#------------------------------------------------------------------------------
#$Date: 2024-11-04 22:28:55 +0200 (Mon, 04 Nov 2024) $
#$Revision: 295760 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/73/7717389.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7717389
loop_
_publ_author_name
'Obey, Tom J. N.'
'Nichol, Gary S.'
'Love, Jason B.'
_publ_section_title
;
 Controlled and sequential single-electron reduction of the uranyl
 dication.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16229
_journal_page_last               16240
_journal_paper_doi               10.1039/d4dt02367f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C66 H77 Cl3 Dy Li2 N12 O2 U, 2(C5 H5 N)'
_chemical_formula_sum            'C76 H87 Cl3 Dy Li2 N14 O2 U'
_chemical_formula_weight         1749.35
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.566(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0653(4)
_cell_length_b                   17.0891(3)
_cell_length_c                   24.4481(5)
_cell_measurement_reflns_used    21649
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5940
_cell_measurement_theta_min      3.5370
_cell_volume                     7634.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  55.00   1.00   15.00    --  -14.44  34.00 -95.00   90
  2  ω    -53.00  36.00   1.00   15.00    --   16.16 -34.00 106.00   89
  3  ω    -87.00 -39.00   1.00   15.00    --  -14.44-178.00 -90.00   48
  4  ω    -11.00  39.00   1.00   15.00    --   16.16  77.00   0.00   50
  5  ω    -11.00  39.00   1.00   15.00    --   16.16  77.00 120.00   50
  6  ω    -51.00  33.00   1.00   15.00    --   16.16 -57.00  60.00   84
  7  ω     -1.00  83.00   1.00   15.00    --   16.16  57.00-150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0281516000
_diffrn_orient_matrix_UB_12      -0.0058810000
_diffrn_orient_matrix_UB_13      0.0132839000
_diffrn_orient_matrix_UB_21      0.0070274000
_diffrn_orient_matrix_UB_22      -0.0408235000
_diffrn_orient_matrix_UB_23      0.0012268000
_diffrn_orient_matrix_UB_31      0.0257625000
_diffrn_orient_matrix_UB_32      0.0047192000
_diffrn_orient_matrix_UB_33      0.0271736000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79648
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.901
_diffrn_reflns_theta_min         3.335
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.224
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             3488
_exptl_crystal_preparation
'Vapour diffusion of hexane into pyridine solution'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         17518
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0231P)²+10.4983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13292
_reflns_number_total             17518
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           to509_refinalised
_cod_database_code               7717389
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H47 N6 U O2 Dy Li2 Cl3'
_chemical_oxdiff_usercomment     Pyr/hex
_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.
;
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.318
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N14-C72 = N14-C76
 1.33 with sigma of 0.02
 C72-C73 = C75-C76
 1.38 with sigma of 0.02
 C73-C74 = C74-C75
 1.37 with sigma of 0.02
 N14-C75
 2.39 with sigma of 0.04
 C73-C75
 2.35 with sigma of 0.04
 C72-C74
 2.36 with sigma of 0.04
 C74-C76
 2.37 with sigma of 0.04
 N14-C73
 2.4 with sigma of 0.04
 N14-C72 \\sim N14-C76
 with sigma of 0.02
 C72-C73 \\sim C73-C74 \\sim C74-C75 \\sim C75-C76
 with sigma of 0.02
 N14-C75 \\sim N14-C73
 with sigma of 0.04
 C74-C76 \\sim C74-C72 \\sim C75-C73 \\sim C76-C72
 with sigma of 0.04
3. Restrained planarity
 N14, C72, C73, C74, C75, C76
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N14 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 N14, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C2(H2A,H2B), C36(H36A,H36B), C24(H24A,H24B), C21(H21A,H21B),
 C14(H14A,H14B), C23(H23A,H23B), C32(H32A,H32B), C22(H22A,H22B), C10(H10A,H10B),
  C35(H35A,H35B), C33(H33A,H33B), C11(H11A,H11B), C13(H13A,H13B), C12(H12A,
 H12B), C34(H34A,H34B)
6.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C19(H19), C41(H41), C17(H17), C28(H28), C27(H27), C16(H16),
 C37(H37), C8(H8), C57(H57), C61(H61), C5(H5), C66(H66), C51(H51), C62(H62),
 C67(H67), C40(H40), C6(H6), C68(H68), C39(H39), C71(H71), C52(H52), C38(H38),
 C54(H54), C56(H56), C46(H46), C58(H58), C60(H60), C65(H65), C47(H47), C70(H70),
  C42(H42), C59(H59), C63(H63), C55(H55), C64(H64), C44(H44), C45(H45),
 C53(H53), C43(H43), C69(H69), C50(H50), C48(H48), C49(H49), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.716
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.43198(2) 0.22235(2) 0.63379(2) 0.01158(5) Uani 1 1 d . . . . .
Dy1 Dy 0.49923(2) 0.08005(2) 0.75634(2) 0.01523(6) Uani 1 1 d . . . . .
Cl3 Cl 0.52686(6) 0.34787(6) 0.64329(5) 0.0203(2) Uani 1 1 d . . . . .
Cl2 Cl 0.61355(6) 0.15907(7) 0.82011(4) 0.0218(3) Uani 1 1 d . . . . .
Cl1 Cl 0.59154(7) -0.00889(7) 0.72672(5) 0.0279(3) Uani 1 1 d . . . . .
N5 N 0.3311(2) 0.1679(2) 0.66930(14) 0.0141(8) Uani 1 1 d . . . . .
N4 N 0.5276(2) 0.1697(2) 0.58570(14) 0.0159(8) Uani 1 1 d . . . . .
N3 N 0.4211(2) 0.0776(2) 0.62001(14) 0.0150(8) Uani 1 1 d . . . . .
N6 N 0.3667(2) 0.3284(2) 0.67651(14) 0.0173(8) Uani 1 1 d . . . . .
N7 N 0.4298(2) 0.1620(2) 0.81127(14) 0.0204(9) Uani 1 1 d . . . . .
N1 N 0.4033(2) -0.0111(2) 0.74513(14) 0.0150(8) Uani 1 1 d . . . . .
C29 C 0.2984(2) 0.2225(2) 0.69699(16) 0.0134(9) Uani 1 1 d . . . . .
N9 N 0.6791(2) 0.2459(2) 0.71986(16) 0.0261(10) Uani 1 1 d . . . . .
C26 C 0.2970(2) 0.0988(2) 0.67242(17) 0.0152(10) Uani 1 1 d . . . . .
C15 C 0.3747(2) 0.0175(2) 0.62172(16) 0.0148(10) Uani 1 1 d . . . . .
N2 N 0.5186(2) -0.0029(2) 0.84485(14) 0.0195(9) Uani 1 1 d . . . . .
N10 N 0.3084(2) 0.1876(2) 0.43678(15) 0.0222(9) Uani 1 1 d . . . . .
N12 N 0.2052(2) 0.2872(2) 0.50526(15) 0.0194(9) Uani 1 1 d . . . . .
N11 N 0.3353(2) 0.3776(2) 0.44978(15) 0.0214(9) Uani 1 1 d . . . . .
C30 C 0.3178(2) 0.3029(3) 0.69922(17) 0.0161(10) Uani 1 1 d . . . . .
H30 H 0.294144 0.338755 0.717855 0.019 Uiso 1 1 calc R U . . .
C18 C 0.4691(2) 0.0476(2) 0.59124(17) 0.0151(10) Uani 1 1 d . . . . .
C19 C 0.5211(2) 0.0958(2) 0.57596(17) 0.0156(10) Uani 1 1 d . . . . .
H19 H 0.553151 0.071908 0.557403 0.019 Uiso 1 1 calc R U . . .
N8 N 0.5928(2) 0.3638(2) 0.79718(16) 0.0254(10) Uani 1 1 d . . . . .
C4 C 0.3407(2) -0.0321(2) 0.70431(17) 0.0140(9) Uani 1 1 d . . . . .
C3 C 0.3146(2) 0.0196(2) 0.65138(17) 0.0155(10) Uani 1 1 d . . . . .
C41 C 0.4436(3) 0.2387(3) 0.81913(19) 0.0234(11) Uani 1 1 d . . . . .
H41 H 0.476558 0.262069 0.801197 0.028 Uiso 1 1 calc R U . . .
C31 C 0.3799(3) 0.4136(2) 0.67444(17) 0.0168(10) Uani 1 1 d . . . . .
H31 H 0.434208 0.420646 0.686120 0.020 Uiso 1 1 calc R U . . .
N13 N 0.5169(3) -0.3225(3) 0.7381(2) 0.0402(12) Uani 1 1 d . . . . .
C7 C 0.4111(3) -0.0661(3) 0.78802(17) 0.0185(10) Uani 1 1 d . . . . .
C20 C 0.5797(2) 0.2150(2) 0.56366(17) 0.0156(10) Uani 1 1 d . . . . .
H20 H 0.604184 0.253355 0.593989 0.019 Uiso 1 1 calc R U . . .
C17 C 0.4529(2) -0.0295(2) 0.57658(17) 0.0168(10) Uani 1 1 d . . . . .
H17 H 0.477706 -0.063144 0.557336 0.020 Uiso 1 1 calc R U . . .
C9 C 0.5813(3) -0.0041(3) 0.89743(17) 0.0198(11) Uani 1 1 d . . . . .
H9 H 0.605371 0.048342 0.900263 0.024 Uiso 1 1 calc R U . . .
C25 C 0.5372(3) 0.2622(3) 0.51199(19) 0.0209(11) Uani 1 1 d . . . . .
H25A H 0.498767 0.292980 0.522147 0.025 Uiso 1 1 calc R U . . .
H25B H 0.512886 0.225947 0.480759 0.025 Uiso 1 1 calc R U . . .
C28 C 0.2454(3) 0.1864(3) 0.71711(18) 0.0191(10) Uani 1 1 d . . . . .
H28 H 0.215678 0.210436 0.737596 0.023 Uiso 1 1 calc R U . . .
C27 C 0.2444(3) 0.1087(3) 0.70153(18) 0.0204(10) Uani 1 1 d . . . . .
H27 H 0.213485 0.069091 0.709203 0.025 Uiso 1 1 calc R U . . .
C16 C 0.3927(3) -0.0484(3) 0.59564(17) 0.0194(10) Uani 1 1 d . . . . .
H16 H 0.368426 -0.097512 0.591493 0.023 Uiso 1 1 calc R U . . .
C37 C 0.3828(3) 0.1308(3) 0.83615(19) 0.0262(12) Uani 1 1 d . . . . .
H37 H 0.371608 0.076663 0.830698 0.031 Uiso 1 1 calc R U . . .
C8 C 0.4720(3) -0.0592(3) 0.83805(18) 0.0207(11) Uani 1 1 d . . . . .
H8 H 0.478243 -0.097423 0.867258 0.025 Uiso 1 1 calc R U . . .
C2 C 0.2436(2) -0.0152(3) 0.61087(17) 0.0188(10) Uani 1 1 d . . . . .
H2A H 0.253659 -0.069308 0.600728 0.023 Uiso 1 1 calc R U . . .
H2B H 0.205878 -0.018072 0.631527 0.023 Uiso 1 1 calc R U . . .
C57 C 0.3245(3) 0.1210(3) 0.46610(19) 0.0242(11) Uani 1 1 d . . . . .
H57 H 0.329581 0.122387 0.505883 0.029 Uiso 1 1 calc R U . . .
C36 C 0.3524(3) 0.4420(3) 0.61300(19) 0.0259(12) Uani 1 1 d . . . . .
H36A H 0.298236 0.439637 0.600143 0.031 Uiso 1 1 calc R U . . .
H36B H 0.371318 0.407367 0.587982 0.031 Uiso 1 1 calc R U . . .
C24 C 0.5871(3) 0.3176(3) 0.4912(2) 0.0252(11) Uani 1 1 d . . . . .
H24A H 0.558167 0.345041 0.456390 0.030 Uiso 1 1 calc R U . . .
H24B H 0.607445 0.357410 0.520858 0.030 Uiso 1 1 calc R U . . .
C1 C 0.2128(3) 0.0316(3) 0.55597(18) 0.0273(12) Uani 1 1 d . . . . .
H1A H 0.166996 0.007645 0.533397 0.041 Uiso 1 1 calc R U . . .
H1B H 0.248309 0.031510 0.533797 0.041 Uiso 1 1 calc R U . . .
H1C H 0.203506 0.085530 0.565519 0.041 Uiso 1 1 calc R U . . .
C61 C 0.3022(3) 0.1833(3) 0.38076(19) 0.0304(13) Uani 1 1 d . . . . .
H61 H 0.289650 0.229451 0.358441 0.037 Uiso 1 1 calc R U . . .
C5 C 0.3097(3) -0.0986(3) 0.72069(18) 0.0205(11) Uani 1 1 d . . . . .
H5 H 0.266376 -0.124571 0.699537 0.025 Uiso 1 1 calc R U . . .
C21 C 0.6400(2) 0.1689(3) 0.54856(18) 0.0184(10) Uani 1 1 d . . . . .
H21A H 0.617823 0.131084 0.517792 0.022 Uiso 1 1 calc R U . . .
H21B H 0.668237 0.138963 0.582349 0.022 Uiso 1 1 calc R U . . .
C66 C 0.3944(3) 0.4231(3) 0.4662(2) 0.0248(11) Uani 1 1 d . . . . .
H66 H 0.427360 0.414875 0.503074 0.030 Uiso 1 1 calc R U . . .
C51 C 0.7023(3) 0.1744(3) 0.7127(2) 0.0355(13) Uani 1 1 d . . . . .
H51 H 0.673282 0.131069 0.717226 0.043 Uiso 1 1 calc R U . . .
C14 C 0.6378(3) -0.0640(3) 0.89254(19) 0.0283(12) Uani 1 1 d . . . . .
H14A H 0.654280 -0.052179 0.858528 0.034 Uiso 1 1 calc R U . . .
H14B H 0.615194 -0.116665 0.887338 0.034 Uiso 1 1 calc R U . . .
C23 C 0.6494(3) 0.2730(3) 0.47799(19) 0.0247(11) Uani 1 1 d . . . . .
H23A H 0.683377 0.310607 0.468075 0.030 Uiso 1 1 calc R U . . .
H23B H 0.629436 0.238562 0.444623 0.030 Uiso 1 1 calc R U . . .
C32 C 0.3508(3) 0.4663(3) 0.7136(2) 0.0266(12) Uani 1 1 d . . . . .
H32A H 0.368671 0.447579 0.753485 0.032 Uiso 1 1 calc R U . . .
H32B H 0.296633 0.465077 0.701921 0.032 Uiso 1 1 calc R U . . .
C62 C 0.2897(3) 0.3913(3) 0.39781(19) 0.0229(11) Uani 1 1 d . . . . .
H62 H 0.247121 0.359735 0.385288 0.028 Uiso 1 1 calc R U . . .
C22 C 0.6913(3) 0.2236(3) 0.5289(2) 0.0244(11) Uani 1 1 d . . . . .
H22A H 0.729018 0.192275 0.518111 0.029 Uiso 1 1 calc R U . . .
H22B H 0.716549 0.258473 0.560787 0.029 Uiso 1 1 calc R U . . .
C10 C 0.5593(3) -0.0153(3) 0.95201(18) 0.0288(12) Uani 1 1 d . . . . .
H10A H 0.533108 -0.065704 0.950154 0.035 Uiso 1 1 calc R U . . .
H10B H 0.525552 0.027138 0.955496 0.035 Uiso 1 1 calc R U . . .
C67 C 0.5460(3) -0.3385(3) 0.6961(2) 0.0404(15) Uani 1 1 d . . . . .
H67 H 0.565251 -0.389478 0.694733 0.049 Uiso 1 1 calc R U . . .
C35 C 0.3778(3) 0.5265(3) 0.6082(2) 0.0299(12) Uani 1 1 d . . . . .
H35A H 0.431786 0.527757 0.617307 0.036 Uiso 1 1 calc R U . . .
H35B H 0.357197 0.545248 0.568533 0.036 Uiso 1 1 calc R U . . .
C40 C 0.4126(3) 0.2856(3) 0.8519(2) 0.0308(12) Uani 1 1 d . . . . .
H40 H 0.424091 0.339754 0.856448 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3548(3) -0.1197(3) 0.77418(19) 0.0231(11) Uani 1 1 d . . . . .
H6 H 0.347962 -0.162687 0.796788 0.028 Uiso 1 1 calc R U . . .
C68 C 0.5503(3) -0.2866(3) 0.6548(2) 0.0369(14) Uani 1 1 d . . . . .
H68 H 0.572089 -0.300916 0.625879 0.044 Uiso 1 1 calc R U . . .
C39 C 0.3647(3) 0.2525(3) 0.8778(2) 0.0373(14) Uani 1 1 d . . . . .
H39 H 0.342568 0.283101 0.900868 0.045 Uiso 1 1 calc R U . . .
C71 C 0.4884(3) -0.2512(3) 0.7375(2) 0.0391(14) Uani 1 1 d . . . . .
H71 H 0.465607 -0.238749 0.766196 0.047 Uiso 1 1 calc R U . . .
C52 C 0.1998(3) 0.2719(3) 0.5575(2) 0.0311(13) Uani 1 1 d . . . . .
H52 H 0.243490 0.260726 0.586770 0.037 Uiso 1 1 calc R U . . .
C38 C 0.3494(3) 0.1739(3) 0.8697(2) 0.0357(14) Uani 1 1 d . . . . .
H38 H 0.316265 0.149455 0.886862 0.043 Uiso 1 1 calc R U . . .
C54 C 0.0713(3) 0.2861(3) 0.5299(2) 0.0342(13) Uani 1 1 d . . . . .
H54 H 0.025664 0.285608 0.538265 0.041 Uiso 1 1 calc R U . . .
C56 C 0.1420(3) 0.3021(3) 0.4655(2) 0.0279(12) Uani 1 1 d . . . . .
H56 H 0.143799 0.313833 0.427984 0.033 Uiso 1 1 calc R U . . .
C46 C 0.5781(3) 0.4371(3) 0.7797(2) 0.0295(12) Uani 1 1 d . . . . .
H46 H 0.560146 0.446417 0.739850 0.035 Uiso 1 1 calc R U . . .
C58 C 0.3342(3) 0.0506(3) 0.44234(19) 0.0282(12) Uani 1 1 d . . . . .
H58 H 0.344452 0.004648 0.465119 0.034 Uiso 1 1 calc R U . . .
C60 C 0.3131(3) 0.1152(3) 0.3540(2) 0.0368(14) Uani 1 1 d . . . . .
H60 H 0.309714 0.115416 0.314476 0.044 Uiso 1 1 calc R U . . .
C65 C 0.4104(3) 0.4814(3) 0.4328(2) 0.0300(12) Uani 1 1 d . . . . .
H65 H 0.453192 0.512423 0.446104 0.036 Uiso 1 1 calc R U . . .
C47 C 0.7212(3) 0.3059(4) 0.7126(2) 0.0413(15) Uani 1 1 d . . . . .
H47 H 0.705333 0.357743 0.716443 0.050 Uiso 1 1 calc R U . . .
Li1 Li 0.5853(5) 0.2647(5) 0.7416(3) 0.0264(19) Uani 1 1 d . . . . .
C33 C 0.3777(3) 0.5500(3) 0.7092(2) 0.0328(13) Uani 1 1 d . . . . .
H33A H 0.358382 0.584959 0.733833 0.039 Uiso 1 1 calc R U . . .
H33B H 0.431819 0.551176 0.723355 0.039 Uiso 1 1 calc R U . . .
C11 C 0.6265(3) -0.0149(3) 1.00475(18) 0.0317(13) Uani 1 1 d . . . . .
H11A H 0.650028 0.037254 1.008791 0.038 Uiso 1 1 calc R U . . .
H11B H 0.610823 -0.025000 1.039355 0.038 Uiso 1 1 calc R U . . .
C70 C 0.4898(3) -0.1948(3) 0.6981(2) 0.0397(15) Uani 1 1 d . . . . .
H70 H 0.469087 -0.144651 0.699875 0.048 Uiso 1 1 calc R U . . .
C42 C 0.6190(3) 0.3533(3) 0.8538(2) 0.0330(13) Uani 1 1 d . . . . .
H42 H 0.630549 0.301534 0.867548 0.040 Uiso 1 1 calc R U . . .
C59 C 0.3289(3) 0.0474(3) 0.3849(2) 0.0346(14) Uani 1 1 d . . . . .
H59 H 0.335964 -0.000405 0.367285 0.042 Uiso 1 1 calc R U . . .
C13 C 0.7043(3) -0.0641(3) 0.9460(2) 0.0351(13) Uani 1 1 d . . . . .
H13A H 0.738476 -0.106255 0.942603 0.042 Uiso 1 1 calc R U . . .
H13B H 0.730479 -0.013579 0.948623 0.042 Uiso 1 1 calc R U . . .
C63 C 0.3010(3) 0.4481(3) 0.3615(2) 0.0312(13) Uani 1 1 d . . . . .
H63 H 0.266969 0.455721 0.325037 0.037 Uiso 1 1 calc R U . . .
C55 C 0.0749(3) 0.3016(3) 0.4757(2) 0.0351(14) Uani 1 1 d . . . . .
H55 H 0.031673 0.311702 0.445726 0.042 Uiso 1 1 calc R U . . .
C64 C 0.3622(3) 0.4935(3) 0.3792(2) 0.0335(13) Uani 1 1 d . . . . .
H64 H 0.371667 0.533007 0.354880 0.040 Uiso 1 1 calc R U . . .
C44 C 0.6140(3) 0.4881(3) 0.8732(2) 0.0413(15) Uani 1 1 d . . . . .
H44 H 0.621489 0.530701 0.899212 0.050 Uiso 1 1 calc R U . . .
C45 C 0.5873(3) 0.5011(3) 0.8161(2) 0.0375(14) Uani 1 1 d . . . . .
H45 H 0.575205 0.552475 0.801614 0.045 Uiso 1 1 calc R U . . .
C53 C 0.1350(3) 0.2715(3) 0.5715(2) 0.0343(13) Uani 1 1 d . . . . .
H53 H 0.134477 0.261180 0.609531 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6812(3) -0.0765(3) 0.9997(2) 0.0325(13) Uani 1 1 d . . . . .
H12A H 0.659024 -0.129078 0.998700 0.039 Uiso 1 1 calc R U . . .
H12B H 0.724693 -0.073969 1.033415 0.039 Uiso 1 1 calc R U . . .
C43 C 0.6301(3) 0.4132(3) 0.8931(2) 0.0398(15) Uani 1 1 d . . . . .
H43 H 0.648389 0.402952 0.932809 0.048 Uiso 1 1 calc R U . . .
C34 C 0.3536(3) 0.5802(3) 0.6484(2) 0.0347(13) Uani 1 1 d . . . . .
H34A H 0.299613 0.584944 0.635770 0.042 Uiso 1 1 calc R U . . .
H34B H 0.374519 0.632952 0.646983 0.042 Uiso 1 1 calc R U . . .
C69 C 0.5218(3) -0.2124(3) 0.6564(2) 0.0437(16) Uani 1 1 d . . . . .
H69 H 0.524532 -0.174223 0.628832 0.052 Uiso 1 1 calc R U . . .
C50 C 0.7663(4) 0.1597(5) 0.6989(2) 0.058(2) Uani 1 1 d . . . . .
H50 H 0.780033 0.107461 0.693640 0.070 Uiso 1 1 calc R U . . .
Li2 Li 0.3074(5) 0.2815(5) 0.4907(3) 0.0224(18) Uani 1 1 d . . . . .
C48 C 0.7869(4) 0.2953(5) 0.6998(2) 0.065(2) Uani 1 1 d . . . . .
H48 H 0.815885 0.338936 0.695807 0.078 Uiso 1 1 calc R U . . .
C49 C 0.8094(4) 0.2199(7) 0.6929(3) 0.078(3) Uani 1 1 d . . . . .
H49 H 0.854214 0.210625 0.684225 0.094 Uiso 1 1 calc R U . . .
O2 O 0.37205(17) 0.24972(17) 0.56262(12) 0.0186(7) Uani 1 1 d . . . . .
O1 O 0.49608(16) 0.19390(16) 0.70808(11) 0.0153(7) Uani 1 1 d . . . . .
N14 N 0.0126(4) 0.1422(5) 0.6212(3) 0.102(2) Uani 1 1 d D U . . .
C72 C 0.0297(5) 0.1002(4) 0.5814(5) 0.092(3) Uani 1 1 d D U . . .
H72 H 0.072911 0.069342 0.590727 0.111 Uiso 1 1 calc R U . . .
C73 C -0.0148(6) 0.1015(5) 0.5273(4) 0.111(3) Uani 1 1 d D U . . .
H73 H -0.002153 0.071269 0.498870 0.134 Uiso 1 1 calc R U . . .
C74 C -0.0763(5) 0.1445(5) 0.5128(3) 0.099(4) Uani 1 1 d D U . . .
H74 H -0.107779 0.145535 0.474879 0.118 Uiso 1 1 calc R U . . .
C75 C -0.0904(4) 0.1850(5) 0.5541(4) 0.090(3) Uani 1 1 d D U . . .
H75 H -0.133943 0.215329 0.545659 0.108 Uiso 1 1 calc R U . . .
C76 C -0.0463(5) 0.1855(5) 0.6074(4) 0.077(2) Uani 1 1 d D U . . .
H76 H -0.057822 0.217524 0.635437 0.092 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 23 9 0.1059
-11 16 -17 0.2107
-12 5 -24 0.1959
2 -24 -5 0.1093
-24 -3 23 0.0115
25 3 -22 0.0394
13 -3 24 0.2437
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
N5 U1 Cl3 143.68(8) . . ?
N5 U1 N4 137.40(11) . . ?
N5 U1 N6 67.32(12) . . ?
N4 U1 Cl3 77.32(8) . . ?
N3 U1 Cl3 143.59(9) . . ?
N3 U1 N5 68.66(11) . . ?
N3 U1 N4 68.75(11) . . ?
N3 U1 N6 135.97(12) . . ?
N6 U1 Cl3 78.53(9) . . ?
N6 U1 N4 155.27(12) . . ?
O2 U1 Cl3 95.53(10) . . ?
O2 U1 N5 95.20(12) . . ?
O2 U1 N4 89.24(12) . . ?
O2 U1 N3 96.80(12) . . ?
O2 U1 N6 87.90(12) . . ?
O2 U1 O1 179.17(13) . . ?
O1 U1 Cl3 83.90(9) . . ?
O1 U1 N5 85.60(12) . . ?
O1 U1 N4 90.06(11) . . ?
O1 U1 N3 83.33(11) . . ?
O1 U1 N6 92.57(11) . . ?
Cl1 Dy1 Cl2 87.31(4) . . ?
N7 Dy1 Cl2 82.79(9) . . ?
N7 Dy1 Cl1 165.28(8) . . ?
N1 Dy1 Cl2 151.98(8) . . ?
N1 Dy1 Cl1 98.44(9) . . ?
N1 Dy1 N7 85.54(12) . . ?
N1 Dy1 N2 69.38(12) . . ?
N2 Dy1 Cl2 83.54(9) . . ?
N2 Dy1 Cl1 87.97(9) . . ?
N2 Dy1 N7 80.14(11) . . ?
O1 Dy1 Cl2 76.40(7) . . ?
O1 Dy1 Cl1 106.16(8) . . ?
O1 Dy1 N7 82.10(11) . . ?
O1 Dy1 N1 127.00(11) . . ?
O1 Dy1 N2 154.65(11) . . ?
Li1 Cl3 U1 76.40(17) . . ?
Li1 Cl2 Dy1 87.53(18) . . ?
C29 N5 U1 114.3(3) . . ?
C26 N5 U1 140.2(3) . . ?
C26 N5 C29 105.4(4) . . ?
C19 N4 U1 112.5(3) . . ?
C19 N4 C20 119.1(4) . . ?
C20 N4 U1 128.0(3) . . ?
C15 N3 U1 140.4(3) . . ?
C15 N3 C18 105.3(3) . . ?
C18 N3 U1 112.8(3) . . ?
C30 N6 U1 115.4(3) . . ?
C30 N6 C31 119.8(4) . . ?
C31 N6 U1 124.8(3) . . ?
C41 N7 Dy1 120.1(3) . . ?
C37 N7 Dy1 122.6(3) . . ?
C37 N7 C41 117.2(4) . . ?
C4 N1 Dy1 138.1(3) . . ?
C4 N1 C7 105.0(4) . . ?
C7 N1 Dy1 116.6(3) . . ?
N5 C29 C30 121.1(4) . . ?
C28 C29 N5 110.1(4) . . ?
C28 C29 C30 128.7(4) . . ?
C51 N9 C47 116.7(5) . . ?
C51 N9 Li1 122.1(4) . . ?
C47 N9 Li1 121.2(5) . . ?
N5 C26 C3 126.8(4) . . ?
N5 C26 C27 110.4(4) . . ?
C27 C26 C3 122.7(4) . . ?
N3 C15 C3 125.5(4) . . ?
N3 C15 C16 110.4(4) . . ?
C16 C15 C3 123.9(4) . . ?
C9 N2 Dy1 129.4(3) . . ?
C8 N2 Dy1 112.4(3) . . ?
C8 N2 C9 117.2(4) . . ?
C57 N10 C61 116.2(4) . . ?
C57 N10 Li2 111.1(3) . . ?
C61 N10 Li2 132.4(4) . . ?
C52 N12 C56 115.6(4) . . ?
C52 N12 Li2 119.0(4) . . ?
C56 N12 Li2 125.3(4) . . ?
C66 N11 C62 116.6(4) . . ?
C66 N11 Li2 128.9(4) . . ?
C62 N11 Li2 114.3(4) . . ?
N6 C30 C29 121.5(4) . . ?
N6 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
N3 C18 C19 121.8(4) . . ?
C17 C18 N3 110.4(4) . . ?
C17 C18 C19 127.5(4) . . ?
N4 C19 C18 124.0(4) . . ?
N4 C19 H19 118.0 . . ?
C18 C19 H19 118.0 . . ?
C46 N8 Li1 124.8(4) . . ?
C46 N8 C42 116.1(4) . . ?
C42 N8 Li1 118.9(4) . . ?
N1 C4 C3 118.2(4) . . ?
N1 C4 C5 110.9(4) . . ?
C5 C4 C3 130.8(4) . . ?
C26 C3 C15 116.8(4) . . ?
C26 C3 C4 106.2(3) . . ?
C26 C3 C2 108.8(4) . . ?
C15 C3 C4 106.4(4) . . ?
C15 C3 C2 109.0(3) . . ?
C4 C3 C2 109.4(3) . . ?
N7 C41 H41 118.3 . . ?
N7 C41 C40 123.5(5) . . ?
C40 C41 H41 118.3 . . ?
N6 C31 H31 106.3 . . ?
N6 C31 C36 109.4(3) . . ?
N6 C31 C32 117.6(4) . . ?
C36 C31 H31 106.3 . . ?
C36 C31 C32 110.2(4) . . ?
C32 C31 H31 106.3 . . ?
C67 N13 C71 116.0(5) . . ?
N1 C7 C8 118.5(4) . . ?
C6 C7 N1 110.9(4) . . ?
C6 C7 C8 130.6(4) . . ?
N4 C20 H20 107.1 . . ?
N4 C20 C25 109.1(4) . . ?
N4 C20 C21 116.7(4) . . ?
C25 C20 H20 107.1 . . ?
C25 C20 C21 109.4(3) . . ?
C21 C20 H20 107.1 . . ?
C18 C17 H17 126.9 . . ?
C18 C17 C16 106.3(4) . . ?
C16 C17 H17 126.9 . . ?
N2 C9 H9 106.8 . . ?
N2 C9 C14 110.8(4) . . ?
N2 C9 C10 114.0(4) . . ?
C14 C9 H9 106.8 . . ?
C14 C9 C10 111.3(4) . . ?
C10 C9 H9 106.8 . . ?
C20 C25 H25A 109.3 . . ?
C20 C25 H25B 109.3 . . ?
C20 C25 C24 111.7(4) . . ?
H25A C25 H25B 107.9 . . ?
C24 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
C29 C28 H28 126.7 . . ?
C27 C28 C29 106.6(4) . . ?
C27 C28 H28 126.7 . . ?
C26 C27 H27 126.2 . . ?
C28 C27 C26 107.5(4) . . ?
C28 C27 H27 126.2 . . ?
C15 C16 C17 107.6(4) . . ?
C15 C16 H16 126.2 . . ?
C17 C16 H16 126.2 . . ?
N7 C37 H37 118.6 . . ?
N7 C37 C38 122.7(5) . . ?
C38 C37 H37 118.6 . . ?
N2 C8 C7 122.3(4) . . ?
N2 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C1 C2 C3 114.0(4) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
N10 C57 H57 118.0 . . ?
N10 C57 C58 124.0(4) . . ?
C58 C57 H57 118.0 . . ?
C31 C36 H36A 109.6 . . ?
C31 C36 H36B 109.6 . . ?
C31 C36 C35 110.3(4) . . ?
H36A C36 H36B 108.1 . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C23 C24 C25 111.0(4) . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N10 C61 H61 118.4 . . ?
N10 C61 C60 123.3(5) . . ?
C60 C61 H61 118.4 . . ?
C4 C5 H5 126.8 . . ?
C6 C5 C4 106.4(4) . . ?
C6 C5 H5 126.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 C22 110.8(4) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
N11 C66 H66 118.2 . . ?
N11 C66 C65 123.6(4) . . ?
C65 C66 H66 118.2 . . ?
N9 C51 H51 118.3 . . ?
N9 C51 C50 123.4(6) . . ?
C50 C51 H51 118.3 . . ?
C9 C14 H14A 109.3 . . ?
C9 C14 H14B 109.3 . . ?
C9 C14 C13 111.5(4) . . ?
H14A C14 H14B 108.0 . . ?
C13 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C24 C23 C22 111.3(4) . . ?
H23A C23 H23B 108.0 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
C31 C32 C33 108.5(4) . . ?
H32A C32 H32B 108.4 . . ?
C33 C32 H32A 110.0 . . ?
C33 C32 H32B 110.0 . . ?
N11 C62 H62 118.0 . . ?
N11 C62 C63 124.0(5) . . ?
C63 C62 H62 118.0 . . ?
C21 C22 C23 111.2(4) . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C9 C10 C11 111.3(4) . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
N13 C67 H67 117.8 . . ?
N13 C67 C68 124.4(5) . . ?
C68 C67 H67 117.8 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C34 C35 C36 111.1(4) . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
C41 C40 H40 120.6 . . ?
C39 C40 C41 118.7(5) . . ?
C39 C40 H40 120.6 . . ?
C7 C6 C5 106.7(4) . . ?
C7 C6 H6 126.6 . . ?
C5 C6 H6 126.6 . . ?
C67 C68 H68 121.0 . . ?
C67 C68 C69 118.0(5) . . ?
C69 C68 H68 121.0 . . ?
C40 C39 H39 120.8 . . ?
C40 C39 C38 118.4(5) . . ?
C38 C39 H39 120.8 . . ?
N13 C71 H71 117.8 . . ?
N13 C71 C70 124.3(5) . . ?
C70 C71 H71 117.8 . . ?
N12 C52 H52 118.0 . . ?
N12 C52 C53 124.0(5) . . ?
C53 C52 H52 118.0 . . ?
C37 C38 H38 120.3 . . ?
C39 C38 C37 119.5(5) . . ?
C39 C38 H38 120.3 . . ?
C55 C54 H54 120.8 . . ?
C53 C54 H54 120.8 . . ?
C53 C54 C55 118.4(5) . . ?
N12 C56 H56 118.0 . . ?
N12 C56 C55 124.1(4) . . ?
C55 C56 H56 118.0 . . ?
N8 C46 H46 118.0 . . ?
N8 C46 C45 124.1(5) . . ?
C45 C46 H46 118.0 . . ?
C57 C58 H58 120.4 . . ?
C57 C58 C59 119.1(5) . . ?
C59 C58 H58 120.4 . . ?
C61 C60 H60 120.3 . . ?
C59 C60 C61 119.5(5) . . ?
C59 C60 H60 120.3 . . ?
C66 C65 H65 120.9 . . ?
C66 C65 C64 118.1(5) . . ?
C64 C65 H65 120.9 . . ?
N9 C47 H47 118.6 . . ?
N9 C47 C48 122.8(6) . . ?
C48 C47 H47 118.6 . . ?
Cl2 Li1 Cl3 164.3(3) . . ?
N9 Li1 Cl3 91.2(3) . . ?
N9 Li1 Cl2 94.1(3) . . ?
N9 Li1 N8 112.7(4) . . ?
N9 Li1 O1 119.5(4) . . ?
N8 Li1 Cl3 94.7(3) . . ?
N8 Li1 Cl2 96.8(3) . . ?
O1 Li1 Cl3 82.7(3) . . ?
O1 Li1 Cl2 81.8(3) . . ?
O1 Li1 N8 127.8(4) . . ?
C32 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 111.8(4) . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 110.9(4) . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C71 C70 H70 120.9 . . ?
C69 C70 C71 118.3(5) . . ?
C69 C70 H70 120.9 . . ?
N8 C42 H42 118.1 . . ?
N8 C42 C43 123.9(5) . . ?
C43 C42 H42 118.1 . . ?
C58 C59 H59 121.1 . . ?
C60 C59 C58 117.9(5) . . ?
C60 C59 H59 121.1 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 C14 111.3(4) . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C62 C63 H63 120.8 . . ?
C64 C63 C62 118.3(5) . . ?
C64 C63 H63 120.8 . . ?
C54 C55 H55 120.6 . . ?
C56 C55 C54 118.8(5) . . ?
C56 C55 H55 120.6 . . ?
C65 C64 H64 120.3 . . ?
C63 C64 C65 119.4(5) . . ?
C63 C64 H64 120.3 . . ?
C45 C44 H44 120.1 . . ?
C45 C44 C43 119.8(5) . . ?
C43 C44 H44 120.1 . . ?
C46 C45 H45 121.0 . . ?
C44 C45 C46 118.1(5) . . ?
C44 C45 H45 121.0 . . ?
C52 C53 H53 120.5 . . ?
C54 C53 C52 119.1(5) . . ?
C54 C53 H53 120.5 . . ?
C11 C12 C13 110.6(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C42 C43 H43 120.9 . . ?
C44 C43 C42 118.1(5) . . ?
C44 C43 H43 120.9 . . ?
C35 C34 C33 111.6(4) . . ?
C35 C34 H34A 109.3 . . ?
C35 C34 H34B 109.3 . . ?
C33 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C68 C69 H69 120.5 . . ?
C70 C69 C68 119.0(5) . . ?
C70 C69 H69 120.5 . . ?
C51 C50 H50 120.1 . . ?
C49 C50 C51 119.8(7) . . ?
C49 C50 H50 120.1 . . ?
N10 Li2 N12 108.8(4) . . ?
N11 Li2 N10 104.9(3) . . ?
N11 Li2 N12 115.3(4) . . ?
O2 Li2 N10 104.1(4) . . ?
O2 Li2 N12 104.2(4) . . ?
O2 Li2 N11 118.8(4) . . ?
C47 C48 H48 120.6 . . ?
C49 C48 C47 118.7(7) . . ?
C49 C48 H48 120.6 . . ?
C50 C49 C48 118.4(7) . . ?
C50 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
U1 O2 Li2 177.2(3) . . ?
U1 O1 Dy1 128.20(14) . . ?
U1 O1 Li1 117.0(3) . . ?
Li1 O1 Dy1 113.6(3) . . ?
C76 N14 C72 119.4(8) . . ?
N14 C72 H72 120.2 . . ?
N14 C72 C73 119.6(8) . . ?
C73 C72 H72 120.2 . . ?
C72 C73 H73 119.2 . . ?
C74 C73 C72 121.6(7) . . ?
C74 C73 H73 119.2 . . ?
C73 C74 H74 122.0 . . ?
C75 C74 C73 116.1(7) . . ?
C75 C74 H74 122.0 . . ?
C74 C75 H75 118.5 . . ?
C74 C75 C76 123.0(7) . . ?
C76 C75 H75 118.5 . . ?
N14 C76 C75 120.3(8) . . ?
N14 C76 H76 119.9 . . ?
C75 C76 H76 119.9 . . ?
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 Cl3 2.7726(11) . ?
U1 N5 2.504(4) . ?
U1 N4 2.595(4) . ?
U1 N3 2.498(3) . ?
U1 N6 2.581(4) . ?
U1 O2 1.849(3) . ?
U1 O1 1.940(3) . ?
Dy1 Cl2 2.6583(11) . ?
Dy1 Cl1 2.5804(12) . ?
Dy1 N7 2.555(4) . ?
Dy1 N1 2.359(4) . ?
Dy1 N2 2.525(3) . ?
Dy1 O1 2.267(3) . ?
Cl3 Li1 2.741(8) . ?
Cl2 Li1 2.577(8) . ?
N5 C29 1.401(5) . ?
N5 C26 1.360(5) . ?
N4 C19 1.285(5) . ?
N4 C20 1.477(5) . ?
N3 C15 1.363(5) . ?
N3 C18 1.401(5) . ?
N6 C30 1.291(5) . ?
N6 C31 1.480(5) . ?
N7 C41 1.341(6) . ?
N7 C37 1.330(6) . ?
N1 C4 1.367(5) . ?
N1 C7 1.384(5) . ?
C29 C30 1.419(6) . ?
C29 C28 1.388(6) . ?
N9 C51 1.329(6) . ?
N9 C47 1.345(7) . ?
N9 Li1 2.031(10) . ?
C26 C3 1.518(6) . ?
C26 C27 1.396(6) . ?
C15 C3 1.521(6) . ?
C15 C16 1.385(6) . ?
N2 C9 1.485(5) . ?
N2 C8 1.288(6) . ?
N10 C57 1.333(6) . ?
N10 C61 1.343(6) . ?
N10 Li2 2.080(8) . ?
N12 C52 1.336(6) . ?
N12 C56 1.338(6) . ?
N12 Li2 2.082(9) . ?
N11 C66 1.335(6) . ?
N11 C62 1.339(6) . ?
N11 Li2 2.069(8) . ?
C30 H30 0.9500 . ?
C18 C19 1.417(6) . ?
C18 C17 1.379(6) . ?
C19 H19 0.9500 . ?
N8 C46 1.327(6) . ?
N8 Li1 2.151(9) . ?
N8 C42 1.342(6) . ?
C4 C3 1.528(6) . ?
C4 C5 1.392(6) . ?
C3 C2 1.551(6) . ?
C41 H41 0.9500 . ?
C41 C40 1.381(7) . ?
C31 H31 1.0000 . ?
C31 C36 1.522(6) . ?
C31 C32 1.529(6) . ?
N13 C67 1.328(7) . ?
N13 C71 1.332(7) . ?
C7 C8 1.431(6) . ?
C7 C6 1.378(6) . ?
C20 H20 1.0000 . ?
C20 C25 1.522(6) . ?
C20 C21 1.524(6) . ?
C17 H17 0.9500 . ?
C17 C16 1.394(6) . ?
C9 H9 1.0000 . ?
C9 C14 1.516(6) . ?
C9 C10 1.520(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.528(6) . ?
C28 H28 0.9500 . ?
C28 C27 1.381(6) . ?
C27 H27 0.9500 . ?
C16 H16 0.9500 . ?
C37 H37 0.9500 . ?
C37 C38 1.384(7) . ?
C8 H8 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.528(6) . ?
C57 H57 0.9500 . ?
C57 C58 1.371(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.540(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.521(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C61 H61 0.9500 . ?
C61 C60 1.379(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.527(6) . ?
C66 H66 0.9500 . ?
C66 C65 1.376(7) . ?
C51 H51 0.9500 . ?
C51 C50 1.377(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.540(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.528(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.534(6) . ?
C62 H62 0.9500 . ?
C62 C63 1.373(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.537(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.362(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.508(7) . ?
C40 H40 0.9500 . ?
C40 C39 1.373(7) . ?
C6 H6 0.9500 . ?
C68 H68 0.9500 . ?
C68 C69 1.385(7) . ?
C39 H39 0.9500 . ?
C39 C38 1.377(8) . ?
C71 H71 0.9500 . ?
C71 C70 1.367(7) . ?
C52 H52 0.9500 . ?
C52 C53 1.372(7) . ?
C38 H38 0.9500 . ?
C54 H54 0.9500 . ?
C54 C55 1.371(7) . ?
C54 C53 1.367(7) . ?
C56 H56 0.9500 . ?
C56 C55 1.371(7) . ?
C46 H46 0.9500 . ?
C46 C45 1.389(7) . ?
C58 H58 0.9500 . ?
C58 C59 1.381(6) . ?
C60 H60 0.9500 . ?
C60 C59 1.369(7) . ?
C65 H65 0.9500 . ?
C65 C64 1.385(7) . ?
C47 H47 0.9500 . ?
C47 C48 1.386(9) . ?
Li1 O1 2.058(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.517(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.511(7) . ?
C70 H70 0.9500 . ?
C70 C69 1.362(8) . ?
C42 H42 0.9500 . ?
C42 C43 1.379(7) . ?
C59 H59 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.514(7) . ?
C63 H63 0.9500 . ?
C63 C64 1.364(7) . ?
C55 H55 0.9500 . ?
C64 H64 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.360(7) . ?
C44 C43 1.372(7) . ?
C45 H45 0.9500 . ?
C53 H53 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C43 H43 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C69 H69 0.9500 . ?
C50 H50 0.9500 . ?
C50 C49 1.350(10) . ?
Li2 O2 1.916(8) . ?
C48 H48 0.9500 . ?
C48 C49 1.384(11) . ?
C49 H49 0.9500 . ?
N14 C72 1.323(8) . ?
N14 C76 1.307(8) . ?
C72 H72 0.9500 . ?
C72 C73 1.352(9) . ?
C73 H73 0.9500 . ?
C73 C74 1.344(9) . ?
C74 H74 0.9500 . ?
C74 C75 1.315(8) . ?
C75 H75 0.9500 . ?
C75 C76 1.334(8) . ?
C76 H76 0.9500 . ?
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 N5 C29 C30 5.4(5) . . . . ?
U1 N5 C29 C28 -177.6(3) . . . . ?
U1 N5 C26 C3 0.6(7) . . . . ?
U1 N5 C26 C27 177.0(3) . . . . ?
U1 N4 C19 C18 -1.8(5) . . . . ?
U1 N4 C20 C25 -67.5(4) . . . . ?
U1 N4 C20 C21 167.9(3) . . . . ?
U1 N3 C15 C3 -18.9(7) . . . . ?
U1 N3 C15 C16 165.0(3) . . . . ?
U1 N3 C18 C19 4.2(5) . . . . ?
U1 N3 C18 C17 -170.2(3) . . . . ?
U1 N6 C30 C29 -4.1(5) . . . . ?
U1 N6 C31 C36 67.6(4) . . . . ?
U1 N6 C31 C32 -165.7(3) . . . . ?
Dy1 N7 C41 C40 -174.9(4) . . . . ?
Dy1 N7 C37 C38 174.8(4) . . . . ?
Dy1 N1 C4 C3 -9.3(6) . . . . ?
Dy1 N1 C4 C5 172.9(3) . . . . ?
Dy1 N1 C7 C8 6.2(5) . . . . ?
Dy1 N1 C7 C6 -174.9(3) . . . . ?
Dy1 N2 C9 C14 -91.6(4) . . . . ?
Dy1 N2 C9 C10 141.9(3) . . . . ?
Dy1 N2 C8 C7 -7.4(6) . . . . ?
N5 C29 C30 N6 -0.8(6) . . . . ?
N5 C29 C28 C27 -0.5(5) . . . . ?
N5 C26 C3 C15 -2.4(6) . . . . ?
N5 C26 C3 C4 116.0(4) . . . . ?
N5 C26 C3 C2 -126.3(4) . . . . ?
N5 C26 C27 C28 0.1(5) . . . . ?
N4 C20 C25 C24 173.5(4) . . . . ?
N4 C20 C21 C22 -177.5(4) . . . . ?
N3 C15 C3 C26 10.5(6) . . . . ?
N3 C15 C3 C4 -107.8(4) . . . . ?
N3 C15 C3 C2 134.2(4) . . . . ?
N3 C15 C16 C17 0.0(5) . . . . ?
N3 C18 C19 N4 -1.7(7) . . . . ?
N3 C18 C17 C16 0.9(5) . . . . ?
N6 C31 C36 C35 -169.8(4) . . . . ?
N6 C31 C32 C33 173.9(4) . . . . ?
N7 C41 C40 C39 -0.3(8) . . . . ?
N7 C37 C38 C39 0.3(8) . . . . ?
N1 C4 C3 C26 -63.2(5) . . . . ?
N1 C4 C3 C15 61.9(5) . . . . ?
N1 C4 C3 C2 179.5(4) . . . . ?
N1 C4 C5 C6 0.4(5) . . . . ?
N1 C7 C8 N2 1.3(7) . . . . ?
N1 C7 C6 C5 0.4(5) . . . . ?
C29 N5 C26 C3 -176.8(4) . . . . ?
C29 N5 C26 C27 -0.4(5) . . . . ?
C29 C28 C27 C26 0.3(5) . . . . ?
N9 C51 C50 C49 1.0(9) . . . . ?
N9 C47 C48 C49 1.4(9) . . . . ?
C26 N5 C29 C30 -176.5(4) . . . . ?
C26 N5 C29 C28 0.6(5) . . . . ?
C26 C3 C2 C1 65.0(5) . . . . ?
C15 N3 C18 C19 173.4(4) . . . . ?
C15 N3 C18 C17 -1.0(5) . . . . ?
C15 C3 C2 C1 -63.4(5) . . . . ?
N2 C9 C14 C13 178.2(4) . . . . ?
N2 C9 C10 C11 -179.3(4) . . . . ?
N10 C57 C58 C59 1.6(8) . . . . ?
N10 C61 C60 C59 2.1(9) . . . . ?
N12 C52 C53 C54 1.1(9) . . . . ?
N12 C56 C55 C54 1.1(8) . . . . ?
N11 C66 C65 C64 0.2(8) . . . . ?
N11 C62 C63 C64 0.2(8) . . . . ?
C30 N6 C31 C36 -109.9(4) . . . . ?
C30 N6 C31 C32 16.8(6) . . . . ?
C30 C29 C28 C27 176.2(4) . . . . ?
C18 N3 C15 C3 176.7(4) . . . . ?
C18 N3 C15 C16 0.6(5) . . . . ?
C18 C17 C16 C15 -0.5(5) . . . . ?
C19 N4 C20 C25 104.6(4) . . . . ?
C19 N4 C20 C21 -20.0(6) . . . . ?
C19 C18 C17 C16 -173.1(4) . . . . ?
N8 C46 C45 C44 1.0(9) . . . . ?
N8 C42 C43 C44 -0.5(9) . . . . ?
C4 N1 C7 C8 -179.0(4) . . . . ?
C4 N1 C7 C6 -0.1(5) . . . . ?
C4 C3 C2 C1 -179.4(4) . . . . ?
C4 C5 C6 C7 -0.4(5) . . . . ?
C3 C26 C27 C28 176.6(4) . . . . ?
C3 C15 C16 C17 -176.2(4) . . . . ?
C3 C4 C5 C6 -177.0(4) . . . . ?
C41 N7 C37 C38 -0.9(7) . . . . ?
C41 C40 C39 C38 -0.4(8) . . . . ?
C31 N6 C30 C29 173.6(4) . . . . ?
C31 C36 C35 C34 -55.9(6) . . . . ?
C31 C32 C33 C34 57.8(6) . . . . ?
N13 C67 C68 C69 -0.5(9) . . . . ?
N13 C71 C70 C69 0.6(9) . . . . ?
C7 N1 C4 C3 177.6(4) . . . . ?
C7 N1 C4 C5 -0.2(5) . . . . ?
C20 N4 C19 C18 -175.1(4) . . . . ?
C20 C25 C24 C23 56.0(5) . . . . ?
C20 C21 C22 C23 -57.2(5) . . . . ?
C17 C18 C19 N4 171.7(4) . . . . ?
C9 N2 C8 C7 -177.4(4) . . . . ?
C9 C14 C13 C12 55.1(6) . . . . ?
C9 C10 C11 C12 -56.3(6) . . . . ?
C25 C20 C21 C22 58.1(5) . . . . ?
C25 C24 C23 C22 -53.8(5) . . . . ?
C28 C29 C30 N6 -177.3(4) . . . . ?
C27 C26 C3 C15 -178.4(4) . . . . ?
C27 C26 C3 C4 -60.0(5) . . . . ?
C27 C26 C3 C2 57.7(5) . . . . ?
C16 C15 C3 C26 -174.0(4) . . . . ?
C16 C15 C3 C4 67.7(5) . . . . ?
C16 C15 C3 C2 -50.2(5) . . . . ?
C37 N7 C41 C40 0.9(7) . . . . ?
C8 N2 C9 C14 76.3(5) . . . . ?
C8 N2 C9 C10 -50.2(6) . . . . ?
C8 C7 C6 C5 179.0(5) . . . . ?
C57 N10 C61 C60 -1.4(8) . . . . ?
C57 C58 C59 C60 -0.8(8) . . . . ?
C36 C31 C32 C33 -59.8(5) . . . . ?
C36 C35 C34 C33 53.8(6) . . . . ?
C24 C23 C22 C21 54.8(5) . . . . ?
C61 N10 C57 C58 -0.4(8) . . . . ?
C61 C60 C59 C58 -0.9(9) . . . . ?
C5 C4 C3 C26 114.0(5) . . . . ?
C5 C4 C3 C15 -120.9(5) . . . . ?
C5 C4 C3 C2 -3.2(6) . . . . ?
C21 C20 C25 C24 -57.8(5) . . . . ?
C66 N11 C62 C63 0.3(7) . . . . ?
C66 C65 C64 C63 0.4(8) . . . . ?
C51 N9 C47 C48 -1.7(7) . . . . ?
C51 C50 C49 C48 -1.3(10) . . . . ?
C14 C9 C10 C11 54.5(6) . . . . ?
C14 C13 C12 C11 -56.7(6) . . . . ?
C32 C31 C36 C35 59.5(5) . . . . ?
C32 C33 C34 C35 -55.5(6) . . . . ?
C62 N11 C66 C65 -0.5(7) . . . . ?
C62 C63 C64 C65 -0.5(8) . . . . ?
C10 C9 C14 C13 -53.8(6) . . . . ?
C10 C11 C12 C13 57.2(6) . . . . ?
C67 N13 C71 C70 -2.2(9) . . . . ?
C67 C68 C69 C70 -1.2(9) . . . . ?
C40 C39 C38 C37 0.4(8) . . . . ?
C6 C7 C8 N2 -177.2(5) . . . . ?
C71 N13 C67 C68 2.1(9) . . . . ?
C71 C70 C69 C68 1.1(9) . . . . ?
C52 N12 C56 C55 -0.8(7) . . . . ?
C56 N12 C52 C53 -0.4(8) . . . . ?
C46 N8 C42 C43 0.7(8) . . . . ?
C47 N9 C51 C50 0.5(7) . . . . ?
C47 C48 C49 C50 0.1(10) . . . . ?
Li1 N9 C51 C50 -178.8(5) . . . . ?
Li1 N9 C47 C48 177.6(5) . . . . ?
Li1 N8 C46 C45 -176.0(5) . . . . ?
Li1 N8 C42 C43 176.1(5) . . . . ?
C42 N8 C46 C45 -0.9(8) . . . . ?
C55 C54 C53 C52 -0.7(8) . . . . ?
C45 C44 C43 C42 0.6(9) . . . . ?
C53 C54 C55 C56 -0.3(8) . . . . ?
C43 C44 C45 C46 -0.8(9) . . . . ?
Li2 N10 C57 C58 -175.1(5) . . . . ?
Li2 N10 C61 C60 171.9(5) . . . . ?
Li2 N12 C52 C53 -177.8(5) . . . . ?
Li2 N12 C56 C55 176.5(5) . . . . ?
Li2 N11 C66 C65 173.8(5) . . . . ?
Li2 N11 C62 C63 -174.8(5) . . . . ?
N14 C72 C73 C74 -0.1(12) . . . . ?
C72 N14 C76 C75 2.7(12) . . . . ?
C72 C73 C74 C75 0.1(13) . . . . ?
C73 C74 C75 C76 1.2(13) . . . . ?
C74 C75 C76 N14 -2.7(13) . . . . ?
C76 N14 C72 C73 -1.3(11) . . . . ?
loop_
_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
0.2846 23.1391 9.0700 -0.0236 -0.9315 0.3630
-10.5377 16.4041 -16.5877 -0.0202 -0.7641 -0.6448
-12.1526 4.9591 -24.2335 -0.0090 -0.3176 -0.9482
1.5794 -23.7972 -5.3155 0.0249 0.9761 -0.2161
-24.0729 -2.8242 22.9849 0.9996 -0.0257 -0.0089
24.5199 2.9337 -21.8960 -0.9984 0.0257 0.0505
12.6853 -2.9539 24.2102 -0.0181 0.2394 0.9707
