#------------------------------------------------------------------------------
#$Date: 2024-11-04 22:28:55 +0200 (Mon, 04 Nov 2024) $
#$Revision: 295760 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/73/7717380.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_7717380
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         'C51 H62 Li N9 O2 U'
_chemical_formula_sum            'C51 H62 Li N9 O2 U'
_chemical_formula_weight         1078.06
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-11
_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                 108.143(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3220(7)
_cell_length_b                   13.2763(4)
_cell_length_c                   20.5072(9)
_cell_measurement_reflns_used    9284
_cell_measurement_temperature    119.99(11)
_cell_measurement_theta_max      26.0820
_cell_measurement_theta_min      3.6190
_cell_volume                     4740.3(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      119.99(11)
_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 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  53.00   1.00   40.00    --  -15.66  44.00 -21.00   86
  2  ω    -51.00  35.00   1.00   40.00    --   17.38 -44.00-171.00   86
  3  ω      0.00  86.00   1.00   40.00    --   17.38  44.00 -21.00   86
  4  ω    -88.00 -39.00   1.00   40.00    --  -15.66-178.00 -30.00   49
  5  ω    -39.00  11.00   1.00   40.00    --  -15.66 -77.00 -60.00   50
  6  ω    -20.00  56.00   1.00   40.00    --   17.38 -99.00-180.00   76
  7  ω     -9.00  39.00   1.00   40.00    --   17.38  77.00-150.00   48
  8  ω     -9.00  18.00   1.00   40.00    --   17.38  77.00 120.00   27
;
_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      0.0406514000
_diffrn_orient_matrix_UB_12      0.0033310000
_diffrn_orient_matrix_UB_13      0.0100194000
_diffrn_orient_matrix_UB_21      -0.0026612000
_diffrn_orient_matrix_UB_22      0.0294108000
_diffrn_orient_matrix_UB_23      -0.0295370000
_diffrn_orient_matrix_UB_31      -0.0012706000
_diffrn_orient_matrix_UB_32      0.0444528000
_diffrn_orient_matrix_UB_33      0.0187558000
_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  0.0769
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50829
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         3.284
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.593
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2168
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0399
_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)+(0.0179P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7881
_reflns_number_total             10030
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           to334_refinalize
_cod_database_code               7717380
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H62 Li N9 O2 U'
_chemical_oxdiff_usercomment     'Precipitation from pyridine'
_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   0.903
_shelx_estimated_absorpt_t_min   0.642
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C20(H20), C31(H31), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C21(H21A,H21B), C32(H32A,H32B), C13(H13A,H13B), C2(H2A,H2B),
 C14(H14A,H14B), C12(H12A,H12B), C35(H35A,H35B), C33(H33A,H33B), C11(H11A,H11B),
  C34(H34A,H34B), C22(H22A,H22B), C25(H25A,H25B), C10(H10A,H10B), C23(H23A,
 H23B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C19(H19), C30(H30), C37(H37), C17(H17), C28(H28), C16(H16),
 C47(H47), C48(H48), C49(H49), C27(H27), C40(H40), C8(H8), C6(H6), C50(H50),
 C42(H42), C38(H38), C45(H45), C43(H43), C51(H51), C46(H46), C44(H44), C39(H39)
2.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 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.839
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.54090(2) 0.48420(2) 0.37142(2) 0.01013(5) Uani 1 1 d . . . . .
N7 N 0.4167(2) 0.4010(2) 0.37591(17) 0.0133(8) Uani 1 1 d . . . . .
N4 N 0.46032(19) 0.6365(2) 0.38517(16) 0.0108(8) Uani 1 1 d . . . . .
N3 N 0.60903(18) 0.6444(2) 0.37811(16) 0.0095(7) Uani 1 1 d . . . . .
N6 N 0.5628(2) 0.2983(2) 0.35394(17) 0.0124(8) Uani 1 1 d . . . . .
N5 N 0.66285(19) 0.4539(2) 0.35082(16) 0.0118(8) Uani 1 1 d . . . . .
N1 N 0.86881(19) 0.7062(2) 0.42296(17) 0.0116(8) Uani 1 1 d . . . . .
C41 C 0.4100(2) 0.3655(3) 0.4359(2) 0.0138(10) Uani 1 1 d . . . . .
H41 H 0.452046 0.373244 0.476669 0.017 Uiso 1 1 calc R U . . .
C29 C 0.6656(2) 0.3615(3) 0.3189(2) 0.0130(9) Uani 1 1 d . . . . .
C19 C 0.4886(2) 0.7218(3) 0.3736(2) 0.0126(9) Uani 1 1 d . . . . .
H19 H 0.458029 0.780815 0.368385 0.015 Uiso 1 1 calc R U . . .
N9 N 0.9564(2) 0.6537(2) 0.60055(18) 0.0195(9) Uani 1 1 d . . . . .
C30 C 0.6145(2) 0.2843(3) 0.3238(2) 0.0123(9) Uani 1 1 d . . . . .
H30 H 0.618204 0.220193 0.304461 0.015 Uiso 1 1 calc R U . . .
C20 C 0.3819(2) 0.6365(3) 0.3913(2) 0.0118(9) Uani 1 1 d . . . . .
H20 H 0.375741 0.571421 0.413619 0.014 Uiso 1 1 calc R U . . .
C31 C 0.5187(2) 0.2113(3) 0.3667(2) 0.0120(9) Uani 1 1 d . . . . .
H31 H 0.493499 0.234598 0.400766 0.014 Uiso 1 1 calc R U . . .
C26 C 0.7251(2) 0.5065(3) 0.34892(19) 0.0104(8) Uani 1 1 d . . . . .
N2 N 1.0035(2) 0.8189(2) 0.49122(18) 0.0148(8) Uani 1 1 d . . . . .
C18 C 0.5632(2) 0.7295(3) 0.3684(2) 0.0130(10) Uani 1 1 d . . . . .
N8 N 0.8526(2) 0.8607(2) 0.56188(18) 0.0183(8) Uani 1 1 d . . . . .
C15 C 0.6784(2) 0.6750(3) 0.37487(19) 0.0103(9) Uani 1 1 d . . . . .
C37 C 0.3558(2) 0.3877(3) 0.3189(2) 0.0161(10) Uani 1 1 d . . . . .
H37 H 0.359662 0.410929 0.276256 0.019 Uiso 1 1 calc R U . . .
C3 C 0.7469(2) 0.6042(3) 0.3897(2) 0.0097(9) Uani 1 1 d . . . . .
C36 C 0.4541(2) 0.1790(3) 0.3033(2) 0.0143(10) Uani 1 1 d . . . . .
H36A H 0.423129 0.238476 0.282241 0.017 Uiso 1 1 calc R U . . .
H36B H 0.476045 0.149457 0.269188 0.017 Uiso 1 1 calc R U . . .
C17 C 0.6048(2) 0.8132(3) 0.3590(2) 0.0146(10) Uani 1 1 d . . . . .
H17 H 0.587027 0.880725 0.352090 0.017 Uiso 1 1 calc R U . . .
C4 C 0.8125(2) 0.6585(3) 0.3731(2) 0.0098(9) Uani 1 1 d . . . . .
C28 C 0.7306(2) 0.3593(3) 0.2977(2) 0.0160(10) Uani 1 1 d . . . . .
H28 H 0.746476 0.305047 0.275117 0.019 Uiso 1 1 calc R U . . .
C5 C 0.8196(2) 0.6747(3) 0.3079(2) 0.0122(9) Uani 1 1 d . . . . .
C16 C 0.6771(2) 0.7789(3) 0.3618(2) 0.0140(10) Uani 1 1 d . . . . .
H16 H 0.717972 0.818239 0.356050 0.017 Uiso 1 1 calc R U . . .
C21 C 0.3662(2) 0.7210(3) 0.4362(2) 0.0167(10) Uani 1 1 d . . . . .
H21A H 0.405433 0.719150 0.482066 0.020 Uiso 1 1 calc R U . . .
H21B H 0.369753 0.787119 0.415066 0.020 Uiso 1 1 calc R U . . .
C47 C 1.0028(2) 0.5834(3) 0.5877(2) 0.0214(11) Uani 1 1 d . . . . .
H47 H 1.024631 0.596147 0.552172 0.026 Uiso 1 1 calc R U . . .
C32 C 0.5678(2) 0.1200(3) 0.3991(2) 0.0136(9) Uani 1 1 d . . . . .
H32A H 0.589987 0.088891 0.365651 0.016 Uiso 1 1 calc R U . . .
H32B H 0.610502 0.141419 0.439686 0.016 Uiso 1 1 calc R U . . .
C48 C 1.0206(2) 0.4937(3) 0.6232(2) 0.0216(10) Uani 1 1 d . . . . .
H48 H 1.053588 0.445952 0.612264 0.026 Uiso 1 1 calc R U . . .
C13 C 1.1488(2) 0.9853(3) 0.6192(2) 0.0216(10) Uani 1 1 d . . . . .
H13A H 1.153642 1.040121 0.588017 0.026 Uiso 1 1 calc R U . . .
H13B H 1.147454 1.016239 0.662674 0.026 Uiso 1 1 calc R U . . .
C49 C 0.9893(3) 0.4754(3) 0.6747(2) 0.0279(11) Uani 1 1 d . . . . .
H49 H 0.999825 0.413851 0.699544 0.033 Uiso 1 1 calc R U . . .
C27 C 0.7681(2) 0.4508(3) 0.3155(2) 0.0147(9) Uani 1 1 d . . . . .
H27 H 0.813779 0.471684 0.306809 0.018 Uiso 1 1 calc R U . . .
C40 C 0.3442(3) 0.3184(3) 0.4395(2) 0.0180(10) Uani 1 1 d . . . . .
H40 H 0.341125 0.294186 0.482121 0.022 Uiso 1 1 calc R U . . .
C2 C 0.7692(2) 0.5746(3) 0.46685(19) 0.0121(9) Uani 1 1 d . . . . .
H2A H 0.788951 0.635151 0.494958 0.014 Uiso 1 1 calc R U . . .
H2B H 0.722353 0.552394 0.477039 0.014 Uiso 1 1 calc R U . . .
C14 C 1.0735(2) 0.9274(3) 0.5862(2) 0.0194(10) Uani 1 1 d . . . . .
H14A H 1.065605 0.878019 0.619527 0.023 Uiso 1 1 calc R U . . .
H14B H 1.029896 0.975236 0.574631 0.023 Uiso 1 1 calc R U . . .
C8 C 0.9810(2) 0.8069(3) 0.4256(2) 0.0156(10) Uani 1 1 d . . . . .
H8 H 1.011242 0.835984 0.400367 0.019 Uiso 1 1 calc R U . . .
C12 C 1.2178(2) 0.9166(3) 0.6333(2) 0.0231(11) Uani 1 1 d . . . . .
H12A H 1.217391 0.868983 0.670397 0.028 Uiso 1 1 calc R U . . .
H12B H 1.265221 0.957412 0.649567 0.028 Uiso 1 1 calc R U . . .
C9 C 1.0754(2) 0.8728(3) 0.5217(2) 0.0152(10) Uani 1 1 d . . . . .
H9 H 1.081487 0.923929 0.487993 0.018 Uiso 1 1 calc R U . . .
C35 C 0.4030(2) 0.1019(3) 0.3225(2) 0.0190(10) Uani 1 1 d . . . . .
H35A H 0.363594 0.078165 0.280311 0.023 Uiso 1 1 calc R U . . .
H35B H 0.376198 0.134345 0.352052 0.023 Uiso 1 1 calc R U . . .
C33 C 0.5169(2) 0.0440(3) 0.4205(2) 0.0168(10) Uani 1 1 d . . . . .
H33A H 0.547801 -0.016168 0.440351 0.020 Uiso 1 1 calc R U . . .
H33B H 0.498127 0.074239 0.456369 0.020 Uiso 1 1 calc R U . . .
C11 C 1.2186(2) 0.8575(3) 0.5704(2) 0.0210(10) Uani 1 1 d . . . . .
H11A H 1.261444 0.808457 0.583273 0.025 Uiso 1 1 calc R U . . .
H11B H 1.227722 0.904249 0.536053 0.025 Uiso 1 1 calc R U . . .
C7 C 0.9137(2) 0.7525(3) 0.3884(2) 0.0139(9) Uani 1 1 d . . . . .
C6 C 0.8847(2) 0.7347(3) 0.3180(2) 0.0152(10) Uani 1 1 d . . . . .
H6 H 0.905200 0.758717 0.283712 0.018 Uiso 1 1 calc R U . . .
C50 C 0.9428(3) 0.5463(3) 0.6903(2) 0.0298(12) Uani 1 1 d . . . . .
H50 H 0.921348 0.535861 0.726357 0.036 Uiso 1 1 calc R U . . .
C1 C 0.8291(2) 0.4919(3) 0.4884(2) 0.0190(10) Uani 1 1 d . . . . .
H1A H 0.807900 0.429075 0.464962 0.028 Uiso 1 1 calc R U . . .
H1B H 0.843220 0.482013 0.538161 0.028 Uiso 1 1 calc R U . . .
H1C H 0.874682 0.511085 0.476048 0.028 Uiso 1 1 calc R U . . .
C42 C 0.7796(3) 0.8826(3) 0.5283(2) 0.0238(11) Uani 1 1 d . . . . .
H42 H 0.757546 0.854991 0.483732 0.029 Uiso 1 1 calc R U . . .
C38 C 0.2883(3) 0.3422(3) 0.3195(2) 0.0215(11) Uani 1 1 d . . . . .
H38 H 0.246347 0.335433 0.278513 0.026 Uiso 1 1 calc R U . . .
C45 C 0.8412(3) 0.9634(3) 0.6538(3) 0.0329(13) Uani 1 1 d . . . . .
H45 H 0.864944 0.991240 0.698033 0.039 Uiso 1 1 calc R U . . .
C43 C 0.7340(3) 0.9436(3) 0.5547(3) 0.0312(12) Uani 1 1 d . . . . .
H43 H 0.682114 0.957406 0.528945 0.037 Uiso 1 1 calc R U . . .
C34 C 0.4485(2) 0.0118(3) 0.3602(2) 0.0202(10) Uani 1 1 d . . . . .
H34A H 0.414358 -0.031624 0.377083 0.024 Uiso 1 1 calc R U . . .
H34B H 0.466998 -0.028280 0.327757 0.024 Uiso 1 1 calc R U . . .
C51 C 0.9285(3) 0.6332(3) 0.6517(2) 0.0242(11) Uani 1 1 d . . . . .
H51 H 0.896206 0.682234 0.662463 0.029 Uiso 1 1 calc R U . . .
C22 C 0.2869(3) 0.7087(3) 0.4438(2) 0.0227(11) Uani 1 1 d . . . . .
H22A H 0.276908 0.765448 0.471170 0.027 Uiso 1 1 calc R U . . .
H22B H 0.285343 0.645595 0.468979 0.027 Uiso 1 1 calc R U . . .
C46 C 0.8820(3) 0.9019(3) 0.6235(2) 0.0261(11) Uani 1 1 d . . . . .
H46 H 0.934192 0.888272 0.648204 0.031 Uiso 1 1 calc R U . . .
C25 C 0.3205(2) 0.6382(3) 0.3211(2) 0.0164(10) Uani 1 1 d . . . . .
H25A H 0.330384 0.583063 0.292452 0.020 Uiso 1 1 calc R U . . .
H25B H 0.323267 0.702819 0.297972 0.020 Uiso 1 1 calc R U . . .
C44 C 0.7661(3) 0.9835(3) 0.6192(3) 0.0366(13) Uani 1 1 d . . . . .
H44 H 0.736416 1.024515 0.639351 0.044 Uiso 1 1 calc R U . . .
C39 C 0.2833(3) 0.3071(3) 0.3808(2) 0.0234(11) Uani 1 1 d . . . . .
H39 H 0.237723 0.274877 0.382578 0.028 Uiso 1 1 calc R U . . .
C10 C 1.1436(2) 0.8019(3) 0.5386(2) 0.0168(10) Uani 1 1 d . . . . .
H10A H 1.137511 0.749561 0.570916 0.020 Uiso 1 1 calc R U . . .
H10B H 1.145159 0.767739 0.496115 0.020 Uiso 1 1 calc R U . . .
C23 C 0.2241(3) 0.7058(3) 0.3746(2) 0.0258(11) Uani 1 1 d . . . . .
H23A H 0.174116 0.691597 0.381769 0.031 Uiso 1 1 calc R U . . .
H23B H 0.220504 0.772469 0.352153 0.031 Uiso 1 1 calc R U . . .
C24 C 0.2404(3) 0.6256(3) 0.3280(2) 0.0230(11) Uani 1 1 d . . . . .
H24A H 0.201570 0.630282 0.281992 0.028 Uiso 1 1 calc R U . . .
H24B H 0.236020 0.558098 0.346910 0.028 Uiso 1 1 calc R U . . .
Li1 Li 0.9167(4) 0.7572(5) 0.5222(4) 0.0192(17) Uani 1 1 d . . . . .
O1 O 0.57822(15) 0.46755(17) 0.46130(13) 0.0125(6) Uani 1 1 d . . . . .
O2 O 0.49313(15) 0.49461(17) 0.28211(13) 0.0139(6) Uani 1 1 d . . . . .
H5 H 0.785(2) 0.650(2) 0.2642(19) 0.014(11) Uiso 1 1 d . . . . .
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'
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
4 17 -12 0.0691
-10 0 29 0.0568
-5 -16 14 0.0476
5 -16 -15 0.0443
10 1 -29 0.0573
-3 16 16 0.0576
-25 -1 0 0.0016
6 -16 -16 0.0459
25 1 0 0.0328
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
N7 U1 N4 77.74(10) . . ?
N3 U1 N7 144.80(10) . . ?
N3 U1 N4 67.10(10) . . ?
N3 U1 N6 138.66(11) . . ?
N6 U1 N7 76.53(10) . . ?
N6 U1 N4 154.14(11) . . ?
N5 U1 N7 144.14(10) . . ?
N5 U1 N4 137.66(10) . . ?
N5 U1 N3 70.97(10) . . ?
N5 U1 N6 67.75(10) . . ?
O1 U1 N7 88.17(11) . . ?
O1 U1 N4 91.89(10) . . ?
O1 U1 N3 91.45(11) . . ?
O1 U1 N6 89.93(10) . . ?
O1 U1 N5 94.72(11) . . ?
O1 U1 O2 173.13(12) . . ?
O2 U1 N7 84.97(11) . . ?
O2 U1 N4 86.35(11) . . ?
O2 U1 N3 93.97(11) . . ?
O2 U1 N6 88.78(10) . . ?
O2 U1 N5 91.04(11) . . ?
C41 N7 U1 121.0(3) . . ?
C37 N7 U1 121.9(3) . . ?
C37 N7 C41 117.1(4) . . ?
C19 N4 U1 113.0(3) . . ?
C19 N4 C20 117.9(3) . . ?
C20 N4 U1 128.0(2) . . ?
C18 N3 U1 115.1(2) . . ?
C15 N3 U1 136.6(2) . . ?
C15 N3 C18 106.6(3) . . ?
C30 N6 U1 112.2(2) . . ?
C30 N6 C31 119.5(3) . . ?
C31 N6 U1 127.9(2) . . ?
C29 N5 U1 113.3(3) . . ?
C26 N5 U1 138.6(2) . . ?
C26 N5 C29 106.6(3) . . ?
C4 N1 C7 104.7(3) . . ?
C4 N1 Li1 152.0(4) . . ?
C7 N1 Li1 102.8(3) . . ?
N7 C41 H41 118.9 . . ?
N7 C41 C40 122.2(4) . . ?
C40 C41 H41 118.9 . . ?
N5 C29 C30 118.8(4) . . ?
C28 C29 N5 108.9(3) . . ?
C28 C29 C30 131.2(4) . . ?
N4 C19 H19 119.0 . . ?
N4 C19 C18 122.0(4) . . ?
C18 C19 H19 119.0 . . ?
C47 N9 Li1 113.6(4) . . ?
C51 N9 C47 115.8(4) . . ?
C51 N9 Li1 128.3(4) . . ?
N6 C30 C29 121.9(3) . . ?
N6 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
N4 C20 H20 106.8 . . ?
N4 C20 C21 114.8(3) . . ?
N4 C20 C25 111.7(3) . . ?
C21 C20 H20 106.8 . . ?
C25 C20 H20 106.8 . . ?
C25 C20 C21 109.6(3) . . ?
N6 C31 H31 106.1 . . ?
N6 C31 C36 113.1(3) . . ?
N6 C31 C32 114.6(3) . . ?
C36 C31 H31 106.1 . . ?
C36 C31 C32 110.1(3) . . ?
C32 C31 H31 106.1 . . ?
N5 C26 C3 120.2(3) . . ?
N5 C26 C27 110.5(3) . . ?
C27 C26 C3 128.6(4) . . ?
C8 N2 C9 117.5(3) . . ?
C8 N2 Li1 104.3(3) . . ?
C9 N2 Li1 138.2(3) . . ?
N3 C18 C19 119.4(3) . . ?
N3 C18 C17 109.6(4) . . ?
C17 C18 C19 130.9(4) . . ?
C42 N8 Li1 121.8(4) . . ?
C46 N8 C42 116.6(4) . . ?
C46 N8 Li1 121.5(4) . . ?
N3 C15 C3 122.2(3) . . ?
N3 C15 C16 110.0(3) . . ?
C16 C15 C3 127.5(4) . . ?
N7 C37 H37 118.3 . . ?
N7 C37 C38 123.3(4) . . ?
C38 C37 H37 118.3 . . ?
C26 C3 C2 106.4(3) . . ?
C15 C3 C26 110.9(3) . . ?
C15 C3 C4 108.8(3) . . ?
C15 C3 C2 107.4(3) . . ?
C4 C3 C26 111.6(3) . . ?
C4 C3 C2 111.7(3) . . ?
C31 C36 H36A 109.6 . . ?
C31 C36 H36B 109.6 . . ?
H36A C36 H36B 108.1 . . ?
C35 C36 C31 110.3(3) . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
C18 C17 H17 126.6 . . ?
C16 C17 C18 106.9(3) . . ?
C16 C17 H17 126.6 . . ?
N1 C4 C3 121.2(4) . . ?
N1 C4 C5 111.8(4) . . ?
C5 C4 C3 126.8(4) . . ?
C29 C28 H28 126.2 . . ?
C27 C28 C29 107.5(3) . . ?
C27 C28 H28 126.2 . . ?
C4 C5 H5 126(2) . . ?
C6 C5 C4 106.0(4) . . ?
C6 C5 H5 128(2) . . ?
C15 C16 H16 126.6 . . ?
C17 C16 C15 106.9(4) . . ?
C17 C16 H16 126.6 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 C20 110.3(3) . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
N9 C47 H47 118.1 . . ?
N9 C47 C48 123.8(4) . . ?
C48 C47 H47 118.1 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 C31 108.6(3) . . ?
C33 C32 H32A 110.0 . . ?
C33 C32 H32B 110.0 . . ?
C47 C48 H48 120.9 . . ?
C49 C48 C47 118.2(4) . . ?
C49 C48 H48 120.9 . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C12 C13 C14 111.4(3) . . ?
C48 C49 H49 120.1 . . ?
C48 C49 C50 119.7(4) . . ?
C50 C49 H49 120.1 . . ?
C26 C27 H27 126.8 . . ?
C28 C27 C26 106.4(4) . . ?
C28 C27 H27 126.8 . . ?
C41 C40 H40 120.4 . . ?
C39 C40 C41 119.2(4) . . ?
C39 C40 H40 120.4 . . ?
C3 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C1 C2 C3 114.6(3) . . ?
C1 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C13 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C9 C14 C13 111.1(4) . . ?
C9 C14 H14A 109.4 . . ?
C9 C14 H14B 109.4 . . ?
N2 C8 H8 117.9 . . ?
N2 C8 C7 124.2(4) . . ?
C7 C8 H8 117.9 . . ?
C13 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C13 C12 C11 112.2(4) . . ?
H12A C12 H12B 107.9 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
N2 C9 C14 110.3(3) . . ?
N2 C9 H9 108.5 . . ?
N2 C9 C10 111.3(3) . . ?
C14 C9 H9 108.5 . . ?
C14 C9 C10 109.8(3) . . ?
C10 C9 H9 108.5 . . ?
C36 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
C36 C35 C34 112.1(3) . . ?
H35A C35 H35B 107.9 . . ?
C34 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 111.9(3) . . ?
C34 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C12 C11 C10 111.7(4) . . ?
H11A C11 H11B 107.9 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
N1 C7 C8 120.2(4) . . ?
N1 C7 C6 111.0(4) . . ?
C6 C7 C8 128.7(4) . . ?
C5 C6 C7 106.5(4) . . ?
C5 C6 H6 126.8 . . ?
C7 C6 H6 126.8 . . ?
C49 C50 H50 121.2 . . ?
C49 C50 C51 117.6(4) . . ?
C51 C50 H50 121.2 . . ?
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 . . ?
N8 C42 H42 118.2 . . ?
N8 C42 C43 123.7(4) . . ?
C43 C42 H42 118.2 . . ?
C37 C38 H38 120.9 . . ?
C39 C38 C37 118.2(4) . . ?
C39 C38 H38 120.9 . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C44 C45 C46 118.8(5) . . ?
C42 C43 H43 121.0 . . ?
C44 C43 C42 118.0(4) . . ?
C44 C43 H43 121.0 . . ?
C35 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C33 C34 C35 112.0(3) . . ?
C33 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
N9 C51 C50 124.9(4) . . ?
N9 C51 H51 117.5 . . ?
C50 C51 H51 117.5 . . ?
C21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C21 C22 C23 112.2(4) . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
N8 C46 C45 123.8(5) . . ?
N8 C46 H46 118.1 . . ?
C45 C46 H46 118.1 . . ?
C20 C25 H25A 109.4 . . ?
C20 C25 H25B 109.4 . . ?
C20 C25 C24 111.1(3) . . ?
H25A C25 H25B 108.0 . . ?
C24 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C45 C44 C43 119.0(5) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C40 C39 H39 120.0 . . ?
C38 C39 C40 120.0(4) . . ?
C38 C39 H39 120.0 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 C9 111.6(3) . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 C22 111.4(4) . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C23 C24 C25 111.3(4) . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N1 Li1 N9 119.2(3) . . ?
N1 Li1 N8 118.3(4) . . ?
N9 Li1 N8 103.5(3) . . ?
N2 Li1 N1 87.6(3) . . ?
N2 Li1 N9 112.7(4) . . ?
N2 Li1 N8 115.6(3) . . ?
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 N7 2.557(3) . ?
U1 N4 2.570(3) . ?
U1 N3 2.449(3) . ?
U1 N6 2.544(3) . ?
U1 N5 2.433(3) . ?
U1 O1 1.769(3) . ?
U1 O2 1.772(3) . ?
N7 C41 1.357(5) . ?
N7 C37 1.354(5) . ?
N4 C19 1.298(5) . ?
N4 C20 1.481(5) . ?
N3 C18 1.384(5) . ?
N3 C15 1.356(5) . ?
N6 C30 1.296(5) . ?
N6 C31 1.479(5) . ?
N5 C29 1.398(5) . ?
N5 C26 1.349(5) . ?
N1 C4 1.361(5) . ?
N1 C7 1.385(5) . ?
N1 Li1 2.063(8) . ?
C41 H41 0.9500 . ?
C41 C40 1.381(6) . ?
C29 C30 1.413(5) . ?
C29 C28 1.389(6) . ?
C19 H19 0.9500 . ?
C19 C18 1.406(6) . ?
N9 C47 1.342(5) . ?
N9 C51 1.331(5) . ?
N9 Li1 2.068(8) . ?
C30 H30 0.9500 . ?
C20 H20 1.0000 . ?
C20 C21 1.534(5) . ?
C20 C25 1.526(5) . ?
C31 H31 1.0000 . ?
C31 C36 1.522(5) . ?
C31 C32 1.532(5) . ?
C26 C3 1.528(5) . ?
C26 C27 1.404(5) . ?
N2 C8 1.288(5) . ?
N2 C9 1.458(5) . ?
N2 Li1 2.057(8) . ?
C18 C17 1.395(5) . ?
N8 C42 1.331(6) . ?
N8 C46 1.328(5) . ?
N8 Li1 2.128(8) . ?
C15 C3 1.520(5) . ?
C15 C16 1.405(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.380(6) . ?
C3 C4 1.528(5) . ?
C3 C2 1.557(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.519(5) . ?
C17 H17 0.9500 . ?
C17 C16 1.384(6) . ?
C4 C5 1.401(5) . ?
C28 H28 0.9500 . ?
C28 C27 1.387(5) . ?
C5 C6 1.394(5) . ?
C5 H5 0.98(4) . ?
C16 H16 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.517(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.528(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.370(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.539(5) . ?
C13 C12 1.511(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.373(6) . ?
C27 H27 0.9500 . ?
C40 H40 0.9500 . ?
C40 C39 1.371(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.516(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C9 1.517(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.428(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.516(5) . ?
C9 H9 1.0000 . ?
C9 C10 1.518(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.523(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.522(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.517(5) . ?
C7 C6 1.395(5) . ?
C6 H6 0.9500 . ?
C50 H50 0.9500 . ?
C50 C51 1.377(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C42 H42 0.9500 . ?
C42 C43 1.390(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.369(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.378(6) . ?
C45 C44 1.364(7) . ?
C43 H43 0.9500 . ?
C43 C44 1.376(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C51 H51 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.524(6) . ?
C46 H46 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.527(6) . ?
C44 H44 0.9500 . ?
C39 H39 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.521(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
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 N7 C41 C40 -178.7(3) . . . . ?
U1 N7 C37 C38 179.3(3) . . . . ?
U1 N4 C19 C18 -12.4(5) . . . . ?
U1 N4 C20 C21 147.6(3) . . . . ?
U1 N4 C20 C25 -86.9(3) . . . . ?
U1 N3 C18 C19 16.4(5) . . . . ?
U1 N3 C18 C17 -167.7(3) . . . . ?
U1 N3 C15 C3 -22.0(6) . . . . ?
U1 N3 C15 C16 162.6(3) . . . . ?
U1 N6 C30 C29 15.7(5) . . . . ?
U1 N6 C31 C36 93.0(4) . . . . ?
U1 N6 C31 C32 -139.8(3) . . . . ?
U1 N5 C29 C30 -21.8(4) . . . . ?
U1 N5 C29 C28 168.8(3) . . . . ?
U1 N5 C26 C3 25.5(6) . . . . ?
U1 N5 C26 C27 -163.6(3) . . . . ?
N7 C41 C40 C39 -0.1(6) . . . . ?
N7 C37 C38 C39 -1.3(6) . . . . ?
N4 C19 C18 N3 -2.1(6) . . . . ?
N4 C19 C18 C17 -177.1(4) . . . . ?
N4 C20 C21 C22 -175.3(3) . . . . ?
N4 C20 C25 C24 173.3(3) . . . . ?
N3 C18 C17 C16 1.1(5) . . . . ?
N3 C15 C3 C26 50.1(5) . . . . ?
N3 C15 C3 C4 173.2(3) . . . . ?
N3 C15 C3 C2 -65.8(4) . . . . ?
N3 C15 C16 C17 1.7(5) . . . . ?
N6 C31 C36 C35 -170.3(3) . . . . ?
N6 C31 C32 C33 170.3(3) . . . . ?
N5 C29 C30 N6 3.6(6) . . . . ?
N5 C29 C28 C27 -0.8(5) . . . . ?
N5 C26 C3 C15 -51.1(5) . . . . ?
N5 C26 C3 C4 -172.6(3) . . . . ?
N5 C26 C3 C2 65.4(4) . . . . ?
N5 C26 C27 C28 -1.3(4) . . . . ?
N1 C4 C5 C6 0.9(4) . . . . ?
N1 C7 C6 C5 -0.4(4) . . . . ?
C41 N7 C37 C38 1.2(6) . . . . ?
C41 C40 C39 C38 0.0(6) . . . . ?
C29 N5 C26 C3 -170.1(3) . . . . ?
C29 N5 C26 C27 0.8(4) . . . . ?
C29 C28 C27 C26 1.2(5) . . . . ?
C19 N4 C20 C21 -45.3(5) . . . . ?
C19 N4 C20 C25 80.2(4) . . . . ?
C19 C18 C17 C16 176.4(4) . . . . ?
N9 C47 C48 C49 -0.2(7) . . . . ?
C30 N6 C31 C36 -79.2(5) . . . . ?
C30 N6 C31 C32 48.1(5) . . . . ?
C30 C29 C28 C27 -168.4(4) . . . . ?
C20 N4 C19 C18 178.6(4) . . . . ?
C20 C21 C22 C23 -56.5(4) . . . . ?
C20 C25 C24 C23 56.3(4) . . . . ?
C31 N6 C30 C29 -171.0(4) . . . . ?
C31 C36 C35 C34 -54.9(4) . . . . ?
C31 C32 C33 C34 57.4(4) . . . . ?
C26 N5 C29 C30 169.3(3) . . . . ?
C26 N5 C29 C28 0.0(4) . . . . ?
C26 C3 C4 N1 -141.6(3) . . . . ?
C26 C3 C4 C5 45.1(5) . . . . ?
C26 C3 C2 C1 52.5(4) . . . . ?
N2 C8 C7 N1 -1.8(6) . . . . ?
N2 C8 C7 C6 -179.7(4) . . . . ?
N2 C9 C10 C11 180.0(3) . . . . ?
C18 N3 C15 C3 174.3(3) . . . . ?
C18 N3 C15 C16 -1.1(4) . . . . ?
C18 C17 C16 C15 -1.7(5) . . . . ?
N8 C42 C43 C44 0.0(7) . . . . ?
C15 N3 C18 C19 -175.9(4) . . . . ?
C15 N3 C18 C17 0.0(4) . . . . ?
C15 C3 C4 N1 95.7(4) . . . . ?
C15 C3 C4 C5 -77.7(4) . . . . ?
C15 C3 C2 C1 171.3(3) . . . . ?
C37 N7 C41 C40 -0.5(5) . . . . ?
C37 C38 C39 C40 0.6(6) . . . . ?
C3 C26 C27 C28 168.6(4) . . . . ?
C3 C15 C16 C17 -173.4(4) . . . . ?
C3 C4 C5 C6 174.8(3) . . . . ?
C36 C31 C32 C33 -60.9(4) . . . . ?
C36 C35 C34 C33 51.3(5) . . . . ?
C4 N1 C7 C8 -177.4(3) . . . . ?
C4 N1 C7 C6 0.9(4) . . . . ?
C4 C3 C2 C1 -69.6(4) . . . . ?
C4 C5 C6 C7 -0.3(4) . . . . ?
C28 C29 C30 N6 170.2(4) . . . . ?
C16 C15 C3 C26 -135.4(4) . . . . ?
C16 C15 C3 C4 -12.2(5) . . . . ?
C16 C15 C3 C2 108.8(4) . . . . ?
C21 C20 C25 C24 -58.4(4) . . . . ?
C21 C22 C23 C24 54.0(5) . . . . ?
C47 N9 C51 C50 -1.1(7) . . . . ?
C47 C48 C49 C50 -1.1(7) . . . . ?
C32 C31 C36 C35 60.1(4) . . . . ?
C32 C33 C34 C35 -53.0(5) . . . . ?
C48 C49 C50 C51 1.2(7) . . . . ?
C13 C14 C9 N2 -179.8(3) . . . . ?
C13 C14 C9 C10 57.2(4) . . . . ?
C13 C12 C11 C10 -52.9(5) . . . . ?
C49 C50 C51 N9 -0.1(7) . . . . ?
C27 C26 C3 C15 139.9(4) . . . . ?
C27 C26 C3 C4 18.4(5) . . . . ?
C27 C26 C3 C2 -103.7(4) . . . . ?
C2 C3 C4 N1 -22.6(5) . . . . ?
C2 C3 C4 C5 164.0(3) . . . . ?
C14 C13 C12 C11 52.6(5) . . . . ?
C14 C9 C10 C11 -57.6(4) . . . . ?
C8 N2 C9 C14 150.3(3) . . . . ?
C8 N2 C9 C10 -87.6(4) . . . . ?
C8 C7 C6 C5 177.7(4) . . . . ?
C12 C13 C14 C9 -55.2(5) . . . . ?
C12 C11 C10 C9 55.5(5) . . . . ?
C9 N2 C8 C7 177.4(3) . . . . ?
C7 N1 C4 C3 -175.4(3) . . . . ?
C7 N1 C4 C5 -1.1(4) . . . . ?
C42 N8 C46 C45 1.0(7) . . . . ?
C42 C43 C44 C45 1.2(7) . . . . ?
C51 N9 C47 C48 1.3(6) . . . . ?
C22 C23 C24 C25 -53.3(5) . . . . ?
C46 N8 C42 C43 -1.1(6) . . . . ?
C46 C45 C44 C43 -1.3(7) . . . . ?
C25 C20 C21 C22 58.2(4) . . . . ?
C44 C45 C46 N8 0.2(7) . . . . ?
Li1 N1 C4 C3 -6.2(8) . . . . ?
Li1 N1 C4 C5 168.1(6) . . . . ?
Li1 N1 C7 C8 7.8(4) . . . . ?
Li1 N1 C7 C6 -173.9(3) . . . . ?
Li1 N9 C47 C48 -163.1(4) . . . . ?
Li1 N9 C51 C50 160.6(4) . . . . ?
Li1 N2 C8 C7 -5.6(5) . . . . ?
Li1 N2 C9 C14 -25.3(6) . . . . ?
Li1 N2 C9 C10 96.8(5) . . . . ?
Li1 N8 C42 C43 174.9(4) . . . . ?
Li1 N8 C46 C45 -175.0(4) . . . . ?
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
4.2588 17.0437 -11.8956 0.1107 0.8413 0.5291
-9.7688 -0.2883 28.8375 -0.1091 -0.8343 0.5405
-4.9890 -16.3250 14.0808 -0.1161 -0.8828 -0.4553
4.9736 -15.8798 -15.3226 -0.0042 -0.0277 -0.9996
9.7646 1.0290 -28.7954 0.1119 0.8548 -0.5067
-3.3342 15.6100 15.9389 0.0762 -0.0028 0.9971
-24.5807 -1.0399 0.3073 -0.9996 0.0258 -0.0092
6.3272 -15.5311 -16.0245 0.0449 -0.0003 -0.9990
24.5807 1.0399 -0.3073 0.9996 -0.0258 0.0092
