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#$Date: 2024-07-05 19:37:00 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293095 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/59/7715939.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_7715939
loop_
_publ_author_name
'Grasruck, Alexander'
'Schall, Kristina'
'Heinemann, Frank W.'
'Langer, Jens'
'Herrera, Alberto'
'Frieß, Sybille'
'Schmid, Günter'
'Dorta, Romano'
_publ_section_title
;
 Dibenzoazepine hydrazine is a building block for N-alkene hybrid
 ligands: exploratory syntheses of complexes of Cu, Fe, and Li.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8642
_journal_page_last               8656
_journal_paper_doi               10.1039/d4dt00749b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H39 Li N2 O3'
_chemical_formula_sum            'C29 H39 Li N2 O3'
_chemical_formula_weight         470.56
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-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     direct
_audit_creation_date             2023-10-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-07 deposited with the CCDC.	2024-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.616(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8126(17)
_cell_length_b                   16.863(3)
_cell_length_c                   17.707(4)
_cell_measurement_reflns_used    9219
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.31
_cell_volume                     2626.1(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'Bruker APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ImuS Duo Photon II CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS high brilliance micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.090
_diffrn_reflns_theta_min         2.305
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1133 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.9044.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuan, n-hexane'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5790
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0615
_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)+(0.0634P)²+2.4510P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4596
_reflns_number_total             5790
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00749b2.cif
_cod_data_source_block           rd1905
_cod_depositor_comments
'Adding full bibliography for 7715932--7715940.cif.'
_cod_original_cell_volume        2626.2(9)
_cod_database_code               7715939
_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.
;
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.986
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H18A,H18B} of C18, {H19A,H19B} of C19, {H21A,H21B} of C21,
   {H20A,H20B} of C20, {H29C,H29D} of C29A, {H28C,H28D} of C28A, {H27C,H27D} of
  C27A, {H26C,H26D} of C26A, {H27A,H27B} of C27, {H29A,H29B} of C29, {H28A,
  H28B} of C28, {H26A,H26B} of C26, {H22A,H22B} of C22, {H24A,H24B} of C24,
  {H25A,H25B} of C25, {H23A,H23B} of C23
 At 1.5 times of:
  All C(H,H,H) groups, {H16A,H16B} of C16
2. Uiso/Uaniso restraints and constraints
O3 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim O3A \\sim C26A \\sim C27A
\\sim C28A \\sim C29A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3. Others
 Sof(O3A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=
 Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(O3)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C26A(H26C,H26D), C27A(H27C,
 H27D), C28A(H28C,H28D), C29A(H29C,H29D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13)
4.c X=CH2 refined with riding coordinates:
 C16(H16A,H16B)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_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
Li1 Li 0.2323(4) 0.73269(19) 0.44685(18) 0.0246(7) Uani 1 1 d . . . . .
O1 O 0.08574(16) 0.65089(9) 0.41302(9) 0.0311(3) Uani 1 1 d . . . . .
O2 O 0.14558(15) 0.78101(9) 0.53598(8) 0.0274(3) Uani 1 1 d . . . . .
N1 N 0.54164(17) 0.72584(9) 0.40501(9) 0.0214(3) Uani 1 1 d . . . . .
N2 N 0.44453(17) 0.69927(10) 0.46261(9) 0.0217(3) Uani 1 1 d . . . . .
C1 C 0.6071(2) 0.80142(11) 0.41835(10) 0.0211(4) Uani 1 1 d . . . . .
C2 C 0.5957(2) 0.83325(11) 0.49101(11) 0.0249(4) Uani 1 1 d . . . . .
H2 H 0.547324 0.802731 0.527663 0.030 Uiso 1 1 calc R U . . .
C3 C 0.6520(3) 0.90740(13) 0.51135(12) 0.0348(5) Uani 1 1 d . . . . .
H3 H 0.637469 0.927587 0.560461 0.042 Uiso 1 1 calc R U . . .
C4 C 0.7288(3) 0.95210(13) 0.46125(14) 0.0428(6) Uani 1 1 d . . . . .
H4 H 0.771793 1.001957 0.475560 0.051 Uiso 1 1 calc R U . . .
C5 C 0.7413(3) 0.92209(13) 0.38957(13) 0.0371(5) Uani 1 1 d . . . . .
H5 H 0.793534 0.952865 0.354516 0.045 Uiso 1 1 calc R U . . .
C6 C 0.6816(2) 0.84911(11) 0.36554(11) 0.0255(4) Uani 1 1 d . . . . .
C7 C 0.6961(2) 0.83197(13) 0.28543(12) 0.0294(4) Uani 1 1 d . . . . .
H7 H 0.745669 0.872118 0.258513 0.035 Uiso 1 1 calc R U . . .
C8 C 0.6516(2) 0.76958(13) 0.24404(11) 0.0284(4) Uani 1 1 d . . . . .
H8 H 0.667435 0.773576 0.191606 0.034 Uiso 1 1 calc R U . . .
C9 C 0.5817(2) 0.69568(12) 0.26730(11) 0.0243(4) Uani 1 1 d . . . . .
C10 C 0.5578(2) 0.64010(13) 0.20909(12) 0.0301(5) Uani 1 1 d . . . . .
H10 H 0.584106 0.654544 0.159722 0.036 Uiso 1 1 calc R U . . .
C11 C 0.4982(2) 0.56530(14) 0.21940(12) 0.0334(5) Uani 1 1 d . . . . .
H11 H 0.480999 0.529620 0.178231 0.040 Uiso 1 1 calc R U . . .
C12 C 0.4645(2) 0.54450(13) 0.29208(12) 0.0319(5) Uani 1 1 d . . . . .
H12 H 0.426653 0.492948 0.301591 0.038 Uiso 1 1 calc R U . . .
C13 C 0.4855(2) 0.59820(12) 0.35119(11) 0.0269(4) Uani 1 1 d . . . . .
H13 H 0.462272 0.582021 0.400543 0.032 Uiso 1 1 calc R U . . .
C14 C 0.5397(2) 0.67554(11) 0.34096(10) 0.0220(4) Uani 1 1 d . . . . .
C15 C 0.5205(2) 0.65561(11) 0.51826(10) 0.0226(4) Uani 1 1 d . . . . .
C16 C 0.6692(2) 0.63727(12) 0.52651(12) 0.0287(4) Uani 1 1 d . . . . .
H16A H 0.736750 0.655462 0.490509 0.043 Uiso 1 1 calc R U . . .
H16B H 0.706698 0.606143 0.568347 0.043 Uiso 1 1 calc R U . . .
C17 C 0.4129(2) 0.62517(13) 0.57501(12) 0.0302(5) Uani 1 1 d . . . . .
H17A H 0.318247 0.655794 0.570543 0.045 Uiso 1 1 calc R U . . .
H17B H 0.460281 0.630931 0.626291 0.045 Uiso 1 1 calc R U . . .
H17C H 0.390542 0.569099 0.564933 0.045 Uiso 1 1 calc R U . . .
C18 C 0.1094(3) 0.56818(13) 0.42999(14) 0.0395(6) Uani 1 1 d . . . . .
H18A H 0.064153 0.553999 0.477966 0.047 Uiso 1 1 calc R U . . .
H18B H 0.219283 0.555617 0.434633 0.047 Uiso 1 1 calc R U . . .
C19 C 0.0314(3) 0.52374(15) 0.36433(16) 0.0470(6) Uani 1 1 d . . . . .
H19A H 0.097185 0.519817 0.321167 0.056 Uiso 1 1 calc R U . . .
H19B H 0.000406 0.469882 0.379390 0.056 Uiso 1 1 calc R U . . .
C20 C -0.1045(3) 0.57621(17) 0.34588(19) 0.0592(9) Uani 1 1 d . . . . .
H20A H -0.187369 0.564426 0.379399 0.071 Uiso 1 1 calc R U . . .
H20B H -0.143122 0.569315 0.292572 0.071 Uiso 1 1 calc R U . . .
C21 C -0.0432(2) 0.65947(14) 0.35957(13) 0.0347(5) Uani 1 1 d . . . . .
H21A H -0.011996 0.683165 0.311802 0.042 Uiso 1 1 calc R U . . .
H21B H -0.121411 0.693824 0.380507 0.042 Uiso 1 1 calc R U . . .
C22 C -0.0121(2) 0.77365(18) 0.55096(14) 0.0458(6) Uani 1 1 d . . . . .
H22A H -0.042579 0.717147 0.550517 0.055 Uiso 1 1 calc R U . . .
H22B H -0.076386 0.802148 0.511942 0.055 Uiso 1 1 calc R U . . .
C23 C -0.0303(3) 0.80922(17) 0.62753(14) 0.0427(6) Uani 1 1 d . . . . .
H23A H -0.022516 0.768233 0.667619 0.051 Uiso 1 1 calc R U . . .
H23B H -0.129017 0.836956 0.629328 0.051 Uiso 1 1 calc R U . . .
C24 C 0.1003(3) 0.86655(15) 0.63566(15) 0.0431(6) Uani 1 1 d . . . . .
H24A H 0.131227 0.876267 0.689587 0.052 Uiso 1 1 calc R U . . .
H24B H 0.073954 0.917729 0.610785 0.052 Uiso 1 1 calc R U . . .
C25 C 0.2244(2) 0.82432(13) 0.59617(12) 0.0298(5) Uani 1 1 d . . . . .
H25A H 0.296164 0.862873 0.575902 0.036 Uiso 1 1 calc R U . . .
H25B H 0.281630 0.787914 0.631362 0.036 Uiso 1 1 calc R U . . .
O3 O 0.204(4) 0.8188(18) 0.3703(19) 0.032(2) Uani 0.431(8) 1 d . U P A 1
C26 C 0.1582(15) 0.8928(9) 0.3861(8) 0.054(2) Uani 0.431(8) 1 d . U P A 1
H26A H 0.219935 0.913562 0.430384 0.065 Uiso 0.431(8) 1 calc R U P A 1
H26B H 0.050611 0.891426 0.399131 0.065 Uiso 0.431(8) 1 calc R U P A 1
C27 C 0.1726(17) 0.9425(12) 0.3248(8) 0.0334(19) Uani 0.431(8) 1 d . U P A 1
H27A H 0.234674 0.989662 0.339279 0.040 Uiso 0.431(8) 1 calc R U P A 1
H27B H 0.071902 0.960011 0.303121 0.040 Uiso 0.431(8) 1 calc R U P A 1
C28 C 0.2543(9) 0.8890(3) 0.2680(3) 0.0355(14) Uani 0.431(8) 1 d . U P A 1
H28A H 0.193614 0.885996 0.219104 0.043 Uiso 0.431(8) 1 calc R U P A 1
H28B H 0.355676 0.911021 0.258774 0.043 Uiso 0.431(8) 1 calc R U P A 1
C29 C 0.2673(10) 0.8227(6) 0.2969(6) 0.0400(17) Uani 0.431(8) 1 d . U P A 1
H29A H 0.376384 0.808277 0.302316 0.048 Uiso 0.431(8) 1 calc R U P A 1
H29B H 0.215045 0.783385 0.262870 0.048 Uiso 0.431(8) 1 calc R U P A 1
O3A O 0.197(3) 0.8130(13) 0.3705(15) 0.0330(18) Uani 0.569(8) 1 d . U P A 2
C26A C 0.1993(6) 0.8969(5) 0.3925(5) 0.0256(11) Uani 0.569(8) 1 d . U P A 2
H26C H 0.302289 0.913603 0.411815 0.031 Uiso 0.569(8) 1 calc R U P A 2
H26D H 0.126061 0.907988 0.431321 0.031 Uiso 0.569(8) 1 calc R U P A 2
C27A C 0.1487(15) 0.9404(9) 0.3119(6) 0.0393(18) Uani 0.569(8) 1 d . U P A 2
H27C H 0.042327 0.959347 0.311622 0.047 Uiso 0.569(8) 1 calc R U P A 2
H27D H 0.215685 0.986224 0.303100 0.047 Uiso 0.569(8) 1 calc R U P A 2
C28A C 0.1643(8) 0.8796(3) 0.2537(3) 0.0458(13) Uani 0.569(8) 1 d . U P A 2
H28C H 0.065458 0.870984 0.225123 0.055 Uiso 0.569(8) 1 calc R U P A 2
H28D H 0.239432 0.896662 0.217789 0.055 Uiso 0.569(8) 1 calc R U P A 2
C29A C 0.2144(9) 0.8070(4) 0.2913(4) 0.0406(14) Uani 0.569(8) 1 d . U P A 2
H29C H 0.153892 0.761791 0.270190 0.049 Uiso 0.569(8) 1 calc R U P A 2
H29D H 0.322523 0.797210 0.282343 0.049 Uiso 0.569(8) 1 calc R U 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
O1 Li1 O2 104.74(16) . . ?
O1 Li1 O3 104.8(10) . . ?
O2 Li1 O3 101.9(10) . . ?
N2 Li1 O1 116.55(18) . . ?
N2 Li1 O2 114.84(17) . . ?
N2 Li1 O3 112.5(11) . . ?
O3A Li1 O1 101.9(8) . . ?
O3A Li1 O2 102.5(8) . . ?
O3A Li1 N2 114.6(9) . . ?
C18 O1 Li1 122.35(15) . . ?
C18 O1 C21 109.42(16) . . ?
C21 O1 Li1 127.48(16) . . ?
C22 O2 Li1 122.70(16) . . ?
C25 O2 Li1 127.65(15) . . ?
C25 O2 C22 109.60(16) . . ?
C1 N1 N2 114.58(14) . . ?
C1 N1 C14 131.20(16) . . ?
C14 N1 N2 113.73(15) . . ?
N1 N2 Li1 114.44(14) . . ?
C15 N2 Li1 132.58(16) . . ?
C15 N2 N1 112.97(15) . . ?
N1 C1 C6 126.86(17) . . ?
C2 C1 N1 116.49(16) . . ?
C2 C1 C6 116.65(18) . . ?
C1 C2 H2 118.7 . . ?
C3 C2 C1 122.58(18) . . ?
C3 C2 H2 118.7 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 121.2 . . ?
C3 C4 C5 117.7(2) . . ?
C5 C4 H4 121.2 . . ?
C4 C5 H5 118.1 . . ?
C4 C5 C6 123.7(2) . . ?
C6 C5 H5 118.1 . . ?
C1 C6 C7 126.70(19) . . ?
C5 C6 C1 118.58(18) . . ?
C5 C6 C7 114.63(18) . . ?
C6 C7 H7 114.7 . . ?
C8 C7 C6 130.69(19) . . ?
C8 C7 H7 114.7 . . ?
C7 C8 H8 115.3 . . ?
C7 C8 C9 129.48(18) . . ?
C9 C8 H8 115.3 . . ?
C10 C9 C8 114.21(18) . . ?
C10 C9 C14 118.75(19) . . ?
C14 C9 C8 127.03(18) . . ?
C9 C10 H10 118.2 . . ?
C11 C10 C9 123.7(2) . . ?
C11 C10 H10 118.2 . . ?
C10 C11 H11 121.3 . . ?
C10 C11 C12 117.36(19) . . ?
C12 C11 H11 121.3 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.7(2) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 118.7 . . ?
C12 C13 C14 122.60(19) . . ?
C14 C13 H13 118.7 . . ?
N1 C14 C9 127.04(18) . . ?
C13 C14 N1 116.10(17) . . ?
C13 C14 C9 116.83(18) . . ?
N2 C15 C17 111.18(16) . . ?
C16 C15 N2 129.04(18) . . ?
C16 C15 C17 119.77(18) . . ?
C15 C16 H16A 120.0 . . ?
C15 C16 H16B 120.0 . . ?
H16A C16 H16B 120.0 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O1 C18 H18A 110.6 . . ?
O1 C18 H18B 110.6 . . ?
O1 C18 C19 105.50(19) . . ?
H18A C18 H18B 108.8 . . ?
C19 C18 H18A 110.6 . . ?
C19 C18 H18B 110.6 . . ?
C18 C19 H19A 111.6 . . ?
C18 C19 H19B 111.6 . . ?
H19A C19 H19B 109.4 . . ?
C20 C19 C18 101.1(2) . . ?
C20 C19 H19A 111.6 . . ?
C20 C19 H19B 111.6 . . ?
C19 C20 H20A 111.0 . . ?
C19 C20 H20B 111.0 . . ?
C19 C20 C21 103.79(19) . . ?
H20A C20 H20B 109.0 . . ?
C21 C20 H20A 111.0 . . ?
C21 C20 H20B 111.0 . . ?
O1 C21 C20 105.66(19) . . ?
O1 C21 H21A 110.6 . . ?
O1 C21 H21B 110.6 . . ?
C20 C21 H21A 110.6 . . ?
C20 C21 H21B 110.6 . . ?
H21A C21 H21B 108.7 . . ?
O2 C22 H22A 110.3 . . ?
O2 C22 H22B 110.3 . . ?
O2 C22 C23 107.00(18) . . ?
H22A C22 H22B 108.6 . . ?
C23 C22 H22A 110.3 . . ?
C23 C22 H22B 110.3 . . ?
C22 C23 H23A 111.2 . . ?
C22 C23 H23B 111.2 . . ?
C22 C23 C24 102.62(19) . . ?
H23A C23 H23B 109.2 . . ?
C24 C23 H23A 111.2 . . ?
C24 C23 H23B 111.2 . . ?
C23 C24 H24A 111.2 . . ?
C23 C24 H24B 111.2 . . ?
C23 C24 C25 102.98(19) . . ?
H24A C24 H24B 109.1 . . ?
C25 C24 H24A 111.2 . . ?
C25 C24 H24B 111.2 . . ?
O2 C25 C24 104.65(17) . . ?
O2 C25 H25A 110.8 . . ?
O2 C25 H25B 110.8 . . ?
C24 C25 H25A 110.8 . . ?
C24 C25 H25B 110.8 . . ?
H25A C25 H25B 108.9 . . ?
C26 O3 Li1 124(2) . . ?
C26 O3 C29 106(2) . . ?
C29 O3 Li1 127(2) . . ?
O3 C26 H26A 109.5 . . ?
O3 C26 H26B 109.5 . . ?
O3 C26 C27 111(2) . . ?
H26A C26 H26B 108.1 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C26 C27 H27A 111.2 . . ?
C26 C27 H27B 111.2 . . ?
C26 C27 C28 103.0(14) . . ?
H27A C27 H27B 109.1 . . ?
C28 C27 H27A 111.2 . . ?
C28 C27 H27B 111.2 . . ?
C27 C28 H28A 110.3 . . ?
C27 C28 H28B 110.3 . . ?
H28A C28 H28B 108.6 . . ?
C29 C28 C27 106.9(9) . . ?
C29 C28 H28A 110.3 . . ?
C29 C28 H28B 110.3 . . ?
O3 C29 H29A 109.1 . . ?
O3 C29 H29B 109.1 . . ?
C28 C29 O3 112.6(13) . . ?
C28 C29 H29A 109.1 . . ?
C28 C29 H29B 109.1 . . ?
H29A C29 H29B 107.8 . . ?
C26A O3A Li1 119.5(16) . . ?
C29A O3A Li1 128.1(15) . . ?
C29A O3A C26A 109.2(17) . . ?
O3A C26A H26C 111.4 . . ?
O3A C26A H26D 111.4 . . ?
O3A C26A C27A 101.6(13) . . ?
H26C C26A H26D 109.3 . . ?
C27A C26A H26C 111.4 . . ?
C27A C26A H26D 111.4 . . ?
C26A C27A H27C 110.7 . . ?
C26A C27A H27D 110.7 . . ?
H27C C27A H27D 108.8 . . ?
C28A C27A C26A 105.4(9) . . ?
C28A C27A H27C 110.7 . . ?
C28A C27A H27D 110.7 . . ?
C27A C28A H28C 110.1 . . ?
C27A C28A H28D 110.1 . . ?
H28C C28A H28D 108.4 . . ?
C29A C28A C27A 108.0(6) . . ?
C29A C28A H28C 110.1 . . ?
C29A C28A H28D 110.1 . . ?
O3A C29A C28A 110.0(10) . . ?
O3A C29A H29C 109.7 . . ?
O3A C29A H29D 109.7 . . ?
C28A C29A H29C 109.7 . . ?
C28A C29A H29D 109.7 . . ?
H29C C29A H29D 108.2 . . ?
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
Li1 O1 1.958(4) . ?
Li1 O2 1.973(4) . ?
Li1 N2 1.956(4) . ?
Li1 O3 1.99(3) . ?
Li1 O3A 1.93(3) . ?
O1 C18 1.439(3) . ?
O1 C21 1.440(2) . ?
O2 C22 1.436(3) . ?
O2 C25 1.435(2) . ?
N1 N2 1.443(2) . ?
N1 C1 1.413(2) . ?
N1 C14 1.416(2) . ?
N2 C15 1.370(2) . ?
C1 C2 1.404(3) . ?
C1 C6 1.425(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.374(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.377(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(3) . ?
C6 C7 1.461(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.327(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.461(3) . ?
C9 C10 1.399(3) . ?
C9 C14 1.419(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.384(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.405(3) . ?
C15 C16 1.346(3) . ?
C15 C17 1.514(3) . ?
C16 H16A 0.9500 . ?
C16 H16B 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.511(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.508(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.518(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.501(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.503(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.512(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
O3 C26 1.35(4) . ?
O3 C29 1.45(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.38(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.561(17) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.233(11) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
O3A C26A 1.47(2) . ?
O3A C29A 1.43(3) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C26A C27A 1.643(15) . ?
C27A H27C 0.9900 . ?
C27A H27D 0.9900 . ?
C27A C28A 1.466(14) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C28A C29A 1.449(8) . ?
C29A H29C 0.9900 . ?
C29A H29D 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
Li1 O1 C18 C19 -149.4(2) . . . . ?
Li1 O1 C21 C20 172.4(2) . . . . ?
Li1 O2 C22 C23 173.23(19) . . . . ?
Li1 O2 C25 C24 164.37(19) . . . . ?
Li1 N2 C15 C16 -177.4(2) . . . . ?
Li1 N2 C15 C17 3.6(3) . . . . ?
Li1 O3 C26 C27 170.4(19) . . . . ?
Li1 O3 C29 C28 -167.3(18) . . . . ?
Li1 O3A C26A C27A -175.1(15) . . . . ?
Li1 O3A C29A C28A 175.7(16) . . . . ?
O1 C18 C19 C20 -35.8(3) . . . . ?
O2 C22 C23 C24 25.0(3) . . . . ?
N1 N2 C15 C16 2.1(3) . . . . ?
N1 N2 C15 C17 -176.84(15) . . . . ?
N1 C1 C2 C3 -178.67(19) . . . . ?
N1 C1 C6 C5 -179.11(19) . . . . ?
N1 C1 C6 C7 4.6(3) . . . . ?
N2 N1 C1 C2 12.5(2) . . . . ?
N2 N1 C1 C6 -166.61(17) . . . . ?
N2 N1 C14 C9 158.89(17) . . . . ?
N2 N1 C14 C13 -18.8(2) . . . . ?
C1 N1 N2 Li1 87.81(19) . . . . ?
C1 N1 N2 C15 -91.81(19) . . . . ?
C1 N1 C14 C9 -12.5(3) . . . . ?
C1 N1 C14 C13 169.77(18) . . . . ?
C1 C2 C3 C4 -3.0(3) . . . . ?
C1 C6 C7 C8 -2.9(4) . . . . ?
C2 C1 C6 C5 1.8(3) . . . . ?
C2 C1 C6 C7 -174.47(18) . . . . ?
C2 C3 C4 C5 2.9(4) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C4 C5 C6 C1 -1.9(4) . . . . ?
C4 C5 C6 C7 174.8(2) . . . . ?
C5 C6 C7 C8 -179.3(2) . . . . ?
C6 C1 C2 C3 0.5(3) . . . . ?
C6 C7 C8 C9 -4.3(4) . . . . ?
C7 C8 C9 C10 -176.1(2) . . . . ?
C7 C8 C9 C14 2.8(3) . . . . ?
C8 C9 C10 C11 177.62(19) . . . . ?
C8 C9 C14 N1 7.4(3) . . . . ?
C8 C9 C14 C13 -174.89(18) . . . . ?
C9 C10 C11 C12 -1.7(3) . . . . ?
C10 C9 C14 N1 -173.69(17) . . . . ?
C10 C9 C14 C13 4.0(3) . . . . ?
C10 C11 C12 C13 2.2(3) . . . . ?
C11 C12 C13 C14 0.6(3) . . . . ?
C12 C13 C14 N1 174.25(18) . . . . ?
C12 C13 C14 C9 -3.7(3) . . . . ?
C14 N1 N2 Li1 -85.09(19) . . . . ?
C14 N1 N2 C15 95.29(18) . . . . ?
C14 N1 C1 C2 -176.16(17) . . . . ?
C14 N1 C1 C6 4.7(3) . . . . ?
C14 C9 C10 C11 -1.4(3) . . . . ?
C18 O1 C21 C20 2.2(3) . . . . ?
C18 C19 C20 C21 36.4(3) . . . . ?
C19 C20 C21 O1 -24.8(3) . . . . ?
C21 O1 C18 C19 21.4(3) . . . . ?
C22 O2 C25 C24 -18.3(2) . . . . ?
C22 C23 C24 C25 -35.2(3) . . . . ?
C23 C24 C25 O2 33.4(2) . . . . ?
C25 O2 C22 C23 -4.3(3) . . . . ?
O3 C26 C27 C28 -6(2) . . . . ?
C26 O3 C29 C28 -4(3) . . . . ?
C26 C27 C28 C29 3.6(13) . . . . ?
C27 C28 C29 O3 0.0(18) . . . . ?
C29 O3 C26 C27 6(3) . . . . ?
O3A C26A C27A C28A -14.6(16) . . . . ?
C26A O3A C29A C28A -25(2) . . . . ?
C26A C27A C28A C29A 1.0(10) . . . . ?
C27A C28A C29A O3A 13.9(14) . . . . ?
C29A O3A C26A C27A 23(2) . . . . ?
