(3) . . ?
C21 C20 C19 119.4(3) . . ?
C21 C20 Cl2 120.5(3) . . ?
C19 C20 Cl2 120.1(3) . . ?
N4 C48 C47 121.1(3) . . ?
N4 C48 C43 119.2(3) . . ?
C47 C48 C43 119.7(3) . . ?
C39 C28 C29 119.3(3) . . ?
C39 C28 C27 116.2(3) . . ?
C29 C28 C27 124.5(3) . . ?
N3 C35 C34 121.0(3) . . ?
N3 C35 C30 119.0(3) . . ?
C34 C35 C30 120.0(3) . . ?
C18 C19 F2 119.8(3) . . ?
C18 C19 C20 122.1(3) . . ?
F2 C19 C20 118.1(3) . . ?
N3 C39 C28 124.9(3) . . ?
N2 C26 C15 125.7(3) . . ?
C19 C18 C17 120.3(3) . . ?
O1 C1 O2 124.5(3) . . ?
O1 C1 C2 118.7(3) . . ?
O2 C1 C2 116.8(3) . . ?
N2 C23 C25 119.3(3) . . ?
N2 C23 C24 119.1(3) . . ?
C25 C23 C24 60.2(3) . . ?
N4 C52 C41 125.4(3) . . ?
C31 C30 C35 119.0(3) . . ?
C31 C30 C29 119.6(3) . . ?
C35 C30 C29 121.4(3) . . ?
C9 C4 C5 119.3(3) . . ?
C9 C4 C3 121.9(3) . . ?
C5 C4 C3 118.8(3) . . ?
N2 C22 C17 119.0(3) . . ?
N2 C22 C21 120.4(3) . . ?
C17 C22 C21 120.6(3) . . ?
C22 C17 C18 117.9(3) . . ?
C22 C17 C16 121.8(3) . . ?
C18 C17 C16 120.2(3) . . ?
O8 C27 O7 123.7(3) . . ?
O8 C27 C28 118.0(3) . . ?
O7 C27 C28 118.3(3) . . ?
O5 C14 O4 123.8(3) . . ?
O5 C14 C15 117.4(3) . . ?
O4 C14 C15 118.8(3) . . ?
C20 C21 C22 119.7(3) . . ?
C13 C2 C3 118.7(3) . . ?
C13 C2 C1 117.3(3) . . ?
C3 C2 C1 124.0(3) . . ?
N3 C36 C38 118.6(4) . . ?
N3 C36 C37 119.3(4) . . ?
C38 C36 C37 61.0(3) . . ?
O12 C40 O10 124.9(4) . . ?
O12 C40 C41 117.0(3) . . ?
O10 C40 C41 118.1(3) . . ?
C44 C43 C48 119.5(3) . . ?
C44 C43 C42 119.2(3) . . ?
C48 C43 C42 121.2(3) . . ?
C45 C44 C43 119.7(3) . . ?
C52 C41 C42 118.3(3) . . ?
C52 C41 C40 117.7(3) . . ?
C42 C41 C40 123.9(3) . . ?
C49 C51 C50 60.2(3) . . ?
C36 C38 C37 59.4(3) . . ?
C44 C45 F4 119.9(3) . . ?
C44 C45 C46 121.3(3) . . ?
F4 C45 C46 118.7(4) . . ?
C46 C47 C48 119.7(3) . . ?
C49 C50 C51 59.6(3) . . ?
C47 C46 C45 120.0(4) . . ?
C47 C46 Cl4 120.6(3) . . ?
C45 C46 Cl4 119.4(3) . . ?
C10 C12 C11 60.6(3) . . ?
C24 C25 C23 60.2(3) . . ?
C12 C11 C10 59.5(3) . . ?
O11 C42 C41 125.3(3) . . ?
O11 C42 C43 118.3(3) . . ?
C41 C42 C43 116.4(3) . . ?
C34 C33 C32 120.6(3) . . ?
C34 C33 Cl3 120.0(3) . . ?
C32 C33 Cl3 119.4(3) . . ?
C26 C15 C16 119.2(3) . . ?
C26 C15 C14 116.1(3) . . ?
C16 C15 C14 124.8(3) . . ?
O6 C16 C15 125.0(3) . . ?
O6 C16 C17 119.8(3) . . ?
C15 C16 C17 115.3(3) . . ?
C32 C31 C30 120.0(3) . . ?
F3 C32 C31 120.1(3) . . ?
F3 C32 C33 118.9(3) . . ?
C31 C32 C33 120.9(3) . . ?
C33 C34 C35 119.6(3) . . ?
C25 C24 C23 59.5(3) . . ?
N4 C49 C51 119.3(3) . . ?
N4 C49 C50 118.9(3) . . ?
C51 C49 C50 60.2(3) . . ?
C36 C37 C38 59.6(3) . . ?
K1' O1W K1 20.49(19) . . ?
O5 K1' O1W 155.7(5) 1_655 . ?
O5 K1' O2W 98.6(3) 1_655 . ?
O1W K1' O2W 86.6(2) . . ?
O5 K1' O4 53.79(17) 1_655 1_655 ?
O1W K1' O4 109.9(4) . 1_655 ?
O2W K1' O4 143.6(3) . 1_655 ?

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
O7 Pr1 O1 C1 114.5(3) . . . . ?
O4 Pr1 O1 C1 3.5(4) . . . . ?
O11 Pr1 O1 C1 -162.3(4) . . . . ?
O3 Pr1 O1 C1 -42.8(3) . . . . ?
O10 Pr1 O1 C1 -107.0(3) . . . . ?
O9 Pr1 O1 C1 156.4(3) . . . . ?
O6 Pr1 O1 C1 35.5(3) . . . . ?
O7 Pr1 O3 C3 -11.4(4) . . . . ?
O4 Pr1 O3 C3 -117.9(3) . . . . ?
O1 Pr1 O3 C3 30.8(3) . . . . ?
O11 Pr1 O3 C3 93.5(3) . . . . ?
O10 Pr1 O3 C3 155.4(3) . . . . ?
O9 Pr1 O3 C3 -170.0(3) . . . . ?
O6 Pr1 O3 C3 -47.0(3) . . . . ?
O7 Pr1 O10 C40 9.8(4) . . . . ?
O4 Pr1 O10 C40 122.1(4) . . . . ?
O1 Pr1 O10 C40 -99.2(4) . . . . ?
O11 Pr1 O10 C40 -41.8(4) . . . . ?
O3 Pr1 O10 C40 -159.4(4) . . . . ?
O9 Pr1 O10 C40 40.5(3) . . . . ?
O6 Pr1 O10 C40 162.1(3) . . . . ?
O7 Pr1 O10 K1'' -152.9(2) . . . 1_455 ?
O4 Pr1 O10 K1'' -40.6(2) . . . 1_455 ?
O1 Pr1 O10 K1'' 98.1(2) . . . 1_455 ?
O11 Pr1 O10 K1'' 155.5(3) . . . 1_455 ?
O3 Pr1 O10 K1'' 37.9(2) . . . 1_455 ?
O9 Pr1 O10 K1'' -122.2(2) . . . 1_455 ?
O6 Pr1 O10 K1'' -0.6(3) . . . 1_455 ?
O7 Pr1 O4 C14 -109.9(4) . . . . ?
O1 Pr1 O4 C14 -9.7(4) . . . . ?
O11 Pr1 O4 C14 143.3(4) . . . . ?
O3 Pr1 O4 C14 34.5(4) . . . . ?
O10 Pr1 O4 C14 113.2(4) . . . . ?
O9 Pr1 O4 C14 -172.9(4) . . . . ?
O6 Pr1 O4 C14 -42.8(4) . . . . ?
O7 Pr1 O4 K1' 133.1(3) . . . 1_455 ?
O1 Pr1 O4 K1' -126.7(3) . . . 1_455 ?
O11 Pr1 O4 K1' 26.3(4) . . . 1_455 ?
O3 Pr1 O4 K1' -82.5(3) . . . 1_455 ?
O10 Pr1 O4 K1' -3.8(3) . . . 1_455 ?
O9 Pr1 O4 K1' 70.1(3) . . . 1_455 ?
O6 Pr1 O4 K1' -159.8(3) . . . 1_455 ?
O7 Pr1 O11 C42 -99.9(3) . . . . ?
O4 Pr1 O11 C42 14.3(5) . . . . ?
O1 Pr1 O11 C42 174.9(4) . . . . ?
O3 Pr1 O11 C42 114.0(3) . . . . ?
O10 Pr1 O11 C42 46.6(3) . . . . ?
O9 Pr1 O11 C42 -30.1(3) . . . . ?
O6 Pr1 O11 C42 -156.4(3) . . . . ?
O7 Pr1 O9 C29 33.2(3) . . . . ?
O4 Pr1 O9 C29 148.8(3) . . . . ?
O1 Pr1 O9 C29 -12.3(3) . . . . ?
O11 Pr1 O9 C29 -52.7(3) . . . . ?
O3 Pr1 O9 C29 -159.8(3) . . . . ?
O10 Pr1 O9 C29 -124.4(3) . . . . ?
O6 Pr1 O9 C29 91.9(3) . . . . ?
O4 Pr1 O7 C27 -107.0(4) . . . . ?
O1 Pr1 O7 C27 117.1(4) . . . . ?
O11 Pr1 O7 C27 43.0(4) . . . . ?
O3 Pr1 O7 C27 156.7(4) . . . . ?
O10 Pr1 O7 C27 -4.6(5) . . . . ?
O9 Pr1 O7 C27 -36.3(4) . . . . ?
O6 Pr1 O7 C27 -168.3(4) . . . . ?
O7 Pr1 O6 C16 159.1(3) . . . . ?
O4 Pr1 O6 C16 41.9(3) . . . . ?
O1 Pr1 O6 C16 -114.5(3) . . . . ?
O11 Pr1 O6 C16 -143.3(3) . . . . ?
O3 Pr1 O6 C16 -40.8(3) . . . . ?
O10 Pr1 O6 C16 -1.5(4) . . . . ?
O9 Pr1 O6 C16 104.5(3) . . . . ?
Pr1 O3 C3 C2 -21.8(5) . . . . ?
Pr1 O3 C3 C4 157.0(2) . . . . ?
C13 N1 C9 C4 -2.3(5) . . . . ?
C10 N1 C9 C4 -179.1(3) . . . . ?
C13 N1 C9 C8 177.6(3) . . . . ?
C10 N1 C9 C8 0.8(5) . . . . ?
C13 N1 C10 C12 44.9(5) . . . . ?
C9 N1 C10 C12 -138.3(4) . . . . ?
C13 N1 C10 C11 114.4(4) . . . . ?
C9 N1 C10 C11 -68.9(5) . . . . ?
C9 N1 C13 C2 0.8(6) . . . . ?
C10 N1 C13 C2 177.6(4) . . . . ?
C6 C7 C8 C9 1.2(6) . . . . ?
Cl1 C7 C8 C9 -179.7(3) . . . . ?
N1 C9 C8 C7 177.9(3) . . . . ?
C4 C9 C8 C7 -2.3(5) . . . . ?
C4 C5 C6 F1 -179.9(3) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C8 C7 C6 F1 179.7(4) . . . . ?
Cl1 C7 C6 F1 0.6(5) . . . . ?
C8 C7 C6 C5 0.1(6) . . . . ?
Cl1 C7 C6 C5 -179.0(3) . . . . ?
Pr1 O9 C29 C28 -27.4(5) . . . . ?
Pr1 O9 C29 C30 153.1(2) . . . . ?
C52 N4 C48 C47 -177.1(3) . . . . ?
C49 N4 C48 C47 9.4(5) . . . . ?
C52 N4 C48 C43 2.7(5) . . . . ?
C49 N4 C48 C43 -170.7(3) . . . . ?
O9 C29 C28 C39 -178.2(3) . . . . ?
C30 C29 C28 C39 1.3(5) . . . . ?
O9 C29 C28 C27 0.3(5) . . . . ?
C30 C29 C28 C27 179.8(3) . . . . ?
C39 N3 C35 C34 179.6(3) . . . . ?
C36 N3 C35 C34 7.5(5) . . . . ?
C39 N3 C35 C30 -0.2(5) . . . . ?
C36 N3 C35 C30 -172.2(3) . . . . ?
C21 C20 C19 C18 -0.4(7) . . . . ?
Cl2 C20 C19 C18 178.9(3) . . . . ?
C21 C20 C19 F2 -179.8(4) . . . . ?
Cl2 C20 C19 F2 -0.5(6) . . . . ?
C35 N3 C39 C28 1.4(5) . . . . ?
C36 N3 C39 C28 173.5(3) . . . . ?
C29 C28 C39 N3 -2.0(5) . . . . ?
C27 C28 C39 N3 179.4(3) . . . . ?
C22 N2 C26 C15 2.0(6) . . . . ?
C23 N2 C26 C15 -179.0(4) . . . . ?
F2 C19 C18 C17 179.3(4) . . . . ?
C20 C19 C18 C17 -0.1(6) . . . . ?
Pr1 O1 C1 O2 -138.7(3) . . . . ?
Pr1 O1 C1 C2 41.5(5) . . . . ?
C26 N2 C23 C25 37.8(6) . . . . ?
C22 N2 C23 C25 -143.3(4) . . . . ?
C26 N2 C23 C24 107.9(4) . . . . ?
C22 N2 C23 C24 -73.1(5) . . . . ?
C48 N4 C52 C41 0.4(6) . . . . ?
C49 N4 C52 C41 173.8(4) . . . . ?
N3 C35 C30 C31 179.3(3) . . . . ?
C34 C35 C30 C31 -0.4(5) . . . . ?
N3 C35 C30 C29 -0.3(5) . . . . ?
C34 C35 C30 C29 179.9(3) . . . . ?
O9 C29 C30 C31 -0.3(5) . . . . ?
C28 C29 C30 C31 -179.9(3) . . . . ?
O9 C29 C30 C35 179.3(3) . . . . ?
C28 C29 C30 C35 -0.3(5) . . . . ?
N1 C9 C4 C5 -178.1(3) . . . . ?
C8 C9 C4 C5 2.1(5) . . . . ?
N1 C9 C4 C3 2.6(5) . . . . ?
C8 C9 C4 C3 -177.2(3) . . . . ?
C6 C5 C4 C9 -0.7(5) . . . . ?
C6 C5 C4 C3 178.6(3) . . . . ?
O3 C3 C4 C9 179.6(3) . . . . ?
C2 C3 C4 C9 -1.4(5) . . . . ?
O3 C3 C4 C5 0.3(5) . . . . ?
C2 C3 C4 C5 179.3(3) . . . . ?
C26 N2 C22 C17 -2.4(5) . . . . ?
C23 N2 C22 C17 178.7(3) . . . . ?
C26 N2 C22 C21 177.8(4) . . . . ?
C23 N2 C22 C21 -1.2(5) . . . . ?
N2 C22 C17 C18 -177.7(3) . . . . ?
C21 C22 C17 C18 2.1(5) . . . . ?
N2 C22 C17 C16 0.8(5) . . . . ?
C21 C22 C17 C16 -179.4(3) . . . . ?
C19 C18 C17 C22 -0.8(6) . . . . ?
C19 C18 C17 C16 -179.3(4) . . . . ?
Pr1 O7 C27 O8 -153.2(3) . . . . ?
Pr1 O7 C27 C28 28.2(6) . . . . ?
C39 C28 C27 O8 2.0(5) . . . . ?
C29 C28 C27 O8 -176.5(4) . . . . ?
C39 C28 C27 O7 -179.2(3) . . . . ?
C29 C28 C27 O7 2.2(5) . . . . ?
K1' O5 C14 O4 21.8(5) 1_455 . . . ?
K1' O5 C14 C15 -158.8(4) 1_455 . . . ?
Pr1 O4 C14 O5 -150.4(3) . . . . ?
K1' O4 C14 O5 -19.2(5) 1_455 . . . ?
Pr1 O4 C14 C15 30.3(6) . . . . ?
K1' O4 C14 C15 161.5(4) 1_455 . . . ?
C19 C20 C21 C22 1.8(6) . . . . ?
Cl2 C20 C21 C22 -177.5(3) . . . . ?
N2 C22 C21 C20 177.2(4) . . . . ?
C17 C22 C21 C20 -2.7(6) . . . . ?
N1 C13 C2 C3 0.3(6) . . . . ?
N1 C13 C2 C1 178.5(3) . . . . ?
O3 C3 C2 C13 178.8(3) . . . . ?
C4 C3 C2 C13 -0.1(5) . . . . ?
O3 C3 C2 C1 0.8(6) . . . . ?
C4 C3 C2 C1 -178.1(3) . . . . ?
O1 C1 C2 C13 172.5(3) . . . . ?
O2 C1 C2 C13 -7.2(5) . . . . ?
O1 C1 C2 C3 -9.4(5) . . . . ?
O2 C1 C2 C3 170.9(3) . . . . ?
C39 N3 C36 C38 43.4(5) . . . . ?
C35 N3 C36 C38 -144.5(4) . . . . ?
C39 N3 C36 C37 114.3(4) . . . . ?
C35 N3 C36 C37 -73.7(5) . . . . ?
Pr1 O10 C40 O12 -150.7(3) . . . . ?
K1'' O10 C40 O12 11.3(6) 1_455 . . . ?
Pr1 O10 C40 C41 27.4(5) . . . . ?
K1'' O10 C40 C41 -170.5(4) 1_455 . . . ?
N4 C48 C43 C44 178.5(3) . . . . ?
C47 C48 C43 C44 -1.7(5) . . . . ?
N4 C48 C43 C42 -2.5(5) . . . . ?
C47 C48 C43 C42 177.4(3) . . . . ?
C48 C43 C44 C45 0.4(6) . . . . ?
C42 C43 C44 C45 -178.7(4) . . . . ?
N4 C52 C41 C42 -3.8(6) . . . . ?
N4 C52 C41 C40 174.6(3) . . . . ?
O12 C40 C41 C52 4.6(6) . . . . ?
O10 C40 C41 C52 -173.7(4) . . . . ?
O12 C40 C41 C42 -177.1(4) . . . . ?
O10 C40 C41 C42 4.6(6) . . . . ?
N3 C36 C38 C37 109.5(4) . . . . ?
C43 C44 C45 F4 -177.7(4) . . . . ?
C43 C44 C45 C46 1.5(6) . . . . ?
N4 C48 C47 C46 -179.0(4) . . . . ?
C43 C48 C47 C46 1.1(6) . . . . ?
C48 C47 C46 C45 0.7(6) . . . . ?
C48 C47 C46 Cl4 180.0(3) . . . . ?
C44 C45 C46 C47 -2.1(6) . . . . ?
F4 C45 C46 C47 177.1(4) . . . . ?
C44 C45 C46 Cl4 178.6(3) . . . . ?
F4 C45 C46 Cl4 -2.1(5) . . . . ?
N1 C10 C12 C11 107.8(4) . . . . ?
N2 C23 C25 C24 108.8(4) . . . . ?
N1 C10 C11 C12 -109.1(4) . . . . ?
Pr1 O11 C42 C41 -43.3(6) . . . . ?
Pr1 O11 C42 C43 136.1(3) . . . . ?
C52 C41 C42 O11 -176.9(4) . . . . ?
C40 C41 C42 O11 4.8(6) . . . . ?
C52 C41 C42 C43 3.8(5) . . . . ?
C40 C41 C42 C43 -174.6(3) . . . . ?
C44 C43 C42 O11 -1.1(5) . . . . ?
C48 C43 C42 O11 179.8(4) . . . . ?
C44 C43 C42 C41 178.3(3) . . . . ?
C48 C43 C42 C41 -0.8(5) . . . . ?
N2 C26 C15 C16 0.0(6) . . . . ?
N2 C26 C15 C14 179.0(4) . . . . ?
O5 C14 C15 C26 8.2(6) . . . . ?
O4 C14 C15 C26 -172.4(4) . . . . ?
O5 C14 C15 C16 -172.8(4) . . . . ?
O4 C14 C15 C16 6.6(6) . . . . ?
Pr1 O6 C16 C15 -34.3(5) . . . . ?
Pr1 O6 C16 C17 145.3(2) . . . . ?
C26 C15 C16 O6 178.1(3) . . . . ?
C14 C15 C16 O6 -0.8(6) . . . . ?
C26 C15 C16 C17 -1.6(5) . . . . ?
C14 C15 C16 C17 179.5(3) . . . . ?
C22 C17 C16 O6 -178.5(3) . . . . ?
C18 C17 C16 O6 0.0(5) . . . . ?
C22 C17 C16 C15 1.2(5) . . . . ?
C18 C17 C16 C15 179.7(3) . . . . ?
C35 C30 C31 C32 0.8(5) . . . . ?
C29 C30 C31 C32 -179.6(3) . . . . ?
C30 C31 C32 F3 -179.8(3) . . . . ?
C30 C31 C32 C33 0.4(5) . . . . ?
C34 C33 C32 F3 178.2(3) . . . . ?
Cl3 C33 C32 F3 -2.8(5) . . . . ?
C34 C33 C32 C31 -2.0(6) . . . . ?
Cl3 C33 C32 C31 177.0(3) . . . . ?
C32 C33 C34 C35 2.4(5) . . . . ?
Cl3 C33 C34 C35 -176.7(3) . . . . ?
N3 C35 C34 C33 179.1(3) . . . . ?
C30 C35 C34 C33 -1.1(5) . . . . ?
N2 C23 C24 C25 -109.0(4) . . . . ?
C52 N4 C49 C51 41.1(6) . . . . ?
C48 N4 C49 C51 -145.5(4) . . . . ?
C52 N4 C49 C50 111.2(4) . . . . ?
C48 N4 C49 C50 -75.5(4) . . . . ?
C50 C51 C49 N4 108.5(4) . . . . ?
C51 C50 C49 N4 -109.1(4) . . . . ?
N3 C36 C37 C38 -108.4(4) . . . . ?
K1 O1W K1' O5 157.4(14) . . . 1_655 ?
K1 O1W K1' O2W -99.2(7) . . . . ?
K1 O1W K1' O4 114.1(7) . . . 1_655 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.070

# start Validation Reply Form 
_vrf_PLAT415_2b                  
;
PROBLEM:  
RESPONSE: The disorder of H2WA. 
;
_vrf_PLAT420_2b                  
;
PROBLEM:  
RESPONSE: The disorder of H2WA and H2WB. 
;
_vrf_PLAT910_2b                  
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature. 
;
# end Validation Reply Form

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

data_1c
_database_code_depnum_ccdc_archive 'CCDC 1855011'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 Cl4 F4 N4 Na O16 Tb'
_chemical_formula_weight         1376.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1720 4.1540 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0564(2)
_cell_length_b                   12.7324(4)
_cell_length_c                   22.0394(7)
_cell_angle_alpha                73.580(3)
_cell_angle_beta                 85.371(2)
_cell_angle_gamma                72.185(2)
_cell_volume                     2577.03(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16556
_cell_measurement_theta_min      3.7580
_cell_measurement_theta_max      28.9510

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7407
_exptl_absorpt_correction_T_max  0.8635
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24978
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         25.01
_reflns_number_total             9007
_reflns_number_gt                8039
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0569P)²+0.3722P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9007
_refine_ls_number_parameters     751
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0955
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      4.450
_refine_ls_shift/su_max          0.020
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.62250(8) 0.48961(7) 0.25854(4) 0.0271(4) Uani 1 1 d . . .
Cl4 Cl 0.4598(6) 0.2524(5) -0.0647(3) 0.0556(15) Uani 1 1 d . . .
Cl2 Cl 0.0859(5) 0.8149(5) 0.5401(3) 0.0530(15) Uani 1 1 d . . .
Cl3 Cl 1.2220(5) -0.0637(6) 0.1108(3) 0.0591(16) Uani 1 1 d . . .
C11 C 0.2436(19) 1.0281(16) 0.3360(10) 0.038(5) Uani 1 1 d . . .
H11 H 0.2407 1.1038 0.3079 0.045 Uiso 1 1 calc R . .
Cl1 Cl 0.7371(6) 1.0409(6) 0.3962(3) 0.0651(17) Uani 1 1 d . . .
F4 F 0.3034(12) 0.3368(13) 0.0379(6) 0.063(4) Uani 1 1 d . . .
F3 F 1.2399(12) 0.1105(13) 0.1690(7) 0.064(4) Uani 1 1 d . . .
F1 F 0.9079(11) 0.8661(11) 0.3383(7) 0.060(4) Uani 1 1 d . . .
F2 F 0.0511(11) 0.7041(12) 0.4462(6) 0.056(4) Uani 1 1 d . . .
O10 O 0.3907(16) 0.2411(16) 0.2665(10) 0.081(6) Uani 1 1 d . . .
O11 O 0.5031(13) 0.3541(11) 0.2852(6) 0.041(3) Uani 1 1 d . . .
O12 O 0.7842(12) 0.3006(11) 0.2549(6) 0.035(3) Uani 1 1 d . . .
O13 O 0.8036(13) 0.5298(11) 0.1921(6) 0.036(3) Uani 1 1 d . . .
O14 O 1.0073(15) 0.4600(16) 0.1492(8) 0.063(5) Uani 1 1 d . . .
O17 O 0.1935(14) 0.7281(13) 0.2486(8) 0.056(4) Uani 1 1 d . . .
O18 O 0.4025(13) 0.6221(11) 0.2266(6) 0.038(3) Uani 1 1 d . . .
O19 O 0.9203(14) 0.4833(15) 0.3967(7) 0.056(4) Uani 1 1 d . . .
O20 O 0.7848(13) 0.4454(12) 0.3368(6) 0.042(3) Uani 1 1 d . . .
O21 O 0.5028(12) 0.5216(11) 0.3555(6) 0.032(3) Uani 1 1 d . . .
O22 O 0.5832(12) 0.4692(11) 0.1585(6) 0.034(3) Uani 1 1 d . . .
C5 C 0.4880(19) 0.9128(15) 0.3256(9) 0.031(4) Uani 1 1 d . . .
N2 N 0.6018(15) 0.6481(14) 0.4919(7) 0.035(4) Uani 1 1 d . . .
O23 O 0.6287(13) 0.6751(11) 0.2578(7) 0.040(3) Uani 1 1 d . . .
C16 C 0.5379(18) 0.5580(15) 0.3969(8) 0.028(4) Uani 1 1 d . . .
C44 C 0.7068(18) 0.3519(15) 0.0256(8) 0.028(4) Uani 1 1 d . . .
N1 N 0.3444(15) 0.9306(13) 0.3190(8) 0.034(4) Uani 1 1 d . . .
C42 C 0.6665(18) 0.4366(15) 0.1172(8) 0.028(4) Uani 1 1 d . . .
N3 N 0.7129(16) 0.0622(13) 0.1798(8) 0.035(4) Uani 1 1 d . . .
C14 C 0.8044(19) 0.4883(17) 0.3790(9) 0.035(5) Uani 1 1 d . . .
C15 C 0.6777(17) 0.5485(15) 0.4115(8) 0.028(4) Uani 1 1 d . . .
N4 N 0.8446(15) 0.3561(14) 0.0232(7) 0.034(4) Uani 1 1 d . . .
C29 C 0.7591(19) 0.2267(15) 0.2342(8) 0.029(4) Uani 1 1 d . . .
C47 C 0.523(2) 0.3048(16) -0.0128(9) 0.036(5) Uani 1 1 d . . .
C50 C 0.939(2) 0.3229(19) -0.0253(9) 0.041(5) Uani 1 1 d . . .
H50 H 0.9235 0.3782 -0.0672 0.049 Uiso 1 1 calc RD . .
C21 C 0.2189(19) 0.7370(16) 0.5018(9) 0.035(5) Uani 1 1 d . . .
C3 C 0.5381(18) 0.7530(14) 0.2747(8) 0.029(4) Uani 1 1 d . . .
C20 C 0.3547(19) 0.7216(16) 0.5146(9) 0.036(5) Uani 1 1 d . . .
H20 H 0.3769 0.7493 0.5460 0.043 Uiso 1 1 calc R . .
C31 C 0.8473(18) 0.0721(15) 0.1787(9) 0.031(4) Uani 1 1 d . . .
C41 C 0.8082(18) 0.4390(15) 0.1104(8) 0.030(4) Uani 1 1 d . . .
C30 C 0.8719(18) 0.1530(15) 0.2047(8) 0.029(4) Uani 1 1 d . . .
C46 C 0.6567(19) 0.3102(16) -0.0176(9) 0.033(4) Uani 1 1 d . . .
H46 H 0.7145 0.2865 -0.0494 0.040 Uiso 1 1 calc R . .
C6 C 0.304(2) 0.8634(15) 0.2922(9) 0.034(4) Uani 1 1 d . . .
H6 H 0.2085 0.8781 0.2875 0.041 Uiso 1 1 calc R . .
C43 C 0.6184(18) 0.3906(15) 0.0725(8) 0.028(4) Uani 1 1 d . . .
C32 C 0.610(2) 0.1282(16) 0.2080(9) 0.036(5) Uani 1 1 d . . .
H32 H 0.5214 0.1190 0.2088 0.043 Uiso 1 1 calc R . .
C49 C 0.4819(19) 0.3850(16) 0.0762(9) 0.034(4) Uani 1 1 d . . .
H49 H 0.4221 0.4102 0.1071 0.040 Uiso 1 1 calc R . .
C40 C 0.878(2) 0.4796(17) 0.1537(9) 0.036(5) Uani 1 1 d . . .
C4 C 0.5831(19) 0.8272(15) 0.3031(9) 0.032(4) Uani 1 1 d . . .
C10 C 0.7273(19) 0.8114(16) 0.3082(10) 0.037(5) Uani 1 1 d . . .
H10 H 0.7923 0.7553 0.2929 0.045 Uiso 1 1 calc R . .
C48 C 0.4365(19) 0.3423(17) 0.0344(9) 0.038(5) Uani 1 1 d . . .
C17 C 0.4288(17) 0.6196(15) 0.4339(8) 0.027(4) Uani 1 1 d . . .
C19 C 0.7010(19) 0.5914(16) 0.4579(9) 0.034(4) Uani 1 1 d . . .
H19 H 0.7936 0.5810 0.4671 0.041 Uiso 1 1 calc R . .
C27 C 0.497(2) 0.2725(18) 0.2643(10) 0.043(5) Uani 1 1 d . . .
C7 C 0.536(2) 0.9788(17) 0.3547(10) 0.041(5) Uani 1 1 d . . .
H7 H 0.4720 1.0352 0.3703 0.049 Uiso 1 1 calc R . .
C18 C 0.4618(17) 0.6632(15) 0.4800(8) 0.028(4) Uani 1 1 d . . .
C1 C 0.323(2) 0.7037(15) 0.2465(9) 0.035(4) Uani 1 1 d . . .
C34 C 1.086(2) 0.0169(18) 0.1471(10) 0.040(5) Uani 1 1 d . . .
C8 C 0.675(2) 0.9607(17) 0.3604(10) 0.041(5) Uani 1 1 d . . .
C2 C 0.3903(18) 0.7747(15) 0.2708(9) 0.031(4) Uani 1 1 d . . .
C45 C 0.887(2) 0.3987(16) 0.0642(8) 0.034(4) Uani 1 1 d . . .
H45 H 0.9792 0.4011 0.0608 0.041 Uiso 1 1 calc R . .
C22 C 0.1862(18) 0.6913(16) 0.4565(9) 0.035(5) Uani 1 1 d . . .
C35 C 1.1101(19) 0.0988(18) 0.1721(10) 0.042(5) Uani 1 1 d . . .
C28 C 0.6260(18) 0.2077(15) 0.2354(9) 0.031(4) Uani 1 1 d . . .
C33 C 0.957(2) 0.0020(17) 0.1508(9) 0.039(5) Uani 1 1 d . . .
H33 H 0.9408 -0.0538 0.1352 0.047 Uiso 1 1 calc R . .
C23 C 0.2871(18) 0.6340(16) 0.4225(9) 0.033(4) Uani 1 1 d . . .
H23 H 0.2632 0.6047 0.3922 0.040 Uiso 1 1 calc R . .
C9 C 0.7701(19) 0.8778(17) 0.3352(10) 0.041(5) Uani 1 1 d . . .
C36 C 1.0064(19) 0.1647(16) 0.2010(9) 0.036(5) Uani 1 1 d . . .
H36 H 1.0250 0.2175 0.2184 0.043 Uiso 1 1 calc R . .
C13 C 0.217(2) 1.0230(19) 0.4037(11) 0.048(6) Uani 1 1 d . . .
H13A H 0.2006 1.0932 0.4161 0.058 Uiso 1 1 calc R . .
H13B H 0.2662 0.9536 0.4348 0.058 Uiso 1 1 calc R . .
C12 C 0.108(2) 1.0159(19) 0.3638(11) 0.049(6) Uani 1 1 d . . .
H12A H 0.0917 0.9423 0.3708 0.059 Uiso 1 1 calc R . .
H12B H 0.0261 1.0818 0.3521 0.059 Uiso 1 1 calc R . .
C24 C 0.640(2) 0.677(2) 0.5464(11) 0.047(5) Uani 1 1 d . . .
H24 H 0.6272 0.6276 0.5879 0.057 Uiso 1 1 calc R . .
C37 C 0.688(2) -0.0217(17) 0.1521(10) 0.040(5) Uani 1 1 d . . .
H37 H 0.7293 -0.1021 0.1752 0.048 Uiso 1 1 calc R . .
C52 C 1.085(2) 0.253(2) -0.0104(12) 0.060(7) Uani 1 1 d . . .
H52A H 1.1154 0.2317 0.0332 0.072 Uiso 1 1 calc R . .
H52B H 1.1550 0.2680 -0.0416 0.072 Uiso 1 1 calc R . .
C39 C 0.684(2) 0.002(2) 0.0823(11) 0.052(6) Uani 1 1 d . . .
H39A H 0.7230 -0.0617 0.0641 0.062 Uiso 1 1 calc R . .
H39B H 0.6954 0.0747 0.0569 0.062 Uiso 1 1 calc R . .
C26 C 0.761(2) 0.720(2) 0.5413(12) 0.057(6) Uani 1 1 d . . .
H26A H 0.8097 0.7309 0.5011 0.068 Uiso 1 1 calc R . .
H26B H 0.8203 0.6968 0.5783 0.068 Uiso 1 1 calc R . .
C51 C 0.985(2) 0.198(2) -0.0254(12) 0.056(6) Uani 1 1 d . . .
H51A H 0.9936 0.1807 -0.0659 0.067 Uiso 1 1 calc R . .
H51B H 0.9538 0.1443 0.0091 0.067 Uiso 1 1 calc R . .
C38 C 0.553(2) 0.005(2) 0.1201(13) 0.068(8) Uani 1 1 d . . .
H38A H 0.4856 0.0793 0.1176 0.082 Uiso 1 1 calc R . .
H38B H 0.5132 -0.0571 0.1248 0.082 Uiso 1 1 calc R . .
C25 C 0.616(2) 0.798(2) 0.5437(14) 0.070(8) Uani 1 1 d . . .
H25A H 0.5866 0.8208 0.5822 0.084 Uiso 1 1 calc R . .
H25B H 0.5760 0.8549 0.5050 0.084 Uiso 1 1 calc R . .
O4W O -0.063(2) 0.7180(17) 0.1828(9) 0.077(5) Uani 1 1 d G . .
H4WA H -0.0464 0.6804 0.2214 0.115 Uiso 1 1 d G . .
H4WB H 0.0016 0.7488 0.1689 0.115 Uiso 1 1 d G . .
O3W O 0.130(2) 0.528(2) 0.3143(13) 0.129(10) Uani 1 1 d . . .
H3WA H 0.1011 0.4929 0.3491 0.193 Uiso 1 1 d R A 1
H3WB H 0.0682 0.5910 0.2987 0.193 Uiso 1 1 d R A 1
O2W O 1.0487(15) 0.3068(15) 0.3102(9) 0.072(5) Uani 1 1 d . . .
H2WA H 1.0956 0.2364 0.3219 0.107 Uiso 1 1 d R B 1
H2WB H 0.9725 0.3135 0.2933 0.107 Uiso 1 1 d R B 1
O1W O 1.2465(17) 0.532(2) 0.1656(8) 0.101(8) Uani 1 1 d . . .
H1WA H 1.2182 0.5360 0.1295 0.151 Uiso 1 1 d RD C 1
H1WB H 1.3352 0.5122 0.1661 0.151 Uiso 1 1 d R C 1
Na1 Na 1.1762(13) 0.4055(12) 0.2387(7) 0.058(4) Uani 0.70 1 d P . 1
Na1' Na 1.248(3) 0.394(3) 0.2832(14) 0.052(8) Uani 0.30 1 d P . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O20 2.302(13) . ?
Tb1 O11 2.313(13) . ?
Tb1 O13 2.332(12) . ?
Tb1 O18 2.352(12) . ?
Tb1 O22 2.368(12) . ?
Tb1 O23 2.377(13) . ?
Tb1 O21 2.442(11) . ?
Tb1 O12 2.476(12) . ?
Cl4 C47 1.72(2) . ?
Cl2 C21 1.721(18) . ?
Cl3 C34 1.728(19) . ?
C11 N1 1.46(2) . ?
C11 C12 1.48(3) . ?
C11 C13 1.48(3) . ?
C11 H11 0.9800 . ?
Cl1 C8 1.72(2) . ?
F4 C48 1.36(2) . ?
F3 C35 1.35(2) . ?
F1 C9 1.35(2) . ?
F2 C22 1.35(2) . ?
O10 C27 1.25(3) . ?
O10 Na1' 2.15(3) 1_455 ?
O10 Na1 2.48(2) 1_455 ?
O11 C27 1.27(2) . ?
O11 Na1' 2.46(3) 1_455 ?
O12 C29 1.25(2) . ?
O13 C40 1.26(2) . ?
O14 C40 1.25(2) . ?
O14 Na1 2.51(2) . ?
O17 C1 1.25(2) . ?
O18 C1 1.26(2) . ?
O19 C14 1.24(2) . ?
O20 C14 1.26(2) . ?
O21 C16 1.25(2) . ?
O22 C42 1.26(2) . ?
C5 C4 1.39(2) . ?
C5 C7 1.40(3) . ?
C5 N1 1.40(2) . ?
N2 C19 1.35(2) . ?
N2 C18 1.40(2) . ?
N2 C24 1.46(3) . ?
O23 C3 1.25(2) . ?
C16 C15 1.43(2) . ?
C16 C17 1.48(2) . ?
C44 N4 1.40(2) . ?
C44 C46 1.40(3) . ?
C44 C43 1.40(2) . ?
N1 C6 1.33(2) . ?
C42 C41 1.43(2) . ?
C42 C43 1.46(2) . ?
N3 C32 1.35(2) . ?
N3 C31 1.39(2) . ?
N3 C37 1.46(2) . ?
C14 C15 1.51(2) . ?
C15 C19 1.35(3) . ?
N4 C45 1.33(2) . ?
N4 C50 1.44(2) . ?
C29 C28 1.43(3) . ?
C29 C30 1.47(2) . ?
C47 C46 1.36(3) . ?
C47 C48 1.40(3) . ?
C50 C52 1.47(3) . ?
C50 C51 1.51(3) . ?
C50 H50 0.9800 . ?
C21 C20 1.36(3) . ?
C21 C22 1.40(3) . ?
C3 C2 1.43(2) . ?
C3 C4 1.46(3) . ?
C20 C18 1.41(2) . ?
C20 H20 0.9300 . ?
C31 C30 1.40(3) . ?
C31 C33 1.41(2) . ?
C41 C45 1.36(2) . ?
C41 C40 1.51(3) . ?
C30 C36 1.40(3) . ?
C46 H46 0.9300 . ?
C6 C2 1.37(2) . ?
C6 H6 0.9300 . ?
C43 C49 1.39(2) . ?
C32 C28 1.37(3) . ?
C32 H32 0.9300 . ?
C49 C48 1.36(3) . ?
C49 H49 0.9300 . ?
C4 C10 1.41(3) . ?
C10 C9 1.34(3) . ?
C10 H10 0.9300 . ?
C17 C18 1.39(3) . ?
C17 C23 1.41(2) . ?
C19 H19 0.9300 . ?
C27 C28 1.51(3) . ?
C27 Na1' 2.58(3) 1_455 ?
C7 C8 1.36(3) . ?
C7 H7 0.9300 . ?
C1 C2 1.50(3) . ?
C34 C33 1.37(3) . ?
C34 C35 1.40(3) . ?
C8 C9 1.40(3) . ?
C45 H45 0.9300 . ?
C22 C23 1.36(3) . ?
C35 C36 1.36(3) . ?
C33 H33 0.9300 . ?
C23 H23 0.9300 . ?
C36 H36 0.9300 . ?
C13 C12 1.50(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C24 C26 1.46(3) . ?
C24 C25 1.46(3) . ?
C24 H24 0.9800 . ?
C37 C38 1.48(3) . ?
C37 C39 1.48(3) . ?
C37 H37 0.9800 . ?
C52 C51 1.49(3) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C39 C38 1.49(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C26 C25 1.50(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
O4W H4WA 0.8501 . ?
O4W H4WB 0.8499 . ?
O3W Na1' 2.02(4) 1_455 ?
O3W Na1 2.51(3) 1_455 ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8500 . ?
O2W Na1 2.29(2) . ?
O2W Na1' 2.54(4) . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O1W Na1 2.18(3) . ?
O1W Na1' 2.68(4) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
Na1 O10 2.48(2) 1_655 ?
Na1 O3W 2.51(3) 1_655 ?
Na1 H1WA 2.5952 . ?
Na1 H1WB 2.5780 . ?
Na1' O3W 2.02(4) 1_655 ?
Na1' O10 2.15(3) 1_655 ?
Na1' O11 2.46(3) 1_655 ?
Na1' C27 2.58(3) 1_655 ?

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
O20 Tb1 O11 108.1(5) . . ?
O20 Tb1 O13 83.1(5) . . ?
O11 Tb1 O13 138.7(4) . . ?
O20 Tb1 O18 137.9(4) . . ?
O11 Tb1 O18 85.1(5) . . ?
O13 Tb1 O18 113.5(5) . . ?
O20 Tb1 O22 145.3(4) . . ?
O11 Tb1 O22 77.8(5) . . ?
O13 Tb1 O22 72.3(4) . . ?
O18 Tb1 O22 75.7(4) . . ?
O20 Tb1 O23 78.7(5) . . ?
O11 Tb1 O23 147.9(4) . . ?
O13 Tb1 O23 72.3(4) . . ?
O18 Tb1 O23 71.1(5) . . ?
O22 Tb1 O23 114.9(5) . . ?
O20 Tb1 O21 70.5(4) . . ?
O11 Tb1 O21 77.3(4) . . ?
O13 Tb1 O21 141.9(4) . . ?
O18 Tb1 O21 74.1(4) . . ?
O22 Tb1 O21 142.0(4) . . ?
O23 Tb1 O21 75.8(4) . . ?
O20 Tb1 O12 75.3(4) . . ?
O11 Tb1 O12 70.6(4) . . ?
O13 Tb1 O12 74.5(4) . . ?
O18 Tb1 O12 145.0(5) . . ?
O22 Tb1 O12 74.8(4) . . ?
O23 Tb1 O12 139.8(4) . . ?
O21 Tb1 O12 121.9(4) . . ?
N1 C11 C12 119.2(17) . . ?
N1 C11 C13 119.1(17) . . ?
C12 C11 C13 60.6(14) . . ?
N1 C11 H11 115.6 . . ?
C12 C11 H11 115.6 . . ?
C13 C11 H11 115.6 . . ?
C27 O10 Na1' 95.4(16) . 1_455 ?
C27 O10 Na1 112.1(15) . 1_455 ?
Na1' O10 Na1 29.4(9) 1_455 1_455 ?
C27 O11 Tb1 135.8(12) . . ?
C27 O11 Na1' 81.0(14) . 1_455 ?
Tb1 O11 Na1' 125.8(9) . 1_455 ?
C29 O12 Tb1 127.4(11) . . ?
C40 O13 Tb1 131.8(12) . . ?
C40 O14 Na1 126.3(13) . . ?
C1 O18 Tb1 133.8(12) . . ?
C14 O20 Tb1 137.2(12) . . ?
C16 O21 Tb1 129.5(11) . . ?
C42 O22 Tb1 131.5(12) . . ?
C4 C5 C7 120.1(17) . . ?
C4 C5 N1 119.0(18) . . ?
C7 C5 N1 120.9(17) . . ?
C19 N2 C18 118.4(17) . . ?
C19 N2 C24 120.5(16) . . ?
C18 N2 C24 120.4(15) . . ?
C3 O23 Tb1 129.6(11) . . ?
O21 C16 C15 125.8(16) . . ?
O21 C16 C17 119.2(16) . . ?
C15 C16 C17 115.0(17) . . ?
N4 C44 C46 121.3(16) . . ?
N4 C44 C43 118.6(17) . . ?
C46 C44 C43 120.2(16) . . ?
C6 N1 C5 118.6(15) . . ?
C6 N1 C11 121.6(16) . . ?
C5 N1 C11 119.5(16) . . ?
O22 C42 C41 125.3(17) . . ?
O22 C42 C43 118.8(16) . . ?
C41 C42 C43 116.0(15) . . ?
C32 N3 C31 119.1(17) . . ?
C32 N3 C37 121.9(16) . . ?
C31 N3 C37 119.0(15) . . ?
O19 C14 O20 124.6(17) . . ?
O19 C14 C15 117.3(18) . . ?
O20 C14 C15 118.0(17) . . ?
C19 C15 C16 119.6(16) . . ?
C19 C15 C14 117.1(17) . . ?
C16 C15 C14 123.2(17) . . ?
C45 N4 C44 119.5(15) . . ?
C45 N4 C50 118.8(16) . . ?
C44 N4 C50 121.5(16) . . ?
O12 C29 C28 125.2(17) . . ?
O12 C29 C30 119.5(17) . . ?
C28 C29 C30 115.3(17) . . ?
C46 C47 C48 119.8(19) . . ?
C46 C47 Cl4 120.6(15) . . ?
C48 C47 Cl4 119.6(15) . . ?
N4 C50 C52 121.1(18) . . ?
N4 C50 C51 118.1(18) . . ?
C52 C50 C51 60.0(15) . . ?
N4 C50 H50 115.4 . . ?
C52 C50 H50 115.4 . . ?
C51 C50 H50 115.4 . . ?
C20 C21 C22 120.0(17) . . ?
C20 C21 Cl2 120.7(17) . . ?
C22 C21 Cl2 119.3(15) . . ?
O23 C3 C2 125.5(18) . . ?
O23 C3 C4 118.7(17) . . ?
C2 C3 C4 115.8(16) . . ?
C21 C20 C18 119.7(19) . . ?
C21 C20 H20 120.2 . . ?
C18 C20 H20 120.2 . . ?
N3 C31 C30 119.5(16) . . ?
N3 C31 C33 119.8(18) . . ?
C30 C31 C33 120.6(17) . . ?
C45 C41 C42 118.9(18) . . ?
C45 C41 C40 117.5(16) . . ?
C42 C41 C40 123.6(15) . . ?
C36 C30 C31 118.7(17) . . ?
C36 C30 C29 119.9(17) . . ?
C31 C30 C29 121.4(17) . . ?
C47 C46 C44 119.6(17) . . ?
C47 C46 H46 120.2 . . ?
C44 C46 H46 120.2 . . ?
N1 C6 C2 126.2(18) . . ?
N1 C6 H6 116.9 . . ?
C2 C6 H6 116.9 . . ?
C49 C43 C44 119.3(17) . . ?
C49 C43 C42 119.3(16) . . ?
C44 C43 C42 121.4(16) . . ?
N3 C32 C28 124.8(18) . . ?
N3 C32 H32 117.6 . . ?
C28 C32 H32 117.6 . . ?
C48 C49 C43 119.5(17) . . ?
C48 C49 H49 120.3 . . ?
C43 C49 H49 120.3 . . ?
O14 C40 O13 124.3(19) . . ?
O14 C40 C41 116.9(16) . . ?
O13 C40 C41 118.7(16) . . ?
C5 C4 C10 119.0(18) . . ?
C5 C4 C3 122.0(17) . . ?
C10 C4 C3 119.0(16) . . ?
C9 C10 C4 119.6(18) . . ?
C9 C10 H10 120.2 . . ?
C4 C10 H10 120.2 . . ?
F4 C48 C49 119.6(17) . . ?
F4 C48 C47 118.7(18) . . ?
C49 C48 C47 121.6(18) . . ?
C18 C17 C23 119.3(16) . . ?
C18 C17 C16 121.7(16) . . ?
C23 C17 C16 119.1(17) . . ?
N2 C19 C15 125.8(18) . . ?
N2 C19 H19 117.1 . . ?
C15 C19 H19 117.1 . . ?
O10 C27 O11 124.0(18) . . ?
O10 C27 C28 117.1(19) . . ?
O11 C27 C28 119.0(18) . . ?
O10 C27 Na1' 55.9(13) . 1_455 ?
O11 C27 Na1' 70.0(13) . 1_455 ?
C28 C27 Na1' 164.1(17) . 1_455 ?
C8 C7 C5 120.1(18) . . ?
C8 C7 H7 120.0 . . ?
C5 C7 H7 120.0 . . ?
C17 C18 N2 119.5(15) . . ?
C17 C18 C20 120.2(17) . . ?
N2 C18 C20 120.3(17) . . ?
O17 C1 O18 124.5(19) . . ?
O17 C1 C2 117.5(17) . . ?
O18 C1 C2 118.0(16) . . ?
C33 C34 C35 120.1(18) . . ?
C33 C34 Cl3 120.7(17) . . ?
C35 C34 Cl3 119.3(15) . . ?
C7 C8 C9 119(2) . . ?
C7 C8 Cl1 121.0(16) . . ?
C9 C8 Cl1 119.7(16) . . ?
C6 C2 C3 118.3(18) . . ?
C6 C2 C1 117.8(16) . . ?
C3 C2 C1 123.9(16) . . ?
N4 C45 C41 125.6(18) . . ?
N4 C45 H45 117.2 . . ?
C41 C45 H45 117.2 . . ?
F2 C22 C23 119.3(19) . . ?
F2 C22 C21 118.9(16) . . ?
C23 C22 C21 121.7(18) . . ?
F3 C35 C36 119.6(19) . . ?
F3 C35 C34 119.0(17) . . ?
C36 C35 C34 121.4(19) . . ?
C32 C28 C29 119.7(17) . . ?
C32 C28 C27 116.4(17) . . ?
C29 C28 C27 123.9(18) . . ?
C34 C33 C31 119.1(19) . . ?
C34 C33 H33 120.4 . . ?
C31 C33 H33 120.4 . . ?
C22 C23 C17 119.1(19) . . ?
C22 C23 H23 120.4 . . ?
C17 C23 H23 120.4 . . ?
C10 C9 F1 120.1(18) . . ?
C10 C9 C8 121.8(18) . . ?
F1 C9 C8 118.0(19) . . ?
C35 C36 C30 120.0(19) . . ?
C35 C36 H36 120.0 . . ?
C30 C36 H36 120.0 . . ?
C11 C13 C12 59.7(14) . . ?
C11 C13 H13A 117.8 . . ?
C12 C13 H13A 117.8 . . ?
C11 C13 H13B 117.8 . . ?
C12 C13 H13B 117.8 . . ?
H13A C13 H13B 114.9 . . ?
C11 C12 C13 59.7(14) . . ?
C11 C12 H12A 117.8 . . ?
C13 C12 H12A 117.8 . . ?
C11 C12 H12B 117.8 . . ?
C13 C12 H12B 117.8 . . ?
H12A C12 H12B 114.9 . . ?
N2 C24 C26 118.8(19) . . ?
N2 C24 C25 119(2) . . ?
C26 C24 C25 61.8(16) . . ?
N2 C24 H24 115.5 . . ?
C26 C24 H24 115.5 . . ?
C25 C24 H24 115.5 . . ?
N3 C37 C38 119.2(18) . . ?
N3 C37 C39 119.4(18) . . ?
C38 C37 C39 60.5(16) . . ?
N3 C37 H37 115.5 . . ?
C38 C37 H37 115.5 . . ?
C39 C37 H37 115.5 . . ?
C50 C52 C51 61.5(14) . . ?
C50 C52 H52A 117.6 . . ?
C51 C52 H52A 117.6 . . ?
C50 C52 H52B 117.6 . . ?
C51 C52 H52B 117.6 . . ?
H52A C52 H52B 114.7 . . ?
C37 C39 C38 59.7(15) . . ?
C37 C39 H39A 117.8 . . ?
C38 C39 H39A 117.8 . . ?
C37 C39 H39B 117.8 . . ?
C38 C39 H39B 117.8 . . ?
H39A C39 H39B 114.9 . . ?
C24 C26 C25 59.0(15) . . ?
C24 C26 H26A 117.9 . . ?
C25 C26 H26A 117.9 . . ?
C24 C26 H26B 117.9 . . ?
C25 C26 H26B 117.9 . . ?
H26A C26 H26B 115.0 . . ?
C50 C51 C52 58.5(15) . . ?
C50 C51 H51A 117.9 . . ?
C52 C51 H51A 117.9 . . ?
C50 C51 H51B 117.9 . . ?
C52 C51 H51B 117.9 . . ?
H51A C51 H51B 115.1 . . ?
C37 C38 C39 59.8(14) . . ?
C37 C38 H38A 117.8 . . ?
C39 C38 H38A 117.8 . . ?
C37 C38 H38B 117.8 . . ?
C39 C38 H38B 117.8 . . ?
H38A C38 H38B 114.9 . . ?
C24 C25 C26 59.2(15) . . ?
C24 C25 H25A 117.9 . . ?
C26 C25 H25A 117.9 . . ?
C24 C25 H25B 117.9 . . ?
C26 C25 H25B 117.9 . . ?
H25A C25 H25B 115.0 . . ?
H4WA O4W H4WB 109.5 . . ?
Na1' O3W Na1 28.6(10) 1_455 1_455 ?
Na1' O3W H3WA 100.7 1_455 . ?
Na1 O3W H3WA 109.2 1_455 . ?
Na1' O3W H3WB 136.4 1_455 . ?
Na1 O3W H3WB 109.4 1_455 . ?
H3WA O3W H3WB 109.5 . . ?
Na1 O2W Na1' 28.6(7) . . ?
Na1 O2W H2WA 109.2 . . ?
Na1' O2W H2WA 99.2 . . ?
Na1 O2W H2WB 109.7 . . ?
Na1' O2W H2WB 137.3 . . ?
H2WA O2W H2WB 109.5 . . ?
Na1 O1W Na1' 26.5(8) . . ?
Na1 O1W H1WA 110.2 . . ?
Na1' O1W H1WA 135.7 . . ?
Na1 O1W H1WB 108.8 . . ?
Na1' O1W H1WB 89.9 . . ?
H1WA O1W H1WB 109.5 . . ?
O1W Na1 O2W 165.6(9) . . ?
O1W Na1 O10 103.3(8) . 1_655 ?
O2W Na1 O10 91.2(7) . 1_655 ?
O1W Na1 O14 76.2(7) . . ?
O2W Na1 O14 94.2(7) . . ?
O10 Na1 O14 129.1(8) 1_655 . ?
O1W Na1 O3W 92.0(8) . 1_655 ?
O2W Na1 O3W 83.0(8) . 1_655 ?
O10 Na1 O3W 112.3(10) 1_655 1_655 ?
O14 Na1 O3W 118.6(9) . 1_655 ?
O1W Na1 H1WA 17.9 . . ?
O2W Na1 H1WA 153.9 . . ?
O10 Na1 H1WA 107.2 1_655 . ?
O14 Na1 H1WA 59.9 . . ?
O3W Na1 H1WA 105.8 1_655 . ?
O1W Na1 H1WB 18.2 . . ?
O2W Na1 H1WB 174.9 . . ?
O10 Na1 H1WB 85.7 1_655 . ?
O14 Na1 H1WB 90.8 . . ?
O3W Na1 H1WB 94.5 1_655 . ?
H1WA Na1 H1WB 31.1 . . ?
O3W Na1' O10 169.8(19) 1_655 1_655 ?
O3W Na1' O11 117.8(18) 1_655 1_655 ?
O10 Na1' O11 57.2(8) 1_655 1_655 ?
O3W Na1' O2W 88.2(12) 1_655 . ?
O10 Na1' O2W 93.1(13) 1_655 . ?
O11 Na1' O2W 144.8(13) 1_655 . ?
O3W Na1' C27 146.8(19) 1_655 1_655 ?
O10 Na1' C27 28.7(7) 1_655 1_655 ?
O11 Na1' C27 29.0(6) 1_655 1_655 ?
O2W Na1' C27 121.1(14) . 1_655 ?
O3W Na1' O1W 90.9(13) 1_655 . ?
O10 Na1' O1W 97.7(12) 1_655 . ?
O11 Na1' O1W 88.5(10) 1_655 . ?
O2W Na1' O1W 116.2(14) . . ?
C27 Na1' O1W 89.4(10) 1_655 . ?

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
O20 Tb1 O11 C27 -110(2) . . . . ?
O13 Tb1 O11 C27 -10(2) . . . . ?
O18 Tb1 O11 C27 111(2) . . . . ?
O22 Tb1 O11 C27 34(2) . . . . ?
O23 Tb1 O11 C27 152.2(18) . . . . ?
O21 Tb1 O11 C27 -174(2) . . . . ?
O12 Tb1 O11 C27 -43.6(19) . . . . ?
O20 Tb1 O11 Na1' 132.2(11) . . . 1_455 ?
O13 Tb1 O11 Na1' -127.4(11) . . . 1_455 ?
O18 Tb1 O11 Na1' -6.9(11) . . . 1_455 ?
O22 Tb1 O11 Na1' -83.3(11) . . . 1_455 ?
O23 Tb1 O11 Na1' 34.5(16) . . . 1_455 ?
O21 Tb1 O11 Na1' 67.9(11) . . . 1_455 ?
O12 Tb1 O11 Na1' -161.3(12) . . . 1_455 ?
O20 Tb1 O12 C29 156.0(15) . . . . ?
O11 Tb1 O12 C29 40.3(14) . . . . ?
O13 Tb1 O12 C29 -117.2(15) . . . . ?
O18 Tb1 O12 C29 -8.2(18) . . . . ?
O22 Tb1 O12 C29 -41.8(14) . . . . ?
O23 Tb1 O12 C29 -152.6(13) . . . . ?
O21 Tb1 O12 C29 100.7(14) . . . . ?
O20 Tb1 O13 C40 110.2(17) . . . . ?
O11 Tb1 O13 C40 0(2) . . . . ?
O18 Tb1 O13 C40 -110.2(17) . . . . ?
O22 Tb1 O13 C40 -45.0(17) . . . . ?
O23 Tb1 O13 C40 -169.5(18) . . . . ?
O21 Tb1 O13 C40 155.9(15) . . . . ?
O12 Tb1 O13 C40 33.6(17) . . . . ?
O20 Tb1 O18 C1 2(2) . . . . ?
O11 Tb1 O18 C1 113.5(17) . . . . ?
O13 Tb1 O18 C1 -104.8(16) . . . . ?
O22 Tb1 O18 C1 -167.9(17) . . . . ?
O23 Tb1 O18 C1 -44.7(16) . . . . ?
O21 Tb1 O18 C1 35.4(16) . . . . ?
O12 Tb1 O18 C1 158.7(15) . . . . ?
O11 Tb1 O20 C14 -112.4(19) . . . . ?
O13 Tb1 O20 C14 108.4(19) . . . . ?
O18 Tb1 O20 C14 -9(2) . . . . ?
O22 Tb1 O20 C14 152.9(17) . . . . ?
O23 Tb1 O20 C14 35.1(19) . . . . ?
O21 Tb1 O20 C14 -43.6(18) . . . . ?
O12 Tb1 O20 C14 -176(2) . . . . ?
O20 Tb1 O21 C16 35.7(14) . . . . ?
O11 Tb1 O21 C16 150.4(15) . . . . ?
O13 Tb1 O21 C16 -13.2(18) . . . . ?
O18 Tb1 O21 C16 -121.1(15) . . . . ?
O22 Tb1 O21 C16 -159.6(13) . . . . ?
O23 Tb1 O21 C16 -47.1(14) . . . . ?
O12 Tb1 O21 C16 93.2(15) . . . . ?
O20 Tb1 O22 C42 -14(2) . . . . ?
O11 Tb1 O22 C42 -118.6(16) . . . . ?
O13 Tb1 O22 C42 32.6(16) . . . . ?
O18 Tb1 O22 C42 153.5(17) . . . . ?
O23 Tb1 O22 C42 92.7(16) . . . . ?
O21 Tb1 O22 C42 -168.4(14) . . . . ?
O12 Tb1 O22 C42 -45.6(16) . . . . ?
O20 Tb1 O23 C3 -110.6(16) . . . . ?
O11 Tb1 O23 C3 -4(2) . . . . ?
O13 Tb1 O23 C3 163.1(17) . . . . ?
O18 Tb1 O23 C3 39.6(15) . . . . ?
O22 Tb1 O23 C3 103.1(16) . . . . ?
O21 Tb1 O23 C3 -38.1(15) . . . . ?
O12 Tb1 O23 C3 -161.1(14) . . . . ?
Tb1 O21 C16 C15 -26(3) . . . . ?
Tb1 O21 C16 C17 152.0(12) . . . . ?
C4 C5 N1 C6 1(3) . . . . ?
C7 C5 N1 C6 -178.4(18) . . . . ?
C4 C5 N1 C11 -173.3(17) . . . . ?
C7 C5 N1 C11 7(3) . . . . ?
C12 C11 N1 C6 40(3) . . . . ?
C13 C11 N1 C6 111(2) . . . . ?
C12 C11 N1 C5 -145.6(19) . . . . ?
C13 C11 N1 C5 -75(2) . . . . ?
Tb1 O22 C42 C41 -23(3) . . . . ?
Tb1 O22 C42 C43 156.5(12) . . . . ?
Tb1 O20 C14 O19 -145.5(17) . . . . ?
Tb1 O20 C14 C15 36(3) . . . . ?
O21 C16 C15 C19 -179.7(17) . . . . ?
C17 C16 C15 C19 2(2) . . . . ?
O21 C16 C15 C14 -2(3) . . . . ?
C17 C16 C15 C14 179.8(16) . . . . ?
O19 C14 C15 C19 -1(3) . . . . ?
O20 C14 C15 C19 178.3(17) . . . . ?
O19 C14 C15 C16 -178.4(18) . . . . ?
O20 C14 C15 C16 0(3) . . . . ?
C46 C44 N4 C45 178.4(17) . . . . ?
C43 C44 N4 C45 -2(3) . . . . ?
C46 C44 N4 C50 3(3) . . . . ?
C43 C44 N4 C50 -177.0(17) . . . . ?
Tb1 O12 C29 C28 -31(2) . . . . ?
Tb1 O12 C29 C30 147.9(12) . . . . ?
C45 N4 C50 C52 47(3) . . . . ?
C44 N4 C50 C52 -137(2) . . . . ?
C45 N4 C50 C51 117(2) . . . . ?
C44 N4 C50 C51 -67(3) . . . . ?
Tb1 O23 C3 C2 -31(3) . . . . ?
Tb1 O23 C3 C4 146.2(13) . . . . ?
C22 C21 C20 C18 3(3) . . . . ?
Cl2 C21 C20 C18 -176.3(14) . . . . ?
C32 N3 C31 C30 -2(3) . . . . ?
C37 N3 C31 C30 179.5(17) . . . . ?
C32 N3 C31 C33 178.5(17) . . . . ?
C37 N3 C31 C33 0(3) . . . . ?
O22 C42 C41 C45 178.7(18) . . . . ?
C43 C42 C41 C45 0(3) . . . . ?
O22 C42 C41 C40 1(3) . . . . ?
C43 C42 C41 C40 -177.8(16) . . . . ?
N3 C31 C30 C36 -177.7(17) . . . . ?
C33 C31 C30 C36 2(3) . . . . ?
N3 C31 C30 C29 1(3) . . . . ?
C33 C31 C30 C29 -179.8(16) . . . . ?
O12 C29 C30 C36 1(3) . . . . ?
C28 C29 C30 C36 180.0(17) . . . . ?
O12 C29 C30 C31 -177.6(16) . . . . ?
C28 C29 C30 C31 1(3) . . . . ?
C48 C47 C46 C44 1(3) . . . . ?
Cl4 C47 C46 C44 -179.2(14) . . . . ?
N4 C44 C46 C47 178.3(17) . . . . ?
C43 C44 C46 C47 -2(3) . . . . ?
C5 N1 C6 C2 1(3) . . . . ?
C11 N1 C6 C2 175.6(17) . . . . ?
N4 C44 C43 C49 -178.8(16) . . . . ?
C46 C44 C43 C49 1(3) . . . . ?
N4 C44 C43 C42 1(3) . . . . ?
C46 C44 C43 C42 -178.7(16) . . . . ?
O22 C42 C43 C49 1(3) . . . . ?
C41 C42 C43 C49 179.8(16) . . . . ?
O22 C42 C43 C44 -179.5(16) . . . . ?
C41 C42 C43 C44 0(2) . . . . ?
C31 N3 C32 C28 1(3) . . . . ?
C37 N3 C32 C28 179.4(19) . . . . ?
C44 C43 C49 C48 0(3) . . . . ?
C42 C43 C49 C48 179.9(17) . . . . ?
Na1 O14 C40 O13 37(3) . . . . ?
Na1 O14 C40 C41 -142.6(14) . . . . ?
Tb1 O13 C40 O14 -135.5(18) . . . . ?
Tb1 O13 C40 C41 44(3) . . . . ?
C45 C41 C40 O14 -9(3) . . . . ?
C42 C41 C40 O14 168.6(18) . . . . ?
C45 C41 C40 O13 171.7(18) . . . . ?
C42 C41 C40 O13 -11(3) . . . . ?
C7 C5 C4 C10 -2(3) . . . . ?
N1 C5 C4 C10 178.3(17) . . . . ?
C7 C5 C4 C3 177.4(17) . . . . ?
N1 C5 C4 C3 -2(3) . . . . ?
O23 C3 C4 C5 -177.1(16) . . . . ?
C2 C3 C4 C5 1(3) . . . . ?
O23 C3 C4 C10 3(3) . . . . ?
C2 C3 C4 C10 -179.6(16) . . . . ?
C5 C4 C10 C9 1(3) . . . . ?
C3 C4 C10 C9 -178.9(18) . . . . ?
C43 C49 C48 F4 -179.9(17) . . . . ?
C43 C49 C48 C47 -1(3) . . . . ?
C46 C47 C48 F4 179.5(18) . . . . ?
Cl4 C47 C48 F4 0(3) . . . . ?
C46 C47 C48 C49 0(3) . . . . ?
Cl4 C47 C48 C49 -179.6(16) . . . . ?
O21 C16 C17 C18 -179.2(16) . . . . ?
C15 C16 C17 C18 -1(2) . . . . ?
O21 C16 C17 C23 1(2) . . . . ?
C15 C16 C17 C23 179.6(16) . . . . ?
C18 N2 C19 C15 1(3) . . . . ?
C24 N2 C19 C15 172.0(19) . . . . ?
C16 C15 C19 N2 -2(3) . . . . ?
C14 C15 C19 N2 179.7(17) . . . . ?
Na1' O10 C27 O11 17(3) 1_455 . . . ?
Na1 O10 C27 O11 42(3) 1_455 . . . ?
Na1' O10 C27 C28 -163.5(18) 1_455 . . . ?
Na1 O10 C27 C28 -138.4(15) 1_455 . . . ?
Na1 O10 C27 Na1' 25.0(9) 1_455 . . 1_455 ?
Tb1 O11 C27 O10 -148.4(19) . . . . ?
Na1' O11 C27 O10 -15(2) 1_455 . . . ?
Tb1 O11 C27 C28 32(3) . . . . ?
Na1' O11 C27 C28 166(2) 1_455 . . . ?
Tb1 O11 C27 Na1' -133.3(18) . . . 1_455 ?
C4 C5 C7 C8 1(3) . . . . ?
N1 C5 C7 C8 -179.6(18) . . . . ?
C23 C17 C18 N2 179.3(16) . . . . ?
C16 C17 C18 N2 0(3) . . . . ?
C23 C17 C18 C20 0(3) . . . . ?
C16 C17 C18 C20 -179.9(16) . . . . ?
C19 N2 C18 C17 0(3) . . . . ?
C24 N2 C18 C17 -170.6(18) . . . . ?
C19 N2 C18 C20 179.8(17) . . . . ?
C24 N2 C18 C20 9(3) . . . . ?
C21 C20 C18 C17 -1(3) . . . . ?
C21 C20 C18 N2 179.1(17) . . . . ?
Tb1 O18 C1 O17 -141.9(17) . . . . ?
Tb1 O18 C1 C2 37(2) . . . . ?
C5 C7 C8 C9 2(3) . . . . ?
C5 C7 C8 Cl1 -180.0(16) . . . . ?
N1 C6 C2 C3 -3(3) . . . . ?
N1 C6 C2 C1 175.4(17) . . . . ?
O23 C3 C2 C6 179.2(17) . . . . ?
C4 C3 C2 C6 2(2) . . . . ?
O23 C3 C2 C1 1(3) . . . . ?
C4 C3 C2 C1 -176.4(16) . . . . ?
O17 C1 C2 C6 -2(3) . . . . ?
O18 C1 C2 C6 179.8(16) . . . . ?
O17 C1 C2 C3 176.4(17) . . . . ?
O18 C1 C2 C3 -2(3) . . . . ?
C44 N4 C45 C41 1(3) . . . . ?
C50 N4 C45 C41 176.5(19) . . . . ?
C42 C41 C45 N4 0(3) . . . . ?
C40 C41 C45 N4 177.6(18) . . . . ?
C20 C21 C22 F2 177.6(17) . . . . ?
Cl2 C21 C22 F2 -4(2) . . . . ?
C20 C21 C22 C23 -2(3) . . . . ?
Cl2 C21 C22 C23 176.6(15) . . . . ?
C33 C34 C35 F3 178.7(19) . . . . ?
Cl3 C34 C35 F3 -2(3) . . . . ?
C33 C34 C35 C36 1(3) . . . . ?
Cl3 C34 C35 C36 179.8(16) . . . . ?
N3 C32 C28 C29 1(3) . . . . ?
N3 C32 C28 C27 179.9(18) . . . . ?
O12 C29 C28 C32 176.4(17) . . . . ?
C30 C29 C28 C32 -2(3) . . . . ?
O12 C29 C28 C27 -2(3) . . . . ?
C30 C29 C28 C27 179.0(17) . . . . ?
O10 C27 C28 C32 7(3) . . . . ?
O11 C27 C28 C32 -173.7(19) . . . . ?
Na1' C27 C28 C32 -53(6) 1_455 . . . ?
O10 C27 C28 C29 -175(2) . . . . ?
O11 C27 C28 C29 5(3) . . . . ?
Na1' C27 C28 C29 126(6) 1_455 . . . ?
C35 C34 C33 C31 2(3) . . . . ?
Cl3 C34 C33 C31 -177.7(15) . . . . ?
N3 C31 C33 C34 176.6(18) . . . . ?
C30 C31 C33 C34 -3(3) . . . . ?
F2 C22 C23 C17 -179.3(16) . . . . ?
C21 C22 C23 C17 1(3) . . . . ?
C18 C17 C23 C22 1(3) . . . . ?
C16 C17 C23 C22 -179.7(16) . . . . ?
C4 C10 C9 F1 -177.7(17) . . . . ?
C4 C10 C9 C8 2(3) . . . . ?
C7 C8 C9 C10 -3(3) . . . . ?
Cl1 C8 C9 C10 178.4(17) . . . . ?
C7 C8 C9 F1 176.3(19) . . . . ?
Cl1 C8 C9 F1 -2(3) . . . . ?
F3 C35 C36 C30 -179.8(18) . . . . ?
C34 C35 C36 C30 -2(3) . . . . ?
C31 C30 C36 C35 1(3) . . . . ?
C29 C30 C36 C35 -178.1(17) . . . . ?
N1 C11 C13 C12 -109(2) . . . . ?
N1 C11 C12 C13 109(2) . . . . ?
C19 N2 C24 C26 42(3) . . . . ?
C18 N2 C24 C26 -147(2) . . . . ?
C19 N2 C24 C25 114(2) . . . . ?
C18 N2 C24 C25 -75(3) . . . . ?
C32 N3 C37 C38 36(3) . . . . ?
C31 N3 C37 C38 -146(2) . . . . ?
C32 N3 C37 C39 107(2) . . . . ?
C31 N3 C37 C39 -75(2) . . . . ?
N4 C50 C52 C51 107(2) . . . . ?
N3 C37 C39 C38 -109(2) . . . . ?
N2 C24 C26 C25 110(2) . . . . ?
N4 C50 C51 C52 -112(2) . . . . ?
N3 C37 C38 C39 109(2) . . . . ?
N2 C24 C25 C26 -109(2) . . . . ?
Na1' O1W Na1 O2W 121(5) . . . . ?
Na1' O1W Na1 O10 -61.5(15) . . . 1_655 ?
Na1' O1W Na1 O14 171.0(16) . . . . ?
Na1' O1W Na1 O3W 52.0(15) . . . 1_655 ?
Na1' O2W Na1 O1W -123(5) . . . . ?
Na1' O2W Na1 O10 59.9(15) . . . 1_655 ?
Na1' O2W Na1 O14 -170.8(17) . . . . ?
Na1' O2W Na1 O3W -52.4(15) . . . 1_655 ?
C40 O14 Na1 O1W -136.4(19) . . . . ?
C40 O14 Na1 O2W 32.6(19) . . . . ?
C40 O14 Na1 O10 127.6(18) . . . 1_655 ?
C40 O14 Na1 O3W -52(2) . . . 1_655 ?
Na1 O2W Na1' O3W 101.0(18) . . . 1_655 ?
Na1 O2W Na1' O10 -89.1(18) . . . 1_655 ?
Na1 O2W Na1' O11 -119(3) . . . 1_655 ?
Na1 O2W Na1' C27 -96(2) . . . 1_655 ?
Na1 O2W Na1' O1W 10.9(9) . . . . ?
Na1 O1W Na1' O3W -100.8(18) . . . 1_655 ?
Na1 O1W Na1' O10 84.8(19) . . . 1_655 ?
Na1 O1W Na1' O11 141(2) . . . 1_655 ?
Na1 O1W Na1' O2W -12.4(10) . . . . ?
Na1 O1W Na1' C27 112.4(19) . . . 1_655 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.095

# start Validation Reply Form 
_vrf_PLAT342_1c                  
;
PROBLEM:  
RESPONSE: Because there is a large amount of disorder in the structure. 
;
_vrf_PLAT415_1c                  
;
PROBLEM:  
RESPONSE: Because the disorder of the hydrogen. 
;
_vrf_PLAT417_1c                  
;
PROBLEM:  
RESPONSE: Because the disorder of H4WA. 
;
_vrf_PLAT420_1c                  
;
PROBLEM:  
RESPONSE: Because the disorder of THE hydrogen. 
;
_vrf_PLAT910_1c                  
;
PROBLEM:
RESPONSE: Theta min = 3.7580 deg. The theta value of the missing reflections 
are less than 3.7580 deg. and therefore reflections were excluded. 
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2c
_database_code_depnum_ccdc_archive 'CCDC 1855013'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H38 Cl4 F4 K N4 O15 Tb'
_chemical_formula_weight         1374.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1720 4.1540 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0496(3)
_cell_length_b                   12.7645(4)
_cell_length_c                   21.6687(7)
_cell_angle_alpha                74.538(3)
_cell_angle_beta                 86.700(3)
_cell_angle_gamma                73.095(3)
_cell_volume                     2562.65(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9438
_cell_measurement_theta_min      3.5540
_cell_measurement_theta_max      27.8240

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7088
_exptl_absorpt_correction_T_max  0.8299
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19626
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         25.01
_reflns_number_total             8985
_reflns_number_gt                7988
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0397P)²+3.1132P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8985
_refine_ls_number_parameters     748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0833
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb2 Tb 0.11261(2) 0.488918(16) 0.256778(9) 0.02833(7) Uani 1 1 d . . .
Cl1 Cl 0.22167(13) 1.03552(12) 0.39542(7) 0.0610(4) Uani 1 1 d . . .
Cl3 Cl -0.05057(14) 0.25773(11) -0.07788(6) 0.0559(3) Uani 1 1 d . . .
Cl2 Cl -0.40718(12) 0.81802(11) 0.54236(6) 0.0531(3) Uani 1 1 d . . .
Cl4 Cl 0.71419(12) -0.04632(12) 0.10345(7) 0.0607(4) Uani 1 1 d . . .
F2 F -0.4491(2) 0.7128(3) 0.44446(13) 0.0556(8) Uani 1 1 d . . .
F4 F 0.7300(3) 0.1276(3) 0.16369(17) 0.0676(9) Uani 1 1 d . . .
O10 O -0.0036(3) 0.3515(2) 0.28328(14) 0.0396(7) Uani 1 1 d . . .
O1 O -0.1168(3) 0.6087(2) 0.22475(14) 0.0367(7) Uani 1 1 d . . .
O3 O 0.1091(3) 0.6757(2) 0.24858(15) 0.0419(7) Uani 1 1 d . . .
O4 O 0.2757(3) 0.4498(3) 0.33573(14) 0.0423(8) Uani 1 1 d . . .
O5 O 0.4140(3) 0.4683(3) 0.40516(16) 0.0530(9) Uani 1 1 d . . .
O6 O -0.0048(3) 0.5251(2) 0.35452(13) 0.0333(7) Uani 1 1 d . . .
O9 O 0.0786(3) 0.4641(2) 0.15503(13) 0.0343(7) Uani 1 1 d . . .
O7 O 0.2988(3) 0.5269(2) 0.19190(13) 0.0358(7) Uani 1 1 d . . .
O12 O 0.2779(3) 0.3030(2) 0.25450(14) 0.0363(7) Uani 1 1 d . . .
O2 O -0.3234(3) 0.7292(3) 0.2302(2) 0.0704(12) Uani 1 1 d . . .
O8 O 0.4995(3) 0.4707(3) 0.14478(16) 0.0510(9) Uani 1 1 d . . .
O11 O -0.1085(4) 0.2311(3) 0.2673(2) 0.0716(12) Uani 1 1 d . . .
N4 N 0.2100(3) 0.0631(3) 0.17651(17) 0.0343(8) Uani 1 1 d . . .
N3 N 0.3361(4) 0.3600(3) 0.01629(16) 0.0348(8) Uani 1 1 d . . .
N2 N 0.1033(3) 0.6464(3) 0.49561(16) 0.0312(8) Uani 1 1 d . . .
N1 N -0.1727(3) 0.9253(3) 0.31231(17) 0.0340(8) Uani 1 1 d . . .
C16 C 0.0330(4) 0.5605(3) 0.39723(17) 0.0246(8) Uani 1 1 d . . .
C25 C -0.2781(4) 0.7401(3) 0.5030(2) 0.0350(10) Uani 1 1 d . . .
C26 C -0.1406(4) 0.7223(3) 0.51756(19) 0.0326(9) Uani 1 1 d . . .
H26 H -0.1166 0.7485 0.5503 0.039 Uiso 1 1 calc R . .
C29 C 0.1621(4) 0.4337(3) 0.11351(18) 0.0283(9) Uani 1 1 d . . .
F1 F 0.3888(3) 0.8621(2) 0.33693(16) 0.0616(8) Uani 1 1 d . . .
C35 C 0.5741(5) 0.2565(5) -0.0162(3) 0.0582(14) Uani 1 1 d . . .
H35A H 0.6033 0.2370 0.0283 0.070 Uiso 1 1 calc R . .
H35B H 0.6452 0.2704 -0.0469 0.070 Uiso 1 1 calc R . .
C8 C -0.2969(5) 1.0183(4) 0.3987(2) 0.0465(12) Uani 1 1 d . . .
H8A H -0.2480 0.9500 0.4302 0.056 Uiso 1 1 calc R . .
H8B H -0.3119 1.0881 0.4114 0.056 Uiso 1 1 calc R . .
C34 C 0.4736(5) 0.2022(5) -0.0328(3) 0.0600(15) Uani 1 1 d . . .
H34A H 0.4414 0.1499 0.0017 0.072 Uiso 1 1 calc R . .
H34B H 0.4833 0.1833 -0.0736 0.072 Uiso 1 1 calc R . .
C45 C 0.1094(4) 0.1248(3) 0.2066(2) 0.0346(10) Uani 1 1 d . . .
H45 H 0.0230 0.1112 0.2087 0.041 Uiso 1 1 calc R . .
C46 C 0.1837(5) -0.0193(4) 0.1469(2) 0.0406(11) Uani 1 1 d . . .
H46 H 0.2238 -0.0993 0.1694 0.049 Uiso 1 1 calc R . .
C43 C 0.3671(4) 0.1585(3) 0.20197(19) 0.0304(9) Uani 1 1 d . . .
C23 C -0.2150(4) 0.6384(3) 0.42232(19) 0.0321(9) Uani 1 1 d . . .
H23 H -0.2412 0.6094 0.3914 0.038 Uiso 1 1 calc R . .
C14 C 0.2979(4) 0.4843(3) 0.38262(19) 0.0328(9) Uani 1 1 d . . .
C3 C 0.0173(4) 0.7515(3) 0.26703(19) 0.0319(9) Uani 1 1 d . . .
C42 C 0.2544(4) 0.2282(3) 0.23288(18) 0.0294(9) Uani 1 1 d . . .
C18 C -0.0373(4) 0.6645(3) 0.48266(18) 0.0272(8) Uani 1 1 d . . .
C19 C 0.2004(4) 0.5892(3) 0.46194(19) 0.0320(9) Uani 1 1 d . . .
H19 H 0.2932 0.5777 0.4720 0.038 Uiso 1 1 calc R . .
C15 C 0.1732(4) 0.5464(3) 0.41405(18) 0.0271(8) Uani 1 1 d . . .
C1 C -0.1939(4) 0.6976(3) 0.2370(2) 0.0369(10) Uani 1 1 d . . .
C27 C 0.3730(5) 0.4819(3) 0.15147(19) 0.0339(10) Uani 1 1 d . . .
C2 C -0.1290(4) 0.7706(3) 0.2627(2) 0.0323(9) Uani 1 1 d . . .
C5 C -0.0305(4) 0.9090(3) 0.3204(2) 0.0317(9) Uani 1 1 d . . .
C17 C -0.0735(4) 0.6222(3) 0.43426(17) 0.0261(8) Uani 1 1 d . . .
C4 C 0.0642(4) 0.8243(3) 0.29736(19) 0.0294(9) Uani 1 1 d . . .
C10 C 0.2074(4) 0.8084(3) 0.3038(2) 0.0348(10) Uani 1 1 d . . .
H10 H 0.2715 0.7529 0.2884 0.042 Uiso 1 1 calc R . .
C11 C 0.2514(4) 0.8743(4) 0.3327(2) 0.0377(10) Uani 1 1 d . . .
C13 C 0.0180(5) 0.9744(4) 0.3511(2) 0.0384(10) Uani 1 1 d . . .
H13 H -0.0446 1.0299 0.3671 0.046 Uiso 1 1 calc R . .
C7 C -0.2710(4) 1.0225(3) 0.3294(2) 0.0374(10) Uani 1 1 d . . .
H7 H -0.2736 1.0972 0.3012 0.045 Uiso 1 1 calc R . .
C9 C -0.4063(5) 1.0105(4) 0.3582(3) 0.0501(13) Uani 1 1 d . . .
H9A H -0.4878 1.0755 0.3463 0.060 Uiso 1 1 calc R . .
H9B H -0.4239 0.9374 0.3651 0.060 Uiso 1 1 calc R . .
C6 C -0.2159(4) 0.8585(3) 0.2842(2) 0.0354(10) Uani 1 1 d . . .
H6 H -0.3112 0.8725 0.2790 0.042 Uiso 1 1 calc R . .
C49 C 0.4999(4) 0.1747(4) 0.1980(2) 0.0381(10) Uani 1 1 d . . .
H49 H 0.5178 0.2280 0.2158 0.046 Uiso 1 1 calc R . .
C40 C -0.0058(5) 0.2663(3) 0.2641(2) 0.0393(11) Uani 1 1 d . . .
C12 C 0.1580(5) 0.9563(4) 0.3576(2) 0.0374(10) Uani 1 1 d . . .
C32 C 0.3805(5) 0.4019(3) 0.0593(2) 0.0356(10) Uani 1 1 d . . .
H32 H 0.4718 0.4056 0.0563 0.043 Uiso 1 1 calc R . .
C31 C 0.1993(4) 0.3537(3) 0.01807(19) 0.0312(9) Uani 1 1 d . . .
C33 C 0.4288(5) 0.3244(4) -0.0335(2) 0.0437(11) Uani 1 1 d . . .
H33 H 0.4140 0.3781 -0.0760 0.052 Uiso 1 1 calc R A 1
C39 C 0.1477(5) 0.3150(3) -0.0273(2) 0.0362(10) Uani 1 1 d . . .
H39 H 0.2033 0.2957 -0.0607 0.043 Uiso 1 1 calc R . .
C38 C 0.0153(5) 0.3056(3) -0.0225(2) 0.0367(10) Uani 1 1 d . . .
C20 C 0.1445(5) 0.6797(4) 0.5494(2) 0.0447(11) Uani 1 1 d . . .
H20 H 0.1339 0.6318 0.5919 0.054 Uiso 1 1 calc R . .
C22 C 0.1218(5) 0.7993(5) 0.5457(3) 0.0598(15) Uani 1 1 d . . .
H22A H 0.0961 0.8238 0.5846 0.072 Uiso 1 1 calc R . .
H22B H 0.0801 0.8545 0.5066 0.072 Uiso 1 1 calc R . .
C21 C 0.2652(5) 0.7243(5) 0.5426(3) 0.0581(15) Uani 1 1 d . . .
H21A H 0.3107 0.7337 0.5016 0.070 Uiso 1 1 calc R . .
H21B H 0.3267 0.7030 0.5796 0.070 Uiso 1 1 calc R . .
C28 C 0.3027(4) 0.4394(3) 0.10708(19) 0.0295(9) Uani 1 1 d . . .
C30 C 0.1134(4) 0.3874(3) 0.06698(18) 0.0295(9) Uani 1 1 d . . .
C41 C 0.1224(4) 0.2052(3) 0.23433(19) 0.0317(9) Uani 1 1 d . . .
C44 C 0.3428(4) 0.0769(3) 0.17474(19) 0.0317(9) Uani 1 1 d . . .
C52 C 0.4522(4) 0.0104(4) 0.1459(2) 0.0390(10) Uani 1 1 d . . .
H52 H 0.4380 -0.0461 0.1297 0.047 Uiso 1 1 calc R . .
C51 C 0.5799(4) 0.0299(4) 0.1420(2) 0.0407(11) Uani 1 1 d . . .
C50 C 0.6021(4) 0.1119(4) 0.1679(2) 0.0433(11) Uani 1 1 d . . .
C24 C -0.3128(4) 0.6964(4) 0.4560(2) 0.0346(10) Uani 1 1 d . . .
C47 C 0.1778(5) 0.0064(4) 0.0762(2) 0.0529(13) Uani 1 1 d . . .
H47A H 0.2151 -0.0559 0.0567 0.063 Uiso 1 1 calc R . .
H47B H 0.1901 0.0785 0.0518 0.063 Uiso 1 1 calc R . .
C48 C 0.0493(5) 0.0083(5) 0.1136(3) 0.0679(17) Uani 1 1 d . . .
H48A H -0.0169 0.0815 0.1120 0.082 Uiso 1 1 calc R . .
H48B H 0.0081 -0.0529 0.1168 0.082 Uiso 1 1 calc R . .
C36 C -0.0215(4) 0.3774(4) 0.0708(2) 0.0367(10) Uani 1 1 d . . .
H36 H -0.0793 0.3988 0.1031 0.044 Uiso 1 1 calc R B 1
F3 F -0.1984(3) 0.3271(3) 0.03079(15) 0.0644(8) Uani 1 1 d . . .
O1W O 0.5431(4) 0.3098(3) 0.3123(2) 0.0653(10) Uani 1 1 d G . .
H1WA H 0.4963 0.3430 0.3391 0.098 Uiso 1 1 d G C 2
H1WB H 0.5367 0.3570 0.2758 0.098 Uiso 1 1 d G D 2
O3W O 0.4156(4) 0.7243(3) 0.1849(2) 0.0725(12) Uani 1 1 d G . .
H3WA H 0.3966 0.6614 0.1933 0.109 Uiso 1 1 d G . .
H3WB H 0.5028 0.7121 0.1893 0.109 Uiso 1 1 d G . .
O2W O 0.6089(5) 0.5525(5) 0.3324(2) 0.0940(15) Uani 1 1 d G . .
H2WA H 0.5554 0.5250 0.3596 0.141 Uiso 1 1 d G E 2
H2WB H 0.5604 0.6035 0.3018 0.141 Uiso 1 1 d G F 2
K1 K 0.70139(16) 0.44917(15) 0.24194(8) 0.0796(5) Uani 0.90 1 d P G 1
K1' K 0.7448(18) 0.503(2) 0.1687(9) 0.135(9) Uani 0.10 1 d P H 2
C37 C -0.0685(4) 0.3362(4) 0.0273(2) 0.0390(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb2 O4 2.292(3) . ?
Tb2 O10 2.312(3) . ?
Tb2 O3 2.332(3) . ?
Tb2 O7 2.361(3) . ?
Tb2 O9 2.367(3) . ?
Tb2 O1 2.388(3) . ?
Tb2 O6 2.451(3) . ?
Tb2 O12 2.480(3) . ?
Cl1 C12 1.727(4) . ?
Cl3 C38 1.723(4) . ?
Cl2 C25 1.724(4) . ?
Cl4 C51 1.734(4) . ?
F2 C24 1.352(5) . ?
F4 C50 1.351(5) . ?
O10 C40 1.269(5) . ?
O1 C1 1.259(5) . ?
O3 C3 1.262(4) . ?
O4 C14 1.264(5) . ?
O5 C14 1.231(5) . ?
O6 C16 1.252(4) . ?
O9 C29 1.254(4) . ?
O7 C27 1.264(5) . ?
O12 C42 1.253(5) . ?
O2 C1 1.250(5) . ?
O8 C27 1.241(5) . ?
O11 C40 1.232(5) . ?
N4 C45 1.343(5) . ?
N4 C44 1.393(5) . ?
N4 C46 1.460(5) . ?
N3 C32 1.345(5) . ?
N3 C31 1.397(5) . ?
N3 C33 1.463(5) . ?
N2 C19 1.344(5) . ?
N2 C18 1.396(5) . ?
N2 C20 1.460(5) . ?
N1 C6 1.344(5) . ?
N1 C5 1.398(5) . ?
N1 C7 1.464(5) . ?
C16 C15 1.423(5) . ?
C16 C17 1.469(5) . ?
C25 C26 1.374(6) . ?
C25 C24 1.389(6) . ?
C26 C18 1.399(5) . ?
C26 H26 0.9300 . ?
C29 C28 1.432(6) . ?
C29 C30 1.465(5) . ?
F1 C11 1.350(5) . ?
C35 C33 1.475(7) . ?
C35 C34 1.487(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C8 C9 1.487(7) . ?
C8 C7 1.497(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C34 C33 1.488(7) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C45 C41 1.359(6) . ?
C45 H45 0.9300 . ?
C46 C48 1.472(7) . ?
C46 C47 1.479(7) . ?
C46 H46 0.9800 . ?
C43 C49 1.403(6) . ?
C43 C44 1.409(5) . ?
C43 C42 1.472(5) . ?
C23 C24 1.352(5) . ?
C23 C17 1.405(5) . ?
C23 H23 0.9300 . ?
C14 C15 1.508(5) . ?
C3 C2 1.422(6) . ?
C3 C4 1.461(6) . ?
C42 C41 1.437(6) . ?
C18 C17 1.409(5) . ?
C19 C15 1.368(5) . ?
C19 H19 0.9300 . ?
C1 C2 1.510(6) . ?
C27 C28 1.515(5) . ?
C2 C6 1.378(5) . ?
C5 C4 1.400(5) . ?
C5 C13 1.395(6) . ?
C4 C10 1.403(6) . ?
C10 C11 1.350(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.392(6) . ?
C13 C12 1.367(6) . ?
C13 H13 0.9300 . ?
C7 C9 1.494(6) . ?
C7 H7 0.9800 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C6 H6 0.9300 . ?
C49 C50 1.359(6) . ?
C49 H49 0.9300 . ?
C40 C41 1.508(5) . ?
C32 C28 1.366(5) . ?
C32 H32 0.9300 . ?
C31 C39 1.395(6) . ?
C31 C30 1.406(5) . ?
C33 H33 0.9800 . ?
C39 C38 1.366(6) . ?
C39 H39 0.9300 . ?
C38 C37 1.399(6) . ?
C20 C22 1.457(7) . ?
C20 C21 1.468(7) . ?
C20 H20 0.9800 . ?
C22 C21 1.490(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C30 C36 1.395(6) . ?
C44 C52 1.406(5) . ?
C52 C51 1.370(6) . ?
C52 H52 0.9300 . ?
C51 C50 1.386(6) . ?
C47 C48 1.483(7) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C36 C37 1.359(6) . ?
C36 H36 0.9300 . ?
F3 C37 1.340(5) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8501 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb2 O10 108.25(12) . . ?
O4 Tb2 O3 82.69(11) . . ?
O10 Tb2 O3 148.01(10) . . ?
O4 Tb2 O7 81.08(10) . . ?
O10 Tb2 O7 138.27(9) . . ?
O3 Tb2 O7 72.03(9) . . ?
O4 Tb2 O9 143.63(9) . . ?
O10 Tb2 O9 78.50(10) . . ?
O3 Tb2 O9 110.84(11) . . ?
O7 Tb2 O9 72.18(9) . . ?
O4 Tb2 O1 139.61(9) . . ?
O10 Tb2 O1 81.69(10) . . ?
O3 Tb2 O1 71.73(10) . . ?
O7 Tb2 O1 117.93(10) . . ?
O9 Tb2 O1 76.08(9) . . ?
O4 Tb2 O6 70.63(9) . . ?
O10 Tb2 O6 78.52(9) . . ?
O3 Tb2 O6 77.11(10) . . ?
O7 Tb2 O6 140.29(9) . . ?
O9 Tb2 O6 144.00(9) . . ?
O1 Tb2 O6 73.47(9) . . ?
O4 Tb2 O12 74.35(9) . . ?
O10 Tb2 O12 70.96(10) . . ?
O3 Tb2 O12 140.53(10) . . ?
O7 Tb2 O12 73.00(10) . . ?
O9 Tb2 O12 74.53(9) . . ?
O1 Tb2 O12 143.06(9) . . ?
O6 Tb2 O12 122.45(9) . . ?
C40 O10 Tb2 136.5(3) . . ?
C1 O1 Tb2 135.0(3) . . ?
C3 O3 Tb2 128.6(3) . . ?
C14 O4 Tb2 140.8(2) . . ?
C16 O6 Tb2 129.9(2) . . ?
C29 O9 Tb2 132.2(3) . . ?
C27 O7 Tb2 134.4(3) . . ?
C42 O12 Tb2 126.9(2) . . ?
C45 N4 C44 119.0(3) . . ?
C45 N4 C46 121.4(4) . . ?
C44 N4 C46 119.6(3) . . ?
C32 N3 C31 119.7(3) . . ?
C32 N3 C33 120.3(4) . . ?
C31 N3 C33 120.0(3) . . ?
C19 N2 C18 119.5(3) . . ?
C19 N2 C20 120.2(3) . . ?
C18 N2 C20 120.1(3) . . ?
C6 N1 C5 120.0(3) . . ?
C6 N1 C7 121.5(3) . . ?
C5 N1 C7 118.3(3) . . ?
O6 C16 C15 125.7(3) . . ?
O6 C16 C17 118.9(3) . . ?
C15 C16 C17 115.4(3) . . ?
C26 C25 C24 119.8(4) . . ?
C26 C25 Cl2 120.1(3) . . ?
C24 C25 Cl2 120.1(3) . . ?
C25 C26 C18 119.3(4) . . ?
C25 C26 H26 120.3 . . ?
C18 C26 H26 120.3 . . ?
O9 C29 C28 126.1(3) . . ?
O9 C29 C30 117.8(4) . . ?
C28 C29 C30 116.1(3) . . ?
C33 C35 C34 60.3(3) . . ?
C33 C35 H35A 117.7 . . ?
C34 C35 H35A 117.7 . . ?
C33 C35 H35B 117.7 . . ?
C34 C35 H35B 117.7 . . ?
H35A C35 H35B 114.9 . . ?
C9 C8 C7 60.1(3) . . ?
C9 C8 H8A 117.8 . . ?
C7 C8 H8A 117.8 . . ?
C9 C8 H8B 117.8 . . ?
C7 C8 H8B 117.8 . . ?
H8A C8 H8B 114.9 . . ?
C35 C34 C33 59.5(3) . . ?
C35 C34 H34A 117.8 . . ?
C33 C34 H34A 117.8 . . ?
C35 C34 H34B 117.8 . . ?
C33 C34 H34B 117.8 . . ?
H34A C34 H34B 115.0 . . ?
N4 C45 C41 125.9(4) . . ?
N4 C45 H45 117.0 . . ?
C41 C45 H45 117.0 . . ?
N4 C46 C48 118.9(4) . . ?
N4 C46 C47 118.9(4) . . ?
C48 C46 C47 60.3(4) . . ?
N4 C46 H46 115.8 . . ?
C48 C46 H46 115.8 . . ?
C47 C46 H46 115.8 . . ?
C49 C43 C44 119.1(4) . . ?
C49 C43 C42 120.0(4) . . ?
C44 C43 C42 120.9(4) . . ?
C24 C23 C17 119.7(4) . . ?
C24 C23 H23 120.2 . . ?
C17 C23 H23 120.2 . . ?
O5 C14 O4 124.4(4) . . ?
O5 C14 C15 118.0(4) . . ?
O4 C14 C15 117.6(4) . . ?
O3 C3 C2 125.8(4) . . ?
O3 C3 C4 117.6(4) . . ?
C2 C3 C4 116.5(3) . . ?
O12 C42 C41 124.9(3) . . ?
O12 C42 C43 119.4(4) . . ?
C41 C42 C43 115.7(3) . . ?
N2 C18 C26 120.8(3) . . ?
N2 C18 C17 118.8(3) . . ?
C26 C18 C17 120.4(4) . . ?
N2 C19 C15 125.0(4) . . ?
N2 C19 H19 117.5 . . ?
C15 C19 H19 117.5 . . ?
C19 C15 C16 119.8(3) . . ?
C19 C15 C14 116.3(3) . . ?
C16 C15 C14 123.8(3) . . ?
O2 C1 O1 123.9(4) . . ?
O2 C1 C2 117.0(4) . . ?
O1 C1 C2 119.1(4) . . ?
O8 C27 O7 124.9(4) . . ?
O8 C27 C28 117.2(4) . . ?
O7 C27 C28 117.9(4) . . ?
C6 C2 C3 118.7(4) . . ?
C6 C2 C1 118.2(4) . . ?
C3 C2 C1 123.1(3) . . ?
N1 C5 C4 118.5(4) . . ?
N1 C5 C13 121.5(4) . . ?
C4 C5 C13 119.9(4) . . ?
C23 C17 C18 118.7(3) . . ?
C23 C17 C16 119.9(3) . . ?
C18 C17 C16 121.5(3) . . ?
C5 C4 C10 119.3(4) . . ?
C5 C4 C3 121.4(4) . . ?
C10 C4 C3 119.2(3) . . ?
C11 C10 C4 119.5(4) . . ?
C11 C10 H10 120.3 . . ?
C4 C10 H10 120.3 . . ?
F1 C11 C10 119.7(4) . . ?
F1 C11 C12 118.8(4) . . ?
C10 C11 C12 121.5(4) . . ?
C12 C13 C5 119.6(4) . . ?
C12 C13 H13 120.2 . . ?
C5 C13 H13 120.2 . . ?
N1 C7 C9 119.0(4) . . ?
N1 C7 C8 119.2(4) . . ?
C9 C7 C8 59.6(3) . . ?
N1 C7 H7 115.8 . . ?
C9 C7 H7 115.8 . . ?
C8 C7 H7 115.8 . . ?
C8 C9 C7 60.3(3) . . ?
C8 C9 H9A 117.7 . . ?
C7 C9 H9A 117.7 . . ?
C8 C9 H9B 117.7 . . ?
C7 C9 H9B 117.7 . . ?
H9A C9 H9B 114.9 . . ?
N1 C6 C2 124.7(4) . . ?
N1 C6 H6 117.7 . . ?
C2 C6 H6 117.7 . . ?
C50 C49 C43 119.6(4) . . ?
C50 C49 H49 120.2 . . ?
C43 C49 H49 120.2 . . ?
O11 C40 O10 123.7(4) . . ?
O11 C40 C41 117.3(4) . . ?
O10 C40 C41 119.1(4) . . ?
C13 C12 C11 120.1(4) . . ?
C13 C12 Cl1 120.8(3) . . ?
C11 C12 Cl1 119.1(3) . . ?
N3 C32 C28 125.4(4) . . ?
N3 C32 H32 117.3 . . ?
C28 C32 H32 117.3 . . ?
N3 C31 C39 121.4(4) . . ?
N3 C31 C30 118.5(3) . . ?
C39 C31 C30 120.1(4) . . ?
N3 C33 C35 119.3(4) . . ?
N3 C33 C34 118.8(4) . . ?
C35 C33 C34 60.2(3) . . ?
N3 C33 H33 115.7 . . ?
C35 C33 H33 115.7 . . ?
C34 C33 H33 115.7 . . ?
C38 C39 C31 119.8(4) . . ?
C38 C39 H39 120.1 . . ?
C31 C39 H39 120.1 . . ?
C39 C38 C37 119.9(4) . . ?
C39 C38 Cl3 120.6(3) . . ?
C37 C38 Cl3 119.5(3) . . ?
N2 C20 C22 120.0(4) . . ?
N2 C20 C21 118.7(4) . . ?
C22 C20 C21 61.2(3) . . ?
N2 C20 H20 115.4 . . ?
C22 C20 H20 115.4 . . ?
C21 C20 H20 115.4 . . ?
C20 C22 C21 59.7(3) . . ?
C20 C22 H22A 117.8 . . ?
C21 C22 H22A 117.8 . . ?
C20 C22 H22B 117.8 . . ?
C21 C22 H22B 117.8 . . ?
H22A C22 H22B 114.9 . . ?
C20 C21 C22 59.0(3) . . ?
C20 C21 H21A 117.9 . . ?
C22 C21 H21A 117.9 . . ?
C20 C21 H21B 117.9 . . ?
C22 C21 H21B 117.9 . . ?
H21A C21 H21B 115.0 . . ?
C32 C28 C29 118.7(4) . . ?
C32 C28 C27 117.3(4) . . ?
C29 C28 C27 124.0(3) . . ?
C36 C30 C31 119.0(4) . . ?
C36 C30 C29 119.5(4) . . ?
C31 C30 C29 121.5(4) . . ?
C45 C41 C42 119.0(3) . . ?
C45 C41 C40 116.9(4) . . ?
C42 C41 C40 124.1(4) . . ?
N4 C44 C52 120.6(4) . . ?
N4 C44 C43 119.4(3) . . ?
C52 C44 C43 120.0(4) . . ?
C51 C52 C44 119.3(4) . . ?
C51 C52 H52 120.4 . . ?
C44 C52 H52 120.4 . . ?
C52 C51 C50 120.3(4) . . ?
C52 C51 Cl4 120.2(3) . . ?
C50 C51 Cl4 119.5(4) . . ?
F4 C50 C49 119.7(4) . . ?
F4 C50 C51 118.5(4) . . ?
C49 C50 C51 121.7(4) . . ?
F2 C24 C23 120.0(4) . . ?
F2 C24 C25 118.0(3) . . ?
C23 C24 C25 122.0(4) . . ?
C46 C47 C48 59.6(3) . . ?
C46 C47 H47A 117.8 . . ?
C48 C47 H47A 117.8 . . ?
C46 C47 H47B 117.8 . . ?
C48 C47 H47B 117.8 . . ?
H47A C47 H47B 114.9 . . ?
C46 C48 C47 60.1(3) . . ?
C46 C48 H48A 117.8 . . ?
C47 C48 H48A 117.8 . . ?
C46 C48 H48B 117.8 . . ?
C47 C48 H48B 117.8 . . ?
H48A C48 H48B 114.9 . . ?
C37 C36 C30 120.0(4) . . ?
C37 C36 H36 120.0 . . ?
C30 C36 H36 120.0 . . ?
H1WA O1W H1WB 109.5 . . ?
H3WA O3W H3WB 109.5 . . ?
H2WA O2W H2WB 109.5 . . ?
F3 C37 C36 119.9(4) . . ?
F3 C37 C38 118.9(4) . . ?
C36 C37 C38 121.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Tb2 O10 C40 -106.5(4) . . . . ?
O3 Tb2 O10 C40 147.6(4) . . . . ?
O7 Tb2 O10 C40 -9.3(5) . . . . ?
O9 Tb2 O10 C40 36.5(4) . . . . ?
O1 Tb2 O10 C40 113.9(4) . . . . ?
O6 Tb2 O10 C40 -171.4(4) . . . . ?
O12 Tb2 O10 C40 -40.9(4) . . . . ?
O4 Tb2 O1 C1 18.2(5) . . . . ?
O10 Tb2 O1 C1 126.7(4) . . . . ?
O3 Tb2 O1 C1 -35.3(4) . . . . ?
O7 Tb2 O1 C1 -92.4(4) . . . . ?
O9 Tb2 O1 C1 -153.2(4) . . . . ?
O6 Tb2 O1 C1 46.2(4) . . . . ?
O12 Tb2 O1 C1 168.7(4) . . . . ?
O4 Tb2 O3 C3 -105.8(4) . . . . ?
O10 Tb2 O3 C3 7.2(5) . . . . ?
O7 Tb2 O3 C3 171.2(4) . . . . ?
O9 Tb2 O3 C3 109.1(3) . . . . ?
O1 Tb2 O3 C3 42.5(3) . . . . ?
O6 Tb2 O3 C3 -34.1(3) . . . . ?
O12 Tb2 O3 C3 -160.1(3) . . . . ?
O10 Tb2 O4 C14 -105.6(5) . . . . ?
O3 Tb2 O4 C14 43.5(5) . . . . ?
O7 Tb2 O4 C14 116.4(5) . . . . ?
O9 Tb2 O4 C14 159.0(4) . . . . ?
O1 Tb2 O4 C14 -6.8(6) . . . . ?
O6 Tb2 O4 C14 -35.3(5) . . . . ?
O12 Tb2 O4 C14 -168.9(5) . . . . ?
O4 Tb2 O6 C16 33.2(3) . . . . ?
O10 Tb2 O6 C16 147.4(3) . . . . ?
O3 Tb2 O6 C16 -53.5(3) . . . . ?
O7 Tb2 O6 C16 -13.9(4) . . . . ?
O9 Tb2 O6 C16 -161.3(3) . . . . ?
O1 Tb2 O6 C16 -127.9(3) . . . . ?
O12 Tb2 O6 C16 89.0(3) . . . . ?
O4 Tb2 O9 C29 -14.8(4) . . . . ?
O10 Tb2 O9 C29 -120.0(4) . . . . ?
O3 Tb2 O9 C29 91.9(3) . . . . ?
O7 Tb2 O9 C29 29.9(3) . . . . ?
O1 Tb2 O9 C29 155.8(4) . . . . ?
O6 Tb2 O9 C29 -171.3(3) . . . . ?
O12 Tb2 O9 C29 -46.8(3) . . . . ?
O4 Tb2 O7 C27 114.3(4) . . . . ?
O10 Tb2 O7 C27 6.8(4) . . . . ?
O3 Tb2 O7 C27 -160.6(4) . . . . ?
O9 Tb2 O7 C27 -40.8(4) . . . . ?
O1 Tb2 O7 C27 -103.6(4) . . . . ?
O6 Tb2 O7 C27 158.7(3) . . . . ?
O12 Tb2 O7 C27 38.0(4) . . . . ?
O4 Tb2 O12 C42 157.1(3) . . . . ?
O10 Tb2 O12 C42 40.9(3) . . . . ?
O3 Tb2 O12 C42 -146.2(3) . . . . ?
O7 Tb2 O12 C42 -117.7(3) . . . . ?
O9 Tb2 O12 C42 -42.0(3) . . . . ?
O1 Tb2 O12 C42 -3.6(4) . . . . ?
O6 Tb2 O12 C42 103.0(3) . . . . ?
Tb2 O6 C16 C15 -27.1(6) . . . . ?
Tb2 O6 C16 C17 153.0(3) . . . . ?
C24 C25 C26 C18 2.8(6) . . . . ?
Cl2 C25 C26 C18 -176.4(3) . . . . ?
Tb2 O9 C29 C28 -21.6(6) . . . . ?
Tb2 O9 C29 C30 158.1(3) . . . . ?
C44 N4 C45 C41 2.9(6) . . . . ?
C46 N4 C45 C41 -178.3(4) . . . . ?
C45 N4 C46 C48 38.3(6) . . . . ?
C44 N4 C46 C48 -142.9(5) . . . . ?
C45 N4 C46 C47 108.4(5) . . . . ?
C44 N4 C46 C47 -72.9(5) . . . . ?
Tb2 O4 C14 O5 -156.6(4) . . . . ?
Tb2 O4 C14 C15 25.1(7) . . . . ?
Tb2 O3 C3 C2 -39.0(6) . . . . ?
Tb2 O3 C3 C4 139.0(3) . . . . ?
Tb2 O12 C42 C41 -32.6(6) . . . . ?
Tb2 O12 C42 C43 145.9(3) . . . . ?
C49 C43 C42 O12 1.2(6) . . . . ?
C44 C43 C42 O12 -177.3(4) . . . . ?
C49 C43 C42 C41 179.8(4) . . . . ?
C44 C43 C42 C41 1.3(6) . . . . ?
C19 N2 C18 C26 179.0(4) . . . . ?
C20 N2 C18 C26 5.0(6) . . . . ?
C19 N2 C18 C17 -0.2(6) . . . . ?
C20 N2 C18 C17 -174.2(4) . . . . ?
C25 C26 C18 N2 179.1(4) . . . . ?
C25 C26 C18 C17 -1.7(6) . . . . ?
C18 N2 C19 C15 0.7(6) . . . . ?
C20 N2 C19 C15 174.7(4) . . . . ?
N2 C19 C15 C16 -0.7(6) . . . . ?
N2 C19 C15 C14 -179.7(4) . . . . ?
O6 C16 C15 C19 -179.9(4) . . . . ?
C17 C16 C15 C19 0.1(5) . . . . ?
O6 C16 C15 C14 -0.9(6) . . . . ?
C17 C16 C15 C14 179.1(4) . . . . ?
O5 C14 C15 C19 5.7(6) . . . . ?
O4 C14 C15 C19 -175.9(4) . . . . ?
O5 C14 C15 C16 -173.3(4) . . . . ?
O4 C14 C15 C16 5.1(6) . . . . ?
Tb2 O1 C1 O2 -158.5(4) . . . . ?
Tb2 O1 C1 C2 20.2(6) . . . . ?
Tb2 O7 C27 O8 -142.2(4) . . . . ?
Tb2 O7 C27 C28 38.6(6) . . . . ?
O3 C3 C2 C6 -179.0(4) . . . . ?
C4 C3 C2 C6 3.0(6) . . . . ?
O3 C3 C2 C1 2.4(7) . . . . ?
C4 C3 C2 C1 -175.6(4) . . . . ?
O2 C1 C2 C6 7.7(6) . . . . ?
O1 C1 C2 C6 -171.0(4) . . . . ?
O2 C1 C2 C3 -173.6(4) . . . . ?
O1 C1 C2 C3 7.6(6) . . . . ?
C6 N1 C5 C4 1.5(6) . . . . ?
C7 N1 C5 C4 -172.8(4) . . . . ?
C6 N1 C5 C13 -177.9(4) . . . . ?
C7 N1 C5 C13 7.8(6) . . . . ?
C24 C23 C17 C18 1.8(6) . . . . ?
C24 C23 C17 C16 -179.2(4) . . . . ?
N2 C18 C17 C23 178.6(4) . . . . ?
C26 C18 C17 C23 -0.6(6) . . . . ?
N2 C18 C17 C16 -0.3(6) . . . . ?
C26 C18 C17 C16 -179.6(4) . . . . ?
O6 C16 C17 C23 1.4(5) . . . . ?
C15 C16 C17 C23 -178.6(4) . . . . ?
O6 C16 C17 C18 -179.7(4) . . . . ?
C15 C16 C17 C18 0.4(5) . . . . ?
N1 C5 C4 C10 178.7(4) . . . . ?
C13 C5 C4 C10 -1.9(6) . . . . ?
N1 C5 C4 C3 -1.7(6) . . . . ?
C13 C5 C4 C3 177.7(4) . . . . ?
O3 C3 C4 C5 -178.7(4) . . . . ?
C2 C3 C4 C5 -0.5(6) . . . . ?
O3 C3 C4 C10 0.9(6) . . . . ?
C2 C3 C4 C10 179.1(4) . . . . ?
C5 C4 C10 C11 0.6(6) . . . . ?
C3 C4 C10 C11 -179.0(4) . . . . ?
C4 C10 C11 F1 -177.6(4) . . . . ?
C4 C10 C11 C12 1.5(7) . . . . ?
N1 C5 C13 C12 -179.5(4) . . . . ?
C4 C5 C13 C12 1.1(6) . . . . ?
C6 N1 C7 C9 41.4(6) . . . . ?
C5 N1 C7 C9 -144.4(4) . . . . ?
C6 N1 C7 C8 110.7(5) . . . . ?
C5 N1 C7 C8 -75.1(5) . . . . ?
C9 C8 C7 N1 -108.5(4) . . . . ?
N1 C7 C9 C8 108.7(5) . . . . ?
C5 N1 C6 C2 1.1(7) . . . . ?
C7 N1 C6 C2 175.2(4) . . . . ?
C3 C2 C6 N1 -3.4(7) . . . . ?
C1 C2 C6 N1 175.3(4) . . . . ?
C44 C43 C49 C50 0.2(6) . . . . ?
C42 C43 C49 C50 -178.3(4) . . . . ?
Tb2 O10 C40 O11 -151.0(4) . . . . ?
Tb2 O10 C40 C41 27.5(6) . . . . ?
C5 C13 C12 C11 1.0(7) . . . . ?
C5 C13 C12 Cl1 -179.9(3) . . . . ?
F1 C11 C12 C13 176.7(4) . . . . ?
C10 C11 C12 C13 -2.4(7) . . . . ?
F1 C11 C12 Cl1 -2.3(6) . . . . ?
C10 C11 C12 Cl1 178.6(4) . . . . ?
C31 N3 C32 C28 0.7(7) . . . . ?
C33 N3 C32 C28 178.8(4) . . . . ?
C32 N3 C31 C39 177.4(4) . . . . ?
C33 N3 C31 C39 -0.7(6) . . . . ?
C32 N3 C31 C30 -2.6(6) . . . . ?
C33 N3 C31 C30 179.3(4) . . . . ?
C32 N3 C33 C35 44.3(6) . . . . ?
C31 N3 C33 C35 -137.6(4) . . . . ?
C32 N3 C33 C34 114.4(5) . . . . ?
C31 N3 C33 C34 -67.5(6) . . . . ?
C34 C35 C33 N3 108.4(5) . . . . ?
C35 C34 C33 N3 -109.2(5) . . . . ?
N3 C31 C39 C38 177.3(4) . . . . ?
C30 C31 C39 C38 -2.7(6) . . . . ?
C31 C39 C38 C37 0.8(6) . . . . ?
C31 C39 C38 Cl3 -179.8(3) . . . . ?
C19 N2 C20 C22 113.4(5) . . . . ?
C18 N2 C20 C22 -72.6(6) . . . . ?
C19 N2 C20 C21 41.9(6) . . . . ?
C18 N2 C20 C21 -144.1(4) . . . . ?
N2 C20 C22 C21 -108.4(5) . . . . ?
N2 C20 C21 C22 110.5(5) . . . . ?
N3 C32 C28 C29 0.7(7) . . . . ?
N3 C32 C28 C27 179.0(4) . . . . ?
O9 C29 C28 C32 179.5(4) . . . . ?
C30 C29 C28 C32 -0.3(5) . . . . ?
O9 C29 C28 C27 1.3(6) . . . . ?
C30 C29 C28 C27 -178.4(4) . . . . ?
O8 C27 C28 C32 -5.9(6) . . . . ?
O7 C27 C28 C32 173.3(4) . . . . ?
O8 C27 C28 C29 172.3(4) . . . . ?
O7 C27 C28 C29 -8.5(6) . . . . ?
N3 C31 C30 C36 -177.5(4) . . . . ?
C39 C31 C30 C36 2.5(6) . . . . ?
N3 C31 C30 C29 3.0(6) . . . . ?
C39 C31 C30 C29 -177.0(4) . . . . ?
O9 C29 C30 C36 -0.8(6) . . . . ?
C28 C29 C30 C36 178.9(4) . . . . ?
O9 C29 C30 C31 178.6(4) . . . . ?
C28 C29 C30 C31 -1.6(6) . . . . ?
N4 C45 C41 C42 -0.7(7) . . . . ?
N4 C45 C41 C40 178.5(4) . . . . ?
O12 C42 C41 C45 177.1(4) . . . . ?
C43 C42 C41 C45 -1.4(6) . . . . ?
O12 C42 C41 C40 -1.9(6) . . . . ?
C43 C42 C41 C40 179.5(4) . . . . ?
O11 C40 C41 C45 7.5(6) . . . . ?
O10 C40 C41 C45 -171.2(4) . . . . ?
O11 C40 C41 C42 -173.4(4) . . . . ?
O10 C40 C41 C42 7.9(6) . . . . ?
C45 N4 C44 C52 177.4(4) . . . . ?
C46 N4 C44 C52 -1.4(6) . . . . ?
C45 N4 C44 C43 -2.8(6) . . . . ?
C46 N4 C44 C43 178.4(4) . . . . ?
C49 C43 C44 N4 -177.8(4) . . . . ?
C42 C43 C44 N4 0.8(6) . . . . ?
C49 C43 C44 C52 2.0(6) . . . . ?
C42 C43 C44 C52 -179.5(4) . . . . ?
N4 C44 C52 C51 176.7(4) . . . . ?
C43 C44 C52 C51 -3.1(7) . . . . ?
C44 C52 C51 C50 1.9(7) . . . . ?
C44 C52 C51 Cl4 -177.0(3) . . . . ?
C43 C49 C50 F4 179.7(4) . . . . ?
C43 C49 C50 C51 -1.5(7) . . . . ?
C52 C51 C50 F4 179.3(4) . . . . ?
Cl4 C51 C50 F4 -1.8(6) . . . . ?
C52 C51 C50 C49 0.4(7) . . . . ?
Cl4 C51 C50 C49 179.3(4) . . . . ?
C17 C23 C24 F2 179.6(4) . . . . ?
C17 C23 C24 C25 -0.7(6) . . . . ?
C26 C25 C24 F2 178.0(4) . . . . ?
Cl2 C25 C24 F2 -2.8(6) . . . . ?
C26 C25 C24 C23 -1.7(7) . . . . ?
Cl2 C25 C24 C23 177.5(3) . . . . ?
N4 C46 C47 C48 -108.7(5) . . . . ?
N4 C46 C48 C47 108.8(5) . . . . ?
C31 C30 C36 C37 -0.5(6) . . . . ?
C29 C30 C36 C37 179.0(4) . . . . ?
C30 C36 C37 F3 -179.7(4) . . . . ?
C30 C36 C37 C38 -1.3(7) . . . . ?
C39 C38 C37 F3 179.5(4) . . . . ?
Cl3 C38 C37 F3 0.2(6) . . . . ?
C39 C38 C37 C36 1.2(7) . . . . ?
Cl3 C38 C37 C36 -178.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.687
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.082

# start Validation Reply Form 
_vrf_PLAT420_2c                  
;
PROBLEM: 
RESPONSE: Disorder of the H1WB. 
;
_vrf_PLAT910_2c                  
;
PROBLEM: 
RESPONSE: The diffractions were collected at room temperature. 
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1d
_database_code_depnum_ccdc_archive 'CCDC 1855009'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 Cl4 F4 Ho N4 Na O16'
_chemical_formula_weight         1382.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2180 4.6780 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0360 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0685(2)
_cell_length_b                   12.7366(3)
_cell_length_c                   22.0035(7)
_cell_angle_alpha                73.668(2)
_cell_angle_beta                 85.270(2)
_cell_angle_gamma                72.024(2)
_cell_volume                     2575.63(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15835
_cell_measurement_theta_min      3.3980
_cell_measurement_theta_max      28.9130

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1380
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7325
_exptl_absorpt_correction_T_max  0.7568
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19587
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         25.01
_reflns_number_total             8802
_reflns_number_gt                8050
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0566P)²+0.5129P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8802
_refine_ls_number_parameters     745
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0957
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.010
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho2 Ho 0.377930(16) 0.010603(14) 0.241342(8) 0.02765(8) Uani 1 1 d . . .
Cl4 Cl 0.91485(12) -0.31624(11) -0.03944(7) 0.0546(3) Uani 1 1 d . . .
Cl3 Cl 0.26271(13) -0.54287(12) 0.10507(8) 0.0660(4) Uani 1 1 d . . .
Cl1 Cl -0.22100(12) 0.56348(12) 0.38923(7) 0.0619(4) Uani 1 1 d . . .
Cl2 Cl 0.54003(12) 0.24764(12) 0.56460(7) 0.0565(3) Uani 1 1 d . . .
O3 O 0.2180(3) 0.1974(2) 0.24512(14) 0.0354(7) Uani 1 1 d . . .
O7 O 0.5949(3) -0.1208(2) 0.27332(14) 0.0385(7) Uani 1 1 d . . .
O10 O 0.2168(3) 0.0578(2) 0.16366(14) 0.0412(7) Uani 1 1 d . . .
O4 O 0.1977(3) -0.0292(2) 0.30689(14) 0.0365(7) Uani 1 1 d . . .
O1 O 0.4986(3) 0.1435(2) 0.21534(15) 0.0404(7) Uani 1 1 d . . .
O12 O 0.4980(3) -0.0211(2) 0.14510(13) 0.0329(6) Uani 1 1 d . . .
F1 F -0.2385(3) 0.3890(3) 0.33082(17) 0.0672(9) Uani 1 1 d . . .
F3 F 0.0918(3) -0.3658(2) 0.16160(15) 0.0616(8) Uani 1 1 d . . .
O6 O 0.4170(3) 0.0300(2) 0.34045(13) 0.0341(6) Uani 1 1 d . . .
F4 F 0.9495(3) -0.2040(3) 0.05380(14) 0.0595(8) Uani 1 1 d . . .
N4 N 0.3993(3) -0.1478(3) 0.00916(17) 0.0357(8) Uani 1 1 d . . .
N1 N 0.2883(3) 0.4365(3) 0.32042(18) 0.0355(8) Uani 1 1 d . . .
C51 C 0.7829(4) -0.2380(4) -0.0011(2) 0.0382(10) Uani 1 1 d . . .
O9 O 0.3696(3) -0.1718(2) 0.24087(15) 0.0404(7) Uani 1 1 d . . .
C42 C 0.4628(4) -0.0575(3) 0.10391(18) 0.0278(8) Uani 1 1 d . . .
C31 C 0.5118(4) -0.4133(3) 0.1747(2) 0.0338(9) Uani 1 1 d . . .
O11 O 0.0810(3) 0.0200(3) 0.10387(16) 0.0553(9) Uani 1 1 d . . .
C12 C -0.0859(4) 0.4823(4) 0.3525(2) 0.0409(11) Uani 1 1 d . . .
C18 C 0.2936(4) 0.1476(3) 0.47417(19) 0.0298(9) Uani 1 1 d . . .
N2 N 0.1565(3) 0.1435(3) 0.47666(16) 0.0334(8) Uani 1 1 d . . .
C41 C 0.3238(4) -0.0470(3) 0.08896(18) 0.0278(8) Uani 1 1 d . . .
F2 F 0.6963(3) 0.1633(3) 0.46152(15) 0.0643(9) Uani 1 1 d . . .
C24 C 0.5638(4) 0.1575(4) 0.4656(2) 0.0372(10) Uani 1 1 d . . .
C52 C 0.6459(4) -0.2221(3) -0.0137(2) 0.0360(10) Uani 1 1 d . . .
H52 H 0.6238 -0.2500 -0.0451 0.043 Uiso 1 1 calc R . .
C26 C 0.3431(4) 0.1893(3) 0.5175(2) 0.0344(10) Uani 1 1 d . . .
H26 H 0.2855 0.2124 0.5496 0.041 Uiso 1 1 calc R . .
N3 N 0.6537(3) -0.4309(3) 0.18144(17) 0.0351(8) Uani 1 1 d . . .
C40 C 0.1965(4) 0.0145(4) 0.1215(2) 0.0350(10) Uani 1 1 d . . .
O5 O -0.0053(3) 0.0392(3) 0.35008(18) 0.0651(11) Uani 1 1 d . . .
O8 O 0.8037(3) -0.2271(3) 0.25154(19) 0.0586(10) Uani 1 1 d . . .
C16 C 0.3345(4) 0.0626(3) 0.38247(18) 0.0278(8) Uani 1 1 d . . .
C3 C 0.2423(4) 0.2718(3) 0.26599(19) 0.0303(9) Uani 1 1 d . . .
C6 C 0.3906(4) 0.3708(4) 0.2919(2) 0.0388(10) Uani 1 1 d . . .
H6 H 0.4787 0.3807 0.2905 0.047 Uiso 1 1 calc R . .
C45 C 0.2988(4) -0.0898(3) 0.0426(2) 0.0351(10) Uani 1 1 d . . .
H45 H 0.2062 -0.0785 0.0331 0.042 Uiso 1 1 calc R . .
C23 C 0.5202(4) 0.1142(4) 0.4234(2) 0.0358(10) Uani 1 1 d . . .
H23 H 0.5807 0.0885 0.3928 0.043 Uiso 1 1 calc R . .
C32 C 0.6952(4) -0.3630(3) 0.2078(2) 0.0348(9) Uani 1 1 d . . .
H32 H 0.7908 -0.3773 0.2121 0.042 Uiso 1 1 calc R . .
C5 C 0.1534(4) 0.4264(3) 0.3216(2) 0.0322(9) Uani 1 1 d . . .
C25 C 0.4764(4) 0.1957(4) 0.5122(2) 0.0365(10) Uani 1 1 d . . .
C11 C -0.1091(4) 0.4007(4) 0.3272(2) 0.0425(11) Uani 1 1 d . . .
C14 C 0.1231(4) 0.0202(4) 0.3454(2) 0.0355(10) Uani 1 1 d . . .
C20 C 0.0621(4) 0.1790(4) 0.5260(2) 0.0406(11) Uani 1 1 d . . .
H20 H 0.0775 0.1246 0.5682 0.049 Uiso 1 1 calc R . .
C35 C 0.7820(4) -0.5242(4) 0.0967(2) 0.0482(12) Uani 1 1 d . . .
H35A H 0.7327 -0.4550 0.0654 0.058 Uiso 1 1 calc R . .
H35B H 0.7984 -0.5946 0.0845 0.058 Uiso 1 1 calc R . .
C2 C 0.3756(4) 0.2907(3) 0.2648(2) 0.0334(9) Uani 1 1 d . . .
C17 C 0.3821(4) 0.1093(3) 0.42706(19) 0.0286(8) Uani 1 1 d . . .
C1 C 0.5043(5) 0.2251(4) 0.2358(2) 0.0426(11) Uani 1 1 d . . .
C30 C 0.4156(4) -0.3267(3) 0.1968(2) 0.0318(9) Uani 1 1 d . . .
C37 C 0.2280(4) -0.3776(4) 0.1644(2) 0.0410(10) Uani 1 1 d . . .
C29 C 0.4607(4) -0.2516(3) 0.2248(2) 0.0328(9) Uani 1 1 d . . .
C27 C 0.6741(4) -0.2026(3) 0.2531(2) 0.0341(9) Uani 1 1 d . . .
C13 C 0.0428(4) 0.4971(4) 0.3489(2) 0.0400(11) Uani 1 1 d . . .
H13 H 0.0577 0.5535 0.3643 0.048 Uiso 1 1 calc R . .
C39 C 0.4642(5) -0.4803(4) 0.1461(2) 0.0427(11) Uani 1 1 d . . .
H39 H 0.5279 -0.5375 0.1310 0.051 Uiso 1 1 calc R . .
C4 C 0.1299(4) 0.3458(3) 0.29476(19) 0.0303(9) Uani 1 1 d . . .
C33 C 0.7554(4) -0.5283(3) 0.1648(2) 0.0368(10) Uani 1 1 d . . .
H33 H 0.7587 -0.6039 0.1930 0.044 Uiso 1 1 calc R . .
C44 C 0.5384(4) -0.1638(3) 0.0208(2) 0.0309(9) Uani 1 1 d . . .
C19 C 0.1134(4) 0.1002(3) 0.43591(19) 0.0333(9) Uani 1 1 d . . .
H19 H 0.0219 0.0970 0.4396 0.040 Uiso 1 1 calc R . .
C15 C 0.1938(4) 0.0602(3) 0.38905(19) 0.0310(9) Uani 1 1 d . . .
O2 O 0.6111(4) 0.2550(3) 0.2343(2) 0.0839(15) Uani 1 1 d . . .
C48 C 0.3842(6) -0.2979(5) -0.0429(3) 0.0770(19) Uani 1 1 d . . .
H48A H 0.4238 -0.3554 -0.0043 0.092 Uiso 1 1 calc R . .
H48B H 0.4123 -0.3209 -0.0816 0.092 Uiso 1 1 calc R . .
C49 C 0.7131(4) -0.1333(4) 0.0775(2) 0.0346(9) Uani 1 1 d . . .
H49 H 0.7371 -0.1034 0.1075 0.042 Uiso 1 1 calc R . .
C50 C 0.8145(4) -0.1913(4) 0.0440(2) 0.0369(10) Uani 1 1 d . . .
C43 C 0.5724(4) -0.1187(3) 0.06669(18) 0.0269(8) Uani 1 1 d . . .
C7 C 0.3129(5) 0.5205(4) 0.3476(2) 0.0421(11) Uani 1 1 d . . .
H7 H 0.2723 0.6009 0.3242 0.051 Uiso 1 1 calc R . .
C36 C 0.2717(4) -0.3102(4) 0.1915(2) 0.0396(10) Uani 1 1 d . . .
H36 H 0.2068 -0.2534 0.2064 0.048 Uiso 1 1 calc R . .
C38 C 0.3241(5) -0.4615(4) 0.1403(2) 0.0409(11) Uani 1 1 d . . .
C10 C -0.0050(4) 0.3345(4) 0.2985(2) 0.0381(10) Uani 1 1 d . . .
H10 H -0.0234 0.2816 0.2813 0.046 Uiso 1 1 calc R . .
C28 C 0.6081(4) -0.2744(3) 0.2289(2) 0.0334(9) Uani 1 1 d . . .
C46 C 0.3608(5) -0.1777(4) -0.0453(3) 0.0531(13) Uani 1 1 d . . .
H46 H 0.3739 -0.1282 -0.0869 0.064 Uiso 1 1 calc R . .
C34 C 0.8906(5) -0.5167(4) 0.1365(2) 0.0481(13) Uani 1 1 d . . .
H34A H 0.9727 -0.5826 0.1483 0.058 Uiso 1 1 calc R . .
H34B H 0.9071 -0.4430 0.1292 0.058 Uiso 1 1 calc R . .
C9 C 0.3167(5) 0.4975(5) 0.4173(3) 0.0543(13) Uani 1 1 d . . .
H9A H 0.3048 0.4253 0.4427 0.065 Uiso 1 1 calc R . .
H9B H 0.2771 0.5618 0.4353 0.065 Uiso 1 1 calc R . .
C21 C -0.0836(5) 0.2468(5) 0.5099(3) 0.0626(16) Uani 1 1 d . . .
H21A H -0.1546 0.2322 0.5409 0.075 Uiso 1 1 calc R . .
H21B H -0.1127 0.2666 0.4661 0.075 Uiso 1 1 calc R . .
C8 C 0.4464(5) 0.4939(5) 0.3802(3) 0.0694(18) Uani 1 1 d . . .
H8A H 0.4863 0.5560 0.3756 0.083 Uiso 1 1 calc R . .
H8B H 0.5141 0.4195 0.3831 0.083 Uiso 1 1 calc R . .
C47 C 0.2392(5) -0.2200(5) -0.0399(3) 0.0614(16) Uani 1 1 d . . .
H47A H 0.1796 -0.1959 -0.0769 0.074 Uiso 1 1 calc R . .
H47B H 0.1912 -0.2303 0.0004 0.074 Uiso 1 1 calc R . .
C22 C 0.0149(5) 0.3024(5) 0.5250(3) 0.0582(15) Uani 1 1 d . . .
H22A H 0.0462 0.3556 0.4903 0.070 Uiso 1 1 calc R . .
H22B H 0.0042 0.3212 0.5652 0.070 Uiso 1 1 calc R . .
O1W O -0.0482(3) 0.1931(3) 0.1905(2) 0.0716(12) Uani 1 1 d . . .
H1WA H -0.0965 0.2632 0.1785 0.107 Uiso 1 1 d R A 1
H1WB H -0.0295 0.1656 0.1588 0.107 Uiso 1 1 d R A 1
O2W O -0.2498(4) -0.0343(5) 0.3339(2) 0.0966(17) Uani 1 1 d . . .
H2WA H -0.2206 -0.0403 0.3702 0.145 Uiso 1 1 d R B 1
H2WB H -0.2190 -0.0987 0.3255 0.145 Uiso 1 1 d R B 1
O4W O 1.0632(5) -0.2186(4) 0.3168(2) 0.0834(13) Uani 1 1 d G . .
H4WA H 1.0383 -0.1695 0.2814 0.125 Uiso 1 1 d G . .
H4WB H 0.9967 -0.2459 0.3320 0.125 Uiso 1 1 d G . .
O3W O -0.1286(4) -0.0269(3) 0.1844(2) 0.0828(8) Uani 1 1 d . . .
H3WA H -0.1812 -0.0700 0.1929 0.124 Uiso 1 1 d R C 1
H3WB H -0.0437 -0.0679 0.1880 0.124 Uiso 1 1 d R C 1
Na1 Na -0.1731(4) 0.0921(3) 0.2627(2) 0.0828(8) Uani 0.70 1 d P D 1
Na2 Na -0.2506(7) 0.1046(6) 0.2155(4) 0.067(2) Uani 0.30 1 d P . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho2 O10 2.279(3) . ?
Ho2 O1 2.297(3) . ?
Ho2 O4 2.314(3) . ?
Ho2 O7 2.325(3) . ?
Ho2 O6 2.340(3) . ?
Ho2 O9 2.354(3) . ?
Ho2 O12 2.422(3) . ?
Ho2 O3 2.446(2) . ?
Cl4 C51 1.714(4) . ?
Cl3 C38 1.727(4) . ?
Cl1 C12 1.730(4) . ?
Cl2 C25 1.728(4) . ?
O3 C3 1.255(4) . ?
O7 C27 1.269(4) . ?
O10 C40 1.263(5) . ?
O4 C14 1.258(4) . ?
O1 C1 1.262(5) . ?
O12 C42 1.246(4) . ?
F1 C11 1.350(5) . ?
F3 C37 1.338(5) . ?
O6 C16 1.263(4) . ?
F4 C50 1.348(5) . ?
N4 C45 1.353(5) . ?
N4 C44 1.387(5) . ?
N4 C46 1.469(5) . ?
N1 C6 1.346(5) . ?
N1 C5 1.401(5) . ?
N1 C7 1.454(5) . ?
C51 C52 1.371(6) . ?
C51 C50 1.393(6) . ?
O9 C29 1.254(4) . ?
C42 C41 1.421(5) . ?
C42 C43 1.474(5) . ?
C31 N3 1.390(5) . ?
C31 C30 1.400(5) . ?
C31 C39 1.399(6) . ?
O11 C40 1.231(5) . ?
C12 C13 1.358(6) . ?
C12 C11 1.393(6) . ?
C18 N2 1.394(5) . ?
C18 C26 1.402(5) . ?
C18 C17 1.404(5) . ?
N2 C19 1.336(5) . ?
N2 C20 1.459(5) . ?
C41 C45 1.358(5) . ?
C41 C40 1.521(5) . ?
F2 C24 1.353(5) . ?
C24 C23 1.365(6) . ?
C24 C25 1.389(6) . ?
C52 C44 1.409(5) . ?
C52 H52 0.9300 . ?
C26 C25 1.363(6) . ?
C26 H26 0.9300 . ?
N3 C32 1.344(5) . ?
N3 C33 1.461(5) . ?
O5 C14 1.241(5) . ?
O8 C27 1.245(5) . ?
C16 C15 1.421(5) . ?
C16 C17 1.458(5) . ?
C3 C2 1.431(5) . ?
C3 C4 1.460(5) . ?
C6 C2 1.368(5) . ?
C6 H6 0.9300 . ?
C45 H45 0.9300 . ?
C23 C17 1.405(5) . ?
C23 H23 0.9300 . ?
C32 C28 1.369(5) . ?
C32 H32 0.9300 . ?
C5 C4 1.405(5) . ?
C5 C13 1.409(5) . ?
C11 C10 1.361(6) . ?
C14 C15 1.516(5) . ?
C20 C21 1.468(6) . ?
C20 C22 1.489(7) . ?
C20 H20 0.9800 . ?
C35 C33 1.489(6) . ?
C35 C34 1.496(6) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C2 C1 1.511(5) . ?
C1 O2 1.242(5) . ?
C30 C36 1.409(6) . ?
C30 C29 1.464(5) . ?
C37 C36 1.358(6) . ?
C37 C38 1.399(6) . ?
C29 C28 1.427(6) . ?
C27 C28 1.506(5) . ?
C13 H13 0.9300 . ?
C39 C38 1.367(6) . ?
C39 H39 0.9300 . ?
C4 C10 1.402(6) . ?
C33 C34 1.481(6) . ?
C33 H33 0.9800 . ?
C44 C43 1.403(5) . ?
C19 C15 1.372(5) . ?
C19 H19 0.9300 . ?
O2 Na2 2.118(7) 1_655 ?
C48 C46 1.461(7) . ?
C48 C47 1.499(7) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C50 1.359(5) . ?
C49 C43 1.403(5) . ?
C49 H49 0.9300 . ?
C7 C9 1.479(7) . ?
C7 C8 1.476(7) . ?
C7 H7 0.9800 . ?
C36 H36 0.9300 . ?
C10 H10 0.9300 . ?
C46 C47 1.467(7) . ?
C46 H46 0.9800 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C9 C8 1.477(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C21 C22 1.489(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8498 . ?
O2W H2WB 0.8501 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8501 . ?
O3W Na2 2.005(8) . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
Na2 O2 2.118(7) 1_455 ?

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 Ho2 O1 107.83(11) . . ?
O10 Ho2 O4 83.01(10) . . ?
O1 Ho2 O4 139.26(9) . . ?
O10 Ho2 O7 138.85(9) . . ?
O1 Ho2 O7 84.57(10) . . ?
O4 Ho2 O7 113.34(11) . . ?
O10 Ho2 O6 144.96(9) . . ?
O1 Ho2 O6 77.71(10) . . ?
O4 Ho2 O6 72.64(9) . . ?
O7 Ho2 O6 75.27(9) . . ?
O10 Ho2 O9 78.88(11) . . ?
O1 Ho2 O9 147.73(9) . . ?
O4 Ho2 O9 72.02(9) . . ?
O7 Ho2 O9 71.77(10) . . ?
O6 Ho2 O9 115.36(11) . . ?
O10 Ho2 O12 71.07(9) . . ?
O1 Ho2 O12 76.85(9) . . ?
O4 Ho2 O12 141.85(9) . . ?
O7 Ho2 O12 74.17(10) . . ?
O6 Ho2 O12 141.64(9) . . ?
O9 Ho2 O12 75.78(10) . . ?
O10 Ho2 O3 74.44(9) . . ?
O1 Ho2 O3 71.16(9) . . ?
O4 Ho2 O3 74.59(9) . . ?
O7 Ho2 O3 144.88(9) . . ?
O6 Ho2 O3 75.02(9) . . ?
O9 Ho2 O3 139.23(9) . . ?
O12 Ho2 O3 121.91(10) . . ?
C3 O3 Ho2 127.7(2) . . ?
C27 O7 Ho2 133.4(3) . . ?
C40 O10 Ho2 136.5(2) . . ?
C14 O4 Ho2 132.0(2) . . ?
C1 O1 Ho2 135.9(3) . . ?
C42 O12 Ho2 129.0(2) . . ?
C16 O6 Ho2 132.0(2) . . ?
C45 N4 C44 119.4(3) . . ?
C45 N4 C46 119.9(3) . . ?
C44 N4 C46 120.0(3) . . ?
C6 N1 C5 118.9(3) . . ?
C6 N1 C7 121.8(3) . . ?
C5 N1 C7 119.3(3) . . ?
C52 C51 C50 119.4(4) . . ?
C52 C51 Cl4 120.6(3) . . ?
C50 C51 Cl4 120.0(3) . . ?
C29 O9 Ho2 129.8(3) . . ?
O12 C42 C41 126.0(3) . . ?
O12 C42 C43 118.9(3) . . ?
C41 C42 C43 115.1(3) . . ?
N3 C31 C30 119.0(4) . . ?
N3 C31 C39 121.2(4) . . ?
C30 C31 C39 119.9(4) . . ?
C13 C12 C11 120.1(4) . . ?
C13 C12 Cl1 120.2(3) . . ?
C11 C12 Cl1 119.7(3) . . ?
N2 C18 C26 121.1(3) . . ?
N2 C18 C17 118.6(3) . . ?
C26 C18 C17 120.2(4) . . ?
C19 N2 C18 119.8(3) . . ?
C19 N2 C20 119.5(3) . . ?
C18 N2 C20 120.5(3) . . ?
C45 C41 C42 120.4(3) . . ?
C45 C41 C40 116.5(3) . . ?
C42 C41 C40 123.1(3) . . ?
F2 C24 C23 118.6(4) . . ?
F2 C24 C25 119.3(4) . . ?
C23 C24 C25 122.0(4) . . ?
C51 C52 C44 120.2(4) . . ?
C51 C52 H52 119.9 . . ?
C44 C52 H52 119.9 . . ?
C25 C26 C18 119.5(4) . . ?
C25 C26 H26 120.3 . . ?
C18 C26 H26 120.3 . . ?
C32 N3 C31 119.4(3) . . ?
C32 N3 C33 120.6(3) . . ?
C31 N3 C33 119.8(3) . . ?
O11 C40 O10 124.9(4) . . ?
O11 C40 C41 117.4(4) . . ?
O10 C40 C41 117.8(3) . . ?
O6 C16 C15 124.4(3) . . ?
O6 C16 C17 119.4(3) . . ?
C15 C16 C17 116.2(3) . . ?
O3 C3 C2 125.0(3) . . ?
O3 C3 C4 119.7(3) . . ?
C2 C3 C4 115.3(3) . . ?
N1 C6 C2 125.3(4) . . ?
N1 C6 H6 117.4 . . ?
C2 C6 H6 117.4 . . ?
N4 C45 C41 124.5(4) . . ?
N4 C45 H45 117.8 . . ?
C41 C45 H45 117.8 . . ?
C24 C23 C17 118.8(4) . . ?
C24 C23 H23 120.6 . . ?
C17 C23 H23 120.6 . . ?
N3 C32 C28 125.2(4) . . ?
N3 C32 H32 117.4 . . ?
C28 C32 H32 117.4 . . ?
N1 C5 C4 119.1(3) . . ?
N1 C5 C13 120.3(3) . . ?
C4 C5 C13 120.7(4) . . ?
C26 C25 C24 120.1(4) . . ?
C26 C25 Cl2 120.5(3) . . ?
C24 C25 Cl2 119.3(3) . . ?
F1 C11 C10 120.0(4) . . ?
F1 C11 C12 118.7(4) . . ?
C10 C11 C12 121.4(4) . . ?
O5 C14 O4 124.4(4) . . ?
O5 C14 C15 117.3(3) . . ?
O4 C14 C15 118.3(4) . . ?
N2 C20 C21 119.5(4) . . ?
N2 C20 C22 118.8(4) . . ?
C21 C20 C22 60.4(3) . . ?
N2 C20 H20 115.6 . . ?
C21 C20 H20 115.6 . . ?
C22 C20 H20 115.6 . . ?
C33 C35 C34 59.5(3) . . ?
C33 C35 H35A 117.8 . . ?
C34 C35 H35A 117.8 . . ?
C33 C35 H35B 117.8 . . ?
C34 C35 H35B 117.8 . . ?
H35A C35 H35B 115.0 . . ?
C6 C2 C3 119.6(4) . . ?
C6 C2 C1 116.9(4) . . ?
C3 C2 C1 123.5(3) . . ?
C23 C17 C18 119.3(3) . . ?
C23 C17 C16 119.3(3) . . ?
C18 C17 C16 121.4(3) . . ?
O2 C1 O1 123.9(4) . . ?
O2 C1 C2 116.9(4) . . ?
O1 C1 C2 119.2(4) . . ?
C31 C30 C36 119.2(4) . . ?
C31 C30 C29 121.7(4) . . ?
C36 C30 C29 119.1(3) . . ?
F3 C37 C36 120.2(4) . . ?
F3 C37 C38 118.9(4) . . ?
C36 C37 C38 120.9(4) . . ?
O9 C29 C28 125.7(4) . . ?
O9 C29 C30 118.7(4) . . ?
C28 C29 C30 115.6(3) . . ?
O8 C27 O7 124.0(4) . . ?
O8 C27 C28 117.6(3) . . ?
O7 C27 C28 118.4(4) . . ?
C12 C13 C5 119.5(4) . . ?
C12 C13 H13 120.3 . . ?
C5 C13 H13 120.3 . . ?
C38 C39 C31 119.9(4) . . ?
C38 C39 H39 120.0 . . ?
C31 C39 H39 120.0 . . ?
C10 C4 C5 118.0(4) . . ?
C10 C4 C3 120.1(3) . . ?
C5 C4 C3 121.8(4) . . ?
N3 C33 C35 119.0(4) . . ?
N3 C33 C34 119.7(3) . . ?
C35 C33 C34 60.5(3) . . ?
N3 C33 H33 115.5 . . ?
C35 C33 H33 115.5 . . ?
C34 C33 H33 115.5 . . ?
N4 C44 C43 119.4(3) . . ?
N4 C44 C52 121.1(4) . . ?
C43 C44 C52 119.6(4) . . ?
N2 C19 C15 125.0(4) . . ?
N2 C19 H19 117.5 . . ?
C15 C19 H19 117.5 . . ?
C19 C15 C16 119.0(3) . . ?
C19 C15 C14 116.9(3) . . ?
C16 C15 C14 124.0(3) . . ?
C1 O2 Na2 95.3(4) . 1_655 ?
C46 C48 C47 59.4(3) . . ?
C46 C48 H48A 117.8 . . ?
C47 C48 H48A 117.8 . . ?
C46 C48 H48B 117.8 . . ?
C47 C48 H48B 117.8 . . ?
H48A C48 H48B 115.0 . . ?
C50 C49 C43 119.9(4) . . ?
C50 C49 H49 120.1 . . ?
C43 C49 H49 120.1 . . ?
F4 C50 C49 119.8(4) . . ?
F4 C50 C51 118.4(3) . . ?
C49 C50 C51 121.8(4) . . ?
C44 C43 C49 119.2(3) . . ?
C44 C43 C42 121.1(3) . . ?
C49 C43 C42 119.7(3) . . ?
N1 C7 C9 119.1(4) . . ?
N1 C7 C8 119.6(4) . . ?
C9 C7 C8 60.0(4) . . ?
N1 C7 H7 115.6 . . ?
C9 C7 H7 115.6 . . ?
C8 C7 H7 115.6 . . ?
C37 C36 C30 119.8(4) . . ?
C37 C36 H36 120.1 . . ?
C30 C36 H36 120.1 . . ?
C39 C38 C37 120.2(4) . . ?
C39 C38 Cl3 120.8(3) . . ?
C37 C38 Cl3 119.0(3) . . ?
C11 C10 C4 120.3(4) . . ?
C11 C10 H10 119.8 . . ?
C4 C10 H10 119.8 . . ?
C32 C28 C29 119.1(4) . . ?
C32 C28 C27 117.6(4) . . ?
C29 C28 C27 123.3(3) . . ?
C48 C46 N4 119.8(5) . . ?
C48 C46 C47 61.6(3) . . ?
N4 C46 C47 118.6(5) . . ?
C48 C46 H46 115.4 . . ?
N4 C46 H46 115.4 . . ?
C47 C46 H46 115.4 . . ?
C33 C34 C35 60.0(3) . . ?
C33 C34 H34A 117.8 . . ?
C35 C34 H34A 117.8 . . ?
C33 C34 H34B 117.8 . . ?
C35 C34 H34B 117.8 . . ?
H34A C34 H34B 114.9 . . ?
C7 C9 C8 59.9(4) . . ?
C7 C9 H9A 117.8 . . ?
C8 C9 H9A 117.8 . . ?
C7 C9 H9B 117.8 . . ?
C8 C9 H9B 117.8 . . ?
H9A C9 H9B 114.9 . . ?
C20 C21 C22 60.5(3) . . ?
C20 C21 H21A 117.7 . . ?
C22 C21 H21A 117.7 . . ?
C20 C21 H21B 117.7 . . ?
C22 C21 H21B 117.7 . . ?
H21A C21 H21B 114.8 . . ?
C7 C8 C9 60.1(3) . . ?
C7 C8 H8A 117.8 . . ?
C9 C8 H8A 117.8 . . ?
C7 C8 H8B 117.8 . . ?
C9 C8 H8B 117.8 . . ?
H8A C8 H8B 114.9 . . ?
C46 C47 C48 59.0(3) . . ?
C46 C47 H47A 117.9 . . ?
C48 C47 H47A 117.9 . . ?
C46 C47 H47B 117.9 . . ?
C48 C47 H47B 117.9 . . ?
H47A C47 H47B 115.0 . . ?
C20 C22 C21 59.1(3) . . ?
C20 C22 H22A 117.9 . . ?
C21 C22 H22A 117.9 . . ?
C20 C22 H22B 117.9 . . ?
C21 C22 H22B 117.9 . . ?
H22A C22 H22B 115.0 . . ?
H1WA O1W H1WB 109.5 . . ?
H2WA O2W H2WB 109.5 . . ?
H4WA O4W H4WB 109.5 . . ?
Na2 O3W H3WA 99.3 . . ?
Na2 O3W H3WB 137.5 . . ?
H3WA O3W H3WB 109.5 . . ?
O3W Na2 O2 171.6(5) . 1_455 ?

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
O10 Ho2 O3 C3 -155.6(3) . . . . ?
O1 Ho2 O3 C3 -40.1(3) . . . . ?
O4 Ho2 O3 C3 117.5(3) . . . . ?
O7 Ho2 O3 C3 8.7(4) . . . . ?
O6 Ho2 O3 C3 41.8(3) . . . . ?
O9 Ho2 O3 C3 153.4(3) . . . . ?
O12 Ho2 O3 C3 -100.4(3) . . . . ?
O10 Ho2 O7 C27 -2.3(5) . . . . ?
O1 Ho2 O7 C27 -113.3(4) . . . . ?
O4 Ho2 O7 C27 104.7(4) . . . . ?
O6 Ho2 O7 C27 168.0(4) . . . . ?
O9 Ho2 O7 C27 44.5(4) . . . . ?
O12 Ho2 O7 C27 -35.4(4) . . . . ?
O3 Ho2 O7 C27 -158.9(3) . . . . ?
O1 Ho2 O10 C40 113.4(4) . . . . ?
O4 Ho2 O10 C40 -107.0(4) . . . . ?
O7 Ho2 O10 C40 10.8(5) . . . . ?
O6 Ho2 O10 C40 -152.7(4) . . . . ?
O9 Ho2 O10 C40 -34.0(4) . . . . ?
O12 Ho2 O10 C40 44.6(4) . . . . ?
O3 Ho2 O10 C40 177.1(4) . . . . ?
O10 Ho2 O4 C14 -109.6(4) . . . . ?
O1 Ho2 O4 C14 -0.3(5) . . . . ?
O7 Ho2 O4 C14 109.7(4) . . . . ?
O6 Ho2 O4 C14 44.9(4) . . . . ?
O9 Ho2 O4 C14 169.9(4) . . . . ?
O12 Ho2 O4 C14 -156.3(3) . . . . ?
O3 Ho2 O4 C14 -33.9(4) . . . . ?
O10 Ho2 O1 C1 108.6(4) . . . . ?
O4 Ho2 O1 C1 8.4(5) . . . . ?
O7 Ho2 O1 C1 -111.6(4) . . . . ?
O6 Ho2 O1 C1 -35.5(4) . . . . ?
O9 Ho2 O1 C1 -154.0(4) . . . . ?
O12 Ho2 O1 C1 173.4(4) . . . . ?
O3 Ho2 O1 C1 42.6(4) . . . . ?
O10 Ho2 O12 C42 -36.7(3) . . . . ?
O1 Ho2 O12 C42 -151.1(3) . . . . ?
O4 Ho2 O12 C42 13.1(4) . . . . ?
O7 Ho2 O12 C42 120.9(3) . . . . ?
O6 Ho2 O12 C42 159.3(3) . . . . ?
O9 Ho2 O12 C42 46.2(3) . . . . ?
O3 Ho2 O12 C42 -93.5(3) . . . . ?
O10 Ho2 O6 C16 15.4(4) . . . . ?
O1 Ho2 O6 C16 119.0(3) . . . . ?
O4 Ho2 O6 C16 -32.7(3) . . . . ?
O7 Ho2 O6 C16 -153.4(4) . . . . ?
O9 Ho2 O6 C16 -92.3(3) . . . . ?
O12 Ho2 O6 C16 168.5(3) . . . . ?
O3 Ho2 O6 C16 45.5(3) . . . . ?
O10 Ho2 O9 C29 112.5(4) . . . . ?
O1 Ho2 O9 C29 6.6(5) . . . . ?
O4 Ho2 O9 C29 -161.3(4) . . . . ?
O7 Ho2 O9 C29 -38.3(4) . . . . ?
O6 Ho2 O9 C29 -101.4(4) . . . . ?
O12 Ho2 O9 C29 39.4(4) . . . . ?
O3 Ho2 O9 C29 162.2(3) . . . . ?
Ho2 O12 C42 C41 27.0(6) . . . . ?
Ho2 O12 C42 C43 -152.3(3) . . . . ?
C26 C18 N2 C19 -178.0(4) . . . . ?
C17 C18 N2 C19 2.1(6) . . . . ?
C26 C18 N2 C20 -2.1(6) . . . . ?
C17 C18 N2 C20 178.0(4) . . . . ?
O12 C42 C41 C45 179.6(4) . . . . ?
C43 C42 C41 C45 -1.1(6) . . . . ?
O12 C42 C41 C40 1.5(6) . . . . ?
C43 C42 C41 C40 -179.2(4) . . . . ?
C50 C51 C52 C44 -3.0(7) . . . . ?
Cl4 C51 C52 C44 176.1(3) . . . . ?
N2 C18 C26 C25 -177.7(4) . . . . ?
C17 C18 C26 C25 2.1(6) . . . . ?
C30 C31 N3 C32 -1.4(6) . . . . ?
C39 C31 N3 C32 178.5(4) . . . . ?
C30 C31 N3 C33 173.5(4) . . . . ?
C39 C31 N3 C33 -6.6(7) . . . . ?
Ho2 O10 C40 O11 144.7(4) . . . . ?
Ho2 O10 C40 C41 -36.6(6) . . . . ?
C45 C41 C40 O11 0.6(6) . . . . ?
C42 C41 C40 O11 178.8(4) . . . . ?
C45 C41 C40 O10 -178.2(4) . . . . ?
C42 C41 C40 O10 -0.1(6) . . . . ?
Ho2 O6 C16 C15 22.6(6) . . . . ?
Ho2 O6 C16 C17 -155.7(3) . . . . ?
Ho2 O3 C3 C2 30.8(6) . . . . ?
Ho2 O3 C3 C4 -148.4(3) . . . . ?
C5 N1 C6 C2 -2.0(7) . . . . ?
C7 N1 C6 C2 -179.4(4) . . . . ?
C44 N4 C45 C41 -1.7(7) . . . . ?
C46 N4 C45 C41 -172.3(4) . . . . ?
C42 C41 C45 N4 2.5(7) . . . . ?
C40 C41 C45 N4 -179.3(4) . . . . ?
F2 C24 C23 C17 -179.3(4) . . . . ?
C25 C24 C23 C17 0.6(7) . . . . ?
C31 N3 C32 C28 -0.6(7) . . . . ?
C33 N3 C32 C28 -175.5(4) . . . . ?
C6 N1 C5 C4 1.9(6) . . . . ?
C7 N1 C5 C4 179.4(4) . . . . ?
C6 N1 C5 C13 -177.5(4) . . . . ?
C7 N1 C5 C13 0.1(6) . . . . ?
C18 C26 C25 C24 -2.2(7) . . . . ?
C18 C26 C25 Cl2 179.6(3) . . . . ?
F2 C24 C25 C26 -179.2(4) . . . . ?
C23 C24 C25 C26 0.9(7) . . . . ?
F2 C24 C25 Cl2 -1.0(6) . . . . ?
C23 C24 C25 Cl2 179.1(3) . . . . ?
C13 C12 C11 F1 -179.1(5) . . . . ?
Cl1 C12 C11 F1 1.5(7) . . . . ?
C13 C12 C11 C10 -0.1(8) . . . . ?
Cl1 C12 C11 C10 -179.4(4) . . . . ?
Ho2 O4 C14 O5 136.0(4) . . . . ?
Ho2 O4 C14 C15 -43.6(6) . . . . ?
C19 N2 C20 C21 -45.1(6) . . . . ?
C18 N2 C20 C21 139.0(4) . . . . ?
C19 N2 C20 C22 -115.5(5) . . . . ?
C18 N2 C20 C22 68.6(5) . . . . ?
N1 C6 C2 C3 -0.3(7) . . . . ?
N1 C6 C2 C1 -179.4(4) . . . . ?
O3 C3 C2 C6 -176.8(4) . . . . ?
C4 C3 C2 C6 2.5(6) . . . . ?
O3 C3 C2 C1 2.3(7) . . . . ?
C4 C3 C2 C1 -178.5(4) . . . . ?
C24 C23 C17 C18 -0.7(6) . . . . ?
C24 C23 C17 C16 -179.7(4) . . . . ?
N2 C18 C17 C23 179.2(4) . . . . ?
C26 C18 C17 C23 -0.7(6) . . . . ?
N2 C18 C17 C16 -1.8(6) . . . . ?
C26 C18 C17 C16 178.3(4) . . . . ?
O6 C16 C17 C23 -1.6(6) . . . . ?
C15 C16 C17 C23 179.9(4) . . . . ?
O6 C16 C17 C18 179.4(4) . . . . ?
C15 C16 C17 C18 0.9(6) . . . . ?
Ho2 O1 C1 O2 148.2(4) . . . . ?
Ho2 O1 C1 C2 -30.9(7) . . . . ?
C6 C2 C1 O2 -5.4(7) . . . . ?
C3 C2 C1 O2 175.5(5) . . . . ?
C6 C2 C1 O1 173.7(4) . . . . ?
C3 C2 C1 O1 -5.4(7) . . . . ?
N3 C31 C30 C36 -178.5(4) . . . . ?
C39 C31 C30 C36 1.6(7) . . . . ?
N3 C31 C30 C29 2.3(6) . . . . ?
C39 C31 C30 C29 -177.6(4) . . . . ?
Ho2 O9 C29 C28 29.5(6) . . . . ?
Ho2 O9 C29 C30 -147.9(3) . . . . ?
C31 C30 C29 O9 176.4(4) . . . . ?
C36 C30 C29 O9 -2.8(6) . . . . ?
C31 C30 C29 C28 -1.2(6) . . . . ?
C36 C30 C29 C28 179.6(4) . . . . ?
Ho2 O7 C27 O8 142.2(4) . . . . ?
Ho2 O7 C27 C28 -37.3(6) . . . . ?
C11 C12 C13 C5 -2.5(7) . . . . ?
Cl1 C12 C13 C5 176.9(4) . . . . ?
N1 C5 C13 C12 -176.7(4) . . . . ?
C4 C5 C13 C12 4.0(7) . . . . ?
N3 C31 C39 C38 179.7(4) . . . . ?
C30 C31 C39 C38 -0.5(7) . . . . ?
N1 C5 C4 C10 177.8(4) . . . . ?
C13 C5 C4 C10 -2.8(6) . . . . ?
N1 C5 C4 C3 0.4(6) . . . . ?
C13 C5 C4 C3 179.7(4) . . . . ?
O3 C3 C4 C10 -0.6(6) . . . . ?
C2 C3 C4 C10 -179.9(4) . . . . ?
O3 C3 C4 C5 176.8(4) . . . . ?
C2 C3 C4 C5 -2.5(6) . . . . ?
C32 N3 C33 C35 -110.8(5) . . . . ?
C31 N3 C33 C35 74.4(5) . . . . ?
C32 N3 C33 C34 -40.2(6) . . . . ?
C31 N3 C33 C34 145.0(4) . . . . ?
C34 C35 C33 N3 109.7(4) . . . . ?
C45 N4 C44 C43 -0.5(6) . . . . ?
C46 N4 C44 C43 170.1(4) . . . . ?
C45 N4 C44 C52 -179.0(4) . . . . ?
C46 N4 C44 C52 -8.4(6) . . . . ?
C51 C52 C44 N4 -179.4(4) . . . . ?
C51 C52 C44 C43 2.1(7) . . . . ?
C18 N2 C19 C15 -1.6(7) . . . . ?
C20 N2 C19 C15 -177.6(4) . . . . ?
N2 C19 C15 C16 0.7(7) . . . . ?
N2 C19 C15 C14 -176.9(4) . . . . ?
O6 C16 C15 C19 -178.7(4) . . . . ?
C17 C16 C15 C19 -0.3(6) . . . . ?
O6 C16 C15 C14 -1.3(7) . . . . ?
C17 C16 C15 C14 177.0(4) . . . . ?
O5 C14 C15 C19 8.6(6) . . . . ?
O4 C14 C15 C19 -171.8(4) . . . . ?
O5 C14 C15 C16 -168.8(4) . . . . ?
O4 C14 C15 C16 10.8(6) . . . . ?
O1 C1 O2 Na2 -14.7(6) . . . 1_655 ?
C2 C1 O2 Na2 164.4(4) . . . 1_655 ?
C43 C49 C50 F4 179.1(4) . . . . ?
C43 C49 C50 C51 -0.4(7) . . . . ?
C52 C51 C50 F4 -177.3(4) . . . . ?
Cl4 C51 C50 F4 3.6(6) . . . . ?
C52 C51 C50 C49 2.2(7) . . . . ?
Cl4 C51 C50 C49 -176.9(4) . . . . ?
N4 C44 C43 C49 -178.9(4) . . . . ?
C52 C44 C43 C49 -0.3(6) . . . . ?
N4 C44 C43 C42 1.7(6) . . . . ?
C52 C44 C43 C42 -179.8(4) . . . . ?
C50 C49 C43 C44 -0.5(6) . . . . ?
C50 C49 C43 C42 178.9(4) . . . . ?
O12 C42 C43 C44 178.5(4) . . . . ?
C41 C42 C43 C44 -0.9(6) . . . . ?
O12 C42 C43 C49 -1.0(6) . . . . ?
C41 C42 C43 C49 179.7(4) . . . . ?
C6 N1 C7 C9 -107.7(5) . . . . ?
C5 N1 C7 C9 74.8(5) . . . . ?
C6 N1 C7 C8 -37.8(7) . . . . ?
C5 N1 C7 C8 144.8(5) . . . . ?
F3 C37 C36 C30 177.1(4) . . . . ?
C38 C37 C36 C30 -1.6(7) . . . . ?
C31 C30 C36 C37 -0.6(7) . . . . ?
C29 C30 C36 C37 178.7(4) . . . . ?
C31 C39 C38 C37 -1.7(7) . . . . ?
C31 C39 C38 Cl3 179.9(4) . . . . ?
F3 C37 C38 C39 -176.0(4) . . . . ?
C36 C37 C38 C39 2.8(8) . . . . ?
F3 C37 C38 Cl3 2.5(6) . . . . ?
C36 C37 C38 Cl3 -178.8(4) . . . . ?
F1 C11 C10 C4 -179.8(4) . . . . ?
C12 C11 C10 C4 1.2(7) . . . . ?
C5 C4 C10 C11 0.3(7) . . . . ?
C3 C4 C10 C11 177.8(4) . . . . ?
N3 C32 C28 C29 1.6(7) . . . . ?
N3 C32 C28 C27 -175.9(4) . . . . ?
O9 C29 C28 C32 -178.1(4) . . . . ?
C30 C29 C28 C32 -0.7(6) . . . . ?
O9 C29 C28 C27 -0.7(7) . . . . ?
C30 C29 C28 C27 176.7(4) . . . . ?
O8 C27 C28 C32 1.0(6) . . . . ?
O7 C27 C28 C32 -179.4(4) . . . . ?
O8 C27 C28 C29 -176.4(4) . . . . ?
O7 C27 C28 C29 3.1(6) . . . . ?
C47 C48 C46 N4 108.5(5) . . . . ?
C45 N4 C46 C48 -113.9(5) . . . . ?
C44 N4 C46 C48 75.5(6) . . . . ?
C45 N4 C46 C47 -42.1(7) . . . . ?
C44 N4 C46 C47 147.4(5) . . . . ?
N3 C33 C34 C35 -108.6(5) . . . . ?
N1 C7 C9 C8 109.3(5) . . . . ?
N2 C20 C21 C22 -108.4(5) . . . . ?
N1 C7 C8 C9 -108.6(5) . . . . ?
N4 C46 C47 C48 -110.4(6) . . . . ?
N2 C20 C22 C21 109.6(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         2.240
_refine_diff_density_min         -2.318
_refine_diff_density_rms         0.085

# start Validation Reply Form 
_vrf_PLAT415_1d                  
; 
PROBLEM: 
RESPONSE: Because the disorder of the hydrogen. 
;
_vrf_PLAT420_1d                  
; 
PROBLEM: 
RESPONSE: Because the disorder of the hydrogen. 
;
_vrf_PLAT910_1d                  
; 
PROBLEM: 
RESPONSE: Theta min = 3.3980 deg. The theta value of the missing reflections 
are less than 3.5050 deg. and therefore reflections were excluded. 
;
_vrf_PLAT973_1d                  
; 
PROBLEM: 
RESPONSE: The diffractions were collected at room temperature. 
;
# end Validation Reply Form 
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2d
_database_code_depnum_ccdc_archive 'CCDC 1855014'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H38 Cl4 Dy F4 K N4 O15'
_chemical_formula_weight         1378.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1890 4.4100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0542(5)
_cell_length_b                   12.7549(7)
_cell_length_c                   21.7465(12)
_cell_angle_alpha                74.531(5)
_cell_angle_beta                 86.276(4)
_cell_angle_gamma                72.965(5)
_cell_volume                     2569.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9777
_cell_measurement_theta_min      3.5900
_cell_measurement_theta_max      28.5330

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1374
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19649
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9005
_reflns_number_gt                8021
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0632P)²+19.7189P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9005
_refine_ls_number_parameters     735
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0666
_refine_ls_wR_factor_ref         0.1567
_refine_ls_wR_factor_gt          0.1510
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.008
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy2 Dy 0.61395(4) 0.48905(3) 0.256921(17) 0.02956(13) Uani 1 1 d . . .
K2 K 0.2023(4) 0.4462(4) 0.2428(2) 0.1192(13) Uani 1 1 d . . .
Cl3 Cl 0.0915(2) 0.8178(2) 0.54171(12) 0.0549(6) Uani 1 1 d . . .
Cl4 Cl 0.7239(3) 1.0368(2) 0.39502(14) 0.0645(7) Uani 1 1 d . . .
Cl2 Cl 0.4511(3) 0.2564(2) -0.07514(13) 0.0597(7) Uani 1 1 d . . .
Cl1 Cl 1.2161(2) -0.0499(2) 0.10528(14) 0.0628(7) Uani 1 1 d . . .
F3 F 0.0498(5) 0.7111(5) 0.4446(3) 0.0604(15) Uani 1 1 d . . .
F4 F 0.8921(5) 0.8626(5) 0.3370(3) 0.0657(16) Uani 1 1 d . . .
F1 F 1.2318(5) 0.1251(6) 0.1648(3) 0.0704(18) Uani 1 1 d . . .
F2 F 0.3012(6) 0.3280(6) 0.0326(3) 0.0693(17) Uani 1 1 d . . .
O11 O 0.1794(7) 0.7293(6) 0.2329(4) 0.070(2) Uani 1 1 d . . .
O10 O 0.3875(6) 0.6099(5) 0.2253(3) 0.0391(13) Uani 1 1 d . . .
O12 O 0.6116(6) 0.6738(5) 0.2509(3) 0.0443(14) Uani 1 1 d . . .
O5 O 0.9987(6) 0.4714(6) 0.1452(3) 0.0562(18) Uani 1 1 d . . .
O4 O 0.7985(6) 0.5282(5) 0.1920(3) 0.0405(14) Uani 1 1 d . . .
O6 O 0.5786(6) 0.4656(5) 0.1564(3) 0.0385(13) Uani 1 1 d . . .
O3 O 0.7782(6) 0.3048(5) 0.2536(3) 0.0379(13) Uani 1 1 d . . .
O2 O 0.4985(6) 0.3520(5) 0.2840(3) 0.0390(13) Uani 1 1 d . . .
O1 O 0.3940(7) 0.2304(6) 0.2697(5) 0.078(3) Uani 1 1 d . . .
O8 O 0.9150(6) 0.4695(6) 0.4027(3) 0.0532(17) Uani 1 1 d . . .
O7 O 0.7759(6) 0.4477(5) 0.3353(3) 0.0470(15) Uani 1 1 d . . .
O9 O 0.4968(5) 0.5235(5) 0.3544(2) 0.0341(12) Uani 1 1 d . . .
N1 N 0.7118(7) 0.0623(5) 0.1773(3) 0.0349(15) Uani 1 1 d . . .
N2 N 0.8357(7) 0.3579(6) 0.0183(3) 0.0389(16) Uani 1 1 d . . .
N4 N 0.3302(7) 0.9262(5) 0.3136(3) 0.0358(15) Uani 1 1 d . . .
N3 N 0.6034(7) 0.6470(6) 0.4941(3) 0.0342(15) Uani 1 1 d . . .
C29 C 0.5328(8) 0.5596(6) 0.3967(3) 0.0269(15) Uani 1 1 d . . .
C34 C 0.3583(9) 0.7221(7) 0.5171(4) 0.0373(18) Uani 1 1 d . . .
H34 H 0.3818 0.7485 0.5496 0.045 Uiso 1 1 calc R . .
C33 C 0.2207(8) 0.7399(7) 0.5028(4) 0.0374(19) Uani 1 1 d . . .
C16 C 0.6605(8) 0.4343(6) 0.1146(3) 0.0297(16) Uani 1 1 d . . .
C18 C 0.4776(9) 0.3788(7) 0.0722(4) 0.0401(19) Uani 1 1 d . . .
H18 H 0.4188 0.4010 0.1041 0.048 Uiso 1 1 calc R . .
C3 C 0.7558(8) 0.2288(6) 0.2336(3) 0.0296(16) Uani 1 1 d . . .
C28 C 0.6738(8) 0.5466(6) 0.4127(3) 0.0296(16) Uani 1 1 d . . .
C27 C 0.7971(8) 0.4845(7) 0.3810(4) 0.0355(18) Uani 1 1 d . . .
C9 C 0.8445(8) 0.0759(7) 0.1761(4) 0.0334(17) Uani 1 1 d . . .
C14 C 0.8720(9) 0.4827(7) 0.1518(4) 0.0353(18) Uani 1 1 d . . .
C5 C 1.0005(8) 0.1736(7) 0.1983(4) 0.0396(19) Uani 1 1 d . . .
H5 H 1.0178 0.2279 0.2153 0.048 Uiso 1 1 calc R . .
C41 C 0.3741(8) 0.7707(6) 0.2651(4) 0.0343(17) Uani 1 1 d . . .
C13 C 0.6100(8) 0.1259(7) 0.2078(4) 0.0375(19) Uani 1 1 d . . .
H13 H 0.5230 0.1134 0.2100 0.045 Uiso 1 1 calc R . .
C31 C 0.2852(8) 0.6370(7) 0.4226(4) 0.0351(18) Uani 1 1 d . . .
H31 H 0.2594 0.6074 0.3921 0.042 Uiso 1 1 calc R . .
C21 C 0.6483(9) 0.3131(7) -0.0248(4) 0.0393(19) Uani 1 1 d . . .
H21 H 0.7050 0.2919 -0.0575 0.047 Uiso 1 1 calc R . .
C39 C 0.7006(8) 0.5897(7) 0.4611(4) 0.0362(18) Uani 1 1 d . . .
H39 H 0.7931 0.5778 0.4713 0.043 Uiso 1 1 calc R . .
C48 C 0.4717(8) 0.9091(6) 0.3211(4) 0.0337(17) Uani 1 1 d . . .
C2 C 0.6247(8) 0.2055(6) 0.2350(4) 0.0343(18) Uani 1 1 d . . .
C35 C 0.4633(8) 0.6636(6) 0.4821(3) 0.0280(16) Uani 1 1 d . . .
C22 C 0.6987(8) 0.3530(6) 0.0197(4) 0.0328(17) Uani 1 1 d . . .
C42 C 0.5217(8) 0.7506(6) 0.2692(4) 0.0338(18) Uani 1 1 d . . .
C51 C 0.0976(9) 1.0124(8) 0.3587(5) 0.052(2) Uani 1 1 d . . .
H51A H 0.0800 0.9394 0.3654 0.062 Uiso 1 1 calc R . .
H51B H 0.0160 1.0775 0.3472 0.062 Uiso 1 1 calc R . .
C20 C 0.5147(9) 0.3049(7) -0.0204(4) 0.041(2) Uani 1 1 d . . .
C1 C 0.4959(9) 0.2665(6) 0.2649(4) 0.040(2) Uani 1 1 d . . .
C4 C 0.8671(8) 0.1574(6) 0.2028(4) 0.0332(17) Uani 1 1 d . . .
C30 C 0.4267(8) 0.6208(6) 0.4339(3) 0.0275(15) Uani 1 1 d . . .
C46 C 0.6612(9) 0.9575(7) 0.3576(4) 0.041(2) Uani 1 1 d . . .
C10 C 0.6862(9) -0.0203(7) 0.1488(4) 0.043(2) Uani 1 1 d . . .
H10 H 0.7270 -0.1001 0.1715 0.051 Uiso 1 1 calc R . .
C44 C 0.7113(8) 0.8082(7) 0.3047(4) 0.0377(19) Uani 1 1 d . . .
H44 H 0.7757 0.7517 0.2899 0.045 Uiso 1 1 calc R . .
C43 C 0.5666(8) 0.8252(6) 0.2981(4) 0.0304(16) Uani 1 1 d . . .
C6 C 1.1041(8) 0.1093(8) 0.1688(4) 0.044(2) Uani 1 1 d . . .
C17 C 0.6145(8) 0.3880(6) 0.0687(4) 0.0334(17) Uani 1 1 d . . .
C49 C 0.2304(9) 1.0244(7) 0.3300(4) 0.0397(19) Uani 1 1 d . . .
H49 H 0.2282 1.0990 0.3018 0.048 Uiso 1 1 calc R . .
C52 C 0.2884(8) 0.8579(6) 0.2855(4) 0.0379(19) Uani 1 1 d . . .
H52 H 0.1932 0.8723 0.2799 0.045 Uiso 1 1 calc R . .
C47 C 0.5212(9) 0.9767(7) 0.3513(4) 0.042(2) Uani 1 1 d . . .
H47 H 0.4588 1.0334 0.3666 0.050 Uiso 1 1 calc R . .
C32 C 0.1864(8) 0.6953(7) 0.4559(4) 0.0356(18) Uani 1 1 d . . .
C37 C 0.6211(11) 0.7988(10) 0.5446(6) 0.071(3) Uani 1 1 d . . .
H37A H 0.5954 0.8235 0.5833 0.085 Uiso 1 1 calc R . .
H37B H 0.5798 0.8539 0.5056 0.085 Uiso 1 1 calc R . .
C8 C 0.9538(8) 0.0097(7) 0.1465(4) 0.040(2) Uani 1 1 d . . .
H8 H 0.9387 -0.0453 0.1293 0.048 Uiso 1 1 calc R . .
C7 C 1.0817(8) 0.0271(7) 0.1432(4) 0.041(2) Uani 1 1 d . . .
C36 C 0.6443(9) 0.6793(8) 0.5483(5) 0.046(2) Uani 1 1 d . . .
H36 H 0.6334 0.6312 0.5906 0.055 Uiso 1 1 calc R . .
C26 C 0.8802(9) 0.4020(7) 0.0603(4) 0.0389(19) Uani 1 1 d . . .
H26 H 0.9709 0.4071 0.0563 0.047 Uiso 1 1 calc R . .
C15 C 0.8024(8) 0.4396(6) 0.1084(4) 0.0329(17) Uani 1 1 d . . .
C23 C 0.9296(10) 0.3231(8) -0.0318(4) 0.048(2) Uani 1 1 d . . .
H23 H 0.9145 0.3766 -0.0742 0.057 Uiso 1 1 calc R . .
C50 C 0.2044(9) 1.0198(8) 0.3988(4) 0.047(2) Uani 1 1 d . . .
H50A H 0.2531 0.9512 0.4300 0.057 Uiso 1 1 calc R . .
H50B H 0.1891 1.0894 0.4118 0.057 Uiso 1 1 calc R . .
C40 C 0.3094(8) 0.6973(6) 0.2389(4) 0.0384(19) Uani 1 1 d . . .
C11 C 0.6799(10) 0.0044(9) 0.0779(5) 0.056(3) Uani 1 1 d . . .
H11A H 0.7179 -0.0585 0.0587 0.068 Uiso 1 1 calc R . .
H11B H 0.6915 0.0765 0.0531 0.068 Uiso 1 1 calc R . .
C45 C 0.7540(9) 0.8753(7) 0.3327(4) 0.041(2) Uani 1 1 d . . .
C19 C 0.4322(9) 0.3377(7) 0.0291(4) 0.041(2) Uani 1 1 d . . .
C25 C 1.0741(10) 0.2556(10) -0.0148(6) 0.064(3) Uani 1 1 d . . .
H25A H 1.1029 0.2371 0.0295 0.076 Uiso 1 1 calc R . .
H25B H 1.1453 0.2689 -0.0456 0.076 Uiso 1 1 calc R . .
C38 C 0.7628(10) 0.7233(10) 0.5413(5) 0.062(3) Uani 1 1 d . . .
H38A H 0.8086 0.7324 0.5003 0.074 Uiso 1 1 calc R . .
H38B H 0.8242 0.7019 0.5780 0.074 Uiso 1 1 calc R . .
C12 C 0.5503(10) 0.0061(11) 0.1161(6) 0.073(4) Uani 1 1 d . . .
H12A H 0.4835 0.0793 0.1143 0.088 Uiso 1 1 calc R . .
H12B H 0.5099 -0.0557 0.1199 0.088 Uiso 1 1 calc R . .
C24 C 0.9745(10) 0.2004(9) -0.0304(5) 0.060(3) Uani 1 1 d . . .
H24A H 0.9847 0.1804 -0.0708 0.072 Uiso 1 1 calc R . .
H24B H 0.9422 0.1485 0.0044 0.072 Uiso 1 1 calc R . .
O2W O 0.0434(7) 0.3118(7) 0.3121(4) 0.076(2) Uani 1 1 d . . .
H2WA H 0.0905 0.2424 0.3193 0.114 Uiso 1 1 d R . .
H2WB H -0.0250 0.3173 0.2892 0.114 Uiso 1 1 d R . .
O3W O -0.0768(9) 0.7225(7) 0.1853(5) 0.076(2) Uani 1 1 d G . .
H3WA H -0.0617 0.6551 0.2087 0.114 Uiso 1 1 d G . .
H3WB H -0.1378 0.7344 0.1569 0.114 Uiso 1 1 d G . .
O1W O 0.1084(11) 0.5491(9) 0.3301(5) 0.109(3) Uani 1 1 d . . .
H1WA H 0.1491 0.5997 0.3281 0.164 Uiso 1 1 d R . .
H1WB H 0.1320 0.5029 0.3665 0.164 Uiso 1 1 d R . .


_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
Dy2 O7 2.284(6) . ?
Dy2 O2 2.303(5) . ?
Dy2 O12 2.318(5) . ?
Dy2 O6 2.346(5) . ?
Dy2 O4 2.348(5) . ?
Dy2 O10 2.370(6) . ?
Dy2 O9 2.438(5) . ?
Dy2 O3 2.461(5) . ?
Cl3 C33 1.715(7) . ?
Cl4 C46 1.722(8) . ?
Cl2 C20 1.713(8) . ?
Cl1 C7 1.727(8) . ?
F3 C32 1.357(9) . ?
F4 C45 1.356(10) . ?
F1 C6 1.351(10) . ?
F2 C19 1.354(10) . ?
O11 C40 1.254(10) . ?
O10 C40 1.257(9) . ?
O12 C42 1.256(9) . ?
O5 C14 1.243(10) . ?
O4 C14 1.257(9) . ?
O6 C16 1.252(9) . ?
O3 C3 1.242(9) . ?
O2 C1 1.273(9) . ?
O1 C1 1.228(10) . ?
O8 C27 1.248(10) . ?
O7 C27 1.260(9) . ?
O9 C29 1.246(8) . ?
N1 C13 1.363(10) . ?
N1 C9 1.392(10) . ?
N1 C10 1.446(10) . ?
N2 C26 1.350(10) . ?
N2 C22 1.395(10) . ?
N2 C23 1.469(10) . ?
N4 C52 1.357(10) . ?
N4 C48 1.388(10) . ?
N4 C49 1.469(9) . ?
N3 C39 1.332(10) . ?
N3 C35 1.393(10) . ?
N3 C36 1.465(10) . ?
C29 C28 1.433(10) . ?
C29 C30 1.463(10) . ?
C34 C33 1.377(11) . ?
C34 C35 1.411(10) . ?
C34 H34 0.9300 . ?
C33 C32 1.398(11) . ?
C16 C15 1.444(11) . ?
C16 C17 1.446(10) . ?
C18 C19 1.350(11) . ?
C18 C17 1.411(11) . ?
C18 H18 0.9300 . ?
C3 C2 1.431(11) . ?
C3 C4 1.472(10) . ?
C28 C39 1.385(10) . ?
C28 C27 1.497(10) . ?
C9 C4 1.396(10) . ?
C9 C8 1.410(10) . ?
C14 C15 1.507(10) . ?
C5 C6 1.365(11) . ?
C5 C4 1.408(11) . ?
C5 H5 0.9300 . ?
C41 C52 1.353(11) . ?
C41 C42 1.435(11) . ?
C41 C40 1.520(11) . ?
C13 C2 1.350(11) . ?
C13 H13 0.9300 . ?
C31 C32 1.350(11) . ?
C31 C30 1.405(11) . ?
C31 H31 0.9300 . ?
C21 C20 1.373(12) . ?
C21 C22 1.389(11) . ?
C21 H21 0.9300 . ?
C39 H39 0.9300 . ?
C48 C43 1.389(10) . ?
C48 C47 1.420(11) . ?
C2 C1 1.509(11) . ?
C35 C30 1.415(10) . ?
C22 C17 1.404(10) . ?
C42 C43 1.453(11) . ?
C51 C49 1.468(12) . ?
C51 C50 1.466(13) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C20 C19 1.393(12) . ?
C46 C47 1.366(12) . ?
C46 C45 1.387(12) . ?
C10 C12 1.488(14) . ?
C10 C11 1.490(13) . ?
C10 H10 0.9800 . ?
C44 C45 1.347(12) . ?
C44 C43 1.417(11) . ?
C44 H44 0.9300 . ?
C6 C7 1.386(12) . ?
C49 C50 1.490(12) . ?
C49 H49 0.9800 . ?
C52 H52 0.9300 . ?
C47 H47 0.9300 . ?
C37 C36 1.453(14) . ?
C37 C38 1.477(14) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C8 C7 1.361(11) . ?
C8 H8 0.9300 . ?
C36 C38 1.443(13) . ?
C36 H36 0.9800 . ?
C26 C15 1.369(11) . ?
C26 H26 0.9300 . ?
C23 C25 1.468(14) . ?
C23 C24 1.489(13) . ?
C23 H23 0.9800 . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C11 C12 1.496(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C25 C24 1.482(13) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8500 . ?

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
O7 Dy2 O2 107.3(2) . . ?
O7 Dy2 O12 82.4(2) . . ?
O2 Dy2 O12 147.84(19) . . ?
O7 Dy2 O6 143.99(18) . . ?
O2 Dy2 O6 78.7(2) . . ?
O12 Dy2 O6 111.7(2) . . ?
O7 Dy2 O4 81.6(2) . . ?
O2 Dy2 O4 138.71(18) . . ?
O12 Dy2 O4 72.09(19) . . ?
O6 Dy2 O4 72.51(19) . . ?
O7 Dy2 O10 139.80(18) . . ?
O2 Dy2 O10 82.5(2) . . ?
O12 Dy2 O10 71.67(19) . . ?
O6 Dy2 O10 75.58(18) . . ?
O4 Dy2 O10 117.0(2) . . ?
O7 Dy2 O9 70.59(18) . . ?
O2 Dy2 O9 77.92(18) . . ?
O12 Dy2 O9 76.7(2) . . ?
O6 Dy2 O9 143.47(18) . . ?
O4 Dy2 O9 140.45(18) . . ?
O10 Dy2 O9 73.84(18) . . ?
O7 Dy2 O3 74.05(19) . . ?
O2 Dy2 O3 71.09(19) . . ?
O12 Dy2 O3 140.29(19) . . ?
O6 Dy2 O3 74.77(19) . . ?
O4 Dy2 O3 73.17(19) . . ?
O10 Dy2 O3 143.39(18) . . ?
O9 Dy2 O3 122.37(18) . . ?
C40 O10 Dy2 135.2(5) . . ?
C42 O12 Dy2 130.0(5) . . ?
C14 O4 Dy2 133.6(5) . . ?
C16 O6 Dy2 132.7(5) . . ?
C3 O3 Dy2 127.7(5) . . ?
C1 O2 Dy2 136.6(5) . . ?
C27 O7 Dy2 139.5(5) . . ?
C29 O9 Dy2 130.1(5) . . ?
C13 N1 C9 118.1(6) . . ?
C13 N1 C10 121.7(7) . . ?
C9 N1 C10 120.1(6) . . ?
C26 N2 C22 120.3(6) . . ?
C26 N2 C23 119.4(7) . . ?
C22 N2 C23 120.1(6) . . ?
C52 N4 C48 118.8(6) . . ?
C52 N4 C49 121.5(7) . . ?
C48 N4 C49 119.4(6) . . ?
C39 N3 C35 119.7(6) . . ?
C39 N3 C36 119.7(7) . . ?
C35 N3 C36 120.1(6) . . ?
O9 C29 C28 125.0(6) . . ?
O9 C29 C30 119.7(7) . . ?
C28 C29 C30 115.3(6) . . ?
C33 C34 C35 119.5(7) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C33 C32 119.9(7) . . ?
C34 C33 Cl3 120.2(6) . . ?
C32 C33 Cl3 119.9(6) . . ?
O6 C16 C15 124.6(7) . . ?
O6 C16 C17 119.7(7) . . ?
C15 C16 C17 115.7(6) . . ?
C19 C18 C17 119.8(7) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
O3 C3 C2 125.4(7) . . ?
O3 C3 C4 120.3(7) . . ?
C2 C3 C4 114.2(6) . . ?
C39 C28 C29 119.6(7) . . ?
C39 C28 C27 117.0(7) . . ?
C29 C28 C27 123.4(6) . . ?
O8 C27 O7 123.8(7) . . ?
O8 C27 C28 117.9(7) . . ?
O7 C27 C28 118.4(7) . . ?
N1 C9 C4 119.5(6) . . ?
N1 C9 C8 120.0(7) . . ?
C4 C9 C8 120.5(7) . . ?
O5 C14 O4 124.3(7) . . ?
O5 C14 C15 117.5(7) . . ?
O4 C14 C15 118.2(7) . . ?
C6 C5 C4 119.7(7) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C52 C41 C42 119.0(7) . . ?
C52 C41 C40 118.3(7) . . ?
C42 C41 C40 122.7(7) . . ?
C2 C13 N1 125.5(7) . . ?
C2 C13 H13 117.2 . . ?
N1 C13 H13 117.2 . . ?
C32 C31 C30 120.4(7) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C20 C21 C22 120.0(7) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
N3 C39 C28 124.8(7) . . ?
N3 C39 H39 117.6 . . ?
C28 C39 H39 117.6 . . ?
N4 C48 C43 119.5(7) . . ?
N4 C48 C47 121.1(7) . . ?
C43 C48 C47 119.4(7) . . ?
C13 C2 C3 120.3(7) . . ?
C13 C2 C1 115.8(7) . . ?
C3 C2 C1 123.9(7) . . ?
N3 C35 C30 119.2(6) . . ?
N3 C35 C34 120.9(7) . . ?
C30 C35 C34 119.9(7) . . ?
N2 C22 C21 121.6(7) . . ?
N2 C22 C17 117.2(7) . . ?
C21 C22 C17 121.3(7) . . ?
O12 C42 C41 125.0(7) . . ?
O12 C42 C43 119.3(7) . . ?
C41 C42 C43 115.8(6) . . ?
C49 C51 C50 61.0(6) . . ?
C49 C51 H51A 117.7 . . ?
C50 C51 H51A 117.7 . . ?
C49 C51 H51B 117.7 . . ?
C50 C51 H51B 117.7 . . ?
H51A C51 H51B 114.8 . . ?
C21 C20 C19 118.6(7) . . ?
C21 C20 Cl2 120.4(7) . . ?
C19 C20 Cl2 121.0(7) . . ?
O1 C1 O2 123.5(8) . . ?
O1 C1 C2 117.9(7) . . ?
O2 C1 C2 118.6(7) . . ?
C9 C4 C5 118.5(7) . . ?
C9 C4 C3 122.3(7) . . ?
C5 C4 C3 119.1(7) . . ?
C31 C30 C35 118.7(7) . . ?
C31 C30 C29 119.9(6) . . ?
C35 C30 C29 121.4(7) . . ?
C47 C46 C45 120.2(8) . . ?
C47 C46 Cl4 120.3(6) . . ?
C45 C46 Cl4 119.5(7) . . ?
N1 C10 C12 119.1(8) . . ?
N1 C10 C11 119.0(8) . . ?
C12 C10 C11 60.3(7) . . ?
N1 C10 H10 115.7 . . ?
C12 C10 H10 115.7 . . ?
C11 C10 H10 115.7 . . ?
C45 C44 C43 118.9(7) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C48 C43 C44 119.9(7) . . ?
C48 C43 C42 121.6(7) . . ?
C44 C43 C42 118.4(7) . . ?
F1 C6 C5 119.4(8) . . ?
F1 C6 C7 119.2(7) . . ?
C5 C6 C7 121.5(8) . . ?
C22 C17 C18 117.7(7) . . ?
C22 C17 C16 123.3(7) . . ?
C18 C17 C16 119.1(7) . . ?
N4 C49 C51 119.1(7) . . ?
N4 C49 C50 118.2(7) . . ?
C51 C49 C50 59.4(6) . . ?
N4 C49 H49 116.1 . . ?
C51 C49 H49 116.1 . . ?
C50 C49 H49 116.1 . . ?
C41 C52 N4 125.2(8) . . ?
C41 C52 H52 117.4 . . ?
N4 C52 H52 117.4 . . ?
C46 C47 C48 119.4(7) . . ?
C46 C47 H47 120.3 . . ?
C48 C47 H47 120.3 . . ?
F3 C32 C31 120.1(7) . . ?
F3 C32 C33 118.2(7) . . ?
C31 C32 C33 121.6(7) . . ?
C36 C37 C38 59.0(7) . . ?
C36 C37 H37A 117.9 . . ?
C38 C37 H37A 117.9 . . ?
C36 C37 H37B 117.9 . . ?
C38 C37 H37B 117.9 . . ?
H37A C37 H37B 115.0 . . ?
C7 C8 C9 119.5(7) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C8 C7 C6 120.2(7) . . ?
C8 C7 Cl1 120.5(6) . . ?
C6 C7 Cl1 119.3(6) . . ?
C38 C36 N3 118.3(8) . . ?
C38 C36 C37 61.3(7) . . ?
N3 C36 C37 119.3(9) . . ?
C38 C36 H36 115.7 . . ?
N3 C36 H36 115.7 . . ?
C37 C36 H36 115.7 . . ?
N2 C26 C15 125.2(8) . . ?
N2 C26 H26 117.4 . . ?
C15 C26 H26 117.4 . . ?
C26 C15 C16 118.2(7) . . ?
C26 C15 C14 117.4(7) . . ?
C16 C15 C14 124.4(6) . . ?
N2 C23 C25 119.1(8) . . ?
N2 C23 C24 117.7(8) . . ?
C25 C23 C24 60.2(7) . . ?
N2 C23 H23 116.1 . . ?
C25 C23 H23 116.1 . . ?
C24 C23 H23 116.1 . . ?
C51 C50 C49 59.6(6) . . ?
C51 C50 H50A 117.8 . . ?
C49 C50 H50A 117.8 . . ?
C51 C50 H50B 117.8 . . ?
C49 C50 H50B 117.8 . . ?
H50A C50 H50B 115.0 . . ?
O11 C40 O10 124.6(8) . . ?
O11 C40 C41 116.5(7) . . ?
O10 C40 C41 118.9(7) . . ?
C10 C11 C12 59.8(7) . . ?
C10 C11 H11A 117.8 . . ?
C12 C11 H11A 117.8 . . ?
C10 C11 H11B 117.8 . . ?
C12 C11 H11B 117.8 . . ?
H11A C11 H11B 114.9 . . ?
F4 C45 C44 119.3(7) . . ?
F4 C45 C46 118.6(7) . . ?
C44 C45 C46 122.2(8) . . ?
F2 C19 C18 119.9(7) . . ?
F2 C19 C20 117.4(7) . . ?
C18 C19 C20 122.7(8) . . ?
C23 C25 C24 60.6(7) . . ?
C23 C25 H25A 117.7 . . ?
C24 C25 H25A 117.7 . . ?
C23 C25 H25B 117.7 . . ?
C24 C25 H25B 117.7 . . ?
H25A C25 H25B 114.8 . . ?
C36 C38 C37 59.7(6) . . ?
C36 C38 H38A 117.8 . . ?
C37 C38 H38A 117.8 . . ?
C36 C38 H38B 117.8 . . ?
C37 C38 H38B 117.8 . . ?
H38A C38 H38B 114.9 . . ?
C10 C12 C11 59.9(6) . . ?
C10 C12 H12A 117.8 . . ?
C11 C12 H12A 117.8 . . ?
C10 C12 H12B 117.8 . . ?
C11 C12 H12B 117.8 . . ?
H12A C12 H12B 114.9 . . ?
C23 C24 C25 59.2(7) . . ?
C23 C24 H24A 117.9 . . ?
C25 C24 H24A 117.9 . . ?
C23 C24 H24B 117.9 . . ?
C25 C24 H24B 117.9 . . ?
H24A C24 H24B 115.0 . . ?
H2WA O2W H2WB 104.5 . . ?
H3WA O3W H3WB 109.5 . . ?
H1WA O1W H1WB 104.5 . . ?

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
O7 Dy2 O10 C40 15.8(9) . . . . ?
O2 Dy2 O10 C40 123.9(8) . . . . ?
O12 Dy2 O10 C40 -36.7(7) . . . . ?
O6 Dy2 O10 C40 -155.9(8) . . . . ?
O4 Dy2 O10 C40 -94.6(8) . . . . ?
O9 Dy2 O10 C40 44.3(7) . . . . ?
O3 Dy2 O10 C40 167.3(7) . . . . ?
O7 Dy2 O12 C42 -106.5(7) . . . . ?
O2 Dy2 O12 C42 4.2(10) . . . . ?
O6 Dy2 O12 C42 107.9(7) . . . . ?
O4 Dy2 O12 C42 170.0(8) . . . . ?
O10 Dy2 O12 C42 42.4(7) . . . . ?
O9 Dy2 O12 C42 -34.7(7) . . . . ?
O3 Dy2 O12 C42 -160.0(6) . . . . ?
O7 Dy2 O4 C14 113.3(8) . . . . ?
O2 Dy2 O4 C14 6.6(9) . . . . ?
O12 Dy2 O4 C14 -162.0(8) . . . . ?
O6 Dy2 O4 C14 -41.4(8) . . . . ?
O10 Dy2 O4 C14 -104.4(8) . . . . ?
O9 Dy2 O4 C14 158.3(7) . . . . ?
O3 Dy2 O4 C14 37.5(8) . . . . ?
O7 Dy2 O6 C16 -14.7(9) . . . . ?
O2 Dy2 O6 C16 -118.7(7) . . . . ?
O12 Dy2 O6 C16 93.1(7) . . . . ?
O4 Dy2 O6 C16 31.3(7) . . . . ?
O10 Dy2 O6 C16 156.2(7) . . . . ?
O9 Dy2 O6 C16 -169.9(6) . . . . ?
O3 Dy2 O6 C16 -45.5(7) . . . . ?
O7 Dy2 O3 C3 154.6(7) . . . . ?
O2 Dy2 O3 C3 39.5(6) . . . . ?
O12 Dy2 O3 C3 -149.4(6) . . . . ?
O6 Dy2 O3 C3 -43.6(6) . . . . ?
O4 Dy2 O3 C3 -119.5(6) . . . . ?
O10 Dy2 O3 C3 -6.7(8) . . . . ?
O9 Dy2 O3 C3 100.8(6) . . . . ?
O7 Dy2 O2 C1 -106.7(8) . . . . ?
O12 Dy2 O2 C1 149.7(8) . . . . ?
O6 Dy2 O2 C1 36.6(8) . . . . ?
O4 Dy2 O2 C1 -9.6(10) . . . . ?
O10 Dy2 O2 C1 113.3(8) . . . . ?
O9 Dy2 O2 C1 -171.7(9) . . . . ?
O3 Dy2 O2 C1 -41.0(8) . . . . ?
O2 Dy2 O7 C27 -107.8(9) . . . . ?
O12 Dy2 O7 C27 40.8(9) . . . . ?
O6 Dy2 O7 C27 157.6(8) . . . . ?
O4 Dy2 O7 C27 113.7(9) . . . . ?
O10 Dy2 O7 C27 -8.7(11) . . . . ?
O9 Dy2 O7 C27 -37.8(9) . . . . ?
O3 Dy2 O7 C27 -171.5(9) . . . . ?
O7 Dy2 O9 C29 34.8(6) . . . . ?
O2 Dy2 O9 C29 148.3(6) . . . . ?
O12 Dy2 O9 C29 -51.7(6) . . . . ?
O6 Dy2 O9 C29 -160.4(6) . . . . ?
O4 Dy2 O9 C29 -13.1(8) . . . . ?
O10 Dy2 O9 C29 -126.1(6) . . . . ?
O3 Dy2 O9 C29 90.2(6) . . . . ?
Dy2 O9 C29 C28 -27.4(11) . . . . ?
Dy2 O9 C29 C30 152.4(5) . . . . ?
C35 C34 C33 C32 3.0(12) . . . . ?
C35 C34 C33 Cl3 -176.3(6) . . . . ?
Dy2 O6 C16 C15 -22.3(11) . . . . ?
Dy2 O6 C16 C17 157.1(5) . . . . ?
Dy2 O3 C3 C2 -30.0(11) . . . . ?
Dy2 O3 C3 C4 146.9(6) . . . . ?
O9 C29 C28 C39 -179.4(7) . . . . ?
C30 C29 C28 C39 0.8(11) . . . . ?
O9 C29 C28 C27 -1.6(12) . . . . ?
C30 C29 C28 C27 178.7(7) . . . . ?
Dy2 O7 C27 O8 -154.2(7) . . . . ?
Dy2 O7 C27 C28 27.7(13) . . . . ?
C39 C28 C27 O8 4.3(12) . . . . ?
C29 C28 C27 O8 -173.6(8) . . . . ?
C39 C28 C27 O7 -177.6(8) . . . . ?
C29 C28 C27 O7 4.5(12) . . . . ?
C13 N1 C9 C4 -3.4(12) . . . . ?
C10 N1 C9 C4 178.9(8) . . . . ?
C13 N1 C9 C8 178.4(8) . . . . ?
C10 N1 C9 C8 0.6(12) . . . . ?
Dy2 O4 C14 O5 -141.8(7) . . . . ?
Dy2 O4 C14 C15 38.7(11) . . . . ?
C9 N1 C13 C2 3.0(13) . . . . ?
C10 N1 C13 C2 -179.3(8) . . . . ?
C35 N3 C39 C28 2.2(13) . . . . ?
C36 N3 C39 C28 174.4(8) . . . . ?
C29 C28 C39 N3 -2.1(13) . . . . ?
C27 C28 C39 N3 180.0(8) . . . . ?
C52 N4 C48 C43 1.7(11) . . . . ?
C49 N4 C48 C43 -171.8(7) . . . . ?
C52 N4 C48 C47 -178.8(8) . . . . ?
C49 N4 C48 C47 7.7(12) . . . . ?
N1 C13 C2 C3 -0.3(13) . . . . ?
N1 C13 C2 C1 178.8(8) . . . . ?
O3 C3 C2 C13 175.2(8) . . . . ?
C4 C3 C2 C13 -1.8(11) . . . . ?
O3 C3 C2 C1 -3.8(13) . . . . ?
C4 C3 C2 C1 179.1(7) . . . . ?
C39 N3 C35 C30 -1.1(11) . . . . ?
C36 N3 C35 C30 -173.3(7) . . . . ?
C39 N3 C35 C34 178.8(8) . . . . ?
C36 N3 C35 C34 6.7(11) . . . . ?
C33 C34 C35 N3 178.2(7) . . . . ?
C33 C34 C35 C30 -1.8(12) . . . . ?
C26 N2 C22 C21 177.0(8) . . . . ?
C23 N2 C22 C21 1.5(12) . . . . ?
C26 N2 C22 C17 -4.3(12) . . . . ?
C23 N2 C22 C17 -179.7(8) . . . . ?
C20 C21 C22 N2 177.2(8) . . . . ?
C20 C21 C22 C17 -1.5(13) . . . . ?
Dy2 O12 C42 C41 -37.5(12) . . . . ?
Dy2 O12 C42 C43 141.1(6) . . . . ?
C52 C41 C42 O12 -178.9(8) . . . . ?
C40 C41 C42 O12 1.4(13) . . . . ?
C52 C41 C42 C43 2.5(11) . . . . ?
C40 C41 C42 C43 -177.2(7) . . . . ?
C22 C21 C20 C19 0.2(13) . . . . ?
C22 C21 C20 Cl2 179.7(6) . . . . ?
Dy2 O2 C1 O1 -152.3(8) . . . . ?
Dy2 O2 C1 C2 28.1(13) . . . . ?
C13 C2 C1 O1 9.2(13) . . . . ?
C3 C2 C1 O1 -171.7(9) . . . . ?
C13 C2 C1 O2 -171.2(8) . . . . ?
C3 C2 C1 O2 7.9(13) . . . . ?
N1 C9 C4 C5 -176.9(8) . . . . ?
C8 C9 C4 C5 1.4(12) . . . . ?
N1 C9 C4 C3 1.2(12) . . . . ?
C8 C9 C4 C3 179.5(8) . . . . ?
C6 C5 C4 C9 -0.6(13) . . . . ?
C6 C5 C4 C3 -178.9(8) . . . . ?
O3 C3 C4 C9 -175.9(8) . . . . ?
C2 C3 C4 C9 1.3(11) . . . . ?
O3 C3 C4 C5 2.3(12) . . . . ?
C2 C3 C4 C5 179.5(7) . . . . ?
C32 C31 C30 C35 2.0(12) . . . . ?
C32 C31 C30 C29 -178.7(7) . . . . ?
N3 C35 C30 C31 179.3(7) . . . . ?
C34 C35 C30 C31 -0.7(11) . . . . ?
N3 C35 C30 C29 0.0(11) . . . . ?
C34 C35 C30 C29 -179.9(7) . . . . ?
O9 C29 C30 C31 1.0(11) . . . . ?
C28 C29 C30 C31 -179.2(7) . . . . ?
O9 C29 C30 C35 -179.7(7) . . . . ?
C28 C29 C30 C35 0.1(10) . . . . ?
C13 N1 C10 C12 38.0(13) . . . . ?
C9 N1 C10 C12 -144.3(9) . . . . ?
C13 N1 C10 C11 108.2(9) . . . . ?
C9 N1 C10 C11 -74.2(11) . . . . ?
N4 C48 C43 C44 179.1(7) . . . . ?
C47 C48 C43 C44 -0.4(12) . . . . ?
N4 C48 C43 C42 -3.0(12) . . . . ?
C47 C48 C43 C42 177.4(8) . . . . ?
C45 C44 C43 C48 -0.7(12) . . . . ?
C45 C44 C43 C42 -178.6(8) . . . . ?
O12 C42 C43 C48 -177.8(7) . . . . ?
C41 C42 C43 C48 0.9(11) . . . . ?
O12 C42 C43 C44 0.0(11) . . . . ?
C41 C42 C43 C44 178.8(7) . . . . ?
C4 C5 C6 F1 -179.8(8) . . . . ?
C4 C5 C6 C7 -0.4(14) . . . . ?
N2 C22 C17 C18 -177.4(7) . . . . ?
C21 C22 C17 C18 1.4(12) . . . . ?
N2 C22 C17 C16 3.7(12) . . . . ?
C21 C22 C17 C16 -177.5(7) . . . . ?
C19 C18 C17 C22 -0.2(12) . . . . ?
C19 C18 C17 C16 178.8(8) . . . . ?
O6 C16 C17 C22 178.7(7) . . . . ?
C15 C16 C17 C22 -1.9(11) . . . . ?
O6 C16 C17 C18 -0.1(11) . . . . ?
C15 C16 C17 C18 179.2(7) . . . . ?
C52 N4 C49 C51 42.5(12) . . . . ?
C48 N4 C49 C51 -144.1(8) . . . . ?
C52 N4 C49 C50 111.2(9) . . . . ?
C48 N4 C49 C50 -75.4(10) . . . . ?
C50 C51 C49 N4 107.4(9) . . . . ?
C42 C41 C52 N4 -4.0(13) . . . . ?
C40 C41 C52 N4 175.6(8) . . . . ?
C48 N4 C52 C41 1.9(13) . . . . ?
C49 N4 C52 C41 175.3(8) . . . . ?
C45 C46 C47 C48 2.2(14) . . . . ?
Cl4 C46 C47 C48 -179.1(7) . . . . ?
N4 C48 C47 C46 -179.9(8) . . . . ?
C43 C48 C47 C46 -0.4(13) . . . . ?
C30 C31 C32 F3 179.7(7) . . . . ?
C30 C31 C32 C33 -0.9(13) . . . . ?
C34 C33 C32 F3 177.7(8) . . . . ?
Cl3 C33 C32 F3 -3.0(11) . . . . ?
C34 C33 C32 C31 -1.7(13) . . . . ?
Cl3 C33 C32 C31 177.6(7) . . . . ?
N1 C9 C8 C7 177.3(8) . . . . ?
C4 C9 C8 C7 -1.0(13) . . . . ?
C9 C8 C7 C6 -0.1(14) . . . . ?
C9 C8 C7 Cl1 -178.1(7) . . . . ?
F1 C6 C7 C8 -179.8(9) . . . . ?
C5 C6 C7 C8 0.8(15) . . . . ?
F1 C6 C7 Cl1 -1.7(13) . . . . ?
C5 C6 C7 Cl1 178.9(7) . . . . ?
C39 N3 C36 C38 42.9(12) . . . . ?
C35 N3 C36 C38 -145.0(9) . . . . ?
C39 N3 C36 C37 114.1(10) . . . . ?
C35 N3 C36 C37 -73.8(11) . . . . ?
C38 C37 C36 N3 -108.2(10) . . . . ?
C22 N2 C26 C15 3.2(13) . . . . ?
C23 N2 C26 C15 178.7(8) . . . . ?
N2 C26 C15 C16 -1.2(13) . . . . ?
N2 C26 C15 C14 178.1(8) . . . . ?
O6 C16 C15 C26 179.8(8) . . . . ?
C17 C16 C15 C26 0.4(11) . . . . ?
O6 C16 C15 C14 0.6(12) . . . . ?
C17 C16 C15 C14 -178.8(7) . . . . ?
O5 C14 C15 C26 -6.7(12) . . . . ?
O4 C14 C15 C26 172.9(8) . . . . ?
O5 C14 C15 C16 172.6(8) . . . . ?
O4 C14 C15 C16 -7.9(12) . . . . ?
C26 N2 C23 C25 46.1(12) . . . . ?
C22 N2 C23 C25 -138.4(9) . . . . ?
C26 N2 C23 C24 115.5(9) . . . . ?
C22 N2 C23 C24 -69.0(12) . . . . ?
N4 C49 C50 C51 -108.9(8) . . . . ?
Dy2 O10 C40 O11 -156.7(7) . . . . ?
Dy2 O10 C40 C41 22.7(12) . . . . ?
C52 C41 C40 O11 6.1(12) . . . . ?
C42 C41 C40 O11 -174.2(8) . . . . ?
C52 C41 C40 O10 -173.4(8) . . . . ?
C42 C41 C40 O10 6.2(12) . . . . ?
N1 C10 C11 C12 -108.9(9) . . . . ?
C43 C44 C45 F4 -177.4(8) . . . . ?
C43 C44 C45 C46 2.6(13) . . . . ?
C47 C46 C45 F4 176.6(8) . . . . ?
Cl4 C46 C45 F4 -2.1(12) . . . . ?
C47 C46 C45 C44 -3.3(14) . . . . ?
Cl4 C46 C45 C44 177.9(7) . . . . ?
C17 C18 C19 F2 179.5(8) . . . . ?
C17 C18 C19 C20 -1.1(14) . . . . ?
C21 C20 C19 F2 -179.5(8) . . . . ?
Cl2 C20 C19 F2 1.0(12) . . . . ?
C21 C20 C19 C18 1.0(14) . . . . ?
Cl2 C20 C19 C18 -178.4(7) . . . . ?
N2 C23 C25 C24 107.1(9) . . . . ?
N3 C36 C38 C37 109.9(10) . . . . ?
N1 C10 C12 C11 108.7(9) . . . . ?
N2 C23 C24 C25 -109.4(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.187
_refine_diff_density_min         -2.075
_refine_diff_density_rms         0.129

# start Validation Reply Form 
_vrf_PLAT414_2d                  
;
PROBLEM:  
RESPONSE: The disorder of H1WA. 
;
_vrf_PLAT415_2d                  
;
PROBLEM:  
RESPONSE: The disorder of H2WA. 
;
_vrf_PLAT420_2d                  
;
PROBLEM:  
RESPONSE: The disorder of H2WA and H3WB. 
;
_vrf_PLAT910_2d                  
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature. 
;
# end Validation Reply Form

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

data_2e
_database_code_depnum_ccdc_archive 'CCDC 1855017'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_vrf_PLAT910_2e                  
;
PROBLEM:  Missing # of FCF Reflection(s) Below Theta(Min).         23 Note
RESPONSE: Unimportant number of missing reflections.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Eu K (H2 O)2 (C13 H8 Cl F N O3)4, (H2 O)'
_chemical_formula_sum            'C52 H38 Cl4 Er F4 K N4 O15'
_chemical_formula_weight         1383.02

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   10.0569(5)
_cell_length_b                   12.7687(6)
_cell_length_c                   21.6123(9)
_cell_angle_alpha                74.868(4)
_cell_angle_beta                 86.659(4)
_cell_angle_gamma                72.952(4)
_cell_volume                     2560.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9279
_cell_measurement_theta_min      3.7590
_cell_measurement_theta_max      27.5130

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_F_000             1378
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    2.019
_shelx_estimated_absorpt_T_min   0.403
_shelx_estimated_absorpt_T_max   0.632
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23652
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.391
_diffrn_reflns_theta_max         27.621
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11405
_reflns_number_gt                9458
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.0646P)²+6.1032P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11405
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1516
_refine_ls_wR_factor_gt          0.1415
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_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
Er1 Er 0.38840(3) 0.51162(2) 0.24319(2) 0.03145(10) Uani 1 1 d . . . . .
K1 K 0.7989(3) 0.5493(2) 0.25780(14) 0.0978(8) Uani 1 1 d . . . . .
Cl1 Cl -0.2125(2) 1.04600(19) 0.39677(11) 0.0645(6) Uani 1 1 d . . . . .
Cl2 Cl 0.5511(2) 0.74231(18) 0.57825(10) 0.0582(5) Uani 1 1 d . . . . .
Cl3 Cl 0.90751(19) 0.18023(17) -0.04200(10) 0.0553(5) Uani 1 1 d . . . . .
Cl4 Cl 0.2791(2) -0.03813(18) 0.10615(11) 0.0635(6) Uani 1 1 d . . . . .
F1 F -0.2282(4) 0.8713(4) 0.3366(3) 0.0691(14) Uani 1 1 d . . . . .
F2 F 0.6988(5) 0.6740(5) 0.4687(2) 0.0681(14) Uani 1 1 d . . . . .
F3 F 0.9504(4) 0.2877(4) 0.0553(2) 0.0614(12) Uani 1 1 d . . . . .
F4 F 0.1106(4) 0.1378(4) 0.1631(3) 0.0655(13) Uani 1 1 d . . . . .
O1 O 0.6090(6) 0.7674(5) 0.2309(4) 0.0731(19) Uani 1 1 d . . . . .
O2 O 0.5026(5) 0.6465(4) 0.2162(2) 0.0396(10) Uani 1 1 d . . . . .
O3 O 0.2243(5) 0.6944(3) 0.2463(2) 0.0375(10) Uani 1 1 d . . . . .
O4 O 0.0037(5) 0.5262(5) 0.3547(2) 0.0535(14) Uani 1 1 d . . . . .
O5 O 0.2051(5) 0.4727(4) 0.3070(2) 0.0382(10) Uani 1 1 d . . . . .
O6 O 0.4241(4) 0.5359(4) 0.3432(2) 0.0361(10) Uani 1 1 d . . . . .
O7 O 0.0873(5) 0.5350(5) 0.0962(2) 0.0536(14) Uani 1 1 d . . . . .
O8 O 0.2267(5) 0.5534(4) 0.1651(2) 0.0434(11) Uani 1 1 d . . . . .
O9 O 0.5060(4) 0.4766(4) 0.14606(19) 0.0348(10) Uani 1 1 d . . . . .
O10 O 0.8207(5) 0.2737(5) 0.2708(3) 0.0702(18) Uani 1 1 d . . . . .
O11 O 0.6132(5) 0.3932(4) 0.2754(2) 0.0376(10) Uani 1 1 d . . . . .
O12 O 0.3895(5) 0.3293(4) 0.2483(2) 0.0423(11) Uani 1 1 d . . . . .
O1W O 0.8964(9) 0.4451(7) 0.1680(4) 0.105(3) Uani 1 1 d . . . . .
H11 H 0.9561 0.4734 0.1470 0.157 Uiso 1 1 d R U . . .
H12 H 0.9334 0.3759 0.1848 0.157 Uiso 1 1 d R U . . .
O2W O 0.9562(6) 0.6882(5) 0.1887(3) 0.0751(19) Uani 1 1 d . . . . .
H21 H 1.0183 0.6891 0.2128 0.113 Uiso 1 1 d R U . . .
H22 H 0.9935 0.6628 0.1578 0.113 Uiso 1 1 d R U . . .
O3W O 1.0844(7) 0.2759(5) 0.3142(3) 0.0775(19) Uani 1 1 d . . . . .
H31 H 1.1026 0.3378 0.3089 0.116 Uiso 1 1 d R U . . .
H32 H 1.0041 0.2890 0.2993 0.116 Uiso 1 1 d R U . . .
N1 N 0.2906(6) 0.9355(4) 0.3236(3) 0.0369(12) Uani 1 1 d . . . . .
N2 N 0.1674(6) 0.6392(5) 0.4834(2) 0.0368(12) Uani 1 1 d . . . . .
N3 N 0.3980(5) 0.3533(4) 0.0056(3) 0.0346(12) Uani 1 1 d . . . . .
N4 N 0.6717(5) 0.0750(4) 0.1882(3) 0.0371(12) Uani 1 1 d . . . . .
C1 C 0.5064(7) 0.7318(5) 0.2355(3) 0.0408(16) Uani 1 1 d . . . . .
C2 C 0.3927(7) 0.8736(5) 0.2933(3) 0.0377(14) Uani 1 1 d . . . . .
H2 H 0.4791 0.8871 0.2912 0.045 Uiso 1 1 calc R U . . .
C3 C 0.3787(6) 0.7928(5) 0.2653(3) 0.0335(13) Uani 1 1 d . . . . .
C4 C 0.2471(6) 0.7700(5) 0.2670(3) 0.0306(12) Uani 1 1 d . . . . .
C5 C 0.1345(6) 0.8410(5) 0.2981(3) 0.0339(13) Uani 1 1 d . . . . .
C6 C 0.0021(7) 0.8247(6) 0.3023(3) 0.0411(15) Uani 1 1 d . . . . .
H6 H -0.0149 0.7706 0.2847 0.049 Uiso 1 1 calc R U . . .
C7 C -0.1019(7) 0.8879(6) 0.3321(4) 0.0460(17) Uani 1 1 d . . . . .
C8 C -0.0786(7) 0.9700(6) 0.3583(3) 0.0430(16) Uani 1 1 d . . . . .
C9 C 0.0488(7) 0.9890(6) 0.3547(3) 0.0414(16) Uani 1 1 d . . . . .
H9 H 0.0629 1.0453 0.3713 0.050 Uiso 1 1 calc R U . . .
C10 C 0.1591(7) 0.9222(5) 0.3253(3) 0.0355(14) Uani 1 1 d . . . . .
C11 C 0.3164(7) 1.0194(6) 0.3529(4) 0.0442(16) Uani 1 1 d . . . . .
H11A H 0.2751 1.0990 0.3304 0.053 Uiso 1 1 calc R U . . .
C12 C 0.3232(8) 0.9941(7) 0.4236(4) 0.056(2) Uani 1 1 d . . . . .
H12A H 0.3118 0.9220 0.4481 0.068 Uiso 1 1 calc R U . . .
H12B H 0.2853 1.0565 0.4433 0.068 Uiso 1 1 calc R U . . .
C13 C 0.4515(9) 0.9928(8) 0.3857(5) 0.070(3) Uani 1 1 d . . . . .
H13A H 0.4918 1.0543 0.3824 0.084 Uiso 1 1 calc R U . . .
H13B H 0.5183 0.9198 0.3871 0.084 Uiso 1 1 calc R U . . .
C14 C 0.1299(7) 0.5166(5) 0.3475(3) 0.0340(13) Uani 1 1 d . . . . .
C15 C 0.1228(7) 0.5961(5) 0.4409(3) 0.0391(15) Uani 1 1 d . . . . .
H15 H 0.0324 0.5905 0.4447 0.047 Uiso 1 1 calc R U . . .
C16 C 0.2018(7) 0.5594(5) 0.3919(3) 0.0322(13) Uani 1 1 d . . . . .
C17 C 0.3402(6) 0.5661(5) 0.3854(3) 0.0297(12) Uani 1 1 d . . . . .
C18 C 0.3890(7) 0.6121(5) 0.4326(3) 0.0318(13) Uani 1 1 d . . . . .
C19 C 0.5228(7) 0.6224(6) 0.4287(3) 0.0391(15) Uani 1 1 d . . . . .
H19 H 0.5806 0.6011 0.3962 0.047 Uiso 1 1 calc R U . . .
C20 C 0.5701(7) 0.6641(6) 0.4726(3) 0.0390(15) Uani 1 1 d . . . . .
C21 C 0.4856(7) 0.6949(5) 0.5224(3) 0.0378(15) Uani 1 1 d . . . . .
C22 C 0.3547(7) 0.6848(5) 0.5273(3) 0.0372(14) Uani 1 1 d . . . . .
H22A H 0.2993 0.7041 0.5609 0.045 Uiso 1 1 calc R U . . .
C23 C 0.3025(7) 0.6454(5) 0.4817(3) 0.0316(13) Uani 1 1 d . . . . .
C24 C 0.0738(8) 0.6744(6) 0.5335(3) 0.0457(17) Uani 1 1 d . . . . .
H24 H 0.0882 0.6206 0.5758 0.055 Uiso 1 1 calc R U . . .
C25 C -0.0713(8) 0.7421(8) 0.5159(4) 0.062(2) Uani 1 1 d . . . . .
H25A H -0.1428 0.7282 0.5464 0.075 Uiso 1 1 calc R U . . .
H25B H -0.0997 0.7617 0.4712 0.075 Uiso 1 1 calc R U . . .
C26 C 0.0283(8) 0.7958(7) 0.5332(5) 0.064(2) Uani 1 1 d . . . . .
H26A H 0.0608 0.8481 0.4991 0.077 Uiso 1 1 calc R U . . .
H26B H 0.0177 0.8146 0.5742 0.077 Uiso 1 1 calc R U . . .
C27 C 0.2047(7) 0.5187(5) 0.1186(3) 0.0349(14) Uani 1 1 d . . . . .
C28 C 0.3007(6) 0.4126(5) 0.0384(3) 0.0335(13) Uani 1 1 d . . . . .
H28 H 0.2080 0.4262 0.0275 0.040 Uiso 1 1 calc R U . . .
C29 C 0.3285(6) 0.4547(5) 0.0870(3) 0.0285(12) Uani 1 1 d . . . . .
C30 C 0.4679(6) 0.4408(5) 0.1035(3) 0.0302(12) Uani 1 1 d . . . . .
C31 C 0.5751(6) 0.3780(5) 0.0665(3) 0.0292(12) Uani 1 1 d . . . . .
C32 C 0.7148(6) 0.3620(5) 0.0779(3) 0.0348(14) Uani 1 1 d . . . . .
H32A H 0.7405 0.3915 0.1088 0.042 Uiso 1 1 calc R U . . .
C33 C 0.8141(6) 0.3039(6) 0.0445(3) 0.0380(14) Uani 1 1 d . . . . .
C34 C 0.7785(7) 0.2587(5) -0.0028(3) 0.0382(15) Uani 1 1 d . . . . .
C35 C 0.6418(7) 0.2773(5) -0.0173(3) 0.0369(14) Uani 1 1 d . . . . .
H35 H 0.6176 0.2514 -0.0502 0.044 Uiso 1 1 calc R U . . .
C36 C 0.5375(6) 0.3360(5) 0.0181(3) 0.0297(12) Uani 1 1 d . . . . .
C37 C 0.3556(8) 0.3193(7) -0.0481(4) 0.0484(18) Uani 1 1 d . . . . .
H37 H 0.3664 0.3664 -0.0907 0.058 Uiso 1 1 calc R U . . .
C38 C 0.2363(8) 0.2758(7) -0.0413(4) 0.061(2) Uani 1 1 d . . . . .
H38A H 0.1751 0.2967 -0.0783 0.073 Uiso 1 1 calc R U . . .
H38B H 0.1905 0.2674 -0.0003 0.073 Uiso 1 1 calc R U . . .
C39 C 0.3791(9) 0.2002(8) -0.0441(5) 0.067(3) Uani 1 1 d . . . . .
H39A H 0.4205 0.1457 -0.0048 0.081 Uiso 1 1 calc R U . . .
H39B H 0.4051 0.1750 -0.0829 0.081 Uiso 1 1 calc R U . . .
C40 C 0.6923(7) 0.3044(5) 0.2633(3) 0.0379(14) Uani 1 1 d . . . . .
C41 C 0.7147(7) 0.1424(5) 0.2169(3) 0.0368(14) Uani 1 1 d . . . . .
H41 H 0.8099 0.1274 0.2232 0.044 Uiso 1 1 calc R U . . .
C42 C 0.6276(6) 0.2311(5) 0.2372(3) 0.0327(13) Uani 1 1 d . . . . .
C43 C 0.4808(6) 0.2516(5) 0.2314(3) 0.0299(12) Uani 1 1 d . . . . .
C44 C 0.4353(6) 0.1772(5) 0.2025(3) 0.0318(13) Uani 1 1 d . . . . .
C45 C 0.2914(7) 0.1933(5) 0.1957(3) 0.0378(14) Uani 1 1 d . . . . .
H45 H 0.2269 0.2501 0.2102 0.045 Uiso 1 1 calc R U . . .
C46 C 0.2485(7) 0.1249(6) 0.1676(4) 0.0422(16) Uani 1 1 d . . . . .
C47 C 0.3427(7) 0.0420(5) 0.1433(3) 0.0390(15) Uani 1 1 d . . . . .
C48 C 0.4824(7) 0.0244(5) 0.1500(3) 0.0400(15) Uani 1 1 d . . . . .
H48 H 0.5455 -0.0322 0.1348 0.048 Uiso 1 1 calc R U . . .
C49 C 0.5301(7) 0.0919(5) 0.1800(3) 0.0350(14) Uani 1 1 d . . . . .
C50 C 0.7704(7) -0.0231(5) 0.1719(3) 0.0406(15) Uani 1 1 d . . . . .
H50 H 0.7727 -0.0974 0.2002 0.049 Uiso 1 1 calc R U . . .
C51 C 0.9063(8) -0.0109(6) 0.1428(4) 0.0525(19) Uani 1 1 d . . . . .
H51A H 0.9236 0.0621 0.1360 0.063 Uiso 1 1 calc R U . . .
H51B H 0.9880 -0.0759 0.1543 0.063 Uiso 1 1 calc R U . . .
C52 C 0.7960(8) -0.0188(6) 0.1025(4) 0.0475(17) Uani 1 1 d . . . . .
H52A H 0.8110 -0.0885 0.0894 0.057 Uiso 1 1 calc R U . . .
H52B H 0.7466 0.0493 0.0711 0.057 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O8 2.262(4) . ?
Er1 O2 2.277(5) . ?
Er1 O12 2.298(4) . ?
Er1 O6 2.324(4) . ?
Er1 O5 2.331(5) . ?
Er1 O11 2.348(4) . ?
Er1 O9 2.428(4) . ?
Er1 O3 2.446(4) . ?
Er1 K1 4.332(3) . ?
K1 O1W 2.618(8) . ?
K1 O2W 2.805(8) . ?
K1 O1 2.812(6) . ?
K1 O4 2.922(6) 1_655 ?
K1 O2 2.965(5) . ?
K1 O11 3.051(6) . ?
K1 O10 3.399(6) . ?
Cl1 C8 1.724(7) . ?
Cl2 C21 1.723(6) . ?
Cl3 C34 1.720(6) . ?
Cl4 C47 1.725(6) . ?
F1 C7 1.342(8) . ?
F2 C20 1.333(8) . ?
F3 C33 1.349(7) . ?
F4 C46 1.354(8) . ?
O1 C1 1.234(8) . ?
O2 C1 1.275(7) . ?
O3 C4 1.246(7) . ?
O4 C14 1.243(8) . ?
O4 K1 2.922(6) 1_455 ?
O5 C14 1.258(7) . ?
O6 C17 1.263(7) . ?
O7 C27 1.242(8) . ?
O8 C27 1.254(7) . ?
O9 C30 1.251(7) . ?
O10 C40 1.242(8) . ?
O11 C40 1.261(7) . ?
O12 C43 1.256(7) . ?
N1 C2 1.351(8) . ?
N1 C10 1.379(8) . ?
N1 C11 1.467(8) . ?
N2 C15 1.344(8) . ?
N2 C23 1.382(8) . ?
N2 C24 1.465(8) . ?
N3 C28 1.340(7) . ?
N3 C36 1.386(8) . ?
N3 C37 1.465(8) . ?
N4 C41 1.357(8) . ?
N4 C49 1.390(8) . ?
N4 C50 1.463(7) . ?
C1 C3 1.500(8) . ?
C2 C3 1.367(8) . ?
C3 C4 1.433(8) . ?
C4 C5 1.479(8) . ?
C5 C6 1.401(9) . ?
C5 C10 1.403(8) . ?
C6 C7 1.363(9) . ?
C7 C8 1.393(9) . ?
C8 C9 1.367(9) . ?
C9 C10 1.417(8) . ?
C11 C12 1.478(11) . ?
C11 C13 1.477(11) . ?
C12 C13 1.486(12) . ?
C14 C16 1.526(8) . ?
C15 C16 1.384(8) . ?
C16 C17 1.416(8) . ?
C17 C18 1.471(8) . ?
C18 C19 1.386(9) . ?
C18 C23 1.406(8) . ?
C19 C20 1.369(9) . ?
C20 C21 1.396(9) . ?
C21 C22 1.355(9) . ?
C22 C23 1.405(8) . ?
C24 C26 1.481(11) . ?
C24 C25 1.474(11) . ?
C25 C26 1.481(11) . ?
C27 C29 1.509(8) . ?
C28 C29 1.374(8) . ?
C29 C30 1.416(8) . ?
C30 C31 1.474(7) . ?
C31 C32 1.387(8) . ?
C31 C36 1.407(8) . ?
C32 C33 1.352(8) . ?
C33 C34 1.407(9) . ?
C34 C35 1.366(9) . ?
C35 C36 1.411(8) . ?
C37 C38 1.448(10) . ?
C37 C39 1.449(11) . ?
C38 C39 1.485(11) . ?
C40 C42 1.514(8) . ?
C41 C42 1.369(8) . ?
C42 C43 1.428(8) . ?
C43 C44 1.450(8) . ?
C44 C49 1.395(8) . ?
C44 C45 1.411(9) . ?
C45 C46 1.359(9) . ?
C46 C47 1.392(9) . ?
C47 C48 1.366(9) . ?
C48 C49 1.401(9) . ?
C50 C52 1.496(10) . ?
C50 C51 1.503(10) . ?
C51 C52 1.492(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Er1 O2 106.97(18) . . ?
O8 Er1 O12 82.33(17) . . ?
O2 Er1 O12 147.81(15) . . ?
O8 Er1 O6 143.62(15) . . ?
O2 Er1 O6 78.81(16) . . ?
O12 Er1 O6 112.25(17) . . ?
O8 Er1 O5 81.09(17) . . ?
O2 Er1 O5 139.36(14) . . ?
O12 Er1 O5 71.69(15) . . ?
O6 Er1 O5 73.13(15) . . ?
O8 Er1 O11 140.69(14) . . ?
O2 Er1 O11 82.13(16) . . ?
O12 Er1 O11 72.50(15) . . ?
O6 Er1 O11 75.16(14) . . ?
O5 Er1 O11 117.15(16) . . ?
O8 Er1 O9 71.24(15) . . ?
O2 Er1 O9 77.44(15) . . ?
O12 Er1 O9 76.71(16) . . ?
O6 Er1 O9 143.02(15) . . ?
O5 Er1 O9 140.25(14) . . ?
O11 Er1 O9 73.85(14) . . ?
O8 Er1 O3 73.38(15) . . ?
O2 Er1 O3 71.43(15) . . ?
O12 Er1 O3 139.80(15) . . ?
O6 Er1 O3 74.85(15) . . ?
O5 Er1 O3 73.24(15) . . ?
O11 Er1 O3 143.13(14) . . ?
O9 Er1 O3 122.48(15) . . ?
O8 Er1 K1 137.08(14) . . ?
O2 Er1 K1 39.77(12) . . ?
O12 Er1 K1 113.72(12) . . ?
O6 Er1 K1 69.28(11) . . ?
O5 Er1 K1 141.01(11) . . ?
O11 Er1 K1 42.59(11) . . ?
O9 Er1 K1 74.31(11) . . ?
O3 Er1 K1 105.83(11) . . ?
O1W K1 O2W 79.5(2) . . ?
O1W K1 O1 122.3(3) . . ?
O2W K1 O1 76.47(18) . . ?
O1W K1 O4 115.0(2) . 1_655 ?
O2W K1 O4 78.43(18) . 1_655 ?
O1 K1 O4 110.37(19) . 1_655 ?
O1W K1 O2 100.0(2) . . ?
O2W K1 O2 110.16(18) . . ?
O1 K1 O2 44.93(14) . . ?
O4 K1 O2 145.07(15) 1_655 . ?
O1W K1 O11 80.31(19) . . ?
O2W K1 O11 155.78(18) . . ?
O1 K1 O11 103.58(16) . . ?
O4 K1 O11 122.62(17) 1_655 . ?
O2 K1 O11 60.66(13) . . ?
O1W K1 O10 56.4(2) . . ?
O2W K1 O10 131.58(18) . . ?
O1 K1 O10 142.03(17) . . ?
O4 K1 O10 101.34(17) 1_655 . ?
O2 K1 O10 97.21(14) . . ?
O11 K1 O10 39.61(12) . . ?
O1W K1 Er1 92.65(18) . . ?
O2W K1 Er1 137.17(15) . . ?
O1 K1 Er1 72.59(12) . . ?
O4 K1 Er1 140.28(14) 1_655 . ?
O2 K1 Er1 29.43(9) . . ?
O11 K1 Er1 31.39(9) . . ?
O10 K1 Er1 69.69(10) . . ?
C1 O1 K1 93.7(4) . . ?
C1 O2 Er1 136.6(4) . . ?
C1 O2 K1 85.9(4) . . ?
Er1 O2 K1 110.80(17) . . ?
C4 O3 Er1 127.2(4) . . ?
C14 O4 K1 127.7(4) . 1_455 ?
C14 O5 Er1 134.7(4) . . ?
C17 O6 Er1 131.8(4) . . ?
C27 O8 Er1 139.9(4) . . ?
C30 O9 Er1 129.1(4) . . ?
C40 O10 K1 87.3(4) . . ?
C40 O11 Er1 135.7(4) . . ?
C40 O11 K1 103.6(4) . . ?
Er1 O11 K1 106.01(15) . . ?
C43 O12 Er1 129.8(4) . . ?
C2 N1 C10 119.5(5) . . ?
C2 N1 C11 121.0(5) . . ?
C10 N1 C11 119.5(5) . . ?
C15 N2 C23 120.2(5) . . ?
C15 N2 C24 119.4(6) . . ?
C23 N2 C24 120.3(5) . . ?
C28 N3 C36 119.7(5) . . ?
C28 N3 C37 119.4(5) . . ?
C36 N3 C37 120.5(5) . . ?
C41 N4 C49 119.6(5) . . ?
C41 N4 C50 121.3(5) . . ?
C49 N4 C50 118.8(5) . . ?
O1 C1 O2 123.7(6) . . ?
O1 C1 C3 118.0(6) . . ?
O2 C1 C3 118.3(6) . . ?
N1 C2 C3 125.0(6) . . ?
C2 C3 C4 119.4(5) . . ?
C2 C3 C1 116.4(6) . . ?
C4 C3 C1 124.2(5) . . ?
O3 C4 C3 125.0(5) . . ?
O3 C4 C5 119.7(6) . . ?
C3 C4 C5 115.3(5) . . ?
C6 C5 C10 119.4(5) . . ?
C6 C5 C4 119.5(5) . . ?
C10 C5 C4 121.0(6) . . ?
C7 C6 C5 120.1(6) . . ?
F1 C7 C6 120.0(6) . . ?
F1 C7 C8 119.3(6) . . ?
C6 C7 C8 120.7(7) . . ?
C9 C8 C7 120.8(6) . . ?
C9 C8 Cl1 120.2(5) . . ?
C7 C8 Cl1 119.0(5) . . ?
C8 C9 C10 119.3(6) . . ?
N1 C10 C5 119.7(5) . . ?
N1 C10 C9 120.7(5) . . ?
C5 C10 C9 119.6(6) . . ?
C12 C11 N1 118.6(6) . . ?
C12 C11 C13 60.4(6) . . ?
N1 C11 C13 118.7(6) . . ?
C11 C12 C13 59.7(6) . . ?
C11 C13 C12 59.9(5) . . ?
O4 C14 O5 125.5(6) . . ?
O4 C14 C16 118.0(5) . . ?
O5 C14 C16 116.6(6) . . ?
N2 C15 C16 124.7(6) . . ?
C15 C16 C17 118.8(5) . . ?
C15 C16 C14 116.4(6) . . ?
C17 C16 C14 124.8(5) . . ?
O6 C17 C16 125.8(5) . . ?
O6 C17 C18 117.9(5) . . ?
C16 C17 C18 116.3(5) . . ?
C19 C18 C23 119.3(5) . . ?
C19 C18 C17 119.5(5) . . ?
C23 C18 C17 121.2(6) . . ?
C20 C19 C18 120.1(6) . . ?
F2 C20 C19 119.9(6) . . ?
F2 C20 C21 119.3(6) . . ?
C19 C20 C21 120.8(6) . . ?
C22 C21 C20 120.1(6) . . ?
C22 C21 Cl2 120.6(5) . . ?
C20 C21 Cl2 119.3(5) . . ?
C21 C22 C23 120.2(6) . . ?
N2 C23 C18 118.8(5) . . ?
N2 C23 C22 121.7(5) . . ?
C18 C23 C22 119.5(6) . . ?
N2 C24 C26 118.7(6) . . ?
N2 C24 C25 119.1(6) . . ?
C26 C24 C25 60.2(5) . . ?
C24 C25 C26 60.1(5) . . ?
C24 C26 C25 59.7(5) . . ?
O8 C27 O7 124.1(6) . . ?
O8 C27 C29 118.2(5) . . ?
O7 C27 C29 117.8(5) . . ?
N3 C28 C29 124.5(6) . . ?
C28 C29 C30 119.9(5) . . ?
C28 C29 C27 116.8(5) . . ?
C30 C29 C27 123.3(5) . . ?
O9 C30 C29 125.7(5) . . ?
O9 C30 C31 118.6(5) . . ?
C29 C30 C31 115.6(5) . . ?
C32 C31 C36 119.1(5) . . ?
C32 C31 C30 120.2(5) . . ?
C36 C31 C30 120.8(5) . . ?
C33 C32 C31 120.7(6) . . ?
F3 C33 C32 121.2(6) . . ?
F3 C33 C34 117.8(5) . . ?
C32 C33 C34 121.0(6) . . ?
C35 C34 C33 119.8(6) . . ?
C35 C34 Cl3 120.4(5) . . ?
C33 C34 Cl3 119.8(5) . . ?
C34 C35 C36 119.5(6) . . ?
N3 C36 C31 119.4(5) . . ?
N3 C36 C35 120.7(5) . . ?
C31 C36 C35 119.8(5) . . ?
C38 C37 C39 61.7(5) . . ?
C38 C37 N3 119.1(6) . . ?
C39 C37 N3 119.8(7) . . ?
C37 C38 C39 59.2(5) . . ?
C37 C39 C38 59.1(5) . . ?
O10 C40 O11 123.9(6) . . ?
O10 C40 C42 117.7(6) . . ?
O11 C40 C42 118.3(6) . . ?
N4 C41 C42 124.4(6) . . ?
C41 C42 C43 118.7(5) . . ?
C41 C42 C40 118.0(6) . . ?
C43 C42 C40 123.2(5) . . ?
O12 C43 C42 125.3(5) . . ?
O12 C43 C44 118.1(5) . . ?
C42 C43 C44 116.5(5) . . ?
C49 C44 C45 119.4(6) . . ?
C49 C44 C43 121.6(6) . . ?
C45 C44 C43 119.0(5) . . ?
C46 C45 C44 119.1(6) . . ?
F4 C46 C45 119.2(6) . . ?
F4 C46 C47 119.2(6) . . ?
C45 C46 C47 121.7(6) . . ?
C48 C47 C46 120.0(6) . . ?
C48 C47 Cl4 121.4(5) . . ?
C46 C47 Cl4 118.6(5) . . ?
C47 C48 C49 119.7(6) . . ?
N4 C49 C48 121.0(5) . . ?
N4 C49 C44 119.0(5) . . ?
C48 C49 C44 120.0(6) . . ?
N4 C50 C52 118.1(6) . . ?
N4 C50 C51 118.6(6) . . ?
C52 C50 C51 59.6(5) . . ?
C52 C51 C50 60.0(5) . . ?
C51 C52 C50 60.4(5) . . ?

_refine_diff_density_max         1.890
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.132

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1855010'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 Cl4 F4 Gd N4 Na O16'
_chemical_formula_weight         1374.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1650 3.9040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0360 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0529(2)
_cell_length_b                   12.7458(3)
_cell_length_c                   22.0524(5)
_cell_angle_alpha                73.527(2)
_cell_angle_beta                 85.433(2)
_cell_angle_gamma                72.228(2)
_cell_volume                     2580.26(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24379
_cell_measurement_theta_min      3.5050
_cell_measurement_theta_max      29.0100

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1374
_exptl_absorpt_coefficient_mu    1.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7734
_exptl_absorpt_correction_T_max  0.8196
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24561
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         25.01
_reflns_number_total             8891
_reflns_number_gt                8406
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0519P)²+1.5907P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8891
_refine_ls_number_parameters     745
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.008
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.122584(15) 0.489717(12) 0.258461(7) 0.02615(7) Uani 1 1 d . . .
Cl1 Cl -0.04122(11) 0.25235(10) -0.06505(5) 0.0556(3) Uani 1 1 d . . .
Cl4 Cl 0.23678(12) 1.03988(11) 0.39683(6) 0.0648(3) Uani 1 1 d . . .
Cl3 Cl -0.41363(10) 0.81404(9) 0.54036(5) 0.0522(3) Uani 1 1 d . . .
Cl2 Cl 0.72219(10) -0.06349(10) 0.11057(6) 0.0585(3) Uani 1 1 d . . .
C3 C 0.1670(3) 0.4369(3) 0.11666(15) 0.0276(7) Uani 1 1 d . . .
O3 O 0.0834(2) 0.4691(2) 0.15809(11) 0.0345(5) Uani 1 1 d . . .
C2 C 0.3081(3) 0.4392(3) 0.10972(15) 0.0297(7) Uani 1 1 d . . .
C4 C 0.1185(3) 0.3903(3) 0.07205(15) 0.0279(7) Uani 1 1 d . . .
C10 C -0.0190(4) 0.3846(3) 0.07603(16) 0.0349(8) Uani 1 1 d . . .
H10 H -0.0788 0.4097 0.1068 0.042 Uiso 1 1 calc R . .
C11 C -0.0640(4) 0.3415(3) 0.03412(17) 0.0371(8) Uani 1 1 d . . .
C12 C 0.0229(4) 0.3048(3) -0.01295(16) 0.0345(8) Uani 1 1 d . . .
C5 C 0.2067(3) 0.3517(3) 0.02526(15) 0.0284(7) Uani 1 1 d . . .
C13 C 0.1568(4) 0.3100(3) -0.01822(16) 0.0333(8) Uani 1 1 d . . .
H13 H 0.2143 0.2864 -0.0500 0.040 Uiso 1 1 calc R . .
F1 F -0.1967(2) 0.3358(2) 0.03775(12) 0.0630(7) Uani 1 1 d . . .
N1 N 0.3439(3) 0.3555(2) 0.02282(12) 0.0320(6) Uani 1 1 d . . .
C6 C 0.3884(4) 0.3989(3) 0.06352(15) 0.0326(7) Uani 1 1 d . . .
H6 H 0.4802 0.4017 0.0600 0.039 Uiso 1 1 calc R . .
C7 C 0.4378(4) 0.3198(3) -0.02665(17) 0.0407(9) Uani 1 1 d . . .
H7 H 0.4218 0.3741 -0.0688 0.049 Uiso 1 1 calc R . .
C8 C 0.4845(4) 0.1967(4) -0.0251(2) 0.0565(12) Uani 1 1 d . . .
H8A H 0.4943 0.1777 -0.0651 0.068 Uiso 1 1 calc R . .
H8B H 0.4533 0.1437 0.0097 0.068 Uiso 1 1 calc R . .
C9 C 0.5849(4) 0.2521(4) -0.0105(2) 0.0577(12) Uani 1 1 d . . .
H9A H 0.6146 0.2325 0.0331 0.069 Uiso 1 1 calc R . .
H9B H 0.6555 0.2664 -0.0417 0.069 Uiso 1 1 calc R . .
C1 C 0.3792(4) 0.4795(3) 0.15305(16) 0.0343(8) Uani 1 1 d . . .
O1 O 0.3051(2) 0.5295(2) 0.19125(11) 0.0361(6) Uani 1 1 d . . .
O2 O 0.5079(3) 0.4598(3) 0.14864(16) 0.0658(9) Uani 1 1 d . . .
C15 C 0.1264(4) 0.2068(3) 0.23543(16) 0.0330(8) Uani 1 1 d . . .
C16 C 0.2595(3) 0.2256(3) 0.23409(15) 0.0291(7) Uani 1 1 d . . .
C17 C 0.3724(3) 0.1524(3) 0.20485(15) 0.0287(7) Uani 1 1 d . . .
C18 C 0.3483(3) 0.0719(3) 0.17842(16) 0.0303(7) Uani 1 1 d . . .
N2 N 0.2135(3) 0.0617(2) 0.17987(14) 0.0344(7) Uani 1 1 d . . .
C20 C 0.1888(4) -0.0224(3) 0.15258(19) 0.0405(9) Uani 1 1 d . . .
H20 H 0.2292 -0.1028 0.1759 0.049 Uiso 1 1 calc R . .
C14 C -0.0019(4) 0.2707(3) 0.26479(19) 0.0416(9) Uani 1 1 d . . .
O5 O -0.1071(3) 0.2386(3) 0.2669(2) 0.0834(12) Uani 1 1 d . . .
O4 O 0.0031(3) 0.3519(2) 0.28520(12) 0.0407(6) Uani 1 1 d . . .
O6 O 0.2843(2) 0.29996(19) 0.25498(11) 0.0349(5) Uani 1 1 d . . .
C44 C -0.0140(4) 0.9126(3) 0.32585(17) 0.0332(8) Uani 1 1 d . . .
C43 C 0.0823(4) 0.8274(3) 0.30305(16) 0.0315(7) Uani 1 1 d . . .
C42 C 0.0363(4) 0.7540(3) 0.27422(16) 0.0311(7) Uani 1 1 d . . .
N4 N -0.1562(3) 0.9306(2) 0.31929(14) 0.0331(6) Uani 1 1 d . . .
C45 C -0.1982(4) 0.8633(3) 0.29233(16) 0.0331(8) Uani 1 1 d . . .
H45 H -0.2939 0.8776 0.2881 0.040 Uiso 1 1 calc R . .
C41 C -0.1118(4) 0.7757(3) 0.27072(16) 0.0317(7) Uani 1 1 d . . .
C40 C -0.1784(4) 0.7041(3) 0.24642(17) 0.0349(8) Uani 1 1 d . . .
O7 O -0.0994(3) 0.6223(2) 0.22656(11) 0.0382(6) Uani 1 1 d . . .
O8 O -0.3078(3) 0.7290(2) 0.24842(16) 0.0570(8) Uani 1 1 d . . .
C49 C 0.2260(4) 0.8113(3) 0.30806(17) 0.0374(8) Uani 1 1 d . . .
H49 H 0.2908 0.7556 0.2925 0.045 Uiso 1 1 calc R . .
C50 C 0.2698(4) 0.8779(3) 0.33575(19) 0.0422(9) Uani 1 1 d . . .
F4 F 0.4068(2) 0.8662(2) 0.33842(13) 0.0620(7) Uani 1 1 d . . .
C51 C 0.1745(4) 0.9601(3) 0.36080(18) 0.0406(9) Uani 1 1 d . . .
C52 C 0.0341(4) 0.9784(3) 0.35526(18) 0.0399(9) Uani 1 1 d . . .
H52 H -0.0294 1.0345 0.3710 0.048 Uiso 1 1 calc R . .
C30 C -0.0711(3) 0.6199(3) 0.43399(14) 0.0261(7) Uani 1 1 d . . .
C29 C 0.0382(3) 0.5590(3) 0.39707(14) 0.0274(7) Uani 1 1 d . . .
C28 C 0.1785(3) 0.5487(3) 0.41191(14) 0.0286(7) Uani 1 1 d . . .
C32 C 0.2018(4) 0.5918(3) 0.45857(16) 0.0331(8) Uani 1 1 d . . .
H32 H 0.2942 0.5819 0.4679 0.040 Uiso 1 1 calc R . .
N3 N 0.1018(3) 0.6478(2) 0.49234(14) 0.0341(7) Uani 1 1 d . . .
C31 C -0.0379(3) 0.6635(3) 0.48047(15) 0.0288(7) Uani 1 1 d . . .
C27 C 0.3050(4) 0.4898(3) 0.37960(16) 0.0340(8) Uani 1 1 d . . .
O11 O 0.4207(3) 0.4848(3) 0.39703(14) 0.0558(8) Uani 1 1 d . . .
O10 O 0.2865(3) 0.4461(2) 0.33718(11) 0.0417(6) Uani 1 1 d . . .
C33 C 0.1414(4) 0.6767(4) 0.5470(2) 0.0479(10) Uani 1 1 d . . .
H33 H 0.1294 0.6263 0.5885 0.058 Uiso 1 1 calc R . .
C35 C 0.2616(4) 0.7212(4) 0.5415(2) 0.0579(12) Uani 1 1 d . . .
H35A H 0.3091 0.7326 0.5012 0.069 Uiso 1 1 calc R . .
H35B H 0.3216 0.6974 0.5783 0.069 Uiso 1 1 calc R . .
C34 C 0.1162(5) 0.7976(4) 0.5447(3) 0.0655(13) Uani 1 1 d . . .
H34A H 0.0882 0.8199 0.5835 0.079 Uiso 1 1 calc R . .
H34B H 0.0757 0.8551 0.5063 0.079 Uiso 1 1 calc R . .
O12 O 0.0031(2) 0.5220(2) 0.35589(10) 0.0322(5) Uani 1 1 d . . .
C46 C -0.2569(4) 1.0275(3) 0.33602(18) 0.0361(8) Uani 1 1 d . . .
H46 H -0.2601 1.1031 0.3079 0.043 Uiso 1 1 calc R . .
C47 C -0.2837(4) 1.0223(4) 0.4041(2) 0.0471(10) Uani 1 1 d . . .
H47A H -0.3003 1.0925 0.4164 0.056 Uiso 1 1 calc R . .
H47B H -0.2344 0.9531 0.4353 0.056 Uiso 1 1 calc R . .
C48 C -0.3923(4) 1.0150(4) 0.3642(2) 0.0484(10) Uani 1 1 d . . .
H48A H -0.4088 0.9414 0.3712 0.058 Uiso 1 1 calc R . .
H48B H -0.4746 1.0807 0.3524 0.058 Uiso 1 1 calc R . .
C19 C 0.1115(4) 0.1264(3) 0.20858(17) 0.0354(8) Uani 1 1 d . . .
H19 H 0.0237 0.1156 0.2104 0.042 Uiso 1 1 calc R . .
C23 C 0.5076(4) 0.1643(3) 0.20079(17) 0.0366(8) Uani 1 1 d . . .
H23 H 0.5263 0.2171 0.2179 0.044 Uiso 1 1 calc R . .
C24 C 0.6107(4) 0.0990(3) 0.17204(19) 0.0409(9) Uani 1 1 d . . .
C25 C 0.5868(4) 0.0169(3) 0.14703(18) 0.0398(9) Uani 1 1 d . . .
C26 C 0.4579(4) 0.0022(3) 0.15079(17) 0.0382(8) Uani 1 1 d . . .
H26 H 0.4423 -0.0536 0.1352 0.046 Uiso 1 1 calc R . .
F2 F 0.7398(2) 0.1113(2) 0.16840(14) 0.0650(7) Uani 1 1 d . . .
C36 C -0.2124(3) 0.6345(3) 0.42295(15) 0.0325(7) Uani 1 1 d . . .
H36 H -0.2363 0.6051 0.3927 0.039 Uiso 1 1 calc R . .
C39 C -0.1442(4) 0.7214(3) 0.51486(17) 0.0353(8) Uani 1 1 d . . .
H39 H -0.1219 0.7490 0.5463 0.042 Uiso 1 1 calc R . .
F3 F -0.4486(2) 0.7044(2) 0.44617(11) 0.0563(6) Uani 1 1 d . . .
C37 C -0.3135(3) 0.6912(3) 0.45629(16) 0.0343(8) Uani 1 1 d . . .
C38 C -0.2813(4) 0.7370(3) 0.50185(16) 0.0345(8) Uani 1 1 d . . .
C22 C 0.0540(4) 0.0053(5) 0.1198(3) 0.0684(15) Uani 1 1 d . . .
H22A H -0.0131 0.0796 0.1172 0.082 Uiso 1 1 calc R . .
H22B H 0.0134 -0.0564 0.1243 0.082 Uiso 1 1 calc R . .
C21 C 0.1843(4) 0.0019(4) 0.0823(2) 0.0513(10) Uani 1 1 d . . .
H21A H 0.2229 -0.0619 0.0641 0.062 Uiso 1 1 calc R . .
H21B H 0.1964 0.0742 0.0570 0.062 Uiso 1 1 calc R . .
O9 O 0.1275(2) 0.6768(2) 0.25655(13) 0.0410(6) Uani 1 1 d . . .
O1W O 0.5481(3) 0.3073(3) 0.31008(17) 0.0704(9) Uani 1 1 d . . .
H1WA H 0.5930 0.2365 0.3214 0.106 Uiso 1 1 d R A 1
H1WB H 0.4715 0.3162 0.2927 0.106 Uiso 1 1 d R A 1
O2W O 0.6291(4) 0.5274(3) 0.3158(2) 0.0847(7) Uani 1 1 d . . .
H2WA H 0.6834 0.5692 0.3079 0.127 Uiso 1 1 d R B 1
H2WB H 0.6430 0.4846 0.3535 0.127 Uiso 1 1 d R B 1
O4W O 0.4386(4) 0.7190(3) 0.18239(18) 0.0763(10) Uani 1 1 d G . .
H4WA H 0.4069 0.6647 0.2032 0.114 Uiso 1 1 d G . .
H4WB H 0.5062 0.7203 0.2027 0.114 Uiso 1 1 d G . .
O3W O 0.7480(3) 0.5318(4) 0.16677(17) 0.1051(16) Uani 1 1 d . . .
H3WA H 0.7198 0.5350 0.1308 0.158 Uiso 1 1 d R C 1
H3WB H 0.8368 0.5126 0.1672 0.158 Uiso 1 1 d R C 1
Na1 Na 0.6781(3) 0.4041(3) 0.24001(18) 0.0847(7) Uani 0.70 1 d P D 1
Na1' Na 0.7512(5) 0.3936(4) 0.2835(2) 0.0455(12) Uani 0.30 1 d P E 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O10 2.321(2) . ?
Gd1 O4 2.337(2) . ?
Gd1 O1 2.352(2) . ?
Gd1 O7 2.368(2) . ?
Gd1 O3 2.378(2) . ?
Gd1 O9 2.388(2) . ?
Gd1 O12 2.453(2) . ?
Gd1 O6 2.487(2) . ?
Cl1 C12 1.732(3) . ?
Cl4 C51 1.727(4) . ?
Cl3 C38 1.718(3) . ?
Cl2 C25 1.729(4) . ?
C3 O3 1.261(4) . ?
C3 C2 1.423(4) . ?
C3 C4 1.464(4) . ?
C2 C6 1.366(5) . ?
C2 C1 1.517(4) . ?
C4 C5 1.403(5) . ?
C4 C10 1.400(5) . ?
C10 C11 1.366(5) . ?
C10 H10 0.9300 . ?
C11 F1 1.353(4) . ?
C11 C12 1.393(5) . ?
C12 C13 1.362(5) . ?
C5 N1 1.391(4) . ?
C5 C13 1.408(4) . ?
C13 H13 0.9300 . ?
N1 C6 1.345(4) . ?
N1 C7 1.464(4) . ?
C6 H6 0.9300 . ?
C7 C9 1.480(6) . ?
C7 C8 1.486(6) . ?
C7 H7 0.9800 . ?
C8 C9 1.495(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C1 O2 1.242(4) . ?
C1 O1 1.259(4) . ?
C15 C19 1.370(5) . ?
C15 C16 1.425(5) . ?
C15 C14 1.507(5) . ?
C16 O6 1.259(4) . ?
C16 C17 1.468(5) . ?
C17 C18 1.401(5) . ?
C17 C23 1.406(5) . ?
C18 N2 1.398(4) . ?
C18 C26 1.407(5) . ?
N2 C19 1.345(4) . ?
N2 C20 1.457(4) . ?
C20 C22 1.484(6) . ?
C20 C21 1.494(6) . ?
C20 H20 0.9800 . ?
C14 O5 1.239(4) . ?
C14 O4 1.255(4) . ?
C44 N4 1.390(4) . ?
C44 C43 1.400(5) . ?
C44 C52 1.400(5) . ?
C43 C49 1.405(5) . ?
C43 C42 1.464(5) . ?
C42 O9 1.253(4) . ?
C42 C41 1.433(5) . ?
N4 C45 1.349(4) . ?
N4 C46 1.456(4) . ?
C45 C41 1.368(5) . ?
C45 H45 0.9300 . ?
C41 C40 1.509(5) . ?
C40 O8 1.242(4) . ?
C40 O7 1.268(4) . ?
C49 C50 1.360(5) . ?
C49 H49 0.9300 . ?
C50 F4 1.344(4) . ?
C50 C51 1.398(5) . ?
C51 C52 1.368(5) . ?
C52 H52 0.9300 . ?
C30 C31 1.400(4) . ?
C30 C36 1.407(5) . ?
C30 C29 1.473(4) . ?
C29 O12 1.252(4) . ?
C29 C28 1.431(4) . ?
C28 C32 1.361(5) . ?
C28 C27 1.505(5) . ?
C32 N3 1.349(4) . ?
C32 H32 0.9300 . ?
N3 C31 1.392(4) . ?
N3 C33 1.471(4) . ?
C31 C39 1.402(5) . ?
C27 O11 1.232(4) . ?
C27 O10 1.267(4) . ?
C33 C34 1.470(6) . ?
C33 C35 1.467(6) . ?
C33 H33 0.9800 . ?
C35 C34 1.497(6) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C46 C47 1.491(5) . ?
C46 C48 1.485(5) . ?
C46 H46 0.9800 . ?
C47 C48 1.496(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C19 H19 0.9300 . ?
C23 C24 1.355(5) . ?
C23 H23 0.9300 . ?
C24 F2 1.347(4) . ?
C24 C25 1.399(5) . ?
C25 C26 1.358(5) . ?
C26 H26 0.9300 . ?
C36 C37 1.353(5) . ?
C36 H36 0.9300 . ?
C39 C38 1.373(5) . ?
C39 H39 0.9300 . ?
F3 C37 1.346(4) . ?
C37 C38 1.398(5) . ?
C22 C21 1.488(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W Na1' 2.047(6) . ?
O2W H2WA 0.8499 . ?
O2W H2WB 0.8501 . ?
O4W H4WA 0.8500 . ?
O4W H4WB 0.8499 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8501 . ?

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 O4 108.31(9) . . ?
O10 Gd1 O1 83.11(9) . . ?
O4 Gd1 O1 138.04(8) . . ?
O10 Gd1 O7 137.76(8) . . ?
O4 Gd1 O7 85.13(9) . . ?
O1 Gd1 O7 113.78(9) . . ?
O10 Gd1 O3 145.26(8) . . ?
O4 Gd1 O3 77.65(8) . . ?
O1 Gd1 O3 71.96(8) . . ?
O7 Gd1 O3 75.87(8) . . ?
O10 Gd1 O9 79.03(9) . . ?
O4 Gd1 O9 148.25(8) . . ?
O1 Gd1 O9 72.54(8) . . ?
O7 Gd1 O9 70.81(8) . . ?
O3 Gd1 O9 114.39(9) . . ?
O10 Gd1 O12 70.39(8) . . ?
O4 Gd1 O12 77.73(8) . . ?
O1 Gd1 O12 141.99(7) . . ?
O7 Gd1 O12 74.02(8) . . ?
O3 Gd1 O12 142.33(8) . . ?
O9 Gd1 O12 75.95(8) . . ?
O10 Gd1 O6 75.60(8) . . ?
O4 Gd1 O6 70.06(8) . . ?
O1 Gd1 O6 74.42(8) . . ?
O7 Gd1 O6 144.75(8) . . ?
O3 Gd1 O6 74.65(8) . . ?
O9 Gd1 O6 140.23(8) . . ?
O12 Gd1 O6 121.85(8) . . ?
O3 C3 C2 125.7(3) . . ?
O3 C3 C4 118.5(3) . . ?
C2 C3 C4 115.8(3) . . ?
C3 O3 Gd1 131.5(2) . . ?
C6 C2 C3 119.6(3) . . ?
C6 C2 C1 116.7(3) . . ?
C3 C2 C1 123.7(3) . . ?
C5 C4 C10 119.4(3) . . ?
C5 C4 C3 121.3(3) . . ?
C10 C4 C3 119.3(3) . . ?
C11 C10 C4 119.1(3) . . ?
C11 C10 H10 120.5 . . ?
C4 C10 H10 120.5 . . ?
F1 C11 C10 119.3(3) . . ?
F1 C11 C12 119.1(3) . . ?
C10 C11 C12 121.6(3) . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 Cl1 120.1(3) . . ?
C11 C12 Cl1 119.2(3) . . ?
N1 C5 C4 118.7(3) . . ?
N1 C5 C13 120.9(3) . . ?
C4 C5 C13 120.4(3) . . ?
C12 C13 C5 118.9(3) . . ?
C12 C13 H13 120.6 . . ?
C5 C13 H13 120.6 . . ?
C6 N1 C5 120.0(3) . . ?
C6 N1 C7 119.5(3) . . ?
C5 N1 C7 120.4(3) . . ?
N1 C6 C2 124.5(3) . . ?
N1 C6 H6 117.8 . . ?
C2 C6 H6 117.8 . . ?
N1 C7 C9 119.5(3) . . ?
N1 C7 C8 118.7(3) . . ?
C9 C7 C8 60.6(3) . . ?
N1 C7 H7 115.7 . . ?
C9 C7 H7 115.7 . . ?
C8 C7 H7 115.7 . . ?
C7 C8 C9 59.5(3) . . ?
C7 C8 H8A 117.8 . . ?
C9 C8 H8A 117.8 . . ?
C7 C8 H8B 117.8 . . ?
C9 C8 H8B 117.8 . . ?
H8A C8 H8B 115.0 . . ?
C7 C9 C8 59.9(3) . . ?
C7 C9 H9A 117.8 . . ?
C8 C9 H9A 117.8 . . ?
C7 C9 H9B 117.8 . . ?
C8 C9 H9B 117.8 . . ?
H9A C9 H9B 114.9 . . ?
O2 C1 O1 124.3(3) . . ?
O2 C1 C2 117.2(3) . . ?
O1 C1 C2 118.4(3) . . ?
C1 O1 Gd1 132.1(2) . . ?
C19 C15 C16 119.2(3) . . ?
C19 C15 C14 116.8(3) . . ?
C16 C15 C14 124.0(3) . . ?
O6 C16 C15 124.8(3) . . ?
O6 C16 C17 119.4(3) . . ?
C15 C16 C17 115.8(3) . . ?
C18 C17 C23 118.2(3) . . ?
C18 C17 C16 121.4(3) . . ?
C23 C17 C16 120.4(3) . . ?
N2 C18 C17 119.1(3) . . ?
N2 C18 C26 120.2(3) . . ?
C17 C18 C26 120.7(3) . . ?
C19 N2 C18 119.2(3) . . ?
C19 N2 C20 121.8(3) . . ?
C18 N2 C20 119.0(3) . . ?
N2 C20 C22 119.0(3) . . ?
N2 C20 C21 119.0(3) . . ?
C22 C20 C21 59.9(3) . . ?
N2 C20 H20 115.8 . . ?
C22 C20 H20 115.8 . . ?
C21 C20 H20 115.8 . . ?
O5 C14 O4 124.2(3) . . ?
O5 C14 C15 116.6(3) . . ?
O4 C14 C15 119.2(3) . . ?
C14 O4 Gd1 136.0(2) . . ?
C16 O6 Gd1 127.7(2) . . ?
N4 C44 C43 119.6(3) . . ?
N4 C44 C52 120.7(3) . . ?
C43 C44 C52 119.7(3) . . ?
C44 C43 C49 119.6(3) . . ?
C44 C43 C42 121.3(3) . . ?
C49 C43 C42 119.1(3) . . ?
O9 C42 C41 125.8(3) . . ?
O9 C42 C43 118.3(3) . . ?
C41 C42 C43 115.8(3) . . ?
C45 N4 C44 118.9(3) . . ?
C45 N4 C46 120.9(3) . . ?
C44 N4 C46 120.0(3) . . ?
N4 C45 C41 125.4(3) . . ?
N4 C45 H45 117.3 . . ?
C41 C45 H45 117.3 . . ?
C45 C41 C42 118.9(3) . . ?
C45 C41 C40 117.7(3) . . ?
C42 C41 C40 123.4(3) . . ?
O8 C40 O7 124.7(3) . . ?
O8 C40 C41 117.0(3) . . ?
O7 C40 C41 118.3(3) . . ?
C40 O7 Gd1 133.7(2) . . ?
C50 C49 C43 119.5(3) . . ?
C50 C49 H49 120.2 . . ?
C43 C49 H49 120.2 . . ?
F4 C50 C49 119.9(3) . . ?
F4 C50 C51 118.9(3) . . ?
C49 C50 C51 121.2(3) . . ?
C52 C51 C50 120.1(3) . . ?
C52 C51 Cl4 121.0(3) . . ?
C50 C51 Cl4 119.0(3) . . ?
C51 C52 C44 119.9(3) . . ?
C51 C52 H52 120.0 . . ?
C44 C52 H52 120.0 . . ?
C31 C30 C36 118.8(3) . . ?
C31 C30 C29 121.5(3) . . ?
C36 C30 C29 119.7(3) . . ?
O12 C29 C28 125.6(3) . . ?
O12 C29 C30 119.0(3) . . ?
C28 C29 C30 115.3(3) . . ?
C32 C28 C29 119.4(3) . . ?
C32 C28 C27 116.9(3) . . ?
C29 C28 C27 123.6(3) . . ?
N3 C32 C28 125.3(3) . . ?
N3 C32 H32 117.4 . . ?
C28 C32 H32 117.4 . . ?
C32 N3 C31 119.3(3) . . ?
C32 N3 C33 119.7(3) . . ?
C31 N3 C33 120.4(3) . . ?
N3 C31 C30 119.1(3) . . ?
N3 C31 C39 120.6(3) . . ?
C30 C31 C39 120.3(3) . . ?
O11 C27 O10 123.9(3) . . ?
O11 C27 C28 117.8(3) . . ?
O10 C27 C28 118.3(3) . . ?
C27 O10 Gd1 136.8(2) . . ?
N3 C33 C34 119.4(4) . . ?
N3 C33 C35 118.9(4) . . ?
C34 C33 C35 61.3(3) . . ?
N3 C33 H33 115.5 . . ?
C34 C33 H33 115.5 . . ?
C35 C33 H33 115.5 . . ?
C33 C35 C34 59.4(3) . . ?
C33 C35 H35A 117.8 . . ?
C34 C35 H35A 117.8 . . ?
C33 C35 H35B 117.8 . . ?
C34 C35 H35B 117.8 . . ?
H35A C35 H35B 115.0 . . ?
C33 C34 C35 59.3(3) . . ?
C33 C34 H34A 117.8 . . ?
C35 C34 H34A 117.8 . . ?
C33 C34 H34B 117.8 . . ?
C35 C34 H34B 117.8 . . ?
H34A C34 H34B 115.0 . . ?
C29 O12 Gd1 129.6(2) . . ?
N4 C46 C47 119.1(3) . . ?
N4 C46 C48 119.3(3) . . ?
C47 C46 C48 60.3(3) . . ?
N4 C46 H46 115.6 . . ?
C47 C46 H46 115.6 . . ?
C48 C46 H46 115.6 . . ?
C46 C47 C48 59.6(3) . . ?
C46 C47 H47A 117.8 . . ?
C48 C47 H47A 117.8 . . ?
C46 C47 H47B 117.8 . . ?
C48 C47 H47B 117.8 . . ?
H47A C47 H47B 114.9 . . ?
C46 C48 C47 60.0(3) . . ?
C46 C48 H48A 117.8 . . ?
C47 C48 H48A 117.8 . . ?
C46 C48 H48B 117.8 . . ?
C47 C48 H48B 117.8 . . ?
H48A C48 H48B 114.9 . . ?
N2 C19 C15 125.3(3) . . ?
N2 C19 H19 117.4 . . ?
C15 C19 H19 117.4 . . ?
C24 C23 C17 120.3(3) . . ?
C24 C23 H23 119.9 . . ?
C17 C23 H23 119.9 . . ?
F2 C24 C23 119.7(3) . . ?
F2 C24 C25 119.0(3) . . ?
C23 C24 C25 121.3(3) . . ?
C26 C25 C24 120.0(3) . . ?
C26 C25 Cl2 120.7(3) . . ?
C24 C25 Cl2 119.3(3) . . ?
C25 C26 C18 119.5(3) . . ?
C25 C26 H26 120.2 . . ?
C18 C26 H26 120.2 . . ?
C37 C36 C30 120.1(3) . . ?
C37 C36 H36 120.0 . . ?
C30 C36 H36 120.0 . . ?
C38 C39 C31 119.6(3) . . ?
C38 C39 H39 120.2 . . ?
C31 C39 H39 120.2 . . ?
F3 C37 C36 120.2(3) . . ?
F3 C37 C38 118.4(3) . . ?
C36 C37 C38 121.4(3) . . ?
C39 C38 C37 119.8(3) . . ?
C39 C38 Cl3 120.5(3) . . ?
C37 C38 Cl3 119.7(3) . . ?
C20 C22 C21 60.4(3) . . ?
C20 C22 H22A 117.7 . . ?
C21 C22 H22A 117.7 . . ?
C20 C22 H22B 117.7 . . ?
C21 C22 H22B 117.7 . . ?
H22A C22 H22B 114.9 . . ?
C20 C21 C22 59.7(3) . . ?
C20 C21 H21A 117.8 . . ?
C22 C21 H21A 117.8 . . ?
C20 C21 H21B 117.8 . . ?
C22 C21 H21B 117.8 . . ?
H21A C21 H21B 114.9 . . ?
C42 O9 Gd1 129.1(2) . . ?
H1WA O1W H1WB 109.5 . . ?
Na1' O2W H2WA 99.0 . . ?
Na1' O2W H2WB 89.6 . . ?
H2WA O2W H2WB 109.5 . . ?
H4WA O4W H4WB 109.5 . . ?
H3WA O3W H3WB 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
C2 C3 O3 Gd1 -22.1(5) . . . . ?
C4 C3 O3 Gd1 156.4(2) . . . . ?
O10 Gd1 O3 C3 -14.2(4) . . . . ?
O4 Gd1 O3 C3 -118.6(3) . . . . ?
O1 Gd1 O3 C3 32.1(3) . . . . ?
O7 Gd1 O3 C3 153.4(3) . . . . ?
O9 Gd1 O3 C3 92.5(3) . . . . ?
O12 Gd1 O3 C3 -168.9(2) . . . . ?
O6 Gd1 O3 C3 -46.2(3) . . . . ?
O3 C3 C2 C6 178.4(3) . . . . ?
C4 C3 C2 C6 -0.2(5) . . . . ?
O3 C3 C2 C1 1.2(5) . . . . ?
C4 C3 C2 C1 -177.3(3) . . . . ?
O3 C3 C4 C5 -179.3(3) . . . . ?
C2 C3 C4 C5 -0.6(5) . . . . ?
O3 C3 C4 C10 1.0(5) . . . . ?
C2 C3 C4 C10 179.7(3) . . . . ?
C5 C4 C10 C11 -0.1(5) . . . . ?
C3 C4 C10 C11 179.7(3) . . . . ?
C4 C10 C11 F1 -180.0(3) . . . . ?
C4 C10 C11 C12 -0.9(6) . . . . ?
F1 C11 C12 C13 179.6(3) . . . . ?
C10 C11 C12 C13 0.5(6) . . . . ?
F1 C11 C12 Cl1 -0.4(5) . . . . ?
C10 C11 C12 Cl1 -179.4(3) . . . . ?
C10 C4 C5 N1 -178.5(3) . . . . ?
C3 C4 C5 N1 1.7(5) . . . . ?
C10 C4 C5 C13 1.5(5) . . . . ?
C3 C4 C5 C13 -178.3(3) . . . . ?
C11 C12 C13 C5 0.9(5) . . . . ?
Cl1 C12 C13 C5 -179.2(3) . . . . ?
N1 C5 C13 C12 178.1(3) . . . . ?
C4 C5 C13 C12 -1.8(5) . . . . ?
C4 C5 N1 C6 -2.1(5) . . . . ?
C13 C5 N1 C6 177.9(3) . . . . ?
C4 C5 N1 C7 -177.8(3) . . . . ?
C13 C5 N1 C7 2.2(5) . . . . ?
C5 N1 C6 C2 1.4(5) . . . . ?
C7 N1 C6 C2 177.2(3) . . . . ?
C3 C2 C6 N1 -0.2(5) . . . . ?
C1 C2 C6 N1 177.1(3) . . . . ?
C6 N1 C7 C9 44.7(5) . . . . ?
C5 N1 C7 C9 -139.5(4) . . . . ?
C6 N1 C7 C8 115.2(4) . . . . ?
C5 N1 C7 C8 -69.1(4) . . . . ?
N1 C7 C8 C9 -109.6(4) . . . . ?
N1 C7 C9 C8 108.3(4) . . . . ?
C6 C2 C1 O2 -8.8(5) . . . . ?
C3 C2 C1 O2 168.4(4) . . . . ?
C6 C2 C1 O1 171.7(3) . . . . ?
C3 C2 C1 O1 -11.0(5) . . . . ?
O2 C1 O1 Gd1 -135.3(3) . . . . ?
C2 C1 O1 Gd1 44.1(5) . . . . ?
O10 Gd1 O1 C1 110.4(3) . . . . ?
O4 Gd1 O1 C1 0.6(4) . . . . ?
O7 Gd1 O1 C1 -110.0(3) . . . . ?
O3 Gd1 O1 C1 -45.0(3) . . . . ?
O9 Gd1 O1 C1 -168.9(3) . . . . ?
O12 Gd1 O1 C1 155.7(3) . . . . ?
O6 Gd1 O1 C1 33.5(3) . . . . ?
C19 C15 C16 O6 177.1(3) . . . . ?
C14 C15 C16 O6 -2.7(5) . . . . ?
C19 C15 C16 C17 -1.8(5) . . . . ?
C14 C15 C16 C17 178.4(3) . . . . ?
O6 C16 C17 C18 -177.1(3) . . . . ?
C15 C16 C17 C18 1.9(5) . . . . ?
O6 C16 C17 C23 0.7(5) . . . . ?
C15 C16 C17 C23 179.7(3) . . . . ?
C23 C17 C18 N2 -177.7(3) . . . . ?
C16 C17 C18 N2 0.2(5) . . . . ?
C23 C17 C18 C26 2.4(5) . . . . ?
C16 C17 C18 C26 -179.8(3) . . . . ?
C17 C18 N2 C19 -2.4(5) . . . . ?
C26 C18 N2 C19 177.6(3) . . . . ?
C17 C18 N2 C20 -179.7(3) . . . . ?
C26 C18 N2 C20 0.2(5) . . . . ?
C19 N2 C20 C22 38.2(5) . . . . ?
C18 N2 C20 C22 -144.5(4) . . . . ?
C19 N2 C20 C21 107.8(4) . . . . ?
C18 N2 C20 C21 -74.9(4) . . . . ?
C19 C15 C14 O5 5.8(6) . . . . ?
C16 C15 C14 O5 -174.3(4) . . . . ?
C19 C15 C14 O4 -174.0(3) . . . . ?
C16 C15 C14 O4 5.8(6) . . . . ?
O5 C14 O4 Gd1 -148.5(4) . . . . ?
C15 C14 O4 Gd1 31.3(6) . . . . ?
O10 Gd1 O4 C14 -109.7(4) . . . . ?
O1 Gd1 O4 C14 -9.4(4) . . . . ?
O7 Gd1 O4 C14 111.3(4) . . . . ?
O3 Gd1 O4 C14 34.7(4) . . . . ?
O9 Gd1 O4 C14 151.5(3) . . . . ?
O12 Gd1 O4 C14 -174.0(4) . . . . ?
O6 Gd1 O4 C14 -43.2(4) . . . . ?
C15 C16 O6 Gd1 -31.1(5) . . . . ?
C17 C16 O6 Gd1 147.8(2) . . . . ?
O10 Gd1 O6 C16 156.4(3) . . . . ?
O4 Gd1 O6 C16 40.4(3) . . . . ?
O1 Gd1 O6 C16 -116.8(3) . . . . ?
O7 Gd1 O6 C16 -7.5(3) . . . . ?
O3 Gd1 O6 C16 -41.7(3) . . . . ?
O9 Gd1 O6 C16 -151.6(2) . . . . ?
O12 Gd1 O6 C16 101.0(3) . . . . ?
N4 C44 C43 C49 178.2(3) . . . . ?
C52 C44 C43 C49 -2.1(5) . . . . ?
N4 C44 C43 C42 -2.1(5) . . . . ?
C52 C44 C43 C42 177.6(3) . . . . ?
C44 C43 C42 O9 -177.7(3) . . . . ?
C49 C43 C42 O9 2.0(5) . . . . ?
C44 C43 C42 C41 0.4(5) . . . . ?
C49 C43 C42 C41 -179.9(3) . . . . ?
C43 C44 N4 C45 1.6(5) . . . . ?
C52 C44 N4 C45 -178.1(3) . . . . ?
C43 C44 N4 C46 -172.8(3) . . . . ?
C52 C44 N4 C46 7.5(5) . . . . ?
C44 N4 C45 C41 0.7(5) . . . . ?
C46 N4 C45 C41 175.0(3) . . . . ?
N4 C45 C41 C42 -2.4(5) . . . . ?
N4 C45 C41 C40 175.5(3) . . . . ?
O9 C42 C41 C45 179.7(3) . . . . ?
C43 C42 C41 C45 1.8(5) . . . . ?
O9 C42 C41 C40 1.9(5) . . . . ?
C43 C42 C41 C40 -176.0(3) . . . . ?
C45 C41 C40 O8 -0.8(5) . . . . ?
C42 C41 C40 O8 177.0(3) . . . . ?
C45 C41 C40 O7 -179.6(3) . . . . ?
C42 C41 C40 O7 -1.9(5) . . . . ?
O8 C40 O7 Gd1 -142.6(3) . . . . ?
C41 C40 O7 Gd1 36.1(5) . . . . ?
O10 Gd1 O7 C40 2.1(4) . . . . ?
O4 Gd1 O7 C40 114.1(3) . . . . ?
O1 Gd1 O7 C40 -104.8(3) . . . . ?
O3 Gd1 O7 C40 -167.4(3) . . . . ?
O9 Gd1 O7 C40 -44.8(3) . . . . ?
O12 Gd1 O7 C40 35.5(3) . . . . ?
O6 Gd1 O7 C40 158.6(3) . . . . ?
C44 C43 C49 C50 0.9(5) . . . . ?
C42 C43 C49 C50 -178.9(3) . . . . ?
C43 C49 C50 F4 -177.3(3) . . . . ?
C43 C49 C50 C51 1.6(6) . . . . ?
F4 C50 C51 C52 176.0(4) . . . . ?
C49 C50 C51 C52 -2.9(6) . . . . ?
F4 C50 C51 Cl4 -2.4(5) . . . . ?
C49 C50 C51 Cl4 178.7(3) . . . . ?
C50 C51 C52 C44 1.6(6) . . . . ?
Cl4 C51 C52 C44 -180.0(3) . . . . ?
N4 C44 C52 C51 -179.4(3) . . . . ?
C43 C44 C52 C51 0.9(6) . . . . ?
C31 C30 C29 O12 -179.8(3) . . . . ?
C36 C30 C29 O12 0.6(4) . . . . ?
C31 C30 C29 C28 -0.4(4) . . . . ?
C36 C30 C29 C28 -180.0(3) . . . . ?
O12 C29 C28 C32 -179.2(3) . . . . ?
C30 C29 C28 C32 1.5(4) . . . . ?
O12 C29 C28 C27 -0.6(5) . . . . ?
C30 C29 C28 C27 -179.9(3) . . . . ?
C29 C28 C32 N3 -1.8(5) . . . . ?
C27 C28 C32 N3 179.6(3) . . . . ?
C28 C32 N3 C31 0.7(5) . . . . ?
C28 C32 N3 C33 172.0(3) . . . . ?
C32 N3 C31 C30 0.5(5) . . . . ?
C33 N3 C31 C30 -170.7(3) . . . . ?
C32 N3 C31 C39 180.0(3) . . . . ?
C33 N3 C31 C39 8.8(5) . . . . ?
C36 C30 C31 N3 179.0(3) . . . . ?
C29 C30 C31 N3 -0.6(5) . . . . ?
C36 C30 C31 C39 -0.5(5) . . . . ?
C29 C30 C31 C39 179.9(3) . . . . ?
C32 C28 C27 O11 -0.4(5) . . . . ?
C29 C28 C27 O11 -179.0(3) . . . . ?
C32 C28 C27 O10 178.1(3) . . . . ?
C29 C28 C27 O10 -0.5(5) . . . . ?
O11 C27 O10 Gd1 -146.0(3) . . . . ?
C28 C27 O10 Gd1 35.6(5) . . . . ?
O4 Gd1 O10 C27 -112.2(3) . . . . ?
O1 Gd1 O10 C27 109.3(3) . . . . ?
O7 Gd1 O10 C27 -8.8(4) . . . . ?
O3 Gd1 O10 C27 153.1(3) . . . . ?
O9 Gd1 O10 C27 35.8(3) . . . . ?
O12 Gd1 O10 C27 -43.1(3) . . . . ?
O6 Gd1 O10 C27 -175.1(4) . . . . ?
C32 N3 C33 C34 114.0(4) . . . . ?
C31 N3 C33 C34 -74.8(5) . . . . ?
C32 N3 C33 C35 42.6(5) . . . . ?
C31 N3 C33 C35 -146.2(4) . . . . ?
N3 C33 C35 C34 109.7(5) . . . . ?
N3 C33 C34 C35 -108.9(4) . . . . ?
C28 C29 O12 Gd1 -27.2(5) . . . . ?
C30 C29 O12 Gd1 152.1(2) . . . . ?
O10 Gd1 O12 C29 35.9(3) . . . . ?
O4 Gd1 O12 C29 150.6(3) . . . . ?
O1 Gd1 O12 C29 -12.6(3) . . . . ?
O7 Gd1 O12 C29 -121.0(3) . . . . ?
O3 Gd1 O12 C29 -159.1(2) . . . . ?
O9 Gd1 O12 C29 -47.3(3) . . . . ?
O6 Gd1 O12 C29 93.7(3) . . . . ?
C45 N4 C46 C47 110.7(4) . . . . ?
C44 N4 C46 C47 -75.0(4) . . . . ?
C45 N4 C46 C48 40.4(5) . . . . ?
C44 N4 C46 C48 -145.3(4) . . . . ?
N4 C46 C47 C48 -109.2(4) . . . . ?
N4 C46 C48 C47 108.8(4) . . . . ?
C18 N2 C19 C15 2.6(5) . . . . ?
C20 N2 C19 C15 179.9(3) . . . . ?
C16 C15 C19 N2 -0.4(6) . . . . ?
C14 C15 C19 N2 179.5(3) . . . . ?
C18 C17 C23 C24 -0.1(5) . . . . ?
C16 C17 C23 C24 -178.0(3) . . . . ?
C17 C23 C24 F2 179.9(3) . . . . ?
C17 C23 C24 C25 -1.4(6) . . . . ?
F2 C24 C25 C26 179.3(4) . . . . ?
C23 C24 C25 C26 0.6(6) . . . . ?
F2 C24 C25 Cl2 -1.6(5) . . . . ?
C23 C24 C25 Cl2 179.7(3) . . . . ?
C24 C25 C26 C18 1.7(6) . . . . ?
Cl2 C25 C26 C18 -177.4(3) . . . . ?
N2 C18 C26 C25 176.9(3) . . . . ?
C17 C18 C26 C25 -3.2(5) . . . . ?
C31 C30 C36 C37 0.9(5) . . . . ?
C29 C30 C36 C37 -179.4(3) . . . . ?
N3 C31 C39 C38 179.3(3) . . . . ?
C30 C31 C39 C38 -1.2(5) . . . . ?
C30 C36 C37 F3 -179.4(3) . . . . ?
C30 C36 C37 C38 0.3(5) . . . . ?
C31 C39 C38 C37 2.5(5) . . . . ?
C31 C39 C38 Cl3 -176.6(3) . . . . ?
F3 C37 C38 C39 177.7(3) . . . . ?
C36 C37 C38 C39 -2.1(5) . . . . ?
F3 C37 C38 Cl3 -3.2(5) . . . . ?
C36 C37 C38 Cl3 177.0(3) . . . . ?
N2 C20 C22 C21 108.6(4) . . . . ?
N2 C20 C21 C22 -108.7(4) . . . . ?
C41 C42 O9 Gd1 -33.1(5) . . . . ?
C43 C42 O9 Gd1 144.8(2) . . . . ?
O10 Gd1 O9 C42 -109.3(3) . . . . ?
O4 Gd1 O9 C42 -2.2(4) . . . . ?
O1 Gd1 O9 C42 164.5(3) . . . . ?
O7 Gd1 O9 C42 40.7(3) . . . . ?
O3 Gd1 O9 C42 104.5(3) . . . . ?
O12 Gd1 O9 C42 -37.0(3) . . . . ?
O6 Gd1 O9 C42 -160.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.935
_refine_diff_density_rms         0.073

# start Validation Reply Form 
_vrf_PLAT415_1b                  
;
PROBLEM:  
RESPONSE: Because the disorder of H1WA and H3WA. 
;
_vrf_PLAT420_1b                  
;
PROBLEM:  
RESPONSE: Because the disorder of H1WA. 
;
_vrf_PLAT910_1b                  
;
PROBLEM:
RESPONSE: Theta min = 2.965 deg. The theta value of the missing reflections 
are less than 3.5050 deg. and therefore reflections were excluded. 
;
_vrf_PLAT973_1b                  
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature. 
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2f
_database_code_depnum_ccdc_archive 'CCDC 1855016'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_vrf_PLAT910_2f                  
;
PROBLEM:  Missing # of FCF Reflection(s) Below Theta(Min).         21 Note
RESPONSE: Unimportant number of missing reflections.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Yb K (H2 O)2 (C13 H8 Cl F N O3)4, (H2 O)'
_chemical_formula_sum            'C52 H38 Cl4 F4 K N4 O15 Yb'
_chemical_formula_weight         1388.80

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   10.0457(4)
_cell_length_b                   12.7511(5)
_cell_length_c                   21.5690(8)
_cell_angle_alpha                74.844(3)
_cell_angle_beta                 86.508(3)
_cell_angle_gamma                72.910(3)
_cell_volume                     2548.62(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9772
_cell_measurement_theta_min      3.8200
_cell_measurement_theta_max      27.4350

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_F_000             1382
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    2.217
_shelx_estimated_absorpt_T_min   0.435
_shelx_estimated_absorpt_T_max   0.556
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22974
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.344
_diffrn_reflns_theta_max         27.580
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11307
_reflns_number_gt                9679
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_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)+(0.0574P)²+8.3922P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11307
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_ref         0.1395
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_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
Yb1 Yb 0.38798(3) 0.51189(2) 0.24299(2) 0.02898(9) Uani 1 1 d . . . . .
K1 K 0.7979(3) 0.5500(3) 0.25712(16) 0.1111(10) Uani 1 1 d . . . . .
Cl1 Cl -0.21373(19) 1.04740(19) 0.39617(11) 0.0620(6) Uani 1 1 d . . . . .
Cl2 Cl 0.5511(2) 0.74291(17) 0.57724(10) 0.0565(5) Uani 1 1 d . . . . .
Cl3 Cl 0.90845(18) 0.18003(16) -0.04154(10) 0.0528(5) Uani 1 1 d . . . . .
Cl4 Cl 0.2784(2) -0.03888(18) 0.10647(12) 0.0615(5) Uani 1 1 d . . . . .
F1 F -0.2282(4) 0.8715(4) 0.3363(3) 0.0672(14) Uani 1 1 d . . . . .
F2 F 0.6998(5) 0.6732(4) 0.4679(2) 0.0655(13) Uani 1 1 d . . . . .
F3 F 0.9509(4) 0.2885(4) 0.0554(2) 0.0594(12) Uani 1 1 d . . . . .
F4 F 0.1094(4) 0.1381(4) 0.1629(3) 0.0632(13) Uani 1 1 d . . . . .
O1 O 0.6081(5) 0.7665(4) 0.2296(3) 0.0682(19) Uani 1 1 d . . . . .
O2 O 0.5030(5) 0.6451(4) 0.2161(2) 0.0392(10) Uani 1 1 d . . . . .
O3 O 0.2241(4) 0.6929(3) 0.2467(2) 0.0351(10) Uani 1 1 d . . . . .
O4 O 0.0055(5) 0.5252(5) 0.3539(3) 0.0568(14) Uani 1 1 d . . . . .
O5 O 0.2061(4) 0.4726(4) 0.3059(2) 0.0358(10) Uani 1 1 d . . . . .
O6 O 0.4242(4) 0.5352(4) 0.3429(2) 0.0339(9) Uani 1 1 d . . . . .
O7 O 0.0879(5) 0.5353(5) 0.0970(3) 0.0511(13) Uani 1 1 d . . . . .
O8 O 0.2275(4) 0.5550(4) 0.1657(2) 0.0390(10) Uani 1 1 d . . . . .
O9 O 0.5065(4) 0.4775(3) 0.14645(19) 0.0300(9) Uani 1 1 d . . . . .
O10 O 0.8176(5) 0.2745(4) 0.2701(4) 0.0681(18) Uani 1 1 d . . . . .
O11 O 0.6105(5) 0.3941(4) 0.2751(2) 0.0382(10) Uani 1 1 d . . . . .
O12 O 0.3871(4) 0.3315(4) 0.2468(2) 0.0393(11) Uani 1 1 d . . . . .
O1W O 0.8949(9) 0.4465(7) 0.1687(4) 0.109(3) Uani 1 1 d . . . . .
H11 H 0.9524 0.4764 0.1467 0.163 Uiso 1 1 d R U . . .
H12 H 0.9344 0.3777 0.1855 0.163 Uiso 1 1 d R U . . .
O2W O 0.9565(6) 0.6882(5) 0.1892(3) 0.0700(17) Uani 1 1 d . . . . .
H21 H 1.0358 0.6475 0.1827 0.105 Uiso 1 1 d R U . . .
H22 H 0.9169 0.7261 0.1538 0.105 Uiso 1 1 d R U . . .
O3W O 1.0825(6) 0.2754(5) 0.3144(3) 0.0770(19) Uani 1 1 d . . . . .
H31 H 1.1018 0.3370 0.3086 0.115 Uiso 1 1 d R U . . .
H32 H 1.0026 0.2887 0.2991 0.115 Uiso 1 1 d R U . . .
N1 N 0.2904(5) 0.9355(4) 0.3230(3) 0.0358(12) Uani 1 1 d . . . . .
N2 N 0.1674(6) 0.6390(5) 0.4828(3) 0.0358(12) Uani 1 1 d . . . . .
N3 N 0.3990(5) 0.3529(4) 0.0060(2) 0.0314(11) Uani 1 1 d . . . . .
N4 N 0.6701(5) 0.0758(4) 0.1881(3) 0.0360(12) Uani 1 1 d . . . . .
C1 C 0.5062(7) 0.7302(5) 0.2354(3) 0.0382(15) Uani 1 1 d . . . . .
C2 C 0.3919(7) 0.8724(5) 0.2932(3) 0.0355(14) Uani 1 1 d . . . . .
H2 H 0.4789 0.8848 0.2916 0.043 Uiso 1 1 calc R U . . .
C3 C 0.3783(6) 0.7922(5) 0.2653(3) 0.0332(13) Uani 1 1 d . . . . .
C4 C 0.2460(6) 0.7692(5) 0.2670(3) 0.0287(12) Uani 1 1 d . . . . .
C5 C 0.1344(6) 0.8397(5) 0.2981(3) 0.0308(13) Uani 1 1 d . . . . .
C6 C 0.0015(7) 0.8240(5) 0.3023(3) 0.0376(14) Uani 1 1 d . . . . .
H6 H -0.0160 0.7695 0.2851 0.045 Uiso 1 1 calc R U . . .
C7 C -0.1023(7) 0.8891(6) 0.3317(4) 0.0434(16) Uani 1 1 d . . . . .
C8 C -0.0792(7) 0.9712(6) 0.3577(3) 0.0403(15) Uani 1 1 d . . . . .
C9 C 0.0485(7) 0.9888(5) 0.3540(3) 0.0384(15) Uani 1 1 d . . . . .
H9 H 0.0634 1.0449 0.3706 0.046 Uiso 1 1 calc R U . . .
C10 C 0.1578(6) 0.9218(5) 0.3251(3) 0.0320(13) Uani 1 1 d . . . . .
C11 C 0.3155(7) 1.0191(6) 0.3523(4) 0.0419(16) Uani 1 1 d . . . . .
H11A H 0.2756 1.0987 0.3293 0.050 Uiso 1 1 calc R U . . .
C12 C 0.3215(8) 0.9949(7) 0.4233(4) 0.0515(19) Uani 1 1 d . . . . .
H12A H 0.2846 1.0581 0.4426 0.062 Uiso 1 1 calc R U . . .
H12B H 0.3087 0.9233 0.4482 0.062 Uiso 1 1 calc R U . . .
C13 C 0.4505(9) 0.9913(8) 0.3854(5) 0.071(3) Uani 1 1 d . . . . .
H13A H 0.5164 0.9176 0.3873 0.085 Uiso 1 1 calc R U . . .
H13B H 0.4922 1.0523 0.3817 0.085 Uiso 1 1 calc R U . . .
C14 C 0.1314(7) 0.5160(5) 0.3471(3) 0.0326(13) Uani 1 1 d . . . . .
C15 C 0.1228(7) 0.5961(5) 0.4400(3) 0.0358(14) Uani 1 1 d . . . . .
H15 H 0.0321 0.5910 0.4436 0.043 Uiso 1 1 calc R U . . .
C16 C 0.2020(6) 0.5591(5) 0.3913(3) 0.0285(12) Uani 1 1 d . . . . .
C17 C 0.3410(6) 0.5647(5) 0.3846(3) 0.0273(12) Uani 1 1 d . . . . .
C18 C 0.3896(6) 0.6114(5) 0.4317(3) 0.0298(12) Uani 1 1 d . . . . .
C19 C 0.5246(7) 0.6211(5) 0.4280(3) 0.0355(14) Uani 1 1 d . . . . .
H19 H 0.5833 0.5985 0.3959 0.043 Uiso 1 1 calc R U . . .
C20 C 0.5704(7) 0.6639(6) 0.4718(3) 0.0383(15) Uani 1 1 d . . . . .
C21 C 0.4861(7) 0.6942(5) 0.5217(3) 0.0379(15) Uani 1 1 d . . . . .
C22 C 0.3539(7) 0.6855(5) 0.5265(3) 0.0360(14) Uani 1 1 d . . . . .
H22A H 0.2979 0.7056 0.5599 0.043 Uiso 1 1 calc R U . . .
C23 C 0.3026(6) 0.6460(5) 0.4808(3) 0.0307(13) Uani 1 1 d . . . . .
C24 C 0.0735(8) 0.6744(6) 0.5328(3) 0.0446(17) Uani 1 1 d . . . . .
H24 H 0.0877 0.6206 0.5753 0.054 Uiso 1 1 calc R U . . .
C25 C -0.0720(8) 0.7425(7) 0.5152(4) 0.057(2) Uani 1 1 d . . . . .
H25A H -0.1438 0.7289 0.5457 0.069 Uiso 1 1 calc R U . . .
H25B H -0.1003 0.7621 0.4704 0.069 Uiso 1 1 calc R U . . .
C26 C 0.0282(8) 0.7964(7) 0.5324(5) 0.061(2) Uani 1 1 d . . . . .
H26A H 0.0611 0.8486 0.4981 0.073 Uiso 1 1 calc R U . . .
H26B H 0.0176 0.8154 0.5735 0.073 Uiso 1 1 calc R U . . .
C27 C 0.2058(6) 0.5196(5) 0.1188(3) 0.0318(13) Uani 1 1 d . . . . .
C28 C 0.3008(6) 0.4128(5) 0.0394(3) 0.0304(13) Uani 1 1 d . . . . .
H28 H 0.2079 0.4257 0.0290 0.037 Uiso 1 1 calc R U . . .
C29 C 0.3289(6) 0.4556(5) 0.0874(3) 0.0261(11) Uani 1 1 d . . . . .
C30 C 0.4687(6) 0.4420(4) 0.1037(3) 0.0256(11) Uani 1 1 d . . . . .
C31 C 0.5760(6) 0.3788(4) 0.0668(3) 0.0260(12) Uani 1 1 d . . . . .
C32 C 0.7171(6) 0.3630(5) 0.0781(3) 0.0322(13) Uani 1 1 d . . . . .
H32A H 0.7435 0.3930 0.1087 0.039 Uiso 1 1 calc R U . . .
C33 C 0.8148(6) 0.3037(5) 0.0444(3) 0.0359(14) Uani 1 1 d . . . . .
C34 C 0.7797(7) 0.2588(5) -0.0021(3) 0.0342(14) Uani 1 1 d . . . . .
C35 C 0.6421(6) 0.2766(5) -0.0168(3) 0.0320(13) Uani 1 1 d . . . . .
H35 H 0.6179 0.2498 -0.0494 0.038 Uiso 1 1 calc R U . . .
C36 C 0.5388(6) 0.3360(5) 0.0186(3) 0.0283(12) Uani 1 1 d . . . . .
C37 C 0.3562(7) 0.3200(6) -0.0477(4) 0.0442(17) Uani 1 1 d . . . . .
H37 H 0.3669 0.3671 -0.0905 0.053 Uiso 1 1 calc R U . . .
C38 C 0.2373(8) 0.2762(8) -0.0403(4) 0.061(2) Uani 1 1 d . . . . .
H38A H 0.1759 0.2966 -0.0773 0.073 Uiso 1 1 calc R U . . .
H38B H 0.1915 0.2684 0.0008 0.073 Uiso 1 1 calc R U . . .
C39 C 0.3809(8) 0.1994(7) -0.0432(5) 0.063(2) Uani 1 1 d . . . . .
H39A H 0.4224 0.1454 -0.0037 0.075 Uiso 1 1 calc R U . . .
H39B H 0.4068 0.1736 -0.0819 0.075 Uiso 1 1 calc R U . . .
C40 C 0.6888(7) 0.3053(5) 0.2628(3) 0.0360(14) Uani 1 1 d . . . . .
C41 C 0.7128(7) 0.1430(5) 0.2161(3) 0.0358(14) Uani 1 1 d . . . . .
H41 H 0.8080 0.1280 0.2223 0.043 Uiso 1 1 calc R U . . .
C42 C 0.6251(6) 0.2324(5) 0.2364(3) 0.0317(13) Uani 1 1 d . . . . .
C43 C 0.4786(6) 0.2528(5) 0.2303(3) 0.0308(13) Uani 1 1 d . . . . .
C44 C 0.4342(6) 0.1778(5) 0.2018(3) 0.0301(13) Uani 1 1 d . . . . .
C45 C 0.2897(7) 0.1936(5) 0.1951(3) 0.0376(15) Uani 1 1 d . . . . .
H45 H 0.2250 0.2501 0.2100 0.045 Uiso 1 1 calc R U . . .
C46 C 0.2463(7) 0.1262(5) 0.1669(3) 0.0392(15) Uani 1 1 d . . . . .
C47 C 0.3412(7) 0.0419(5) 0.1436(3) 0.0386(15) Uani 1 1 d . . . . .
C48 C 0.4809(7) 0.0242(5) 0.1501(3) 0.0385(15) Uani 1 1 d . . . . .
H48 H 0.5440 -0.0325 0.1347 0.046 Uiso 1 1 calc R U . . .
C49 C 0.5285(6) 0.0915(5) 0.1797(3) 0.0316(13) Uani 1 1 d . . . . .
C50 C 0.7684(7) -0.0230(5) 0.1715(4) 0.0397(15) Uani 1 1 d . . . . .
H50 H 0.7709 -0.0973 0.2001 0.048 Uiso 1 1 calc R U . . .
C51 C 0.9039(7) -0.0108(6) 0.1424(4) 0.0505(19) Uani 1 1 d . . . . .
H51A H 0.9208 0.0625 0.1352 0.061 Uiso 1 1 calc R U . . .
H51B H 0.9859 -0.0756 0.1541 0.061 Uiso 1 1 calc R U . . .
C52 C 0.7948(7) -0.0197(6) 0.1025(4) 0.0469(17) Uani 1 1 d . . . . .
H52A H 0.7453 0.0482 0.0709 0.056 Uiso 1 1 calc R U . . .
H52B H 0.8104 -0.0898 0.0898 0.056 Uiso 1 1 calc R U . . .


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
Yb1 O8 2.238(4) . ?
Yb1 O2 2.262(4) . ?
Yb1 O12 2.282(4) . ?
Yb1 O5 2.304(4) . ?
Yb1 O6 2.314(4) . ?
Yb1 O11 2.325(4) . ?
Yb1 O9 2.411(4) . ?
Yb1 O3 2.427(4) . ?
Yb1 K1 4.324(3) . ?
K1 O1W 2.580(9) . ?
K1 O1 2.792(6) . ?
K1 O2W 2.793(7) . ?
K1 O4 2.932(6) 1_655 ?
K1 O2 2.945(6) . ?
K1 O11 3.059(6) . ?
K1 O10 3.398(6) . ?
Cl1 C8 1.724(6) . ?
Cl2 C21 1.723(6) . ?
Cl3 C34 1.719(6) . ?
Cl4 C47 1.726(6) . ?
F1 C7 1.341(8) . ?
F2 C20 1.335(7) . ?
F3 C33 1.350(7) . ?
F4 C46 1.345(7) . ?
O1 C1 1.228(8) . ?
O2 C1 1.267(7) . ?
O3 C4 1.244(7) . ?
O4 C14 1.239(8) . ?
O4 K1 2.932(6) 1_455 ?
O5 C14 1.261(7) . ?
O6 C17 1.245(7) . ?
O7 C27 1.242(8) . ?
O8 C27 1.264(7) . ?
O9 C30 1.250(6) . ?
O10 C40 1.244(8) . ?
O11 C40 1.256(7) . ?
O12 C43 1.258(7) . ?
N1 C2 1.344(8) . ?
N1 C10 1.391(8) . ?
N1 C11 1.459(8) . ?
N2 C15 1.345(8) . ?
N2 C23 1.385(8) . ?
N2 C24 1.461(8) . ?
N3 C28 1.355(7) . ?
N3 C36 1.389(8) . ?
N3 C37 1.457(8) . ?
N4 C41 1.342(8) . ?
N4 C49 1.393(8) . ?
N4 C50 1.467(7) . ?
C1 C3 1.504(8) . ?
C2 C3 1.357(9) . ?
C3 C4 1.440(9) . ?
C4 C5 1.465(8) . ?
C5 C6 1.402(9) . ?
C5 C10 1.404(8) . ?
C6 C7 1.367(9) . ?
C7 C8 1.388(9) . ?
C8 C9 1.360(9) . ?
C9 C10 1.403(8) . ?
C11 C13 1.477(11) . ?
C11 C12 1.483(11) . ?
C12 C13 1.485(12) . ?
C14 C16 1.517(8) . ?
C15 C16 1.377(8) . ?
C16 C17 1.416(8) . ?
C17 C18 1.475(8) . ?
C18 C19 1.393(9) . ?
C18 C23 1.408(8) . ?
C19 C20 1.368(9) . ?
C20 C21 1.393(9) . ?
C21 C22 1.361(9) . ?
C22 C23 1.401(8) . ?
C24 C26 1.485(10) . ?
C24 C25 1.478(11) . ?
C25 C26 1.487(10) . ?
C27 C29 1.499(7) . ?
C28 C29 1.368(8) . ?
C29 C30 1.418(8) . ?
C30 C31 1.472(7) . ?
C31 C32 1.399(8) . ?
C31 C36 1.408(8) . ?
C32 C33 1.352(8) . ?
C33 C34 1.386(9) . ?
C34 C35 1.376(9) . ?
C35 C36 1.405(8) . ?
C37 C38 1.444(10) . ?
C37 C39 1.461(10) . ?
C38 C39 1.494(11) . ?
C40 C42 1.506(8) . ?
C41 C42 1.375(8) . ?
C42 C43 1.426(9) . ?
C43 C44 1.443(8) . ?
C44 C49 1.393(8) . ?
C44 C45 1.417(9) . ?
C45 C46 1.350(9) . ?
C46 C47 1.392(9) . ?
C47 C48 1.363(9) . ?
C48 C49 1.393(9) . ?
C50 C52 1.486(10) . ?
C50 C51 1.496(9) . ?
C51 C52 1.480(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Yb1 O2 106.85(17) . . ?
O8 Yb1 O12 82.00(17) . . ?
O2 Yb1 O12 147.61(15) . . ?
O8 Yb1 O5 80.88(16) . . ?
O2 Yb1 O5 140.00(14) . . ?
O12 Yb1 O5 71.39(15) . . ?
O8 Yb1 O6 143.55(15) . . ?
O2 Yb1 O6 78.85(16) . . ?
O12 Yb1 O6 112.81(16) . . ?
O5 Yb1 O6 73.58(15) . . ?
O8 Yb1 O11 141.14(15) . . ?
O2 Yb1 O11 81.89(16) . . ?
O12 Yb1 O11 73.05(15) . . ?
O5 Yb1 O11 117.01(16) . . ?
O6 Yb1 O11 74.82(15) . . ?
O8 Yb1 O9 71.77(14) . . ?
O2 Yb1 O9 76.90(14) . . ?
O12 Yb1 O9 76.61(15) . . ?
O5 Yb1 O9 140.26(14) . . ?
O6 Yb1 O9 142.45(14) . . ?
O11 Yb1 O9 73.73(15) . . ?
O8 Yb1 O3 72.92(14) . . ?
O2 Yb1 O3 72.14(15) . . ?
O12 Yb1 O3 139.10(15) . . ?
O5 Yb1 O3 73.09(15) . . ?
O6 Yb1 O3 75.01(15) . . ?
O11 Yb1 O3 143.27(14) . . ?
O9 Yb1 O3 122.77(14) . . ?
O8 Yb1 K1 136.87(13) . . ?
O2 Yb1 K1 39.29(13) . . ?
O12 Yb1 K1 114.33(12) . . ?
O5 Yb1 K1 141.37(12) . . ?
O6 Yb1 K1 69.18(11) . . ?
O11 Yb1 K1 42.83(12) . . ?
O9 Yb1 K1 73.88(10) . . ?
O3 Yb1 K1 106.00(11) . . ?
O1W K1 O1 122.1(3) . . ?
O1W K1 O2W 79.9(2) . . ?
O1 K1 O2W 76.79(17) . . ?
O1W K1 O4 114.3(2) . 1_655 ?
O1 K1 O4 111.4(2) . 1_655 ?
O2W K1 O4 77.77(18) . 1_655 ?
O1W K1 O2 99.9(2) . . ?
O1 K1 O2 44.92(14) . . ?
O2W K1 O2 110.98(18) . . ?
O4 K1 O2 145.75(17) 1_655 . ?
O1W K1 O11 80.43(19) . . ?
O1 K1 O11 103.05(15) . . ?
O2W K1 O11 156.39(19) . . ?
O4 K1 O11 122.63(18) 1_655 . ?
O2 K1 O11 60.05(13) . . ?
O1W K1 O10 56.3(2) . . ?
O1 K1 O10 141.30(17) . . ?
O2W K1 O10 131.94(18) . . ?
O4 K1 O10 101.24(18) 1_655 . ?
O2 K1 O10 96.45(15) . . ?
O11 K1 O10 39.49(12) . . ?
O1W K1 Yb1 92.69(19) . . ?
O1 K1 Yb1 72.32(12) . . ?
O2W K1 Yb1 137.78(16) . . ?
O4 K1 Yb1 140.50(14) 1_655 . ?
O2 K1 Yb1 29.10(9) . . ?
O11 K1 Yb1 31.11(9) . . ?
O10 K1 Yb1 69.26(10) . . ?
C1 O1 K1 93.6(4) . . ?
C1 O2 Yb1 136.3(4) . . ?
C1 O2 K1 85.8(4) . . ?
Yb1 O2 K1 111.61(18) . . ?
C4 O3 Yb1 127.5(4) . . ?
C14 O4 K1 128.6(4) . 1_455 ?
C14 O5 Yb1 134.4(4) . . ?
C17 O6 Yb1 131.4(4) . . ?
C27 O8 Yb1 139.2(4) . . ?
C30 O9 Yb1 128.9(4) . . ?
C40 O10 K1 87.7(4) . . ?
C40 O11 Yb1 135.4(4) . . ?
C40 O11 K1 103.6(4) . . ?
Yb1 O11 K1 106.07(16) . . ?
C43 O12 Yb1 130.1(4) . . ?
C2 N1 C10 119.1(5) . . ?
C2 N1 C11 121.7(5) . . ?
C10 N1 C11 119.2(5) . . ?
C15 N2 C23 120.3(5) . . ?
C15 N2 C24 119.4(5) . . ?
C23 N2 C24 120.3(5) . . ?
C28 N3 C36 119.2(5) . . ?
C28 N3 C37 119.3(5) . . ?
C36 N3 C37 121.1(5) . . ?
C41 N4 C49 120.4(5) . . ?
C41 N4 C50 121.7(5) . . ?
C49 N4 C50 117.6(5) . . ?
O1 C1 O2 123.3(6) . . ?
O1 C1 C3 117.8(6) . . ?
O2 C1 C3 118.8(6) . . ?
N1 C2 C3 125.6(6) . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 C1 116.9(6) . . ?
C4 C3 C1 123.8(5) . . ?
O3 C4 C3 124.7(5) . . ?
O3 C4 C5 120.0(5) . . ?
C3 C4 C5 115.2(5) . . ?
C6 C5 C10 118.8(5) . . ?
C6 C5 C4 119.7(5) . . ?
C10 C5 C4 121.5(5) . . ?
C7 C6 C5 119.7(6) . . ?
F1 C7 C8 119.8(6) . . ?
F1 C7 C6 118.8(6) . . ?
C8 C7 C6 121.4(6) . . ?
C9 C8 C7 120.3(6) . . ?
C9 C8 Cl1 120.9(5) . . ?
C7 C8 Cl1 118.8(5) . . ?
C8 C9 C10 119.6(6) . . ?
N1 C10 C5 119.2(5) . . ?
N1 C10 C9 120.5(5) . . ?
C5 C10 C9 120.3(6) . . ?
N1 C11 C13 118.2(6) . . ?
N1 C11 C12 119.1(6) . . ?
C13 C11 C12 60.2(6) . . ?
C13 C12 C11 59.7(5) . . ?
C12 C13 C11 60.1(5) . . ?
O4 C14 O5 124.6(6) . . ?
O4 C14 C16 118.2(5) . . ?
O5 C14 C16 117.2(5) . . ?
N2 C15 C16 124.7(6) . . ?
C15 C16 C17 119.3(5) . . ?
C15 C16 C14 116.6(5) . . ?
C17 C16 C14 124.1(5) . . ?
O6 C17 C16 126.4(5) . . ?
O6 C17 C18 117.7(5) . . ?
C16 C17 C18 115.8(5) . . ?
C19 C18 C23 119.2(5) . . ?
C19 C18 C17 119.4(5) . . ?
C23 C18 C17 121.4(5) . . ?
C20 C19 C18 119.7(6) . . ?
F2 C20 C19 119.4(6) . . ?
F2 C20 C21 119.4(6) . . ?
C19 C20 C21 121.2(6) . . ?
C22 C21 C20 120.3(6) . . ?
C22 C21 Cl2 120.4(5) . . ?
C20 C21 Cl2 119.3(5) . . ?
C21 C22 C23 119.6(6) . . ?
N2 C23 C22 121.5(5) . . ?
N2 C23 C18 118.5(5) . . ?
C22 C23 C18 120.0(6) . . ?
N2 C24 C26 118.6(6) . . ?
N2 C24 C25 119.2(6) . . ?
C26 C24 C25 60.2(5) . . ?
C24 C25 C26 60.2(5) . . ?
C24 C26 C25 59.6(5) . . ?
O7 C27 O8 123.6(5) . . ?
O7 C27 C29 118.0(5) . . ?
O8 C27 C29 118.4(5) . . ?
N3 C28 C29 124.5(5) . . ?
C28 C29 C30 120.1(5) . . ?
C28 C29 C27 116.6(5) . . ?
C30 C29 C27 123.2(5) . . ?
O9 C30 C29 125.6(5) . . ?
O9 C30 C31 118.7(5) . . ?
C29 C30 C31 115.7(5) . . ?
C32 C31 C36 119.0(5) . . ?
C32 C31 C30 120.1(5) . . ?
C36 C31 C30 120.9(5) . . ?
C33 C32 C31 119.6(6) . . ?
C32 C33 F3 119.6(6) . . ?
C32 C33 C34 122.0(6) . . ?
F3 C33 C34 118.4(5) . . ?
C33 C34 C35 120.3(5) . . ?
C33 C34 Cl3 120.0(5) . . ?
C35 C34 Cl3 119.7(5) . . ?
C34 C35 C36 118.6(6) . . ?
N3 C36 C35 120.0(5) . . ?
N3 C36 C31 119.6(5) . . ?
C35 C36 C31 120.4(5) . . ?
C38 C37 N3 118.8(6) . . ?
C38 C37 C39 61.9(5) . . ?
N3 C37 C39 118.7(7) . . ?
C37 C38 C39 59.6(5) . . ?
C37 C39 C38 58.5(5) . . ?
O10 C40 O11 123.7(6) . . ?
O10 C40 C42 117.4(5) . . ?
O11 C40 C42 118.9(6) . . ?
N4 C41 C42 124.4(6) . . ?
C41 C42 C43 118.4(6) . . ?
C41 C42 C40 118.3(6) . . ?
C43 C42 C40 123.3(5) . . ?
O12 C43 C42 125.0(6) . . ?
O12 C43 C44 118.5(5) . . ?
C42 C43 C44 116.5(5) . . ?
C49 C44 C45 118.9(6) . . ?
C49 C44 C43 122.3(5) . . ?
C45 C44 C43 118.8(5) . . ?
C46 C45 C44 119.6(6) . . ?
C45 C46 F4 119.6(6) . . ?
C45 C46 C47 121.1(6) . . ?
F4 C46 C47 119.2(6) . . ?
C48 C47 C46 120.4(6) . . ?
C48 C47 Cl4 121.0(5) . . ?
C46 C47 Cl4 118.6(5) . . ?
C47 C48 C49 119.7(6) . . ?
N4 C49 C48 121.8(5) . . ?
N4 C49 C44 117.9(5) . . ?
C48 C49 C44 120.3(6) . . ?
N4 C50 C52 118.6(6) . . ?
N4 C50 C51 118.2(5) . . ?
C52 C50 C51 59.5(5) . . ?
C52 C51 C50 59.9(5) . . ?
C50 C52 C51 60.6(5) . . ?

_refine_diff_density_max         2.014
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.129

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1855015'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;

_vrf_PLAT910_2a                  
;
PROBLEM:  Missing # of FCF Reflection(s) Below Theta(Min).         20 Note
RESPONSE: Unimportant number of missing reflections.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Eu K (H2 O)2 (C13 H8 Cl F N O3)4, (H2 O)'
_chemical_formula_sum            'C52 H38 Cl4 Eu F4 K N4 O15'
_chemical_formula_weight         1367.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.0362 0.0249 '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           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

_cell_length_a                   10.0373(6)
_cell_length_b                   12.7525(8)
_cell_length_c                   21.8207(14)
_cell_angle_alpha                74.266(6)
_cell_angle_beta                 86.381(5)
_cell_angle_gamma                72.833(6)
_cell_volume                     2568.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6742
_cell_measurement_theta_min      3.8760
_cell_measurement_theta_max      27.3490

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.528
_shelx_estimated_absorpt_T_min   0.437
_shelx_estimated_absorpt_T_max   0.803
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31580
_diffrn_reflns_av_unetI/netI     0.059
_diffrn_reflns_v_R_equivalents   0.060
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.284
_diffrn_reflns_theta_max         27.622
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             17062
_reflns_number_gt                13727
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0798P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17062
_refine_ls_number_parameters     731
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1332
_refine_ls_wR_factor_gt          0.1289
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_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
Eu1 Eu 0.38382(3) 0.51037(2) 0.24303(2) 0.02788(9) Uani 1 1 d . . . . .
K1 K 0.7977(3) 0.5576(3) 0.25706(17) 0.0767(10) Uani 1 1 d . . . . .
Cl1 Cl -0.21914(16) 1.05135(17) 0.39400(10) 0.0609(5) Uani 1 1 d . . . . .
Cl2 Cl 0.54927(19) 0.74460(16) 0.57410(9) 0.0578(5) Uani 1 1 d . . . . .
Cl3 Cl 0.90917(16) 0.18473(15) -0.04200(9) 0.0540(5) Uani 1 1 d . . . . .
Cl4 Cl 0.27268(19) -0.03391(17) 0.10338(10) 0.0626(5) Uani 1 1 d . . . . .
F1 F -0.2356(4) 0.8771(4) 0.3353(2) 0.0673(13) Uani 1 1 d . . . . .
F2 F 0.6994(4) 0.6703(4) 0.4674(2) 0.0638(12) Uani 1 1 d . . . . .
F3 F 0.9484(3) 0.2899(4) 0.05466(19) 0.0562(11) Uani 1 1 d . . . . .
F4 F 0.1055(4) 0.1372(4) 0.1628(2) 0.0620(12) Uani 1 1 d . . . . .
O1 O 0.6043(5) 0.7710(4) 0.2305(3) 0.0721(17) Uani 1 1 d . . . . .
O2 O 0.5004(5) 0.6509(3) 0.2159(2) 0.0428(11) Uani 1 1 d . . . . .
O3 O 0.2178(4) 0.6999(3) 0.2451(2) 0.0342(10) Uani 1 1 d . . . . .
O4 O -0.0011(5) 0.5300(4) 0.3572(2) 0.0571(13) Uani 1 1 d . . . . .
O5 O 0.1973(4) 0.4724(3) 0.30944(19) 0.0364(10) Uani 1 1 d . . . . .
O6 O 0.4179(4) 0.5348(3) 0.34476(19) 0.0335(10) Uani 1 1 d . . . . .
O7 O 0.0832(4) 0.5252(4) 0.0965(2) 0.0594(14) Uani 1 1 d . . . . .
O8 O 0.2199(4) 0.5480(4) 0.1639(2) 0.0423(11) Uani 1 1 d . . . . .
O9 O 0.5017(4) 0.4746(3) 0.14437(18) 0.0304(9) Uani 1 1 d . . . . .
O10 O 0.8215(5) 0.2678(4) 0.2650(3) 0.0680(17) Uani 1 1 d . . . . .
O11 O 0.6141(4) 0.3852(3) 0.2743(2) 0.0394(10) Uani 1 1 d . . . . .
O12 O 0.3876(4) 0.3198(3) 0.2514(2) 0.0417(11) Uani 1 1 d . . . . .
O1W O 0.8791(7) 0.4581(6) 0.1706(3) 0.113(3) Uani 1 1 d . . . . .
H11 H 0.9158 0.4986 0.1417 0.170 Uiso 1 1 d R U . . .
H12 H 0.9380 0.3950 0.1857 0.170 Uiso 1 1 d R U . . .
O2W O 0.9527(5) 0.6891(4) 0.1886(3) 0.0741(17) Uani 1 1 d . . . . .
H21 H 0.9798 0.6684 0.1554 0.111 Uiso 1 1 d R U . . .
H22 H 1.0222 0.6822 0.2105 0.111 Uiso 1 1 d R U . . .
O3W O 1.0769(5) 0.2755(4) 0.3169(3) 0.0733(16) Uani 1 1 d . . . . .
H31 H 1.0955 0.3376 0.3105 0.110 Uiso 1 1 d R U . . .
H32 H 1.0002 0.2874 0.2989 0.110 Uiso 1 1 d R U . . .
N1 N 0.2852(5) 0.9385(4) 0.3216(2) 0.0304(11) Uani 1 1 d . . . . .
N2 N 0.1626(5) 0.6424(4) 0.4822(2) 0.0344(12) Uani 1 1 d . . . . .
N3 N 0.3968(5) 0.3520(4) 0.0048(2) 0.0299(11) Uani 1 1 d . . . . .
N4 N 0.6684(5) 0.0740(4) 0.1854(2) 0.0330(11) Uani 1 1 d . . . . .
C1 C 0.5038(6) 0.7355(5) 0.2352(3) 0.0372(15) Uani 1 1 d . . . . .
C2 C 0.3864(6) 0.8762(5) 0.2921(3) 0.0330(13) Uani 1 1 d . . . . .
H2 H 0.4734 0.8889 0.2901 0.040 Uiso 1 1 calc R U . . .
C3 C 0.3725(6) 0.7969(5) 0.2650(3) 0.0318(14) Uani 1 1 d . . . . .
C4 C 0.2416(6) 0.7745(4) 0.2660(3) 0.0266(12) Uani 1 1 d . . . . .
C5 C 0.1294(6) 0.8440(4) 0.2970(3) 0.0269(12) Uani 1 1 d . . . . .
C6 C -0.0018(6) 0.8295(5) 0.3009(3) 0.0357(14) Uani 1 1 d . . . . .
H6 H -0.0194 0.7758 0.2834 0.043 Uiso 1 1 calc R U . . .
C7 C -0.1072(7) 0.8938(5) 0.3304(3) 0.0413(16) Uani 1 1 d . . . . .
C8 C -0.0848(6) 0.9755(5) 0.3561(3) 0.0411(16) Uani 1 1 d . . . . .
C9 C 0.0431(6) 0.9924(5) 0.3525(3) 0.0361(15) Uani 1 1 d . . . . .
H9 H 0.0583 1.0484 0.3687 0.043 Uiso 1 1 calc R U . . .
C10 C 0.1530(6) 0.9243(5) 0.3241(3) 0.0301(13) Uani 1 1 d . . . . .
C11 C 0.3112(6) 1.0215(5) 0.3506(3) 0.0391(15) Uani 1 1 d . . . . .
H11A H 0.2696 1.1017 0.3283 0.047 Uiso 1 1 calc R U . . .
C12 C 0.3194(7) 0.9944(6) 0.4223(3) 0.0516(18) Uani 1 1 d . . . . .
H12A H 0.2813 1.0566 0.4419 0.062 Uiso 1 1 calc R U . . .
H12B H 0.3085 0.9217 0.4467 0.062 Uiso 1 1 calc R U . . .
C13 C 0.4494(7) 0.9939(7) 0.3841(4) 0.069(3) Uani 1 1 d . . . . .
H13A H 0.5167 0.9208 0.3856 0.083 Uiso 1 1 calc R U . . .
H13B H 0.4895 1.0557 0.3807 0.083 Uiso 1 1 calc R U . . .
C14 C 0.1248(6) 0.5179(5) 0.3485(3) 0.0304(14) Uani 1 1 d . . . . .
C15 C 0.1184(7) 0.6002(5) 0.4402(3) 0.0339(14) Uani 1 1 d . . . . .
H15 H 0.0267 0.5972 0.4435 0.041 Uiso 1 1 calc R U . . .
C16 C 0.1963(6) 0.5610(4) 0.3928(3) 0.0269(12) Uani 1 1 d . . . . .
C17 C 0.3357(6) 0.5663(4) 0.3861(2) 0.0246(11) Uani 1 1 d . . . . .
C18 C 0.3851(6) 0.6129(5) 0.4324(3) 0.0280(13) Uani 1 1 d . . . . .
C19 C 0.5215(6) 0.6200(5) 0.4284(3) 0.0336(14) Uani 1 1 d . . . . .
H19 H 0.5800 0.5962 0.3969 0.040 Uiso 1 1 calc R U . . .
C20 C 0.5671(6) 0.6615(5) 0.4702(3) 0.0401(16) Uani 1 1 d . . . . .
C21 C 0.4844(7) 0.6946(5) 0.5196(3) 0.0380(15) Uani 1 1 d . . . . .
C22 C 0.3495(7) 0.6862(5) 0.5242(3) 0.0408(16) Uani 1 1 d . . . . .
H22A H 0.2932 0.7063 0.5572 0.049 Uiso 1 1 calc R U . . .
C23 C 0.2990(6) 0.6477(4) 0.4796(3) 0.0295(13) Uani 1 1 d . . . . .
C24 C 0.0701(7) 0.6777(6) 0.5318(3) 0.0453(17) Uani 1 1 d . . . . .
H24 H 0.0860 0.6248 0.5744 0.054 Uiso 1 1 calc R U . . .
C25 C -0.0773(7) 0.7473(6) 0.5146(4) 0.062(2) Uani 1 1 d . . . . .
H25A H -0.1483 0.7351 0.5457 0.074 Uiso 1 1 calc R U . . .
H25B H -0.1073 0.7652 0.4706 0.074 Uiso 1 1 calc R U . . .
C26 C 0.0252(7) 0.8032(6) 0.5290(4) 0.061(2) Uani 1 1 d . . . . .
H26A H 0.0162 0.8242 0.5690 0.074 Uiso 1 1 calc R U . . .
H26B H 0.0573 0.8543 0.4938 0.074 Uiso 1 1 calc R U . . .
C27 C 0.1997(6) 0.5121(5) 0.1182(3) 0.0326(13) Uani 1 1 d . . . . .
C28 C 0.2998(6) 0.4100(5) 0.0384(3) 0.0313(13) Uani 1 1 d . . . . .
H28 H 0.2069 0.4230 0.0278 0.038 Uiso 1 1 calc R U . . .
C29 C 0.3249(5) 0.4513(5) 0.0865(3) 0.0267(12) Uani 1 1 d . . . . .
C30 C 0.4640(6) 0.4392(4) 0.1025(3) 0.0256(12) Uani 1 1 d . . . . .
C31 C 0.5719(5) 0.3782(4) 0.0657(3) 0.0241(12) Uani 1 1 d . . . . .
C32 C 0.7139(6) 0.3621(5) 0.0772(3) 0.0303(13) Uani 1 1 d . . . . .
H32A H 0.7398 0.3904 0.1082 0.036 Uiso 1 1 calc R U . . .
C33 C 0.8131(6) 0.3050(5) 0.0431(3) 0.0329(14) Uani 1 1 d . . . . .
C34 C 0.7800(6) 0.2624(5) -0.0030(3) 0.0317(13) Uani 1 1 d . . . . .
C35 C 0.6431(6) 0.2797(5) -0.0183(3) 0.0333(14) Uani 1 1 d . . . . .
H35 H 0.6205 0.2549 -0.0515 0.040 Uiso 1 1 calc R U . . .
C36 C 0.5365(5) 0.3363(4) 0.0176(3) 0.0256(12) Uani 1 1 d . . . . .
C37 C 0.3557(7) 0.3214(6) -0.0495(3) 0.0437(16) Uani 1 1 d . . . . .
H37 H 0.3663 0.3707 -0.0915 0.052 Uiso 1 1 calc R U . . .
C38 C 0.2346(7) 0.2756(6) -0.0432(4) 0.055(2) Uani 1 1 d . . . . .
H38A H 0.1734 0.2975 -0.0800 0.066 Uiso 1 1 calc R U . . .
H38B H 0.1890 0.2646 -0.0024 0.066 Uiso 1 1 calc R U . . .
C39 C 0.3792(7) 0.2024(6) -0.0468(4) 0.063(2) Uani 1 1 d . . . . .
H39A H 0.4213 0.1463 -0.0081 0.076 Uiso 1 1 calc R U . . .
H39B H 0.4057 0.1792 -0.0857 0.076 Uiso 1 1 calc R U . . .
C40 C 0.6919(6) 0.2988(5) 0.2603(3) 0.0347(15) Uani 1 1 d . . . . .
C41 C 0.7135(6) 0.1401(5) 0.2133(3) 0.0322(14) Uani 1 1 d . . . . .
H41 H 0.8092 0.1260 0.2179 0.039 Uiso 1 1 calc R U . . .
C42 C 0.6255(6) 0.2275(4) 0.2354(3) 0.0311(13) Uani 1 1 d . . . . .
C43 C 0.4787(6) 0.2469(4) 0.2316(3) 0.0293(13) Uani 1 1 d . . . . .
C44 C 0.4318(6) 0.1742(4) 0.2014(3) 0.0278(13) Uani 1 1 d . . . . .
C45 C 0.2878(6) 0.1901(5) 0.1958(3) 0.0342(14) Uani 1 1 d . . . . .
H45 H 0.2236 0.2447 0.2120 0.041 Uiso 1 1 calc R U . . .
C46 C 0.2437(6) 0.1249(5) 0.1663(3) 0.0386(16) Uani 1 1 d . . . . .
C47 C 0.3361(7) 0.0446(5) 0.1417(3) 0.0390(15) Uani 1 1 d . . . . .
C48 C 0.4783(6) 0.0251(5) 0.1469(3) 0.0363(15) Uani 1 1 d . . . . .
H48 H 0.5406 -0.0300 0.1303 0.044 Uiso 1 1 calc R U . . .
C49 C 0.5262(6) 0.0904(4) 0.1777(3) 0.0302(14) Uani 1 1 d . . . . .
C50 C 0.7669(6) -0.0230(5) 0.1680(3) 0.0369(15) Uani 1 1 d . . . . .
H50 H 0.7707 -0.0980 0.1965 0.044 Uiso 1 1 calc R U . . .
C51 C 0.9023(6) -0.0102(6) 0.1392(3) 0.0470(17) Uani 1 1 d . . . . .
H51A H 0.9186 0.0635 0.1316 0.056 Uiso 1 1 calc R U . . .
H51B H 0.9847 -0.0750 0.1510 0.056 Uiso 1 1 calc R U . . .
C52 C 0.7926(6) -0.0196(6) 0.1004(4) 0.0494(18) Uani 1 1 d . . . . .
H52A H 0.7424 0.0484 0.0689 0.059 Uiso 1 1 calc R U . . .
H52B H 0.8084 -0.0900 0.0882 0.059 Uiso 1 1 calc R U . . .


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 O8 2.316(4) . ?
Eu1 O2 2.346(4) . ?
Eu1 O5 2.377(4) . ?
Eu1 O12 2.376(4) . ?
Eu1 O6 2.382(4) . ?
Eu1 O11 2.406(4) . ?
Eu1 O9 2.477(4) . ?
Eu1 O3 2.508(4) . ?
K1 O1W 2.515(8) . ?
K1 O2W 2.711(7) . ?
K1 O1 2.771(6) . ?
K1 O4 2.948(6) 1_655 ?
K1 O2 2.965(5) . ?
Cl1 C8 1.720(6) . ?
Cl2 C21 1.732(6) . ?
Cl3 C34 1.716(5) . ?
Cl4 C47 1.733(6) . ?
F1 C7 1.360(7) . ?
F2 C20 1.361(7) . ?
F3 C33 1.344(6) . ?
F4 C46 1.355(7) . ?
O1 C1 1.210(7) . ?
O2 C1 1.271(7) . ?
O3 C4 1.247(6) . ?
O4 C14 1.235(7) . ?
O4 K1 2.948(6) 1_455 ?
O5 C14 1.239(6) . ?
O6 C17 1.250(6) . ?
O7 C27 1.238(7) . ?
O8 C27 1.253(7) . ?
O9 C30 1.246(6) . ?
O10 C40 1.245(7) . ?
O11 C40 1.249(7) . ?
O12 C43 1.247(6) . ?
N1 C2 1.341(7) . ?
N1 C10 1.387(7) . ?
N1 C11 1.462(7) . ?
N2 C15 1.335(7) . ?
N2 C23 1.388(8) . ?
N2 C24 1.460(7) . ?
N3 C28 1.347(7) . ?
N3 C36 1.392(7) . ?
N3 C37 1.462(7) . ?
N4 C41 1.350(7) . ?
N4 C49 1.394(7) . ?
N4 C50 1.462(7) . ?
C1 C3 1.527(8) . ?
C2 C3 1.344(7) . ?
C3 C4 1.423(8) . ?
C4 C5 1.466(7) . ?
C5 C6 1.378(8) . ?
C5 C10 1.394(7) . ?
C6 C7 1.376(8) . ?
C7 C8 1.387(8) . ?
C8 C9 1.357(8) . ?
C9 C10 1.413(8) . ?
C11 C13 1.511(9) . ?
C11 C12 1.509(9) . ?
C12 C13 1.503(10) . ?
C14 C16 1.535(8) . ?
C15 C16 1.371(7) . ?
C16 C17 1.418(8) . ?
C17 C18 1.477(7) . ?
C18 C23 1.384(7) . ?
C18 C19 1.395(8) . ?
C19 C20 1.335(8) . ?
C20 C21 1.397(9) . ?
C21 C22 1.385(9) . ?
C22 C23 1.383(8) . ?
C24 C25 1.494(9) . ?
C24 C26 1.515(9) . ?
C25 C26 1.505(9) . ?
C27 C29 1.505(7) . ?
C28 C29 1.361(8) . ?
C29 C30 1.414(7) . ?
C30 C31 1.468(7) . ?
C31 C36 1.405(7) . ?
C31 C32 1.408(8) . ?
C32 C33 1.359(8) . ?
C33 C34 1.366(8) . ?
C34 C35 1.373(8) . ?
C35 C36 1.423(7) . ?
C37 C39 1.450(9) . ?
C37 C38 1.480(9) . ?
C38 C39 1.486(9) . ?
C40 C42 1.497(8) . ?
C41 C42 1.382(7) . ?
C42 C43 1.424(8) . ?
C43 C44 1.463(8) . ?
C44 C49 1.396(7) . ?
C44 C45 1.408(8) . ?
C45 C46 1.357(8) . ?
C46 C47 1.368(8) . ?
C47 C48 1.381(8) . ?
C48 C49 1.400(8) . ?
C50 C52 1.473(9) . ?
C50 C51 1.496(8) . ?
C51 C52 1.481(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Eu1 O2 108.58(16) . . ?
O8 Eu1 O5 81.80(14) . . ?
O2 Eu1 O5 137.53(13) . . ?
O8 Eu1 O12 81.83(15) . . ?
O2 Eu1 O12 148.36(14) . . ?
O5 Eu1 O12 72.37(13) . . ?
O8 Eu1 O6 144.21(13) . . ?
O2 Eu1 O6 78.51(14) . . ?
O5 Eu1 O6 71.43(13) . . ?
O12 Eu1 O6 110.89(15) . . ?
O8 Eu1 O11 137.86(13) . . ?
O2 Eu1 O11 83.25(14) . . ?
O5 Eu1 O11 117.04(14) . . ?
O12 Eu1 O11 70.42(14) . . ?
O6 Eu1 O11 76.93(13) . . ?
O8 Eu1 O9 69.91(13) . . ?
O2 Eu1 O9 78.77(13) . . ?
O5 Eu1 O9 140.82(12) . . ?
O12 Eu1 O9 77.12(14) . . ?
O6 Eu1 O9 144.28(12) . . ?
O11 Eu1 O9 73.33(13) . . ?
O8 Eu1 O3 75.42(13) . . ?
O2 Eu1 O3 70.06(13) . . ?
O5 Eu1 O3 73.40(13) . . ?
O12 Eu1 O3 141.05(12) . . ?
O6 Eu1 O3 74.47(13) . . ?
O11 Eu1 O3 144.00(13) . . ?
O9 Eu1 O3 121.98(13) . . ?
O1W K1 O2W 80.05(19) . . ?
O1W K1 O1 120.6(2) . . ?
O2W K1 O1 78.81(17) . . ?
O1W K1 O4 118.7(2) . 1_655 ?
O2W K1 O4 80.75(16) . 1_655 ?
O1 K1 O4 111.53(18) . 1_655 ?
O1W K1 O2 96.5(2) . . ?
O2W K1 O2 111.42(18) . . ?
O1 K1 O2 44.69(13) . . ?
O4 K1 O2 144.59(16) 1_655 . ?
C1 O1 K1 94.9(4) . . ?
C1 O2 Eu1 136.9(4) . . ?
C1 O2 K1 84.8(4) . . ?
Eu1 O2 K1 111.76(17) . . ?
C4 O3 Eu1 127.2(3) . . ?
C14 O4 K1 124.2(4) . 1_455 ?
C14 O5 Eu1 134.1(3) . . ?
C17 O6 Eu1 133.0(4) . . ?
C27 O8 Eu1 140.4(4) . . ?
C30 O9 Eu1 129.9(3) . . ?
C40 O11 Eu1 135.7(4) . . ?
C43 O12 Eu1 127.4(4) . . ?
C2 N1 C10 119.1(5) . . ?
C2 N1 C11 121.3(5) . . ?
C10 N1 C11 119.6(5) . . ?
C15 N2 C23 119.3(5) . . ?
C15 N2 C24 120.2(5) . . ?
C23 N2 C24 120.5(5) . . ?
C28 N3 C36 118.1(5) . . ?
C28 N3 C37 120.4(5) . . ?
C36 N3 C37 120.9(5) . . ?
C41 N4 C49 120.8(5) . . ?
C41 N4 C50 120.7(5) . . ?
C49 N4 C50 118.2(5) . . ?
O1 C1 O2 123.7(6) . . ?
O1 C1 C3 118.3(5) . . ?
O2 C1 C3 117.9(5) . . ?
N1 C2 C3 125.3(6) . . ?
C2 C3 C4 119.9(5) . . ?
C2 C3 C1 115.7(5) . . ?
C4 C3 C1 124.4(5) . . ?
O3 C4 C3 125.6(5) . . ?
O3 C4 C5 119.2(5) . . ?
C3 C4 C5 115.2(5) . . ?
C6 C5 C10 118.6(5) . . ?
C6 C5 C4 120.2(5) . . ?
C10 C5 C4 121.2(5) . . ?
C7 C6 C5 120.4(6) . . ?
F1 C7 C6 120.1(5) . . ?
F1 C7 C8 118.7(6) . . ?
C6 C7 C8 121.1(6) . . ?
C9 C8 C7 119.7(6) . . ?
C9 C8 Cl1 121.1(5) . . ?
C7 C8 Cl1 119.2(5) . . ?
C8 C9 C10 119.6(6) . . ?
N1 C10 C5 119.3(5) . . ?
N1 C10 C9 120.2(5) . . ?
C5 C10 C9 120.5(6) . . ?
N1 C11 C13 119.1(5) . . ?
N1 C11 C12 118.8(5) . . ?
C13 C11 C12 59.7(5) . . ?
C13 C12 C11 60.2(5) . . ?
C12 C13 C11 60.1(4) . . ?
O4 C14 O5 126.4(6) . . ?
O4 C14 C16 115.4(5) . . ?
O5 C14 C16 118.2(5) . . ?
N2 C15 C16 125.8(6) . . ?
C15 C16 C17 118.4(5) . . ?
C15 C16 C14 117.6(5) . . ?
C17 C16 C14 123.9(5) . . ?
O6 C17 C16 125.3(5) . . ?
O6 C17 C18 118.7(5) . . ?
C16 C17 C18 116.0(5) . . ?
C23 C18 C19 120.0(6) . . ?
C23 C18 C17 121.1(5) . . ?
C19 C18 C17 118.8(5) . . ?
C20 C19 C18 119.2(6) . . ?
C19 C20 F2 120.7(6) . . ?
C19 C20 C21 122.3(6) . . ?
F2 C20 C21 117.0(6) . . ?
C22 C21 C20 118.7(6) . . ?
C22 C21 Cl2 120.6(5) . . ?
C20 C21 Cl2 120.8(5) . . ?
C23 C22 C21 119.6(6) . . ?
C22 C23 C18 120.1(6) . . ?
C22 C23 N2 120.5(5) . . ?
C18 C23 N2 119.4(5) . . ?
N2 C24 C25 119.1(6) . . ?
N2 C24 C26 117.2(6) . . ?
C25 C24 C26 60.0(4) . . ?
C24 C25 C26 60.7(4) . . ?
C25 C26 C24 59.3(4) . . ?
O7 C27 O8 124.2(5) . . ?
O7 C27 C29 117.5(5) . . ?
O8 C27 C29 118.3(5) . . ?
N3 C28 C29 126.1(5) . . ?
C28 C29 C30 119.5(5) . . ?
C28 C29 C27 116.9(5) . . ?
C30 C29 C27 123.6(5) . . ?
O9 C30 C29 126.2(5) . . ?
O9 C30 C31 118.3(5) . . ?
C29 C30 C31 115.5(5) . . ?
C36 C31 C32 118.4(5) . . ?
C36 C31 C30 121.2(5) . . ?
C32 C31 C30 120.4(5) . . ?
C33 C32 C31 120.0(5) . . ?
F3 C33 C32 119.5(5) . . ?
F3 C33 C34 118.5(5) . . ?
C32 C33 C34 122.1(5) . . ?
C33 C34 C35 120.5(5) . . ?
C33 C34 Cl3 120.3(4) . . ?
C35 C34 Cl3 119.1(5) . . ?
C34 C35 C36 118.9(5) . . ?
N3 C36 C31 119.6(5) . . ?
N3 C36 C35 120.4(5) . . ?
C31 C36 C35 120.0(5) . . ?
C39 C37 N3 119.4(6) . . ?
C39 C37 C38 60.9(4) . . ?
N3 C37 C38 118.6(6) . . ?
C37 C38 C39 58.5(4) . . ?
C37 C39 C38 60.5(5) . . ?
O10 C40 O11 124.8(6) . . ?
O10 C40 C42 117.1(5) . . ?
O11 C40 C42 118.0(5) . . ?
N4 C41 C42 123.7(5) . . ?
C41 C42 C43 119.0(5) . . ?
C41 C42 C40 117.1(5) . . ?
C43 C42 C40 123.8(5) . . ?
O12 C43 C42 126.0(5) . . ?
O12 C43 C44 117.5(5) . . ?
C42 C43 C44 116.5(5) . . ?
C49 C44 C45 119.3(5) . . ?
C49 C44 C43 121.6(5) . . ?
C45 C44 C43 119.1(5) . . ?
C46 C45 C44 119.2(5) . . ?
F4 C46 C45 119.3(6) . . ?
F4 C46 C47 119.2(6) . . ?
C45 C46 C47 121.5(6) . . ?
C46 C47 C48 121.3(6) . . ?
C46 C47 Cl4 119.1(5) . . ?
C48 C47 Cl4 119.6(5) . . ?
C47 C48 C49 118.2(5) . . ?
C44 C49 N4 118.4(5) . . ?
C44 C49 C48 120.4(5) . . ?
N4 C49 C48 121.2(5) . . ?
N4 C50 C52 119.8(5) . . ?
N4 C50 C51 118.8(5) . . ?
C52 C50 C51 59.8(4) . . ?
C52 C51 C50 59.3(4) . . ?
C50 C52 C51 60.8(4) . . ?

_refine_diff_density_max         2.501
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.127

_shelxl_version_number           2014/6

