data_oae416c_sq
_audit_creation_date               2018-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
;
# end Validation Reply Form
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C84 H60 F6 O34 U6'
_chemical_formula_sum              'C84 H60 F6 O34 U6'
_chemical_formula_weight           3155.50
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'U' 'U' -9.6767 9.6646 '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        'tetragonal'
_space_group_IT_number             131
_space_group_name_H-M_alt          'P 42/m m c'
_space_group_name_Hall             '-P 4c 2'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z+1/2'
 'y, -x, z+1/2'
 '-x, y, -z'
 'x, -y, -z'
 'y, x, -z+1/2'
 '-y, -x, -z+1/2'
 '-x, -y, -z'
 'x, y, -z'
 'y, -x, -z-1/2'
 '-y, x, -z-1/2'
 'x, -y, z'
 '-x, y, z'
 '-y, -x, z-1/2'
 'y, x, z-1/2'

_cell_length_a                     23.6374(10)
_cell_length_b                     23.6374(10)
_cell_length_c                     19.3363(9)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       10803.7(10)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      9912
_cell_measurement_temperature      100(2)
_cell_measurement_theta_max        22.399
_cell_measurement_theta_min        2.196
_shelx_estimated_absorpt_T_max     0.714
_shelx_estimated_absorpt_T_min     0.497
_exptl_absorpt_coefficient_mu      4.521
_exptl_absorpt_correction_T_max    0.6453
_exptl_absorpt_correction_T_min    0.5428
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0834 before and 0.0741 after correction.
The Ratio of minimum to maximum transmission is 0.8412.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour              green
_exptl_crystal_colour_primary      green
_exptl_crystal_density_diffrn      0.970
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         plate
_exptl_crystal_F_000               2884
_exptl_crystal_size_max            0.18
_exptl_crystal_size_mid            0.1
_exptl_crystal_size_min            0.08
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1185
_diffrn_reflns_av_unetI/netI       0.0382
_diffrn_reflns_Laue_measured_fraction_full  0.997
_diffrn_reflns_Laue_measured_fraction_max  0.997
_diffrn_reflns_limit_h_max         25
_diffrn_reflns_limit_h_min         -25
_diffrn_reflns_limit_k_max         25
_diffrn_reflns_limit_k_min         -25
_diffrn_reflns_limit_l_max         20
_diffrn_reflns_limit_l_min         -20
_diffrn_reflns_number              71450
_diffrn_reflns_point_group_measured_fraction_full  0.997
_diffrn_reflns_point_group_measured_fraction_max  0.997
_diffrn_reflns_theta_full          22.493
_diffrn_reflns_theta_max           22.493
_diffrn_reflns_theta_min           2.196
_diffrn_ambient_temperature        100(2)
_diffrn_detector                   'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean   10.4
_diffrn_detector_type              'CMOS area detector'
_diffrn_measured_fraction_theta_full  0.997
_diffrn_measured_fraction_theta_max  0.997
_diffrn_measurement_device         'three-circle diffractometer'
_diffrn_measurement_device_type    'Bruker D8 QUEST'
_diffrn_measurement_method         'ω and φ scans'
_diffrn_radiation_monochromator    'mirror optics'
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'microfocus sealed X-ray tube'
_diffrn_source_type                'Incoatec I\ms'
_diffrn_special_details            ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  2879
_reflns_number_total               3860
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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         'SAINT V8.38A (?, 2016)'
_computing_data_collection         'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction          'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'XL (Sheldrick, 2008)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           1.552
_refine_diff_density_min           -1.803
_refine_diff_density_rms           0.126
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.035
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       143
_refine_ls_number_reflns           3860
_refine_ls_number_restraints       124
_refine_ls_R_factor_all            0.0671
_refine_ls_R_factor_gt             0.0480
_refine_ls_restrained_S_all        1.065
_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)+(0.0679P)²+78.3595P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1233
_refine_ls_wR_factor_ref           0.1359
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C13_$2
 1.5 with sigma of 0.02
 C9-C10
 1.48 with sigma of 0.015
 C11-C10 = C12-C11 = C13-C12
 1.39 with sigma of 0.015
 C14-C12
 1.54 with sigma of 0.02
 C8-C4
 1.54 with sigma of 0.01
 C11-C11_$3
 2.41 with sigma of 0.02
 C12-C12_$3
 2.41 with sigma of 0.02
 O8-O8_$4
 2.3 with sigma of 0.02
 C16-C15
 1.48 with sigma of 0.02
 C11-C14 \\sim C13-C14
 with sigma of 0.015
3. Restrained planarity
 C9, C10, C11, C12, C13
 with sigma of 0.01
 C13, C14, C12, C11, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uiso(C9) = Uiso(C10) = Uiso(C11) = Uiso(C12) = Uiso(C13)
5. Rigid body (RIGU) restrains
 C8, C4, C5, C3, C6, C7, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C11(0.5) H11(0.5) C12(0.5) H12(0.25) C14(0.25) H14A(0.25)
 H14B(0.25) H14C(0.25) F16A(0.25) F16B(0.25) F16C(0.25)
 Fixed Uiso: C14(0.2) C16(0.15) F16A(0.25) F16B(0.25) F16C(0.25)
 Fixed X: F16A(0.04736) F16B(-0.00298) F16C(-0.04438)
 Fixed Y: F16A(0.22082) F16B(0.22082) F16C(0.22082)
 Fixed Z: F16A(0.529221) F16B(0.435249) F16C(0.53552)
7.a Riding coordinates:
 C11(H11), C12(H12), C14(H14A,H14B,H14C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_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
 U1 U 0.000000 0.41960(3) 0.40202(3) 0.0614(3) Uani 1 2 d S T P . .
 U2 U 0.11640(3) 0.500000 0.500000 0.0306(2) Uani 1 4 d S T P . .
 O1 O 0.0560(5) 0.5784(5) 0.500000 0.079(4) Uani 1 2 d S T P . .
 O2 O 0.0542(4) 0.500000 0.4081(6) 0.076(4) Uani 1 2 d S T P . .
 O3 O 0.1588(3) 0.4341(4) 0.4210(4) 0.074(2) Uani 1 1 d . . . . .
 O4 O 0.0906(4) 0.3895(5) 0.3634(6) 0.130(5) Uani 1 1 d . . . . .
 C1 C 0.1411(6) 0.4013(7) 0.3776(8) 0.090(4) Uani 1 1 d . U . . .
 C2 C 0.1835(6) 0.3656(6) 0.3384(7) 0.093(4) Uani 1 1 d . U . . .
 C3 C 0.2405(6) 0.3690(6) 0.3585(8) 0.100(4) Uani 1 1 d . U . . .
 H3 H 0.251190 0.392901 0.395798 0.120 Uiso 1 1 calc R . . . .
 C4 C 0.2818(6) 0.3369(7) 0.3234(8) 0.118(5) Uani 1 1 d D U . . .
 C7 C 0.1628(7) 0.3324(7) 0.2832(8) 0.123(5) Uani 1 1 d . U . . .
 H7 H 0.123762 0.334263 0.271713 0.147 Uiso 1 1 calc R . . . .
 C5 C 0.2600(7) 0.2998(7) 0.2706(9) 0.123(5) Uani 1 1 d . U . . .
 C6 C 0.1989(8) 0.2962(8) 0.2443(9) 0.142(6) Uani 1 1 d . U . . .
 H6 H 0.186823 0.272969 0.207017 0.171 Uiso 1 1 calc R . . . .
 C8 C 0.3437(7) 0.3381(11) 0.3508(12) 0.221(10) Uani 1 1 d D U . . .
 H8A H 0.369982 0.334600 0.311812 0.332 Uiso 1 1 calc GR . . . .
 H8B H 0.349494 0.306494 0.382819 0.332 Uiso 1 1 calc GR . . . .
 H8C H 0.350548 0.373878 0.374899 0.332 Uiso 1 1 calc GR . . . .
 O5 O 0.000000 0.4499(7) 0.2845(7) 0.122(5) Uani 1 2 d S TU P . .
 C9 C 0.000000 0.500000 0.261(2) 0.225(13) Uiso 1 4 d DS T P . .
 C10 C 0.000000 0.500000 0.1836(19) 0.225(13) Uiso 1 4 d DS T P . .
 C11 C 0.0293(8) 0.4583(6) 0.1485(14) 0.225(13) Uiso 0.5 1 d D . . . .
 H11 H 0.046299 0.427962 0.173081 0.270 Uiso 0.5 1 d R . . . .
 C12 C 0.0291(8) 0.4587(6) 0.0764(13) 0.225(13) Uiso 0.5 1 d D . . . .
 H12 H 0.046103 0.428461 0.051593 0.270 Uiso 0.25 1 d R . . . .
 C13 C 0.000000 0.500000 0.0389(5) 0.225(13) Uiso 1 4 d DS T P . .
 C14 C 0.0617(17) 0.4127(14) 0.0378(16) 0.200 Uiso 0.25 1 d D . . . .
 H14A H 0.059603 0.416422 -0.010726 0.300 Uiso 0.25 1 d R . . . .
 H14B H 0.100283 0.411412 0.051544 0.300 Uiso 0.25 1 d R . . . .
 H14C H 0.043113 0.378852 0.051454 0.300 Uiso 0.25 1 d R . . . .
 O6 O 0.2286(8) 0.500000 0.500000 0.115(7) Uani 1 4 d S T P . .
 O8 O 0.000000 0.3185(7) 0.4384(4) 0.119(5) Uiso 1 2 d DS T P . .
 C15 C 0.000000 0.3097(14) 0.500000 0.124(12) Uiso 1 4 d DS T P . .
 C16 C 0.000000 0.2482(14) 0.500000 0.150 Uiso 1 4 d DS T P . .
 F16A F 0.047360 0.220820 0.529221 0.250 Uiso 0.25 1 d . . . . .
 F16B F -0.002980 0.220820 0.435249 0.250 Uiso 0.25 1 d . . . . .
 F16C F -0.044380 0.220820 0.535520 0.250 Uiso 0.25 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 U1 U1 3.7892(13) 10_556 ?
 U1 U1 3.8007(13) 2_565 ?
 U1 U2 3.8434(6) . ?
 U1 U2 3.8434(6) 9_566 ?
 U1 O1 2.312(6) 13_565 ?
 U1 O1 2.312(6) 9_566 ?
 U1 O2 2.295(6) 2_565 ?
 U1 O2 2.295(6) . ?
 U1 O4 2.377(8) 14 ?
 U1 O4 2.377(8) . ?
 U1 O5 2.383(15) . ?
 U1 O8 2.491(15) . ?
 U2 O1 2.340(10) . ?
 U2 O1 2.340(10) 13_565 ?
 U2 O2 2.305(10) . ?
 U2 O2 2.305(10) 10_556 ?
 U2 O3 2.401(7) . ?
 U2 O3 2.401(7) 10_556 ?
 U2 O3 2.401(7) 6_566 ?
 U2 O3 2.401(7) 13_565 ?
 U2 O6 2.653(18) . ?
 O3 C1 1.217(16) . ?
 O4 C1 1.255(17) . ?
 C1 C2 1.514(17) . ?
 C2 C3 1.403(19) . ?
 C2 C7 1.413(19) . ?
 C3 H3 0.9500 . ?
 C3 C4 1.412(17) . ?
 C4 C5 1.44(2) . ?
 C4 C8 1.555(10) . ?
 C7 H7 0.9500 . ?
 C7 C6 1.424(19) . ?
 C5 C5 1.55(3) 7 ?
 C5 C6 1.53(2) . ?
 C6 H6 0.9500 . ?
 C8 H8A 0.9800 . ?
 C8 H8B 0.9800 . ?
 C8 H8C 0.9800 . ?
 O5 C9 1.27(2) . ?
 C9 C10 1.493(15) . ?
 C10 C11 1.384(14) . ?
 C10 C11 1.384(14) 2_565 ?
 C10 C11 1.384(14) 13_565 ?
 C10 C11 1.384(14) 14 ?
 C11 C11 1.39(4) 14 ?
 C11 C11 1.97(3) 13_565 ?
 C11 H11 0.9490 . ?
 C11 C12 1.395(15) . ?
 C11 C12 1.96(3) 14 ?
 C12 C12 1.95(3) 13_565 ?
 C12 C12 1.38(4) 14 ?
 C12 H12 0.9485 . ?
 C12 C13 1.397(12) . ?
 C12 C14 1.53(2) . ?
 C13 C13 1.51(2) 5 ?
 C14 H12 0.5873 . ?
 C14 C14 1.46(6) 10 ?
 C14 H14A 0.9431 . ?
 C14 H14A 0.53(6) 10 ?
 C14 H14B 0.9512 . ?
 C14 H14C 0.9509 . ?
 O8 C15 1.208(10) . ?
 C15 C16 1.454(19) . ?
 C16 F16A 1.411(16) 10_556 ?
 C16 F16A 1.411(16) 14 ?
 C16 F16A 1.411(16) 5_556 ?
 C16 F16A 1.411(16) . ?
 C16 F16B 1.411(16) . ?
 C16 F16B 1.411(16) 14 ?
 C16 F16B 1.411(16) 5_556 ?
 C16 F16B 1.411(16) 10_556 ?
 C16 F16C 1.411(16) 14 ?
 C16 F16C 1.411(16) 10_556 ?
 C16 F16C 1.411(16) 5_556 ?
 C16 F16C 1.411(16) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 U1 U1 U1 90.0 10_556 2_565 ?
 U1 U1 U2 60.366(11) 2_565 9_566 ?
 U1 U1 U2 60.464(10) 10_556 . ?
 U1 U1 U2 60.365(11) 2_565 . ?
 U1 U1 U2 60.465(10) 10_556 9_566 ?
 U2 U1 U2 91.433(18) . 9_566 ?
 O1 U1 U1 35.0(2) 9_566 10_556 ?
 O1 U1 U1 88.9(3) 9_566 2_565 ?
 O1 U1 U1 35.0(2) 13_565 10_556 ?
 O1 U1 U1 88.9(3) 13_565 2_565 ?
 O1 U1 U2 89.8(3) 9_566 . ?
 O1 U1 U2 34.5(2) 9_566 9_566 ?
 O1 U1 U2 89.8(3) 13_565 9_566 ?
 O1 U1 U2 34.5(2) 13_565 . ?
 O1 U1 O1 69.9(4) 13_565 9_566 ?
 O1 U1 O4 75.4(4) 13_565 . ?
 O1 U1 O4 141.2(4) 9_566 . ?
 O1 U1 O4 141.2(4) 13_565 14 ?
 O1 U1 O4 75.4(4) 9_566 14 ?
 O1 U1 O5 140.9(3) 13_565 . ?
 O1 U1 O5 140.9(3) 9_566 . ?
 O1 U1 O8 77.7(3) 13_565 . ?
 O1 U1 O8 77.7(3) 9_566 . ?
 O2 U1 U1 87.0(3) . 10_556 ?
 O2 U1 U1 34.1(2) . 2_565 ?
 O2 U1 U1 34.1(2) 2_565 2_565 ?
 O2 U1 U1 87.0(3) 2_565 10_556 ?
 O2 U1 U2 88.0(3) 2_565 . ?
 O2 U1 U2 88.0(3) . 9_566 ?
 O2 U1 U2 33.4(2) 2_565 9_566 ?
 O2 U1 U2 33.4(2) . . ?
 O2 U1 O1 105.1(4) . 9_566 ?
 O2 U1 O1 67.7(4) 2_565 9_566 ?
 O2 U1 O1 105.1(4) 2_565 13_565 ?
 O2 U1 O1 67.7(4) . 13_565 ?
 O2 U1 O2 67.9(4) 2_565 . ?
 O2 U1 O4 76.1(4) . . ?
 O2 U1 O4 140.1(4) . 14 ?
 O2 U1 O4 76.1(4) 2_565 14 ?
 O2 U1 O4 140.1(4) 2_565 . ?
 O2 U1 O5 78.5(4) . . ?
 O2 U1 O5 78.5(4) 2_565 . ?
 O2 U1 O8 141.2(2) . . ?
 O2 U1 O8 141.2(2) 2_565 . ?
 O4 U1 U1 108.3(3) . 10_556 ?
 O4 U1 U1 107.4(3) . 2_565 ?
 O4 U1 U1 108.3(3) 14 10_556 ?
 O4 U1 U1 107.4(3) 14 2_565 ?
 O4 U1 U2 161.4(2) 14 . ?
 O4 U1 U2 161.4(2) . 9_566 ?
 O4 U1 U2 70.0(2) 14 9_566 ?
 O4 U1 U2 70.0(2) . . ?
 O4 U1 O4 128.6(5) 14 . ?
 O4 U1 O5 77.9(3) . . ?
 O4 U1 O5 77.9(3) 14 . ?
 O4 U1 O8 78.6(3) . . ?
 O4 U1 O8 78.6(3) 14 . ?
 O5 U1 U1 72.5(4) . 2_565 ?
 O5 U1 U1 162.5(4) . 10_556 ?
 O5 U1 U2 108.8(3) . 9_566 ?
 O5 U1 U2 108.8(3) . . ?
 O5 U1 O8 123.9(5) . . ?
 O8 U1 U1 73.6(2) . 10_556 ?
 O8 U1 U1 163.6(2) . 2_565 ?
 O8 U1 U2 109.57(14) . 9_566 ?
 O8 U1 U2 109.57(14) . . ?
 U1 U2 U1 59.07(2) 2_565 9_566 ?
 U1 U2 U1 59.27(2) 10_556 9_566 ?
 U1 U2 U1 88.566(18) 2_565 10_556 ?
 O1 U2 U1 34.05(15) . 9_566 ?
 O1 U2 U1 87.4(3) . 10_556 ?
 O1 U2 U1 34.05(15) 13_565 10_556 ?
 O1 U2 U1 87.4(3) 13_565 9_566 ?
 O1 U2 U1 34.05(15) . 2_565 ?
 O1 U2 U1 87.4(3) 13_565 2_565 ?
 O1 U2 O1 104.8(6) 13_565 . ?
 O1 U2 O3 74.9(3) . 13_565 ?
 O1 U2 O3 140.2(2) . . ?
 O1 U2 O3 74.9(3) . 6_566 ?
 O1 U2 O3 74.9(3) 13_565 10_556 ?
 O1 U2 O3 140.2(2) 13_565 13_565 ?
 O1 U2 O3 140.2(2) 13_565 6_566 ?
 O1 U2 O3 140.2(2) . 10_556 ?
 O1 U2 O3 74.9(3) 13_565 . ?
 O1 U2 O6 127.6(3) 13_565 . ?
 O1 U2 O6 127.6(3) . . ?
 O2 U2 U1 85.6(3) . 9_566 ?
 O2 U2 U1 85.6(3) . 10_556 ?
 O2 U2 U1 33.26(14) 10_556 10_556 ?
 O2 U2 U1 85.6(3) 10_556 2_565 ?
 O2 U2 U1 33.26(14) . 2_565 ?
 O2 U2 U1 33.26(14) 10_556 9_566 ?
 O2 U2 O1 67.1(2) 10_556 . ?
 O2 U2 O1 67.1(2) 10_556 13_565 ?
 O2 U2 O1 67.1(2) . . ?
 O2 U2 O1 67.1(2) . 13_565 ?
 O2 U2 O2 100.8(6) 10_556 . ?
 O2 U2 O3 77.0(3) 10_556 6_566 ?
 O2 U2 O3 139.1(2) . 10_556 ?
 O2 U2 O3 139.1(2) 10_556 . ?
 O2 U2 O3 77.0(3) 10_556 10_556 ?
 O2 U2 O3 139.1(2) 10_556 13_565 ?
 O2 U2 O3 77.0(3) . . ?
 O2 U2 O3 139.1(2) . 6_566 ?
 O2 U2 O3 77.0(3) . 13_565 ?
 O2 U2 O6 129.6(3) . . ?
 O2 U2 O6 129.6(3) 10_556 . ?
 O3 U2 U1 106.9(2) 13_565 9_566 ?
 O3 U2 U1 158.92(19) 10_556 2_565 ?
 O3 U2 U1 107.8(2) 6_566 10_556 ?
 O3 U2 U1 158.92(19) . 9_566 ?
 O3 U2 U1 107.8(2) . 2_565 ?
 O3 U2 U1 70.36(19) 13_565 2_565 ?
 O3 U2 U1 158.92(19) 13_565 10_556 ?
 O3 U2 U1 70.36(19) 10_556 10_556 ?
 O3 U2 U1 106.9(2) 6_566 2_565 ?
 O3 U2 U1 70.36(19) 6_566 9_566 ?
 O3 U2 U1 106.9(2) . 10_556 ?
 O3 U2 U1 107.8(2) 10_556 9_566 ?
 O3 U2 O3 130.7(4) 13_565 10_556 ?
 O3 U2 O3 130.7(4) . 6_566 ?
 O3 U2 O3 81.0(4) . 13_565 ?
 O3 U2 O3 79.0(4) . 10_556 ?
 O3 U2 O3 81.0(4) 6_566 10_556 ?
 O3 U2 O3 79.0(4) 6_566 13_565 ?
 O3 U2 O6 65.36(19) 13_565 . ?
 O3 U2 O6 65.36(19) . . ?
 O3 U2 O6 65.36(19) 6_566 . ?
 O3 U2 O6 65.36(19) 10_556 . ?
 O6 U2 U1 135.717(9) . 2_565 ?
 O6 U2 U1 135.717(9) . 9_566 ?
 O6 U2 U1 135.717(9) . 10_556 ?
 U1 O1 U1 110.1(4) 2_565 9_566 ?
 U1 O1 U2 111.4(3) 2_565 . ?
 U1 O1 U2 111.4(3) 9_566 . ?
 U1 O2 U1 111.8(4) 2_565 . ?
 U1 O2 U2 113.3(3) . . ?
 U1 O2 U2 113.3(3) 2_565 . ?
 C1 O3 U2 135.2(8) . . ?
 C1 O4 U1 136.2(9) . . ?
 O3 C1 O4 128.2(12) . . ?
 O3 C1 C2 118.2(14) . . ?
 O4 C1 C2 113.4(14) . . ?
 C3 C2 C1 117.7(13) . . ?
 C3 C2 C7 125.0(13) . . ?
 C7 C2 C1 117.2(14) . . ?
 C2 C3 H3 120.0 . . ?
 C2 C3 C4 120.0(13) . . ?
 C4 C3 H3 120.0 . . ?
 C3 C4 C5 114.8(14) . . ?
 C3 C4 C8 118.5(15) . . ?
 C5 C4 C8 126.1(15) . . ?
 C2 C7 H7 119.2 . . ?
 C2 C7 C6 121.7(16) . . ?
 C6 C7 H7 119.2 . . ?
 C4 C5 C5 121.0(14) . 7 ?
 C4 C5 C6 127.3(14) . . ?
 C6 C5 C5 111.5(14) . 7 ?
 C7 C6 C5 110.8(15) . . ?
 C7 C6 H6 124.6 . . ?
 C5 C6 H6 124.6 . . ?
 C4 C8 H8A 109.5 . . ?
 C4 C8 H8B 109.5 . . ?
 C4 C8 H8C 109.5 . . ?
 H8A C8 H8B 109.5 . . ?
 H8A C8 H8C 109.5 . . ?
 H8B C8 H8C 109.5 . . ?
 C9 O5 U1 129(2) . . ?
 O5 C9 O5 138(4) 2_565 . ?
 O5 C9 C10 111.1(19) . . ?
 O5 C9 C10 111.1(19) 2_565 . ?
 C11 C10 C9 119.4(13) 2_565 . ?
 C11 C10 C9 119.4(13) 13_565 . ?
 C11 C10 C9 119.4(13) . . ?
 C11 C10 C9 119.4(13) 14 . ?
 C11 C10 C11 91(2) 2_565 14 ?
 C11 C10 C11 60.1(19) . 14 ?
 C11 C10 C11 121(3) 14 13_565 ?
 C11 C10 C11 60.1(19) 2_565 13_565 ?
 C11 C10 C11 121(3) . 2_565 ?
 C11 C10 C11 91(2) . 13_565 ?
 C10 C11 C11 60.0(10) . 14 ?
 C10 C11 C11 44.5(11) . 13_565 ?
 C10 C11 H11 120.3 . . ?
 C10 C11 C12 119.0(16) . . ?
 C10 C11 C12 89.6(16) . 14 ?
 C11 C11 C11 90.004(3) 14 13_565 ?
 C11 C11 H11 139.0 13_565 . ?
 C11 C11 H11 115.0 14 . ?
 C11 C11 C12 89.8(4) 14 . ?
 C11 C11 C12 45.3(8) 14 14 ?
 C12 C11 C11 89.7(4) 14 13_565 ?
 C12 C11 C11 89.6(5) . 13_565 ?
 C12 C11 H11 131.1 14 . ?
 C12 C11 H11 120.5 . . ?
 C12 C11 C12 44.5(9) . 14 ?
 C11 C12 C11 44.9(9) . 14 ?
 C11 C12 C12 90.4(5) . 13_565 ?
 C11 C12 H12 119.9 . . ?
 C11 C12 H12 130.8 14 . ?
 C11 C12 C13 121.6(14) . . ?
 C11 C12 C14 118.9(10) . . ?
 C12 C12 C11 90.2(4) 14 . ?
 C12 C12 C11 90.3(4) 13_565 14 ?
 C12 C12 C11 45.3(8) 14 14 ?
 C12 C12 C12 90.004(1) 14 13_565 ?
 C12 C12 H12 115.0 14 . ?
 C12 C12 H12 138.8 13_565 . ?
 C12 C12 C13 60.5(9) 14 . ?
 C12 C12 C14 120.3(11) 14 . ?
 C13 C12 C11 91.4(14) . 14 ?
 C13 C12 C12 45.6(9) . 13_565 ?
 C13 C12 H12 118.3 . . ?
 C13 C12 C14 119.5(13) . . ?
 C14 C12 C11 134.4(11) . 14 ?
 C14 C12 C12 135.4(11) . 13_565 ?
 C12 C13 C12 88.8(18) . 13_565 ?
 C12 C13 C12 88.8(18) 2_565 14 ?
 C12 C13 C12 59.0(18) 2_565 13_565 ?
 C12 C13 C12 59.0(18) . 14 ?
 C12 C13 C12 118(2) 13_565 14 ?
 C12 C13 C12 118(2) 2_565 . ?
 C12 C13 C13 121.2(10) . 5 ?
 C12 C13 C13 121.2(10) 14 5 ?
 C12 C13 C13 121.2(10) 2_565 5 ?
 C12 C13 C13 121.2(10) 13_565 5 ?
 C12 C14 H14A 108.5(11) . 10 ?
 C12 C14 H14A 113.2 . . ?
 C12 C14 H14B 111.8 . . ?
 C12 C14 H14C 103.3 . . ?
 H12 C14 H14A 111.2 . . ?
 H12 C14 H14B 119.7 . . ?
 H12 C14 H14C 96.7 . . ?
 C14 C14 C12 119.3(8) 10 . ?
 C14 C14 H12 117.1 10 . ?
 C14 C14 H14B 106.3 10 . ?
 C14 C14 H14C 106.2 10 . ?
 H14A C14 H14A 4.7 . 10 ?
 H14A C14 H14B 109.3 . . ?
 H14A C14 H14C 109.3 . . ?
 H14B C14 H14A 111.6 . 10 ?
 H14B C14 H14C 109.7 . . ?
 H14C C14 H14A 111.6 . 10 ?
 C15 O8 U1 116.4(19) . . ?
 O8 C15 O8 160(4) 5_556 . ?
 O8 C15 C16 99.9(18) . . ?
 O8 C15 C16 99.9(18) 5_556 . ?
 F16A C16 F16B 100.6(15) . . ?
 F16C C16 F16A 100.6(15) . . ?

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
 U1 O4 C1 O3 2(3) . . . . ?
 U1 O4 C1 C2 176.7(11) . . . . ?
 U1 O5 C9 O5 0.000(10) . . . 2_565 ?
 U1 O5 C9 C10 180.000(6) . . . . ?
 U1 O8 C15 O8 0.000(12) . . . 5_556 ?
 U1 O8 C15 C16 180.000(4) . . . . ?
 U2 O3 C1 O4 -5(3) . . . . ?
 U2 O3 C1 C2 -179.2(9) . . . . ?
 O3 C1 C2 C3 5(2) . . . . ?
 O3 C1 C2 C7 -173.3(15) . . . . ?
 O4 C1 C2 C3 -170.0(15) . . . . ?
 O4 C1 C2 C7 11(2) . . . . ?
 C1 C2 C3 C4 -179.6(15) . . . . ?
 C1 C2 C7 C6 -178.3(16) . . . . ?
 C2 C3 C4 C5 -3(2) . . . . ?
 C2 C3 C4 C8 -175.3(18) . . . . ?
 C2 C7 C6 C5 0(3) . . . . ?
 C3 C2 C7 C6 3(3) . . . . ?
 C3 C4 C5 C5 -177.5(17) . . . 7 ?
 C3 C4 C5 C6 7(3) . . . . ?
 C4 C5 C6 C7 -5(3) . . . . ?
 C7 C2 C3 C4 -1(3) . . . . ?
 C5 C5 C6 C7 179.2(16) 7 . . . ?
 C8 C4 C5 C5 -6(3) . . . 7 ?
 C8 C4 C5 C6 178(2) . . . . ?
 O5 C9 C10 C11 144.9(11) 2_565 . . . ?
 O5 C9 C10 C11 35.1(11) . . . 14 ?
 O5 C9 C10 C11 -35.1(11) . . . . ?
 O5 C9 C10 C11 -144.9(11) . . . 13_565 ?
 O5 C9 C10 C11 -35.1(11) 2_565 . . 2_565 ?
 O5 C9 C10 C11 -144.9(11) 2_565 . . 14 ?
 O5 C9 C10 C11 35.1(11) 2_565 . . 13_565 ?
 O5 C9 C10 C11 144.9(11) . . . 2_565 ?
 C9 C10 C11 C11 109.0(10) . . . 14 ?
 C9 C10 C11 C11 -125.0(15) . . . 13_565 ?
 C9 C10 C11 C12 -179.9(3) . . . . ?
 C9 C10 C11 C12 145.0(3) . . . 14 ?
 C10 C11 C12 C11 -55.0(11) . . . 14 ?
 C10 C11 C12 C12 -54.9(11) . . . 14 ?
 C10 C11 C12 C12 35.1(11) . . . 13_565 ?
 C10 C11 C12 C13 -0.1(6) . . . . ?
 C10 C11 C12 C14 179.7(12) . . . . ?
 C11 C10 C11 C11 -71.0(10) 2_565 . . 14 ?
 C11 C10 C11 C11 55.0(15) 2_565 . . 13_565 ?
 C11 C10 C11 C11 -126.0(18) 13_565 . . 14 ?
 C11 C10 C11 C11 126.0(18) 14 . . 13_565 ?
 C11 C10 C11 C12 36.0(11) 14 . . 14 ?
 C11 C10 C11 C12 71.0(11) 14 . . . ?
 C11 C10 C11 C12 -55.0(16) 13_565 . . . ?
 C11 C10 C11 C12 -90.0(15) 13_565 . . 14 ?
 C11 C10 C11 C12 -35.0(3) 2_565 . . 14 ?
 C11 C10 C11 C12 0.1(3) 2_565 . . . ?
 C11 C11 C12 C11 -90.005(5) 13_565 . . 14 ?
 C11 C11 C12 C12 -90.004(5) 13_565 . . 14 ?
 C11 C11 C12 C12 90.007(3) 14 . . 13_565 ?
 C11 C11 C12 C12 0.001(5) 13_565 . . 13_565 ?
 C11 C11 C12 C12 0.001(1) 14 . . 14 ?
 C11 C11 C12 C13 -35.2(11) 13_565 . . . ?
 C11 C11 C12 C13 54.8(11) 14 . . . ?
 C11 C11 C12 C14 144.7(13) 13_565 . . . ?
 C11 C11 C12 C14 -125.3(13) 14 . . . ?
 C11 C12 C13 C12 0.1(3) . . . 2_565 ?
 C11 C12 C13 C12 -69.9(9) . . . 14 ?
 C11 C12 C13 C12 -34.7(10) 14 . . 14 ?
 C11 C12 C13 C12 53.7(14) . . . 13_565 ?
 C11 C12 C13 C12 89.0(13) 14 . . 13_565 ?
 C11 C12 C13 C12 35.3(3) 14 . . 2_565 ?
 C11 C12 C13 C13 -179.9(3) . . . 5 ?
 C11 C12 C13 C13 -144.7(3) 14 . . 5 ?
 C11 C12 C14 C14 179.9(3) . . . 10 ?
 C11 C12 C14 C14 126.2(14) 14 . . 10 ?
 C12 C11 C12 C11 -0.001(1) 14 . . 14 ?
 C12 C11 C12 C12 90.005(3) 14 . . 13_565 ?
 C12 C11 C12 C13 54.8(11) 14 . . . ?
 C12 C11 C12 C14 -125.3(13) 14 . . . ?
 C12 C12 C13 C12 70.0(9) 14 . . 2_565 ?
 C12 C12 C13 C12 -53.7(13) 13_565 . . 2_565 ?
 C12 C12 C13 C12 123.7(14) 14 . . 13_565 ?
 C12 C12 C13 C12 -123.7(14) 13_565 . . 14 ?
 C12 C12 C13 C13 -110.0(9) 14 . . 5 ?
 C12 C12 C13 C13 126.3(13) 13_565 . . 5 ?
 C12 C12 C14 C14 70.9(10) 14 . . 10 ?
 C12 C12 C14 C14 -55.4(15) 13_565 . . 10 ?
 C13 C12 C14 C14 -0.2(11) . . . 10 ?
 C14 C12 C13 C12 -179.8(12) . . . 2_565 ?
 C14 C12 C13 C12 -126.1(16) . . . 13_565 ?
 C14 C12 C13 C12 110.2(13) . . . 14 ?
 C14 C12 C13 C13 0.2(12) . . . 5 ?

_platon_squeeze_details            ?
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
 1 -0.011 -0.007 -0.035 7119 1826 ' '

_platon_squeeze_void_probe_radius  1.20
_olex2_submission_special_instructions  'No special instructions were received'
_vrf_PLAT023_oae416c_sq
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      22.49 Degree
RESPONSE: No diffraction observed at higher angle / better resolution
because of extensive disorder and non-optimum crystallinity. The dataset
was truncated at d = 0.927 Angstroms, at which approximate value the mean
reflection I/sigma(I) fell below ~1.8.
;
_vrf_PLAT201_oae416c_sq
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          6 Report
RESPONSE: Disordered and partially occupied atoms refined isotropically or 
with fixed Uiso values.
;
_vrf_PLAT241_oae416c_sq
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O4 Check 
RESPONSE: O4 is likely affedcted by slight positional disorder, which 
could not be modeled.
;
_vrf_PLAT242_oae416c_sq
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         U2 Check 
RESPONSE: Alert caused by the larger displacement parameter values of
bridging and terminal hydroxyl/aquo ligands, which may be slightly
positionally disordered.
;
_vrf_PLAT342_oae416c_sq
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02533 Ang.  
RESPONSE: Data quality reduced because of the low crystallinity / high
mosaicity of the available crystals. Structure useful for general
connectivity only.
;
# start Validation Reply Form
_vrf_THETM01_oae416c_sq
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: No diffraction observed at higher angle / better resolution
because of extensive disorder and non-optimum crystallinity. The dataset
was truncated at d = 0.927 Angstroms, at which approximate value the mean
reflection I/sigma(I) fell below ~1.8.
;
