#------------------------------------------------------------------------------
#$Date: 2026-06-04 10:24:35 +0100 (Thu, 04 Jun 2026) $
#$Revision: 306203 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577369.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_1577369
loop_
_publ_author_name
'Nahon, Emily'
'Nelmes, Gareth R.'
'Dallerba, Elena'
'Lim, Li Feng'
'Cox, Nicholas'
'McMullin, Claire L.'
'Massi, Massimiliano'
'Kallmeier, Fabian'
'Hicks, Jamie'
_publ_section_title
;
Xanthene-to-fluorene skeletal editing via oxygen deletion mediated
by boron and aluminium radicals.
;
_journal_issue 21
_journal_name_full 'Chemical science'
_journal_page_first 10755
_journal_page_last 10761
_journal_paper_doi 10.1039/d6sc01056c
_journal_volume 17
_journal_year 2026
_chemical_formula_moiety 'C55 H78 B Li N2 O3, 2(C6 H6)'
_chemical_formula_sum 'C67 H90 B Li N2 O3'
_chemical_formula_weight 989.15
_space_group_crystal_system orthorhombic
_space_group_IT_number 18
_space_group_name_Hall 'P 2 2ab'
_space_group_name_H-M_alt 'P 21 21 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_date 2023-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-12-11 deposited with the CCDC. 2026-04-17 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 10.5718(2)
_cell_length_b 18.7926(3)
_cell_length_c 15.2111(2)
_cell_measurement_reflns_used 10226
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 77.5080
_cell_measurement_theta_min 3.7270
_cell_volume 3022.01(8)
_computing_cell_refinement 'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection 'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction 'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (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 150.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -83.00 -48.00 0.50 0.50 -- -46.57-162.00 47.00 70
2 \w -119.00 -87.00 0.50 0.50 -- -46.57-162.00 47.00 64
3 \w 75.00 101.00 0.50 0.50 -- 46.57-162.00 47.00 52
4 \w 87.00 134.00 0.50 1.94 -- 107.75-162.00 47.00 94
5 \w 116.00 149.00 0.50 1.94 -- 107.75 117.00 -75.00 66
6 \w 89.00 114.00 0.50 1.94 -- 107.75 162.00 74.00 50
7 \w -8.00 28.00 0.50 0.50 -- -46.57 19.00 -60.00 72
8 \w -4.00 30.00 0.50 0.50 -- -46.57 19.00-120.00 68
9 \w -7.00 24.00 0.50 0.50 -- -46.57 19.00-150.00 62
10 \w -1.00 29.00 0.50 0.50 -- -46.57 19.00 90.00 60
11 \w -75.00 -50.00 0.50 0.50 -- -46.57 117.00 -75.00 50
12 \w 32.00 58.00 0.50 1.94 -- 107.75 -30.00 60.00 52
13 \w 76.00 105.00 0.50 1.94 -- 107.75 -95.00 -90.00 58
14 \w 33.00 59.00 0.50 1.94 -- 107.75 -30.00 -60.00 52
15 \w 40.00 71.00 0.50 1.94 -- 107.75 -95.00 -90.00 62
16 \w 38.00 69.00 0.50 1.94 -- 107.75 -45.00 90.00 62
17 \w 32.00 58.00 0.50 1.94 -- 107.75 -30.00 0.00 52
18 \w 34.00 59.00 0.50 1.94 -- 107.75 -30.00 30.00 50
19 \w 34.00 59.00 0.50 1.94 -- 107.75 -30.00 90.00 50
20 \w 47.00 73.00 0.50 1.94 -- 107.75 -45.00 150.00 52
21 \w 36.00 63.00 0.50 1.94 -- 107.75 -45.00 30.00 54
22 \w 37.00 93.00 0.50 1.94 -- 107.75 -61.00-120.00 112
23 \w 37.00 62.00 0.50 1.94 -- 107.75 -45.00-120.00 50
24 \w 48.00 73.00 0.50 1.94 -- 107.75 -45.00 -60.00 50
25 \w 36.00 61.00 0.50 1.94 -- 107.75 -45.00 60.00 50
26 \w 32.00 57.00 0.50 1.94 -- 107.75 -30.00-180.00 50
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0078845000
_diffrn_orient_matrix_UB_12 0.0391870000
_diffrn_orient_matrix_UB_13 0.0888167000
_diffrn_orient_matrix_UB_21 0.0284374000
_diffrn_orient_matrix_UB_22 0.0710048000
_diffrn_orient_matrix_UB_23 -0.0466749000
_diffrn_orient_matrix_UB_31 -0.1426330000
_diffrn_orient_matrix_UB_32 0.0119274000
_diffrn_orient_matrix_UB_33 -0.0141915000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0335
_diffrn_reflns_av_unetI/netI 0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 16504
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.881
_diffrn_reflns_theta_min 3.739
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 0.489
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.83591
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.087
_exptl_crystal_description block
_exptl_crystal_F_000 1076
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.249
_refine_diff_density_min -0.190
_refine_diff_density_rms 0.036
_refine_ls_abs_structure_details
;
Flack x determined using 2097 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.03(15)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 431
_refine_ls_number_reflns 6122
_refine_ls_number_restraints 214
_refine_ls_restrained_S_all 1.144
_refine_ls_R_factor_all 0.0516
_refine_ls_R_factor_gt 0.0474
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.2610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1292
_refine_ls_wR_factor_ref 0.1331
_reflns_Friedel_coverage 0.706
_reflns_Friedel_fraction_full 0.964
_reflns_Friedel_fraction_max 0.892
_reflns_number_gt 5541
_reflns_number_total 6122
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d6sc01056c2.cif
_cod_data_source_block 3-Li
_cod_database_code 1577369
_shelx_shelxl_version_number 2018/3
_chemical_oxdiff_formula 'C60 H60 B1 N2 O1 Li1'
_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 0.953
_shelx_estimated_absorpt_t_min 0.867
_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
C24A-C22 = C24-C22 = C23A-C22 = C23-C22
1.53 with sigma of 0.008
C31-C30 = C30-C29 = C31_$2-C29
1.4 with sigma of 0.005
C20A-C19 = C20-C19 = C21A-C19 = C21-C19
1.53 with sigma of 0.008
O2-C28 = O2-C25
1.45 with sigma of 0.02
C28-C27 = C27-C26 = C26-C25
1.5 with sigma of 0.02
O2A-C28A = O2A-C25A
1.45 with sigma of 0.008
C25A-C26A = C26A-C27A = C27A-C28A
1.5 with sigma of 0.008
C23A-C22A = C23-C22 = C24-C22 = C24A-C22A = C22A-C14 = C22-C14
1.53 with sigma of 0.008
C24A-C23A = C24-C23
2.5 with sigma of 0.008
C20A-C20 = C21A-C21
2.5 with sigma of 0.008
C27A-C25A
2.45 with sigma of 0.008
C28A-C26A
2.45 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31: within 2A with sigma of 0.003 and sigma for terminal
atoms of 0.006 within 2A
C23 \\sim C23A \\sim C22 \\sim C22A \\sim C24A \\sim C24: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 2A
C20 \\sim C20A \\sim C21A \\sim C21 \\sim C19: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C28A \\sim C27A \\sim C26A \\sim C25A \\sim O2A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
O2 \\sim C28 \\sim C27 \\sim C26 \\sim C25: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C35 \\sim C34 \\sim C33 \\sim C32 \\sim C37 \\sim C36: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
Sof(H23F)=Sof(C22A)=Sof(H22A)=1-FVAR(1)
Sof(C22)=Sof(H22)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C23)=Sof(H23A)=
Sof(H23B)=Sof(H23C)=FVAR(1)
Sof(H19A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C20A)=Sof(H20D)=
Sof(H20E)=Sof(H20F)=1-FVAR(2)
Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=
Sof(H21C)=FVAR(2)
Sof(O2A)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=
Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=1-FVAR(3)
Sof(O2)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C28)=
Sof(H28A)=Sof(H28B)=Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(3)
Fixed Sof: C36(0.5) H36(0.5) C37(0.5) H37(0.5) C32(0.5) H32(0.5) C33(0.5)
H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5)
5.a Ternary CH refined with riding coordinates:
C22(H22), C19(H19), C19(H19A), C22A(H22A)
5.b Secondary CH2 refined with riding coordinates:
C27(H27A,H27B), C26(H26A,H26B), C28(H28A,H28B), C25(H25A,H25B), C28A(H28C,
H28D), C27A(H27C,H27D), C26A(H26C,H26D), C25A(H25C,H25D)
5.c Aromatic/amide H refined with riding coordinates:
C3(H3), C5(H5), C30(H30), C17(H17), C29(H29), C16(H16), C15(H15), C31(H31),
C36(H36), C37(H37), C32(H32), C33(H33), C34(H34), C35(H35)
5.d Fitted hexagon refined as free rotating group:
C36(C37,C32,C33,C34,C35)
5.e Idealised Me refined as rotating group:
C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C9(H9A,H9B,
H9C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C21(H21A,
H21B,H21C), C24A(H24D,H24E,H24F), C23A(H23D,H23E,H23F), C21A(H21D,H21E,H21F),
C20A(H20D,H20E,H20F)
;
_shelx_res_file
;
TITL en-p61-b(non)li_auto_a.res in P2(1)2(1)2
en-p61-b(non)li_auto.res
created by SHELXL-2018/3 at 11:44:29 on 28-Jun-2023
REM Old TITL en-p61-b(non)li_auto_a.res in P2(1)2(1)2
REM SHELXT solution in P2(1)2(1)2: R1 0.152, Rweak 0.033, Alpha 0.033
REM 0.462 for 17 systematic absences, Orientation as input
REM Flack x = 0.328 ( 0.127 ) from 2152 Parsons quotients
REM Formula found by SHELXT: C61 Li N9 O3
CELL 1.54184 10.5718 18.7926 15.2111 90 90 90
ZERR 2 0.0002 0.0003 0.0002 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H B Li N O
UNIT 134 180 2 2 4 6
EQIV $1 1-X,1-Y,+Z
EQIV $2 -X,1-Y,+Z
DFIX 1.53 0.008 C24A C22 C24 C22 C23A C22 C23 C22
DFIX 1.4 0.005 C31 C30 C30 C29 C31_$2 C29
DANG 2.5 0.008 C24A C23A C24 C23
SIMU 0.003 0.006 2 C29 C30 C31
SIMU 0.005 0.01 2 C23 C23A C22 C22A C24A C24
DANG 2.5 0.008 C20A C20 C21A C21
DFIX 1.53 0.008 C20A C19 C20 C19 C21A C19 C21 C19
SIMU 0.005 0.01 2 C20 C20A C21A C21 C19
DFIX 1.45 O2 C28 O2 C25
DFIX 1.5 C28 C27 C27 C26 C26 C25
DFIX 1.45 0.008 O2A C28A O2A C25A
DFIX 1.5 0.008 C25A C26A C26A C27A C27A C28A
DANG 2.45 0.008 C27A C25A
DANG 2.45 0.008 C28A C26A
SIMU 0.005 0.01 2 C28A C27A C26A C25A O2A
SIMU 0.005 0.01 2 O2 C28 C27 C26 C25
SIMU 0.005 0.01 2 C35 C34 C33 C32 C37 C36
DFIX 1.53 0.008 C23A C22A C23 C22 C24 C22 C24A C22A C22A C14 C22 C14
L.S. 10
PLAN 45
SIZE 0.3 0.15 0.1
TEMP -123
CONF
FREE C25A Li1_$1
FREE C25A Li1
LIST 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.080100 0.261000
FVAR 0.62900 0.74110 0.38631 0.76690
O1 6 0.500000 0.500000 0.411190 10.50000 0.03845 0.05194 =
0.02709 0.00000 0.00000 -0.00718
N1 5 0.470047 0.432043 0.279802 11.00000 0.02821 0.03912 =
0.02633 0.00299 -0.00049 -0.00308
C1 1 0.475313 0.463553 0.122377 11.00000 0.02312 0.03070 =
0.02902 -0.00137 -0.00029 0.00301
C2 1 0.447891 0.415854 0.190752 11.00000 0.02209 0.03467 =
0.02754 0.00072 -0.00105 0.00275
C6 1 0.458838 0.442061 0.034866 11.00000 0.03248 0.03100 =
0.02856 -0.00068 -0.00220 0.00467
C3 1 0.399010 0.349155 0.165966 11.00000 0.02710 0.03350 =
0.03405 0.00313 -0.00066 0.00067
AFIX 43
H3 2 0.378290 0.316265 0.211156 11.00000 -1.20000
AFIX 0
C4 1 0.379061 0.328345 0.078478 11.00000 0.02973 0.03094 =
0.03700 -0.00131 -0.00336 0.00327
C8 1 0.322140 0.254612 0.059903 11.00000 0.03665 0.03234 =
0.04483 -0.00208 -0.00362 0.00215
C7 1 0.500000 0.500000 -0.028130 10.50000 0.04018 0.03279 =
0.02755 0.00000 0.00000 0.00393
C5 1 0.411202 0.375712 0.012157 11.00000 0.03686 0.03298 =
0.03216 -0.00285 -0.00302 0.00504
AFIX 43
H5 2 0.400778 0.362943 -0.047836 11.00000 -1.20000
AFIX 0
PART 1
O2 6 0.435909 0.568817 0.604725 41.00000 0.09174 0.08397 =
0.03498 -0.01724 0.00004 0.02997
PART 0
C13 1 0.458345 0.371827 0.339159 11.00000 0.03835 0.04428 =
0.02691 0.00429 -0.00031 -0.00763
C18 1 0.558923 0.324159 0.346134 11.00000 0.05004 0.05034 =
0.03315 0.00964 -0.00594 -0.00103
C10 1 0.190994 0.250202 0.102016 11.00000 0.04137 0.04108 =
0.05832 -0.00635 0.00003 -0.00775
AFIX 137
H10A 2 0.199092 0.253772 0.166045 11.00000 -1.50000
H10B 2 0.151557 0.204667 0.086692 11.00000 -1.50000
H10C 2 0.138306 0.289340 0.080295 11.00000 -1.50000
AFIX 0
C14 1 0.345491 0.360945 0.385626 11.00000 0.04528 0.05772 =
0.03558 -0.00131 0.00493 -0.01813
C11 1 0.408013 0.196413 0.098113 11.00000 0.05271 0.03425 =
0.06114 0.00068 -0.00712 0.00625
AFIX 137
H11A 2 0.492342 0.200038 0.071737 11.00000 -1.50000
H11B 2 0.371953 0.149550 0.085050 11.00000 -1.50000
H11C 2 0.414545 0.202510 0.161937 11.00000 -1.50000
AFIX 0
C12 1 0.389658 0.525201 -0.085739 11.00000 0.05806 0.04048 =
0.03678 0.00146 -0.01101 0.00397
AFIX 137
H12A 2 0.363856 0.486629 -0.125214 11.00000 -1.50000
H12B 2 0.416420 0.566400 -0.120583 11.00000 -1.50000
H12C 2 0.318202 0.538675 -0.048224 11.00000 -1.50000
AFIX 0
PART 1
C22 1 0.233638 0.409801 0.377129 21.00000 0.03446 0.07238 =
0.05382 -0.01021 0.01380 -0.01458
AFIX 13
H22 2 0.254763 0.450738 0.337779 21.00000 -1.20000
AFIX 0
PART 0
C30 1 0.119458 0.531066 0.113342 11.00000 0.04318 0.04994 =
0.07220 0.00207 0.00685 0.00645
AFIX 43
H30 2 0.200796 0.552555 0.113413 11.00000 -1.20000
AFIX 0
C19 1 0.681807 0.337175 0.297479 11.00000 0.04463 0.07792 =
0.04424 0.01765 -0.00178 0.01929
PART 1
AFIX 13
H19 2 0.666260 0.368086 0.245070 31.00000 -1.20000
AFIX 13
PART 2
H19A 2 0.658238 0.359679 0.240203 -31.00000 -1.20000
AFIX 0
PART 0
C9 1 0.306333 0.241149 -0.038852 11.00000 0.05366 0.03789 =
0.05023 -0.01050 -0.00572 -0.00350
AFIX 137
H9A 2 0.251874 0.278016 -0.064222 11.00000 -1.50000
H9B 2 0.267655 0.194342 -0.048030 11.00000 -1.50000
H9C 2 0.389361 0.242477 -0.067457 11.00000 -1.50000
AFIX 0
C17 1 0.545404 0.265086 0.401435 11.00000 0.08340 0.05767 =
0.04826 0.01972 -0.01322 -0.00129
AFIX 43
H17 2 0.613033 0.232050 0.406485 11.00000 -1.20000
AFIX 0
B1 3 0.500000 0.500000 0.324860 10.50000 0.02153 0.04603 =
0.02654 0.00000 0.00000 0.00021
C29 1 0.106798 0.458895 0.112888 11.00000 0.04549 0.05197 =
0.10135 -0.01156 -0.01359 0.01791
AFIX 43
H29 2 0.180059 0.429630 0.112011 11.00000 -1.20000
AFIX 0
C16 1 0.437094 0.254012 0.448204 11.00000 0.09658 0.06727 =
0.05338 0.02785 -0.00871 -0.02092
AFIX 43
H16 2 0.429951 0.213851 0.485807 11.00000 -1.20000
AFIX 0
C15 1 0.338699 0.301010 0.440742 11.00000 0.07498 0.07821 =
0.04428 0.00933 0.01078 -0.03576
AFIX 43
H15 2 0.263765 0.292893 0.473723 11.00000 -1.20000
AFIX 0
C31 1 0.011723 0.572027 0.113694 11.00000 0.05637 0.04245 =
0.12912 0.01321 0.01781 0.00625
AFIX 43
H31 2 0.018903 0.622413 0.114502 11.00000 -1.20000
AFIX 0
PART 1
C24 1 0.122896 0.366722 0.338493 21.00000 0.03619 0.08523 =
0.07111 -0.00289 0.00493 -0.01386
AFIX 137
H24A 2 0.150834 0.342420 0.284898 21.00000 -1.50000
H24B 2 0.052859 0.398921 0.324388 21.00000 -1.50000
H24C 2 0.094520 0.331410 0.381603 21.00000 -1.50000
AFIX 0
C23 1 0.196147 0.436771 0.468291 21.00000 0.06026 0.08123 =
0.05334 -0.00690 0.01725 0.00345
AFIX 137
H23A 2 0.168123 0.396635 0.504523 21.00000 -1.50000
H23B 2 0.127124 0.471283 0.462670 21.00000 -1.50000
H23C 2 0.269157 0.459685 0.496123 21.00000 -1.50000
AFIX 0
C20 1 0.768866 0.375342 0.362557 31.00000 0.03508 0.10021 =
0.07385 0.02398 -0.00865 0.00735
AFIX 137
H20A 2 0.728551 0.419507 0.382268 31.00000 -1.50000
H20B 2 0.849372 0.386499 0.333744 31.00000 -1.50000
H20C 2 0.784431 0.344465 0.413336 31.00000 -1.50000
AFIX 0
C21 1 0.724697 0.262424 0.267632 31.00000 0.05799 0.10016 =
0.06689 0.00570 -0.00006 0.02888
AFIX 137
H21A 2 0.734667 0.231641 0.319173 31.00000 -1.50000
H21B 2 0.805669 0.266133 0.236603 31.00000 -1.50000
H21C 2 0.660971 0.242063 0.228181 31.00000 -1.50000
AFIX 0
C27 1 0.315723 0.646756 0.689419 41.00000 0.08127 0.07327 =
0.05910 -0.01832 -0.00829 0.02721
AFIX 23
H27A 2 0.265330 0.691083 0.686235 41.00000 -1.20000
H27B 2 0.278579 0.614646 0.734093 41.00000 -1.20000
AFIX 0
C26 1 0.453312 0.661879 0.707887 41.00000 0.07610 0.07185 =
0.06547 -0.01486 0.00568 0.00728
AFIX 23
H26A 2 0.479376 0.707678 0.681313 41.00000 -1.20000
H26B 2 0.469466 0.663691 0.771956 41.00000 -1.20000
AFIX 0
C28 1 0.325919 0.610953 0.600773 41.00000 0.10117 0.08521 =
0.06014 -0.01918 -0.02716 0.03500
AFIX 23
H28A 2 0.250632 0.581005 0.589406 41.00000 -1.20000
H28B 2 0.333015 0.646849 0.553392 41.00000 -1.20000
AFIX 0
C25 1 0.521314 0.602147 0.667234 41.00000 0.07617 0.08995 =
0.06884 -0.02184 0.00238 0.01218
AFIX 23
H25A 2 0.598069 0.619555 0.636777 41.00000 -1.20000
H25B 2 0.547316 0.567413 0.712707 41.00000 -1.20000
AFIX 0
PART 0
LI1 4 0.500000 0.500000 0.522759 10.50000 0.08580 0.09707 =
0.03305 0.00000 0.00000 0.03497
PART 2
C24A 1 0.123590 0.387339 0.310504 -21.00000 0.03489 0.08068 =
0.05809 0.00029 0.01254 -0.01041
AFIX 137
H24D 2 0.160346 0.370197 0.255280 -21.00000 -1.50000
H24E 2 0.069493 0.428581 0.298626 -21.00000 -1.50000
H24F 2 0.072974 0.349398 0.337262 -21.00000 -1.50000
AFIX 0
C23A 1 0.172402 0.452830 0.448843 -21.00000 0.05820 0.08090 =
0.05750 -0.00775 0.01671 0.00325
AFIX 137
H23D 2 0.146491 0.420899 0.496490 -21.00000 -1.50000
H23E 2 0.098461 0.478829 0.426975 -21.00000 -1.50000
H23F 2 0.235245 0.486721 0.470979 -21.00000 -1.50000
AFIX 0
C21A 1 0.767284 0.274256 0.275039 -31.00000 0.04958 0.09568 =
0.05427 -0.00269 -0.00249 0.02574
AFIX 137
H21D 2 0.801402 0.253789 0.329345 -31.00000 -1.50000
H21E 2 0.837106 0.290543 0.237742 -31.00000 -1.50000
H21F 2 0.718209 0.238051 0.243627 -31.00000 -1.50000
AFIX 0
C20A 1 0.764780 0.391607 0.346140 -31.00000 0.03406 0.08162 =
0.06060 0.02355 0.00010 0.00993
AFIX 137
H20D 2 0.711914 0.430914 0.367176 -31.00000 -1.50000
H20E 2 0.829350 0.410114 0.305965 -31.00000 -1.50000
H20F 2 0.805964 0.368488 0.396297 -31.00000 -1.50000
AFIX 0
O2A 6 0.404502 0.557208 0.601098 -41.00000 0.12900
C28A 1 0.279363 0.564799 0.640126 -41.00000 0.13411
AFIX 23
H28C 2 0.254337 0.521357 0.672575 -41.00000 -1.20000
H28D 2 0.214654 0.575597 0.595011 -41.00000 -1.20000
AFIX 0
C27A 1 0.298847 0.627012 0.701716 -41.00000 0.14093
AFIX 23
H27C 2 0.321245 0.610040 0.761331 -41.00000 -1.20000
H27D 2 0.220944 0.656068 0.705693 -41.00000 -1.20000
AFIX 0
C26A 1 0.407165 0.670643 0.662488 -41.00000 0.14001
AFIX 23
H26C 2 0.375625 0.716980 0.640621 -41.00000 -1.20000
H26D 2 0.473254 0.679538 0.707270 -41.00000 -1.20000
AFIX 0
C25A 1 0.459501 0.627051 0.588079 -41.00000 0.14341
AFIX 23
H25C 2 0.434070 0.647155 0.530576 -41.00000 -1.20000
H25D 2 0.552980 0.624888 0.590886 -41.00000 -1.20000
AFIX 66
PART -1
C36 1 0.584493 0.059114 0.197637 10.50000 0.11677 0.10595 =
0.09786 0.00078 0.00308 0.04734
AFIX 43
H36 2 0.641970 0.091989 0.172039 10.50000 -1.20000
AFIX 65
C37 1 0.560791 0.061193 0.287484 10.50000 0.12334 0.12701 =
0.10471 -0.01350 0.00399 0.03584
AFIX 43
H37 2 0.602069 0.095489 0.323292 10.50000 -1.20000
AFIX 65
C32 1 0.476693 0.013093 0.324937 10.50000 0.11639 0.14047 =
0.09675 0.00401 0.00712 0.02688
AFIX 43
H32 2 0.460494 0.014514 0.386343 10.50000 -1.20000
AFIX 65
C33 1 0.416297 -0.037087 0.272543 10.50000 0.11678 0.12860 =
0.11753 0.01587 0.00237 0.02222
AFIX 43
H33 2 0.358820 -0.069962 0.298141 10.50000 -1.20000
AFIX 65
C34 1 0.439998 -0.039167 0.182697 10.50000 0.11363 0.10835 =
0.11089 -0.00921 -0.00267 0.03707
AFIX 43
H34 2 0.398719 -0.073462 0.146888 10.50000 -1.20000
AFIX 65
C35 1 0.524095 0.008933 0.145242 10.50000 0.10608 0.11281 =
0.08267 -0.01072 0.00429 0.05221
AFIX 43
H35 2 0.540293 0.007512 0.083836 10.50000 -1.20000
AFIX 0
PART 2
C22A 1 0.230315 0.409078 0.373864 -21.00000 0.03889 0.07567 =
0.05588 -0.00976 0.01625 -0.00994
AFIX 13
H22A 2 0.269675 0.448295 0.338848 -21.00000 -1.20000
AFIX 0
HKLF 4
REM en-p61-b(non)li_auto_a.res in P2(1)2(1)2
REM wR2 = 0.1331, GooF = S = 1.058, Restrained GooF = 1.144 for all data
REM R1 = 0.0474 for 5541 Fo > 4sig(Fo) and 0.0516 for all 6122 data
REM 431 parameters refined using 214 restraints
END
WGHT 0.0801 0.2581
REM Highest difference peak 0.249, deepest hole -0.190, 1-sigma level 0.036
Q1 1 0.4201 0.5472 0.6972 11.00000 0.05 0.25
Q2 1 0.3651 0.5279 0.6753 11.00000 0.05 0.22
Q3 1 0.4861 0.0468 0.3145 11.00000 0.05 0.21
Q4 1 0.4044 0.6140 0.5740 11.00000 0.05 0.20
Q5 1 0.4008 0.0029 0.2992 11.00000 0.05 0.13
Q6 1 0.6199 0.4985 0.7415 11.00000 0.05 0.12
Q7 1 0.4314 0.4134 0.0212 11.00000 0.05 0.12
Q8 1 0.4253 -0.0215 0.3036 11.00000 0.05 0.12
Q9 1 0.2969 0.3885 0.3767 11.00000 0.05 0.12
Q10 1 -0.0200 0.5516 0.0720 11.00000 0.05 0.12
Q11 1 0.4987 0.6543 0.6291 11.00000 0.05 0.11
Q12 1 0.5618 0.4357 0.2611 11.00000 0.05 0.11
Q13 1 0.5666 0.0721 0.2392 11.00000 0.05 0.11
Q14 1 0.1911 0.6241 0.7832 11.00000 0.05 0.11
Q15 1 0.6316 0.1623 0.3577 11.00000 0.05 0.10
Q16 1 0.6809 0.5553 0.7765 11.00000 0.05 0.10
Q17 1 0.5021 0.6262 0.7161 11.00000 0.05 0.10
Q18 1 0.0154 0.3465 0.3660 11.00000 0.05 0.10
Q19 1 0.4440 -0.0347 0.1501 11.00000 0.05 0.10
Q20 1 0.0339 0.6250 0.1706 11.00000 0.05 0.10
Q21 1 0.3284 0.4770 -0.1195 11.00000 0.05 0.10
Q22 1 0.2582 0.5526 0.0630 11.00000 0.05 0.09
Q23 1 0.0651 0.2513 0.2009 11.00000 0.05 0.09
Q24 1 0.5000 0.5000 0.1340 10.50000 0.05 0.09
Q25 1 0.1232 0.4838 0.0823 11.00000 0.05 0.09
Q26 1 0.8073 0.2350 0.3249 11.00000 0.05 0.09
Q27 1 0.6368 0.3407 0.2078 11.00000 0.05 0.09
Q28 1 0.8529 0.4245 0.3404 11.00000 0.05 0.09
Q29 1 0.5015 0.3355 0.3321 11.00000 0.05 0.09
Q30 1 0.0856 0.5469 0.1205 11.00000 0.05 0.09
Q31 1 -0.0932 0.6254 0.0177 11.00000 0.05 0.09
Q32 1 0.6248 0.5816 0.6638 11.00000 0.05 0.09
Q33 1 0.4015 0.3603 0.3630 11.00000 0.05 0.09
Q34 1 0.1153 0.5119 0.1145 11.00000 0.05 0.09
Q35 1 0.2208 0.2669 -0.0617 11.00000 0.05 0.09
Q36 1 0.0733 0.6253 0.7447 11.00000 0.05 0.09
Q37 1 0.3774 0.3524 -0.0800 11.00000 0.05 0.09
Q38 1 0.6015 0.2120 0.0855 11.00000 0.05 0.09
Q39 1 0.5836 0.5341 0.6845 11.00000 0.05 0.09
Q40 1 0.4986 0.2063 0.1552 11.00000 0.05 0.09
Q41 1 0.0573 0.3891 0.3475 11.00000 0.05 0.08
Q42 1 0.4685 0.0722 0.0836 11.00000 0.05 0.08
Q43 1 0.4322 0.5035 0.3882 11.00000 0.05 0.08
Q44 1 0.2365 0.3092 0.2477 11.00000 0.05 0.08
Q45 1 0.4957 0.1866 0.0428 11.00000 0.05 0.08
;
_shelx_res_checksum 26346
_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 1.648
_oxdiff_exptl_absorpt_empirical_full_min 0.757
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
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
O1 O 0.500000 0.500000 0.41119(14) 0.0392(5) Uani 1 2 d S T P A .
N1 N 0.47005(15) 0.43204(10) 0.27980(11) 0.0312(4) Uani 1 1 d . . . . .
C1 C 0.47531(17) 0.46355(10) 0.12238(13) 0.0276(4) Uani 1 1 d . . . . .
C2 C 0.44789(17) 0.41585(11) 0.19075(13) 0.0281(4) Uani 1 1 d . . . . .
C6 C 0.45884(19) 0.44206(11) 0.03487(13) 0.0307(4) Uani 1 1 d . . . . .
C3 C 0.39901(19) 0.34915(11) 0.16597(14) 0.0316(4) Uani 1 1 d . . . . .
H3 H 0.378290 0.316265 0.211156 0.038 Uiso 1 1 calc R U . . .
C4 C 0.3791(2) 0.32834(11) 0.07848(14) 0.0326(4) Uani 1 1 d . . . . .
C8 C 0.3221(2) 0.25461(12) 0.05990(16) 0.0379(5) Uani 1 1 d . . . . .
C7 C 0.500000 0.500000 -0.02813(19) 0.0335(6) Uani 1 2 d S T P . .
C5 C 0.4112(2) 0.37571(12) 0.01216(14) 0.0340(4) Uani 1 1 d . . . . .
H5 H 0.400778 0.362943 -0.047836 0.041 Uiso 1 1 calc R U . . .
O2 O 0.4359(4) 0.5688(2) 0.6047(2) 0.0702(12) Uani 0.767(8) 1 d D U P A 1
C13 C 0.4583(2) 0.37183(12) 0.33916(13) 0.0365(5) Uani 1 1 d . . . . .
C18 C 0.5589(2) 0.32416(14) 0.34613(15) 0.0445(5) Uani 1 1 d . . . . .
C10 C 0.1910(2) 0.25020(14) 0.10202(19) 0.0469(6) Uani 1 1 d . . . . .
H10A H 0.199092 0.253772 0.166045 0.070 Uiso 1 1 calc R U . . .
H10B H 0.151557 0.204667 0.086692 0.070 Uiso 1 1 calc R U . . .
H10C H 0.138306 0.289340 0.080295 0.070 Uiso 1 1 calc R U . . .
C14 C 0.3455(2) 0.36095(15) 0.38563(16) 0.0462(6) Uani 1 1 d D . . . .
C11 C 0.4080(3) 0.19641(13) 0.0981(2) 0.0494(6) Uani 1 1 d . . . . .
H11A H 0.492342 0.200038 0.071737 0.074 Uiso 1 1 calc R U . . .
H11B H 0.371953 0.149550 0.085050 0.074 Uiso 1 1 calc R U . . .
H11C H 0.414545 0.202510 0.161937 0.074 Uiso 1 1 calc R U . . .
C12 C 0.3897(3) 0.52520(14) -0.08574(16) 0.0451(5) Uani 1 1 d . . . . .
H12A H 0.363856 0.486629 -0.125214 0.068 Uiso 1 1 calc R U . . .
H12B H 0.416420 0.566400 -0.120583 0.068 Uiso 1 1 calc R U . . .
H12C H 0.318202 0.538675 -0.048224 0.068 Uiso 1 1 calc R U . . .
C22 C 0.2336(6) 0.4098(5) 0.3771(7) 0.0536(11) Uani 0.74(3) 1 d D U P B 1
H22 H 0.254763 0.450738 0.337779 0.064 Uiso 0.74(3) 1 calc R U P B 1
C30 C 0.1195(3) 0.53107(15) 0.1133(2) 0.0551(6) Uani 1 1 d D U . . .
H30 H 0.200796 0.552555 0.113413 0.066 Uiso 1 1 calc R U . . .
C19 C 0.6818(3) 0.33717(17) 0.29748(18) 0.0556(7) Uani 1 1 d D U . . .
H19 H 0.666260 0.368086 0.245070 0.067 Uiso 0.39(4) 1 calc R U P C 1
H19A H 0.658238 0.359679 0.240203 0.067 Uiso 0.61(4) 1 calc R U P C 2
C9 C 0.3063(3) 0.24115(14) -0.03885(18) 0.0473(6) Uani 1 1 d . . . . .
H9A H 0.251874 0.278016 -0.064222 0.071 Uiso 1 1 calc R U . . .
H9B H 0.267655 0.194342 -0.048030 0.071 Uiso 1 1 calc R U . . .
H9C H 0.389361 0.242477 -0.067457 0.071 Uiso 1 1 calc R U . . .
C17 C 0.5454(4) 0.26509(17) 0.4014(2) 0.0631(8) Uani 1 1 d . . . . .
H17 H 0.613033 0.232050 0.406485 0.076 Uiso 1 1 calc R U . . .
B1 B 0.500000 0.500000 0.3249(2) 0.0314(6) Uani 1 2 d S T P . .
C29 C 0.1068(3) 0.45890(15) 0.1129(3) 0.0663(8) Uani 1 1 d D U . . .
H29 H 0.180059 0.429630 0.112011 0.080 Uiso 1 1 calc R U . . .
C16 C 0.4371(4) 0.2540(2) 0.4482(2) 0.0724(10) Uani 1 1 d . . . . .
H16 H 0.429951 0.213851 0.485807 0.087 Uiso 1 1 calc R U . . .
C15 C 0.3387(3) 0.3010(2) 0.4407(2) 0.0658(9) Uani 1 1 d . . . . .
H15 H 0.263765 0.292893 0.473723 0.079 Uiso 1 1 calc R U . . .
C31 C 0.0117(3) 0.57203(17) 0.1137(3) 0.0760(9) Uani 1 1 d D U . . .
H31 H 0.018903 0.622413 0.114502 0.091 Uiso 1 1 calc R U . . .
C24 C 0.1229(6) 0.3667(6) 0.3385(8) 0.0642(18) Uani 0.74(3) 1 d D U P B 1
H24A H 0.150834 0.342420 0.284898 0.096 Uiso 0.74(3) 1 calc R U P B 1
H24B H 0.052859 0.398921 0.324388 0.096 Uiso 0.74(3) 1 calc R U P B 1
H24C H 0.094520 0.331410 0.381603 0.096 Uiso 0.74(3) 1 calc R U P B 1
C23 C 0.1961(10) 0.4368(5) 0.4683(6) 0.0649(19) Uani 0.74(3) 1 d D U P B 1
H23A H 0.168123 0.396635 0.504523 0.097 Uiso 0.74(3) 1 calc R U P B 1
H23B H 0.127124 0.471283 0.462670 0.097 Uiso 0.74(3) 1 calc R U P B 1
H23C H 0.269157 0.459685 0.496123 0.097 Uiso 0.74(3) 1 calc R U P B 1
C20 C 0.769(2) 0.3753(14) 0.3626(15) 0.070(4) Uani 0.39(4) 1 d D U P C 1
H20A H 0.728551 0.419507 0.382268 0.105 Uiso 0.39(4) 1 calc R U P C 1
H20B H 0.849372 0.386499 0.333744 0.105 Uiso 0.39(4) 1 calc R U P C 1
H20C H 0.784431 0.344465 0.413336 0.105 Uiso 0.39(4) 1 calc R U P C 1
C21 C 0.725(3) 0.2624(8) 0.2676(15) 0.075(4) Uani 0.39(4) 1 d D U P C 1
H21A H 0.734667 0.231641 0.319173 0.113 Uiso 0.39(4) 1 calc R U P C 1
H21B H 0.805669 0.266133 0.236603 0.113 Uiso 0.39(4) 1 calc R U P C 1
H21C H 0.660971 0.242063 0.228181 0.113 Uiso 0.39(4) 1 calc R U P C 1
C27 C 0.3157(6) 0.6468(3) 0.6894(3) 0.0712(14) Uani 0.767(8) 1 d D U P A 1
H27A H 0.265330 0.691083 0.686235 0.085 Uiso 0.767(8) 1 calc R U P A 1
H27B H 0.278579 0.614646 0.734093 0.085 Uiso 0.767(8) 1 calc R U P A 1
C26 C 0.4533(5) 0.6619(3) 0.7079(3) 0.0711(12) Uani 0.767(8) 1 d D U P A 1
H26A H 0.479376 0.707678 0.681313 0.085 Uiso 0.767(8) 1 calc R U P A 1
H26B H 0.469466 0.663691 0.771956 0.085 Uiso 0.767(8) 1 calc R U P A 1
C28 C 0.3259(6) 0.6110(3) 0.6008(3) 0.0822(15) Uani 0.767(8) 1 d D U P A 1
H28A H 0.250632 0.581005 0.589406 0.099 Uiso 0.767(8) 1 calc R U P A 1
H28B H 0.333015 0.646849 0.553392 0.099 Uiso 0.767(8) 1 calc R U P A 1
C25 C 0.5213(5) 0.6021(3) 0.6672(3) 0.0783(14) Uani 0.767(8) 1 d D U P A 1
H25A H 0.598069 0.619555 0.636777 0.094 Uiso 0.767(8) 1 calc R U P A 1
H25B H 0.547316 0.567413 0.712707 0.094 Uiso 0.767(8) 1 calc R U P A 1
Li1 Li 0.500000 0.500000 0.5228(4) 0.072(2) Uani 1 2 d S T P . .
C24A C 0.1236(18) 0.3873(15) 0.3105(16) 0.058(3) Uani 0.26(3) 1 d D U P B 2
H24D H 0.160346 0.370197 0.255280 0.087 Uiso 0.26(3) 1 calc R U P B 2
H24E H 0.069493 0.428581 0.298626 0.087 Uiso 0.26(3) 1 calc R U P B 2
H24F H 0.072974 0.349398 0.337262 0.087 Uiso 0.26(3) 1 calc R U P B 2
C23A C 0.172(3) 0.4528(15) 0.4488(16) 0.066(4) Uani 0.26(3) 1 d D U P B 2
H23D H 0.146491 0.420899 0.496490 0.098 Uiso 0.26(3) 1 calc R U P B 2
H23E H 0.098461 0.478829 0.426975 0.098 Uiso 0.26(3) 1 calc R U P B 2
H23F H 0.235245 0.486721 0.470979 0.098 Uiso 0.26(3) 1 calc R U P B 2
C21A C 0.7673(15) 0.2743(7) 0.2750(8) 0.067(3) Uani 0.61(4) 1 d D U P C 2
H21D H 0.801402 0.253789 0.329345 0.100 Uiso 0.61(4) 1 calc R U P C 2
H21E H 0.837106 0.290543 0.237742 0.100 Uiso 0.61(4) 1 calc R U P C 2
H21F H 0.718209 0.238051 0.243627 0.100 Uiso 0.61(4) 1 calc R U P C 2
C20A C 0.7648(13) 0.3916(7) 0.3461(8) 0.059(2) Uani 0.61(4) 1 d D U P C 2
H20D H 0.711914 0.430914 0.367176 0.088 Uiso 0.61(4) 1 calc R U P C 2
H20E H 0.829350 0.410114 0.305965 0.088 Uiso 0.61(4) 1 calc R U P C 2
H20F H 0.805964 0.368488 0.396297 0.088 Uiso 0.61(4) 1 calc R U P C 2
O2A O 0.405(2) 0.5572(13) 0.601(2) 0.129(7) Uiso 0.233(8) 1 d D U P A 2
C28A C 0.279(2) 0.5648(14) 0.640(2) 0.134(7) Uiso 0.233(8) 1 d D U P A 2
H28C H 0.254337 0.521357 0.672575 0.161 Uiso 0.233(8) 1 calc R U P A 2
H28D H 0.214654 0.575597 0.595011 0.161 Uiso 0.233(8) 1 calc R U P A 2
C27A C 0.299(4) 0.6270(19) 0.702(2) 0.141(7) Uiso 0.233(8) 1 d D U P A 2
H27C H 0.321245 0.610040 0.761331 0.169 Uiso 0.233(8) 1 calc R U P A 2
H27D H 0.220944 0.656068 0.705693 0.169 Uiso 0.233(8) 1 calc R U P A 2
C26A C 0.407(3) 0.6706(14) 0.662(2) 0.140(7) Uiso 0.233(8) 1 d D U P A 2
H26C H 0.375625 0.716980 0.640621 0.168 Uiso 0.233(8) 1 calc R U P A 2
H26D H 0.473254 0.679538 0.707270 0.168 Uiso 0.233(8) 1 calc R U P A 2
C25A C 0.460(3) 0.6271(14) 0.588(2) 0.143(7) Uiso 0.233(8) 1 d D U P A 2
H25C H 0.434070 0.647155 0.530576 0.172 Uiso 0.233(8) 1 calc R U P A 2
H25D H 0.552980 0.624888 0.590886 0.172 Uiso 0.233(8) 1 calc R U P A 2
C36 C 0.5845(9) 0.0591(6) 0.1976(5) 0.107(3) Uani 0.5 1 d G U P D -1
H36 H 0.641970 0.091989 0.172039 0.128 Uiso 0.5 1 calc R U P D -1
C37 C 0.5608(9) 0.0612(6) 0.2875(5) 0.118(3) Uani 0.5 1 d G U P D -1
H37 H 0.602069 0.095489 0.323292 0.142 Uiso 0.5 1 calc R U P D -1
C32 C 0.4767(11) 0.0131(7) 0.3249(3) 0.118(3) Uani 0.5 1 d G U P D -1
H32 H 0.460494 0.014514 0.386343 0.141 Uiso 0.5 1 calc R U P D -1
C33 C 0.4163(9) -0.0371(6) 0.2725(6) 0.121(3) Uani 0.5 1 d G U P D -1
H33 H 0.358820 -0.069962 0.298141 0.145 Uiso 0.5 1 calc R U P D -1
C34 C 0.4400(10) -0.0392(6) 0.1827(6) 0.111(3) Uani 0.5 1 d G U P D -1
H34 H 0.398719 -0.073462 0.146888 0.133 Uiso 0.5 1 calc R U P D -1
C35 C 0.5241(11) 0.0089(7) 0.1452(3) 0.101(3) Uani 0.5 1 d G U P D -1
H35 H 0.540293 0.007512 0.083836 0.121 Uiso 0.5 1 calc R U P D -1
C22A C 0.230(2) 0.4091(16) 0.3739(19) 0.057(2) Uani 0.26(3) 1 d D U P B 2
H22A H 0.269675 0.448295 0.338848 0.068 Uiso 0.26(3) 1 calc R U P B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0384(11) 0.0519(13) 0.0271(10) 0.000 0.000 -0.0072(10)
N1 0.0282(8) 0.0391(9) 0.0263(8) 0.0030(7) -0.0005(6) -0.0031(7)
C1 0.0231(8) 0.0307(10) 0.0290(9) -0.0014(7) -0.0003(7) 0.0030(7)
C2 0.0221(8) 0.0347(10) 0.0275(9) 0.0007(7) -0.0010(7) 0.0028(7)
C6 0.0325(9) 0.0310(10) 0.0286(9) -0.0007(8) -0.0022(7) 0.0047(8)
C3 0.0271(9) 0.0335(10) 0.0341(9) 0.0031(8) -0.0007(8) 0.0007(8)
C4 0.0297(9) 0.0309(9) 0.0370(10) -0.0013(8) -0.0034(8) 0.0033(8)
C8 0.0366(11) 0.0323(10) 0.0448(12) -0.0021(9) -0.0036(9) 0.0022(9)
C7 0.0402(15) 0.0328(14) 0.0275(13) 0.000 0.000 0.0039(12)
C5 0.0369(10) 0.0330(10) 0.0322(10) -0.0029(8) -0.0030(8) 0.0050(8)
O2 0.092(2) 0.084(2) 0.0350(13) -0.0172(13) 0.0000(14) 0.030(2)
C13 0.0384(10) 0.0443(12) 0.0269(9) 0.0043(8) -0.0003(8) -0.0076(10)
C18 0.0500(13) 0.0503(13) 0.0331(11) 0.0096(10) -0.0059(10) -0.0010(11)
C10 0.0414(12) 0.0411(12) 0.0583(15) -0.0064(11) 0.0000(11) -0.0078(10)
C14 0.0453(12) 0.0577(15) 0.0356(11) -0.0013(11) 0.0049(10) -0.0181(11)
C11 0.0527(14) 0.0343(11) 0.0611(15) 0.0007(11) -0.0071(12) 0.0062(11)
C12 0.0581(14) 0.0405(11) 0.0368(11) 0.0015(9) -0.0110(10) 0.0040(11)
C22 0.0345(18) 0.072(2) 0.054(2) -0.0102(19) 0.0138(17) -0.0146(18)
C30 0.0432(11) 0.0499(13) 0.0722(16) 0.0021(12) 0.0069(11) 0.0065(11)
C19 0.0446(13) 0.0779(19) 0.0442(13) 0.0177(13) -0.0018(11) 0.0193(13)
C9 0.0537(14) 0.0379(11) 0.0502(14) -0.0105(10) -0.0057(11) -0.0035(11)
C17 0.083(2) 0.0577(16) 0.0483(15) 0.0197(13) -0.0132(15) -0.0013(16)
B1 0.0215(12) 0.0460(18) 0.0265(14) 0.000 0.000 0.0002(13)
C29 0.0455(13) 0.0520(15) 0.101(2) -0.0116(15) -0.0136(15) 0.0179(12)
C16 0.097(3) 0.067(2) 0.0534(17) 0.0278(15) -0.0087(16) -0.021(2)
C15 0.075(2) 0.078(2) 0.0443(14) 0.0093(14) 0.0108(14) -0.0358(18)
C31 0.0564(15) 0.0425(13) 0.129(3) 0.0132(17) 0.0178(17) 0.0063(12)
C24 0.0362(19) 0.085(4) 0.071(4) -0.003(3) 0.005(3) -0.014(2)
C23 0.060(3) 0.081(4) 0.053(3) -0.007(3) 0.017(2) 0.003(3)
C20 0.035(4) 0.100(8) 0.074(7) 0.024(6) -0.009(5) 0.007(6)
C21 0.058(8) 0.100(7) 0.067(6) 0.006(5) 0.000(6) 0.029(6)
C27 0.081(3) 0.073(3) 0.059(2) -0.018(2) -0.008(2) 0.027(2)
C26 0.076(2) 0.072(3) 0.065(2) -0.015(2) 0.006(2) 0.007(2)
C28 0.101(3) 0.085(3) 0.060(2) -0.019(2) -0.027(2) 0.035(3)
C25 0.076(3) 0.090(3) 0.069(2) -0.022(2) 0.002(2) 0.012(2)
Li1 0.086(5) 0.097(6) 0.033(3) 0.000 0.000 0.035(5)
C24A 0.035(5) 0.081(7) 0.058(7) 0.000(6) 0.013(5) -0.010(5)
C23A 0.058(7) 0.081(7) 0.057(7) -0.008(6) 0.017(5) 0.003(6)
C21A 0.050(5) 0.096(5) 0.054(3) -0.003(3) -0.002(4) 0.026(4)
C20A 0.034(3) 0.082(5) 0.061(4) 0.024(3) 0.000(3) 0.010(3)
C36 0.117(5) 0.106(7) 0.098(5) 0.001(5) 0.003(4) 0.047(5)
C37 0.123(5) 0.127(8) 0.105(5) -0.014(5) 0.004(5) 0.036(5)
C32 0.116(6) 0.140(8) 0.097(5) 0.004(5) 0.007(4) 0.027(5)
C33 0.117(5) 0.129(8) 0.118(5) 0.016(5) 0.002(5) 0.022(5)
C34 0.114(5) 0.108(8) 0.111(5) -0.009(5) -0.003(5) 0.037(5)
C35 0.106(6) 0.113(7) 0.083(4) -0.011(5) 0.004(4) 0.052(5)
C22A 0.039(4) 0.076(4) 0.056(4) -0.010(4) 0.016(4) -0.010(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
B1 O1 Li1 180.0 . 2_665 ?
B1 O1 Li1 180.0 . . ?
Li1 O1 Li1 0.000(1) 2_665 . ?
C2 N1 C13 114.54(17) . . ?
C2 N1 B1 131.76(19) . . ?
C13 N1 B1 113.67(17) . . ?
C2 C1 C1 132.10(11) . 2_665 ?
C6 C1 C1 108.27(12) . 2_665 ?
C6 C1 C2 119.61(18) . . ?
C1 C2 N1 122.73(18) . . ?
C1 C2 C3 116.50(17) . . ?
C3 C2 N1 120.75(18) . . ?
C1 C6 C7 110.98(18) . . ?
C5 C6 C1 122.69(19) . . ?
C5 C6 C7 126.34(19) . . ?
C2 C3 H3 118.1 . . ?
C4 C3 C2 123.89(19) . . ?
C4 C3 H3 118.1 . . ?
C3 C4 C8 118.98(19) . . ?
C5 C4 C3 118.3(2) . . ?
C5 C4 C8 122.72(19) . . ?
C10 C8 C4 109.07(18) . . ?
C10 C8 C11 109.8(2) . . ?
C10 C8 C9 107.6(2) . . ?
C11 C8 C4 109.94(19) . . ?
C9 C8 C4 111.8(2) . . ?
C9 C8 C11 108.5(2) . . ?
C6 C7 C6 101.5(2) 2_665 . ?
C6 C7 C12 110.98(12) . 2_665 ?
C6 C7 C12 110.98(12) 2_665 . ?
C6 C7 C12 111.40(13) 2_665 2_665 ?
C6 C7 C12 111.41(13) . . ?
C12 C7 C12 110.3(3) 2_665 . ?
C6 C5 H5 120.5 . . ?
C4 C5 C6 118.95(19) . . ?
C4 C5 H5 120.5 . . ?
C28 O2 C25 107.4(4) . . ?
C28 O2 Li1 130.0(3) . 2_665 ?
C28 O2 Li1 130.0(3) . . ?
C25 O2 Li1 119.7(3) . . ?
C25 O2 Li1 119.7(3) . 2_665 ?
Li1 O2 Li1 0.0(3) 2_665 . ?
C18 C13 N1 118.86(19) . . ?
C18 C13 C14 121.1(2) . . ?
C14 C13 N1 120.0(2) . . ?
C13 C18 C19 120.9(2) . . ?
C13 C18 C17 118.5(3) . . ?
C17 C18 C19 120.6(3) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C14 C22 122.5(5) . . ?
C13 C14 C15 117.5(3) . . ?
C13 C14 C22A 122.2(15) . . ?
C15 C14 C22 120.0(6) . . ?
C15 C14 C22A 120.2(15) . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C22 H22 110.2 . . ?
C14 C22 C24 108.1(6) . . ?
C14 C22 C23 109.2(7) . . ?
C24 C22 H22 110.2 . . ?
C23 C22 H22 110.2 . . ?
C23 C22 C24 108.9(6) . . ?
C29 C30 H30 120.8 . . ?
C29 C30 C31 118.4(3) . . ?
C31 C30 H30 120.8 . . ?
C18 C19 H19 110.0 . . ?
C18 C19 H19A 106.3 . . ?
C18 C19 C20 106.0(11) . . ?
C18 C19 C21 104.4(11) . . ?
C18 C19 C21A 119.5(7) . . ?
C18 C19 C20A 111.2(6) . . ?
C20 C19 H19 110.0 . . ?
C20 C19 C21 116.1(11) . . ?
C21 C19 H19 110.0 . . ?
C21A C19 H19A 106.3 . . ?
C21A C19 C20A 106.6(7) . . ?
C20A C19 H19A 106.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C18 C17 H17 119.3 . . ?
C16 C17 C18 121.3(3) . . ?
C16 C17 H17 119.3 . . ?
O1 B1 N1 117.52(12) . . ?
O1 B1 N1 117.51(12) . 2_665 ?
N1 B1 N1 125.0(2) . 2_665 ?
C30 C29 H29 119.7 . . ?
C30 C29 C31 120.5(3) . 2_565 ?
C31 C29 H29 119.7 2_565 . ?
C17 C16 H16 120.1 . . ?
C17 C16 C15 119.7(3) . . ?
C15 C16 H16 120.1 . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.8(3) . . ?
C16 C15 H15 119.1 . . ?
C30 C31 C29 121.1(3) . 2_565 ?
C30 C31 H31 119.5 . . ?
C29 C31 H31 119.5 2_565 . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27A 111.7 . . ?
C26 C27 H27B 111.7 . . ?
C26 C27 C28 100.4(4) . . ?
C28 C27 H27A 111.7 . . ?
C28 C27 H27B 111.7 . . ?
C27 C26 H26A 110.9 . . ?
C27 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
C25 C26 C27 104.4(4) . . ?
C25 C26 H26A 110.9 . . ?
C25 C26 H26B 110.9 . . ?
O2 C28 C27 105.7(4) . . ?
O2 C28 H28A 110.6 . . ?
O2 C28 H28B 110.6 . . ?
C27 C28 H28A 110.6 . . ?
C27 C28 H28B 110.6 . . ?
H28A C28 H28B 108.7 . . ?
O2 C25 C26 107.5(4) . . ?
O2 C25 H25A 110.2 . . ?
O2 C25 H25B 110.2 . . ?
C26 C25 H25A 110.2 . . ?
C26 C25 H25B 110.2 . . ?
H25A C25 H25B 108.5 . . ?
O1 Li1 O2 130.50(19) . 2_665 ?
O1 Li1 O2 130.50(19) . . ?
O1 Li1 O2A 128.9(10) . 2_665 ?
O1 Li1 O2A 128.9(10) . . ?
O1 Li1 C25A 112.3(7) . 2_665 ?
O2 Li1 O2 99.0(4) 2_665 . ?
O2 Li1 C25A 115.2(8) . 2_665 ?
O2 Li1 C25A 23.5(5) 2_665 2_665 ?
Li1 Li1 O1 0(10) 2_665 . ?
Li1 Li1 O2 0(10) 2_665 2_665 ?
Li1 Li1 O2 0(10) 2_665 . ?
Li1 Li1 O2A 0(10) 2_665 . ?
Li1 Li1 O2A 0(10) 2_665 2_665 ?
Li1 Li1 C25A 0(10) 2_665 2_665 ?
O2A Li1 O2A 102(2) 2_665 . ?
O2A Li1 C25A 111.4(13) . 2_665 ?
O2A Li1 C25A 32.7(6) 2_665 2_665 ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C22A C24A H24D 109.5 . . ?
C22A C24A H24E 109.5 . . ?
C22A C24A H24F 109.5 . . ?
H23D C23A H23E 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C22A C23A H23D 109.5 . . ?
C22A C23A H23E 109.5 . . ?
C22A C23A H23F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
Li1 O2A Li1 0.0(3) 2_665 . ?
C28A O2A Li1 143(2) . . ?
C25A O2A Li1 102.4(17) . . ?
C25A O2A C28A 109.3(19) . . ?
O2A C28A H28C 111.4 . . ?
O2A C28A H28D 111.4 . . ?
O2A C28A C27A 101.8(19) . . ?
H28C C28A H28D 109.3 . . ?
C27A C28A H28C 111.4 . . ?
C27A C28A H28D 111.4 . . ?
C28A C27A H27C 110.5 . . ?
C28A C27A H27D 110.5 . . ?
C28A C27A C26A 105.9(9) . . ?
H27C C27A H27D 108.7 . . ?
C26A C27A H27C 110.5 . . ?
C26A C27A H27D 110.5 . . ?
C27A C26A H26C 110.5 . . ?
C27A C26A H26D 110.5 . . ?
H26C C26A H26D 108.7 . . ?
C25A C26A C27A 106.1(9) . . ?
C25A C26A H26C 110.5 . . ?
C25A C26A H26D 110.5 . . ?
O2A C25A C26A 104.1(17) . . ?
O2A C25A H25C 110.9 . . ?
O2A C25A H25D 110.9 . . ?
C26A C25A H25C 110.9 . . ?
C26A C25A H25D 110.9 . . ?
H25C C25A H25D 109.0 . . ?
C37 C36 H36 120.0 . . ?
C37 C36 C35 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 H37 120.0 . . ?
C36 C37 C32 120.0 . . ?
C32 C37 H37 120.0 . . ?
C37 C32 H32 120.0 . . ?
C33 C32 C37 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C14 C22A C24A 120.0(18) . . ?
C14 C22A C23A 123(2) . . ?
C14 C22A H22A 99.6 . . ?
C24A C22A H22A 99.6 . . ?
C23A C22A C24A 108.4(9) . . ?
C23A C22A H22A 99.6 . . ?
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
O1 B1 1.313(4) . ?
O1 Li1 1.697(7) . ?
O1 Li1 1.697(7) 2_665 ?
N1 C2 1.408(3) . ?
N1 C13 1.453(3) . ?
N1 B1 1.484(2) . ?
C1 C1 1.466(4) 2_665 ?
C1 C2 1.403(3) . ?
C1 C6 1.402(3) . ?
C2 C3 1.407(3) . ?
C6 C7 1.514(3) . ?
C6 C5 1.388(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.403(3) . ?
C4 C8 1.537(3) . ?
C4 C5 1.388(3) . ?
C8 C10 1.530(3) . ?
C8 C11 1.536(3) . ?
C8 C9 1.532(3) . ?
C7 C12 1.534(3) . ?
C7 C12 1.534(3) 2_665 ?
C5 H5 0.9500 . ?
O2 C28 1.408(6) . ?
O2 C25 1.453(6) . ?
O2 Li1 1.920(5) 2_665 ?
O2 Li1 1.920(5) . ?
C13 C18 1.394(3) . ?
C13 C14 1.402(3) . ?
C18 C19 1.515(4) . ?
C18 C17 1.400(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C14 C22 1.503(6) . ?
C14 C15 1.406(4) . ?
C14 C22A 1.527(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C24 1.540(6) . ?
C22 C23 1.529(6) . ?
C30 H30 0.9500 . ?
C30 C29 1.363(3) . ?
C30 C31 1.375(4) . ?
C19 H19 1.0000 . ?
C19 H19A 1.0000 . ?
C19 C20 1.530(10) . ?
C19 C21 1.544(10) . ?
C19 C21A 1.527(7) . ?
C19 C20A 1.537(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C17 H17 0.9500 . ?
C17 C16 1.364(5) . ?
C29 H29 0.9500 . ?
C29 C31 1.381(4) 2_565 ?
C16 H16 0.9500 . ?
C16 C15 1.369(6) . ?
C15 H15 0.9500 . ?
C31 H31 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.508(8) . ?
C27 C28 1.511(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C25 1.469(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
Li1 Li1 0.000(13) 2_665 ?
Li1 O2A 1.90(2) 2_665 ?
Li1 O2A 1.90(2) . ?
Li1 C25A 2.62(3) 2_665 ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C24A C22A 1.539(10) . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C23A C22A 1.533(10) . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
O2A C28A 1.457(11) . ?
O2A C25A 1.449(11) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C28A C27A 1.512(11) . ?
C27A H27C 0.9900 . ?
C27A H27D 0.9900 . ?
C27A C26A 1.530(10) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C26A C25A 1.503(11) . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
C36 H36 0.9500 . ?
C36 C37 1.3900 . ?
C36 C35 1.3900 . ?
C37 H37 0.9500 . ?
C37 C32 1.3900 . ?
C32 H32 0.9500 . ?
C32 C33 1.3900 . ?
C33 H33 0.9500 . ?
C33 C34 1.3900 . ?
C34 H34 0.9500 . ?
C34 C35 1.3900 . ?
C35 H35 0.9500 . ?
C22A H22A 1.0000 . ?
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
O1 Li1 O2A Li1 0(100) . . . 2_665 ?
O1 Li1 O2A C28A 79(4) . . . . ?
O1 Li1 O2A C25A -69(2) . . . . ?
N1 C2 C3 C4 -177.49(19) . . . . ?
N1 C13 C18 C19 4.0(3) . . . . ?
N1 C13 C18 C17 -178.1(2) . . . . ?
N1 C13 C14 C22 -0.3(5) . . . . ?
N1 C13 C14 C15 178.7(2) . . . . ?
N1 C13 C14 C22A 2.3(10) . . . . ?
C1 C1 C2 N1 -2.3(4) 2_665 . . . ?
C1 C1 C2 C3 179.1(2) 2_665 . . . ?
C1 C1 C6 C7 1.3(2) 2_665 . . . ?
C1 C1 C6 C5 -178.9(2) 2_665 . . . ?
C1 C2 C3 C4 1.1(3) . . . . ?
C1 C6 C7 C6 -0.52(10) . . . 2_665 ?
C1 C6 C7 C12 118.0(2) . . . 2_665 ?
C1 C6 C7 C12 -118.7(2) . . . . ?
C1 C6 C5 C4 -0.4(3) . . . . ?
C2 N1 C13 C18 79.9(2) . . . . ?
C2 N1 C13 C14 -97.6(2) . . . . ?
C2 N1 B1 O1 171.56(15) . . . . ?
C2 N1 B1 N1 -8.44(15) . . . 2_665 ?
C2 C1 C6 C7 -177.11(15) . . . . ?
C2 C1 C6 C5 2.6(3) . . . . ?
C2 C3 C4 C8 -178.58(18) . . . . ?
C2 C3 C4 C5 1.1(3) . . . . ?
C6 C1 C2 N1 175.68(18) . . . . ?
C6 C1 C2 C3 -2.9(3) . . . . ?
C3 C4 C8 C10 60.7(3) . . . . ?
C3 C4 C8 C11 -59.7(3) . . . . ?
C3 C4 C8 C9 179.6(2) . . . . ?
C3 C4 C5 C6 -1.5(3) . . . . ?
C8 C4 C5 C6 178.20(19) . . . . ?
C7 C6 C5 C4 179.34(17) . . . . ?
C5 C6 C7 C6 179.7(2) . . . 2_665 ?
C5 C6 C7 C12 61.6(3) . . . . ?
C5 C6 C7 C12 -61.8(3) . . . 2_665 ?
C5 C4 C8 C10 -118.9(2) . . . . ?
C5 C4 C8 C11 120.6(2) . . . . ?
C5 C4 C8 C9 0.0(3) . . . . ?
C13 N1 C2 C1 -168.96(18) . . . . ?
C13 N1 C2 C3 9.5(3) . . . . ?
C13 N1 B1 O1 -6.57(16) . . . . ?
C13 N1 B1 N1 173.43(16) . . . 2_665 ?
C13 C18 C19 C20 94.5(11) . . . . ?
C13 C18 C19 C21 -142.4(10) . . . . ?
C13 C18 C19 C21A -155.4(7) . . . . ?
C13 C18 C19 C20A 79.8(7) . . . . ?
C13 C18 C17 C16 -0.4(4) . . . . ?
C13 C14 C22 C24 117.1(7) . . . . ?
C13 C14 C22 C23 -124.7(6) . . . . ?
C13 C14 C15 C16 -1.1(4) . . . . ?
C13 C14 C22A C24A 96(3) . . . . ?
C13 C14 C22A C23A -119(3) . . . . ?
C18 C13 C14 C22 -177.8(4) . . . . ?
C18 C13 C14 C15 1.2(4) . . . . ?
C18 C13 C14 C22A -175.2(10) . . . . ?
C18 C17 C16 C15 0.6(5) . . . . ?
C14 C13 C18 C19 -178.5(2) . . . . ?
C14 C13 C18 C17 -0.5(4) . . . . ?
C22 C14 C15 C16 178.0(4) . . . . ?
C19 C18 C17 C16 177.6(3) . . . . ?
C17 C18 C19 C20 -83.4(12) . . . . ?
C17 C18 C19 C21 39.7(10) . . . . ?
C17 C18 C19 C21A 26.7(7) . . . . ?
C17 C18 C19 C20A -98.1(7) . . . . ?
C17 C16 C15 C14 0.2(5) . . . . ?
B1 N1 C2 C1 12.9(3) . . . . ?
B1 N1 C2 C3 -168.57(16) . . . . ?
B1 N1 C13 C18 -101.6(2) . . . . ?
B1 N1 C13 C14 80.8(2) . . . . ?
C29 C30 C31 C29 -0.5(6) . . . 2_565 ?
C15 C14 C22 C24 -61.9(8) . . . . ?
C15 C14 C22 C23 56.4(7) . . . . ?
C15 C14 C22A C24A -80(3) . . . . ?
C15 C14 C22A C23A 65(3) . . . . ?
C31 C30 C29 C31 -0.7(5) . . . 2_565 ?
C27 C26 C25 O2 18.2(6) . . . . ?
C26 C27 C28 O2 37.8(6) . . . . ?
C28 O2 C25 C26 5.9(6) . . . . ?
C28 C27 C26 C25 -33.3(6) . . . . ?
C25 O2 C28 C27 -27.8(6) . . . . ?
Li1 O1 Li1 O2 0(78) 2_665 . . 2_665 ?
Li1 O1 Li1 O2 0(100) 2_665 . . . ?
Li1 O1 Li1 O2A 0(62) 2_665 . . 2_665 ?
Li1 O1 Li1 O2A 0(100) 2_665 . . . ?
Li1 O1 Li1 C25A 0(100) 2_665 . . 2_665 ?
Li1 O2 C28 C27 172.1(4) . . . . ?
Li1 O2 C28 C27 172.1(4) 2_665 . . . ?
Li1 O2 C25 C26 168.5(4) 2_665 . . . ?
Li1 O2 C25 C26 168.5(4) . . . . ?
Li1 Li1 O2A C28A 0.0(3) 2_665 . . . ?
Li1 Li1 O2A C25A 0.0(6) 2_665 . . . ?
Li1 O2A C28A C27A 176(4) 2_665 . . . ?
Li1 O2A C28A C27A 176(4) . . . . ?
Li1 O2A C25A C26A -168(2) 2_665 . . . ?
Li1 O2A C25A C26A -168(2) . . . . ?
O2A Li1 O2A Li1 0(100) 2_665 . . 2_665 ?
O2A Li1 O2A C28A -101(4) 2_665 . . . ?
O2A Li1 O2A C25A 111(2) 2_665 . . . ?
O2A C28A C27A C26A 26(4) . . . . ?
C28A O2A C25A C26A 32(4) . . . . ?
C28A C27A C26A C25A -8(5) . . . . ?
C27A C26A C25A O2A -13(4) . . . . ?
C25A Li1 O2A Li1 0(100) 2_665 . . 2_665 ?
C25A Li1 O2A C28A -68(4) 2_665 . . . ?
C25A Li1 O2A C25A 143.7(19) 2_665 . . . ?
C25A O2A C28A C27A -37(4) . . . . ?
C36 C37 C32 C33 0.0 . . . . ?
C37 C36 C35 C34 0.0 . . . . ?
C37 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C22A C14 C15 C16 175.5(10) . . . . ?