#------------------------------------------------------------------------------
#$Date: 2026-06-04 10:24:35 +0100 (Thu, 04 Jun 2026) $
#$Revision: 306203 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577372.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_1577372
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 'C52 H74 B Li N2 O3'
_chemical_formula_sum 'C52 H74 B Li N2 O3'
_chemical_formula_weight 792.88
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_date 2023-06-30
_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 90.510(2)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 19.3413(4)
_cell_length_b 10.2642(2)
_cell_length_c 48.7620(8)
_cell_measurement_reflns_used 14946
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 77.8350
_cell_measurement_theta_min 3.6120
_cell_volume 9680.0(3)
_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 0.988
_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 -2.00 24.00 0.50 1.50 -- -46.70 15.00 -38.00 52
2 \w -120.00 -95.00 0.50 1.50 -- -46.70 -15.00 151.00 50
3 \w 36.00 61.00 0.50 1.50 -- 46.70 15.00 -38.00 50
4 \w 127.00 178.00 0.50 4.00 -- 107.75 15.00 -38.00 102
5 \w 93.00 119.00 0.50 4.00 -- 107.75 15.00 -38.00 52
6 \w -86.00 -12.00 0.50 1.50 -- -46.70 125.00-120.00 148
7 \w -42.00 -2.00 0.50 1.50 -- -46.70 57.00 120.00 80
8 \w -36.00 23.00 0.50 1.50 -- -46.70 57.00-150.00 118
9 \w -8.00 21.00 0.50 1.50 -- -46.70 19.00 90.00 58
10 \w -4.00 26.00 0.50 1.50 -- -46.70 38.00 150.00 60
11 \w -22.00 18.00 0.50 1.50 -- -46.70 38.00 30.00 80
12 \w 56.00 91.00 0.50 1.50 -- 46.70-125.00 60.00 70
13 \w 69.00 112.00 0.50 1.50 -- 46.70 15.00 -38.00 86
14 \w -25.00 36.00 0.50 1.50 -- 46.70 -15.00 151.00 122
15 \w 99.00 176.00 0.50 4.00 -- 107.75 30.00-150.00 154
16 \w 39.00 108.00 0.50 4.00 -- 107.75-104.00 114.47 138
17 \w 44.00 107.00 0.50 4.00 -- 107.75-103.00 152.67 126
18 \w 52.00 78.00 0.50 4.00 -- 107.75 -77.00-120.00 52
19 \w 93.00 118.00 0.50 4.00 -- 107.75 -77.00-120.00 50
20 \w 35.00 74.00 0.50 4.00 -- 107.75 -61.00 90.00 78
21 \w 64.00 111.00 0.50 4.00 -- 107.75-125.00 90.00 94
22 \w 34.00 73.00 0.50 4.00 -- 107.75 -95.00-180.00 78
23 \w 96.00 135.00 0.50 4.00 -- 107.75 30.00 -90.00 78
24 \w 77.00 104.00 0.50 4.00 -- 107.75 -95.00 -30.00 54
25 \w 32.00 59.00 0.50 4.00 -- 107.75 -30.00-120.00 54
26 \w 153.00 178.00 0.50 4.00 -- 107.75 30.00 -90.00 50
27 \w 74.00 108.00 0.50 4.00 -- 107.75-104.00-159.17 68
28 \w 79.00 105.00 0.50 4.00 -- 107.75 -95.00-120.00 52
29 \w 35.00 64.00 0.50 4.00 -- 107.75 -45.00 30.00 58
30 \w 45.00 72.00 0.50 4.00 -- 107.75 -45.00 -30.00 54
31 \w 49.00 74.00 0.50 4.00 -- 107.75 -95.00 -30.00 50
32 \w 37.00 63.00 0.50 4.00 -- 107.75 -95.00 0.00 52
33 \w 74.00 106.00 0.50 4.00 -- 107.75 -95.00 0.00 64
34 \w 91.00 116.00 0.50 4.00 -- 107.75 61.00 -60.00 50
35 \w 151.00 176.00 0.50 4.00 -- 107.75 61.00 -60.00 50
36 \w 34.00 59.00 0.50 4.00 -- 107.75 -30.00-150.00 50
37 \w 75.00 110.00 0.50 4.00 -- 107.75-125.00 120.00 70
38 \w 37.00 69.00 0.50 4.00 -- 107.75-125.00 120.00 64
39 \w 35.00 69.00 0.50 4.00 -- 107.75 -45.00 0.00 68
40 \w 72.00 107.00 0.50 4.00 -- 107.75-125.00 -90.00 70
41 \w 37.00 63.00 0.50 4.00 -- 107.75-125.00 -90.00 52
42 \w 41.00 90.00 0.50 4.00 -- 107.75 -61.00 150.00 98
43 \w 100.00 173.00 0.50 4.00 -- 107.75 15.00 0.00 146
44 \w 60.00 106.00 0.50 4.00 -- 107.75 -95.00 -90.00 92
45 \w 75.00 100.00 0.50 4.00 -- 107.75 -95.00 150.00 50
46 \w 39.00 64.00 0.50 4.00 -- 107.75 -45.00-120.00 50
47 \w 116.00 174.00 0.50 4.00 -- 107.75 15.00 30.00 116
48 \w 97.00 138.00 0.50 4.00 -- 107.75 125.00-120.00 82
49 \w 141.00 166.00 0.50 4.00 -- 107.75 125.00-120.00 50
50 \w 57.00 93.00 0.50 4.00 -- 107.75 -61.00 -60.00 72
51 \w 50.00 75.00 0.50 4.00 -- 107.75-141.00 138.26 50
52 \w 36.00 65.00 0.50 4.00 -- 107.75 -95.00-120.00 58
;
_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 0.0331932000
_diffrn_orient_matrix_UB_12 -0.1356110000
_diffrn_orient_matrix_UB_13 0.0034026000
_diffrn_orient_matrix_UB_21 0.0709049000
_diffrn_orient_matrix_UB_22 0.0642635000
_diffrn_orient_matrix_UB_23 0.0051313000
_diffrn_orient_matrix_UB_31 -0.0146404000
_diffrn_orient_matrix_UB_32 0.0041573000
_diffrn_orient_matrix_UB_33 0.0309847000
_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 0.1040
_diffrn_reflns_av_unetI/netI 0.0652
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 60
_diffrn_reflns_limit_l_min -39
_diffrn_reflns_number 65083
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.129
_diffrn_reflns_theta_min 3.626
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 0.498
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.85555
_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 1.088
_exptl_crystal_description block
_exptl_crystal_F_000 3456
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.045
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.339
_refine_diff_density_min -0.255
_refine_diff_density_rms 0.044
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 577
_refine_ls_number_reflns 10240
_refine_ls_number_restraints 122
_refine_ls_restrained_S_all 1.052
_refine_ls_R_factor_all 0.0822
_refine_ls_R_factor_gt 0.0523
_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^)+(0.0603P)^2^+2.7663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1253
_refine_ls_wR_factor_ref 0.1412
_reflns_Friedel_coverage 0.000
_reflns_number_gt 6970
_reflns_number_total 10240
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d6sc01056c2.cif
_cod_data_source_block 4-Li
_cod_database_code 1577372
_shelx_shelxl_version_number 2018/3
_chemical_oxdiff_formula 'C52 H74 B1 Li1 N2 O3'
_chemical_oxdiff_usercomment THF
_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 0.985
_shelx_estimated_absorpt_t_min 0.952
_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
C18-C17 = C18A-C17 = C19A-C17 = C19-C17 = C20-C17 = C20A-C17
1.53 with sigma of 0.008
C18A-C19A = C20A-C20 = C18-C19
2.5 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C18 \\sim C18A \\sim C19A \\sim C19 \\sim C20 \\sim C20A \\sim C17: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C49 \\sim O3 \\sim C52 \\sim C51 \\sim C50: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
O2 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
4. Others
Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
Sof(H20F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
C27(H27), C42(H42), C39(H39), C30(H30)
5.b Secondary CH2 refined with riding coordinates:
C45(H45A,H45B), C52(H52A,H52B), C49(H49A,H49B), C51(H51A,H51B), C48(H48A,
H48B), C46(H46A,H46B), C50(H50A,H50B), C47(H47A,H47B)
5.c Aromatic/amide H refined with riding coordinates:
C3(H3), C13(H13), C6(H6), C5(H5), C16(H16), C15(H15), C37(H37), C35(H35),
C25(H25), C23(H23), C36(H36), C24(H24)
5.d Idealised Me refined as rotating group:
C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C43(H43A,H43B,H43C),
C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C31(H31A,H31B,
H31C), C44(H44A,H44B,H44C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C20(H20A,
H20B,H20C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F),
C20A(H20D,H20E,H20F), C19A(H19D,H19E,H19F)
;
_shelx_res_file
;
TITL en-p66-b(fnon)li_auto_a.res in I2/a
en-p66-b(fnon)li_auto.res
created by SHELXL-2018/3 at 14:42:11 on 28-Jun-2023
REM Old TITL en-p66-b(fnon)li_auto_a.res in I2/a
REM SHELXT solution in I2/a: R1 0.173, Rweak 0.011, Alpha 0.030
REM 0.312 for 569 systematic absences, Orientation as input
REM Formula found by SHELXT: C53 Li N2 O3
CELL 1.54184 19.3413 10.2642 48.762 90 90.51 90
ZERR 8 0.0004 0.0002 0.0008 0 0.002 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H B Li N O
UNIT 416 592 8 8 16 24
DFIX 1.53 0.008 C18 C17 C18A C17 C19A C17 C19 C17 C20 C17 C20A C17
DANG 2.5 0.008 C18A C19A C20A C20 C18 C19
SIMU 0.005 0.01 2 C18 C18A C19A C19 C20 C20A C17
SIMU 0.005 0.01 2 C49 O3 C52 C51 C50
SIMU 0.005 0.01 2 O2 C45 C46 C47 C48
L.S. 4
PLAN 5
SIZE 0.045 0.03 0.1
TEMP -123
CONF
FREE Li1 H44c
BOND
list 4
MORE -1
fmap 2
BOND $H
ACTA
REM
REM
REM
WGHT 0.060300 2.766300
FVAR 0.16771 0.64648
O1 6 0.257320 0.629003 0.375692 11.00000 0.02703 0.04989 =
0.02975 0.00054 0.00210 -0.00696
O2 6 0.140807 0.413286 0.357493 11.00000 0.03065 0.05910 =
0.05083 0.00104 -0.00650 -0.00580
N2 5 0.348353 0.737741 0.400767 11.00000 0.02399 0.03163 =
0.02273 0.00042 0.00249 0.00049
N1 5 0.358470 0.681565 0.349333 11.00000 0.02327 0.02876 =
0.02338 -0.00052 0.00029 -0.00239
O3 6 0.096331 0.643922 0.392360 11.00000 0.03584 0.05923 =
0.05688 -0.00466 0.01033 -0.00865
C21 1 0.325734 0.609271 0.327244 11.00000 0.02603 0.03491 =
0.02172 0.00164 0.00148 -0.00557
C12 1 0.418127 0.761520 0.407505 11.00000 0.02471 0.02709 =
0.02428 -0.00130 -0.00030 0.00252
C11 1 0.466680 0.802038 0.387944 11.00000 0.02522 0.03044 =
0.02388 -0.00164 0.00054 0.00009
C3 1 0.415115 0.801241 0.312502 11.00000 0.02619 0.03044 =
0.02394 -0.00147 -0.00034 0.00155
AFIX 43
H3 2 0.390417 0.748727 0.299710 11.00000 -1.20000
AFIX 0
C2 1 0.407352 0.774647 0.340743 11.00000 0.02267 0.02534 =
0.02556 0.00111 0.00100 0.00276
C13 1 0.440275 0.750776 0.434989 11.00000 0.02898 0.03357 =
0.02288 0.00130 0.00260 0.00008
AFIX 43
H13 2 0.406949 0.728189 0.448371 11.00000 -1.20000
AFIX 0
C33 1 0.300319 0.760167 0.422771 11.00000 0.02343 0.03421 =
0.02340 0.00117 0.00319 0.00174
C1 1 0.450958 0.841484 0.359221 11.00000 0.02282 0.03186 =
0.02446 -0.00051 0.00210 0.00133
C4 1 0.456936 0.900080 0.302434 11.00000 0.02959 0.02902 =
0.02457 0.00016 0.00090 0.00336
C6 1 0.489122 0.946952 0.348839 11.00000 0.03201 0.03244 =
0.02758 -0.00368 0.00087 -0.00613
AFIX 43
H6 2 0.514511 0.999468 0.361417 11.00000 -1.20000
AFIX 0
C5 1 0.491578 0.977984 0.321403 11.00000 0.03489 0.02867 =
0.03002 0.00086 0.00280 -0.00533
AFIX 43
H5 2 0.516767 1.052115 0.315471 11.00000 -1.20000
AFIX 0
C38 1 0.281661 0.889374 0.428345 11.00000 0.02868 0.03373 =
0.03487 0.00021 0.00441 0.00153
C34 1 0.274435 0.657815 0.438859 11.00000 0.02796 0.03545 =
0.02808 0.00408 -0.00033 -0.00004
C14 1 0.507889 0.771221 0.443687 11.00000 0.03232 0.03531 =
0.02368 -0.00069 -0.00164 0.00127
C26 1 0.352365 0.486287 0.320570 11.00000 0.02998 0.03457 =
0.02550 -0.00180 0.00275 -0.00645
C16 1 0.535562 0.813727 0.396711 11.00000 0.02697 0.04559 =
0.02674 0.00054 0.00218 -0.00321
AFIX 43
H16 2 0.569621 0.833227 0.383406 11.00000 -1.20000
AFIX 0
C7 1 0.463231 0.927033 0.271530 11.00000 0.03778 0.03295 =
0.02426 0.00201 0.00269 -0.00158
C27 1 0.407131 0.422724 0.338471 11.00000 0.03212 0.03456 =
0.03675 -0.00435 0.00102 -0.00014
AFIX 13
H27 2 0.434746 0.493584 0.347407 11.00000 -1.20000
AFIX 0
C22 1 0.270591 0.663767 0.312060 11.00000 0.02928 0.04390 =
0.02815 0.00630 -0.00235 -0.00437
C15 1 0.556632 0.798434 0.423652 11.00000 0.02611 0.05222 =
0.02785 -0.00060 -0.00203 -0.00024
AFIX 43
H15 2 0.604133 0.806442 0.428486 11.00000 -1.20000
AFIX 0
C42 1 0.295153 0.516420 0.434621 11.00000 0.03777 0.03339 =
0.03354 0.00522 0.00117 -0.00084
AFIX 13
H42 2 0.324795 0.511917 0.417949 11.00000 -1.20000
AFIX 0
C37 1 0.236930 0.914915 0.449967 11.00000 0.04069 0.03967 =
0.04272 -0.00523 0.01027 0.00561
AFIX 43
H37 2 0.224142 1.002282 0.453875 11.00000 -1.20000
AFIX 0
C35 1 0.229527 0.688066 0.460121 11.00000 0.03702 0.04683 =
0.03373 0.00876 0.00954 -0.00090
AFIX 43
H35 2 0.211233 0.619666 0.470994 11.00000 -1.20000
AFIX 0
C39 1 0.308472 1.001381 0.411230 11.00000 0.04141 0.02973 =
0.04991 0.00485 0.00890 0.00375
AFIX 13
H39 2 0.342887 0.965092 0.398088 11.00000 -1.20000
AFIX 0
C30 1 0.238677 0.794430 0.318768 11.00000 0.03263 0.04902 =
0.03837 0.00624 -0.00579 0.00505
AFIX 13
H30 2 0.263068 0.830127 0.335302 11.00000 -1.20000
AFIX 0
C9 1 0.429304 0.820284 0.254124 11.00000 0.04617 0.04465 =
0.02268 -0.00068 0.00058 -0.00563
AFIX 137
H9A 2 0.451033 0.736276 0.258316 11.00000 -1.50000
H9B 2 0.435277 0.840378 0.234641 11.00000 -1.50000
H9C 2 0.379873 0.815835 0.258267 11.00000 -1.50000
AFIX 0
C25 1 0.325144 0.420691 0.297735 11.00000 0.04634 0.04326 =
0.03368 -0.00782 0.00057 -0.00901
AFIX 43
H25 2 0.343097 0.337842 0.292825 11.00000 -1.20000
AFIX 0
C23 1 0.245173 0.593728 0.289563 11.00000 0.03734 0.05857 =
0.03207 0.00676 -0.01004 -0.00710
AFIX 43
H23 2 0.208074 0.628984 0.279042 11.00000 -1.20000
AFIX 0
C17 1 0.528662 0.758939 0.474020 11.00000 0.03844 0.05614 =
0.02417 0.00331 -0.00463 -0.00529
C10 1 0.428133 1.057662 0.265017 11.00000 0.06058 0.03890 =
0.03059 0.00754 0.00027 0.00520
AFIX 137
H10A 2 0.379701 1.054366 0.270713 11.00000 -1.50000
H10B 2 0.430260 1.074296 0.245252 11.00000 -1.50000
H10C 2 0.452027 1.127733 0.274927 11.00000 -1.50000
AFIX 0
C36 1 0.211013 0.814984 0.465752 11.00000 0.04163 0.05424 =
0.03590 -0.00093 0.01512 0.00470
AFIX 43
H36 2 0.180565 0.833484 0.480428 11.00000 -1.20000
AFIX 0
C24 1 0.272396 0.475314 0.282263 11.00000 0.05184 0.05775 =
0.03094 -0.00356 -0.00879 -0.01272
AFIX 43
H24 2 0.254973 0.430887 0.266570 11.00000 -1.20000
AFIX 0
C8 1 0.539834 0.935430 0.263706 11.00000 0.04313 0.05313 =
0.02973 0.00118 0.00858 -0.00685
AFIX 137
H8A 2 0.562320 1.004628 0.274378 11.00000 -1.50000
H8B 2 0.543561 0.954989 0.244103 11.00000 -1.50000
H8C 2 0.562507 0.852033 0.267643 11.00000 -1.50000
AFIX 0
C45 1 0.076086 0.421512 0.343206 11.00000 0.03196 0.05816 =
0.05187 0.01086 -0.00848 -0.00955
AFIX 23
H45A 2 0.058694 0.512225 0.343251 11.00000 -1.20000
H45B 2 0.041294 0.364735 0.351968 11.00000 -1.20000
AFIX 0
B1 3 0.318695 0.680786 0.375348 11.00000 0.02411 0.03007 =
0.02715 0.00172 0.00040 0.00190
C43 1 0.337475 0.465135 0.458969 11.00000 0.05241 0.03674 =
0.05366 0.00837 -0.01179 0.00226
AFIX 137
H43A 2 0.379324 0.518003 0.461251 11.00000 -1.50000
H43B 2 0.350459 0.374286 0.455595 11.00000 -1.50000
H43C 2 0.309760 0.470255 0.475661 11.00000 -1.50000
AFIX 0
C52 1 0.041850 0.580107 0.407022 11.00000 0.04312 0.06093 =
0.05486 0.00183 0.00968 -0.00815
AFIX 23
H52A 2 0.057540 0.494687 0.414160 11.00000 -1.20000
H52B 2 0.000996 0.566416 0.394989 11.00000 -1.20000
AFIX 0
C29 1 0.456989 0.335840 0.322832 11.00000 0.04925 0.04779 =
0.06244 -0.01894 -0.00034 0.00937
AFIX 137
H29A 2 0.431885 0.260709 0.315350 11.00000 -1.50000
H29B 2 0.493613 0.305455 0.335290 11.00000 -1.50000
H29C 2 0.477549 0.385454 0.307793 11.00000 -1.50000
AFIX 0
C28 1 0.372803 0.343437 0.361130 11.00000 0.04394 0.06009 =
0.05500 0.02059 -0.00360 0.00173
AFIX 137
H28A 2 0.340776 0.399224 0.371248 11.00000 -1.50000
H28B 2 0.408335 0.309827 0.373716 11.00000 -1.50000
H28C 2 0.347291 0.270434 0.352954 11.00000 -1.50000
AFIX 0
C49 1 0.101591 0.777658 0.400963 11.00000 0.05168 0.05893 =
0.05630 0.00210 0.00390 -0.00800
AFIX 23
H49A 2 0.100928 0.836384 0.384858 11.00000 -1.20000
H49B 2 0.145146 0.792063 0.411343 11.00000 -1.20000
AFIX 0
C32 1 0.245849 0.893645 0.295492 11.00000 0.04689 0.05876 =
0.07178 0.02573 0.00998 0.01395
AFIX 137
H32A 2 0.294944 0.907912 0.291701 11.00000 -1.50000
H32B 2 0.224486 0.976181 0.300920 11.00000 -1.50000
H32C 2 0.222705 0.860306 0.278966 11.00000 -1.50000
AFIX 0
C31 1 0.161864 0.781421 0.325589 11.00000 0.03929 0.08284 =
0.04921 0.01842 0.00361 0.01162
AFIX 137
H31A 2 0.136287 0.752641 0.309241 11.00000 -1.50000
H31B 2 0.143987 0.865970 0.331600 11.00000 -1.50000
H31C 2 0.156153 0.717324 0.340291 11.00000 -1.50000
AFIX 0
C44 1 0.232769 0.428541 0.429875 11.00000 0.05345 0.04211 =
0.06619 0.00951 -0.01526 -0.00874
AFIX 137
H44A 2 0.207672 0.417953 0.447103 11.00000 -1.50000
H44B 2 0.248345 0.343158 0.423394 11.00000 -1.50000
H44C 2 0.202134 0.467945 0.416075 11.00000 -1.50000
AFIX 0
C41 1 0.250434 1.062712 0.394505 11.00000 0.05571 0.06108 =
0.07662 0.03010 -0.00075 -0.00016
AFIX 137
H41A 2 0.230011 0.997063 0.382295 11.00000 -1.50000
H41B 2 0.268912 1.134569 0.383551 11.00000 -1.50000
H41C 2 0.214918 1.096092 0.406874 11.00000 -1.50000
AFIX 0
C51 1 0.024960 0.670918 0.430095 11.00000 0.07802 0.07083 =
0.06207 0.00055 0.02867 -0.00812
AFIX 23
H51A 2 -0.024345 0.663744 0.435164 11.00000 -1.20000
H51B 2 0.053993 0.652194 0.446447 11.00000 -1.20000
AFIX 0
C48 1 0.185343 0.326171 0.342940 11.00000 0.04385 0.06934 =
0.07677 0.00957 0.00617 0.00865
AFIX 23
H48A 2 0.200832 0.254096 0.355007 11.00000 -1.20000
H48B 2 0.226540 0.372974 0.336148 11.00000 -1.20000
AFIX 0
C40 1 0.345586 1.102357 0.428937 11.00000 0.07234 0.04629 =
0.07932 0.00208 0.00437 -0.01801
AFIX 137
H40A 2 0.312970 1.139898 0.442016 11.00000 -1.50000
H40B 2 0.363937 1.171527 0.417214 11.00000 -1.50000
H40C 2 0.383711 1.060558 0.438962 11.00000 -1.50000
AFIX 0
C46 1 0.089595 0.377586 0.314765 11.00000 0.05137 0.08519 =
0.05240 -0.00010 -0.00452 -0.02516
AFIX 23
H46A 2 0.107998 0.449431 0.303419 11.00000 -1.20000
H46B 2 0.047171 0.342598 0.305965 11.00000 -1.20000
AFIX 0
C50 1 0.040626 0.803240 0.418763 11.00000 0.06947 0.06325 =
0.07410 -0.00739 0.02042 -0.00259
AFIX 23
H50A 2 0.001120 0.837644 0.407936 11.00000 -1.20000
H50B 2 0.052267 0.865612 0.433586 11.00000 -1.20000
AFIX 0
PART 1
C20 1 0.471421 0.805814 0.492811 21.00000 0.05366 0.11343 =
0.02692 -0.02189 -0.00362 0.00636
AFIX 137
H20A 2 0.458802 0.895452 0.487987 21.00000 -1.50000
H20B 2 0.487673 0.802934 0.511894 21.00000 -1.50000
H20C 2 0.430917 0.749248 0.490655 21.00000 -1.50000
AFIX 0
PART 0
C47 1 0.142113 0.273782 0.318999 11.00000 0.06519 0.07035 =
0.08705 -0.02100 0.02057 -0.02250
AFIX 23
H47A 2 0.170668 0.261808 0.302439 11.00000 -1.20000
H47B 2 0.120060 0.189821 0.323753 11.00000 -1.20000
AFIX 0
PART 1
C19 1 0.544427 0.613552 0.479168 21.00000 0.05744 0.06714 =
0.04694 0.01977 -0.02424 -0.01395
AFIX 137
H19A 2 0.503236 0.561519 0.474895 21.00000 -1.50000
H19B 2 0.557465 0.600866 0.498451 21.00000 -1.50000
H19C 2 0.582590 0.585945 0.467428 21.00000 -1.50000
AFIX 0
C18 1 0.595749 0.834733 0.480564 21.00000 0.04902 0.06631 =
0.03044 -0.00230 -0.00945 -0.01110
AFIX 137
H18A 2 0.634043 0.797364 0.470147 21.00000 -1.50000
H18B 2 0.606086 0.828538 0.500232 21.00000 -1.50000
H18C 2 0.589707 0.926411 0.475467 21.00000 -1.50000
AFIX 0
PART 0
LI1 4 0.175825 0.561908 0.376402 11.00000 0.03151 0.06838 =
0.05322 -0.00200 0.00270 -0.01000
PART 2
C18A 1 0.571366 0.878367 0.481710 -21.00000 0.06472 0.08434 =
0.02979 -0.00693 -0.00282 -0.02766
AFIX 137
H18D 2 0.611426 0.884489 0.469612 -21.00000 -1.50000
H18E 2 0.587261 0.870646 0.500780 -21.00000 -1.50000
H18F 2 0.542889 0.956808 0.479684 -21.00000 -1.50000
AFIX 0
C20A 1 0.464440 0.759482 0.492308 -21.00000 0.05599 0.05645 =
0.01548 -0.00412 -0.00461 -0.00448
AFIX 137
H20D 2 0.436915 0.837665 0.488484 -21.00000 -1.50000
H20E 2 0.478865 0.759376 0.511625 -21.00000 -1.50000
H20F 2 0.436552 0.681753 0.488487 -21.00000 -1.50000
AFIX 0
C19A 1 0.567001 0.633750 0.479747 -21.00000 0.04927 0.07707 =
0.04162 0.01077 -0.01240 0.01284
AFIX 137
H19D 2 0.537991 0.559552 0.474393 -21.00000 -1.50000
H19E 2 0.578029 0.628118 0.499366 -21.00000 -1.50000
H19F 2 0.609893 0.632247 0.469203 -21.00000 -1.50000
AFIX 0
HKLF 4
REM en-p66-b(fnon)li_auto_a.res in I2/a
REM wR2 = 0.1412, GooF = S = 1.026, Restrained GooF = 1.052 for all data
REM R1 = 0.0523 for 6970 Fo > 4sig(Fo) and 0.0822 for all 10240 data
REM 577 parameters refined using 122 restraints
END
WGHT 0.0603 2.7662
REM Highest difference peak 0.339, deepest hole -0.255, 1-sigma level 0.044
Q1 1 0.1660 0.2330 0.3333 11.00000 0.05 0.34
Q2 1 0.5194 0.7805 0.4585 11.00000 0.05 0.20
Q3 1 0.1886 0.4644 0.4291 11.00000 0.05 0.18
Q4 1 0.4739 0.8862 0.4902 11.00000 0.05 0.17
Q5 1 0.4991 0.6192 0.4839 11.00000 0.05 0.16
;
_shelx_res_checksum 34390
_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 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.725
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
O1 O 0.25732(6) 0.62900(13) 0.37569(2) 0.0355(3) Uani 1 1 d . . . . .
O2 O 0.14081(7) 0.41329(15) 0.35749(3) 0.0469(3) Uani 1 1 d . U . . .
N2 N 0.34835(7) 0.73774(13) 0.40077(3) 0.0261(3) Uani 1 1 d . . . . .
N1 N 0.35847(7) 0.68157(13) 0.34933(3) 0.0251(3) Uani 1 1 d . . . . .
O3 O 0.09633(7) 0.64392(16) 0.39236(3) 0.0506(4) Uani 1 1 d . U . . .
C21 C 0.32573(8) 0.60927(17) 0.32724(3) 0.0275(3) Uani 1 1 d . . . . .
C12 C 0.41813(8) 0.76152(16) 0.40751(3) 0.0254(3) Uani 1 1 d . . . . .
C11 C 0.46668(8) 0.80204(16) 0.38794(3) 0.0265(3) Uani 1 1 d . . . . .
C3 C 0.41512(8) 0.80124(16) 0.31250(3) 0.0269(3) Uani 1 1 d . . . . .
H3 H 0.390417 0.748727 0.299710 0.032 Uiso 1 1 calc R U . . .
C2 C 0.40735(8) 0.77465(15) 0.34074(3) 0.0245(3) Uani 1 1 d . . . . .
C13 C 0.44028(9) 0.75078(17) 0.43499(3) 0.0285(3) Uani 1 1 d . . . . .
H13 H 0.406949 0.728189 0.448371 0.034 Uiso 1 1 calc R U . . .
C33 C 0.30032(8) 0.76017(17) 0.42277(3) 0.0270(3) Uani 1 1 d . . . . .
C1 C 0.45096(8) 0.84148(16) 0.35922(3) 0.0264(3) Uani 1 1 d . . . . .
C4 C 0.45694(9) 0.90008(16) 0.30243(3) 0.0277(3) Uani 1 1 d . . . . .
C6 C 0.48912(9) 0.94695(17) 0.34884(3) 0.0307(4) Uani 1 1 d . . . . .
H6 H 0.514511 0.999468 0.361417 0.037 Uiso 1 1 calc R U . . .
C5 C 0.49158(9) 0.97798(17) 0.32140(3) 0.0312(4) Uani 1 1 d . . . . .
H5 H 0.516767 1.052115 0.315471 0.037 Uiso 1 1 calc R U . . .
C38 C 0.28166(9) 0.88937(18) 0.42834(4) 0.0324(4) Uani 1 1 d . . . . .
C34 C 0.27444(9) 0.65781(17) 0.43886(3) 0.0305(4) Uani 1 1 d . . . . .
C14 C 0.50789(9) 0.77122(17) 0.44369(3) 0.0304(4) Uani 1 1 d . . . . .
C26 C 0.35237(9) 0.48629(17) 0.32057(3) 0.0300(3) Uani 1 1 d . . . . .
C16 C 0.53556(9) 0.81373(19) 0.39671(3) 0.0331(4) Uani 1 1 d . . . . .
H16 H 0.569621 0.833227 0.383406 0.040 Uiso 1 1 calc R U . . .
C7 C 0.46323(9) 0.92703(17) 0.27153(3) 0.0317(4) Uani 1 1 d . . . . .
C27 C 0.40713(9) 0.42272(18) 0.33847(4) 0.0345(4) Uani 1 1 d . . . . .
H27 H 0.434746 0.493584 0.347407 0.041 Uiso 1 1 calc R U . . .
C22 C 0.27059(9) 0.66377(19) 0.31206(3) 0.0338(4) Uani 1 1 d . . . . .
C15 C 0.55663(9) 0.7984(2) 0.42365(3) 0.0354(4) Uani 1 1 d . . . . .
H15 H 0.604133 0.806442 0.428486 0.042 Uiso 1 1 calc R U . . .
C42 C 0.29515(10) 0.51642(18) 0.43462(4) 0.0349(4) Uani 1 1 d . . . . .
H42 H 0.324795 0.511917 0.417949 0.042 Uiso 1 1 calc R U . . .
C37 C 0.23693(10) 0.9149(2) 0.44997(4) 0.0410(4) Uani 1 1 d . . . . .
H37 H 0.224142 1.002282 0.453875 0.049 Uiso 1 1 calc R U . . .
C35 C 0.22953(10) 0.6881(2) 0.46012(4) 0.0391(4) Uani 1 1 d . . . . .
H35 H 0.211233 0.619666 0.470994 0.047 Uiso 1 1 calc R U . . .
C39 C 0.30847(11) 1.00138(18) 0.41123(4) 0.0403(4) Uani 1 1 d . . . . .
H39 H 0.342887 0.965092 0.398088 0.048 Uiso 1 1 calc R U . . .
C30 C 0.23868(10) 0.7944(2) 0.31877(4) 0.0400(4) Uani 1 1 d . . . . .
H30 H 0.263068 0.830127 0.335302 0.048 Uiso 1 1 calc R U . . .
C9 C 0.42930(11) 0.8203(2) 0.25412(3) 0.0378(4) Uani 1 1 d . . . . .
H9A H 0.451033 0.736276 0.258316 0.057 Uiso 1 1 calc R U . . .
H9B H 0.435277 0.840378 0.234641 0.057 Uiso 1 1 calc R U . . .
H9C H 0.379873 0.815835 0.258267 0.057 Uiso 1 1 calc R U . . .
C25 C 0.32514(11) 0.4207(2) 0.29773(4) 0.0411(4) Uani 1 1 d . . . . .
H25 H 0.343097 0.337842 0.292825 0.049 Uiso 1 1 calc R U . . .
C23 C 0.24517(10) 0.5937(2) 0.28956(4) 0.0427(5) Uani 1 1 d . . . . .
H23 H 0.208074 0.628984 0.279042 0.051 Uiso 1 1 calc R U . . .
C17 C 0.52866(10) 0.7589(2) 0.47402(3) 0.0396(4) Uani 1 1 d D U . . .
C10 C 0.42813(12) 1.0577(2) 0.26502(4) 0.0434(5) Uani 1 1 d . . . . .
H10A H 0.379701 1.054366 0.270713 0.065 Uiso 1 1 calc R U . . .
H10B H 0.430260 1.074296 0.245252 0.065 Uiso 1 1 calc R U . . .
H10C H 0.452027 1.127733 0.274927 0.065 Uiso 1 1 calc R U . . .
C36 C 0.21101(11) 0.8150(2) 0.46575(4) 0.0438(5) Uani 1 1 d . . . . .
H36 H 0.180565 0.833484 0.480428 0.053 Uiso 1 1 calc R U . . .
C24 C 0.27240(12) 0.4753(2) 0.28226(4) 0.0469(5) Uani 1 1 d . . . . .
H24 H 0.254973 0.430887 0.266570 0.056 Uiso 1 1 calc R U . . .
C8 C 0.53983(10) 0.9354(2) 0.26371(4) 0.0419(4) Uani 1 1 d . . . . .
H8A H 0.562320 1.004628 0.274378 0.063 Uiso 1 1 calc R U . . .
H8B H 0.543561 0.954989 0.244103 0.063 Uiso 1 1 calc R U . . .
H8C H 0.562507 0.852033 0.267643 0.063 Uiso 1 1 calc R U . . .
C45 C 0.07609(10) 0.4215(2) 0.34321(4) 0.0474(5) Uani 1 1 d . U . . .
H45A H 0.058694 0.512225 0.343251 0.057 Uiso 1 1 calc R U . . .
H45B H 0.041294 0.364735 0.351968 0.057 Uiso 1 1 calc R U . . .
B1 B 0.31869(10) 0.68079(19) 0.37535(4) 0.0271(4) Uani 1 1 d . . . . .
C43 C 0.33748(12) 0.4651(2) 0.45897(4) 0.0477(5) Uani 1 1 d . . . . .
H43A H 0.379324 0.518003 0.461251 0.072 Uiso 1 1 calc R U . . .
H43B H 0.350459 0.374286 0.455595 0.072 Uiso 1 1 calc R U . . .
H43C H 0.309760 0.470255 0.475661 0.072 Uiso 1 1 calc R U . . .
C52 C 0.04185(12) 0.5801(2) 0.40702(5) 0.0529(5) Uani 1 1 d . U . . .
H52A H 0.057540 0.494687 0.414160 0.063 Uiso 1 1 calc R U . . .
H52B H 0.000996 0.566416 0.394989 0.063 Uiso 1 1 calc R U . . .
C29 C 0.45699(12) 0.3358(2) 0.32283(5) 0.0532(5) Uani 1 1 d . . . . .
H29A H 0.431885 0.260709 0.315350 0.080 Uiso 1 1 calc R U . . .
H29B H 0.493613 0.305455 0.335290 0.080 Uiso 1 1 calc R U . . .
H29C H 0.477549 0.385454 0.307793 0.080 Uiso 1 1 calc R U . . .
C28 C 0.37280(12) 0.3434(2) 0.36113(5) 0.0530(5) Uani 1 1 d . . . . .
H28A H 0.340776 0.399224 0.371248 0.080 Uiso 1 1 calc R U . . .
H28B H 0.408335 0.309827 0.373716 0.080 Uiso 1 1 calc R U . . .
H28C H 0.347291 0.270434 0.352954 0.080 Uiso 1 1 calc R U . . .
C49 C 0.10159(13) 0.7777(2) 0.40096(5) 0.0556(5) Uani 1 1 d . U . . .
H49A H 0.100928 0.836384 0.384858 0.067 Uiso 1 1 calc R U . . .
H49B H 0.145146 0.792063 0.411343 0.067 Uiso 1 1 calc R U . . .
C32 C 0.24585(13) 0.8936(3) 0.29549(5) 0.0591(6) Uani 1 1 d . . . . .
H32A H 0.294944 0.907912 0.291701 0.089 Uiso 1 1 calc R U . . .
H32B H 0.224486 0.976181 0.300920 0.089 Uiso 1 1 calc R U . . .
H32C H 0.222705 0.860306 0.278966 0.089 Uiso 1 1 calc R U . . .
C31 C 0.16186(11) 0.7814(3) 0.32559(5) 0.0571(6) Uani 1 1 d . . . . .
H31A H 0.136287 0.752641 0.309241 0.086 Uiso 1 1 calc R U . . .
H31B H 0.143987 0.865970 0.331600 0.086 Uiso 1 1 calc R U . . .
H31C H 0.156153 0.717324 0.340291 0.086 Uiso 1 1 calc R U . . .
C44 C 0.23277(12) 0.4285(2) 0.42988(5) 0.0540(5) Uani 1 1 d . . . . .
H44A H 0.207672 0.417953 0.447103 0.081 Uiso 1 1 calc R U . . .
H44B H 0.248345 0.343158 0.423394 0.081 Uiso 1 1 calc R U . . .
H44C H 0.202134 0.467945 0.416075 0.081 Uiso 1 1 calc R U . . .
C41 C 0.25043(13) 1.0627(3) 0.39451(6) 0.0645(7) Uani 1 1 d . . . . .
H41A H 0.230011 0.997063 0.382295 0.097 Uiso 1 1 calc R U . . .
H41B H 0.268912 1.134569 0.383551 0.097 Uiso 1 1 calc R U . . .
H41C H 0.214918 1.096092 0.406874 0.097 Uiso 1 1 calc R U . . .
C51 C 0.02496(16) 0.6709(3) 0.43009(6) 0.0701(7) Uani 1 1 d . U . . .
H51A H -0.024345 0.663744 0.435164 0.084 Uiso 1 1 calc R U . . .
H51B H 0.053993 0.652194 0.446447 0.084 Uiso 1 1 calc R U . . .
C48 C 0.18534(13) 0.3262(3) 0.34294(6) 0.0633(6) Uani 1 1 d . U . . .
H48A H 0.200832 0.254096 0.355007 0.076 Uiso 1 1 calc R U . . .
H48B H 0.226540 0.372974 0.336148 0.076 Uiso 1 1 calc R U . . .
C40 C 0.34559(15) 1.1024(2) 0.42894(6) 0.0660(7) Uani 1 1 d . . . . .
H40A H 0.312970 1.139898 0.442016 0.099 Uiso 1 1 calc R U . . .
H40B H 0.363937 1.171527 0.417214 0.099 Uiso 1 1 calc R U . . .
H40C H 0.383711 1.060558 0.438962 0.099 Uiso 1 1 calc R U . . .
C46 C 0.08960(13) 0.3776(3) 0.31477(5) 0.0630(6) Uani 1 1 d . U . . .
H46A H 0.107998 0.449431 0.303419 0.076 Uiso 1 1 calc R U . . .
H46B H 0.047171 0.342598 0.305965 0.076 Uiso 1 1 calc R U . . .
C50 C 0.04063(16) 0.8032(3) 0.41876(6) 0.0688(7) Uani 1 1 d . U . . .
H50A H 0.001120 0.837644 0.407936 0.083 Uiso 1 1 calc R U . . .
H50B H 0.052267 0.865612 0.433586 0.083 Uiso 1 1 calc R U . . .
C20 C 0.4714(4) 0.8058(11) 0.49281(16) 0.0647(19) Uani 0.646(15) 1 d D U P A 1
H20A H 0.458802 0.895452 0.487987 0.097 Uiso 0.646(15) 1 calc R U P A 1
H20B H 0.487673 0.802934 0.511894 0.097 Uiso 0.646(15) 1 calc R U P A 1
H20C H 0.430917 0.749248 0.490655 0.097 Uiso 0.646(15) 1 calc R U P A 1
C47 C 0.14211(15) 0.2738(3) 0.31900(6) 0.0741(7) Uani 1 1 d . U . . .
H47A H 0.170668 0.261808 0.302439 0.089 Uiso 1 1 calc R U . . .
H47B H 0.120060 0.189821 0.323753 0.089 Uiso 1 1 calc R U . . .
C19 C 0.5444(4) 0.6136(4) 0.47917(18) 0.0573(15) Uani 0.646(15) 1 d D U P A 1
H19A H 0.503236 0.561519 0.474895 0.086 Uiso 0.646(15) 1 calc R U P A 1
H19B H 0.557465 0.600866 0.498451 0.086 Uiso 0.646(15) 1 calc R U P A 1
H19C H 0.582590 0.585945 0.467428 0.086 Uiso 0.646(15) 1 calc R U P A 1
C18 C 0.5957(3) 0.8347(7) 0.48056(11) 0.0486(13) Uani 0.646(15) 1 d D U P A 1
H18A H 0.634043 0.797364 0.470147 0.073 Uiso 0.646(15) 1 calc R U P A 1
H18B H 0.606086 0.828538 0.500232 0.073 Uiso 0.646(15) 1 calc R U P A 1
H18C H 0.589707 0.926411 0.475467 0.073 Uiso 0.646(15) 1 calc R U P A 1
Li1 Li 0.17583(18) 0.5619(4) 0.37640(8) 0.0510(9) Uani 1 1 d . . . . .
C18A C 0.5714(8) 0.8784(11) 0.4817(2) 0.060(2) Uani 0.354(15) 1 d D U P A 2
H18D H 0.611426 0.884489 0.469612 0.089 Uiso 0.354(15) 1 calc R U P A 2
H18E H 0.587261 0.870646 0.500780 0.089 Uiso 0.354(15) 1 calc R U P A 2
H18F H 0.542889 0.956808 0.479684 0.089 Uiso 0.354(15) 1 calc R U P A 2
C20A C 0.4644(6) 0.7595(12) 0.4923(3) 0.043(2) Uani 0.354(15) 1 d D U P A 2
H20D H 0.436915 0.837665 0.488484 0.064 Uiso 0.354(15) 1 calc R U P A 2
H20E H 0.478865 0.759376 0.511625 0.064 Uiso 0.354(15) 1 calc R U P A 2
H20F H 0.436552 0.681753 0.488487 0.064 Uiso 0.354(15) 1 calc R U P A 2
C19A C 0.5670(7) 0.6338(10) 0.4797(3) 0.056(2) Uani 0.354(15) 1 d D U P A 2
H19D H 0.537991 0.559552 0.474393 0.084 Uiso 0.354(15) 1 calc R U P A 2
H19E H 0.578029 0.628118 0.499366 0.084 Uiso 0.354(15) 1 calc R U P A 2
H19F H 0.609893 0.632247 0.469203 0.084 Uiso 0.354(15) 1 calc R U P A 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 0.0270(6) 0.0499(8) 0.0298(6) 0.0005(5) 0.0021(5) -0.0070(5)
O2 0.0307(7) 0.0591(9) 0.0508(8) 0.0010(7) -0.0065(6) -0.0058(6)
N2 0.0240(7) 0.0316(7) 0.0227(6) 0.0004(5) 0.0025(5) 0.0005(5)
N1 0.0233(6) 0.0288(7) 0.0234(6) -0.0005(5) 0.0003(5) -0.0024(5)
O3 0.0358(7) 0.0592(9) 0.0569(8) -0.0047(7) 0.0103(6) -0.0087(6)
C21 0.0260(8) 0.0349(9) 0.0217(7) 0.0016(6) 0.0015(6) -0.0056(6)
C12 0.0247(8) 0.0271(8) 0.0243(7) -0.0013(6) -0.0003(6) 0.0025(6)
C11 0.0252(8) 0.0304(8) 0.0239(7) -0.0016(6) 0.0005(6) 0.0001(6)
C3 0.0262(8) 0.0304(8) 0.0239(7) -0.0015(6) -0.0003(6) 0.0016(6)
C2 0.0227(7) 0.0253(7) 0.0256(7) 0.0011(6) 0.0010(6) 0.0028(6)
C13 0.0290(8) 0.0336(9) 0.0229(7) 0.0013(6) 0.0026(6) 0.0001(7)
C33 0.0234(8) 0.0342(9) 0.0234(7) 0.0012(6) 0.0032(6) 0.0017(6)
C1 0.0228(7) 0.0319(8) 0.0245(7) -0.0005(6) 0.0021(6) 0.0013(6)
C4 0.0296(8) 0.0290(8) 0.0246(7) 0.0002(6) 0.0009(6) 0.0034(6)
C6 0.0320(9) 0.0324(9) 0.0276(8) -0.0037(7) 0.0009(6) -0.0061(7)
C5 0.0349(9) 0.0287(8) 0.0300(8) 0.0009(6) 0.0028(7) -0.0053(7)
C38 0.0287(9) 0.0337(9) 0.0349(8) 0.0002(7) 0.0044(7) 0.0015(7)
C34 0.0280(8) 0.0354(9) 0.0281(8) 0.0041(7) -0.0003(6) 0.0000(7)
C14 0.0323(9) 0.0353(9) 0.0237(7) -0.0007(6) -0.0016(6) 0.0013(7)
C26 0.0300(8) 0.0346(9) 0.0255(7) -0.0018(6) 0.0027(6) -0.0064(7)
C16 0.0270(8) 0.0456(10) 0.0267(8) 0.0005(7) 0.0022(6) -0.0032(7)
C7 0.0378(9) 0.0330(9) 0.0243(8) 0.0020(6) 0.0027(6) -0.0016(7)
C27 0.0321(9) 0.0346(9) 0.0367(9) -0.0044(7) 0.0010(7) -0.0001(7)
C22 0.0293(9) 0.0439(10) 0.0281(8) 0.0063(7) -0.0023(6) -0.0044(7)
C15 0.0261(8) 0.0522(11) 0.0279(8) -0.0006(8) -0.0020(6) -0.0002(7)
C42 0.0378(10) 0.0334(9) 0.0335(9) 0.0052(7) 0.0012(7) -0.0008(7)
C37 0.0407(10) 0.0397(10) 0.0427(10) -0.0052(8) 0.0103(8) 0.0056(8)
C35 0.0370(10) 0.0468(11) 0.0337(9) 0.0088(8) 0.0095(7) -0.0009(8)
C39 0.0414(11) 0.0297(9) 0.0499(10) 0.0049(8) 0.0089(8) 0.0037(8)
C30 0.0326(9) 0.0490(11) 0.0384(9) 0.0062(8) -0.0058(7) 0.0050(8)
C9 0.0462(11) 0.0446(11) 0.0227(8) -0.0007(7) 0.0006(7) -0.0056(8)
C25 0.0463(11) 0.0433(11) 0.0337(9) -0.0078(8) 0.0006(8) -0.0090(9)
C23 0.0373(10) 0.0586(13) 0.0321(9) 0.0068(9) -0.0100(7) -0.0071(9)
C17 0.0384(10) 0.0561(12) 0.0242(8) 0.0033(8) -0.0046(7) -0.0053(8)
C10 0.0606(13) 0.0389(10) 0.0306(9) 0.0075(8) 0.0003(8) 0.0052(9)
C36 0.0416(11) 0.0542(12) 0.0359(9) -0.0009(9) 0.0151(8) 0.0047(9)
C24 0.0518(12) 0.0577(13) 0.0309(9) -0.0036(9) -0.0088(8) -0.0127(10)
C8 0.0431(11) 0.0531(12) 0.0297(8) 0.0012(8) 0.0086(7) -0.0068(9)
C45 0.0320(10) 0.0582(12) 0.0519(11) 0.0109(9) -0.0085(8) -0.0096(9)
B1 0.0241(9) 0.0301(9) 0.0271(8) 0.0017(7) 0.0004(7) 0.0019(7)
C43 0.0524(13) 0.0367(11) 0.0537(12) 0.0084(9) -0.0118(9) 0.0023(9)
C52 0.0431(11) 0.0609(13) 0.0549(11) 0.0018(10) 0.0097(9) -0.0081(10)
C29 0.0492(12) 0.0478(12) 0.0624(13) -0.0189(10) -0.0003(10) 0.0094(10)
C28 0.0439(12) 0.0601(14) 0.0550(12) 0.0206(11) -0.0036(9) 0.0017(10)
C49 0.0517(12) 0.0589(13) 0.0563(12) 0.0021(10) 0.0039(10) -0.0080(10)
C32 0.0469(13) 0.0588(14) 0.0718(15) 0.0257(12) 0.0100(11) 0.0140(11)
C31 0.0393(11) 0.0828(17) 0.0492(12) 0.0184(11) 0.0036(9) 0.0116(11)
C44 0.0534(13) 0.0421(12) 0.0662(14) 0.0095(10) -0.0153(10) -0.0087(10)
C41 0.0557(15) 0.0611(15) 0.0766(16) 0.0301(13) -0.0008(12) -0.0002(12)
C51 0.0780(17) 0.0708(16) 0.0621(14) 0.0005(12) 0.0287(12) -0.0081(13)
C48 0.0438(12) 0.0693(15) 0.0768(15) 0.0096(12) 0.0062(11) 0.0086(11)
C40 0.0723(17) 0.0463(13) 0.0793(17) 0.0021(12) 0.0044(13) -0.0180(12)
C46 0.0514(13) 0.0852(17) 0.0524(12) -0.0001(12) -0.0045(10) -0.0252(12)
C50 0.0695(16) 0.0633(15) 0.0741(15) -0.0074(12) 0.0204(13) -0.0026(13)
C20 0.054(3) 0.113(5) 0.0269(19) -0.022(3) -0.0036(17) 0.006(3)
C47 0.0652(15) 0.0703(16) 0.0871(17) -0.0210(14) 0.0206(13) -0.0225(13)
C19 0.057(3) 0.067(2) 0.047(2) 0.0198(19) -0.024(3) -0.014(2)
C18 0.049(3) 0.066(3) 0.0304(17) -0.0023(18) -0.0094(18) -0.011(2)
Li1 0.0315(17) 0.068(2) 0.0532(19) -0.0020(18) 0.0027(14) -0.0100(16)
C18A 0.065(5) 0.084(5) 0.030(3) -0.007(4) -0.003(4) -0.028(4)
C20A 0.056(4) 0.056(5) 0.015(3) -0.004(3) -0.005(3) -0.004(3)
C19A 0.049(5) 0.077(5) 0.042(3) 0.011(4) -0.012(4) 0.013(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 179.3(2) . . ?
C45 O2 C48 108.84(17) . . ?
C45 O2 Li1 119.66(18) . . ?
C48 O2 Li1 121.78(18) . . ?
C12 N2 C33 114.89(12) . . ?
C12 N2 B1 128.84(13) . . ?
C33 N2 B1 115.96(13) . . ?
C21 N1 B1 113.88(13) . . ?
C2 N1 C21 114.57(12) . . ?
C2 N1 B1 127.54(14) . . ?
C52 O3 C49 109.89(16) . . ?
C52 O3 Li1 126.46(19) . . ?
C49 O3 Li1 118.74(17) . . ?
C26 C21 N1 118.32(15) . . ?
C26 C21 C22 120.88(15) . . ?
C22 C21 N1 120.74(15) . . ?
N2 C12 C11 122.50(14) . . ?
C13 C12 N2 119.45(14) . . ?
C13 C12 C11 117.98(15) . . ?
C12 C11 C1 125.93(14) . . ?
C16 C11 C12 117.20(14) . . ?
C16 C11 C1 116.76(14) . . ?
C2 C3 H3 118.2 . . ?
C4 C3 H3 118.2 . . ?
C4 C3 C2 123.53(15) . . ?
N1 C2 C3 119.84(14) . . ?
C1 C2 N1 122.66(14) . . ?
C1 C2 C3 117.48(14) . . ?
C12 C13 H13 118.1 . . ?
C14 C13 C12 123.87(15) . . ?
C14 C13 H13 118.1 . . ?
C38 C33 N2 117.60(14) . . ?
C38 C33 C34 120.35(15) . . ?
C34 C33 N2 122.01(15) . . ?
C2 C1 C11 125.93(15) . . ?
C6 C1 C11 116.42(14) . . ?
C6 C1 C2 117.26(14) . . ?
C3 C4 C5 117.60(14) . . ?
C3 C4 C7 121.93(15) . . ?
C5 C4 C7 120.43(15) . . ?
C1 C6 H6 118.3 . . ?
C5 C6 C1 123.40(15) . . ?
C5 C6 H6 118.3 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.54(15) . . ?
C6 C5 H5 120.2 . . ?
C33 C38 C39 121.42(15) . . ?
C37 C38 C33 119.14(16) . . ?
C37 C38 C39 119.44(17) . . ?
C33 C34 C42 122.81(15) . . ?
C35 C34 C33 118.43(17) . . ?
C35 C34 C42 118.73(16) . . ?
C13 C14 C15 117.28(15) . . ?
C13 C14 C17 121.35(15) . . ?
C15 C14 C17 121.32(15) . . ?
C21 C26 C27 120.69(15) . . ?
C25 C26 C21 118.75(17) . . ?
C25 C26 C27 120.49(17) . . ?
C11 C16 H16 118.2 . . ?
C15 C16 C11 123.53(15) . . ?
C15 C16 H16 118.2 . . ?
C9 C7 C4 112.17(14) . . ?
C9 C7 C10 108.91(15) . . ?
C9 C7 C8 108.20(15) . . ?
C10 C7 C4 108.73(14) . . ?
C10 C7 C8 109.00(16) . . ?
C8 C7 C4 109.79(14) . . ?
C26 C27 H27 107.8 . . ?
C26 C27 C29 113.98(16) . . ?
C26 C27 C28 109.87(15) . . ?
C29 C27 H27 107.8 . . ?
C29 C27 C28 109.34(18) . . ?
C28 C27 H27 107.8 . . ?
C21 C22 C30 123.14(16) . . ?
C23 C22 C21 117.89(18) . . ?
C23 C22 C30 118.97(17) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 C14 119.64(16) . . ?
C16 C15 H15 120.2 . . ?
C34 C42 H42 108.0 . . ?
C34 C42 C43 111.28(16) . . ?
C34 C42 C44 112.13(16) . . ?
C43 C42 H42 108.0 . . ?
C44 C42 H42 108.0 . . ?
C44 C42 C43 109.39(16) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 C38 120.87(18) . . ?
C36 C37 H37 119.6 . . ?
C34 C35 H35 119.2 . . ?
C36 C35 C34 121.55(17) . . ?
C36 C35 H35 119.2 . . ?
C38 C39 H39 107.7 . . ?
C38 C39 C41 110.82(17) . . ?
C38 C39 C40 111.45(18) . . ?
C41 C39 H39 107.7 . . ?
C41 C39 C40 111.4(2) . . ?
C40 C39 H39 107.7 . . ?
C22 C30 H30 108.0 . . ?
C22 C30 C32 112.90(17) . . ?
C22 C30 C31 111.60(19) . . ?
C32 C30 H30 108.0 . . ?
C31 C30 H30 108.0 . . ?
C31 C30 C32 108.26(17) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C26 C25 H25 119.7 . . ?
C24 C25 C26 120.63(19) . . ?
C24 C25 H25 119.7 . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.74(18) . . ?
C24 C23 H23 119.1 . . ?
C14 C17 C19 106.6(3) . . ?
C14 C17 C18 111.7(2) . . ?
C14 C17 C20A 110.7(6) . . ?
C20 C17 C14 111.6(4) . . ?
C20 C17 C19 110.6(5) . . ?
C20 C17 C18 109.3(4) . . ?
C19 C17 C18 106.8(3) . . ?
C18A C17 C14 107.9(4) . . ?
C18A C17 C20A 107.1(6) . . ?
C19A C17 C14 111.9(6) . . ?
C19A C17 C18A 112.0(5) . . ?
C19A C17 C20A 107.1(7) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C37 C36 H36 120.2 . . ?
C35 C36 C37 119.67(17) . . ?
C35 C36 H36 120.2 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 C25 120.03(18) . . ?
C23 C24 H24 120.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C45 H45A 110.5 . . ?
O2 C45 H45B 110.5 . . ?
O2 C45 C46 106.07(18) . . ?
H45A C45 H45B 108.7 . . ?
C46 C45 H45A 110.5 . . ?
C46 C45 H45B 110.5 . . ?
O1 B1 N2 119.80(15) . . ?
O1 B1 N1 119.44(15) . . ?
N2 B1 N1 120.76(14) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O3 C52 H52A 110.8 . . ?
O3 C52 H52B 110.8 . . ?
O3 C52 C51 104.81(19) . . ?
H52A C52 H52B 108.9 . . ?
C51 C52 H52A 110.8 . . ?
C51 C52 H52B 110.8 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 C49 H49A 110.4 . . ?
O3 C49 H49B 110.4 . . ?
O3 C49 C50 106.44(19) . . ?
H49A C49 H49B 108.6 . . ?
C50 C49 H49A 110.4 . . ?
C50 C49 H49B 110.4 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C52 C51 H51A 111.0 . . ?
C52 C51 H51B 111.0 . . ?
H51A C51 H51B 109.0 . . ?
C50 C51 C52 103.9(2) . . ?
C50 C51 H51A 111.0 . . ?
C50 C51 H51B 111.0 . . ?
O2 C48 H48A 110.6 . . ?
O2 C48 H48B 110.6 . . ?
O2 C48 C47 105.7(2) . . ?
H48A C48 H48B 108.7 . . ?
C47 C48 H48A 110.6 . . ?
C47 C48 H48B 110.6 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C45 C46 H46A 111.3 . . ?
C45 C46 H46B 111.3 . . ?
C45 C46 C47 102.4(2) . . ?
H46A C46 H46B 109.2 . . ?
C47 C46 H46A 111.3 . . ?
C47 C46 H46B 111.3 . . ?
C49 C50 C51 102.6(2) . . ?
C49 C50 H50A 111.2 . . ?
C49 C50 H50B 111.2 . . ?
C51 C50 H50A 111.2 . . ?
C51 C50 H50B 111.2 . . ?
H50A C50 H50B 109.2 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C48 C47 H47A 111.2 . . ?
C48 C47 H47B 111.2 . . ?
C46 C47 C48 102.9(2) . . ?
C46 C47 H47A 111.2 . . ?
C46 C47 H47B 111.2 . . ?
H47A C47 H47B 109.1 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 Li1 O2 129.3(2) . . ?
O1 Li1 O3 124.7(2) . . ?
O2 Li1 O3 105.33(17) . . ?
C17 C18A H18D 109.5 . . ?
C17 C18A H18E 109.5 . . ?
C17 C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C17 C20A H20D 109.5 . . ?
C17 C20A H20E 109.5 . . ?
C17 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C17 C19A H19D 109.5 . . ?
C17 C19A H19E 109.5 . . ?
C17 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
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 1.301(2) . ?
O1 Li1 1.721(4) . ?
O2 C45 1.430(2) . ?
O2 C48 1.434(3) . ?
O2 Li1 1.904(4) . ?
N2 C12 1.407(2) . ?
N2 C33 1.444(2) . ?
N2 B1 1.481(2) . ?
N1 C21 1.449(2) . ?
N1 C2 1.410(2) . ?
N1 B1 1.489(2) . ?
O3 C52 1.437(3) . ?
O3 C49 1.439(3) . ?
O3 Li1 1.923(4) . ?
C21 C26 1.403(2) . ?
C21 C22 1.409(2) . ?
C12 C11 1.407(2) . ?
C12 C13 1.408(2) . ?
C11 C1 1.487(2) . ?
C11 C16 1.401(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.413(2) . ?
C3 C4 1.390(2) . ?
C2 C1 1.407(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(2) . ?
C33 C38 1.402(2) . ?
C33 C34 1.406(2) . ?
C1 C6 1.407(2) . ?
C4 C5 1.390(2) . ?
C4 C7 1.538(2) . ?
C6 H6 0.9500 . ?
C6 C5 1.376(2) . ?
C5 H5 0.9500 . ?
C38 C37 1.395(2) . ?
C38 C39 1.515(3) . ?
C34 C42 1.520(3) . ?
C34 C35 1.393(2) . ?
C14 C15 1.392(2) . ?
C14 C17 1.534(2) . ?
C26 C27 1.514(3) . ?
C26 C25 1.400(2) . ?
C16 H16 0.9500 . ?
C16 C15 1.381(2) . ?
C7 C9 1.530(3) . ?
C7 C10 1.535(3) . ?
C7 C8 1.536(3) . ?
C27 H27 1.0000 . ?
C27 C29 1.523(3) . ?
C27 C28 1.529(3) . ?
C22 C30 1.513(3) . ?
C22 C23 1.397(3) . ?
C15 H15 0.9500 . ?
C42 H42 1.0000 . ?
C42 C43 1.530(3) . ?
C42 C44 1.523(3) . ?
C37 H37 0.9500 . ?
C37 C36 1.379(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.379(3) . ?
C39 H39 1.0000 . ?
C39 C41 1.518(3) . ?
C39 C40 1.524(3) . ?
C30 H30 1.0000 . ?
C30 C32 1.532(3) . ?
C30 C31 1.531(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C25 H25 0.9500 . ?
C25 C24 1.382(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.373(3) . ?
C17 C20 1.521(5) . ?
C17 C19 1.543(5) . ?
C17 C18 1.544(4) . ?
C17 C18A 1.523(6) . ?
C17 C20A 1.536(7) . ?
C17 C19A 1.508(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C36 H36 0.9500 . ?
C24 H24 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.484(3) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C51 1.499(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.494(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C50 1.498(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C47 1.528(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.485(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
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
O2 C45 C46 C47 35.5(2) . . . . ?
O2 C48 C47 C46 24.8(3) . . . . ?
N2 C12 C11 C1 8.4(3) . . . . ?
N2 C12 C11 C16 -175.62(16) . . . . ?
N2 C12 C13 C14 179.49(16) . . . . ?
N2 C33 C38 C37 -178.17(16) . . . . ?
N2 C33 C38 C39 2.4(2) . . . . ?
N2 C33 C34 C42 0.5(2) . . . . ?
N2 C33 C34 C35 178.51(15) . . . . ?
N1 C21 C26 C27 8.5(2) . . . . ?
N1 C21 C26 C25 -174.39(15) . . . . ?
N1 C21 C22 C30 -4.5(2) . . . . ?
N1 C21 C22 C23 174.66(15) . . . . ?
N1 C2 C1 C11 17.9(2) . . . . ?
N1 C2 C1 C6 -169.59(15) . . . . ?
O3 C52 C51 C50 30.3(3) . . . . ?
O3 C49 C50 C51 27.1(3) . . . . ?
C21 N1 C2 C3 7.1(2) . . . . ?
C21 N1 C2 C1 -171.21(15) . . . . ?
C21 N1 B1 O1 -6.4(2) . . . . ?
C21 N1 B1 N2 173.32(15) . . . . ?
C21 C26 C27 C29 -148.66(17) . . . . ?
C21 C26 C27 C28 88.2(2) . . . . ?
C21 C26 C25 C24 -0.8(3) . . . . ?
C21 C22 C30 C32 118.4(2) . . . . ?
C21 C22 C30 C31 -119.34(19) . . . . ?
C21 C22 C23 C24 0.2(3) . . . . ?
C12 N2 C33 C38 78.78(19) . . . . ?
C12 N2 C33 C34 -99.10(18) . . . . ?
C12 N2 B1 O1 158.61(16) . . . . ?
C12 N2 B1 N1 -21.2(3) . . . . ?
C12 C11 C1 C2 -46.2(3) . . . . ?
C12 C11 C1 C6 141.24(17) . . . . ?
C12 C11 C16 C15 -5.6(3) . . . . ?
C12 C13 C14 C15 -2.8(3) . . . . ?
C12 C13 C14 C17 179.56(16) . . . . ?
C11 C12 C13 C14 -3.5(3) . . . . ?
C11 C1 C6 C5 165.91(16) . . . . ?
C11 C16 C15 C14 -0.7(3) . . . . ?
C3 C2 C1 C11 -160.50(15) . . . . ?
C3 C2 C1 C6 12.0(2) . . . . ?
C3 C4 C5 C6 6.6(3) . . . . ?
C3 C4 C7 C9 -9.9(2) . . . . ?
C3 C4 C7 C10 110.63(18) . . . . ?
C3 C4 C7 C8 -130.21(18) . . . . ?
C2 N1 C21 C26 96.81(17) . . . . ?
C2 N1 C21 C22 -80.34(18) . . . . ?
C2 N1 B1 O1 149.55(16) . . . . ?
C2 N1 B1 N2 -30.7(2) . . . . ?
C2 C3 C4 C5 -1.4(2) . . . . ?
C2 C3 C4 C7 -179.17(15) . . . . ?
C2 C1 C6 C5 -7.4(3) . . . . ?
C13 C12 C11 C1 -168.56(16) . . . . ?
C13 C12 C11 C16 7.4(2) . . . . ?
C13 C14 C15 C16 4.9(3) . . . . ?
C13 C14 C17 C20 -35.1(5) . . . . ?
C13 C14 C17 C19 85.7(4) . . . . ?
C13 C14 C17 C18 -157.9(4) . . . . ?
C13 C14 C17 C18A -132.1(7) . . . . ?
C13 C14 C17 C20A -15.2(5) . . . . ?
C13 C14 C17 C19A 104.2(7) . . . . ?
C33 N2 C12 C11 -150.82(15) . . . . ?
C33 N2 C12 C13 26.1(2) . . . . ?
C33 N2 B1 O1 -14.5(2) . . . . ?
C33 N2 B1 N1 165.71(14) . . . . ?
C33 C38 C37 C36 -0.1(3) . . . . ?
C33 C38 C39 C41 111.6(2) . . . . ?
C33 C38 C39 C40 -123.8(2) . . . . ?
C33 C34 C42 C43 112.75(19) . . . . ?
C33 C34 C42 C44 -124.36(19) . . . . ?
C33 C34 C35 C36 -0.8(3) . . . . ?
C1 C11 C16 C15 170.72(18) . . . . ?
C1 C6 C5 C4 -2.3(3) . . . . ?
C4 C3 C2 N1 173.43(15) . . . . ?
C4 C3 C2 C1 -8.2(2) . . . . ?
C5 C4 C7 C9 172.40(16) . . . . ?
C5 C4 C7 C10 -67.1(2) . . . . ?
C5 C4 C7 C8 52.1(2) . . . . ?
C38 C33 C34 C42 -177.30(16) . . . . ?
C38 C33 C34 C35 0.7(3) . . . . ?
C38 C37 C36 C35 0.0(3) . . . . ?
C34 C33 C38 C37 -0.2(3) . . . . ?
C34 C33 C38 C39 -179.64(17) . . . . ?
C34 C35 C36 C37 0.4(3) . . . . ?
C26 C21 C22 C30 178.44(16) . . . . ?
C26 C21 C22 C23 -2.4(2) . . . . ?
C26 C25 C24 C23 -1.4(3) . . . . ?
C16 C11 C1 C2 137.85(17) . . . . ?
C16 C11 C1 C6 -34.8(2) . . . . ?
C7 C4 C5 C6 -175.57(16) . . . . ?
C27 C26 C25 C24 176.31(18) . . . . ?
C22 C21 C26 C27 -174.38(15) . . . . ?
C22 C21 C26 C25 2.8(2) . . . . ?
C22 C23 C24 C25 1.7(3) . . . . ?
C15 C14 C17 C20 147.3(5) . . . . ?
C15 C14 C17 C19 -91.8(4) . . . . ?
C15 C14 C17 C18 24.6(4) . . . . ?
C15 C14 C17 C18A 50.4(7) . . . . ?
C15 C14 C17 C20A 167.3(5) . . . . ?
C15 C14 C17 C19A -73.3(7) . . . . ?
C42 C34 C35 C36 177.28(18) . . . . ?
C37 C38 C39 C41 -67.8(3) . . . . ?
C37 C38 C39 C40 56.8(3) . . . . ?
C35 C34 C42 C43 -65.2(2) . . . . ?
C35 C34 C42 C44 57.7(2) . . . . ?
C39 C38 C37 C36 179.29(19) . . . . ?
C30 C22 C23 C24 179.34(18) . . . . ?
C25 C26 C27 C29 34.3(2) . . . . ?
C25 C26 C27 C28 -88.8(2) . . . . ?
C23 C22 C30 C32 -60.7(2) . . . . ?
C23 C22 C30 C31 61.5(2) . . . . ?
C17 C14 C15 C16 -177.51(18) . . . . ?
C45 O2 C48 C47 -3.0(3) . . . . ?
C45 C46 C47 C48 -36.1(2) . . . . ?
B1 N2 C12 C11 36.0(3) . . . . ?
B1 N2 C12 C13 -147.12(17) . . . . ?
B1 N2 C33 C38 -107.11(18) . . . . ?
B1 N2 C33 C34 75.0(2) . . . . ?
B1 N1 C21 C26 -103.96(17) . . . . ?
B1 N1 C21 C22 78.89(19) . . . . ?
B1 N1 C2 C3 -148.74(16) . . . . ?
B1 N1 C2 C1 32.9(2) . . . . ?
C52 O3 C49 C50 -8.7(3) . . . . ?
C52 C51 C50 C49 -35.0(3) . . . . ?
C49 O3 C52 C51 -13.6(3) . . . . ?
C48 O2 C45 C46 -20.3(2) . . . . ?
Li1 O2 C45 C46 126.3(2) . . . . ?
Li1 O2 C48 C47 -148.7(2) . . . . ?
Li1 O3 C52 C51 141.0(2) . . . . ?
Li1 O3 C49 C50 -165.5(2) . . . . ?