# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

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# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_dytfsa

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H28 Dy N6 O8, 3(C2 F6 N O4 S2)'
_chemical_formula_sum            'C24 H28 Dy F18 N9 O20 S6'
_chemical_formula_weight         1459.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 '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 0.0082 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0142 0.0079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0225 0.0133 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1500 0.1576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1899 5.4020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   19.517(7)
_cell_length_b                   27.899(9)
_cell_length_c                   9.294(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.593(9)
_cell_angle_gamma                90.00
_cell_volume                     4974(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1750
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      29.87

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2876
_exptl_absorpt_coefficient_mu    2.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4365
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'

_exptl_special_details           
; 
Data were measured on the SCD beamline at the ANKA synchrotron, Karlsruhe.
During the course of the measurement, the crystal underwent a rather rapid
loss of crystallinity, that may have been a form of melting in the beam 
(in spite of the crystal being cooled to 150 K), and this resulted in the
low completeness of the dataset. It was not possible to measure a second
crystal. 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.80000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6594
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         30.05
_reflns_number_total             5790
_reflns_number_gt                4168
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker AXS Inc., 2005)'
_computing_cell_refinement       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'Apex2 (Bruker AXS Inc., 2005)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 Of the three (TFSI)- anions, one is fully-ordered, one has one of the
 trifluoromethyl groups two-fold disordered, but the third is extensively
 disordered, with only the two S atoms (approximately) ordered. It was
 necessary to apply extensive similarity restraints to both the geometry 
 and to the temperature factors of the disordered atoms to obtain a
 satisfactory refinement.
 No attempt was made to locate the H-atoms of the aquo ligands, O7 and O8.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1818P)^2^+33.0857P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5790
_refine_ls_number_parameters     687
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0849
_refine_ls_wR_factor_ref         0.2680
_refine_ls_wR_factor_gt          0.2238
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.024
_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
Dy1 Dy 0.32816(4) 0.256144(19) 0.48037(11) 0.0471(4) Uani 1 1 d . . .
O1 O 0.2157(7) 0.2678(3) 0.5312(18) 0.058(4) Uani 1 1 d . . .
O2 O 0.2591(5) 0.2709(3) 0.7654(15) 0.052(3) Uani 1 1 d . . .
C1 C 0.2090(7) 0.2665(4) 0.661(3) 0.045(6) Uani 1 1 d . . .
C2 C 0.1384(9) 0.2627(5) 0.704(2) 0.052(5) Uani 1 1 d . . .
H2A H 0.1413 0.2387 0.7831 0.063 Uiso 1 1 calc R . .
H2B H 0.1272 0.2939 0.7440 0.063 Uiso 1 1 calc R . .
N1 N 0.0802(7) 0.2492(3) 0.5856(18) 0.043(4) Uani 1 1 d . . .
C3 C 0.0327(8) 0.2786(5) 0.515(2) 0.051(5) Uani 1 1 d . . .
H3A H 0.0287 0.3117 0.5357 0.061 Uiso 1 1 calc R . .
N2 N -0.0085(7) 0.2548(4) 0.4097(19) 0.051(4) Uani 1 1 d . . .
C4 C 0.0151(9) 0.2072(5) 0.413(2) 0.061(6) Uani 1 1 d . . .
H4A H -0.0055 0.1817 0.3523 0.073 Uiso 1 1 calc R . .
C5 C 0.0731(9) 0.2044(5) 0.520(2) 0.056(5) Uani 1 1 d . . .
H5A H 0.1025 0.1773 0.5444 0.067 Uiso 1 1 calc R . .
C6 C -0.0666(9) 0.2756(6) 0.307(2) 0.068(6) Uani 1 1 d . . .
H6A H -0.0713 0.3095 0.3308 0.102 Uiso 1 1 calc R . .
H6B H -0.1097 0.2586 0.3152 0.102 Uiso 1 1 calc R . .
H6C H -0.0577 0.2726 0.2073 0.102 Uiso 1 1 calc R . .
O3 O 0.4418(5) 0.2745(3) 0.4369(17) 0.053(4) Uani 1 1 d . . .
O4 O 0.3921(6) 0.2649(3) 0.2111(15) 0.048(3) Uani 1 1 d . . .
C7 C 0.4470(8) 0.2686(4) 0.308(2) 0.039(5) Uani 1 1 d . . .
C8 C 0.5164(8) 0.2658(4) 0.2596(19) 0.042(5) Uani 1 1 d . . .
H8A H 0.5206 0.2342 0.2133 0.051 Uiso 1 1 calc R . .
H8B H 0.5185 0.2909 0.1851 0.051 Uiso 1 1 calc R . .
N3 N 0.5745(6) 0.2721(3) 0.3801(16) 0.043(4) Uani 1 1 d . . .
C9 C 0.6164(8) 0.2368(4) 0.449(2) 0.051(5) Uani 1 1 d . . .
H9A H 0.6148 0.2040 0.4221 0.061 Uiso 1 1 calc R . .
N4 N 0.6590(7) 0.2558(4) 0.559(2) 0.053(5) Uani 1 1 d . . .
C10 C 0.6449(8) 0.3048(5) 0.564(2) 0.060(6) Uani 1 1 d . . .
H10A H 0.6681 0.3271 0.6338 0.072 Uiso 1 1 calc R . .
C11 C 0.5934(8) 0.3145(4) 0.455(2) 0.046(5) Uani 1 1 d . . .
H11A H 0.5729 0.3450 0.4318 0.055 Uiso 1 1 calc R . .
C12 C 0.7150(9) 0.2297(5) 0.659(3) 0.065(6) Uani 1 1 d . . .
H12A H 0.7138 0.1957 0.6328 0.098 Uiso 1 1 calc R . .
H12B H 0.7076 0.2331 0.7604 0.098 Uiso 1 1 calc R . .
H12C H 0.7605 0.2433 0.6512 0.098 Uiso 1 1 calc R . .
O5 O 0.3751(5) 0.1780(3) 0.4205(14) 0.054(3) Uani 1 1 d . . .
O6 O 0.2920(5) 0.1730(3) 0.5536(14) 0.052(3) Uani 1 1 d . . .
C13 C 0.3350(7) 0.1541(5) 0.486(2) 0.057(6) Uani 1 1 d . . .
C14 C 0.3389(8) 0.0994(4) 0.472(2) 0.046(5) Uani 1 1 d . . .
H14A H 0.3103 0.0893 0.3778 0.055 Uiso 1 1 calc R . .
H14B H 0.3878 0.0900 0.4715 0.055 Uiso 1 1 calc R . .
N5 N 0.3142(8) 0.0739(3) 0.593(2) 0.059(5) Uani 1 1 d . . .
C15 C 0.3470(9) 0.0712(4) 0.730(3) 0.062(6) Uani 1 1 d . . .
H15A H 0.3898 0.0863 0.7705 0.074 Uiso 1 1 calc R . .
N6 N 0.3096(8) 0.0439(4) 0.800(2) 0.062(5) Uani 1 1 d . . .
C16 C 0.2519(11) 0.0289(6) 0.705(3) 0.083(8) Uani 1 1 d . . .
H16A H 0.2164 0.0088 0.7288 0.100 Uiso 1 1 calc R . .
C17 C 0.2531(10) 0.0468(6) 0.571(4) 0.103(11) Uani 1 1 d . . .
H17A H 0.2202 0.0422 0.4831 0.124 Uiso 1 1 calc R . .
C18 C 0.3255(11) 0.0346(6) 0.958(3) 0.090(9) Uani 1 1 d . . .
H18A H 0.3709 0.0486 0.9997 0.134 Uiso 1 1 calc R . .
H18B H 0.3268 0.0000 0.9756 0.134 Uiso 1 1 calc R . .
H18C H 0.2894 0.0491 1.0049 0.134 Uiso 1 1 calc R . .
O7 O 0.3516(6) 0.3285(3) 0.6239(16) 0.069(4) Uani 1 1 d . . .
O8 O 0.2942(6) 0.3269(3) 0.3373(18) 0.083(5) Uani 1 1 d . . .
S1 S 0.5493(2) 0.39827(11) 1.0933(6) 0.0543(14) Uani 1 1 d D . .
S2 S 0.5121(2) 0.39736(11) 0.7866(6) 0.0562(14) Uani 1 1 d D . .
N11 N 0.5104(7) 0.4184(4) 0.9469(19) 0.060(5) Uani 1 1 d . . .
O12 O 0.5019(8) 0.3970(4) 1.1940(19) 0.078(5) Uani 1 1 d . . .
O13 O 0.5925(6) 0.3574(3) 1.0939(16) 0.069(4) Uani 1 1 d . . .
O14 O 0.4465(6) 0.4070(3) 0.6921(17) 0.071(4) Uani 1 1 d . . .
O15 O 0.5412(7) 0.3506(3) 0.7802(17) 0.076(4) Uani 1 1 d . . .
C19 C 0.6079(10) 0.4474(6) 1.158(4) 0.081(8) Uani 1 1 d D . .
F1 F 0.6411(8) 0.4372(4) 1.297(2) 0.107(5) Uani 1 1 d . . .
F2 F 0.5765(8) 0.4880(4) 1.165(2) 0.142(7) Uani 1 1 d . . .
F3 F 0.6547(9) 0.4533(5) 1.081(2) 0.143(7) Uani 1 1 d . . .
C20 C 0.5704(12) 0.4368(6) 0.712(3) 0.068(7) Uani 1 1 d D . .
F4 F 0.6358(9) 0.4313(5) 0.781(2) 0.130(7) Uani 1 1 d . . .
F5 F 0.5553(7) 0.4822(3) 0.7207(17) 0.105(5) Uani 1 1 d . . .
F6 F 0.5711(9) 0.4269(4) 0.576(2) 0.125(7) Uani 1 1 d . . .
S3 S 0.1429(3) 0.41050(13) 0.6924(7) 0.0752(18) Uani 1 1 d . A .
S4 S 0.1229(3) 0.38198(12) 0.3981(7) 0.0689(17) Uani 1 1 d . . .
N16 N 0.1045(8) 0.3821(4) 0.560(2) 0.067(5) Uani 1 1 d . . .
O17 O 0.1980(8) 0.4415(5) 0.675(2) 0.107(6) Uani 1 1 d . . .
O18 O 0.1572(10) 0.3798(5) 0.820(2) 0.124(7) Uani 1 1 d . . .
O19 O 0.1948(7) 0.3932(4) 0.391(2) 0.088(6) Uani 1 1 d . . .
O20 O 0.0927(7) 0.3400(4) 0.3266(18) 0.078(5) Uani 1 1 d . . .
C21 C 0.0716(11) 0.4500(6) 0.7332(16) 0.110(11) Uani 1 1 d D . .
F7A F 0.0913(14) 0.4721(9) 0.864(2) 0.085(8) Uiso 0.50 1 d PD A 1
F8A F 0.0675(13) 0.4844(8) 0.625(2) 0.093(7) Uiso 0.50 1 d PD A 1
F9A F 0.0078(13) 0.4310(11) 0.726(3) 0.145(13) Uiso 0.50 1 d PD A 1
F7B F 0.1025(14) 0.4822(8) 0.830(2) 0.090(9) Uiso 0.50 1 d PD A 2
F8B F 0.0332(11) 0.4703(7) 0.616(2) 0.078(6) Uiso 0.50 1 d PD A 2
F9B F 0.0318(13) 0.4192(8) 0.797(3) 0.098(8) Uiso 0.50 1 d PD A 2
C22 C 0.0705(13) 0.4304(6) 0.293(4) 0.091(10) Uani 1 1 d . . .
F10 F 0.0956(7) 0.4726(3) 0.3476(18) 0.107(5) Uani 1 1 d . . .
F11 F 0.0057(7) 0.4270(4) 0.3070(19) 0.108(5) Uani 1 1 d . . .
F12 F 0.0762(9) 0.4268(4) 0.156(2) 0.121(6) Uani 1 1 d . . .
S5 S 0.1529(3) 0.65084(13) 0.3939(7) 0.0728(17) Uani 1 1 d D . .
S6 S 0.1849(3) 0.65615(14) 0.1093(7) 0.0749(17) Uani 1 1 d D . .
N21A N 0.1373(11) 0.6423(9) 0.2217(14) 0.079(9) Uiso 0.50 1 d PD B 1
O22A O 0.1972(12) 0.6910(7) 0.427(3) 0.071(7) Uiso 0.50 1 d PD B 1
O23A O 0.0843(9) 0.6523(8) 0.438(3) 0.071(7) Uiso 0.50 1 d PD B 1
O24A O 0.1475(13) 0.6915(7) 0.008(3) 0.070(7) Uiso 0.50 1 d PD B 1
O25A O 0.2558(8) 0.6593(10) 0.172(4) 0.092(9) Uiso 0.50 1 d PD B 1
N21B N 0.1965(12) 0.6388(10) 0.2742(16) 0.099(11) Uiso 0.50 1 d PD B 2
O22B O 0.1970(12) 0.6793(8) 0.508(2) 0.071(7) Uiso 0.50 1 d PD B 2
O23B O 0.0827(9) 0.6624(11) 0.334(4) 0.106(10) Uiso 0.50 1 d PD B 2
O24B O 0.1427(12) 0.6972(7) 0.088(3) 0.076(8) Uiso 0.50 1 d PD B 2
O25B O 0.2549(10) 0.6603(9) 0.074(3) 0.082(8) Uiso 0.50 1 d PD B 2
C23A C 0.1916(11) 0.5956(7) 0.466(3) 0.115(18) Uiso 0.50 1 d PD B 1
F13A F 0.1564(14) 0.5562(8) 0.427(4) 0.099(9) Uiso 0.50 1 d PD B 1
F14A F 0.2516(10) 0.5918(7) 0.424(3) 0.084(6) Uiso 0.50 1 d PD B 1
F15A F 0.2013(15) 0.5995(10) 0.607(3) 0.122(10) Uiso 0.50 1 d PD B 1
C23B C 0.1574(13) 0.5919(11) 0.480(3) 0.090(13) Uiso 0.50 1 d PD B 2
F13B F 0.1278(14) 0.5618(8) 0.379(3) 0.094(8) Uiso 0.50 1 d PD B 2
F14B F 0.2194(13) 0.5762(12) 0.535(4) 0.142(12) Uiso 0.50 1 d PD B 2
F15B F 0.1205(15) 0.5927(11) 0.585(3) 0.135(11) Uiso 0.50 1 d PD B 2
C24A C 0.1738(14) 0.6045(8) -0.010(3) 0.110(19) Uiso 0.50 1 d PD B 1
F16A F 0.2046(14) 0.5688(8) 0.065(3) 0.088(8) Uiso 0.50 1 d PD B 1
F17A F 0.1094(13) 0.5927(11) -0.057(4) 0.131(11) Uiso 0.50 1 d PD B 1
F18A F 0.2027(17) 0.6093(11) -0.125(4) 0.144(12) Uiso 0.50 1 d PD B 1
C24B C 0.1483(13) 0.6037(7) 0.015(3) 0.061(8) Uiso 0.50 1 d PD B 2
F16B F 0.1764(15) 0.5621(9) 0.037(4) 0.106(11) Uiso 0.50 1 d PD B 2
F17B F 0.0865(15) 0.6006(10) 0.047(4) 0.138(11) Uiso 0.50 1 d PD B 2
F18B F 0.1416(17) 0.6142(10) -0.122(3) 0.126(10) Uiso 0.50 1 d PD B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.0426(5) 0.0420(3) 0.0598(9) 0.0018(3) 0.0175(4) -0.0006(2)
O1 0.079(9) 0.055(5) 0.051(13) 0.000(5) 0.040(8) -0.005(5)
O2 0.032(6) 0.065(5) 0.058(11) 0.022(5) 0.007(7) -0.005(4)
C1 0.016(8) 0.036(6) 0.089(19) 0.009(6) 0.022(11) 0.004(4)
C2 0.067(11) 0.046(7) 0.043(16) 0.008(6) 0.006(10) -0.002(6)
N1 0.045(8) 0.049(6) 0.040(13) -0.004(5) 0.024(8) -0.004(4)
C3 0.044(10) 0.054(7) 0.054(16) 0.005(7) 0.007(10) 0.001(6)
N2 0.049(9) 0.057(6) 0.046(14) 0.005(6) 0.008(8) 0.000(5)
C4 0.066(12) 0.050(7) 0.076(19) -0.008(7) 0.039(12) -0.011(6)
C5 0.051(10) 0.054(7) 0.065(18) -0.004(7) 0.015(11) -0.005(6)
C6 0.056(11) 0.086(11) 0.053(18) 0.006(9) -0.014(11) 0.006(8)
O3 0.042(7) 0.050(5) 0.076(13) -0.006(5) 0.035(7) -0.006(4)
O4 0.039(7) 0.065(5) 0.043(11) -0.019(5) 0.014(7) 0.001(4)
C7 0.034(9) 0.038(6) 0.054(17) -0.007(6) 0.033(10) -0.003(4)
C8 0.054(10) 0.043(6) 0.030(14) -0.008(5) 0.007(9) 0.001(5)
N3 0.047(8) 0.037(5) 0.049(12) -0.004(5) 0.024(8) -0.005(4)
C9 0.031(8) 0.038(6) 0.088(18) -0.007(6) 0.019(10) -0.001(5)
N4 0.047(8) 0.046(6) 0.072(15) -0.001(6) 0.028(9) -0.003(5)
C10 0.036(9) 0.050(7) 0.10(2) -0.021(8) 0.026(11) -0.007(5)
C11 0.043(9) 0.045(6) 0.049(16) -0.011(6) 0.008(9) -0.002(5)
C12 0.061(11) 0.062(8) 0.073(19) 0.007(8) 0.013(11) 0.008(7)
O5 0.056(7) 0.049(5) 0.061(11) 0.013(5) 0.025(7) 0.003(4)
O6 0.049(7) 0.045(5) 0.065(11) -0.008(4) 0.019(7) -0.004(4)
C13 0.033(9) 0.043(7) 0.097(19) 0.002(7) 0.018(10) 0.002(5)
C14 0.057(10) 0.046(7) 0.043(15) -0.003(6) 0.026(9) 0.003(5)
N5 0.073(10) 0.034(5) 0.079(16) 0.006(6) 0.037(10) 0.004(5)
C15 0.059(11) 0.041(7) 0.09(2) 0.003(7) 0.012(12) 0.005(6)
N6 0.071(10) 0.040(6) 0.078(17) 0.002(6) 0.025(10) 0.007(5)
C16 0.071(13) 0.053(9) 0.13(3) 0.012(11) 0.030(15) -0.014(8)
C17 0.066(13) 0.056(9) 0.19(4) 0.001(13) 0.018(16) -0.016(8)
C18 0.089(16) 0.063(10) 0.12(3) 0.022(11) 0.036(16) 0.007(9)
O7 0.063(7) 0.049(5) 0.097(13) -0.018(5) 0.024(8) -0.015(4)
O8 0.081(8) 0.040(5) 0.135(15) 0.018(6) 0.036(9) 0.018(5)
S1 0.062(3) 0.0472(17) 0.058(4) -0.0003(16) 0.024(3) 0.0067(14)
S2 0.067(3) 0.0370(15) 0.068(5) 0.0039(15) 0.020(3) -0.0014(14)
N11 0.059(9) 0.050(6) 0.072(15) 0.006(6) 0.016(9) 0.010(5)
O12 0.081(10) 0.089(8) 0.065(15) 0.007(7) 0.016(10) 0.007(6)
O13 0.082(8) 0.048(5) 0.076(13) -0.005(5) 0.013(8) 0.018(5)
O14 0.071(8) 0.053(5) 0.082(13) 0.013(5) -0.005(8) -0.002(5)
O15 0.092(9) 0.042(5) 0.093(14) -0.006(5) 0.015(8) 0.020(5)
C19 0.071(15) 0.067(10) 0.12(3) -0.002(11) 0.041(17) 0.005(8)
F1 0.122(12) 0.089(8) 0.107(17) -0.022(7) 0.010(11) -0.007(7)
F2 0.164(14) 0.052(5) 0.19(2) -0.031(7) -0.021(12) 0.020(7)
F3 0.123(12) 0.150(13) 0.17(2) -0.041(11) 0.057(13) -0.080(10)
C20 0.089(17) 0.070(10) 0.05(2) -0.010(9) 0.037(14) -0.014(9)
F4 0.095(11) 0.129(11) 0.18(2) -0.007(10) 0.064(13) -0.029(8)
F5 0.166(12) 0.049(5) 0.122(15) -0.003(6) 0.084(10) -0.025(6)
F6 0.172(15) 0.079(7) 0.15(2) 0.002(9) 0.091(14) -0.028(8)
S3 0.076(3) 0.0504(19) 0.100(6) -0.014(2) 0.019(3) 0.0059(18)
S4 0.075(3) 0.0431(17) 0.095(6) -0.0051(19) 0.033(3) 0.0044(16)
N16 0.085(11) 0.050(6) 0.070(16) -0.010(6) 0.025(10) -0.009(6)
O17 0.084(10) 0.084(8) 0.15(2) -0.035(9) 0.030(11) -0.021(7)
O18 0.177(18) 0.064(8) 0.12(2) -0.012(8) -0.002(14) 0.023(9)
O19 0.068(8) 0.053(6) 0.156(19) 0.011(7) 0.049(10) 0.007(5)
O20 0.100(10) 0.059(6) 0.082(14) -0.009(6) 0.034(9) -0.003(6)
C21 0.13(2) 0.086(13) 0.11(3) -0.055(15) 0.02(2) -0.003(13)
C22 0.077(16) 0.058(9) 0.14(3) -0.016(12) 0.031(19) 0.012(8)
F10 0.115(10) 0.046(5) 0.165(17) 0.007(6) 0.040(10) 0.011(5)
F11 0.078(9) 0.099(8) 0.151(18) 0.018(8) 0.031(10) 0.024(6)
F12 0.163(15) 0.085(8) 0.119(19) 0.014(8) 0.039(13) 0.028(8)
S5 0.085(3) 0.0537(19) 0.092(6) 0.005(2) 0.050(3) 0.0047(18)
S6 0.087(4) 0.057(2) 0.090(6) 0.000(2) 0.040(3) 0.0005(19)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.321(12) 4_565 ?
Dy1 O4 2.348(12) 4_566 ?
Dy1 O1 2.351(13) . ?
Dy1 O3 2.381(10) . ?
Dy1 O8 2.405(11) . ?
Dy1 O7 2.416(10) . ?
Dy1 O5 2.469(9) . ?
Dy1 O6 2.552(9) . ?
O1 C1 1.24(2) . ?
O2 C1 1.25(2) . ?
O2 Dy1 2.321(12) 4_566 ?
C1 C2 1.50(2) . ?
C2 N1 1.48(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N1 C3 1.32(2) . ?
N1 C5 1.386(18) . ?
C3 N2 1.32(2) . ?
C3 H3A 0.9500 . ?
N2 C4 1.404(17) . ?
N2 C6 1.46(2) . ?
C4 C5 1.37(3) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
O3 C7 1.23(2) . ?
O4 C7 1.27(2) . ?
O4 Dy1 2.348(12) 4_565 ?
C7 C8 1.51(2) . ?
C8 N3 1.45(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
N3 C9 1.36(2) . ?
N3 C11 1.388(17) . ?
C9 N4 1.30(2) . ?
C9 H9A 0.9500 . ?
N4 C10 1.397(16) . ?
N4 C12 1.49(2) . ?
C10 C11 1.32(2) . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O5 C13 1.264(18) . ?
O6 C13 1.255(18) . ?
C13 C14 1.534(17) . ?
C14 N5 1.48(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
N5 C15 1.32(2) . ?
N5 C17 1.39(2) . ?
C15 N6 1.31(2) . ?
C15 H15A 0.9500 . ?
N6 C16 1.37(3) . ?
N6 C18 1.47(3) . ?
C16 C17 1.34(4) . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
S1 O13 1.417(10) . ?
S1 O12 1.431(17) . ?
S1 N11 1.537(16) . ?
S1 C19 1.817(16) . ?
S2 O15 1.427(9) . ?
S2 O14 1.438(13) . ?
S2 N11 1.607(17) . ?
S2 C20 1.810(16) . ?
C19 F3 1.27(3) . ?
C19 F2 1.29(2) . ?
C19 F1 1.36(3) . ?
C20 F6 1.29(3) . ?
C20 F5 1.307(19) . ?
C20 F4 1.33(3) . ?
S3 O17 1.414(14) . ?
S3 O18 1.45(2) . ?
S3 N16 1.537(17) . ?
S3 C21 1.87(2) . ?
S4 O20 1.420(13) . ?
S4 O19 1.450(13) . ?
S4 N16 1.611(19) . ?
S4 C22 1.86(3) . ?
C21 F8B 1.328(16) . ?
C21 F7B 1.336(16) . ?
C21 F9A 1.344(17) . ?
C21 F7A 1.355(16) . ?
C21 F9B 1.363(16) . ?
C21 F8A 1.381(16) . ?
C22 F11 1.30(3) . ?
C22 F10 1.34(2) . ?
C22 F12 1.30(3) . ?
S5 O22A 1.413(14) . ?
S5 O23B 1.420(16) . ?
S5 O22B 1.471(14) . ?
S5 O23A 1.472(14) . ?
S5 N21B 1.558(13) . ?
S5 N21A 1.591(14) . ?
S5 C23A 1.792(19) . ?
S5 C23B 1.82(3) . ?
S6 O24B 1.403(14) . ?
S6 O25A 1.402(15) . ?
S6 O24A 1.462(14) . ?
S6 O25B 1.467(15) . ?
S6 N21A 1.569(13) . ?
S6 N21B 1.583(14) . ?
S6 C24B 1.785(18) . ?
S6 C24A 1.808(19) . ?
C23A F15A 1.298(18) . ?
C23A F14A 1.305(18) . ?
C23A F13A 1.310(18) . ?
C23B F14B 1.302(19) . ?
C23B F13B 1.313(19) . ?
C23B F15B 1.313(19) . ?
C24A F17A 1.295(18) . ?
C24A F16A 1.301(18) . ?
C24A F18A 1.299(18) . ?
C24B F16B 1.284(17) . ?
C24B F18B 1.291(18) . ?
C24B F17B 1.298(18) . ?

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
O2 Dy1 O4 146.2(4) 4_565 4_566 ?
O2 Dy1 O1 78.6(5) 4_565 . ?
O4 Dy1 O1 102.1(5) 4_566 . ?
O2 Dy1 O3 109.6(5) 4_565 . ?
O4 Dy1 O3 81.6(5) 4_566 . ?
O1 Dy1 O3 159.6(3) . . ?
O2 Dy1 O8 74.6(4) 4_565 . ?
O4 Dy1 O8 139.1(4) 4_566 . ?
O1 Dy1 O8 79.9(4) . . ?
O3 Dy1 O8 84.3(4) . . ?
O2 Dy1 O7 140.2(4) 4_565 . ?
O4 Dy1 O7 71.9(4) 4_566 . ?
O1 Dy1 O7 82.1(4) . . ?
O3 Dy1 O7 80.0(4) . . ?
O8 Dy1 O7 67.9(5) . . ?
O2 Dy1 O5 72.5(4) 4_565 . ?
O4 Dy1 O5 80.1(4) 4_566 . ?
O1 Dy1 O5 124.5(3) . . ?
O3 Dy1 O5 75.8(3) . . ?
O8 Dy1 O5 132.6(5) . . ?
O7 Dy1 O5 145.3(4) . . ?
O2 Dy1 O6 77.8(4) 4_565 . ?
O4 Dy1 O6 69.9(4) 4_566 . ?
O1 Dy1 O6 76.0(3) . . ?
O3 Dy1 O6 123.5(3) . . ?
O8 Dy1 O6 146.3(4) . . ?
O7 Dy1 O6 130.2(4) . . ?
O5 Dy1 O6 52.4(3) . . ?
C1 O1 Dy1 117.5(11) . . ?
C1 O2 Dy1 151.9(9) . 4_566 ?
O1 C1 O2 122.9(15) . . ?
O1 C1 C2 121.6(18) . . ?
O2 C1 C2 115(2) . . ?
N1 C2 C1 116.1(18) . . ?
N1 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
N1 C2 H2B 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
C3 N1 C5 109.8(16) . . ?
C3 N1 C2 125.8(12) . . ?
C5 N1 C2 123.9(13) . . ?
N1 C3 N2 109.3(12) . . ?
N1 C3 H3A 125.4 . . ?
N2 C3 H3A 125.4 . . ?
C3 N2 C4 107.9(14) . . ?
C3 N2 C6 125.0(12) . . ?
C4 N2 C6 127.1(15) . . ?
C5 C4 N2 107.2(14) . . ?
C5 C4 H4A 126.4 . . ?
N2 C4 H4A 126.4 . . ?
C4 C5 N1 105.7(14) . . ?
C4 C5 H5A 127.2 . . ?
N1 C5 H5A 127.2 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 O3 Dy1 112.6(10) . . ?
C7 O4 Dy1 154.8(11) . 4_565 ?
O3 C7 O4 119.4(14) . . ?
O3 C7 C8 122.7(16) . . ?
O4 C7 C8 118.0(18) . . ?
N3 C8 C7 112.3(16) . . ?
N3 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
N3 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C9 N3 C11 107.3(15) . . ?
C9 N3 C8 126.4(11) . . ?
C11 N3 C8 126.1(12) . . ?
N4 C9 N3 108.4(11) . . ?
N4 C9 H9A 125.8 . . ?
N3 C9 H9A 125.8 . . ?
C9 N4 C10 108.9(14) . . ?
C9 N4 C12 125.5(12) . . ?
C10 N4 C12 125.6(15) . . ?
C11 C10 N4 107.5(14) . . ?
C11 C10 H10A 126.3 . . ?
N4 C10 H10A 126.3 . . ?
C10 C11 N3 107.8(13) . . ?
C10 C11 H11A 126.1 . . ?
N3 C11 H11A 126.1 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 O5 Dy1 93.9(9) . . ?
C13 O6 Dy1 90.3(8) . . ?
O6 C13 O5 123.4(12) . . ?
O6 C13 C14 120.5(13) . . ?
O5 C13 C14 116.1(14) . . ?
N5 C14 C13 112.9(13) . . ?
N5 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
N5 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C15 N5 C17 111.1(19) . . ?
C15 N5 C14 126.2(15) . . ?
C17 N5 C14 123(2) . . ?
N6 C15 N5 107.4(17) . . ?
N6 C15 H15A 126.3 . . ?
N5 C15 H15A 126.3 . . ?
C15 N6 C16 109(2) . . ?
C15 N6 C18 124.5(18) . . ?
C16 N6 C18 126.5(18) . . ?
C17 C16 N6 109.6(17) . . ?
C17 C16 H16A 125.2 . . ?
N6 C16 H16A 125.2 . . ?
C16 C17 N5 103(2) . . ?
C16 C17 H17A 128.5 . . ?
N5 C17 H17A 128.5 . . ?
N6 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O13 S1 O12 115.6(8) . . ?
O13 S1 N11 119.6(8) . . ?
O12 S1 N11 108.4(8) . . ?
O13 S1 C19 105.5(8) . . ?
O12 S1 C19 104.1(11) . . ?
N11 S1 C19 101.3(11) . . ?
O15 S2 O14 117.5(8) . . ?
O15 S2 N11 116.6(8) . . ?
O14 S2 N11 109.3(8) . . ?
O15 S2 C20 104.8(9) . . ?
O14 S2 C20 101.8(10) . . ?
N11 S2 C20 104.7(9) . . ?
S1 N11 S2 126.6(8) . . ?
F3 C19 F2 108(2) . . ?
F3 C19 F1 107.4(19) . . ?
F2 C19 F1 107(2) . . ?
F3 C19 S1 112.4(18) . . ?
F2 C19 S1 113.6(15) . . ?
F1 C19 S1 108.5(15) . . ?
F6 C20 F5 108.1(18) . . ?
F6 C20 F4 105.4(19) . . ?
F5 C20 F4 106.8(17) . . ?
F6 C20 S2 111.4(14) . . ?
F5 C20 S2 113.6(14) . . ?
F4 C20 S2 111.2(16) . . ?
O17 S3 O18 114.8(12) . . ?
O17 S3 N16 119.5(11) . . ?
O18 S3 N16 110.0(9) . . ?
O17 S3 C21 105.9(8) . . ?
O18 S3 C21 102.8(10) . . ?
N16 S3 C21 101.2(7) . . ?
O20 S4 O19 118.6(8) . . ?
O20 S4 N16 107.1(8) . . ?
O19 S4 N16 115.1(10) . . ?
O20 S4 C22 102.3(11) . . ?
O19 S4 C22 105.4(10) . . ?
N16 S4 C22 107.0(12) . . ?
S3 N16 S4 126.1(10) . . ?
F8B C21 F7B 112.4(15) . . ?
F9A C21 F7A 109.4(16) . . ?
F8B C21 F9B 110.0(15) . . ?
F7B C21 F9B 110.8(16) . . ?
F9A C21 F8A 107.9(16) . . ?
F7A C21 F8A 107.8(14) . . ?
F8B C21 S3 114.6(16) . . ?
F7B C21 S3 105.9(18) . . ?
F9A C21 S3 118.4(19) . . ?
F7A C21 S3 110.6(17) . . ?
F9B C21 S3 102.9(16) . . ?
F8A C21 S3 102.0(16) . . ?
F11 C22 F10 108.9(18) . . ?
F11 C22 F12 111(3) . . ?
F10 C22 F12 110(2) . . ?
F11 C22 S4 110.3(19) . . ?
F10 C22 S4 108.2(19) . . ?
F12 C22 S4 108.6(14) . . ?
O23B S5 O22B 123.8(16) . . ?
O22A S5 O23A 117.9(14) . . ?
O23B S5 N21B 112.5(13) . . ?
O22B S5 N21B 108.0(12) . . ?
O22A S5 N21A 109.7(12) . . ?
O23A S5 N21A 105.7(11) . . ?
O22A S5 C23A 113.6(13) . . ?
O23A S5 C23A 105.1(12) . . ?
N21A S5 C23A 103.6(13) . . ?
O23B S5 C23B 110.1(16) . . ?
O22B S5 C23B 101.2(14) . . ?
N21B S5 C23B 97.5(13) . . ?
O25A S6 O24A 124.4(16) . . ?
O24B S6 O25B 116.7(15) . . ?
O25A S6 N21A 113.4(13) . . ?
O24A S6 N21A 107.9(11) . . ?
O24B S6 N21B 111.5(13) . . ?
O25B S6 N21B 105.4(12) . . ?
O24B S6 C24B 115.2(15) . . ?
O25B S6 C24B 105.1(14) . . ?
N21B S6 C24B 101.4(14) . . ?
O25A S6 C24A 107.6(15) . . ?
O24A S6 C24A 98.9(14) . . ?
N21A S6 C24A 101.2(13) . . ?
S6 N21A S5 127.3(14) . . ?
S5 N21B S6 128.7(15) . . ?
F15A C23A F14A 109.6(16) . . ?
F15A C23A F13A 108.8(16) . . ?
F14A C23A F13A 107.7(15) . . ?
F15A C23A S5 106(2) . . ?
F14A C23A S5 107.3(17) . . ?
F13A C23A S5 117(2) . . ?
F14B C23B F13B 108.8(19) . . ?
F14B C23B F15B 107.9(19) . . ?
F13B C23B F15B 108.2(19) . . ?
F14B C23B S5 116(2) . . ?
F13B C23B S5 107(2) . . ?
F15B C23B S5 109(2) . . ?
F17A C24A F16A 108.1(16) . . ?
F17A C24A F18A 107.1(16) . . ?
F16A C24A F18A 107.1(16) . . ?
F17A C24A S6 114(2) . . ?
F16A C24A S6 106.7(19) . . ?
F18A C24A S6 114(2) . . ?
F16B C24B F18B 108.8(16) . . ?
F16B C24B F17B 106.9(15) . . ?
F18B C24B F17B 108.1(17) . . ?
F16B C24B S6 123(2) . . ?
F18B C24B S6 105(2) . . ?
F17B C24B S6 104(2) . . ?

_diffrn_measured_fraction_theta_max 0.566
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.585
_refine_diff_density_max         2.293
_refine_diff_density_min         -2.876
_refine_diff_density_rms         0.184
_database_code_depnum_ccdc_archive 'CCDC 896592'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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data_dyilpf6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C24 H34 Dy N8 O9), 3(F6 P), 2(H2 O)'
_chemical_formula_sum            'C24 H38 Dy F18 N8 O11 P3'
_chemical_formula_weight         1212.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 '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 0.0082 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0142 0.0079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0225 0.0133 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1245 0.1209 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1899 5.4020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   26.0839(8)
_cell_length_b                   18.1039(6)
_cell_length_c                   8.7895(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.496(1)
_cell_angle_gamma                90.00
_cell_volume                     4105.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9918
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      30.77

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2396
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.80000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22994
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         30.99
_reflns_number_total             8798
_reflns_number_gt                6802
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker AXS Inc., 2005)'
_computing_cell_refinement       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'Apex2 (Bruker AXS Inc., 2005)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.1197P)^2^+23.2758P] where P=(Fo^2^+2Fc^2^)/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         8798
_refine_ls_number_parameters     637
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_ref         0.2253
_refine_ls_wR_factor_gt          0.2083
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.257525(15) 0.132008(19) 0.67312(4) 0.03251(16) Uani 1 1 d . . .
O1 O 0.2231(3) 0.2018(4) 0.4625(7) 0.0452(14) Uani 1 1 d . . .
O2 O 0.2047(2) 0.2924(3) 0.2930(6) 0.0397(13) Uani 1 1 d . . .
C1 C 0.1953(3) 0.2537(4) 0.4036(9) 0.0342(16) Uani 1 1 d . . .
C2 C 0.1455(4) 0.2677(5) 0.4679(11) 0.044(2) Uani 1 1 d . . .
H2A H 0.1208 0.2272 0.4349 0.053 Uiso 1 1 calc R . .
H2B H 0.1529 0.2668 0.5816 0.053 Uiso 1 1 calc R . .
N1 N 0.1213(3) 0.3375(4) 0.4193(8) 0.0422(16) Uani 1 1 d . . .
C3 C 0.1282(4) 0.3998(6) 0.4986(10) 0.047(2) Uani 1 1 d . . .
H3A H 0.1479 0.4047 0.5980 0.056 Uiso 1 1 calc R . .
N2 N 0.1038(3) 0.4538(4) 0.4192(9) 0.0453(17) Uani 1 1 d . . .
C4 C 0.0789(4) 0.4253(6) 0.2833(11) 0.049(2) Uani 1 1 d . . .
H4A H 0.0576 0.4518 0.2045 0.059 Uiso 1 1 calc R . .
C5 C 0.0902(4) 0.3529(6) 0.2828(10) 0.047(2) Uani 1 1 d . . .
H5A H 0.0788 0.3188 0.2029 0.057 Uiso 1 1 calc R . .
C6 C 0.1016(5) 0.5310(6) 0.4743(15) 0.063(3) Uani 1 1 d . . .
H6A H 0.0677 0.5402 0.5057 0.095 Uiso 1 1 calc R . .
H6B H 0.1069 0.5650 0.3912 0.095 Uiso 1 1 calc R . .
H6C H 0.1289 0.5387 0.5622 0.095 Uiso 1 1 calc R . .
O3 O 0.3094(2) 0.2446(4) 0.6824(7) 0.0444(14) Uani 1 1 d . . .
O4 O 0.3308(3) 0.1621(4) 0.8637(7) 0.0491(15) Uani 1 1 d . . .
C7 C 0.3383(3) 0.2226(5) 0.8039(9) 0.0381(18) Uani 1 1 d . . .
C8 C 0.3812(4) 0.2713(5) 0.8792(10) 0.0425(19) Uani 1 1 d . . .
H8A H 0.3695 0.2961 0.9684 0.051 Uiso 1 1 calc R . .
H8B H 0.4113 0.2399 0.9188 0.051 Uiso 1 1 calc R . .
N3 N 0.3981(3) 0.3281(4) 0.7766(8) 0.0417(16) Uani 1 1 d . . .
C9 C 0.3695(4) 0.3853(5) 0.7144(10) 0.0430(19) Uani 1 1 d . . .
H9A H 0.3353 0.3967 0.7317 0.052 Uiso 1 1 calc R . .
N4 N 0.3963(3) 0.4227(4) 0.6263(8) 0.0441(17) Uani 1 1 d . . .
C10 C 0.4436(4) 0.3887(6) 0.6292(13) 0.055(2) Uani 1 1 d . . .
H10A H 0.4707 0.4039 0.5747 0.066 Uiso 1 1 calc R . .
C11 C 0.4444(4) 0.3301(6) 0.7235(13) 0.054(2) Uani 1 1 d . . .
H11A H 0.4723 0.2963 0.7484 0.065 Uiso 1 1 calc R . .
C12 C 0.3784(5) 0.4874(7) 0.5343(14) 0.068(3) Uani 1 1 d . . .
H12A H 0.3775 0.4759 0.4250 0.102 Uiso 1 1 calc R . .
H12B H 0.4021 0.5288 0.5626 0.102 Uiso 1 1 calc R . .
H12C H 0.3435 0.5008 0.5535 0.102 Uiso 1 1 calc R . .
O5 O 0.3070(2) 0.0166(4) 0.6839(7) 0.0452(14) Uani 1 1 d . . .
O6 O 0.3155(3) 0.0961(4) 0.4990(7) 0.0485(15) Uani 1 1 d . . .
C13 C 0.3279(4) 0.0372(5) 0.5687(10) 0.0412(19) Uani 1 1 d . . .
C14 C 0.3691(5) -0.0100(6) 0.5118(13) 0.059(3) Uani 1 1 d . . .
H14A H 0.3570 -0.0245 0.4038 0.071 Uiso 1 1 calc R . .
H14B H 0.4011 0.0196 0.5136 0.071 Uiso 1 1 calc R . .
N5 N 0.3811(3) -0.0767(5) 0.6047(10) 0.0503(19) Uani 1 1 d . . .
C15 C 0.3513(5) -0.1337(6) 0.6079(17) 0.069(3) Uani 1 1 d . . .
H15A H 0.3184 -0.1397 0.5467 0.083 Uiso 1 1 calc R . .
N6 N 0.3738(4) -0.1826(5) 0.7100(14) 0.067(3) Uani 1 1 d . . .
C16 C 0.4202(4) -0.1563(7) 0.7668(14) 0.062(3) Uani 1 1 d . . .
H16A H 0.4452 -0.1792 0.8415 0.074 Uiso 1 1 calc R . .
C17 C 0.4248(5) -0.0913(7) 0.6983(17) 0.072(3) Uani 1 1 d . . .
H17A H 0.4546 -0.0604 0.7139 0.086 Uiso 1 1 calc R . .
C18 C 0.3546(6) -0.2552(8) 0.751(3) 0.131(9) Uani 1 1 d . . .
H18A H 0.3700 -0.2678 0.8563 0.196 Uiso 1 1 calc R . .
H18B H 0.3642 -0.2926 0.6798 0.196 Uiso 1 1 calc R . .
H18C H 0.3168 -0.2535 0.7444 0.196 Uiso 1 1 calc R . .
O7 O 0.1969(3) 0.0524(4) 0.5589(8) 0.0557(17) Uani 1 1 d . . .
O8 O 0.1867(3) 0.0130(5) 0.3129(9) 0.064(2) Uani 1 1 d D . .
C19 C 0.1789(4) 0.0094(5) 0.4503(11) 0.049(2) Uani 1 1 d . . .
C20 C 0.1468(5) -0.0522(6) 0.5053(13) 0.061(3) Uani 1 1 d . . .
H20A H 0.1700 -0.0843 0.5760 0.073 Uiso 1 1 calc R . .
H20B H 0.1214 -0.0300 0.5651 0.073 Uiso 1 1 calc R . .
N7 N 0.1184(4) -0.0987(5) 0.3829(9) 0.0523(19) Uani 1 1 d . . .
C21 C 0.1392(4) -0.1500(6) 0.2968(13) 0.054(2) Uani 1 1 d . . .
H21A H 0.1749 -0.1618 0.3027 0.065 Uiso 1 1 calc R . .
N8 N 0.1006(4) -0.1804(5) 0.2033(10) 0.055(2) Uani 1 1 d . . .
C22 C 0.0551(5) -0.1499(7) 0.2273(15) 0.063(3) Uani 1 1 d . . .
H22A H 0.0216 -0.1621 0.1751 0.076 Uiso 1 1 calc R . .
C23 C 0.0663(5) -0.0987(7) 0.3399(14) 0.062(3) Uani 1 1 d . . .
H23A H 0.0420 -0.0683 0.3811 0.075 Uiso 1 1 calc R . .
C24 C 0.1048(6) -0.2384(7) 0.0876(15) 0.071(3) Uani 1 1 d . . .
H24A H 0.0858 -0.2230 -0.0119 0.107 Uiso 1 1 calc R . .
H24B H 0.0900 -0.2845 0.1200 0.107 Uiso 1 1 calc R . .
H24C H 0.1414 -0.2461 0.0779 0.107 Uiso 1 1 calc R . .
O9 O 0.2400(3) 0.0653(4) 0.8906(7) 0.0511(16) Uani 1 1 d D . .
H91 H 0.238(4) 0.081(5) 0.991(6) 0.061 Uiso 1 1 d D . .
H92 H 0.244(4) 0.015(2) 0.897(11) 0.061 Uiso 1 1 d D . .
P1 P 0.50461(12) 0.37682(13) 0.2047(3) 0.0509(6) Uani 1 1 d . . .
F1 F 0.5097(3) 0.3089(4) 0.0927(8) 0.0726(19) Uani 1 1 d . . .
F2 F 0.5232(3) 0.3251(4) 0.3484(8) 0.077(2) Uani 1 1 d . . .
F3 F 0.4984(3) 0.4447(4) 0.3198(9) 0.075(2) Uani 1 1 d . . .
F4 F 0.4852(4) 0.4280(4) 0.0600(9) 0.088(2) Uani 1 1 d . . .
F5 F 0.5631(3) 0.3996(5) 0.1958(10) 0.082(2) Uani 1 1 d . . .
F6 F 0.4460(3) 0.3545(4) 0.2129(10) 0.081(2) Uani 1 1 d . . .
P2 P 0.02355(12) 0.12530(14) 0.2893(3) 0.0505(6) Uani 1 1 d U . .
F7 F 0.0246(3) 0.1852(5) 0.4232(9) 0.086(2) Uani 1 1 d . A .
F8 F 0.0223(3) 0.0650(4) 0.1591(9) 0.082(2) Uani 1 1 d . A .
F9A F 0.0398(19) 0.1849(17) 0.185(4) 0.151(14) Uani 0.50 1 d PU A 1
F10A F 0.0797(8) 0.0997(19) 0.331(3) 0.102(7) Uani 0.50 1 d PU A 1
F11A F 0.0060(14) 0.0605(14) 0.401(4) 0.111(9) Uani 0.50 1 d PU A 1
F12A F -0.0341(11) 0.144(2) 0.248(5) 0.134(12) Uani 0.50 1 d PU A 1
F9B F 0.0676(9) 0.1714(15) 0.224(3) 0.091(7) Uani 0.50 1 d PU A 2
F10B F 0.0668(15) 0.0858(15) 0.401(3) 0.127(10) Uani 0.50 1 d PU A 2
F11B F -0.0227(14) 0.0859(17) 0.344(3) 0.121(11) Uani 0.50 1 d PU A 2
F12B F -0.0186(12) 0.1684(16) 0.180(4) 0.098(9) Uani 0.50 1 d PU A 2
P3 P 0.23254(15) -0.16554(18) 0.8897(5) 0.0718(9) Uani 1 1 d . . .
F13 F 0.2407(4) -0.1653(6) 0.7176(10) 0.096(2) Uani 1 1 d . . .
F14 F 0.1728(3) -0.1865(5) 0.8379(11) 0.092(2) Uani 1 1 d . . .
F15 F 0.2241(5) -0.1654(6) 1.0652(11) 0.119(4) Uani 1 1 d . . .
F16 F 0.2905(4) -0.1421(6) 0.9384(14) 0.115(3) Uani 1 1 d . . .
F17 F 0.2462(4) -0.2506(4) 0.9010(14) 0.108(3) Uani 1 1 d . . .
F18 F 0.2168(4) -0.0806(4) 0.8724(14) 0.113(3) Uani 1 1 d . . .
O11 O 0.2412(3) 0.1275(4) 0.1652(8) 0.0591(19) Uani 1 1 d D . .
H111 H 0.224(5) 0.086(6) 0.227(14) 0.089 Uiso 1 1 d D . .
H112 H 0.269(4) 0.170(5) 0.173(15) 0.089 Uiso 1 1 d D . .
O12A O 0.2785(7) -0.0693(11) 0.292(2) 0.106(5) Uiso 0.68 1 d P B 1
O12B O 0.2770(18) -0.030(3) 0.190(5) 0.127(14) Uiso 0.32 1 d P C 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.0425(3) 0.0296(2) 0.0260(2) -0.00016(13) 0.00689(15) 0.00181(14)
O1 0.059(4) 0.043(3) 0.034(3) 0.002(3) 0.007(3) 0.010(3)
O2 0.047(3) 0.042(3) 0.032(3) 0.006(2) 0.010(2) 0.003(3)
C1 0.041(4) 0.030(4) 0.030(4) 0.001(3) 0.000(3) 0.000(3)
C2 0.047(5) 0.042(5) 0.044(5) 0.010(4) 0.011(4) -0.002(4)
N1 0.041(4) 0.048(4) 0.037(4) 0.007(3) 0.004(3) 0.007(3)
C3 0.049(5) 0.053(6) 0.039(4) -0.002(4) 0.011(4) -0.004(4)
N2 0.042(4) 0.044(4) 0.049(4) 0.004(3) 0.005(3) 0.004(3)
C4 0.042(5) 0.059(6) 0.046(5) 0.014(4) 0.006(4) 0.011(4)
C5 0.044(5) 0.061(6) 0.034(4) 0.000(4) -0.004(4) 0.002(4)
C6 0.061(7) 0.045(6) 0.083(8) -0.002(5) 0.008(6) 0.007(5)
O3 0.047(3) 0.048(4) 0.036(3) 0.008(3) 0.000(3) -0.008(3)
O4 0.064(4) 0.040(3) 0.040(3) 0.010(3) -0.003(3) 0.000(3)
C7 0.045(5) 0.039(4) 0.032(4) -0.006(3) 0.009(3) 0.003(3)
C8 0.054(5) 0.039(5) 0.035(4) 0.004(3) 0.008(4) 0.004(4)
N3 0.050(4) 0.036(4) 0.040(4) -0.004(3) 0.010(3) -0.004(3)
C9 0.049(5) 0.043(5) 0.036(4) 0.002(4) 0.004(4) -0.007(4)
N4 0.054(5) 0.038(4) 0.038(4) -0.004(3) -0.001(3) -0.009(3)
C10 0.050(6) 0.057(6) 0.062(6) -0.002(5) 0.015(5) -0.006(5)
C11 0.040(5) 0.055(6) 0.069(6) -0.002(5) 0.011(5) -0.001(4)
C12 0.078(8) 0.062(7) 0.060(6) 0.013(5) -0.004(6) -0.019(6)
O5 0.052(4) 0.045(3) 0.040(3) 0.005(3) 0.010(3) 0.013(3)
O6 0.059(4) 0.048(4) 0.041(3) 0.008(3) 0.017(3) 0.010(3)
C13 0.053(5) 0.037(4) 0.035(4) -0.003(3) 0.010(4) 0.008(4)
C14 0.070(7) 0.050(6) 0.062(6) 0.012(5) 0.025(5) 0.023(5)
N5 0.053(5) 0.045(4) 0.055(5) -0.001(4) 0.015(4) 0.010(4)
C15 0.065(7) 0.061(7) 0.080(8) -0.003(6) 0.005(6) 0.028(6)
N6 0.056(6) 0.043(5) 0.108(8) 0.011(5) 0.031(5) 0.007(4)
C16 0.055(6) 0.057(6) 0.071(7) 0.017(6) 0.000(5) 0.012(5)
C17 0.054(7) 0.064(8) 0.095(9) 0.005(7) 0.007(6) 0.002(5)
C18 0.080(10) 0.049(8) 0.27(3) 0.044(12) 0.041(14) -0.001(7)
O7 0.059(4) 0.055(4) 0.050(4) -0.005(3) 0.001(3) -0.006(3)
O8 0.071(5) 0.073(5) 0.052(4) -0.005(4) 0.018(4) -0.019(4)
C19 0.055(6) 0.041(5) 0.049(5) -0.002(4) 0.003(4) 0.001(4)
C20 0.077(8) 0.052(6) 0.053(6) -0.005(5) 0.011(5) -0.014(5)
N7 0.064(5) 0.046(5) 0.048(4) 0.001(4) 0.010(4) -0.006(4)
C21 0.056(6) 0.048(5) 0.062(6) -0.002(5) 0.019(5) 0.002(4)
N8 0.067(6) 0.043(4) 0.057(5) -0.009(4) 0.014(4) -0.004(4)
C22 0.064(7) 0.062(7) 0.065(7) -0.006(6) 0.016(6) -0.003(5)
C23 0.064(7) 0.062(7) 0.063(6) -0.008(5) 0.016(5) 0.004(5)
C24 0.090(9) 0.057(7) 0.069(7) -0.012(6) 0.018(6) 0.000(6)
O9 0.082(5) 0.036(3) 0.039(3) 0.002(3) 0.019(3) -0.001(3)
P1 0.0660(17) 0.0375(13) 0.0502(14) 0.0022(10) 0.0121(12) -0.0057(11)
F1 0.104(5) 0.052(4) 0.063(4) -0.009(3) 0.015(4) -0.002(3)
F2 0.096(5) 0.076(5) 0.059(4) 0.013(3) 0.007(4) 0.010(4)
F3 0.098(5) 0.047(4) 0.088(5) -0.016(3) 0.036(4) -0.010(3)
F4 0.126(7) 0.061(4) 0.077(5) 0.022(4) 0.018(4) 0.011(4)
F5 0.077(5) 0.076(5) 0.100(5) -0.009(4) 0.032(4) -0.017(4)
F6 0.069(5) 0.072(5) 0.104(6) 0.000(4) 0.018(4) -0.017(3)
P2 0.0604(16) 0.0453(14) 0.0458(13) -0.0084(10) 0.0074(11) -0.0034(11)
F7 0.096(6) 0.084(5) 0.082(5) -0.044(4) 0.024(4) -0.017(4)
F8 0.095(5) 0.067(4) 0.085(5) -0.036(4) 0.019(4) 0.000(4)
F9A 0.29(4) 0.071(14) 0.101(18) 0.029(12) 0.06(3) -0.02(2)
F10A 0.063(8) 0.14(2) 0.097(17) -0.044(14) -0.002(10) 0.020(9)
F11A 0.18(2) 0.066(11) 0.10(2) -0.003(10) 0.085(19) -0.016(14)
F12A 0.094(12) 0.15(3) 0.15(3) -0.083(16) -0.037(16) 0.063(18)
F9B 0.104(13) 0.089(15) 0.093(15) -0.049(10) 0.064(11) -0.047(11)
F10B 0.20(2) 0.082(14) 0.074(14) -0.022(10) -0.051(14) 0.065(16)
F11B 0.18(2) 0.12(2) 0.082(17) -0.045(12) 0.068(17) -0.10(2)
F12B 0.110(14) 0.062(11) 0.11(2) -0.012(10) -0.034(14) 0.019(11)
P3 0.081(2) 0.0495(17) 0.085(2) 0.0010(16) 0.0152(18) -0.0121(15)
F13 0.108(7) 0.101(6) 0.083(5) 0.004(5) 0.022(5) 0.007(5)
F14 0.078(5) 0.074(5) 0.120(7) -0.006(5) 0.008(5) -0.014(4)
F15 0.153(9) 0.124(8) 0.087(6) -0.019(6) 0.039(6) -0.057(7)
F16 0.091(7) 0.116(8) 0.135(9) 0.005(6) 0.006(6) -0.033(5)
F17 0.118(7) 0.057(5) 0.153(9) 0.016(5) 0.034(6) 0.002(4)
F18 0.132(8) 0.048(4) 0.167(10) -0.013(5) 0.042(7) -0.020(5)
O11 0.065(5) 0.070(5) 0.043(4) -0.021(3) 0.009(3) -0.001(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O7 2.262(7) . ?
Dy1 O2 2.304(6) 4_566 ?
Dy1 O1 2.311(6) . ?
Dy1 O9 2.362(6) . ?
Dy1 O6 2.396(6) . ?
Dy1 O4 2.410(6) . ?
Dy1 O3 2.441(6) . ?
Dy1 O5 2.451(6) . ?
O1 C1 1.251(10) . ?
O2 C1 1.252(10) . ?
O2 Dy1 2.304(6) 4_565 ?
C1 C2 1.514(13) . ?
C2 N1 1.448(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N1 C3 1.325(13) . ?
N1 C5 1.374(11) . ?
C3 N2 1.310(12) . ?
C3 H3A 0.9500 . ?
N2 C4 1.374(13) . ?
N2 C6 1.482(13) . ?
C4 C5 1.342(14) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
O3 C7 1.277(10) . ?
O4 C7 1.244(11) . ?
C7 C8 1.498(13) . ?
C8 N3 1.478(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
N3 C9 1.344(12) . ?
N3 C11 1.358(13) . ?
C9 N4 1.307(12) . ?
C9 H9A 0.9500 . ?
N4 C10 1.375(14) . ?
N4 C12 1.460(14) . ?
C10 C11 1.345(16) . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O5 C13 1.275(11) . ?
O6 C13 1.247(11) . ?
C13 C14 1.513(13) . ?
C14 N5 1.466(13) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
N5 C15 1.293(16) . ?
N5 C17 1.330(15) . ?
C15 N6 1.333(16) . ?
C15 H15A 0.9500 . ?
N6 C16 1.327(16) . ?
N6 C18 1.470(16) . ?
C16 C17 1.336(17) . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O7 C19 1.267(12) . ?
O8 C19 1.256(12) . ?
C19 C20 1.516(14) . ?
C20 N7 1.476(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
N7 C23 1.356(15) . ?
N7 C21 1.360(14) . ?
C21 N8 1.321(14) . ?
C21 H21A 0.9500 . ?
N8 C22 1.354(15) . ?
N8 C24 1.477(14) . ?
C22 C23 1.356(17) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O9 H91 0.94(4) . ?
O9 H92 0.92(4) . ?
P1 F2 1.590(7) . ?
P1 F5 1.592(8) . ?
P1 F1 1.593(7) . ?
P1 F6 1.594(8) . ?
P1 F4 1.595(8) . ?
P1 F3 1.615(7) . ?
P2 F9A 1.52(3) . ?
P2 F10A 1.53(2) . ?
P2 F12A 1.53(2) . ?
P2 F11B 1.54(2) . ?
P2 F10B 1.56(2) . ?
P2 F12B 1.56(2) . ?
P2 F8 1.578(7) . ?
P2 F9B 1.59(2) . ?
P2 F7 1.598(7) . ?
P2 F11A 1.64(2) . ?
P3 F13 1.559(10) . ?
P3 F16 1.568(10) . ?
P3 F17 1.581(9) . ?
P3 F15 1.590(10) . ?
P3 F18 1.593(9) . ?
P3 F14 1.603(9) . ?
O11 H111 1.07(3) . ?
O11 H112 1.06(3) . ?

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 Dy1 O2 98.9(2) . 4_566 ?
O7 Dy1 O1 80.2(3) . . ?
O2 Dy1 O1 81.6(2) 4_566 . ?
O7 Dy1 O9 80.0(3) . . ?
O2 Dy1 O9 74.5(2) 4_566 . ?
O1 Dy1 O9 146.0(3) . . ?
O7 Dy1 O6 90.5(3) . . ?
O2 Dy1 O6 158.5(2) 4_566 . ?
O1 Dy1 O6 81.0(2) . . ?
O9 Dy1 O6 126.5(2) . . ?
O7 Dy1 O4 152.0(2) . . ?
O2 Dy1 O4 90.8(2) 4_566 . ?
O1 Dy1 O4 127.4(2) . . ?
O9 Dy1 O4 77.4(2) . . ?
O6 Dy1 O4 89.7(2) . . ?
O7 Dy1 O3 153.5(2) . . ?
O2 Dy1 O3 81.6(2) 4_566 . ?
O1 Dy1 O3 73.6(2) . . ?
O9 Dy1 O3 124.9(2) . . ?
O6 Dy1 O3 81.3(2) . . ?
O4 Dy1 O3 53.8(2) . . ?
O7 Dy1 O5 78.7(2) . . ?
O2 Dy1 O5 146.7(2) 4_566 . ?
O1 Dy1 O5 129.6(2) . . ?
O9 Dy1 O5 72.3(2) . . ?
O6 Dy1 O5 54.1(2) . . ?
O4 Dy1 O5 78.9(2) . . ?
O3 Dy1 O5 115.1(2) . . ?
C1 O1 Dy1 151.1(6) . . ?
C1 O2 Dy1 152.4(6) . 4_565 ?
O1 C1 O2 125.1(8) . . ?
O1 C1 C2 116.6(7) . . ?
O2 C1 C2 118.2(7) . . ?
N1 C2 C1 113.4(7) . . ?
N1 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C3 N1 C5 107.6(8) . . ?
C3 N1 C2 124.7(8) . . ?
C5 N1 C2 127.6(8) . . ?
N2 C3 N1 109.7(8) . . ?
N2 C3 H3A 125.1 . . ?
N1 C3 H3A 125.1 . . ?
C3 N2 C4 108.3(8) . . ?
C3 N2 C6 124.6(9) . . ?
C4 N2 C6 127.0(8) . . ?
C5 C4 N2 107.1(8) . . ?
C5 C4 H4A 126.5 . . ?
N2 C4 H4A 126.5 . . ?
C4 C5 N1 107.3(9) . . ?
C4 C5 H5A 126.3 . . ?
N1 C5 H5A 126.3 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 O3 Dy1 91.4(5) . . ?
C7 O4 Dy1 93.6(5) . . ?
O4 C7 O3 121.1(8) . . ?
O4 C7 C8 119.0(8) . . ?
O3 C7 C8 119.8(8) . . ?
N3 C8 C7 114.3(7) . . ?
N3 C8 H8A 108.7 . . ?
C7 C8 H8A 108.7 . . ?
N3 C8 H8B 108.7 . . ?
C7 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C9 N3 C11 108.0(8) . . ?
C9 N3 C8 125.9(8) . . ?
C11 N3 C8 126.1(8) . . ?
N4 C9 N3 109.1(9) . . ?
N4 C9 H9A 125.5 . . ?
N3 C9 H9A 125.5 . . ?
C9 N4 C10 108.3(8) . . ?
C9 N4 C12 126.0(9) . . ?
C10 N4 C12 125.6(9) . . ?
C11 C10 N4 107.3(9) . . ?
C11 C10 H10A 126.4 . . ?
N4 C10 H10A 126.4 . . ?
C10 C11 N3 107.4(9) . . ?
C10 C11 H11A 126.3 . . ?
N3 C11 H11A 126.3 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 O5 Dy1 90.2(5) . . ?
C13 O6 Dy1 93.5(5) . . ?
O6 C13 O5 122.0(8) . . ?
O6 C13 C14 117.7(8) . . ?
O5 C13 C14 120.3(8) . . ?
N5 C14 C13 112.7(8) . . ?
N5 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
N5 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C15 N5 C17 106.9(10) . . ?
C15 N5 C14 126.1(10) . . ?
C17 N5 C14 126.9(10) . . ?
N5 C15 N6 109.8(12) . . ?
N5 C15 H15A 125.1 . . ?
N6 C15 H15A 125.1 . . ?
C16 N6 C15 107.5(10) . . ?
C16 N6 C18 123.6(12) . . ?
C15 N6 C18 128.9(14) . . ?
N6 C16 C17 106.6(10) . . ?
N6 C16 H16A 126.7 . . ?
C17 C16 H16A 126.7 . . ?
N5 C17 C16 109.1(11) . . ?
N5 C17 H17A 125.5 . . ?
C16 C17 H17A 125.5 . . ?
N6 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 O7 Dy1 152.0(7) . . ?
O8 C19 O7 126.7(10) . . ?
O8 C19 C20 121.4(9) . . ?
O7 C19 C20 111.9(9) . . ?
N7 C20 C19 115.4(9) . . ?
N7 C20 H20A 108.4 . . ?
C19 C20 H20A 108.4 . . ?
N7 C20 H20B 108.4 . . ?
C19 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C23 N7 C21 108.1(9) . . ?
C23 N7 C20 125.3(10) . . ?
C21 N7 C20 126.6(10) . . ?
N8 C21 N7 107.5(9) . . ?
N8 C21 H21A 126.2 . . ?
N7 C21 H21A 126.2 . . ?
C21 N8 C22 109.8(9) . . ?
C21 N8 C24 126.7(10) . . ?
C22 N8 C24 123.5(10) . . ?
N8 C22 C23 107.0(11) . . ?
N8 C22 H22A 126.5 . . ?
C23 C22 H22A 126.5 . . ?
C22 C23 N7 107.6(10) . . ?
C22 C23 H23A 126.2 . . ?
N7 C23 H23A 126.2 . . ?
N8 C24 H24A 109.5 . . ?
N8 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N8 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Dy1 O9 H91 131(6) . . ?
Dy1 O9 H92 121(6) . . ?
H91 O9 H92 105(5) . . ?
F2 P1 F5 90.5(5) . . ?
F2 P1 F1 89.6(4) . . ?
F5 P1 F1 90.1(4) . . ?
F2 P1 F6 89.9(5) . . ?
F5 P1 F6 179.6(5) . . ?
F1 P1 F6 90.0(4) . . ?
F2 P1 F4 179.2(5) . . ?
F5 P1 F4 90.2(5) . . ?
F1 P1 F4 90.1(4) . . ?
F6 P1 F4 89.4(5) . . ?
F2 P1 F3 89.9(4) . . ?
F5 P1 F3 91.1(4) . . ?
F1 P1 F3 178.7(4) . . ?
F6 P1 F3 88.8(4) . . ?
F4 P1 F3 90.5(4) . . ?
F9A P2 F10A 91(2) . . ?
F9A P2 F12A 93(2) . . ?
F10A P2 F12A 175(2) . . ?
F11B P2 F10B 96.8(19) . . ?
F11B P2 F12B 84.8(17) . . ?
F10B P2 F12B 177.3(17) . . ?
F9A P2 F8 91.8(15) . . ?
F10A P2 F8 83.1(10) . . ?
F12A P2 F8 93.8(13) . . ?
F11B P2 F8 88.4(10) . . ?
F10B P2 F8 94.4(9) . . ?
F12B P2 F8 87.7(14) . . ?
F11B P2 F9B 174.6(19) . . ?
F10B P2 F9B 88.5(18) . . ?
F12B P2 F9B 89.8(15) . . ?
F8 P2 F9B 92.3(9) . . ?
F9A P2 F7 89.2(15) . . ?
F10A P2 F7 96.8(10) . . ?
F12A P2 F7 86.3(13) . . ?
F11B P2 F7 90.9(10) . . ?
F10B P2 F7 85.0(9) . . ?
F12B P2 F7 92.8(14) . . ?
F8 P2 F7 179.0(5) . . ?
F9B P2 F7 88.5(9) . . ?
F9A P2 F11A 179.6(18) . . ?
F10A P2 F11A 89.0(16) . . ?
F12A P2 F11A 87.0(19) . . ?
F8 P2 F11A 87.8(12) . . ?
F7 P2 F11A 91.2(12) . . ?
F13 P3 F16 90.0(6) . . ?
F13 P3 F17 90.1(6) . . ?
F16 P3 F17 92.7(6) . . ?
F13 P3 F15 179.7(7) . . ?
F16 P3 F15 90.1(6) . . ?
F17 P3 F15 90.2(7) . . ?
F13 P3 F18 88.6(6) . . ?
F16 P3 F18 89.4(6) . . ?
F17 P3 F18 177.5(7) . . ?
F15 P3 F18 91.2(6) . . ?
F13 P3 F14 89.5(5) . . ?
F16 P3 F14 178.0(6) . . ?
F17 P3 F14 89.3(5) . . ?
F15 P3 F14 90.5(6) . . ?
F18 P3 F14 88.6(5) . . ?
H111 O11 H112 146(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H91 O11 0.94(4) 1.74(4) 2.659(9) 167(10) 1_556
O9 H92 F18 0.92(4) 1.87(7) 2.709(10) 150(10) .
O11 H111 O8 1.07(3) 1.86(3) 2.923(11) 172(12) .
O11 H112 O3 1.06(3) 1.86(3) 2.910(11) 171(12) 4_565
C2 H2A F7 0.99 2.61 3.457(12) 143.8 .
C8 H8A O6 0.99 2.45 3.216(11) 134.4 4_566
C9 H9A O6 0.95 2.48 3.065(11) 119.6 4_566
C14 H14A O12A 0.99 2.29 3.02(2) 130.0 .
C14 H14B F4 0.99 2.37 3.343(16) 167.5 4_566
C20 H20A F13 0.99 2.54 3.512(16) 168.9 .
C21 H21A F14 0.95 2.77 3.093(13) 101.2 4

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         3.495
_refine_diff_density_min         -2.521
_refine_diff_density_rms         0.223
_database_code_depnum_ccdc_archive 'CCDC 896593'