#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:40:52 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252762 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/38/7703886.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_7703886
loop_
_publ_author_name
'Gyton, Matthew R.'
'Leverett, Anthony R.'
'Cole, Marcus L.'
'McKay, Alasdair I.'
_publ_section_title
;
 Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and
 spectroscopic study.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5653
_journal_page_last               5661
_journal_paper_doi               10.1039/d0dt00285b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C32 H50 Li N3 O2'
_chemical_formula_sum            'C32 H50 Li N3 O2'
_chemical_formula_weight         515.69
_chemical_name_systematic        '[Li(THF)2(N3Dipp2)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-14 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.063(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8789(9)
_cell_length_b                   18.6075(9)
_cell_length_c                   19.5150(8)
_cell_measurement_reflns_used    8242
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.31
_cell_volume                     6397.4(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            78234
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.139
_diffrn_reflns_theta_min         1.565
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1022 before and 0.0798 after correction. The Ratio of minimum to maximum transmission is 0.8757. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         14123
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0621
_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)+(0.0750P)²+2.0450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7373
_reflns_number_total             14123
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           5(THF)2
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_database_code               7703886
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64-C63 \\sim C63-C62 \\sim C62-C61
 with sigma of 0.02
 O4-C64 \\sim O4-C61
 with sigma of 0.02
 O4-C63 \\sim O4-C62
 with sigma of 0.04
 C63-C61 \\sim C64-C62
 with sigma of 0.04
 C64A-C63A \\sim C63A-C62A \\sim C62A-C61A
 with sigma of 0.02
 O4A-C64A \\sim O4A-C61A
 with sigma of 0.02
 O4A-C63A \\sim O4A-C62A
 with sigma of 0.04
 C63A-C61A \\sim C64A-C62A
 with sigma of 0.04
 O4-Li3 \\sim O4A-Li3
 with sigma of 0.02
 C30-C31 \\sim C30-C31A \\sim C32-C31A \\sim C32-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C64 \\sim C63 \\sim C62 \\sim C61: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O4A \\sim C64A \\sim C63A \\sim C62A \\sim C61A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C32 \\sim C31 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C32 \\sim C31A \\sim C30: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C64, C63, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, C64A, C63A, C62A, C61A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31A, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4A)=Sof(C64A)=Sof(H64C)=Sof(H64D)=Sof(C63A)=Sof(H63C)=Sof(H63D)=
 Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C61A)=Sof(H61C)=Sof(H61D)=1-FVAR(1)
 Sof(O4)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C62)=
 Sof(H62A)=Sof(H62B)=Sof(C61)=Sof(H61A)=Sof(H61B)=FVAR(1)
 Sof(H32C)=Sof(H32D)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=1-FVAR(2)
 Sof(H32A)=Sof(H32B)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C39(H39), C22(H22), C51(H51), C54(H54), C42(H42), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C57(H57A,H57B), C26(H26A,H26B), C25(H25A,H25B), C29(H29A,
 H29B), C60(H60A,H60B), C27(H27A,H27B), C32(H32A,H32B), C32(H32C,H32D),
 C30(H30A,H30B), C30(H30C,H30D), C58(H58A,H58B), C59(H59A,H59B), C31(H31A,H31B),
  C64(H64A,H64B), C63(H63A,H63B), C62(H62A,H62B), C61(H61A,H61B), C64A(H64C,
 H64D), C63A(H63C,H63D), C62A(H62C,H62D), C61A(H61C,H61D), C31A(H31C,H31D)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C47(H47), C17(H17), C3(H3), C35(H35), C4(H4), C49(H49),
 C48(H48), C5(H5), C37(H37), C36(H36)
6.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C55(H55A,H55B,H55C), C41(H41A,H41B,H41C), C53(H53A,H53B,H53C),
 C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C),
  C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
N1 N 0.24681(10) 0.20966(9) 0.19096(9) 0.0292(4) Uani 1 1 d . . . . .
N3 N 0.16534(10) 0.23868(9) 0.08559(9) 0.0298(4) Uani 1 1 d . . . . .
N2 N 0.17842(10) 0.19779(9) 0.14361(9) 0.0290(4) Uani 1 1 d . . . . .
N5 N 0.30317(10) 0.70593(9) 0.33651(9) 0.0314(4) Uani 1 1 d . . . . .
N4 N 0.30523(10) 0.74259(9) 0.39482(9) 0.0322(4) Uani 1 1 d . . . . .
N6 N 0.23824(10) 0.71513(9) 0.28281(9) 0.0331(4) Uani 1 1 d . . . . .
O3 O 0.12740(9) 0.75248(9) 0.38505(9) 0.0501(4) Uani 1 1 d . . . . .
O1 O 0.31493(9) 0.37211(9) 0.17147(9) 0.0504(4) Uani 1 1 d . . . . .
C13 C 0.09407(12) 0.22542(11) 0.02904(10) 0.0294(5) Uani 1 1 d . . . . .
C1 C 0.26390(12) 0.17362(11) 0.25927(11) 0.0300(5) Uani 1 1 d . . . . .
C33 C 0.37189(12) 0.73165(12) 0.45630(11) 0.0336(5) Uani 1 1 d . . . . .
C14 C 0.07480(12) 0.15835(11) -0.00534(11) 0.0336(5) Uani 1 1 d . . . . .
C45 C 0.23524(12) 0.67974(11) 0.21726(11) 0.0316(5) Uani 1 1 d . . . . .
C46 C 0.19126(12) 0.61759(12) 0.19544(11) 0.0347(5) Uani 1 1 d . . . . .
C50 C 0.27243(13) 0.70926(12) 0.17295(12) 0.0380(5) Uani 1 1 d . . . . .
C34 C 0.39952(13) 0.66328(12) 0.48443(12) 0.0396(6) Uani 1 1 d . . . . .
C2 C 0.32715(12) 0.12810(11) 0.28177(11) 0.0349(5) Uani 1 1 d . . . . .
O2 O 0.32781(10) 0.26079(10) 0.06509(10) 0.0594(5) Uani 1 1 d . . . . .
C7 C 0.36600(12) 0.10813(12) 0.22868(12) 0.0389(5) Uani 1 1 d . . . . .
H7 H 0.357313 0.148437 0.192686 0.047 Uiso 1 1 calc R . . . .
C15 C 0.00465(13) 0.15090(13) -0.06155(12) 0.0420(6) Uani 1 1 d . . . . .
H15 H -0.009433 0.105457 -0.084634 0.050 Uiso 1 1 calc R . . . .
C6 C 0.22363(13) 0.18847(11) 0.30655(12) 0.0352(5) Uani 1 1 d . . . . .
C16 C -0.04504(14) 0.20792(14) -0.08464(13) 0.0465(6) Uani 1 1 d . . . . .
H16 H -0.092981 0.201573 -0.122750 0.056 Uiso 1 1 calc R . . . .
C18 C 0.04432(12) 0.28433(12) 0.00498(11) 0.0336(5) Uani 1 1 d . . . . .
C38 C 0.40908(13) 0.79390(12) 0.49280(12) 0.0393(6) Uani 1 1 d . . . . .
C19 C 0.12906(14) 0.09490(12) 0.01529(12) 0.0397(6) Uani 1 1 d . . . . .
H19 H 0.180254 0.114088 0.045548 0.048 Uiso 1 1 calc R . . . .
C47 C 0.18522(13) 0.58557(12) 0.12940(12) 0.0411(6) Uani 1 1 d . . . . .
H47 H 0.154851 0.543715 0.113772 0.049 Uiso 1 1 calc R . . . .
C39 C 0.36077(15) 0.59398(12) 0.44867(13) 0.0443(6) Uani 1 1 d . . . . .
H39 H 0.309436 0.606822 0.412699 0.053 Uiso 1 1 calc R . . . .
C17 C -0.02443(13) 0.27424(13) -0.05184(12) 0.0418(6) Uani 1 1 d . . . . .
H17 H -0.058121 0.313748 -0.068601 0.050 Uiso 1 1 calc R . . . .
C22 C 0.06769(13) 0.35736(12) 0.04037(12) 0.0403(6) Uani 1 1 d . . . . .
H22 H 0.102999 0.349268 0.092024 0.048 Uiso 1 1 calc R . . . .
C3 C 0.35012(14) 0.09787(13) 0.35133(12) 0.0461(6) Uani 1 1 d . . . . .
H3 H 0.392941 0.066855 0.367011 0.055 Uiso 1 1 calc R . . . .
C51 C 0.15235(14) 0.58496(13) 0.24380(13) 0.0447(6) Uani 1 1 d . . . . .
H51 H 0.159800 0.618885 0.285561 0.054 Uiso 1 1 calc R . . . .
C54 C 0.31925(15) 0.77700(14) 0.19583(13) 0.0494(7) Uani 1 1 d . . . . .
H54 H 0.305335 0.799973 0.235580 0.059 Uiso 1 1 calc R . . . .
C35 C 0.46493(15) 0.65964(15) 0.54670(13) 0.0548(7) Uani 1 1 d . . . . .
H35 H 0.484550 0.613838 0.565721 0.066 Uiso 1 1 calc R . . . .
C4 C 0.31189(16) 0.11207(14) 0.39795(13) 0.0530(7) Uani 1 1 d . . . . .
H4 H 0.328643 0.091305 0.445591 0.064 Uiso 1 1 calc R . . . .
C49 C 0.26562(15) 0.67456(13) 0.10798(13) 0.0462(6) Uani 1 1 d . . . . .
H49 H 0.291230 0.693375 0.077979 0.055 Uiso 1 1 calc R . . . .
C48 C 0.22219(14) 0.61304(13) 0.08609(12) 0.0456(6) Uani 1 1 d . . . . .
H48 H 0.217962 0.589929 0.041378 0.055 Uiso 1 1 calc R . . . .
C42 C 0.38046(15) 0.86744(12) 0.46151(13) 0.0464(6) Uani 1 1 d . . . . .
H42 H 0.323854 0.864537 0.439181 0.056 Uiso 1 1 calc R . . . .
C10 C 0.15705(14) 0.24013(12) 0.28429(13) 0.0422(6) Uani 1 1 d . . . . .
H10 H 0.123809 0.227614 0.232948 0.051 Uiso 1 1 calc R . . . .
C5 C 0.24913(15) 0.15654(13) 0.37549(12) 0.0471(6) Uani 1 1 d . . . . .
H5 H 0.222796 0.165499 0.407950 0.057 Uiso 1 1 calc R . . . .
C37 C 0.47390(15) 0.78651(15) 0.55520(13) 0.0539(7) Uani 1 1 d . . . . .
H37 H 0.499245 0.828291 0.580131 0.065 Uiso 1 1 calc R . . . .
C40 C 0.40505(16) 0.55820(14) 0.40610(14) 0.0566(7) Uani 1 1 d . . . . .
H40A H 0.405297 0.589798 0.366012 0.085 Uiso 1 1 calc GR . . . .
H40B H 0.380923 0.512425 0.385784 0.085 Uiso 1 1 calc GR . . . .
H40C H 0.457355 0.549414 0.439189 0.085 Uiso 1 1 calc GR . . . .
C12 C 0.18391(16) 0.31749(13) 0.28313(15) 0.0572(7) Uani 1 1 d . . . . .
H12A H 0.217819 0.331196 0.332526 0.086 Uiso 1 1 calc GR . . . .
H12B H 0.139926 0.349724 0.267131 0.086 Uiso 1 1 calc GR . . . .
H12C H 0.211203 0.321133 0.249003 0.086 Uiso 1 1 calc GR . . . .
C11 C 0.10811(15) 0.23522(15) 0.33196(14) 0.0552(7) Uani 1 1 d . . . . .
H11A H 0.090060 0.185774 0.331454 0.083 Uiso 1 1 calc GR . . . .
H11B H 0.064521 0.267627 0.312473 0.083 Uiso 1 1 calc GR . . . .
H11C H 0.138429 0.249127 0.382464 0.083 Uiso 1 1 calc GR . . . .
C36 C 0.50199(17) 0.72003(16) 0.58149(14) 0.0633(8) Uani 1 1 d . . . . .
H36 H 0.546984 0.715911 0.623674 0.076 Uiso 1 1 calc R . . . .
C20 C 0.10698(15) 0.04079(13) 0.06259(14) 0.0551(7) Uani 1 1 d . . . . .
H20A H 0.106163 0.064607 0.107088 0.083 Uiso 1 1 calc GR . . . .
H20B H 0.144056 0.001537 0.076237 0.083 Uiso 1 1 calc GR . . . .
H20C H 0.056500 0.021391 0.034896 0.083 Uiso 1 1 calc GR . . . .
C28 C 0.32011(17) 0.43841(14) 0.13808(15) 0.0627(8) Uani 1 1 d . . . . .
H28A H 0.269638 0.461640 0.117911 0.075 Uiso 1 1 calc R . . . .
H28B H 0.339132 0.430762 0.097522 0.075 Uiso 1 1 calc R . . . .
C24 C 0.11089(16) 0.39870(14) 0.00082(14) 0.0563(7) Uani 1 1 d . . . . .
H24A H 0.155441 0.370930 0.002061 0.084 Uiso 1 1 calc GR . . . .
H24B H 0.127300 0.445067 0.025178 0.084 Uiso 1 1 calc GR . . . .
H24C H 0.077811 0.406791 -0.050312 0.084 Uiso 1 1 calc GR . . . .
C21 C 0.13672(18) 0.05862(14) -0.05175(15) 0.0620(8) Uani 1 1 d . . . . .
H21A H 0.088284 0.036299 -0.081122 0.093 Uiso 1 1 calc GR . . . .
H21B H 0.176288 0.021682 -0.035734 0.093 Uiso 1 1 calc GR . . . .
H21C H 0.150498 0.094563 -0.081493 0.093 Uiso 1 1 calc GR . . . .
C57 C 0.15319(18) 0.71033(17) 0.45070(16) 0.0687(9) Uani 1 1 d . . . . .
H57A H 0.140701 0.733813 0.490462 0.082 Uiso 1 1 calc R . . . .
H57B H 0.208678 0.702332 0.467612 0.082 Uiso 1 1 calc R . . . .
C43 C 0.40903(19) 0.88627(15) 0.40061(15) 0.0686(8) Uani 1 1 d . . . . .
H43A H 0.464427 0.890883 0.420881 0.103 Uiso 1 1 calc GR . . . .
H43B H 0.386498 0.931893 0.378085 0.103 Uiso 1 1 calc GR . . . .
H43C H 0.394665 0.848234 0.363388 0.103 Uiso 1 1 calc GR . . . .
C44 C 0.39996(18) 0.92722(14) 0.51899(16) 0.0675(8) Uani 1 1 d . . . . .
H44A H 0.385537 0.912310 0.560337 0.101 Uiso 1 1 calc GR . . . .
H44B H 0.372215 0.970986 0.496968 0.101 Uiso 1 1 calc GR . . . .
H44C H 0.454654 0.936720 0.536517 0.101 Uiso 1 1 calc GR . . . .
C55 C 0.3030(2) 0.83129(15) 0.13409(16) 0.0751(9) Uani 1 1 d . . . . .
H55A H 0.317544 0.811053 0.094702 0.113 Uiso 1 1 calc GR . . . .
H55B H 0.332177 0.875204 0.152789 0.113 Uiso 1 1 calc GR . . . .
H55C H 0.248659 0.842682 0.114890 0.113 Uiso 1 1 calc GR . . . .
C41 C 0.34957(19) 0.54075(14) 0.50392(16) 0.0688(8) Uani 1 1 d . . . . .
H41A H 0.399194 0.524818 0.538038 0.103 Uiso 1 1 calc GR . . . .
H41B H 0.320668 0.499115 0.477589 0.103 Uiso 1 1 calc GR . . . .
H41C H 0.321701 0.564292 0.531444 0.103 Uiso 1 1 calc GR . . . .
C53 C 0.06768(17) 0.5763(2) 0.20417(17) 0.0805(10) Uani 1 1 d . . . . .
H53A H 0.045385 0.622755 0.184011 0.121 Uiso 1 1 calc GR . . . .
H53B H 0.044559 0.558960 0.238717 0.121 Uiso 1 1 calc GR . . . .
H53C H 0.058261 0.541540 0.164134 0.121 Uiso 1 1 calc GR . . . .
C23 C 0.00070(17) 0.40164(15) 0.04338(17) 0.0676(8) Uani 1 1 d . . . . .
H23A H -0.031276 0.416123 -0.006443 0.101 Uiso 1 1 calc GR . . . .
H23B H 0.019667 0.444555 0.073518 0.101 Uiso 1 1 calc GR . . . .
H23C H -0.029266 0.372643 0.064987 0.101 Uiso 1 1 calc GR . . . .
C8 C 0.32844(19) 0.04158(16) 0.18589(17) 0.0758(9) Uani 1 1 d . . . . .
H8A H 0.337326 0.000571 0.219458 0.114 Uiso 1 1 calc GR . . . .
H8B H 0.350050 0.031337 0.148170 0.114 Uiso 1 1 calc GR . . . .
H8C H 0.273734 0.049886 0.162448 0.114 Uiso 1 1 calc GR . . . .
C56 C 0.40375(17) 0.75903(18) 0.22842(18) 0.0762(9) Uani 1 1 d . . . . .
H56A H 0.413371 0.727075 0.270730 0.114 Uiso 1 1 calc GR . . . .
H56B H 0.433040 0.803412 0.244227 0.114 Uiso 1 1 calc GR . . . .
H56C H 0.419068 0.735060 0.191221 0.114 Uiso 1 1 calc GR . . . .
C26 C 0.42222(17) 0.43203(17) 0.25003(16) 0.0686(8) Uani 1 1 d . . . . .
H26A H 0.465094 0.415832 0.236009 0.082 Uiso 1 1 calc R . . . .
H26B H 0.442429 0.452555 0.300158 0.082 Uiso 1 1 calc R . . . .
C25 C 0.36918(19) 0.37277(18) 0.24545(15) 0.0790(10) Uani 1 1 d . . . . .
H25A H 0.396774 0.326475 0.257005 0.095 Uiso 1 1 calc R . . . .
H25B H 0.343159 0.380411 0.280778 0.095 Uiso 1 1 calc R . . . .
Li2 Li 0.2700(2) 0.2842(2) 0.1242(2) 0.0418(9) Uani 1 1 d . . . . .
C29 C 0.40728(16) 0.27354(19) 0.0848(2) 0.0854(11) Uani 1 1 d . . . . .
H29A H 0.429403 0.291087 0.136039 0.102 Uiso 1 1 calc R . . . .
H29B H 0.416304 0.310070 0.051982 0.102 Uiso 1 1 calc R . . . .
C52 C 0.1897(2) 0.51451(16) 0.27629(19) 0.0826(10) Uani 1 1 d . . . . .
H52A H 0.181177 0.479094 0.236969 0.124 Uiso 1 1 calc GR . . . .
H52B H 0.167696 0.496852 0.311592 0.124 Uiso 1 1 calc GR . . . .
H52C H 0.244339 0.522018 0.301337 0.124 Uiso 1 1 calc GR . . . .
C60 C 0.05214(17) 0.73061(19) 0.3421(2) 0.0808(10) Uani 1 1 d . . . . .
H60A H 0.047768 0.722362 0.290656 0.097 Uiso 1 1 calc R . . . .
H60B H 0.015556 0.768554 0.342586 0.097 Uiso 1 1 calc R . . . .
C27 C 0.37431(19) 0.48465(18) 0.19670(18) 0.0866(11) Uani 1 1 d . . . . .
H27A H 0.405201 0.514913 0.176399 0.104 Uiso 1 1 calc R . . . .
H27B H 0.346835 0.516053 0.219730 0.104 Uiso 1 1 calc R . . . .
C32 C 0.30954(17) 0.19919(18) 0.01793(17) 0.0733(9) Uani 1 1 d D U . . .
H32A H 0.295137 0.158460 0.042853 0.088 Uiso 0.565(12) 1 calc R . P A 1
H32B H 0.266160 0.210201 -0.027646 0.088 Uiso 0.565(12) 1 calc R . P A 1
H32C H 0.295384 0.213343 -0.034198 0.088 Uiso 0.435(12) 1 calc R . P A 2
H32D H 0.267396 0.171390 0.023847 0.088 Uiso 0.435(12) 1 calc R . P A 2
C9 C 0.45032(15) 0.09750(19) 0.26386(16) 0.0749(9) Uani 1 1 d . . . . .
H9A H 0.473650 0.141206 0.290455 0.112 Uiso 1 1 calc GR . . . .
H9B H 0.471519 0.087327 0.225824 0.112 Uiso 1 1 calc GR . . . .
H9C H 0.460771 0.057045 0.298225 0.112 Uiso 1 1 calc GR . . . .
Li3 Li 0.1987(2) 0.7833(2) 0.3422(2) 0.0444(10) Uani 1 1 d D . . . .
C30 C 0.44110(18) 0.20605(19) 0.0774(2) 0.0822(10) Uani 1 1 d D U . . .
H30A H 0.446226 0.172844 0.118533 0.099 Uiso 0.565(12) 1 calc R . P A 1
H30B H 0.490889 0.212330 0.071951 0.099 Uiso 0.565(12) 1 calc R . P A 1
H30C H 0.472771 0.212393 0.046929 0.099 Uiso 0.435(12) 1 calc R . P A 2
H30D H 0.473920 0.188211 0.126296 0.099 Uiso 0.435(12) 1 calc R . P A 2
C58 C 0.1105(3) 0.64097(18) 0.4277(3) 0.1100(16) Uani 1 1 d . . . . .
H58A H 0.136873 0.608399 0.404587 0.132 Uiso 1 1 calc R . . . .
H58B H 0.104560 0.616287 0.470267 0.132 Uiso 1 1 calc R . . . .
C59 C 0.0354(3) 0.6639(2) 0.3737(3) 0.1104(16) Uani 1 1 d . . . . .
H59A H 0.014317 0.626894 0.335270 0.132 Uiso 1 1 calc R . . . .
H59B H -0.001320 0.672738 0.398454 0.132 Uiso 1 1 calc R . . . .
C31 C 0.3747(3) 0.1806(4) 0.0007(5) 0.072(2) Uani 0.565(12) 1 d D U P A 1
H31A H 0.376749 0.207787 -0.042198 0.087 Uiso 0.565(12) 1 calc R . P A 1
H31B H 0.377019 0.128423 -0.008159 0.087 Uiso 0.565(12) 1 calc R . P A 1
O4 O 0.1658(7) 0.8789(4) 0.3088(5) 0.070(3) Uani 0.610(10) 1 d D U P B 1
C64 C 0.1931(6) 0.9222(4) 0.2644(6) 0.081(3) Uani 0.610(10) 1 d D U P B 1
H64A H 0.176793 0.902705 0.213836 0.097 Uiso 0.610(10) 1 calc R . P B 1
H64B H 0.249200 0.924541 0.284806 0.097 Uiso 0.610(10) 1 calc R . P B 1
C63 C 0.1612(6) 0.9910(3) 0.2645(5) 0.092(3) Uani 0.610(10) 1 d D U P B 1
H63A H 0.201019 1.028443 0.275568 0.111 Uiso 0.610(10) 1 calc R . P B 1
H63B H 0.122038 1.001445 0.215891 0.111 Uiso 0.610(10) 1 calc R . P B 1
C62 C 0.1298(8) 0.9903(5) 0.3168(8) 0.161(5) Uani 0.610(10) 1 d D U P B 1
H62A H 0.080884 1.016394 0.298737 0.193 Uiso 0.610(10) 1 calc R . P B 1
H62B H 0.163871 1.015423 0.361132 0.193 Uiso 0.610(10) 1 calc R . P B 1
C61 C 0.1175(7) 0.9193(4) 0.3355(7) 0.133(4) Uani 0.610(10) 1 d D U P B 1
H61A H 0.063798 0.904945 0.311024 0.160 Uiso 0.610(10) 1 calc R . P B 1
H61B H 0.132105 0.913681 0.389234 0.160 Uiso 0.610(10) 1 calc R . P B 1
O4A O 0.1848(10) 0.8845(6) 0.3204(7) 0.059(4) Uani 0.390(10) 1 d D U P B 2
C64A C 0.1665(11) 0.9234(9) 0.2531(8) 0.099(6) Uani 0.390(10) 1 d D U P B 2
H64C H 0.137289 0.892332 0.211363 0.119 Uiso 0.390(10) 1 calc R . P B 2
H64D H 0.213708 0.938474 0.246065 0.119 Uiso 0.390(10) 1 calc R . P B 2
C63A C 0.1212(12) 0.9872(9) 0.2557(7) 0.133(7) Uani 0.390(10) 1 d D U P B 2
H63C H 0.069792 0.983620 0.217551 0.159 Uiso 0.390(10) 1 calc R . P B 2
H63D H 0.145786 1.031249 0.246549 0.159 Uiso 0.390(10) 1 calc R . P B 2
C62A C 0.1159(8) 0.9903(8) 0.3295(5) 0.077(4) Uani 0.390(10) 1 d D U P B 2
H62C H 0.128664 1.038630 0.351684 0.092 Uiso 0.390(10) 1 calc R . P B 2
H62D H 0.064714 0.976386 0.328100 0.092 Uiso 0.390(10) 1 calc R . P B 2
C61A C 0.1734(5) 0.9368(4) 0.3689(3) 0.045(2) Uani 0.390(10) 1 d D U P B 2
H61C H 0.221995 0.961609 0.395256 0.054 Uiso 0.390(10) 1 calc R . P B 2
H61D H 0.157204 0.912346 0.405929 0.054 Uiso 0.390(10) 1 calc R . P B 2
C31A C 0.3828(4) 0.1565(4) 0.0440(5) 0.062(2) Uani 0.435(12) 1 d D U P A 2
H31C H 0.381246 0.119213 0.079647 0.075 Uiso 0.435(12) 1 calc R . P A 2
H31D H 0.390821 0.132665 0.002013 0.075 Uiso 0.435(12) 1 calc R . P A 2
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'
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
N2 N1 C1 114.61(16) . . ?
N2 N1 Li2 92.68(15) . . ?
C1 N1 Li2 152.20(18) . . ?
N2 N3 C13 113.67(16) . . ?
N2 N3 Li2 93.75(16) . . ?
C13 N3 Li2 152.12(17) . . ?
N1 N2 N3 110.10(16) . . ?
N6 N5 N4 110.69(16) . . ?
N5 N4 C33 113.70(17) . . ?
N5 N4 Li3 92.29(16) . . ?
C33 N4 Li3 153.87(17) . . ?
N5 N6 C45 112.54(16) . . ?
N5 N6 Li3 93.18(17) . . ?
C45 N6 Li3 153.92(18) . . ?
C57 O3 Li3 119.4(2) . . ?
C60 O3 C57 108.4(2) . . ?
C60 O3 Li3 122.6(2) . . ?
C28 O1 C25 108.20(19) . . ?
C28 O1 Li2 127.85(19) . . ?
C25 O1 Li2 121.5(2) . . ?
C14 C13 N3 122.44(19) . . ?
C14 C13 C18 120.37(19) . . ?
C18 C13 N3 117.06(18) . . ?
C2 C1 N1 117.40(18) . . ?
C2 C1 C6 120.68(19) . . ?
C6 C1 N1 121.61(18) . . ?
N4 C33 C34 123.7(2) . . ?
N4 C33 C38 116.28(19) . . ?
C38 C33 C34 119.9(2) . . ?
C13 C14 C19 122.05(19) . . ?
C15 C14 C13 118.5(2) . . ?
C15 C14 C19 119.5(2) . . ?
C46 C45 N6 118.98(18) . . ?
C46 C45 C50 120.59(19) . . ?
C50 C45 N6 120.33(19) . . ?
C45 C46 C51 120.63(19) . . ?
C47 C46 C45 118.7(2) . . ?
C47 C46 C51 120.7(2) . . ?
C45 C50 C54 120.80(19) . . ?
C49 C50 C45 118.5(2) . . ?
C49 C50 C54 120.7(2) . . ?
C33 C34 C39 122.4(2) . . ?
C35 C34 C33 118.2(2) . . ?
C35 C34 C39 119.3(2) . . ?
C1 C2 C7 120.12(19) . . ?
C3 C2 C1 118.9(2) . . ?
C3 C2 C7 120.8(2) . . ?
C29 O2 Li2 125.1(2) . . ?
C29 O2 C32 107.0(2) . . ?
C32 O2 Li2 121.0(2) . . ?
C2 C7 C8 109.3(2) . . ?
C9 C7 C2 114.42(19) . . ?
C9 C7 C8 110.6(2) . . ?
C16 C15 C14 121.6(2) . . ?
C1 C6 C10 121.35(19) . . ?
C5 C6 C1 117.8(2) . . ?
C5 C6 C10 120.8(2) . . ?
C15 C16 C17 119.4(2) . . ?
C13 C18 C22 119.68(19) . . ?
C17 C18 C13 118.8(2) . . ?
C17 C18 C22 121.5(2) . . ?
C33 C38 C42 119.9(2) . . ?
C37 C38 C33 119.0(2) . . ?
C37 C38 C42 121.1(2) . . ?
C14 C19 C20 111.66(19) . . ?
C14 C19 C21 112.3(2) . . ?
C20 C19 C21 111.0(2) . . ?
C48 C47 C46 121.4(2) . . ?
C34 C39 C40 110.6(2) . . ?
C34 C39 C41 112.9(2) . . ?
C40 C39 C41 110.0(2) . . ?
C16 C17 C18 121.3(2) . . ?
C18 C22 C24 110.12(18) . . ?
C18 C22 C23 113.0(2) . . ?
C24 C22 C23 110.5(2) . . ?
C4 C3 C2 121.1(2) . . ?
C53 C51 C46 112.6(2) . . ?
C53 C51 C52 111.6(2) . . ?
C52 C51 C46 110.5(2) . . ?
C50 C54 C55 113.0(2) . . ?
C50 C54 C56 110.7(2) . . ?
C55 C54 C56 111.1(2) . . ?
C36 C35 C34 122.0(2) . . ?
C3 C4 C5 120.0(2) . . ?
C48 C49 C50 121.2(2) . . ?
C47 C48 C49 119.6(2) . . ?
C38 C42 C44 113.9(2) . . ?
C43 C42 C38 110.4(2) . . ?
C43 C42 C44 110.4(2) . . ?
C6 C10 C12 110.8(2) . . ?
C6 C10 C11 114.0(2) . . ?
C12 C10 C11 109.9(2) . . ?
C4 C5 C6 121.5(2) . . ?
C36 C37 C38 121.2(2) . . ?
C35 C36 C37 119.7(2) . . ?
O1 C28 C27 106.8(2) . . ?
O3 C57 C58 103.3(3) . . ?
C25 C26 C27 102.9(2) . . ?
O1 C25 C26 106.9(2) . . ?
N3 Li2 N1 63.46(13) . . ?
O1 Li2 N1 115.4(2) . . ?
O1 Li2 N3 137.5(2) . . ?
O2 Li2 N1 122.0(2) . . ?
O2 Li2 N3 111.9(2) . . ?
O2 Li2 O1 103.62(19) . . ?
O2 C29 C30 106.8(3) . . ?
O3 C60 C59 108.3(3) . . ?
C26 C27 C28 103.5(3) . . ?
O2 C32 C31A 102.9(3) . . ?
C31 C32 O2 108.4(3) . . ?
N6 Li3 N4 63.82(13) . . ?
O3 Li3 N4 112.9(2) . . ?
O3 Li3 N6 121.6(2) . . ?
O3 Li3 O4 103.5(3) . . ?
O3 Li3 O4A 109.2(5) . . ?
O4 Li3 N4 130.8(4) . . ?
O4 Li3 N6 121.7(3) . . ?
O4A Li3 N4 120.2(6) . . ?
O4A Li3 N6 122.2(4) . . ?
C29 C30 C31 97.0(3) . . ?
C31A C30 C29 108.5(4) . . ?
C59 C58 C57 103.7(3) . . ?
C60 C59 C58 104.1(3) . . ?
C32 C31 C30 98.9(4) . . ?
C64 O4 Li3 126.4(7) . . ?
C64 O4 C61 110.3(7) . . ?
C61 O4 Li3 122.7(5) . . ?
O4 C64 C63 105.4(7) . . ?
C62 C63 C64 107.1(6) . . ?
C63 C62 C61 111.2(7) . . ?
C62 C61 O4 102.4(6) . . ?
C64A O4A Li3 131.8(10) . . ?
C64A O4A C61A 102.7(10) . . ?
C61A O4A Li3 124.1(8) . . ?
O4A C64A C63A 109.2(9) . . ?
C64A C63A C62A 107.9(9) . . ?
C61A C62A C63A 100.8(7) . . ?
O4A C61A C62A 112.0(8) . . ?
C30 C31A C32 106.3(4) . . ?
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
N1 N2 1.309(2) . ?
N1 C1 1.422(2) . ?
N1 Li2 2.055(4) . ?
N3 N2 1.312(2) . ?
N3 C13 1.422(3) . ?
N3 Li2 2.029(4) . ?
N5 N4 1.315(2) . ?
N5 N6 1.306(2) . ?
N4 C33 1.407(3) . ?
N4 Li3 2.047(4) . ?
N6 C45 1.422(2) . ?
N6 Li3 2.033(4) . ?
O3 C57 1.430(3) . ?
O3 C60 1.425(3) . ?
O3 Li3 1.910(4) . ?
O1 C28 1.415(3) . ?
O1 C25 1.439(3) . ?
O1 Li2 1.920(4) . ?
C13 C14 1.402(3) . ?
C13 C18 1.410(3) . ?
C1 C2 1.400(3) . ?
C1 C6 1.418(3) . ?
C33 C34 1.409(3) . ?
C33 C38 1.408(3) . ?
C14 C15 1.390(3) . ?
C14 C19 1.520(3) . ?
C45 C46 1.398(3) . ?
C45 C50 1.407(3) . ?
C46 C47 1.387(3) . ?
C46 C51 1.516(3) . ?
C50 C54 1.512(3) . ?
C50 C49 1.387(3) . ?
C34 C39 1.522(3) . ?
C34 C35 1.388(3) . ?
C2 C7 1.515(3) . ?
C2 C3 1.387(3) . ?
O2 Li2 1.902(4) . ?
O2 C29 1.428(3) . ?
O2 C32 1.432(3) . ?
C7 C8 1.519(3) . ?
C7 C9 1.503(3) . ?
C15 C16 1.380(3) . ?
C6 C10 1.517(3) . ?
C6 C5 1.389(3) . ?
C16 C17 1.380(3) . ?
C18 C17 1.384(3) . ?
C18 C22 1.516(3) . ?
C38 C42 1.516(3) . ?
C38 C37 1.389(3) . ?
C19 C20 1.522(3) . ?
C19 C21 1.524(3) . ?
C47 C48 1.374(3) . ?
C39 C40 1.527(3) . ?
C39 C41 1.534(3) . ?
C22 C24 1.518(3) . ?
C22 C23 1.528(3) . ?
C3 C4 1.375(3) . ?
C51 C53 1.514(4) . ?
C51 C52 1.515(4) . ?
C54 C55 1.517(4) . ?
C54 C56 1.527(4) . ?
C35 C36 1.368(4) . ?
C4 C5 1.381(3) . ?
C49 C48 1.383(3) . ?
C42 C43 1.512(4) . ?
C42 C44 1.528(3) . ?
C10 C12 1.529(3) . ?
C10 C11 1.531(3) . ?
C37 C36 1.371(4) . ?
C28 C27 1.501(4) . ?
C57 C58 1.502(5) . ?
C26 C25 1.470(4) . ?
C26 C27 1.478(4) . ?
C29 C30 1.440(4) . ?
C60 C59 1.471(5) . ?
C32 C31 1.429(6) . ?
C32 C31A 1.515(7) . ?
Li3 O4 1.919(8) . ?
Li3 O4A 1.927(12) . ?
C30 C31 1.640(7) . ?
C30 C31A 1.404(7) . ?
C58 C59 1.493(6) . ?
O4 C64 1.410(9) . ?
O4 C61 1.416(10) . ?
C64 C63 1.416(10) . ?
C63 C62 1.352(9) . ?
C62 C61 1.412(11) . ?
O4A C64A 1.429(15) . ?
O4A C61A 1.428(13) . ?
C64A C63A 1.475(14) . ?
C63A C62A 1.481(12) . ?
C62A C61A 1.469(12) . ?
