# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2020

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

data_201807328
_database_code_depnum_ccdc_archive 'CCDC 1885081'
loop_
_audit_author_name
_audit_author_address
a
;none
China
;
_audit_update_record             
;
2018-12-14 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2018-07-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C22 H24 Dy F2 N4 O14, 13(H2 O), C11 H6 F N2 O4'
_chemical_formula_sum            'C33 H56 Dy F3 N6 O31'
_chemical_formula_weight         1252.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         C33H56O31N6Dy1F3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.5448(2)
_cell_length_b                   20.51697(19)
_cell_length_c                   23.3482(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9841.66(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    10195
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9190
_cell_measurement_theta_min      3.5730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.158
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.3191
_exptl_crystal_size_mid          0.1009
_exptl_crystal_size_min          0.0519
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25165
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         3.585
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -103.00  -60.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000   30.0000 86

#__ type_ start__ end____ width___ exp.time_
  2 omega  -83.00  -22.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000   30.0000 122

#__ type_ start__ end____ width___ exp.time_
  3 omega   19.00   61.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   32.00  103.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000    0.0000 142

#__ type_ start__ end____ width___ exp.time_
  5 omega   16.00   77.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  120.0000 122

#__ type_ start__ end____ width___ exp.time_
  6 omega   80.00  106.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -90.0000 52

#__ type_ start__ end____ width___ exp.time_
  7 omega   87.00  112.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 50

#__ type_ start__ end____ width___ exp.time_
  8 omega   39.00   82.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 86

#__ type_ start__ end____ width___ exp.time_
  9 omega  106.00  157.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -150.0000 102

#__ type_ start__ end____ width___ exp.time_
 10 omega  127.00  175.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 96

#__ type_ start__ end____ width___ exp.time_
 11 omega   39.00   98.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 118

#__ type_ start__ end____ width___ exp.time_
 12 omega   52.00   78.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 52

#__ type_ start__ end____ width___ exp.time_
 13 omega   90.00  177.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0033411000
_diffrn_orient_matrix_UB_12      -0.0706168000
_diffrn_orient_matrix_UB_13      0.0221707000
_diffrn_orient_matrix_UB_21      0.0041475000
_diffrn_orient_matrix_UB_22      0.0250078000
_diffrn_orient_matrix_UB_23      0.0621124000
_diffrn_orient_matrix_UB_31      -0.0748063000
_diffrn_orient_matrix_UB_32      0.0046275000
_diffrn_orient_matrix_UB_33      0.0025496000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7342
_reflns_number_total             8786
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         8786
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0778P)²+3.4120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1253
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C21-F2A
 1.35 with sigma of 0.02
 C19-F2
 1.35 with sigma of 0.02
 C32-F3A
 1.35 with sigma of 0.02
 F1A-C10
 1.35 with sigma of 0.02
 H7A-O7
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
4. Others
 Sof(H8)=Sof(F1A)=1-FVAR(1)
 Sof(H10)=Sof(F1)=FVAR(1)
 Sof(H19)=Sof(F2A)=1-FVAR(2)
 Sof(H21)=Sof(F2)=FVAR(2)
 Sof(H30)=Sof(F3A)=1-FVAR(3)
 Sof(H32)=Sof(F3)=FVAR(3)
5.a Riding coordinates:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O30(H30A,
 H30B), O23(H23A,H23B), O29(H29A,H29B)
5.b Free rotating group:
 O19(H19A,H19B), O21(H21A,H21B), O22(H22A,H22B), O24(H24A,H24B), O26(H26A,
 H26B), O27(H27A,H27B), O28(H28A,H28B), O31(H31A,H31B)
5.c Rotating group:
 O17(H17A,H17B), O18(H18A,H18B)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), N1(H1), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 N6(H6)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3A), O10(H10A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C 0.55597(19) 0.56494(18) 0.60986(16) 0.0238(8) Uani 1 1 d . . . . .
C2 C 0.5424(2) 0.40156(19) 0.60591(17) 0.0307(9) Uani 1 1 d . . . . .
C3 C 0.55209(18) 0.51444(16) 0.65518(15) 0.0194(7) Uani 1 1 d . . . . .
C4 C 0.54553(18) 0.44760(17) 0.65439(15) 0.0217(7) Uani 1 1 d . . . . .
C5 C 0.54852(17) 0.47582(16) 0.74322(15) 0.0200(7) Uani 1 1 d . . . . .
C6 C 0.54843(18) 0.47341(18) 0.80595(15) 0.0223(7) Uani 1 1 d . . . . .
C7 C 0.54380(19) 0.53015(19) 0.83863(17) 0.0274(8) Uani 1 1 d . . . . .
H7 H 0.5404 0.5708 0.8212 0.033 Uiso 1 1 calc R . . . .
C8 C 0.5444(2) 0.5244(2) 0.89742(17) 0.0335(10) Uani 1 1 d . . . . .
H8 H 0.5410 0.5622 0.9192 0.040 Uiso 0.085(6) 1 calc R . P A 2
C9 C 0.5498(2) 0.4658(2) 0.92549(17) 0.0366(10) Uani 1 1 d . . . . .
H9 H 0.5510 0.4637 0.9653 0.044 Uiso 1 1 calc R . . . .
C10 C 0.5533(2) 0.4101(2) 0.89246(18) 0.0361(10) Uani 1 1 d D . . . .
H10 H 0.5561 0.3697 0.9103 0.043 Uiso 0.915(6) 1 calc R . P A 1
C11 C 0.5529(2) 0.41323(19) 0.83348(17) 0.0283(8) Uani 1 1 d . . . . .
H11 H 0.5556 0.3751 0.8120 0.034 Uiso 1 1 calc R . . . .
C12 C 0.60959(18) 0.89211(18) 0.61576(16) 0.0239(8) Uani 1 1 d . . . . .
C13 C 0.61910(19) 1.05445(19) 0.60661(16) 0.0257(8) Uani 1 1 d . . . . .
C14 C 0.61430(17) 0.94359(17) 0.65979(15) 0.0193(7) Uani 1 1 d . . . . .
C15 C 0.61803(17) 1.01092(17) 0.65674(15) 0.0202(7) Uani 1 1 d . . . . .
C16 C 0.61714(17) 0.98685(18) 0.74661(15) 0.0221(8) Uani 1 1 d . . . . .
C17 C 0.61865(18) 0.9911(2) 0.80923(16) 0.0263(8) Uani 1 1 d . . . . .
C18 C 0.62471(19) 0.9356(2) 0.84258(17) 0.0337(9) Uani 1 1 d . . . . .
H18 H 0.6284 0.8949 0.8255 0.040 Uiso 1 1 calc R . . . .
C19 C 0.6253(2) 0.9414(3) 0.90109(18) 0.0445(12) Uani 1 1 d D . . . .
H19 H 0.6286 0.9037 0.9231 0.053 Uiso 0.421(5) 1 calc R . P B 2
C20 C 0.6212(3) 1.0002(3) 0.92855(19) 0.0559(15) Uani 1 1 d . . . . .
H20 H 0.6217 1.0031 0.9683 0.067 Uiso 1 1 calc R . . . .
C21 C 0.6163(3) 1.0547(3) 0.8947(2) 0.0584(16) Uani 1 1 d D . . . .
H21 H 0.6140 1.0953 0.9122 0.070 Uiso 0.579(5) 1 calc R . P B 1
C22 C 0.6146(2) 1.0514(2) 0.83576(19) 0.0414(11) Uani 1 1 d . . . . .
H22 H 0.6108 1.0892 0.8140 0.050 Uiso 1 1 calc R . . . .
Dy1 Dy 0.57642(2) 0.73028(2) 0.59533(2) 0.02059(10) Uani 1 1 d . . . . .
F1 F 0.53977(18) 0.57865(15) 0.92938(13) 0.0564(10) Uani 0.915(6) 1 d . . P A 1
F1A F 0.5637(19) 0.3580(11) 0.9238(12) 0.0564(10) Uani 0.085(6) 1 d D . P A 2
F2 F 0.6325(3) 0.8901(3) 0.9327(2) 0.0768(15) Uani 0.579(5) 1 d D . P B 1
F2A F 0.6177(5) 1.1098(4) 0.9217(3) 0.0768(15) Uani 0.421(5) 1 d D . P B 2
N1 N 0.55383(15) 0.53112(14) 0.71185(12) 0.0204(6) Uani 1 1 d . . . . .
H1 H 0.5576 0.5700 0.7253 0.024 Uiso 1 1 calc R . . . .
N2 N 0.54336(15) 0.42402(14) 0.70911(13) 0.0224(6) Uani 1 1 d . . . . .
N3 N 0.61382(15) 0.92962(15) 0.71694(13) 0.0216(6) Uani 1 1 d . . . . .
H3 H 0.610(2) 0.892(2) 0.7311(19) 0.036(13) Uiso 1 1 d . . . . .
N4 N 0.61959(15) 1.03733(15) 0.71087(13) 0.0238(6) Uani 1 1 d . . . . .
O1 O 0.56313(15) 0.62241(13) 0.62585(12) 0.0321(6) Uani 1 1 d . . . . .
O2 O 0.55236(17) 0.54656(14) 0.55820(11) 0.0361(7) Uani 1 1 d . . . . .
O3 O 0.54363(18) 0.42451(14) 0.55393(11) 0.0408(8) Uani 1 1 d . . . . .
H3A H 0.5430 0.4645 0.5550 0.061 Uiso 1 1 calc GR . . . .
O4 O 0.5400(2) 0.34278(15) 0.61454(14) 0.0561(10) Uani 1 1 d . . . . .
O5 O 0.60150(14) 0.83452(12) 0.63323(11) 0.0290(6) Uani 1 1 d . . . . .
O6 O 0.61341(16) 0.90918(13) 0.56420(11) 0.0351(7) Uani 1 1 d . . . . .
O7 O 0.61959(17) 1.02910(14) 0.55553(12) 0.0378(7) Uani 1 1 d D . . . .
H7A H 0.616(3) 0.9849(10) 0.556(3) 0.068(18) Uiso 1 1 d D . . . .
O8 O 0.62057(15) 1.11427(13) 0.61260(13) 0.0364(7) Uani 1 1 d . . . . .
O13 O 0.52953(14) 0.73461(13) 0.68767(12) 0.0305(6) Uani 1 1 d . . . . .
H13A H 0.4993 0.7051 0.6911 0.046 Uiso 1 1 d R . . . .
H13B H 0.5529 0.7715 0.7047 0.046 Uiso 1 1 d R . . . .
O14 O 0.66280(14) 0.70884(15) 0.66266(13) 0.0358(7) Uani 1 1 d . . . . .
H14A H 0.6938 0.6874 0.6462 0.054 Uiso 1 1 d R . . . .
H14B H 0.6491 0.6826 0.6890 0.054 Uiso 1 1 d R . . . .
O15 O 0.67426(16) 0.72909(18) 0.54365(14) 0.0517(10) Uani 1 1 d . . . . .
H15A H 0.7122 0.7298 0.5576 0.078 Uiso 1 1 d R . . . .
H15B H 0.6701 0.7489 0.5093 0.078 Uiso 1 1 d R . . . .
O16 O 0.54781(19) 0.66898(15) 0.51055(13) 0.0464(8) Uani 1 1 d . . . . .
H16A H 0.5086 0.6525 0.5134 0.070 Uiso 1 1 d R . . . .
H16B H 0.5751 0.6368 0.5059 0.070 Uiso 1 1 d R . . . .
O17 O 0.56111(17) 0.80304(14) 0.51695(12) 0.0378(7) Uani 1 1 d . . . . .
H17A H 0.5278 0.7910 0.4964 0.057 Uiso 1 1 d GR . . . .
H17B H 0.5954 0.8033 0.4950 0.057 Uiso 1 1 d GR . . . .
O18 O 0.46261(16) 0.73635(18) 0.58765(14) 0.0462(9) Uani 1 1 d . . . . .
H18A H 0.4442 0.7352 0.6216 0.069 Uiso 1 1 d GR . . . .
H18B H 0.4474 0.7034 0.5676 0.069 Uiso 1 1 d GR . . . .
O30 O 0.3818(3) 0.7151(3) 0.4971(2) 0.0925(16) Uani 1 1 d . . . . .
H30A H 0.3798 0.6918 0.4671 0.139 Uiso 1 1 d R . . . .
H30B H 0.3588 0.6979 0.5233 0.139 Uiso 1 1 d R . . . .
C23 C 0.2924(2) 0.4425(2) 0.10855(17) 0.0317(9) Uani 1 1 d . . . . .
C24 C 0.2791(2) 0.6067(2) 0.10436(17) 0.0329(9) Uani 1 1 d . . . . .
C25 C 0.28913(19) 0.49186(19) 0.15475(15) 0.0253(8) Uani 1 1 d . . . . .
C26 C 0.28172(18) 0.55864(18) 0.15242(15) 0.0243(8) Uani 1 1 d . . . . .
C27 C 0.28379(17) 0.52576(18) 0.24195(16) 0.0237(8) Uani 1 1 d . . . . .
C28 C 0.28323(18) 0.5287(2) 0.30474(16) 0.0271(8) Uani 1 1 d . . . . .
C29 C 0.2835(2) 0.5881(2) 0.33347(19) 0.0393(10) Uani 1 1 d . . . . .
H29 H 0.2847 0.6270 0.3130 0.047 Uiso 1 1 calc R . . . .
C30 C 0.2818(3) 0.5889(3) 0.3924(2) 0.0521(14) Uani 1 1 d . . . . .
H30 H 0.2810 0.6289 0.4111 0.062 Uiso 0.443(5) 1 calc R . P C 2
C31 C 0.2813(3) 0.5329(3) 0.4244(2) 0.0549(15) Uani 1 1 d . . . . .
H31 H 0.2804 0.5343 0.4642 0.066 Uiso 1 1 calc R . . . .
C32 C 0.2820(3) 0.4749(3) 0.3956(2) 0.0494(13) Uani 1 1 d D . . . .
H32 H 0.2816 0.4364 0.4166 0.059 Uiso 0.557(5) 1 calc R . P C 1
C33 C 0.2833(2) 0.4714(2) 0.33635(19) 0.0366(10) Uani 1 1 d . . . . .
H33 H 0.2842 0.4312 0.3180 0.044 Uiso 1 1 calc R . . . .
F3 F 0.2848(4) 0.6451(4) 0.4196(3) 0.0798(16) Uani 0.557(5) 1 d . . P C 1
F3A F 0.2841(5) 0.4215(4) 0.4251(3) 0.0798(16) Uani 0.443(5) 1 d D . P C 2
N5 N 0.29080(15) 0.47162(15) 0.21104(13) 0.0246(7) Uani 1 1 d . . . . .
N6 N 0.27835(15) 0.57875(16) 0.20789(13) 0.0264(7) Uani 1 1 d . . . . .
H6 H 0.2736 0.6183 0.2193 0.032 Uiso 1 1 calc R . . . .
O9 O 0.29348(18) 0.38473(16) 0.11986(14) 0.0496(9) Uani 1 1 d . . . . .
O10 O 0.29372(18) 0.46330(16) 0.05565(12) 0.0454(8) Uani 1 1 d . . . . .
H10A H 0.2893 0.5030 0.0553 0.068 Uiso 1 1 calc GR . . . .
O11 O 0.28161(17) 0.58413(16) 0.05397(12) 0.0450(8) Uani 1 1 d . . . . .
O12 O 0.27433(16) 0.66512(15) 0.11774(15) 0.0444(8) Uani 1 1 d . . . . .
O19 O 0.37131(18) 0.76337(18) 0.67064(19) 0.0542(9) Uani 1 1 d . . . . .
H19A H 0.3496 0.7286 0.6759 0.081 Uiso 1 1 d G . . . .
H19B H 0.3475 0.7914 0.6540 0.081 Uiso 1 1 d G . . . .
O20 O 0.55047(17) 0.82158(15) 0.77005(13) 0.0330(7) Uani 1 1 d . . . . .
H20A H 0.559(3) 0.799(3) 0.796(2) 0.043(16) Uiso 1 1 d . . . . .
H20B H 0.519(3) 0.845(3) 0.782(2) 0.048(16) Uiso 1 1 d . . . . .
O21 O 0.41242(19) 0.22804(18) 0.65300(16) 0.0490(9) Uani 1 1 d . . . . .
H21A H 0.4479 0.2184 0.6365 0.073 Uiso 1 1 d G . . . .
H21B H 0.3826 0.2329 0.6282 0.073 Uiso 1 1 d G . . . .
O22 O 0.2877(2) 0.30332(18) 0.74160(18) 0.0598(10) Uani 1 1 d . . . . .
H22A H 0.2691 0.2713 0.7254 0.090 Uiso 1 1 d G . . . .
H22B H 0.3090 0.2899 0.7705 0.090 Uiso 1 1 d G . . . .
O23 O 0.19982(17) 0.31932(17) 0.47135(14) 0.0491(8) Uani 1 1 d . . . . .
H23A H 0.1748 0.3440 0.4522 0.074 Uiso 1 1 d R . . . .
H23B H 0.2121 0.3475 0.4971 0.074 Uiso 1 1 d R . . . .
O24 O 0.52012(18) 0.20853(17) 0.57802(17) 0.0486(8) Uani 1 1 d . . . . .
H24A H 0.5422 0.2435 0.5773 0.073 Uiso 1 1 d G . . . .
H24B H 0.5454 0.1762 0.5824 0.073 Uiso 1 1 d G . . . .
O25 O 0.4608(2) 0.6564(2) 0.76680(18) 0.0528(10) Uani 1 1 d . . . . .
H25A H 0.439(3) 0.630(3) 0.775(2) 0.045(17) Uiso 1 1 d . . . . .
H25B H 0.449(3) 0.692(4) 0.779(3) 0.07(2) Uiso 1 1 d . . . . .
O26 O 0.6892(2) 0.75895(19) 0.42893(16) 0.0519(9) Uani 1 1 d . . . . .
H26A H 0.7118 0.7287 0.4141 0.078 Uiso 1 1 d G . . . .
H26B H 0.7068 0.7957 0.4217 0.078 Uiso 1 1 d G . . . .
O27 O 0.7259(2) 0.3184(2) 0.29516(18) 0.0647(11) Uani 1 1 d . . . . .
H27A H 0.7315 0.3500 0.3182 0.097 Uiso 1 1 d G . . . .
H27B H 0.7085 0.3323 0.2645 0.097 Uiso 1 1 d G . . . .
O28 O 0.3900(2) 0.72335(18) 0.2923(2) 0.0650(11) Uani 1 1 d . . . . .
H28A H 0.3793 0.7046 0.2612 0.098 Uiso 1 1 d G . . . .
H28B H 0.4009 0.6947 0.3168 0.098 Uiso 1 1 d G . . . .
O29 O 0.20673(17) 0.3107(2) 0.32293(17) 0.0610(10) Uani 1 1 d . . . . .
H29A H 0.1856 0.3411 0.3392 0.091 Uiso 1 1 d R . . . .
H29B H 0.1945 0.2771 0.3485 0.091 Uiso 1 1 d R . . . .
O31 O 0.37331(14) 0.36058(14) 0.24091(12) 0.0320(6) Uani 1 1 d . . . . .
H31A H 0.3438 0.3868 0.2298 0.048 Uiso 1 1 d G . . . .
H31B H 0.3822 0.3339 0.2143 0.048 Uiso 1 1 d G . . . .


_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
C1 C3 1.483(5) . ?
C1 O1 1.245(5) . ?
C1 O2 1.266(5) . ?
C2 C4 1.476(5) . ?
C2 O3 1.302(5) . ?
C2 O4 1.224(5) . ?
C3 C4 1.378(5) . ?
C3 N1 1.367(4) . ?
C4 N2 1.367(5) . ?
C5 C6 1.465(5) . ?
C5 N1 1.355(4) . ?
C5 N2 1.332(5) . ?
C6 C7 1.395(5) . ?
C6 C11 1.395(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.378(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.375(6) . ?
C8 F1 1.343(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.379(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.379(5) . ?
C10 F1A 1.313(18) . ?
C11 H11 0.9300 . ?
C12 C14 1.477(5) . ?
C12 O5 1.261(5) . ?
C12 O6 1.256(4) . ?
C13 C15 1.472(5) . ?
C13 O7 1.301(5) . ?
C13 O8 1.236(5) . ?
C14 C15 1.385(5) . ?
C14 N3 1.365(4) . ?
C15 N4 1.375(4) . ?
C16 C17 1.465(5) . ?
C16 N3 1.365(5) . ?
C16 N4 1.331(5) . ?
C17 C18 1.385(6) . ?
C17 C22 1.385(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.371(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.369(8) . ?
C19 F2 1.294(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.371(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.379(6) . ?
C21 F2A 1.295(10) . ?
C22 H22 0.9300 . ?
Dy1 O1 2.341(3) . ?
Dy1 O5 2.371(3) . ?
Dy1 O13 2.363(3) . ?
Dy1 O14 2.411(3) . ?
Dy1 O15 2.345(3) . ?
Dy1 O16 2.418(3) . ?
Dy1 O17 2.383(3) . ?
Dy1 O18 2.348(3) . ?
N1 H1 0.8600 . ?
N3 H3 0.85(5) . ?
O3 H3A 0.8200 . ?
O7 H7A 0.91(2) . ?
O13 H13A 0.8714 . ?
O13 H13B 0.9801 . ?
O14 H14A 0.8646 . ?
O14 H14B 0.8641 . ?
O15 H15A 0.8452 . ?
O15 H15B 0.9028 . ?
O16 H16A 0.8772 . ?
O16 H16B 0.8737 . ?
O17 H17A 0.8727 . ?
O17 H17B 0.8718 . ?
O18 H18A 0.8787 . ?
O18 H18B 0.8797 . ?
O30 H30A 0.8499 . ?
O30 H30B 0.8499 . ?
C23 C25 1.482(5) . ?
C23 O9 1.214(5) . ?
C23 O10 1.307(5) . ?
C24 C26 1.495(5) . ?
C24 O11 1.265(5) . ?
C24 O12 1.243(6) . ?
C25 C26 1.380(5) . ?
C25 N5 1.379(5) . ?
C26 N6 1.361(5) . ?
C27 C28 1.467(5) . ?
C27 N5 1.332(5) . ?
C27 N6 1.352(5) . ?
C28 C29 1.390(6) . ?
C28 C33 1.389(6) . ?
C29 H29 0.9300 . ?
C29 C30 1.376(6) . ?
C30 H30 0.9300 . ?
C30 C31 1.371(8) . ?
C30 F3 1.318(8) . ?
C31 H31 0.9300 . ?
C31 C32 1.366(8) . ?
C32 H32 0.9300 . ?
C32 C33 1.386(6) . ?
C32 F3A 1.295(9) . ?
C33 H33 0.9300 . ?
N6 H6 0.8600 . ?
O10 H10A 0.8200 . ?
O19 H19A 0.8499 . ?
O19 H19B 0.8495 . ?
O20 H20A 0.80(6) . ?
O20 H20B 0.85(6) . ?
O21 H21A 0.8478 . ?
O21 H21B 0.8480 . ?
O22 H22A 0.8488 . ?
O22 H22B 0.8505 . ?
O23 H23A 0.8485 . ?
O23 H23B 0.8720 . ?
O24 H24A 0.8496 . ?
O24 H24B 0.8493 . ?
O25 H25A 0.73(6) . ?
O25 H25B 0.83(8) . ?
O26 H26A 0.8500 . ?
O26 H26B 0.8521 . ?
O27 H27A 0.8506 . ?
O27 H27B 0.8488 . ?
O28 H28A 0.8504 . ?
O28 H28B 0.8508 . ?
O29 H29A 0.8502 . ?
O29 H29B 0.9452 . ?
O31 H31A 0.8503 . ?
O31 H31B 0.8480 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C3 117.0(3) . . ?
O1 C1 O2 125.1(4) . . ?
O2 C1 C3 117.9(3) . . ?
O3 C2 C4 118.9(3) . . ?
O4 C2 C4 120.4(4) . . ?
O4 C2 O3 120.7(4) . . ?
C4 C3 C1 133.7(3) . . ?
N1 C3 C1 121.0(3) . . ?
N1 C3 C4 105.3(3) . . ?
C3 C4 C2 130.6(3) . . ?
N2 C4 C2 119.3(3) . . ?
N2 C4 C3 110.1(3) . . ?
N1 C5 C6 124.7(3) . . ?
N2 C5 C6 124.8(3) . . ?
N2 C5 N1 110.6(3) . . ?
C7 C6 C5 121.2(3) . . ?
C11 C6 C5 119.4(3) . . ?
C11 C6 C7 119.4(3) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 C6 118.2(4) . . ?
C8 C7 H7 120.9 . . ?
C7 C8 H8 118.3 . . ?
C9 C8 C7 123.4(4) . . ?
C9 C8 H8 118.3 . . ?
F1 C8 C7 118.8(4) . . ?
F1 C8 C9 117.8(4) . . ?
C8 C9 H9 121.2 . . ?
C8 C9 C10 117.5(4) . . ?
C10 C9 H9 121.2 . . ?
C9 C10 H10 119.3 . . ?
C11 C10 C9 121.3(4) . . ?
C11 C10 H10 119.3 . . ?
F1A C10 C9 111.8(14) . . ?
F1A C10 C11 126.5(14) . . ?
C6 C11 H11 119.9 . . ?
C10 C11 C6 120.1(4) . . ?
C10 C11 H11 119.9 . . ?
O5 C12 C14 117.0(3) . . ?
O6 C12 C14 117.6(3) . . ?
O6 C12 O5 125.4(4) . . ?
O7 C13 C15 119.1(3) . . ?
O8 C13 C15 120.8(4) . . ?
O8 C13 O7 120.0(4) . . ?
C15 C14 C12 132.9(3) . . ?
N3 C14 C12 122.0(3) . . ?
N3 C14 C15 105.1(3) . . ?
C14 C15 C13 130.3(3) . . ?
N4 C15 C13 119.4(3) . . ?
N4 C15 C14 110.3(3) . . ?
N3 C16 C17 124.0(3) . . ?
N4 C16 C17 125.3(3) . . ?
N4 C16 N3 110.7(3) . . ?
C18 C17 C16 120.9(4) . . ?
C22 C17 C16 119.9(4) . . ?
C22 C17 C18 119.2(4) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 C17 119.3(4) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 118.6 . . ?
C20 C19 C18 122.8(5) . . ?
C20 C19 H19 118.6 . . ?
F2 C19 C18 119.9(5) . . ?
F2 C19 C20 117.2(5) . . ?
C19 C20 H20 121.5 . . ?
C19 C20 C21 116.9(4) . . ?
C21 C20 H20 121.5 . . ?
C20 C21 H21 118.8 . . ?
C20 C21 C22 122.4(5) . . ?
C22 C21 H21 118.8 . . ?
F2A C21 C20 115.5(6) . . ?
F2A C21 C22 121.9(7) . . ?
C17 C22 H22 120.4 . . ?
C21 C22 C17 119.3(5) . . ?
C21 C22 H22 120.4 . . ?
O1 Dy1 O5 139.86(10) . . ?
O1 Dy1 O13 73.16(10) . . ?
O1 Dy1 O14 73.44(10) . . ?
O1 Dy1 O15 104.28(11) . . ?
O1 Dy1 O16 74.28(10) . . ?
O1 Dy1 O17 144.17(10) . . ?
O1 Dy1 O18 87.55(12) . . ?
O5 Dy1 O14 76.19(10) . . ?
O5 Dy1 O16 145.85(10) . . ?
O5 Dy1 O17 75.53(9) . . ?
O13 Dy1 O5 73.40(9) . . ?
O13 Dy1 O14 73.27(10) . . ?
O13 Dy1 O16 131.87(11) . . ?
O13 Dy1 O17 128.57(11) . . ?
O14 Dy1 O16 128.15(12) . . ?
O15 Dy1 O5 90.87(12) . . ?
O15 Dy1 O13 145.03(11) . . ?
O15 Dy1 O14 72.70(11) . . ?
O15 Dy1 O16 77.38(13) . . ?
O15 Dy1 O17 74.00(12) . . ?
O15 Dy1 O18 144.57(12) . . ?
O17 Dy1 O14 135.41(11) . . ?
O17 Dy1 O16 70.43(10) . . ?
O18 Dy1 O5 101.37(12) . . ?
O18 Dy1 O13 70.23(11) . . ?
O18 Dy1 O14 142.40(11) . . ?
O18 Dy1 O16 73.92(13) . . ?
O18 Dy1 O17 77.10(12) . . ?
C3 N1 H1 125.9 . . ?
C5 N1 C3 108.2(3) . . ?
C5 N1 H1 125.9 . . ?
C5 N2 C4 105.9(3) . . ?
C14 N3 C16 108.4(3) . . ?
C14 N3 H3 125(3) . . ?
C16 N3 H3 127(3) . . ?
C16 N4 C15 105.6(3) . . ?
C1 O1 Dy1 144.8(3) . . ?
C2 O3 H3A 109.5 . . ?
C12 O5 Dy1 138.9(2) . . ?
C13 O7 H7A 113(4) . . ?
Dy1 O13 H13A 110.4 . . ?
Dy1 O13 H13B 101.6 . . ?
H13A O13 H13B 147.9 . . ?
Dy1 O14 H14A 110.3 . . ?
Dy1 O14 H14B 109.8 . . ?
H14A O14 H14B 103.7 . . ?
Dy1 O15 H15A 126.3 . . ?
Dy1 O15 H15B 111.7 . . ?
H15A O15 H15B 115.0 . . ?
Dy1 O16 H16A 111.3 . . ?
Dy1 O16 H16B 109.8 . . ?
H16A O16 H16B 107.9 . . ?
Dy1 O17 H17A 110.4 . . ?
Dy1 O17 H17B 110.4 . . ?
H17A O17 H17B 108.2 . . ?
Dy1 O18 H18A 111.0 . . ?
Dy1 O18 H18B 110.7 . . ?
H18A O18 H18B 107.8 . . ?
H30A O30 H30B 109.5 . . ?
O9 C23 C25 120.7(4) . . ?
O9 C23 O10 121.6(4) . . ?
O10 C23 C25 117.7(4) . . ?
O11 C24 C26 117.1(4) . . ?
O12 C24 C26 116.8(4) . . ?
O12 C24 O11 126.1(4) . . ?
C26 C25 C23 131.0(3) . . ?
N5 C25 C23 119.1(3) . . ?
N5 C25 C26 109.8(3) . . ?
C25 C26 C24 133.5(4) . . ?
N6 C26 C24 120.8(4) . . ?
N6 C26 C25 105.6(3) . . ?
N5 C27 C28 125.2(3) . . ?
N5 C27 N6 111.2(3) . . ?
N6 C27 C28 123.6(3) . . ?
C29 C28 C27 121.2(4) . . ?
C33 C28 C27 119.7(4) . . ?
C33 C28 C29 119.1(4) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 C28 119.5(5) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 H30 118.8 . . ?
C31 C30 C29 122.4(5) . . ?
C31 C30 H30 118.8 . . ?
F3 C30 C29 119.5(6) . . ?
F3 C30 C31 118.0(5) . . ?
C30 C31 H31 121.2 . . ?
C32 C31 C30 117.5(4) . . ?
C32 C31 H31 121.2 . . ?
C31 C32 H32 118.8 . . ?
C31 C32 C33 122.4(5) . . ?
C33 C32 H32 118.8 . . ?
F3A C32 C31 118.5(6) . . ?
F3A C32 C33 119.0(6) . . ?
C28 C33 H33 120.5 . . ?
C32 C33 C28 119.1(5) . . ?
C32 C33 H33 120.5 . . ?
C27 N5 C25 105.2(3) . . ?
C26 N6 H6 125.9 . . ?
C27 N6 C26 108.2(3) . . ?
C27 N6 H6 125.9 . . ?
C23 O10 H10A 109.5 . . ?
H19A O19 H19B 109.5 . . ?
H20A O20 H20B 104(5) . . ?
H21A O21 H21B 109.7 . . ?
H22A O22 H22B 109.6 . . ?
H23A O23 H23B 98.2 . . ?
H24A O24 H24B 109.5 . . ?
H25A O25 H25B 113(6) . . ?
H26A O26 H26B 109.5 . . ?
H27A O27 H27B 109.5 . . ?
H28A O28 H28B 109.4 . . ?
H29A O29 H29B 96.7 . . ?
H31A O31 H31B 109.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O31 0.86 2.16 2.897(4) 143.5 5_666
N3 H3 O20 0.85(5) 2.09(5) 2.854(4) 148(4) .
O3 H3A O2 0.82 1.70 2.512(4) 172.6 .
O7 H7A O6 0.91(2) 1.57(2) 2.472(4) 173(6) .
O13 H13A O25 0.87 2.18 2.826(5) 130.7 .
O13 H13B O20 0.98 1.84 2.659(4) 139.0 .
O14 H14A O29 0.86 2.17 2.731(5) 122.6 5_666
O14 H14B O31 0.86 1.92 2.766(4) 166.7 5_666
O15 H15A O23 0.85 2.18 2.793(5) 129.7 5_666
O15 H15B O26 0.90 1.93 2.765(5) 153.2 .
O16 H16B F2 0.87 2.15 2.793(7) 130.2 8_575
O17 H17A O24 0.87 2.00 2.785(5) 149.9 5_666
O18 H18A O19 0.88 1.97 2.753(5) 147.4 .
O18 H18B O30 0.88 2.14 2.723(5) 123.1 .
O30 H30B F2A 0.85 2.27 2.874(10) 128.3 4_646
N6 H6 O22 0.86 2.11 2.884(5) 149.9 2_564
O10 H10A O11 0.82 1.67 2.492(5) 179.0 .
O19 H19A O27 0.85 1.95 2.727(5) 152.1 5_666
O19 H19B O12 0.85 1.94 2.765(5) 163.0 8_576
O20 H20A O21 0.80(6) 1.96(6) 2.737(5) 167(6) 4_656
O20 H20B N2 0.85(6) 2.08(6) 2.893(4) 160(5) 4_656
O21 H21A O24 0.85 2.03 2.850(6) 163.6 .
O21 H21B O26 0.85 2.00 2.843(6) 177.8 5_666
O23 H23A O8 0.85 2.07 2.889(4) 163.7 3_466
O23 H23B O11 0.87 1.94 2.791(4) 166.7 2_565
O26 H26A O12 0.85 1.98 2.821(5) 172.6 6_656
O26 H26B O9 0.85 2.07 2.843(5) 150.7 4_655
O27 H27A O9 0.85 2.05 2.778(5) 142.6 6_656
O27 H27B O29 0.85 2.09 2.790(6) 139.3 6_656
O28 H28A O19 0.85 2.22 2.879(7) 134.3 8_575
O29 H29A O8 0.85 1.97 2.787(5) 160.3 3_466
O31 H31B O21 0.85 2.01 2.858(5) 174.5 8_565

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
C1 C3 C4 C2 2.6(7) . . . . ?
C1 C3 C4 N2 -178.9(4) . . . . ?
C1 C3 N1 C5 179.1(3) . . . . ?
C2 C4 N2 C5 178.6(4) . . . . ?
C3 C1 O1 Dy1 178.0(3) . . . . ?
C3 C4 N2 C5 0.0(4) . . . . ?
C4 C3 N1 C5 0.1(4) . . . . ?
C5 C6 C7 C8 -179.6(4) . . . . ?
C5 C6 C11 C10 179.6(4) . . . . ?
C6 C5 N1 C3 180.0(3) . . . . ?
C6 C5 N2 C4 180.0(3) . . . . ?
C6 C7 C8 C9 0.5(7) . . . . ?
C6 C7 C8 F1 -179.8(4) . . . . ?
C7 C6 C11 C10 -0.6(6) . . . . ?
C7 C8 C9 C10 -1.4(7) . . . . ?
C8 C9 C10 C11 1.3(7) . . . . ?
C8 C9 C10 F1A 175(2) . . . . ?
C9 C10 C11 C6 -0.4(7) . . . . ?
C11 C6 C7 C8 0.6(6) . . . . ?
C12 C14 C15 C13 -0.6(7) . . . . ?
C12 C14 C15 N4 178.1(4) . . . . ?
C12 C14 N3 C16 -178.5(3) . . . . ?
C13 C15 N4 C16 179.1(3) . . . . ?
C14 C12 O5 Dy1 169.9(3) . . . . ?
C14 C15 N4 C16 0.3(4) . . . . ?
C15 C14 N3 C16 0.0(4) . . . . ?
C16 C17 C18 C19 -179.3(4) . . . . ?
C16 C17 C22 C21 -179.8(4) . . . . ?
C17 C16 N3 C14 -179.1(3) . . . . ?
C17 C16 N4 C15 179.0(3) . . . . ?
C17 C18 C19 C20 -1.2(7) . . . . ?
C17 C18 C19 F2 -178.3(5) . . . . ?
C18 C17 C22 C21 -0.4(7) . . . . ?
C18 C19 C20 C21 0.1(8) . . . . ?
C19 C20 C21 C22 0.8(9) . . . . ?
C19 C20 C21 F2A -174.7(7) . . . . ?
C20 C21 C22 C17 -0.7(9) . . . . ?
C22 C17 C18 C19 1.3(6) . . . . ?
F1 C8 C9 C10 178.9(4) . . . . ?
F1A C10 C11 C6 -173(2) . . . . ?
F2 C19 C20 C21 177.4(6) . . . . ?
F2A C21 C22 C17 174.6(7) . . . . ?
N1 C3 C4 C2 -178.5(4) . . . . ?
N1 C3 C4 N2 0.0(4) . . . . ?
N1 C5 C6 C7 10.1(6) . . . . ?
N1 C5 C6 C11 -170.1(4) . . . . ?
N1 C5 N2 C4 0.0(4) . . . . ?
N2 C5 C6 C7 -169.9(4) . . . . ?
N2 C5 C6 C11 10.0(6) . . . . ?
N2 C5 N1 C3 -0.1(4) . . . . ?
N3 C14 C15 C13 -178.9(4) . . . . ?
N3 C14 C15 N4 -0.2(4) . . . . ?
N3 C16 C17 C18 7.9(6) . . . . ?
N3 C16 C17 C22 -172.7(4) . . . . ?
N3 C16 N4 C15 -0.2(4) . . . . ?
N4 C16 C17 C18 -171.2(4) . . . . ?
N4 C16 C17 C22 8.2(6) . . . . ?
N4 C16 N3 C14 0.1(4) . . . . ?
O1 C1 C3 C4 -178.8(4) . . . . ?
O1 C1 C3 N1 2.5(6) . . . . ?
O2 C1 C3 C4 0.6(7) . . . . ?
O2 C1 C3 N1 -178.1(4) . . . . ?
O2 C1 O1 Dy1 -1.4(8) . . . . ?
O3 C2 C4 C3 -2.6(7) . . . . ?
O3 C2 C4 N2 179.1(4) . . . . ?
O4 C2 C4 C3 175.9(4) . . . . ?
O4 C2 C4 N2 -2.4(6) . . . . ?
O5 C12 C14 C15 -174.2(4) . . . . ?
O5 C12 C14 N3 3.7(5) . . . . ?
O6 C12 C14 C15 5.2(6) . . . . ?
O6 C12 C14 N3 -176.8(3) . . . . ?
O6 C12 O5 Dy1 -9.5(7) . . . . ?
O7 C13 C15 C14 -3.5(6) . . . . ?
O7 C13 C15 N4 178.0(3) . . . . ?
O8 C13 C15 C14 177.7(4) . . . . ?
O8 C13 C15 N4 -0.9(6) . . . . ?
C23 C25 C26 C24 -5.2(8) . . . . ?
C23 C25 C26 N6 176.6(4) . . . . ?
C23 C25 N5 C27 -176.9(4) . . . . ?
C24 C26 N6 C27 -178.2(3) . . . . ?
C25 C26 N6 C27 0.2(4) . . . . ?
C26 C25 N5 C27 0.6(4) . . . . ?
C27 C28 C29 C30 178.9(4) . . . . ?
C27 C28 C33 C32 -179.3(4) . . . . ?
C28 C27 N5 C25 -179.3(4) . . . . ?
C28 C27 N6 C26 179.1(3) . . . . ?
C28 C29 C30 C31 1.4(8) . . . . ?
C28 C29 C30 F3 177.1(6) . . . . ?
C29 C28 C33 C32 1.5(6) . . . . ?
C29 C30 C31 C32 -0.4(8) . . . . ?
C30 C31 C32 C33 0.0(8) . . . . ?
C30 C31 C32 F3A 177.3(7) . . . . ?
C31 C32 C33 C28 -0.6(8) . . . . ?
C33 C28 C29 C30 -1.9(7) . . . . ?
F3 C30 C31 C32 -176.2(6) . . . . ?
F3A C32 C33 C28 -177.9(6) . . . . ?
N5 C25 C26 C24 177.6(4) . . . . ?
N5 C25 C26 N6 -0.5(4) . . . . ?
N5 C27 C28 C29 172.2(4) . . . . ?
N5 C27 C28 C33 -7.0(6) . . . . ?
N5 C27 N6 C26 0.2(4) . . . . ?
N6 C27 C28 C29 -6.5(6) . . . . ?
N6 C27 C28 C33 174.3(4) . . . . ?
N6 C27 N5 C25 -0.5(4) . . . . ?
O9 C23 C25 C26 -173.6(4) . . . . ?
O9 C23 C25 N5 3.3(6) . . . . ?
O10 C23 C25 C26 6.2(7) . . . . ?
O10 C23 C25 N5 -176.9(4) . . . . ?
O11 C24 C26 C25 3.0(7) . . . . ?
O11 C24 C26 N6 -179.1(4) . . . . ?
O12 C24 C26 C25 -177.2(4) . . . . ?
O12 C24 C26 N6 0.7(6) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -7 -13 0.0312 -1.4369 -6.6114 -13.0570 0.1822 -0.9823 0.0436
13 -1 -2 0.1560 13.1378 -1.4956 -1.9168 0.0192 -0.1020 -0.9946
1 7 13 0.0175 1.1538 6.6333 13.0782 -0.1823 0.9830 -0.0223
-13 0 1 0.1540 -13.2971 -0.0251 1.1062 0.0707 0.0129 0.9974
0 -12 8 0.0311 -0.3350 -11.5218 7.5974 0.9832 0.1824 -0.0089
-1 12 -8 0.0559 -0.8355 11.5389 -7.5128 -0.9786 -0.1815 0.0967

_olex2_date_sample_data_collection 2018-07-12
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_201807325
_database_code_depnum_ccdc_archive 'CCDC 1893411'
loop_
_audit_author_name
_audit_author_address
a
;none
China
;
_audit_update_record             
;
2019-01-25 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_audit_creation_date             2018-07-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H24 Eu F2 N4 O14, C11 H6 F N2 O4, 6(H2 O)'
_chemical_formula_sum            'C33 H42 Eu F3 N6 O24'
_chemical_formula_weight         1115.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         C33H33O24N6Eu1F3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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                   11.4389(5)
_cell_length_b                   12.4406(4)
_cell_length_c                   16.1101(7)
_cell_angle_alpha                96.834(3)
_cell_angle_beta                 108.861(4)
_cell_angle_gamma                96.387(3)
_cell_volume                     2126.54(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6662
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7330
_cell_measurement_theta_min      4.1450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.551
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.3202
_exptl_crystal_size_mid          0.1558
_exptl_crystal_size_min          0.0366
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15140
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.063
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         3.625
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -105.00   38.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000    0.0000  -30.0000 143

#__ type_ start__ end____ width___ exp.time_
  2 omega  -45.00   25.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000   90.0000 70

#__ type_ start__ end____ width___ exp.time_
  3 omega   21.00   60.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000  150.0000 39

#__ type_ start__ end____ width___ exp.time_
  4 omega   -4.00   41.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -180.0000 45

#__ type_ start__ end____ width___ exp.time_
  5 omega   11.00  101.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  -30.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega   57.00   97.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000    0.0000 40

#__ type_ start__ end____ width___ exp.time_
  7 omega   42.00   76.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -90.0000 34

#__ type_ start__ end____ width___ exp.time_
  8 omega   14.00   46.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  150.0000 32

#__ type_ start__ end____ width___ exp.time_
  9 omega    4.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   19.0000  150.0000 29

#__ type_ start__ end____ width___ exp.time_
 10 omega   68.00  108.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   90.0000 40

#__ type_ start__ end____ width___ exp.time_
 11 omega   47.00   77.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000   90.0000 30

#__ type_ start__ end____ width___ exp.time_
 12 omega   44.00  107.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734 -157.0000  -87.0000 63

#__ type_ start__ end____ width___ exp.time_
 13 omega   63.00  105.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   19.0000  150.0000 42

#__ type_ start__ end____ width___ exp.time_
 14 omega   77.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -30.0000 32

#__ type_ start__ end____ width___ exp.time_
 15 omega   23.00   59.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
 16 omega   57.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 51

#__ type_ start__ end____ width___ exp.time_
 17 omega   63.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 115

#__ type_ start__ end____ width___ exp.time_
 18 omega   38.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

#__ type_ start__ end____ width___ exp.time_
 19 omega   83.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 20 omega   42.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 54

#__ type_ start__ end____ width___ exp.time_
 21 omega   42.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 46

#__ type_ start__ end____ width___ exp.time_
 22 omega   42.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 23 omega   59.00  125.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  120.0000 66

#__ type_ start__ end____ width___ exp.time_
 24 omega   38.00   93.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 55

#__ type_ start__ end____ width___ exp.time_
 25 omega   45.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 41

#__ type_ start__ end____ width___ exp.time_
 26 omega  121.00  154.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 33

#__ type_ start__ end____ width___ exp.time_
 27 omega   38.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 61

#__ type_ start__ end____ width___ exp.time_
 28 omega   56.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
 29 omega   43.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 65

#__ type_ start__ end____ width___ exp.time_
 30 omega  111.00  137.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 31 omega   38.00   64.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 32 omega   83.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 33 omega  118.00  146.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 28

#__ type_ start__ end____ width___ exp.time_
 34 omega   44.00  114.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1441210000
_diffrn_orient_matrix_UB_12      -0.0228738000
_diffrn_orient_matrix_UB_13      -0.0359701000
_diffrn_orient_matrix_UB_21      -0.0019804000
_diffrn_orient_matrix_UB_22      0.0324811000
_diffrn_orient_matrix_UB_23      0.0947907000
_diffrn_orient_matrix_UB_31      -0.0027560000
_diffrn_orient_matrix_UB_32      0.1199241000
_diffrn_orient_matrix_UB_33      -0.0147517000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6666
_reflns_number_total             7583
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         7583
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0730P)²+0.3101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1287
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H10A-O10
 0.9 with sigma of 0.02
 F2A-C21
 1.35 with sigma of 0.02
 C8-F1
 1.35 with sigma of 0.02
 C10-F1A
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(O23) = Uanis(O23A)
Uanis(O20) = Uanis(O20A)
4. Others
 Sof(H8)=Sof(F1A)=1-FVAR(1)
 Sof(H10)=Sof(F1)=FVAR(1)
 Sof(H19)=Sof(F2A)=1-FVAR(2)
 Sof(H21)=Sof(F2)=FVAR(2)
 Sof(O23A)=Sof(H23C)=Sof(H23D)=1-FVAR(3)
 Sof(O23)=Sof(H23A)=Sof(H23B)=FVAR(3)
 Sof(O20A)=Sof(H20C)=Sof(H20D)=1-FVAR(4)
 Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(4)
5.a Riding coordinates:
 O15(H15A,H15B), O16(H16A,H16B), O19(H19A,H19B), O20A(H20C,H20D), O22(H22A,
 H22B), O23(H23A,H23B), O24(H24A,H24B)
5.b Free rotating group:
 O20(H20A,H20B), O21(H21A,H21B), O23A(H23C,H23D)
5.c Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O18(H18A,H18B)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), N1(H1), N4(H4), C29(H29), C31(H31), C32(H32), C33(H33),
 N6(H6)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C 0.2528(5) 0.1048(4) 0.0694(4) 0.0407(11) Uani 1 1 d . . . . .
C2 C 0.2301(5) -0.1414(4) -0.0485(4) 0.0445(12) Uani 1 1 d . . . . .
C3 C 0.3445(5) 0.0280(4) 0.0728(3) 0.0371(11) Uani 1 1 d . . . . .
C4 C 0.3371(5) -0.0714(4) 0.0238(3) 0.0381(11) Uani 1 1 d . . . . .
C5 C 0.5253(5) -0.0287(4) 0.1169(4) 0.0403(11) Uani 1 1 d . . . . .
C6 C 0.6562(5) -0.0318(5) 0.1667(4) 0.0417(12) Uani 1 1 d . . . . .
C7 C 0.7287(6) 0.0529(6) 0.2330(5) 0.0609(16) Uani 1 1 d . . . . .
H7 H 0.6946 0.1138 0.2475 0.073 Uiso 1 1 calc R . . . .
C8 C 0.8511(6) 0.0465(7) 0.2773(5) 0.075(2) Uani 1 1 d D . . . .
H8 H 0.8982 0.1040 0.3222 0.090 Uiso 0.308(8) 1 calc R . P A 2
C9 C 0.9075(6) -0.0391(7) 0.2592(5) 0.071(2) Uani 1 1 d . . . . .
H9 H 0.9910 -0.0414 0.2904 0.085 Uiso 1 1 calc R . . . .
C10 C 0.8356(7) -0.1218(6) 0.1928(6) 0.072(2) Uani 1 1 d D . . . .
H10 H 0.8720 -0.1811 0.1781 0.086 Uiso 0.692(8) 1 calc R . P A 1
C11 C 0.7114(6) -0.1210(5) 0.1467(5) 0.0568(15) Uani 1 1 d . . . . .
H11 H 0.6649 -0.1795 0.1026 0.068 Uiso 1 1 calc R . . . .
C12 C 0.2272(5) 0.6002(4) 0.2927(3) 0.0399(11) Uani 1 1 d . . . . .
C13 C 0.3102(5) 0.8027(5) 0.4663(4) 0.0494(14) Uani 1 1 d . . . . .
C14 C 0.3462(5) 0.6313(4) 0.3699(3) 0.0372(11) Uani 1 1 d . . . . .
C15 C 0.3782(5) 0.7179(4) 0.4384(3) 0.0391(11) Uani 1 1 d . . . . .
C16 C 0.5334(5) 0.6251(4) 0.4528(3) 0.0374(11) Uani 1 1 d . . . . .
C17 C 0.6565(5) 0.5920(5) 0.4897(4) 0.0419(12) Uani 1 1 d . . . . .
C18 C 0.6818(5) 0.4965(5) 0.4488(4) 0.0501(13) Uani 1 1 d . . . . .
H18 H 0.6218 0.4549 0.3980 0.060 Uiso 1 1 calc R . . . .
C19 C 0.7956(6) 0.4646(5) 0.4842(5) 0.0575(15) Uani 1 1 d . . . . .
H19 H 0.8115 0.4010 0.4561 0.069 Uiso 0.110(8) 1 calc R . P B 2
C20 C 0.8869(6) 0.5215(6) 0.5587(5) 0.0600(16) Uani 1 1 d . . . . .
H20 H 0.9630 0.4970 0.5819 0.072 Uiso 1 1 calc R . . . .
C21 C 0.8626(6) 0.6161(6) 0.5984(4) 0.0596(16) Uani 1 1 d D . . . .
H21 H 0.9237 0.6568 0.6491 0.072 Uiso 0.890(8) 1 calc R . P B 1
C22 C 0.7496(5) 0.6523(5) 0.5648(4) 0.0512(14) Uani 1 1 d . . . . .
H22 H 0.7357 0.7172 0.5924 0.061 Uiso 1 1 calc R . . . .
Eu1 Eu 0.18904(2) 0.35521(2) 0.14279(2) 0.03367(11) Uani 1 1 d . . . . .
F1 F 0.9186(7) 0.1264(7) 0.3403(6) 0.116(3) Uani 0.692(8) 1 d D . P A 1
F1A F 0.8904(14) -0.2071(14) 0.1886(13) 0.116(3) Uani 0.308(8) 1 d D . P A 2
F2 F 0.8177(5) 0.3705(4) 0.4473(4) 0.0867(17) Uani 0.890(8) 1 d . . P B 1
F2A F 0.965(2) 0.673(3) 0.659(3) 0.0867(17) Uani 0.110(8) 1 d D . P B 2
N1 N 0.4636(4) 0.0545(4) 0.1312(3) 0.0381(9) Uani 1 1 d . . . . .
H1 H 0.4940 0.1132 0.1701 0.046 Uiso 1 1 calc R . . . .
N2 N 0.4501(4) -0.1065(3) 0.0511(3) 0.0402(9) Uani 1 1 d . . . . .
N3 N 0.4421(4) 0.5729(3) 0.3795(3) 0.0360(9) Uani 1 1 d . . . . .
N4 N 0.4969(4) 0.7124(4) 0.4903(3) 0.0410(10) Uani 1 1 d . . . . .
H4 H 0.5409 0.7566 0.5383 0.049 Uiso 1 1 calc R . . . .
O1 O 0.2889(3) 0.1970(3) 0.1166(3) 0.0473(9) Uani 1 1 d . . . . .
O2 O 0.1411(3) 0.0714(3) 0.0161(3) 0.0533(10) Uani 1 1 d . . . . .
O3 O 0.1236(4) -0.1071(3) -0.0715(3) 0.0531(10) Uani 1 1 d . . . . .
H3 H 0.1297 -0.0479 -0.0408 0.080 Uiso 1 1 calc GR . . . .
O4 O 0.2428(4) -0.2296(3) -0.0848(3) 0.0615(12) Uani 1 1 d . . . . .
O5 O 0.2174(4) 0.5168(3) 0.2378(2) 0.0496(9) Uani 1 1 d . . . . .
O6 O 0.1433(4) 0.6590(3) 0.2862(3) 0.0499(9) Uani 1 1 d . . . . .
O7 O 0.2019(4) 0.8123(4) 0.4118(3) 0.0598(11) Uani 1 1 d . . . . .
H7A H 0.1833 0.7661 0.3669 0.090 Uiso 1 1 calc GR . . . .
O8 O 0.3572(4) 0.8588(4) 0.5409(3) 0.0718(15) Uani 1 1 d . . . . .
O13 O 0.0628(4) 0.2651(4) -0.0031(3) 0.0612(12) Uani 1 1 d . . . . .
H13A H -0.0176 0.2666 -0.0126 0.092 Uiso 1 1 d GR . . . .
H13B H 0.0664 0.1940 -0.0093 0.092 Uiso 1 1 d GR . . . .
O14 O -0.0206(4) 0.3770(4) 0.1388(4) 0.0666(13) Uani 1 1 d . . . . .
H14A H -0.0754 0.3334 0.0940 0.100 Uiso 1 1 d GR . . . .
H14B H -0.0348 0.4417 0.1280 0.100 Uiso 1 1 d GR . . . .
O15 O 0.1326(4) 0.4975(3) 0.0494(3) 0.0535(10) Uani 1 1 d . . . . .
H15A H 0.1055 0.5052 -0.0039 0.080 Uiso 1 1 d R . . . .
H15B H 0.1673 0.5633 0.0801 0.080 Uiso 1 1 d R . . . .
O16 O 0.1021(4) 0.2115(3) 0.2041(3) 0.0492(9) Uani 1 1 d . . . . .
H16A H 0.0349 0.1859 0.1477 0.074 Uiso 1 1 d R . . . .
H16B H 0.1498 0.1614 0.2125 0.074 Uiso 1 1 d R . . . .
O17 O 0.3664(4) 0.3576(4) 0.2731(3) 0.0597(11) Uani 1 1 d . . . . .
H17A H 0.4158 0.4206 0.2868 0.090 Uiso 1 1 d GR . . . .
H17B H 0.4130 0.3109 0.2623 0.090 Uiso 1 1 d GR . . . .
O18 O 0.3541(5) 0.4109(4) 0.0889(4) 0.0765(15) Uani 1 1 d . . . . .
H18A H 0.3250 0.4257 0.0323 0.115 Uiso 1 1 d GR . . . .
H18B H 0.3976 0.3553 0.0820 0.115 Uiso 1 1 d GR . . . .
C23 C 0.6877(5) -0.0367(5) 0.6914(4) 0.0501(14) Uani 1 1 d . . . . .
C24 C 0.7721(7) 0.1947(5) 0.8397(4) 0.0585(17) Uani 1 1 d . . . . .
C25 C 0.6209(5) 0.0566(4) 0.7049(4) 0.0412(11) Uani 1 1 d . . . . .
C26 C 0.6502(5) 0.1512(4) 0.7646(4) 0.0421(12) Uani 1 1 d . . . . .
C27 C 0.4597(5) 0.1458(4) 0.6798(4) 0.0412(11) Uani 1 1 d . . . . .
C28 C 0.3340(6) 0.1707(5) 0.6381(4) 0.0497(13) Uani 1 1 d . . . . .
C29 C 0.2968(8) 0.2612(6) 0.6731(5) 0.0676(19) Uani 1 1 d . . . . .
H29 H 0.3523 0.3084 0.7228 0.081 Uiso 1 1 calc R . . . .
C30 C 0.1784(10) 0.2818(9) 0.6349(7) 0.090(3) Uani 1 1 d . . . . .
C31 C 0.0931(9) 0.2150(10) 0.5622(8) 0.104(4) Uani 1 1 d . . . . .
H31 H 0.0127 0.2308 0.5375 0.124 Uiso 1 1 calc R . . . .
C32 C 0.1285(8) 0.1245(8) 0.5265(7) 0.094(3) Uani 1 1 d . . . . .
H32 H 0.0720 0.0778 0.4769 0.113 Uiso 1 1 calc R . . . .
C33 C 0.2490(7) 0.1023(7) 0.5643(6) 0.073(2) Uani 1 1 d . . . . .
H33 H 0.2728 0.0406 0.5397 0.087 Uiso 1 1 calc R . . . .
F3 F 0.1430(8) 0.3716(7) 0.6689(5) 0.155(3) Uani 1 1 d . . . . .
N5 N 0.5504(5) 0.2068(4) 0.7499(3) 0.0455(10) Uani 1 1 d . . . . .
N6 N 0.5014(4) 0.0547(4) 0.6521(3) 0.0409(10) Uani 1 1 d . . . . .
H6 H 0.4587 0.0041 0.6081 0.049 Uiso 1 1 calc R . . . .
O9 O 0.6349(5) -0.1128(4) 0.6317(4) 0.0854(18) Uani 1 1 d . . . . .
O10 O 0.7977(4) -0.0334(4) 0.7456(4) 0.0690(13) Uani 1 1 d D . . . .
H10A H 0.815(6) 0.029(3) 0.785(3) 0.046(17) Uiso 1 1 d D . . . .
O11 O 0.8604(5) 0.1388(4) 0.8493(3) 0.0765(15) Uani 1 1 d . . . . .
O12 O 0.7818(6) 0.2819(4) 0.8878(3) 0.0837(17) Uani 1 1 d . . . . .
O19 O 0.4726(7) 0.6223(5) 0.1235(6) 0.135(3) Uani 1 1 d . . . . .
H19A H 0.4563 0.6700 0.1588 0.202 Uiso 1 1 d R . . . .
H19B H 0.4081 0.6267 0.0683 0.202 Uiso 1 1 d R . . . .
O20 O 0.5237(8) 0.3161(8) 0.0339(7) 0.124(4) Uani 0.826(10) 1 d . . P C 1
H20A H 0.4842 0.3085 -0.0220 0.186 Uiso 0.826(10) 1 d G . P C 1
H20B H 0.6027 0.3195 0.0509 0.186 Uiso 0.826(10) 1 d G . P C 1
O20A O 0.594(4) 0.341(3) 0.144(4) 0.124(4) Uani 0.174(10) 1 d . . P C 2
H20C H 0.6291 0.4041 0.1413 0.186 Uiso 0.174(10) 1 d R . P C 2
H20D H 0.5537 0.3127 0.0907 0.186 Uiso 0.174(10) 1 d R . P C 2
O21 O 0.4458(5) 0.7665(4) 0.7112(4) 0.0706(13) Uani 1 1 d . . . . .
H21A H 0.4035 0.7212 0.7302 0.106 Uiso 1 1 d G . . . .
H21B H 0.4007 0.7653 0.6574 0.106 Uiso 1 1 d G . . . .
O22 O 0.9235(5) 0.5829(4) 0.1433(3) 0.0701(13) Uani 1 1 d . . . . .
H22A H 0.8855 0.6240 0.0993 0.105 Uiso 1 1 d R . . . .
H22B H 0.9613 0.6141 0.1968 0.105 Uiso 1 1 d R . . . .
O23 O 0.6915(15) 0.4971(15) 0.1602(13) 0.114(4) Uani 0.452(11) 1 d . . P D 1
H23A H 0.6727 0.5231 0.2046 0.170 Uiso 0.452(11) 1 d R . P D 1
H23B H 0.7600 0.5368 0.1659 0.170 Uiso 0.452(11) 1 d R . P D 1
O23A O 0.6725(13) 0.5541(13) 0.0987(11) 0.114(4) Uani 0.548(11) 1 d . . P D 2
H23C H 0.6178 0.5830 0.1151 0.170 Uiso 0.548(11) 1 d G . P D 2
H23D H 0.6472 0.4765 0.0761 0.170 Uiso 0.548(11) 1 d G . P D 2
O24 O 0.2510(15) 0.6504(12) 0.7477(10) 0.285(10) Uani 1 1 d . . . . .
H24A H 0.2239 0.6736 0.7886 0.427 Uiso 1 1 d R . . . .
H24B H 0.1969 0.6499 0.6928 0.427 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
C1 C3 1.487(7) . ?
C1 O1 1.244(6) . ?
C1 O2 1.277(6) . ?
C2 C4 1.488(7) . ?
C2 O3 1.291(7) . ?
C2 O4 1.227(6) . ?
C3 C4 1.364(7) . ?
C3 N1 1.360(7) . ?
C4 N2 1.363(7) . ?
C5 C6 1.459(7) . ?
C5 N1 1.354(7) . ?
C5 N2 1.335(7) . ?
C6 C7 1.379(9) . ?
C6 C11 1.393(8) . ?
C7 C8 1.366(9) . ?
C8 C9 1.355(11) . ?
C8 F1 1.303(9) . ?
C9 C10 1.363(11) . ?
C10 C11 1.375(9) . ?
C10 F1A 1.297(14) . ?
C12 C14 1.491(7) . ?
C12 O5 1.250(6) . ?
C12 O6 1.255(6) . ?
C13 C15 1.488(7) . ?
C13 O7 1.293(7) . ?
C13 O8 1.233(7) . ?
C14 C15 1.372(7) . ?
C14 N3 1.360(7) . ?
C15 N4 1.359(7) . ?
C16 C17 1.467(7) . ?
C16 N3 1.333(6) . ?
C16 N4 1.351(7) . ?
C17 C18 1.393(8) . ?
C17 C22 1.391(8) . ?
C18 C19 1.366(8) . ?
C19 C20 1.362(10) . ?
C19 F2 1.337(8) . ?
C20 C21 1.371(10) . ?
C21 C22 1.378(8) . ?
C21 F2A 1.318(19) . ?
Eu1 O1 2.444(4) . ?
Eu1 O5 2.300(3) . ?
Eu1 O13 2.384(4) . ?
Eu1 O14 2.424(4) . ?
Eu1 O15 2.465(4) . ?
Eu1 O16 2.412(4) . ?
Eu1 O17 2.396(4) . ?
Eu1 O18 2.390(5) . ?
C23 C25 1.492(8) . ?
C23 O9 1.211(7) . ?
C23 O10 1.271(7) . ?
C24 C26 1.512(8) . ?
C24 O11 1.269(10) . ?
C24 O12 1.227(8) . ?
C25 C26 1.363(8) . ?
C25 N6 1.352(7) . ?
C26 N5 1.370(7) . ?
C27 C28 1.464(8) . ?
C27 N5 1.338(7) . ?
C27 N6 1.359(7) . ?
C28 C29 1.370(9) . ?
C28 C33 1.382(10) . ?
C29 C30 1.363(12) . ?
C30 C31 1.365(15) . ?
C30 F3 1.346(10) . ?
C31 C32 1.364(14) . ?
C32 C33 1.389(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
O1 C1 C3 119.0(5) . . ?
O1 C1 O2 124.1(5) . . ?
O2 C1 C3 116.9(4) . . ?
O3 C2 C4 118.2(4) . . ?
O4 C2 C4 120.8(5) . . ?
O4 C2 O3 121.1(5) . . ?
C4 C3 C1 132.6(5) . . ?
N1 C3 C1 120.7(4) . . ?
N1 C3 C4 106.7(4) . . ?
C3 C4 C2 130.8(5) . . ?
N2 C4 C2 119.6(5) . . ?
N2 C4 C3 109.6(5) . . ?
N1 C5 C6 124.3(5) . . ?
N2 C5 C6 125.1(5) . . ?
N2 C5 N1 110.6(5) . . ?
C7 C6 C5 121.8(5) . . ?
C7 C6 C11 118.3(5) . . ?
C11 C6 C5 119.9(5) . . ?
C8 C7 C6 119.5(6) . . ?
C9 C8 C7 123.5(7) . . ?
F1 C8 C7 119.1(8) . . ?
F1 C8 C9 117.4(7) . . ?
C8 C9 C10 116.6(6) . . ?
C9 C10 C11 122.7(6) . . ?
F1A C10 C9 112.5(10) . . ?
F1A C10 C11 123.8(10) . . ?
C10 C11 C6 119.4(6) . . ?
O5 C12 C14 117.6(5) . . ?
O5 C12 O6 123.9(5) . . ?
O6 C12 C14 118.5(4) . . ?
O7 C13 C15 118.3(5) . . ?
O8 C13 C15 119.1(5) . . ?
O8 C13 O7 122.6(5) . . ?
C15 C14 C12 128.2(5) . . ?
N3 C14 C12 121.5(4) . . ?
N3 C14 C15 110.3(5) . . ?
C14 C15 C13 134.3(5) . . ?
N4 C15 C13 119.9(4) . . ?
N4 C15 C14 105.7(4) . . ?
N3 C16 C17 125.1(5) . . ?
N3 C16 N4 110.9(4) . . ?
N4 C16 C17 124.0(5) . . ?
C18 C17 C16 119.3(5) . . ?
C22 C17 C16 122.4(5) . . ?
C22 C17 C18 118.3(5) . . ?
C19 C18 C17 119.3(6) . . ?
C20 C19 C18 123.2(6) . . ?
F2 C19 C18 119.2(6) . . ?
F2 C19 C20 117.5(6) . . ?
C19 C20 C21 117.6(6) . . ?
C20 C21 C22 121.4(6) . . ?
F2A C21 C20 111.2(16) . . ?
F2A C21 C22 126.3(17) . . ?
C21 C22 C17 120.2(6) . . ?
O1 Eu1 O15 128.51(14) . . ?
O5 Eu1 O1 142.79(13) . . ?
O5 Eu1 O13 140.48(15) . . ?
O5 Eu1 O14 75.95(15) . . ?
O5 Eu1 O15 73.19(14) . . ?
O5 Eu1 O16 107.19(14) . . ?
O5 Eu1 O17 71.54(14) . . ?
O5 Eu1 O18 95.57(17) . . ?
O13 Eu1 O1 75.70(14) . . ?
O13 Eu1 O14 77.31(17) . . ?
O13 Eu1 O15 72.29(15) . . ?
O13 Eu1 O16 89.53(15) . . ?
O13 Eu1 O17 147.69(15) . . ?
O13 Eu1 O18 90.09(19) . . ?
O14 Eu1 O1 133.94(14) . . ?
O14 Eu1 O15 75.47(16) . . ?
O16 Eu1 O1 74.05(13) . . ?
O16 Eu1 O14 69.10(15) . . ?
O16 Eu1 O15 142.99(14) . . ?
O17 Eu1 O1 71.99(13) . . ?
O17 Eu1 O14 126.36(17) . . ?
O17 Eu1 O15 130.37(15) . . ?
O17 Eu1 O16 81.24(15) . . ?
O18 Eu1 O1 71.07(15) . . ?
O18 Eu1 O14 145.19(18) . . ?
O18 Eu1 O15 69.78(16) . . ?
O18 Eu1 O16 144.07(15) . . ?
O18 Eu1 O17 80.10(19) . . ?
C5 N1 C3 107.3(4) . . ?
C5 N2 C4 105.8(4) . . ?
C16 N3 C14 105.4(4) . . ?
C16 N4 C15 107.8(4) . . ?
C1 O1 Eu1 135.0(3) . . ?
C12 O5 Eu1 175.0(4) . . ?
O9 C23 C25 119.4(5) . . ?
O9 C23 O10 123.0(6) . . ?
O10 C23 C25 117.6(5) . . ?
O11 C24 C26 117.7(6) . . ?
O12 C24 C26 119.2(7) . . ?
O12 C24 O11 123.0(7) . . ?
C26 C25 C23 134.6(5) . . ?
N6 C25 C23 120.1(5) . . ?
N6 C25 C26 105.3(5) . . ?
C25 C26 C24 128.0(6) . . ?
C25 C26 N5 110.8(5) . . ?
N5 C26 C24 121.2(5) . . ?
N5 C27 C28 126.4(5) . . ?
N5 C27 N6 109.6(5) . . ?
N6 C27 C28 124.0(5) . . ?
C29 C28 C27 120.4(6) . . ?
C29 C28 C33 118.5(6) . . ?
C33 C28 C27 121.1(5) . . ?
C30 C29 C28 119.8(9) . . ?
C29 C30 C31 122.5(8) . . ?
F3 C30 C29 119.5(11) . . ?
F3 C30 C31 118.0(9) . . ?
C32 C31 C30 118.5(8) . . ?
C31 C32 C33 119.9(10) . . ?
C28 C33 C32 120.9(8) . . ?
C27 N5 C26 105.3(4) . . ?
C25 N6 C27 109.0(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4 O9 0.86 2.01 2.854(6) 166.3 1_565
O3 H3 O2 0.82 1.62 2.436(5) 177.5 .
O7 H7A O6 0.82 1.66 2.470(5) 171.3 .
O13 H13B O2 0.89 1.85 2.680(6) 154.5 .
O14 H14A O4 0.86 2.14 2.781(6) 130.7 2
O14 H14B O22 0.86 1.88 2.706(6) 159.3 1_455
O15 H15B O12 0.88 1.91 2.759(6) 162.5 2_666
O16 H16A O3 0.97 1.91 2.818(5) 155.5 2
O16 H16B O10 0.87 1.89 2.696(6) 154.8 2_656
O17 H17A N3 0.87 2.19 2.881(6) 135.1 .
O17 H17B O21 0.87 1.93 2.746(7) 156.3 2_666
O18 H18B O20 0.91 1.92 2.703(8) 142.1 .
O18 H18B O20A 0.91 2.19 2.87(4) 131.1 .
N6 H6 O8 0.86 2.01 2.834(6) 159.9 1_545
O10 H10A O11 0.90(2) 1.54(2) 2.435(7) 172(6) .
O19 H19A N5 0.85 2.02 2.861(7) 170.1 2_666
O19 H19B O20 0.97 2.19 2.748(15) 115.1 2_665
O20 H20A N2 0.86 2.73 2.890(9) 91.9 2_655
O20 H20A O19 0.86 2.10 2.748(15) 131.7 2_665
O20 H20B O4 0.85 2.15 2.897(10) 146.2 2_655
O20 H20B O23 0.85 2.54 2.88(2) 105.7 .
O21 H21A O24 0.85 1.98 2.779(13) 155.9 .
O22 H22B O6 0.85 2.08 2.779(6) 139.0 1_655
O23 H23B O22 0.85 2.05 2.856(18) 157.7 .
O23A H23C O19 0.85 1.82 2.655(15) 165.0 .

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 8 -4 0.1135 0.1857 7.6600 -4.4571 -0.0417 -0.1741 0.9839
-3 7 5 0.1033 -3.2828 6.6526 4.5554 0.1571 0.6544 0.7397
-4 4 8 0.1090 -4.1711 3.8522 8.1922 0.2184 0.9099 0.3526
3 -6 -5 0.0498 3.4899 -6.2704 -5.2620 -0.1703 -0.7094 -0.6840
4 -1 -10 0.0574 4.2327 -1.0353 -9.8148 -0.2333 -0.9724 0.0090
6 1 2 0.0252 5.9618 1.3550 2.1054 -0.9659 0.2318 0.1150
1 -8 3 0.1285 1.1441 -7.9118 2.9620 -0.0905 0.0215 -0.9957
-6 -1 -2 0.0010 -6.0455 -0.7135 -2.3417 0.9718 -0.2332 -0.0344
-7 4 3 0.0734 -7.0106 4.0048 2.9960 0.8110 0.4280 0.4554
-7 -2 5 0.1120 -7.0008 -1.9939 5.0011 0.8747 0.4232 -0.2936

_olex2_date_sample_data_collection 2018-07-11
_olex2_submission_special_instructions 'No special instructions were received'
