#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:29:40 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700008.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_7700008
loop_
_publ_author_name
'Liu, Xiaoqing'
'Wang, Yu-Xia'
'Han, Zongsu'
'Han, Tian'
'Shi, Wei'
'Cheng, Peng'
_publ_section_title
;
Tuning the magnetization dynamics of TbIII-based single-chain
magnets through substitution on the nitronyl nitroxide radical.
;
_journal_issue 24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 8989
_journal_page_last 8994
_journal_paper_doi 10.1039/c9dt01704f
_journal_volume 48
_journal_year 2019
_chemical_formula_moiety '0.5(C64 H44 F36 N4 O16 S2 Tb2)'
_chemical_formula_sum 'C32 H22 F18 N2 O8 S Tb'
_chemical_formula_weight 1095.49
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_date 2019-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-22 deposited with the CCDC. 2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 129.695(2)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 20.8845(9)
_cell_length_b 17.2985(7)
_cell_length_c 29.7057(11)
_cell_measurement_reflns_used 6834
_cell_measurement_temperature 120(10)
_cell_measurement_theta_max 29.2117
_cell_measurement_theta_min 2.9168
_cell_volume 8257.6(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature 120(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 39.00 93.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 178.0000 90.0000 54
#__ type_ start__ end____ width___ exp.time_
2 omega -95.00 -36.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -18.6622 -178.0000 150.0000 59
#__ type_ start__ end____ width___ exp.time_
3 omega -95.00 -39.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -18.6622 -178.0000 -30.0000 56
#__ type_ start__ end____ width___ exp.time_
4 omega 17.00 49.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -18.6622 37.0000 120.0000 32
#__ type_ start__ end____ width___ exp.time_
5 omega -56.00 3.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -18.6622 -57.0000 120.0000 59
;
_diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0098778000
_diffrn_orient_matrix_UB_12 -0.0362159000
_diffrn_orient_matrix_UB_13 0.0106499000
_diffrn_orient_matrix_UB_21 0.0304382000
_diffrn_orient_matrix_UB_22 -0.0044729000
_diffrn_orient_matrix_UB_23 0.0157392000
_diffrn_orient_matrix_UB_31 -0.0116610000
_diffrn_orient_matrix_UB_32 0.0186716000
_diffrn_orient_matrix_UB_33 0.0245683000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0655
_diffrn_reflns_av_unetI/netI 0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 36659
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.009
_diffrn_reflns_theta_max 25.009
_diffrn_reflns_theta_min 2.923
_diffrn_source 'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 1.893
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.91098
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour 'metallic light blue'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary blue
_exptl_crystal_density_diffrn 1.762
_exptl_crystal_description plate
_exptl_crystal_F_000 4280
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.15
_refine_diff_density_max 1.405
_refine_diff_density_min -1.065
_refine_diff_density_rms 0.135
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1185
_refine_ls_number_reflns 14526
_refine_ls_number_restraints 132
_refine_ls_restrained_S_all 1.034
_refine_ls_R_factor_all 0.0630
_refine_ls_R_factor_gt 0.0441
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0703
_refine_ls_wR_factor_ref 0.0796
_reflns_Friedel_coverage 0.000
_reflns_number_gt 11283
_reflns_number_total 14526
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file c9dt01704f2.cif
_cod_data_source_block 1
_cod_depositor_comments
'Adding full bibliography for 7700008--7700009.cif.'
_cod_database_code 7700008
_shelx_shelxl_version_number 2018/3
_chemical_oxdiff_formula C1H1N1O1TB1
_chemical_oxdiff_usercomment TBL11A
_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 0.764
_shelx_estimated_absorpt_t_min 0.703
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C59-F30A
1.31 with sigma of 0.02
C59-F28B
1.31 with sigma of 0.02
C59-F29B
1.31 with sigma of 0.02
F30A-F29B
2.2 with sigma of 0.02
F29B-F28B
2.2 with sigma of 0.02
F28B-F30A
2.2 with sigma of 0.02
C59-F30B
1.31 with sigma of 0.02
C59-F28A
1.31 with sigma of 0.02
C59-F29A
1.31 with sigma of 0.02
F30B-F29A
2.2 with sigma of 0.02
F29A-F28A
2.2 with sigma of 0.02
F28A-F30B
2.2 with sigma of 0.02
C58-F27A
1.31 with sigma of 0.02
C58-F26B
1.31 with sigma of 0.02
C58-F25A
1.31 with sigma of 0.02
F25A-F26B
2.2 with sigma of 0.02
F26B-F27A
2.2 with sigma of 0.02
F27A-F25A
2.2 with sigma of 0.02
C63-F32B
1.32 with sigma of 0.02
C63-F33A
1.32 with sigma of 0.02
C63-F31B
1.32 with sigma of 0.02
F32B-F33A
2.13 with sigma of 0.02
F33A-F31B
2.13 with sigma of 0.02
F31B-F32B
2.13 with sigma of 0.02
C63-F32A
1.32 with sigma of 0.02
C63-F33B
1.32 with sigma of 0.02
C63-F31A
1.32 with sigma of 0.02
F32A-F33B
2.13 with sigma of 0.02
F33B-F31A
2.13 with sigma of 0.02
F31A-F32A
2.13 with sigma of 0.02
C58-F27B
1.31 with sigma of 0.02
C58-F26A
1.31 with sigma of 0.02
C58-F25B
1.31 with sigma of 0.02
F25B-F26A
2.2 with sigma of 0.02
F26A-F27B
2.2 with sigma of 0.02
F27B-F25B
2.2 with sigma of 0.02
3. Rigid bond restraints
F31B, F32B, F33A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
F32A, F33B, F31A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F32B \\sim F33A \\sim F31B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F32A \\sim F33B \\sim F31A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(F28A) \\sim Ueq, Uanis(F28B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F32B) \\sim Ueq, Uanis(F33A) \\sim Ueq, Uanis(F31B) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F32A) \\sim Ueq, Uanis(F33B) \\sim Ueq, Uanis(F31A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F27B) \\sim Ueq, Uanis(F25B) \\sim Ueq, Uanis(F26A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F27A) \\sim Ueq, Uanis(F26B) \\sim Ueq, Uanis(F25A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F31B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(F30B) = Uanis(F29A) = Uanis(F28A)
Uanis(F28B) = Uanis(F29B) = Uanis(F30A)
5. Others
Sof(F28B)=Sof(F29B)=Sof(F30A)=1-FVAR(1)
Sof(F28A)=Sof(F29A)=Sof(F30B)=FVAR(1)
Sof(F25B)=Sof(F26A)=Sof(F27B)=1-FVAR(2)
Sof(F25A)=Sof(F26B)=Sof(F27A)=FVAR(2)
Sof(F31B)=Sof(F32B)=Sof(F33A)=1-FVAR(3)
Sof(F31A)=Sof(F32A)=Sof(F33B)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C19(H19),
C24(H24), C29(H29), C35(H35), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42),
C43(H43), C51(H51), C56(H56), C61(H61)
6.b Idealised Me refined as rotating group:
C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,
H17c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C49(H49a,
H49b,H49c)
;
_shelx_res_file
;
TITL P120917F1 in P21/n #14 P21/c
p120917f1.res
created by SHELXL-2018/3 at 10:48:19 on 10-Jan-2019
CELL 0.71073 20.8845 17.2985 29.7057 90 129.695 90
ZERR 8 0.0009 0.0007 0.0011 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F N O S Tb
UNIT 256 176 144 16 64 8 8
DFIX 1.31 C59 F30A
DFIX 1.31 C59 F28B
DFIX 1.31 C59 F29B
DFIX 2.2 F30A F29B
DFIX 2.2 F29B F28B
DFIX 2.2 F28B F30A
DFIX 1.31 C59 F30B
DFIX 1.31 C59 F28A
DFIX 1.31 C59 F29A
DFIX 2.2 F30B F29A
DFIX 2.2 F29A F28A
DFIX 2.2 F28A F30B
DFIX 1.31 C58 F27A
DFIX 1.31 C58 F26B
DFIX 1.31 C58 F25A
DFIX 2.2 F25A F26B
DFIX 2.2 F26B F27A
DFIX 2.2 F27A F25A
DFIX 1.32 C63 F32B
DFIX 1.32 C63 F33A
DFIX 1.32 C63 F31B
DFIX 2.13 F32B F33A
DFIX 2.13 F33A F31B
DFIX 2.13 F31B F32B
DFIX 1.32 C63 F32A
DFIX 1.32 C63 F33B
DFIX 1.32 C63 F31A
DFIX 2.13 F32A F33B
DFIX 2.13 F33B F31A
DFIX 2.13 F31A F32A
DFIX 1.31 C58 F27B
DFIX 1.31 C58 F26A
DFIX 1.31 C58 F25B
DFIX 2.2 F25B F26A
DFIX 2.2 F26A F27B
DFIX 2.2 F27B F25B
DELU F31B F32B F33A
DELU F32A F33B F31A
SIMU F32B F33A F31B
SIMU F32A F33B F31A
ISOR 0.002 0.004 C59 C58
ISOR 0.001 0.002 F28A F28B
ISOR 0.005 0.01 F32B F33A F31B
ISOR 0.005 0.01 F32A F33B F31A
ISOR 0.005 0.01 F27B F25B F26A
ISOR 0.005 0.01 F27A F26B F25A
ISOR 0.002 0.004 F31B
EADP F30B F29A F28A
EADP F28B F29B F30A
L.S. 10
PLAN 20
SIZE 0.15 0.15 0.2
TEMP -153(10)
BOND $H
htab
conf
ABIN
fmap 2
acta
OMIT -3 50.02
OMIT -1 0 22
OMIT -9 0 28
OMIT -13 7 19
OMIT -3 0 28
OMIT -4 1 2
OMIT -13 6 31
OMIT -14 6 32
OMIT -3 2 4
REM
REM
REM
WGHT 0.010000
FVAR 0.60820 0.58272 0.49599 0.89198
C1 1 0.025920 0.571481 0.236960 11.00000 0.01124 0.01333 =
0.01669 -0.00359 0.00729 0.00173
C2 1 0.105049 0.570027 0.295238 11.00000 0.02225 0.00763 =
0.01959 -0.00087 0.01381 0.00250
C3 1 0.169307 0.621909 0.320360 11.00000 0.01959 0.01230 =
0.01938 0.00247 0.01222 0.00121
AFIX 43
H3 2 0.166679 0.667406 0.301325 11.00000 -1.20000
AFIX 0
C4 1 0.240305 0.600269 0.377976 11.00000 0.01597 0.01682 =
0.01743 -0.00096 0.00896 0.00063
C5 1 0.224931 0.533232 0.393880 11.00000 0.01811 0.02847 =
0.01727 0.00678 -0.00386 -0.00962
AFIX 43
H5 2 0.264389 0.510287 0.431311 11.00000 -1.20000
AFIX 0
C6 1 0.318998 0.643682 0.417168 11.00000 0.01874 0.02346 =
0.01212 0.00089 0.00775 -0.00138
C7 1 0.322410 0.723130 0.410982 11.00000 0.02221 0.02347 =
0.02597 -0.00295 0.01615 -0.00381
AFIX 43
H7 2 0.274424 0.749831 0.379085 11.00000 -1.20000
AFIX 0
C8 1 0.396170 0.763261 0.451576 11.00000 0.03064 0.02816 =
0.03706 -0.00711 0.02540 -0.01246
AFIX 43
H8 2 0.398205 0.817313 0.446942 11.00000 -1.20000
AFIX 0
C9 1 0.466225 0.725791 0.498347 11.00000 0.02288 0.05993 =
0.02274 -0.00758 0.01150 -0.02092
AFIX 43
H9 2 0.515762 0.754103 0.526318 11.00000 -1.20000
AFIX 0
C10 1 0.464261 0.647403 0.504429 11.00000 0.02252 0.05601 =
0.02154 0.00766 0.00773 -0.00725
AFIX 43
H10 2 0.512793 0.621098 0.536163 11.00000 -1.20000
AFIX 0
C11 1 0.391182 0.606651 0.464094 11.00000 0.02218 0.03081 =
0.02484 0.00376 0.00971 -0.00212
AFIX 43
H11 2 0.390350 0.552373 0.468569 11.00000 -1.20000
AFIX 0
C12 1 -0.080619 0.608271 0.138279 11.00000 0.02585 0.01826 =
0.00779 -0.00215 0.00506 -0.00387
C13 1 -0.109715 0.534984 0.152157 11.00000 0.02301 0.01414 =
0.01904 -0.00039 0.00713 0.00164
C14 1 -0.046035 0.590950 0.107866 11.00000 0.04280 0.03210 =
0.02236 -0.00454 0.01867 -0.00369
AFIX 137
H14A 2 -0.004253 0.549879 0.128967 11.00000 -1.50000
H14B 2 -0.020161 0.637635 0.107100 11.00000 -1.50000
H14C 2 -0.091152 0.574049 0.067712 11.00000 -1.50000
AFIX 0
C15 1 -0.144824 0.672709 0.107417 11.00000 0.02696 0.01846 =
0.02108 0.00610 -0.00073 -0.00149
AFIX 137
H15A 2 -0.195389 0.653614 0.069998 11.00000 -1.50000
H15B 2 -0.122259 0.716264 0.100344 11.00000 -1.50000
H15C 2 -0.158218 0.689790 0.132012 11.00000 -1.50000
AFIX 0
C16 1 -0.143235 0.469614 0.108038 11.00000 0.03202 0.02197 =
0.01610 -0.00514 0.00260 -0.00499
AFIX 137
H16A 2 -0.190478 0.488405 0.069062 11.00000 -1.50000
H16B 2 -0.161489 0.426945 0.119166 11.00000 -1.50000
H16C 2 -0.099332 0.451383 0.107464 11.00000 -1.50000
AFIX 0
C17 1 -0.169484 0.553603 0.163375 11.00000 0.01822 0.02883 =
0.04045 -0.00267 0.01247 -0.00587
AFIX 137
H17A 2 -0.147943 0.597372 0.190452 11.00000 -1.50000
H17B 2 -0.175070 0.508445 0.180557 11.00000 -1.50000
H17C 2 -0.224025 0.567011 0.126359 11.00000 -1.50000
AFIX 0
C18 1 -0.142361 0.348133 0.265535 11.00000 0.02374 0.01497 =
0.03420 -0.00125 0.01561 -0.00033
C19 1 -0.087199 0.364953 0.325505 11.00000 0.02771 0.02765 =
0.04234 -0.01027 0.02879 -0.00257
AFIX 43
H19 2 -0.108097 0.376671 0.345248 11.00000 -1.20000
AFIX 0
C20 1 -0.001437 0.364479 0.356249 11.00000 0.03917 0.01223 =
0.02929 -0.00028 0.02501 -0.00302
C21 1 -0.235891 0.346694 0.234955 11.00000 0.03513 0.04035 =
0.06919 -0.01110 0.03892 -0.00193
C22 1 0.056307 0.381775 0.422205 11.00000 0.04863 0.04725 =
0.02804 -0.00747 0.02683 -0.00054
C23 1 0.000478 0.171144 0.170168 11.00000 0.02606 0.01784 =
0.02776 -0.00059 0.01921 0.00065
C24 1 -0.070852 0.192796 0.115452 11.00000 0.02824 0.02598 =
0.02029 -0.00785 0.01329 0.00380
AFIX 43
H24 2 -0.083576 0.169374 0.081643 11.00000 -1.20000
AFIX 0
C25 1 -0.124346 0.248295 0.109023 11.00000 0.01579 0.02005 =
0.01391 -0.00196 0.00626 -0.00865
C26 1 0.055600 0.109084 0.172754 11.00000 0.03115 0.03012 =
0.02706 -0.00017 0.01593 0.01392
C27 1 -0.201449 0.265574 0.045243 11.00000 0.02721 0.02544 =
0.02598 -0.00494 0.01685 -0.00798
C28 1 0.194775 0.317519 0.303993 11.00000 0.01404 0.01698 =
0.03393 -0.00560 0.01199 -0.00233
C29 1 0.182206 0.335004 0.253308 11.00000 0.01822 0.02667 =
0.02626 -0.00121 0.01431 -0.00402
AFIX 43
H29 2 0.228631 0.336717 0.254380 11.00000 -1.20000
AFIX 0
C30 1 0.103109 0.350091 0.200928 11.00000 0.03057 0.00925 =
0.03061 -0.00027 0.02288 -0.00009
C31 1 0.282967 0.307509 0.361462 11.00000 0.02045 0.04255 =
0.03051 -0.00265 0.01436 -0.00035
C32 1 0.095436 0.365332 0.147162 11.00000 0.03348 0.03328 =
0.03205 0.00674 0.02499 0.00168
C33 1 0.532393 0.320404 0.259307 11.00000 0.01697 0.01189 =
0.01727 -0.00103 0.01079 -0.00171
C34 1 0.516945 0.323113 0.204893 11.00000 0.01489 0.01887 =
0.01298 -0.00148 0.00961 -0.00312
C35 1 0.478326 0.379520 0.162727 11.00000 0.01777 0.01270 =
0.02073 -0.00161 0.01231 0.00006
AFIX 43
H35 2 0.452774 0.423776 0.164195 11.00000 -1.20000
AFIX 0
C36 1 0.480432 0.365147 0.117165 11.00000 0.01514 0.01660 =
0.01799 -0.00450 0.01050 -0.00057
C37 1 0.521430 0.297618 0.126324 11.00000 0.02362 0.01509 =
0.01937 -0.00266 0.01434 -0.00368
AFIX 43
H37 2 0.528848 0.278457 0.099954 11.00000 -1.20000
AFIX 0
C38 1 0.443026 0.414802 0.064884 11.00000 0.01336 0.01858 =
0.01587 -0.00248 0.00773 -0.00353
C39 1 0.431519 0.493542 0.067140 11.00000 0.03871 0.02527 =
0.01311 0.00243 0.01420 -0.00064
AFIX 43
H39 2 0.443931 0.515358 0.101283 11.00000 -1.20000
AFIX 0
C40 1 0.401865 0.539967 0.019335 11.00000 0.03764 0.02377 =
0.02709 0.00387 0.01705 0.00412
AFIX 43
H40 2 0.394636 0.593785 0.021118 11.00000 -1.20000
AFIX 0
C41 1 0.382749 0.509078 -0.030709 11.00000 0.03319 0.03603 =
0.01836 0.00822 0.01311 -0.00209
AFIX 43
H41 2 0.362448 0.541422 -0.063221 11.00000 -1.20000
AFIX 0
C42 1 0.393202 0.431072 -0.033402 11.00000 0.02495 0.03843 =
0.01806 0.00440 0.01366 0.00532
AFIX 43
H42 2 0.380444 0.409498 -0.067719 11.00000 -1.20000
AFIX 0
C43 1 0.422335 0.384165 0.013996 11.00000 0.02811 0.02457 =
0.02622 -0.00238 0.01821 0.00067
AFIX 43
H43 2 0.428215 0.330213 0.011582 11.00000 -1.20000
AFIX 0
C44 1 0.598214 0.281671 0.356305 11.00000 0.02371 0.01475 =
0.00804 -0.00053 0.01050 -0.00348
C45 1 0.541243 0.352045 0.341177 11.00000 0.03081 0.01431 =
0.01288 -0.00027 0.01613 -0.00230
C46 1 0.688407 0.305020 0.386956 11.00000 0.02623 0.02647 =
0.01498 -0.00288 0.00975 -0.00786
AFIX 137
H46A 2 0.689069 0.346638 0.364873 11.00000 -1.50000
H46B 2 0.718944 0.260305 0.388945 11.00000 -1.50000
H46C 2 0.714873 0.323047 0.426646 11.00000 -1.50000
AFIX 0
C47 1 0.592445 0.215825 0.387371 11.00000 0.03340 0.01511 =
0.01656 0.00375 0.01269 0.00112
AFIX 137
H47A 2 0.603638 0.235526 0.422730 11.00000 -1.50000
H47B 2 0.633507 0.176042 0.398177 11.00000 -1.50000
H47C 2 0.536467 0.193409 0.361257 11.00000 -1.50000
AFIX 0
C48 1 0.580713 0.416323 0.385432 11.00000 0.05353 0.01969 =
0.02346 0.00179 0.02671 0.00287
AFIX 137
H48A 2 0.601412 0.395976 0.423407 11.00000 -1.50000
H48B 2 0.539322 0.456715 0.372656 11.00000 -1.50000
H48C 2 0.627135 0.438183 0.389082 11.00000 -1.50000
AFIX 0
C49 1 0.457273 0.328607 0.323421 11.00000 0.03298 0.02155 =
0.03189 0.00820 0.02222 0.00620
AFIX 137
H49A 2 0.434288 0.285258 0.295880 11.00000 -1.50000
H49B 2 0.418868 0.372544 0.304737 11.00000 -1.50000
H49C 2 0.464828 0.312992 0.358261 11.00000 -1.50000
AFIX 0
C50 1 0.674991 0.053364 0.267178 11.00000 0.02736 0.01386 =
0.03920 0.00582 0.02579 0.00078
C51 1 0.722303 0.037499 0.326671 11.00000 0.01752 0.02940 =
0.02663 0.00632 0.01283 0.00514
AFIX 43
H51 2 0.780642 0.030552 0.349641 11.00000 -1.20000
AFIX 0
C52 1 0.687400 0.031459 0.353652 11.00000 0.02602 0.01329 =
0.02238 0.00187 0.01159 0.00431
C53 1 0.716950 0.053898 0.240287 11.00000 0.04507 0.03817 =
0.05212 0.02252 0.03976 0.01561
C54 1 0.744975 0.009680 0.418616 11.00000 0.03097 0.02825 =
0.03684 0.00416 0.01349 0.01012
C55 1 0.294987 0.033240 0.172734 11.00000 0.02929 0.01331 =
0.01925 0.00112 0.01828 -0.00375
C56 1 0.296783 0.058734 0.217391 11.00000 0.02142 0.03115 =
0.02121 -0.00062 0.01510 -0.00100
AFIX 43
H56 2 0.245753 0.063494 0.210383 11.00000 -1.20000
AFIX 0
C57 1 0.370288 0.077778 0.272307 11.00000 0.03160 0.02363 =
0.02395 -0.00089 0.02264 0.00072
C58 1 0.209604 0.013761 0.113439 11.00000 0.03494 0.03693 =
0.03586 -0.00120 0.02278 -0.00121
C59 1 0.363820 0.098846 0.318700 11.00000 0.04760 0.05724 =
0.05244 -0.00396 0.03566 -0.00355
C60 1 0.374183 0.144124 0.098281 11.00000 0.02428 0.02046 =
0.01517 -0.00273 0.01023 -0.01061
C61 1 0.326995 0.197118 0.101114 11.00000 0.02151 0.02492 =
0.01962 0.00785 0.00867 0.00832
AFIX 43
H61 2 0.281665 0.222333 0.066412 11.00000 -1.20000
AFIX 0
C62 1 0.344730 0.213727 0.153251 11.00000 0.02481 0.01406 =
0.03503 -0.00264 0.02003 -0.00292
C63 1 0.353990 0.132101 0.038750 11.00000 0.03761 0.03588 =
0.02297 -0.00051 0.01840 0.00286
C64 1 0.290667 0.274613 0.153137 11.00000 0.03174 0.02474 =
0.02704 0.00425 0.02237 0.00535
F1 3 -0.254986 0.371798 0.266811 11.00000 0.04279 0.11704 =
0.09892 -0.05744 0.05504 -0.01774
F2 3 -0.263333 0.274660 0.218919 11.00000 0.04442 0.06074 =
0.09126 -0.03740 0.05049 -0.02605
F3 3 -0.279065 0.387399 0.185948 11.00000 0.03662 0.09320 =
0.09794 0.02217 0.03667 0.02317
F4 3 0.018506 0.411040 0.440522 11.00000 0.06933 0.12072 =
0.04232 -0.02316 0.03838 0.01169
F5 3 0.092186 0.317419 0.452322 11.00000 0.11647 0.06340 =
0.03020 0.01161 0.02716 0.02882
F6 3 0.115898 0.429593 0.438431 11.00000 0.08766 0.13069 =
0.03538 -0.04946 0.03899 -0.07478
F7 3 -0.249242 0.320689 0.040744 11.00000 0.02191 0.03177 =
0.02293 -0.00227 0.00307 0.00755
F8 3 -0.179280 0.286351 0.013683 11.00000 0.03434 0.04984 =
0.02663 0.00970 0.01629 -0.00584
F9 3 -0.249441 0.201711 0.019440 11.00000 0.02693 0.02748 =
0.01766 -0.00677 0.00816 -0.00717
F10 3 0.132504 0.132986 0.203244 11.00000 0.03221 0.05811 =
0.10602 -0.02354 0.04501 0.00016
F11 3 0.058510 0.046058 0.199515 11.00000 0.07793 0.02825 =
0.07235 0.01537 0.05679 0.02485
F12 3 0.029278 0.086246 0.121138 11.00000 0.06493 0.07413 =
0.03717 -0.00211 0.03076 0.03547
F13 3 0.300641 0.361534 0.399762 11.00000 0.03086 0.07368 =
0.03928 -0.01864 0.00172 0.00178
F14 3 0.341010 0.313026 0.355825 11.00000 0.01993 0.11481 =
0.04915 0.01426 0.02075 0.00289
F15 3 0.294003 0.240304 0.386151 11.00000 0.02499 0.05492 =
0.05370 0.02448 0.00991 0.01033
F16 3 0.165635 0.388216 0.158831 11.00000 0.05395 0.05202 =
0.05870 -0.00076 0.04694 -0.01058
F17 3 0.073286 0.300722 0.115869 11.00000 0.08575 0.06919 =
0.04337 -0.02407 0.04898 -0.03457
F18 3 0.038613 0.417534 0.112766 11.00000 0.09950 0.11376 =
0.08404 0.08026 0.08085 0.08245
F19 3 0.694361 0.113460 0.205701 11.00000 0.07969 0.05631 =
0.10028 0.03575 0.08172 0.02678
F20 3 0.799446 0.051130 0.278577 11.00000 0.03068 0.13707 =
0.07333 0.02014 0.03833 0.01255
F21 3 0.693461 -0.009082 0.206262 11.00000 0.10088 0.05390 =
0.10699 -0.00990 0.09282 0.00564
F22 3 0.746974 0.065291 0.449652 11.00000 0.08063 0.04180 =
0.02308 -0.00677 0.00918 0.01817
F23 3 0.822553 -0.005277 0.441337 11.00000 0.02937 0.13110 =
0.04336 0.03478 0.01369 0.03359
F24 3 0.718211 -0.052757 0.427994 11.00000 0.06505 0.04618 =
0.03067 0.01410 0.02352 0.00087
PART 1
F25A 3 0.173292 0.084862 0.085325 31.00000 0.03489 0.04758 =
0.03682 0.00784 0.00108 0.00085
PART 0
PART 2
F25B 3 0.150478 0.054206 0.100749 -31.00000 0.02878 0.08651 =
0.05843 -0.02677 0.00964 0.01975
F26A 3 0.212818 0.009509 0.070943 -31.00000 0.04513 0.06917 =
0.03011 -0.01046 0.02302 -0.02372
PART 0
PART 1
F26B 3 0.212410 -0.025337 0.078148 31.00000 0.03590 0.05192 =
0.04109 -0.02678 0.01124 0.00298
F27A 3 0.156711 -0.013741 0.118400 31.00000 0.03769 0.08334 =
0.03739 -0.00187 0.02012 -0.03405
PART 0
PART 2
F27B 3 0.192668 -0.063009 0.117940 -31.00000 0.04004 0.03973 =
0.05144 -0.00630 0.01364 -0.02265
F28A 3 0.424976 0.140695 0.361570 21.00000 0.04441 0.05576 =
0.03960 -0.00769 0.03104 -0.00288
PART 0
PART 1
F28B 3 0.430217 0.129595 0.366600 -21.00000 0.04628 0.04591 =
0.03828 -0.00739 0.03002 -0.00455
PART 0
PART 2
F29A 3 0.379389 0.025331 0.350242 21.00000 0.04441 0.05576 =
0.03960 -0.00769 0.03104 -0.00288
PART 0
PART 1
F29B 3 0.318874 0.058319 0.323173 -21.00000 0.04628 0.04591 =
0.03828 -0.00739 0.03002 -0.00455
F30A 3 0.309187 0.172769 0.293053 -21.00000 0.04628 0.04591 =
0.03828 -0.00739 0.03002 -0.00455
PART 0
PART 2
F30B 3 0.293922 0.117889 0.302655 21.00000 0.04441 0.05576 =
0.03960 -0.00769 0.03104 -0.00288
PART 0
PART 1
F31A 3 0.420133 0.139512 0.043402 41.00000 0.06520 0.13535 =
0.04550 -0.01747 0.04524 -0.02035
PART 0
PART 2
F31B 3 0.402034 0.078473 0.039949 -41.00000 0.03158 0.03213 =
0.02671 -0.00034 0.02011 0.00374
PART 0
PART 1
F32A 3 0.324859 0.062010 0.019488 41.00000 0.12725 0.05746 =
0.03266 -0.02152 0.04559 -0.02812
PART 0
PART 2
F32B 3 0.277053 0.109183 -0.004543 -41.00000 0.03130 0.04560 =
0.02482 -0.00801 0.02079 -0.00924
F33A 3 0.363297 0.195995 0.017938 -41.00000 0.05137 0.02584 =
0.02784 -0.00570 0.02089 -0.01078
PART 0
PART 1
F33B 3 0.296937 0.179714 -0.001999 41.00000 0.09589 0.09726 =
0.03881 0.03265 0.03941 0.05166
PART 0
F34 3 0.332562 0.339852 0.178512 11.00000 0.03932 0.02480 =
0.04549 -0.00449 0.02479 0.00826
F35 3 0.221770 0.293495 0.099643 11.00000 0.03158 0.04900 =
0.03366 0.00477 0.00930 0.02341
F36 3 0.267667 0.249600 0.183318 11.00000 0.05312 0.04033 =
0.06757 0.02252 0.05102 0.02238
TB1 7 -0.005331 0.309961 0.245941 11.00000 0.01282 0.01141 =
0.01722 -0.00022 0.00821 -0.00011
TB2 7 0.491461 0.079464 0.236143 11.00000 0.01762 0.01149 =
0.01731 0.00006 0.01194 0.00048
N1 4 -0.028769 0.512086 0.209884 11.00000 0.01388 0.01130 =
0.02185 -0.00001 0.00659 0.00075
N2 4 -0.008370 0.631805 0.199694 11.00000 0.01607 0.01174 =
0.01695 0.00295 0.00799 0.00208
N3 4 0.563565 0.259373 0.296020 11.00000 0.02276 0.01280 =
0.01776 -0.00117 0.01583 -0.00004
N4 4 0.522969 0.377995 0.285165 11.00000 0.02116 0.00992 =
0.01479 -0.00304 0.01008 -0.00272
O1 5 -0.019332 0.447652 0.235125 11.00000 0.02892 0.00840 =
0.02167 0.00020 0.01216 -0.00213
O2 5 0.023318 0.700492 0.212371 11.00000 0.01955 0.00990 =
0.02337 0.00158 0.01082 -0.00080
O3 5 -0.126437 0.331638 0.232894 11.00000 0.01509 0.01785 =
0.02580 -0.00151 0.01320 -0.00045
O4 5 0.035917 0.350089 0.337277 11.00000 0.01820 0.01639 =
0.02028 -0.00192 0.01150 -0.00201
O5 5 0.028255 0.195935 0.219354 11.00000 0.01792 0.01525 =
0.02089 0.00215 0.01229 0.00485
O6 5 -0.118426 0.285144 0.147335 11.00000 0.01484 0.01756 =
0.01329 -0.00150 0.00439 -0.00207
O7 5 0.139978 0.309314 0.309585 11.00000 0.01025 0.02644 =
0.02387 0.00201 0.00934 0.00361
O8 5 0.036109 0.351057 0.191688 11.00000 0.02013 0.02326 =
0.02342 0.00307 0.01431 0.00075
O9 5 0.578563 0.191955 0.285192 11.00000 0.01878 0.01087 =
0.02049 0.00117 0.01207 0.00170
O10 5 0.490410 0.444466 0.261547 11.00000 0.02653 0.00671 =
0.02363 0.00218 0.01544 0.00356
O11 5 0.598034 0.066001 0.231406 11.00000 0.02543 0.01746 =
0.02905 0.00233 0.02076 0.00550
O12 5 0.613450 0.041824 0.331787 11.00000 0.02107 0.01305 =
0.02314 0.00128 0.01313 0.00531
O13 5 0.443147 0.077692 0.289037 11.00000 0.02167 0.02492 =
0.02104 0.00082 0.01580 -0.00087
O14 5 0.356480 0.024065 0.174087 11.00000 0.01885 0.02244 =
0.02760 -0.00217 0.01549 -0.00063
O15 5 0.432966 0.103214 0.138438 11.00000 0.03023 0.01741 =
0.02150 0.00234 0.02059 0.00095
O16 5 0.401834 0.187231 0.203103 11.00000 0.01448 0.01773 =
0.01865 0.00319 0.00864 0.00384
S1 6 0.130184 0.494372 0.341704 11.00000 0.02870 0.02048 =
0.02504 0.00662 0.00380 -0.00912
S2 6 0.557831 0.251173 0.188993 11.00000 0.02531 0.01680 =
0.02390 0.00315 0.01851 0.00427
HKLF 4 1 1 0 0 0 -1 0 -1 0 -1
REM P120917F1 in P21/n #14 P21/c
REM wR2 = 0.0796, GooF = S = 1.009, Restrained GooF = 1.034 for all data
REM R1 = 0.0441 for 11283 Fo > 4sig(Fo) and 0.0630 for all 14526 data
REM 1185 parameters refined using 132 restraints
END
WGHT 0.0101 0.0000
REM Instructions for potential hydrogen bonds
HTAB C3 O2
EQIV $5 x, -y+1/2, z+1/2
HTAB C5 F32A_$5
HTAB C14 F18
EQIV $1 -x, y+1/2, -z+1/2
HTAB C15 O7_$1
HTAB C16 F7
HTAB C16 O6
HTAB C35 O10
EQIV $2 -x+1, y+1/2, -z+1/2
HTAB C35 O12_$2
EQIV $6 x+1, -y+1/2, z+1/2
HTAB C46 F9_$6
HTAB C47 F28A
HTAB C47 F28B
HTAB C47 O13
HTAB C48 O14_$2
HTAB C49 F14
HTAB C56 F10
REM Highest difference peak 1.405, deepest hole -1.065, 1-sigma level 0.135
Q1 1 0.2900 0.0802 0.3065 11.00000 0.05 1.40
Q2 1 0.3502 0.0390 0.3442 11.00000 0.05 1.10
Q3 1 0.2990 0.1503 0.3030 11.00000 0.05 0.97
Q4 1 -0.0378 0.2602 0.2163 11.00000 0.05 0.78
Q5 1 0.5190 0.0260 0.2624 11.00000 0.05 0.76
Q6 1 0.4110 0.0116 0.3564 11.00000 0.05 0.74
Q7 1 0.3304 0.1956 0.2922 11.00000 0.05 0.73
Q8 1 0.5286 0.1313 0.2671 11.00000 0.05 0.72
Q9 1 -0.0383 0.3524 0.2131 11.00000 0.05 0.71
Q10 1 -0.0292 0.2778 0.2605 11.00000 0.05 0.70
Q11 1 0.5700 0.2760 0.3200 11.00000 0.05 0.65
Q12 1 0.2370 0.3295 0.3314 11.00000 0.05 0.65
Q13 1 -0.1602 0.7569 0.0747 11.00000 0.05 0.61
Q14 1 0.4412 0.0483 0.2384 11.00000 0.05 0.61
Q15 1 0.4000 0.2227 0.3343 11.00000 0.05 0.61
Q16 1 0.2391 -0.0669 0.1178 11.00000 0.05 0.61
Q17 1 -0.3021 0.3157 0.1812 11.00000 0.05 0.59
Q18 1 0.5910 0.2959 0.2865 11.00000 0.05 0.58
Q19 1 0.3704 0.0533 0.0287 11.00000 0.05 0.57
Q20 1 0.0167 0.2667 0.2781 11.00000 0.05 0.57
;
_shelx_res_checksum 42718
_shelx_fab_file
;
-24 0 16 0.3640 0.0717
-24 0 18 1.4521 0.0302
-24 0 20 -1.2837 0.0797
-24 0 22 1.9019 -0.0076
-24 0 24 0.0467 0.0094
-24 0 26 1.9490 0.0224
-24 0 28 2.3584 -0.0569
-24 1 15 3.0064 0.2892
-24 1 16 2.8493 0.1862
-24 1 17 0.1983 -0.0153
-24 1 18 3.7732 0.0763
-24 1 19 -1.2161 0.0369
-24 1 20 3.8932 0.1474
-24 1 21 -0.7530 -0.0586
-24 1 22 3.4766 0.0872
-24 1 23 -0.3187 0.0686
-24 1 24 4.5208 -0.0486
-24 1 25 1.1904 -0.1555
-24 1 26 0.2131 -0.0309
-24 1 27 -1.1343 0.0565
-24 1 28 -0.3781 -0.1111
-24 2 16 2.0508 -0.0373
-24 2 17 0.4581 0.0529
-24 2 18 1.0488 0.1195
-24 2 19 -2.2457 0.0918
-24 2 20 2.2658 -0.1374
-24 2 21 -0.8551 -0.0614
-24 2 22 0.0442 0.0520
-24 2 23 -1.1506 0.1443
-24 2 24 2.1562 -0.0937
-24 2 25 1.0258 0.1151
-24 2 26 2.6863 0.0720
-24 2 27 1.9371 0.0992
-24 2 28 3.0424 -0.0001
-24 3 16 -2.1330 -0.2535
-24 3 17 0.5760 -0.1987
-24 3 18 -0.7488 0.1935
-24 3 19 0.8522 -0.0849
-24 3 20 0.9663 0.1123
-24 3 21 -1.0733 -0.0589
-24 3 22 1.7238 0.1467
-24 3 23 -1.2394 -0.0209
-24 3 24 -0.0939 0.0799
-24 3 25 -3.1862 0.1184
-24 3 26 0.3843 -0.0768
-24 3 27 1.4615 -0.1514
-24 4 18 3.4155 -0.1140
-24 4 19 -2.2841 -0.2212
-24 4 20 4.5671 0.0022
-24 4 21 -1.4995 -0.0015
-24 4 22 3.8449 -0.1113
-24 4 23 1.3928 -0.1436
-24 4 24 -0.8767 0.0543
-24 4 25 0.3188 0.3114
-24 4 26 -7.6306 -0.0170
-24 5 20 -1.5401 0.1402
-24 5 21 -0.8761 0.0899
-24 5 22 -2.1771 0.0400
-24 5 23 -1.7307 -0.0522
-24 5 24 0.1436 -0.1227
-23 0 12 -1.5570 -0.2311
-23 0 14 -1.8745 0.1084
-23 0 16 -0.4914 0.0416
-23 0 18 -2.5912 0.1263
-23 0 20 -2.9856 0.0440
-23 0 22 -2.0522 0.0011
-23 0 24 -1.7040 0.0428
-23 0 26 2.1811 -0.0236
-23 0 28 2.0708 0.0329
-23 0 30 3.5157 0.0119
-23 1 11 1.3204 -0.1688
-23 1 12 2.8282 -0.5289
-23 1 13 1.5743 0.2589
-23 1 14 2.2672 -0.0341
-23 1 15 -0.3860 0.0495
-23 1 16 1.2347 0.1563
-23 1 17 -3.1250 0.0827
-23 1 18 3.8170 0.0889
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12 5 0 0.5145 -0.1548
12 5 1 2.9080 -0.1875
12 5 2 -1.0341 -0.1612
12 5 3 3.4259 -0.1351
12 5 4 1.3598 -0.0706
12 5 5 1.5728 -0.0159
12 5 6 3.2300 0.0719
12 5 7 -1.7277 0.1879
12 5 8 0.0960 0.1754
12 5 9 -1.5233 0.0984
12 5 10 -1.1782 0.1171
12 5 11 1.2811 -0.0821
12 6 0 4.1697 -0.0813
12 6 1 0.4478 0.0969
12 6 2 3.7430 -0.0861
12 6 3 1.2240 0.2270
12 6 4 0.6354 -0.0101
12 6 5 0.8588 0.0816
12 6 6 3.5990 -0.0452
12 6 7 0.3773 -0.0116
12 6 8 4.3775 0.0041
12 6 9 -3.7671 0.0080
12 6 10 -0.1010 0.0465
12 6 11 -3.3426 -0.2739
12 7 0 -0.5333 0.0304
12 7 1 0.4095 0.0006
12 7 2 1.9177 -0.0338
12 7 3 2.4127 -0.1313
12 7 4 -0.9290 -0.0310
12 7 5 2.7040 -0.1284
12 7 6 -5.9598 0.0796
12 7 7 2.5218 -0.2122
12 7 8 -2.9469 -0.1168
12 7 9 2.5035 -0.0731
12 7 10 0.6029 0.0465
12 7 11 0.3146 0.0073
12 8 0 -0.0976 0.0412
12 8 1 -0.3600 0.0361
12 8 2 -1.0241 0.1272
12 8 3 -2.6661 -0.0532
12 8 4 0.6967 -0.0759
12 8 5 -1.9143 0.0183
12 8 6 -1.5303 -0.0751
12 8 7 -4.6377 0.0023
12 8 8 -3.0492 -0.1397
12 8 9 -5.6360 -0.0545
12 8 10 0.7263 -0.4804
12 9 0 -2.0482 -0.0593
12 9 1 -0.3340 0.0658
12 9 2 -3.4144 0.0039
12 9 3 -3.8001 -0.0471
12 9 4 -3.0493 0.0557
12 9 5 -7.4559 -0.0894
12 9 6 -2.9480 -0.1431
12 9 7 -7.6169 -0.2079
12 9 8 -4.8938 0.0002
12 9 9 -7.9990 -0.3160
12 10 0 -5.7400 0.0593
12 10 1 0.6972 0.1169
12 10 2 -7.5080 0.0756
12 10 3 2.5153 0.0143
12 10 4 -4.8245 0.2155
12 10 5 1.8220 0.0194
12 10 6 -0.7930 0.0645
12 10 7 3.2251 0.1229
12 10 8 -2.2608 0.0241
12 11 0 0.5712 0.0156
12 11 1 1.0944 0.0738
12 11 2 -0.7803 0.1326
12 11 3 2.0105 0.0537
12 11 4 -3.8882 0.2189
12 11 5 0.6912 -0.1990
12 11 6 0.2949 0.0901
12 11 7 1.1045 -0.0689
12 12 0 -4.9398 -0.0049
12 12 1 -3.0642 -0.1591
12 12 2 -2.4407 -0.0225
12 12 3 0.2709 0.0652
12 12 4 -2.1197 0.1465
12 12 5 1.0883 0.0116
12 12 6 -3.5104 0.2263
12 13 0 2.0517 0.0580
12 13 1 -1.4046 -0.1246
12 13 2 -0.9813 0.0770
12 13 3 -2.8375 -0.0346
12 13 4 0.6279 -0.0121
12 13 5 1.5642 0.2124
12 14 0 0.1001 -0.1391
12 14 1 -0.1539 0.1498
12 14 2 -0.5503 0.0478
12 14 3 -2.8728 -0.0142
12 14 4 -2.9253 -0.1045
12 15 0 2.6059 0.1979
12 15 1 0.2887 0.1640
12 15 2 5.6257 0.0732
12 16 0 0.1866 0.2507
13 0 0 2.5450 -3.2155
13 0 2 3.4981 -2.3297
13 0 4 1.6854 -1.0127
13 0 6 -1.3570 -0.1307
13 0 8 0.4416 0.2100
13 0 10 1.4362 0.1828
13 1 0 -2.6375 -0.1151
13 1 1 3.2647 0.2700
13 1 2 -2.2793 -0.0468
13 1 3 2.5262 0.0240
13 1 4 0.4878 0.1394
13 1 5 1.3871 -0.2410
13 1 6 -1.4838 0.2761
13 1 7 3.1880 -0.0972
13 1 8 -3.1133 0.2855
13 1 9 3.6774 0.0500
13 1 10 -0.8565 0.2697
13 1 11 2.4383 -0.2300
13 2 0 1.1329 0.3715
13 2 1 1.2324 0.2516
13 2 2 -1.8348 0.0416
13 2 3 3.9381 0.3969
13 2 4 -0.2117 -0.1352
13 2 5 1.9264 0.2690
13 2 6 1.6978 -0.1977
13 2 7 0.0722 -0.0235
13 2 8 -0.6892 -0.2107
13 2 9 2.4265 0.0081
13 2 10 -1.2075 -0.0783
13 2 11 1.1563 -0.0063
13 3 0 3.2345 0.0845
13 3 1 -5.6526 0.1098
13 3 2 2.0623 0.0998
13 3 3 -3.6851 -0.0026
13 3 4 -1.5117 0.1034
13 3 5 -0.2815 -0.0623
13 3 6 -0.3547 0.2460
13 3 7 -1.5324 -0.1080
13 3 8 -2.0451 0.3213
13 3 9 -1.5113 -0.1051
13 3 10 -4.2149 0.2083
13 3 11 1.7457 0.1063
13 4 0 -4.1438 -0.1361
13 4 1 -6.4460 0.0036
13 4 2 -1.6931 0.0711
13 4 3 -8.0346 0.1017
13 4 4 -3.8723 0.1048
13 4 5 -4.5161 0.1330
13 4 6 -4.3054 0.0353
13 4 7 2.0597 0.1836
13 4 8 -1.6589 -0.0626
13 4 9 2.8194 0.2637
13 4 10 -2.3005 -0.0841
13 5 0 -0.8469 -0.1158
13 5 1 4.0003 -0.1643
13 5 2 0.6227 -0.1455
13 5 3 4.4512 -0.0617
13 5 4 4.4313 -0.0835
13 5 5 1.1257 0.1495
13 5 6 1.3312 0.1346
13 5 7 -0.6199 0.1287
13 5 8 -0.9714 0.1820
13 5 9 2.1106 0.0605
13 5 10 -2.5004 0.1463
13 6 0 3.6161 -0.0946
13 6 1 1.2735 0.2587
13 6 2 0.4589 -0.0490
13 6 3 1.9933 0.2247
13 6 4 2.7439 -0.0885
13 6 5 3.4042 0.0824
13 6 6 6.1579 -0.0736
13 6 7 0.1664 0.0047
13 6 8 2.7946 0.2572
13 6 9 -0.8086 -0.2316
13 7 0 3.2783 -0.0235
13 7 1 2.1848 -0.1496
13 7 2 3.5605 -0.0587
13 7 3 3.1404 -0.0977
13 7 4 -2.3246 0.0550
13 7 5 3.1269 -0.0884
13 7 6 -2.2621 -0.1629
13 7 7 4.1404 0.0508
13 7 8 2.0056 -0.0959
13 7 9 1.5308 0.1732
13 8 0 -1.4141 0.0369
13 8 1 0.5823 -0.0936
13 8 2 0.3993 -0.0904
13 8 3 0.7402 -0.0882
13 8 4 0.2096 -0.1534
13 8 5 -1.4966 0.0384
13 8 6 -3.0559 -0.0612
13 8 7 -4.0717 0.0798
13 8 8 -0.9185 -0.3985
13 9 0 -1.2296 -0.1409
13 9 1 -2.4188 -0.0266
13 9 2 -1.6940 -0.0142
13 9 3 -7.1654 -0.1550
13 9 4 0.1148 -0.1255
13 9 5 -8.9456 -0.1932
13 9 6 -1.0542 0.0040
13 9 7 -9.5261 -0.2763
13 9 8 -2.3569 0.0241
13 10 0 -6.1561 -0.0108
13 10 1 1.5929 0.0659
13 10 2 -5.9716 0.1329
13 10 3 2.0677 -0.0269
13 10 4 -1.9318 0.1825
13 10 5 2.7340 0.0347
13 10 6 -0.4679 0.0065
13 10 7 2.8199 -0.1011
13 11 0 0.5201 0.0988
13 11 1 1.8379 0.0176
13 11 2 -1.7154 0.1147
13 11 3 1.5850 -0.2053
13 11 4 -1.5311 0.0296
13 11 5 0.7194 -0.2593
13 11 6 3.7321 -0.2477
13 12 0 -3.2704 -0.0097
13 12 1 -0.9975 0.0072
13 12 2 -0.5149 0.0707
13 12 3 1.8124 0.0572
13 12 4 -2.2128 0.1633
13 12 5 -0.9048 0.0177
13 13 0 0.1350 0.0179
13 13 1 -2.3710 -0.1114
13 13 2 -0.8344 -0.0830
13 13 3 0.2383 0.1358
13 14 0 0.4629 -0.0761
13 14 1 -1.6283 -0.0594
13 14 2 -3.7121 0.0176
13 15 0 2.4469 -0.0557
14 0 0 2.8846 -3.1565
14 0 2 2.1910 -2.1861
14 0 4 -1.1338 -0.9765
14 0 6 -0.8703 -0.1568
14 0 8 2.2912 0.1778
14 1 0 -0.7790 -0.0898
14 1 1 2.5827 0.2499
14 1 2 1.6719 -0.0362
14 1 3 1.3308 -0.1264
14 1 4 1.3075 0.0422
14 1 5 2.3909 -0.0749
14 1 6 -1.8172 0.2429
14 1 7 4.1597 0.2069
14 1 8 -1.2040 0.4228
14 1 9 3.0615 -0.1568
14 2 0 -0.3544 0.2623
14 2 1 2.9210 0.2897
14 2 2 -1.0958 0.1168
14 2 3 3.3687 0.5202
14 2 4 1.4760 -0.0380
14 2 5 0.2207 0.2634
14 2 6 0.2747 -0.2636
14 2 7 2.1096 0.2089
14 2 8 -1.3768 -0.0204
14 2 9 2.9369 0.1274
14 3 0 3.6301 0.1266
14 3 1 -5.2210 0.0489
14 3 2 0.1538 0.1277
14 3 3 -1.6442 0.0147
14 3 4 0.6777 0.3700
14 3 5 -1.4591 0.0455
14 3 6 0.8328 0.3369
14 3 7 -3.3287 -0.0425
14 3 8 -1.4374 0.1619
14 3 9 1.0809 0.0760
14 4 0 -3.7493 -0.0520
14 4 1 -8.0178 0.1355
14 4 2 -5.0039 0.0592
14 4 3 -7.4780 0.0835
14 4 4 -7.7223 0.1082
14 4 5 -0.1714 0.0908
14 4 6 -4.5214 0.0956
14 4 7 3.1520 0.2924
14 4 8 -3.7361 -0.0701
14 4 9 2.7952 0.2718
14 5 0 -1.1405 -0.0375
14 5 1 4.4584 -0.0877
14 5 2 3.2315 -0.0772
14 5 3 2.2163 0.1675
14 5 4 1.4580 0.0219
14 5 5 -1.2062 0.1342
14 5 6 -1.4324 0.2294
14 5 7 1.2009 0.1112
14 5 8 -2.4024 0.0406
14 6 0 -0.0729 -0.0076
14 6 1 1.2331 0.3202
14 6 2 0.1322 -0.0313
14 6 3 3.4131 0.2259
14 6 4 4.9769 -0.1257
14 6 5 2.7626 0.0962
14 6 6 3.7878 0.2503
14 6 7 0.7616 -0.2543
14 6 8 -0.8888 0.3049
14 7 0 4.9041 -0.0259
14 7 1 2.7186 -0.0713
14 7 2 0.7962 0.1067
14 7 3 2.3988 -0.0341
14 7 4 -1.5946 -0.0702
14 7 5 4.1579 0.1256
14 7 6 1.6263 -0.2675
14 7 7 2.4344 0.2119
14 8 0 -0.9979 -0.0589
14 8 1 1.6236 -0.1019
14 8 2 0.4843 -0.1444
14 8 3 0.8061 0.0578
14 8 4 -1.6690 -0.0391
14 8 5 -2.3159 0.1948
14 8 6 -2.2145 -0.2679
14 8 7 -5.5615 0.2616
14 9 0 -0.6986 -0.1019
14 9 1 -4.4367 -0.0911
14 9 2 0.3676 -0.1068
14 9 3 -7.9349 -0.1790
14 9 4 1.5550 0.0041
14 9 5 -9.3697 -0.1804
14 9 6 -0.0110 0.2082
14 10 0 -4.0833 0.0675
14 10 1 0.5847 0.0365
14 10 2 -1.7757 0.1936
14 10 3 1.0405 -0.0215
14 10 4 1.2172 0.0999
14 10 5 1.4908 0.0165
14 11 0 -0.7683 0.0668
14 11 1 2.5746 -0.1329
14 11 2 -1.9988 -0.0510
14 11 3 2.2488 -0.2514
14 11 4 1.7044 -0.2439
14 12 0 0.6579 0.0692
14 12 1 1.3272 0.0161
14 12 2 1.5301 0.1232
14 12 3 0.7781 -0.0196
14 13 0 -1.0980 -0.1512
14 13 1 0.6057 0.0591
14 14 0 -0.9858 0.0010
15 0 0 1.4370 -3.0109
15 0 2 -0.8408 -2.0821
15 0 4 -2.4114 -0.9641
15 0 6 0.2320 -0.1565
15 0 8 0.6818 0.1341
15 1 0 2.2374 -0.0919
15 1 1 1.1427 0.0907
15 1 2 3.3751 -0.1832
15 1 3 0.9406 -0.1316
15 1 4 1.1032 -0.0965
15 1 5 2.8746 0.2658
15 1 6 -0.2904 0.3137
15 1 7 1.9022 0.0074
15 1 8 2.1973 0.3256
15 2 0 -0.7669 0.2126
15 2 1 3.3081 0.4358
15 2 2 0.2078 0.1888
15 2 3 0.8164 0.4755
15 2 4 -0.1427 -0.2240
15 2 5 1.2456 0.3665
15 2 6 -1.9324 -0.1303
15 2 7 3.9550 0.3551
15 3 0 2.4659 0.0290
15 3 1 -2.4591 -0.0194
15 3 2 1.9736 0.2936
15 3 3 -0.3476 0.1467
15 3 4 3.0140 0.4312
15 3 5 -3.4059 0.1110
15 3 6 0.9294 0.1114
15 3 7 -0.5431 0.0818
15 4 0 -4.1599 -0.0451
15 4 1 -9.4267 0.0710
15 4 2 -7.8089 0.0037
15 4 3 -3.9643 -0.0700
15 4 4 -5.7585 0.2137
15 4 5 1.6736 0.2101
15 4 6 -4.4161 0.0413
15 4 7 1.2814 0.2977
15 5 0 0.0583 -0.0331
15 5 1 3.0985 0.1499
15 5 2 -0.1699 -0.0510
15 5 3 -0.9974 0.1753
15 5 4 -3.7565 0.1738
15 5 5 -0.4178 0.0577
15 5 6 -3.5457 0.1230
15 5 7 0.1547 0.3454
15 6 0 -1.5006 0.0685
15 6 1 0.8447 0.1818
15 6 2 2.9052 -0.0730
15 6 3 1.5817 0.2209
15 6 4 3.4284 0.1130
15 6 5 -0.1281 -0.1760
15 6 6 0.5111 0.4648
15 7 0 1.4984 0.0886
15 7 1 1.9276 -0.0063
15 7 2 -1.6526 0.0564
15 7 3 2.5293 0.1093
15 7 4 -1.1492 -0.2524
15 7 5 2.7428 0.2329
15 8 0 -1.5456 -0.0696
15 8 1 0.3543 0.0371
15 8 2 -1.6484 0.0446
15 8 3 -1.9038 0.2067
15 8 4 -2.5077 -0.1201
15 8 5 -5.2917 0.3949
15 9 0 -1.0626 -0.1987
15 9 1 -6.5283 -0.0956
15 9 2 -0.5438 -0.0225
15 9 3 -9.0655 -0.0217
15 9 4 0.4098 0.2318
15 10 0 -1.4861 0.1888
15 10 1 -2.2233 -0.0003
15 10 2 0.7220 0.2113
15 10 3 -2.9160 0.0197
15 11 0 -3.3217 -0.0567
15 11 1 1.5957 -0.0290
15 11 2 -1.4505 -0.2486
15 12 0 1.6932 0.1724
15 12 1 0.7194 -0.0497
16 0 0 -0.6072 -2.8610
16 0 2 -2.0465 -2.0253
16 0 4 -1.1064 -0.9154
16 0 6 0.8294 -0.2309
16 1 0 3.4062 -0.1928
16 1 1 0.5744 -0.0303
16 1 2 3.1879 -0.3925
16 1 3 2.1186 0.1582
16 1 4 1.3042 -0.0310
16 1 5 1.3830 0.1211
16 1 6 2.5947 0.1832
16 2 0 0.1076 0.2975
16 2 1 1.0506 0.4285
16 2 2 -0.5931 -0.0414
16 2 3 0.0933 0.3976
16 2 4 -1.9610 -0.2910
16 2 5 3.4375 0.4615
16 2 6 -2.1999 0.1968
16 3 0 3.8221 0.0339
16 3 1 2.0040 0.0949
16 3 2 4.8894 0.3614
16 3 3 -0.2276 0.2315
16 3 4 2.4998 0.0655
16 3 5 0.3097 0.0812
16 4 0 -4.2101 -0.1327
16 4 1 -6.7114 -0.1948
16 4 2 -3.1554 0.1005
16 4 3 -0.5367 -0.0327
16 4 4 -1.0303 0.1376
16 4 5 -0.1364 0.2086
16 5 0 -0.9484 -0.0931
16 5 1 0.7662 0.2180
16 5 2 -5.0249 -0.0026
16 5 3 -0.1864 -0.0394
16 5 4 -4.4363 0.1654
16 5 5 0.6518 0.2277
16 6 0 1.8605 -0.0017
16 6 1 0.2669 0.1141
16 6 2 3.2914 -0.0130
16 6 3 -0.7273 -0.0598
16 6 4 1.6503 0.3461
16 7 0 0.2855 0.0920
16 7 1 2.0311 -0.0249
16 7 2 -0.8280 -0.1557
16 7 3 1.9678 0.2188
16 7 4 -1.4853 -0.0537
16 8 0 -3.3471 0.0919
16 8 1 0.3113 0.1460
16 8 2 -1.9239 -0.0006
16 8 3 -3.0852 0.2726
16 9 0 -2.0643 -0.1391
16 9 1 -8.6918 0.0410
16 9 2 -1.1276 0.1655
16 10 0 0.1699 0.1513
16 10 1 -5.7971 -0.0862
16 11 0 -3.6747 -0.2365
17 0 0 -1.7366 -2.7679
17 0 2 -1.7626 -1.8682
17 0 4 1.2438 -0.8990
17 1 0 2.7995 -0.3640
17 1 1 1.0361 0.1929
17 1 2 2.3574 -0.2814
17 1 3 1.2359 0.1917
17 1 4 2.5657 -0.0196
17 2 0 -1.9634 0.1521
17 2 1 -1.3109 0.3378
17 2 2 -3.0405 -0.2365
17 2 3 2.0404 0.4200
17 2 4 -2.8314 0.0155
17 3 0 6.2032 0.2000
17 3 1 2.8585 0.2378
17 3 2 3.9657 0.0342
17 3 3 2.1444 0.1258
17 4 0 0.0335 -0.1059
17 4 1 -2.0443 -0.1837
17 4 2 3.8171 0.0848
17 4 3 -0.6824 0.0757
17 5 0 -4.0748 -0.0694
17 5 1 0.2776 -0.0910
17 5 2 -3.8404 0.1113
17 5 3 0.7614 -0.0037
17 6 0 2.9739 -0.0956
17 6 1 -0.0561 0.0175
17 6 2 1.4363 0.0564
17 7 0 3.8206 -0.0034
17 7 1 1.2879 0.0393
17 7 2 0.1941 -0.0196
17 8 0 -1.6865 0.0209
17 8 1 3.3056 0.1079
17 9 0 -2.0026 0.1524
18 0 0 -2.1824 -2.5698
18 0 2 0.3226 -1.7202
18 1 0 1.8502 -0.1809
18 1 1 0.4677 0.3235
18 1 2 1.5847 -0.0493
18 2 0 -5.5729 -0.1115
18 2 1 -0.7222 0.3748
18 2 2 -5.3248 0.1069
18 3 0 3.9899 0.0732
18 3 1 2.0971 0.1555
18 4 0 5.9858 -0.0669
18 4 1 -1.7771 0.1161
18 5 0 -4.2755 0.0899
18 5 1 -0.6973 -0.2117
18 6 0 -0.8600 -0.1512
19 0 0 0.1023 -2.4057
19 1 0 0.4061 0.2068
19 2 0 -6.5559 0.2672
0 0 0 0.0 0.0
;
_shelx_fab_checksum 38733
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0259(3) 0.5715(3) 0.23696(19) 0.0149(11) Uani 1 1 d . . . . .
C2 C 0.1050(3) 0.5700(3) 0.2952(2) 0.0162(11) Uani 1 1 d . . . . .
C3 C 0.1693(3) 0.6219(3) 0.32036(19) 0.0173(11) Uani 1 1 d . . . . .
H3 H 0.166679 0.667406 0.301325 0.021 Uiso 1 1 calc R . . . .
C4 C 0.2403(3) 0.6003(3) 0.3780(2) 0.0180(12) Uani 1 1 d . . . . .
C5 C 0.2249(3) 0.5332(3) 0.3939(2) 0.0322(15) Uani 1 1 d . . . . .
H5 H 0.264389 0.510287 0.431311 0.039 Uiso 1 1 calc R . . . .
C6 C 0.3190(3) 0.6437(3) 0.4172(2) 0.0196(12) Uani 1 1 d . . . . .
C7 C 0.3224(3) 0.7231(3) 0.4110(2) 0.0233(12) Uani 1 1 d . . . . .
H7 H 0.274424 0.749831 0.379085 0.028 Uiso 1 1 calc R . . . .
C8 C 0.3962(3) 0.7633(3) 0.4516(2) 0.0292(14) Uani 1 1 d . . . . .
H8 H 0.398205 0.817313 0.446942 0.035 Uiso 1 1 calc R . . . .
C9 C 0.4662(3) 0.7258(4) 0.4983(2) 0.0374(16) Uani 1 1 d . . . . .
H9 H 0.515762 0.754103 0.526318 0.045 Uiso 1 1 calc R . . . .
C10 C 0.4643(3) 0.6474(4) 0.5044(2) 0.0379(16) Uani 1 1 d . . . . .
H10 H 0.512793 0.621098 0.536163 0.045 Uiso 1 1 calc R . . . .
C11 C 0.3912(3) 0.6067(3) 0.4641(2) 0.0298(14) Uani 1 1 d . . . . .
H11 H 0.390350 0.552373 0.468569 0.036 Uiso 1 1 calc R . . . .
C12 C -0.0806(3) 0.6083(3) 0.13828(19) 0.0214(12) Uani 1 1 d . . . . .
C13 C -0.1097(3) 0.5350(3) 0.1522(2) 0.0233(13) Uani 1 1 d . . . . .
C14 C -0.0460(3) 0.5910(3) 0.1079(2) 0.0340(14) Uani 1 1 d . . . . .
H14A H -0.004253 0.549879 0.128967 0.051 Uiso 1 1 calc GR . . . .
H14B H -0.020161 0.637635 0.107100 0.051 Uiso 1 1 calc GR . . . .
H14C H -0.091152 0.574049 0.067712 0.051 Uiso 1 1 calc GR . . . .
C15 C -0.1448(3) 0.6727(3) 0.1074(2) 0.0337(15) Uani 1 1 d . . . . .
H15A H -0.195389 0.653614 0.069998 0.051 Uiso 1 1 calc GR . . . .
H15B H -0.122259 0.716264 0.100344 0.051 Uiso 1 1 calc GR . . . .
H15C H -0.158218 0.689790 0.132012 0.051 Uiso 1 1 calc GR . . . .
C16 C -0.1432(3) 0.4696(3) 0.1080(2) 0.0325(15) Uani 1 1 d . . . . .
H16A H -0.190478 0.488405 0.069062 0.049 Uiso 1 1 calc GR . . . .
H16B H -0.161489 0.426945 0.119166 0.049 Uiso 1 1 calc GR . . . .
H16C H -0.099332 0.451383 0.107464 0.049 Uiso 1 1 calc GR . . . .
C17 C -0.1695(3) 0.5536(3) 0.1634(2) 0.0337(15) Uani 1 1 d . . . . .
H17A H -0.147943 0.597372 0.190452 0.051 Uiso 1 1 calc GR . . . .
H17B H -0.175070 0.508445 0.180557 0.051 Uiso 1 1 calc GR . . . .
H17C H -0.224025 0.567011 0.126359 0.051 Uiso 1 1 calc GR . . . .
C18 C -0.1424(3) 0.3481(3) 0.2655(2) 0.0264(13) Uani 1 1 d . . . . .
C19 C -0.0872(3) 0.3650(3) 0.3255(2) 0.0279(13) Uani 1 1 d . . . . .
H19 H -0.108097 0.376671 0.345248 0.034 Uiso 1 1 calc R . . . .
C20 C -0.0014(3) 0.3645(3) 0.3562(2) 0.0246(13) Uani 1 1 d . . . . .
C21 C -0.2359(4) 0.3467(4) 0.2350(3) 0.0442(17) Uani 1 1 d . . . . .
C22 C 0.0563(4) 0.3818(4) 0.4222(3) 0.0396(16) Uani 1 1 d . . . . .
C23 C 0.0005(3) 0.1711(3) 0.1702(2) 0.0224(12) Uani 1 1 d . . . . .
C24 C -0.0709(3) 0.1928(3) 0.1155(2) 0.0264(13) Uani 1 1 d . . . . .
H24 H -0.083576 0.169374 0.081643 0.032 Uiso 1 1 calc R . . . .
C25 C -0.1243(3) 0.2483(3) 0.1090(2) 0.0189(12) Uani 1 1 d . . . . .
C26 C 0.0556(3) 0.1091(3) 0.1728(2) 0.0314(14) Uani 1 1 d . . . . .
C27 C -0.2014(3) 0.2656(3) 0.0452(2) 0.0263(13) Uani 1 1 d . . . . .
C28 C 0.1948(3) 0.3175(3) 0.3040(2) 0.0240(13) Uani 1 1 d . . . . .
C29 C 0.1822(3) 0.3350(3) 0.2533(2) 0.0236(13) Uani 1 1 d . . . . .
H29 H 0.228631 0.336717 0.254380 0.028 Uiso 1 1 calc R . . . .
C30 C 0.1031(3) 0.3501(3) 0.2009(2) 0.0211(12) Uani 1 1 d . . . . .
C31 C 0.2830(3) 0.3075(4) 0.3615(2) 0.0325(14) Uani 1 1 d . . . . .
C32 C 0.0954(3) 0.3653(3) 0.1472(2) 0.0300(14) Uani 1 1 d . . . . .
C33 C 0.5324(3) 0.3204(3) 0.2593(2) 0.0155(11) Uani 1 1 d . . . . .
C34 C 0.5169(3) 0.3231(3) 0.2049(2) 0.0151(11) Uani 1 1 d . . . . .
C35 C 0.4783(3) 0.3795(3) 0.16273(19) 0.0171(11) Uani 1 1 d . . . . .
H35 H 0.452774 0.423776 0.164195 0.020 Uiso 1 1 calc R . . . .
C36 C 0.4804(3) 0.3651(3) 0.1172(2) 0.0166(11) Uani 1 1 d . . . . .
C37 C 0.5214(3) 0.2976(3) 0.1263(2) 0.0189(12) Uani 1 1 d . . . . .
H37 H 0.528848 0.278457 0.099954 0.023 Uiso 1 1 calc R . . . .
C38 C 0.4430(3) 0.4148(3) 0.0649(2) 0.0171(11) Uani 1 1 d . . . . .
C39 C 0.4315(3) 0.4935(3) 0.0671(2) 0.0274(13) Uani 1 1 d . . . . .
H39 H 0.443931 0.515358 0.101283 0.033 Uiso 1 1 calc R . . . .
C40 C 0.4019(3) 0.5400(3) 0.0193(2) 0.0321(14) Uani 1 1 d . . . . .
H40 H 0.394636 0.593785 0.021118 0.039 Uiso 1 1 calc R . . . .
C41 C 0.3827(3) 0.5091(3) -0.0307(2) 0.0316(14) Uani 1 1 d . . . . .
H41 H 0.362448 0.541422 -0.063221 0.038 Uiso 1 1 calc R . . . .
C42 C 0.3932(3) 0.4311(3) -0.0334(2) 0.0272(13) Uani 1 1 d . . . . .
H42 H 0.380444 0.409498 -0.067719 0.033 Uiso 1 1 calc R . . . .
C43 C 0.4223(3) 0.3842(3) 0.0140(2) 0.0257(13) Uani 1 1 d . . . . .
H43 H 0.428215 0.330213 0.011582 0.031 Uiso 1 1 calc R . . . .
C44 C 0.5982(3) 0.2817(3) 0.35631(19) 0.0152(11) Uani 1 1 d . . . . .
C45 C 0.5412(3) 0.3520(3) 0.3412(2) 0.0178(11) Uani 1 1 d . . . . .
C46 C 0.6884(3) 0.3050(3) 0.3870(2) 0.0250(13) Uani 1 1 d . . . . .
H46A H 0.689069 0.346638 0.364873 0.038 Uiso 1 1 calc GR . . . .
H46B H 0.718944 0.260305 0.388945 0.038 Uiso 1 1 calc GR . . . .
H46C H 0.714873 0.323047 0.426646 0.038 Uiso 1 1 calc GR . . . .
C47 C 0.5924(3) 0.2158(3) 0.3874(2) 0.0240(13) Uani 1 1 d . . . . .
H47A H 0.603638 0.235526 0.422730 0.036 Uiso 1 1 calc GR . . . .
H47B H 0.633507 0.176042 0.398177 0.036 Uiso 1 1 calc GR . . . .
H47C H 0.536467 0.193409 0.361257 0.036 Uiso 1 1 calc GR . . . .
C48 C 0.5807(3) 0.4163(3) 0.3854(2) 0.0307(14) Uani 1 1 d . . . . .
H48A H 0.601412 0.395976 0.423407 0.046 Uiso 1 1 calc GR . . . .
H48B H 0.539322 0.456715 0.372656 0.046 Uiso 1 1 calc GR . . . .
H48C H 0.627135 0.438183 0.389082 0.046 Uiso 1 1 calc GR . . . .
C49 C 0.4573(3) 0.3286(3) 0.3234(2) 0.0277(13) Uani 1 1 d . . . . .
H49A H 0.434288 0.285258 0.295880 0.042 Uiso 1 1 calc GR . . . .
H49B H 0.418868 0.372544 0.304737 0.042 Uiso 1 1 calc GR . . . .
H49C H 0.464828 0.312992 0.358261 0.042 Uiso 1 1 calc GR . . . .
C50 C 0.6750(3) 0.0534(3) 0.2672(2) 0.0235(13) Uani 1 1 d . . . . .
C51 C 0.7223(3) 0.0375(3) 0.3267(2) 0.0254(13) Uani 1 1 d . . . . .
H51 H 0.780642 0.030552 0.349641 0.031 Uiso 1 1 calc R . . . .
C52 C 0.6874(3) 0.0315(3) 0.3537(2) 0.0233(13) Uani 1 1 d . . . . .
C53 C 0.7169(4) 0.0539(4) 0.2403(3) 0.0389(16) Uani 1 1 d . . . . .
C54 C 0.7450(4) 0.0097(3) 0.4186(3) 0.0379(16) Uani 1 1 d . . . . .
C55 C 0.2950(3) 0.0332(3) 0.1727(2) 0.0186(12) Uani 1 1 d . . . . .
C56 C 0.2968(3) 0.0587(3) 0.2174(2) 0.0235(12) Uani 1 1 d . . . . .
H56 H 0.245753 0.063494 0.210383 0.028 Uiso 1 1 calc R . . . .
C57 C 0.3703(3) 0.0778(3) 0.2723(2) 0.0229(12) Uani 1 1 d . . . . .
C58 C 0.2096(3) 0.0138(3) 0.1134(2) 0.0358(15) Uani 1 1 d D U . . .
C59 C 0.3638(4) 0.0988(4) 0.3187(3) 0.0498(18) Uani 1 1 d D U . . .
C60 C 0.3742(3) 0.1441(3) 0.0983(2) 0.0217(12) Uani 1 1 d . . . . .
C61 C 0.3270(3) 0.1971(3) 0.1011(2) 0.0252(13) Uani 1 1 d . . . . .
H61 H 0.281665 0.222333 0.066412 0.030 Uiso 1 1 calc R . . . .
C62 C 0.3447(3) 0.2137(3) 0.1533(2) 0.0240(13) Uani 1 1 d . . . . .
C63 C 0.3540(3) 0.1321(3) 0.0388(2) 0.0328(14) Uani 1 1 d D . . . .
C64 C 0.2907(3) 0.2746(3) 0.1531(2) 0.0252(13) Uani 1 1 d . . . . .
F1 F -0.2550(2) 0.3718(2) 0.26681(17) 0.0792(15) Uani 1 1 d . . . . .
F2 F -0.26333(19) 0.2747(2) 0.21892(16) 0.0603(11) Uani 1 1 d . . . . .
F3 F -0.2791(2) 0.3874(3) 0.18595(19) 0.0805(14) Uani 1 1 d . . . . .
F4 F 0.0185(2) 0.4110(3) 0.44052(15) 0.0755(13) Uani 1 1 d . . . . .
F5 F 0.0922(3) 0.3174(2) 0.45232(15) 0.0842(15) Uani 1 1 d . . . . .
F6 F 0.1159(2) 0.4296(3) 0.43843(14) 0.0848(15) Uani 1 1 d . . . . .
F7 F -0.24924(16) 0.32069(17) 0.04074(12) 0.0336(8) Uani 1 1 d . . . . .
F8 F -0.17928(17) 0.28635(18) 0.01368(12) 0.0392(8) Uani 1 1 d . . . . .
F9 F -0.24944(16) 0.20171(16) 0.01944(11) 0.0284(7) Uani 1 1 d . . . . .
F10 F 0.1325(2) 0.1330(2) 0.20324(17) 0.0648(12) Uani 1 1 d . . . . .
F11 F 0.0585(2) 0.04606(18) 0.19952(15) 0.0532(10) Uani 1 1 d . . . . .
F12 F 0.0293(2) 0.0862(2) 0.12114(14) 0.0601(11) Uani 1 1 d . . . . .
F13 F 0.30064(19) 0.3615(2) 0.39976(14) 0.0628(12) Uani 1 1 d . . . . .
F14 F 0.34101(18) 0.3130(2) 0.35583(15) 0.0622(12) Uani 1 1 d . . . . .
F15 F 0.29400(18) 0.2403(2) 0.38615(14) 0.0555(11) Uani 1 1 d . . . . .
F16 F 0.16563(19) 0.38822(19) 0.15883(14) 0.0470(9) Uani 1 1 d . . . . .
F17 F 0.0733(2) 0.3007(2) 0.11587(14) 0.0605(11) Uani 1 1 d . . . . .
F18 F 0.0386(2) 0.4175(2) 0.11277(17) 0.0831(15) Uani 1 1 d . . . . .
F19 F 0.6944(2) 0.1135(2) 0.20570(17) 0.0613(11) Uani 1 1 d . . . . .
F20 F 0.7994(2) 0.0511(3) 0.27858(17) 0.0767(14) Uani 1 1 d . . . . .
F21 F 0.6935(2) -0.0091(2) 0.20626(18) 0.0682(12) Uani 1 1 d . . . . .
F22 F 0.7470(2) 0.0653(2) 0.44965(13) 0.0657(12) Uani 1 1 d . . . . .
F23 F 0.8226(2) -0.0053(3) 0.44134(15) 0.0748(14) Uani 1 1 d . . . . .
F24 F 0.7182(2) -0.0528(2) 0.42799(13) 0.0524(10) Uani 1 1 d . . . . .
F25A F 0.1733(6) 0.0849(4) 0.0853(4) 0.055(3) Uani 0.496(13) 1 d D U P A 1
F25B F 0.1505(5) 0.0542(7) 0.1007(4) 0.071(4) Uani 0.504(13) 1 d D U P A 2
F26A F 0.2128(8) 0.0095(7) 0.0709(5) 0.049(3) Uani 0.504(13) 1 d D U P A 2
F26B F 0.2124(7) -0.0253(6) 0.0781(5) 0.053(4) Uani 0.496(13) 1 d D U P A 1
F27A F 0.1567(5) -0.0137(8) 0.1184(3) 0.056(4) Uani 0.496(13) 1 d D U P A 1
F27B F 0.1927(5) -0.0630(5) 0.1179(3) 0.055(3) Uani 0.504(13) 1 d D U P A 2
F28A F 0.4250(6) 0.1407(6) 0.3616(5) 0.0436(16) Uani 0.583(7) 1 d D U P B 2
F28B F 0.4302(8) 0.1296(7) 0.3666(6) 0.041(2) Uani 0.417(7) 1 d D U P B 1
F29A F 0.3794(3) 0.0253(3) 0.3502(2) 0.0436(16) Uani 0.583(7) 1 d D . P B 2
F29B F 0.3189(5) 0.0583(5) 0.3232(3) 0.041(2) Uani 0.417(7) 1 d D . P B 1
F30A F 0.3092(4) 0.1728(5) 0.2931(3) 0.041(2) Uani 0.417(7) 1 d D . P B 1
F30B F 0.2939(3) 0.1179(4) 0.3027(2) 0.0436(16) Uani 0.583(7) 1 d D . P B 2
F31A F 0.4201(3) 0.1395(4) 0.04340(18) 0.075(2) Uani 0.892(8) 1 d D U P C 1
F31B F 0.4020(16) 0.0785(14) 0.0399(12) 0.029(9) Uani 0.108(8) 1 d D U P C 2
F32A F 0.3249(4) 0.0620(3) 0.01949(18) 0.076(2) Uani 0.892(8) 1 d D U P C 1
F32B F 0.2771(11) 0.1092(18) -0.0045(11) 0.032(10) Uani 0.108(8) 1 d D U P C 2
F33A F 0.363(2) 0.1960(11) 0.0179(12) 0.038(10) Uani 0.108(8) 1 d D U P C 2
F33B F 0.2969(3) 0.1797(3) -0.00200(19) 0.080(2) Uani 0.892(8) 1 d D U P C 1
F34 F 0.33256(17) 0.33985(17) 0.17851(13) 0.0382(8) Uani 1 1 d . . . . .
F35 F 0.22177(18) 0.29350(18) 0.09964(13) 0.0464(9) Uani 1 1 d . . . . .
F36 F 0.26767(18) 0.24960(18) 0.18332(14) 0.0447(9) Uani 1 1 d . . . . .
Tb1 Tb -0.00533(2) 0.30996(2) 0.24594(2) 0.01481(7) Uani 1 1 d . . . . .
Tb2 Tb 0.49146(2) 0.07946(2) 0.23614(2) 0.01491(7) Uani 1 1 d . . . . .
N1 N -0.0288(2) 0.5121(2) 0.20988(17) 0.0191(10) Uani 1 1 d . . . . .
N2 N -0.0084(2) 0.6318(2) 0.19969(16) 0.0168(9) Uani 1 1 d . . . . .
N3 N 0.5636(2) 0.2594(2) 0.29602(16) 0.0157(9) Uani 1 1 d . . . . .
N4 N 0.5230(2) 0.3780(2) 0.28517(16) 0.0163(9) Uani 1 1 d . . . . .
O1 O -0.01933(19) 0.44765(17) 0.23513(13) 0.0225(8) Uani 1 1 d . . . . .
O2 O 0.02332(18) 0.70049(17) 0.21237(13) 0.0197(8) Uani 1 1 d . . . . .
O3 O -0.12644(18) 0.33164(18) 0.23289(14) 0.0195(8) Uani 1 1 d . . . . .
O4 O 0.03592(18) 0.35009(18) 0.33728(13) 0.0189(8) Uani 1 1 d . . . . .
O5 O 0.02826(18) 0.19593(18) 0.21935(14) 0.0181(8) Uani 1 1 d . . . . .
O6 O -0.11843(18) 0.28514(18) 0.14734(13) 0.0185(8) Uani 1 1 d . . . . .
O7 O 0.13998(18) 0.30931(19) 0.30958(14) 0.0213(8) Uani 1 1 d . . . . .
O8 O 0.03611(19) 0.35106(19) 0.19169(14) 0.0220(8) Uani 1 1 d . . . . .
O9 O 0.57856(18) 0.19195(17) 0.28519(13) 0.0171(8) Uani 1 1 d . . . . .
O10 O 0.49041(18) 0.44447(17) 0.26155(13) 0.0194(8) Uani 1 1 d . . . . .
O11 O 0.5980(2) 0.06600(18) 0.23141(14) 0.0216(8) Uani 1 1 d . . . . .
O12 O 0.61345(19) 0.04182(17) 0.33179(13) 0.0198(8) Uani 1 1 d . . . . .
O13 O 0.44315(19) 0.07769(18) 0.28904(13) 0.0210(8) Uani 1 1 d . . . . .
O14 O 0.35648(19) 0.02406(18) 0.17409(14) 0.0225(8) Uani 1 1 d . . . . .
O15 O 0.43297(19) 0.10321(18) 0.13844(13) 0.0201(8) Uani 1 1 d . . . . .
O16 O 0.40183(18) 0.18723(18) 0.20310(13) 0.0184(8) Uani 1 1 d . . . . .
S1 S 0.13018(8) 0.49437(8) 0.34170(6) 0.0344(4) Uani 1 1 d . . . . .
S2 S 0.55783(7) 0.25117(7) 0.18899(5) 0.0200(3) Uani 1 1 d . . . . .
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
C1 0.011(3) 0.013(3) 0.017(3) -0.004(2) 0.007(2) 0.002(2)
C2 0.022(3) 0.008(2) 0.020(3) -0.001(2) 0.014(2) 0.002(2)
C3 0.020(3) 0.012(3) 0.019(3) 0.002(2) 0.012(2) 0.001(2)
C4 0.016(3) 0.017(3) 0.017(3) -0.001(2) 0.009(2) 0.001(2)
C5 0.018(3) 0.028(3) 0.017(3) 0.007(3) -0.004(3) -0.010(2)
C6 0.019(3) 0.023(3) 0.012(3) 0.001(2) 0.008(2) -0.001(2)
C7 0.022(3) 0.023(3) 0.026(3) -0.003(2) 0.016(3) -0.004(2)
C8 0.031(3) 0.028(3) 0.037(3) -0.007(3) 0.025(3) -0.012(3)
C9 0.023(3) 0.060(4) 0.023(3) -0.008(3) 0.012(3) -0.021(3)
C10 0.023(3) 0.056(4) 0.022(3) 0.008(3) 0.008(3) -0.007(3)
C11 0.022(3) 0.031(3) 0.025(3) 0.004(3) 0.010(3) -0.002(3)
C12 0.026(3) 0.018(3) 0.008(3) -0.002(2) 0.005(2) -0.004(2)
C13 0.023(3) 0.014(3) 0.019(3) 0.000(2) 0.007(3) 0.002(2)
C14 0.043(4) 0.032(3) 0.022(3) -0.005(3) 0.019(3) -0.004(3)
C15 0.027(3) 0.018(3) 0.021(3) 0.006(2) -0.001(3) -0.001(2)
C16 0.032(3) 0.022(3) 0.016(3) -0.005(2) 0.003(3) -0.005(3)
C17 0.018(3) 0.029(3) 0.040(4) -0.003(3) 0.012(3) -0.006(3)
C18 0.024(3) 0.015(3) 0.034(3) -0.001(3) 0.016(3) 0.000(2)
C19 0.028(3) 0.028(3) 0.042(4) -0.010(3) 0.029(3) -0.003(3)
C20 0.039(4) 0.012(3) 0.029(3) 0.000(2) 0.025(3) -0.003(2)
C21 0.035(4) 0.040(4) 0.069(5) -0.011(4) 0.039(4) -0.002(3)
C22 0.049(4) 0.047(4) 0.028(4) -0.007(3) 0.027(3) -0.001(3)
C23 0.026(3) 0.018(3) 0.028(3) -0.001(2) 0.019(3) 0.001(2)
C24 0.028(3) 0.026(3) 0.020(3) -0.008(2) 0.013(3) 0.004(2)
C25 0.016(3) 0.020(3) 0.014(3) -0.002(2) 0.006(2) -0.009(2)
C26 0.031(4) 0.030(3) 0.027(3) 0.000(3) 0.016(3) 0.014(3)
C27 0.027(3) 0.025(3) 0.026(3) -0.005(3) 0.017(3) -0.008(3)
C28 0.014(3) 0.017(3) 0.034(3) -0.006(2) 0.012(3) -0.002(2)
C29 0.018(3) 0.027(3) 0.026(3) -0.001(3) 0.014(3) -0.004(2)
C30 0.031(3) 0.009(3) 0.031(3) 0.000(2) 0.023(3) 0.000(2)
C31 0.020(3) 0.043(4) 0.031(3) -0.003(3) 0.014(3) 0.000(3)
C32 0.033(4) 0.033(3) 0.032(3) 0.007(3) 0.025(3) 0.002(3)
C33 0.017(3) 0.012(3) 0.017(3) -0.001(2) 0.011(2) -0.002(2)
C34 0.015(3) 0.019(3) 0.013(3) -0.001(2) 0.010(2) -0.003(2)
C35 0.018(3) 0.013(3) 0.021(3) -0.002(2) 0.012(2) 0.000(2)
C36 0.015(3) 0.017(3) 0.018(3) -0.004(2) 0.010(2) -0.001(2)
C37 0.024(3) 0.015(3) 0.019(3) -0.003(2) 0.014(2) -0.004(2)
C38 0.013(3) 0.019(3) 0.016(3) -0.002(2) 0.008(2) -0.004(2)
C39 0.039(3) 0.025(3) 0.013(3) 0.002(2) 0.014(3) -0.001(3)
C40 0.038(4) 0.024(3) 0.027(3) 0.004(3) 0.017(3) 0.004(3)
C41 0.033(3) 0.036(4) 0.018(3) 0.008(3) 0.013(3) -0.002(3)
C42 0.025(3) 0.038(4) 0.018(3) 0.004(3) 0.014(3) 0.005(3)
C43 0.028(3) 0.025(3) 0.026(3) -0.002(3) 0.018(3) 0.001(2)
C44 0.024(3) 0.015(3) 0.008(2) -0.001(2) 0.010(2) -0.003(2)
C45 0.031(3) 0.014(3) 0.013(3) 0.000(2) 0.016(2) -0.002(2)
C46 0.026(3) 0.026(3) 0.015(3) -0.003(2) 0.010(3) -0.008(2)
C47 0.033(3) 0.015(3) 0.017(3) 0.004(2) 0.013(3) 0.001(2)
C48 0.054(4) 0.020(3) 0.023(3) 0.002(2) 0.027(3) 0.003(3)
C49 0.033(3) 0.022(3) 0.032(3) 0.008(3) 0.022(3) 0.006(2)
C50 0.027(3) 0.014(3) 0.039(3) 0.006(3) 0.026(3) 0.001(2)
C51 0.018(3) 0.029(3) 0.027(3) 0.006(3) 0.013(3) 0.005(2)
C52 0.026(3) 0.013(3) 0.022(3) 0.002(2) 0.012(3) 0.004(2)
C53 0.045(4) 0.038(4) 0.052(4) 0.023(3) 0.040(4) 0.016(3)
C54 0.031(4) 0.028(3) 0.037(4) 0.004(3) 0.013(3) 0.010(3)
C55 0.029(3) 0.013(3) 0.019(3) 0.001(2) 0.018(3) -0.004(2)
C56 0.021(3) 0.031(3) 0.021(3) -0.001(2) 0.015(3) -0.001(2)
C57 0.032(3) 0.024(3) 0.024(3) -0.001(2) 0.023(3) 0.001(3)
C58 0.035(2) 0.037(2) 0.036(2) -0.0012(17) 0.0228(17) -0.0012(17)
C59 0.048(2) 0.057(3) 0.052(2) -0.0040(17) 0.0357(18) -0.0036(17)
C60 0.024(3) 0.020(3) 0.015(3) -0.003(2) 0.010(3) -0.011(2)
C61 0.022(3) 0.025(3) 0.020(3) 0.008(2) 0.009(3) 0.008(2)
C62 0.025(3) 0.014(3) 0.035(3) -0.003(3) 0.020(3) -0.003(2)
C63 0.038(4) 0.036(4) 0.023(3) -0.001(3) 0.018(3) 0.003(3)
C64 0.032(3) 0.025(3) 0.027(3) 0.004(3) 0.022(3) 0.005(3)
F1 0.043(2) 0.117(4) 0.099(3) -0.057(3) 0.055(2) -0.018(2)
F2 0.044(2) 0.061(3) 0.091(3) -0.037(2) 0.050(2) -0.0260(19)
F3 0.037(2) 0.093(3) 0.098(3) 0.022(3) 0.037(2) 0.023(2)
F4 0.069(3) 0.121(4) 0.042(2) -0.023(2) 0.038(2) 0.012(3)
F5 0.116(4) 0.063(3) 0.030(2) 0.012(2) 0.027(2) 0.029(3)
F6 0.088(3) 0.131(4) 0.035(2) -0.049(3) 0.039(2) -0.075(3)
F7 0.0219(18) 0.0318(18) 0.0229(17) -0.0023(14) 0.0031(15) 0.0075(14)
F8 0.0343(19) 0.050(2) 0.0266(18) 0.0097(16) 0.0163(16) -0.0058(16)
F9 0.0269(17) 0.0275(17) 0.0177(15) -0.0068(14) 0.0082(14) -0.0072(14)
F10 0.032(2) 0.058(3) 0.106(3) -0.024(2) 0.045(2) 0.0002(19)
F11 0.078(3) 0.028(2) 0.072(3) 0.0154(19) 0.057(2) 0.0249(18)
F12 0.065(3) 0.074(3) 0.037(2) -0.002(2) 0.031(2) 0.035(2)
F13 0.031(2) 0.074(3) 0.039(2) -0.019(2) 0.0017(18) 0.0018(19)
F14 0.020(2) 0.115(4) 0.049(2) 0.014(2) 0.0208(18) 0.003(2)
F15 0.025(2) 0.055(2) 0.054(2) 0.024(2) 0.0099(18) 0.0103(17)
F16 0.054(2) 0.052(2) 0.059(2) -0.0008(19) 0.047(2) -0.0106(18)
F17 0.086(3) 0.069(3) 0.043(2) -0.024(2) 0.049(2) -0.035(2)
F18 0.099(3) 0.114(4) 0.084(3) 0.080(3) 0.081(3) 0.082(3)
F19 0.080(3) 0.056(3) 0.100(3) 0.036(2) 0.082(3) 0.027(2)
F20 0.031(2) 0.137(4) 0.073(3) 0.020(3) 0.038(2) 0.013(2)
F21 0.101(3) 0.054(3) 0.107(3) -0.010(2) 0.093(3) 0.006(2)
F22 0.081(3) 0.042(2) 0.0231(18) -0.0068(17) 0.009(2) 0.018(2)
F23 0.029(2) 0.131(4) 0.043(2) 0.035(2) 0.0137(19) 0.034(2)
F24 0.065(3) 0.046(2) 0.0307(19) 0.0141(18) 0.0235(19) 0.0009(19)
F25A 0.035(5) 0.048(5) 0.037(5) 0.008(4) 0.001(3) 0.001(4)
F25B 0.029(5) 0.087(7) 0.058(6) -0.027(5) 0.010(4) 0.020(5)
F26A 0.045(5) 0.069(7) 0.030(4) -0.010(5) 0.023(4) -0.024(5)
F26B 0.036(5) 0.052(6) 0.041(6) -0.027(5) 0.011(4) 0.003(5)
F27A 0.038(5) 0.083(8) 0.037(4) -0.002(4) 0.020(4) -0.034(5)
F27B 0.040(5) 0.040(5) 0.051(5) -0.006(4) 0.014(4) -0.023(4)
F28A 0.044(2) 0.056(2) 0.040(2) -0.0077(14) 0.0310(16) -0.0029(13)
F28B 0.046(3) 0.046(3) 0.038(3) -0.0074(16) 0.0300(19) -0.0046(16)
F29A 0.044(2) 0.056(2) 0.040(2) -0.0077(14) 0.0310(16) -0.0029(13)
F29B 0.046(3) 0.046(3) 0.038(3) -0.0074(16) 0.0300(19) -0.0046(16)
F30A 0.046(3) 0.046(3) 0.038(3) -0.0074(16) 0.0300(19) -0.0046(16)
F30B 0.044(2) 0.056(2) 0.040(2) -0.0077(14) 0.0310(16) -0.0029(13)
F31A 0.065(3) 0.135(5) 0.045(3) -0.017(3) 0.045(3) -0.020(3)
F31B 0.032(10) 0.032(10) 0.027(10) 0.000(4) 0.020(7) 0.004(4)
F32A 0.127(5) 0.057(3) 0.033(3) -0.022(2) 0.046(3) -0.028(3)
F32B 0.031(12) 0.046(14) 0.025(12) -0.008(8) 0.021(9) -0.009(8)
F33A 0.051(14) 0.026(12) 0.028(12) -0.006(8) 0.021(9) -0.011(9)
F33B 0.096(4) 0.097(4) 0.039(3) 0.033(3) 0.039(3) 0.052(3)
F34 0.039(2) 0.0248(18) 0.045(2) -0.0045(16) 0.0248(17) 0.0083(15)
F35 0.032(2) 0.049(2) 0.0337(19) 0.0048(17) 0.0093(17) 0.0234(16)
F36 0.053(2) 0.040(2) 0.068(2) 0.0225(19) 0.051(2) 0.0224(17)
Tb1 0.01282(14) 0.01141(12) 0.01722(13) -0.00022(10) 0.00821(11) -0.00011(10)
Tb2 0.01762(14) 0.01149(12) 0.01731(13) 0.00006(10) 0.01194(12) 0.00048(10)
N1 0.014(2) 0.011(2) 0.022(2) 0.0000(19) 0.007(2) 0.0007(18)
N2 0.016(2) 0.012(2) 0.017(2) 0.0030(18) 0.0080(19) 0.0021(18)
N3 0.023(2) 0.013(2) 0.018(2) -0.0012(18) 0.016(2) 0.0000(18)
N4 0.021(2) 0.010(2) 0.015(2) -0.0030(18) 0.010(2) -0.0027(18)
O1 0.029(2) 0.0084(17) 0.0217(19) 0.0002(15) 0.0122(17) -0.0021(15)
O2 0.020(2) 0.0099(18) 0.0234(19) 0.0016(15) 0.0108(17) -0.0008(15)
O3 0.0151(19) 0.0178(19) 0.026(2) -0.0015(16) 0.0132(17) -0.0005(14)
O4 0.018(2) 0.0164(18) 0.0203(19) -0.0019(15) 0.0115(17) -0.0020(15)
O5 0.0179(19) 0.0153(18) 0.0209(19) 0.0021(16) 0.0123(17) 0.0049(15)
O6 0.0148(19) 0.0176(19) 0.0133(18) -0.0015(15) 0.0044(16) -0.0021(14)
O7 0.0102(19) 0.026(2) 0.024(2) 0.0020(16) 0.0093(17) 0.0036(15)
O8 0.020(2) 0.023(2) 0.023(2) 0.0031(16) 0.0143(18) 0.0008(16)
O9 0.0188(19) 0.0109(17) 0.0205(18) 0.0012(15) 0.0121(16) 0.0017(14)
O10 0.027(2) 0.0067(17) 0.0236(19) 0.0022(15) 0.0154(17) 0.0036(15)
O11 0.025(2) 0.0175(19) 0.029(2) 0.0023(16) 0.0208(18) 0.0055(16)
O12 0.021(2) 0.0130(18) 0.0231(19) 0.0013(15) 0.0131(17) 0.0053(15)
O13 0.022(2) 0.025(2) 0.0210(19) 0.0008(16) 0.0158(17) -0.0009(16)
O14 0.019(2) 0.022(2) 0.028(2) -0.0022(17) 0.0155(18) -0.0006(16)
O15 0.030(2) 0.0174(19) 0.0215(19) 0.0023(16) 0.0206(18) 0.0009(16)
O16 0.0145(19) 0.0177(18) 0.0186(19) 0.0032(16) 0.0086(16) 0.0038(15)
S1 0.0287(9) 0.0205(7) 0.0250(8) 0.0066(6) 0.0038(7) -0.0091(6)
S2 0.0253(8) 0.0168(7) 0.0239(7) 0.0031(6) 0.0185(6) 0.0043(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
N1 C1 C2 125.9(4) . .
N2 C1 C2 126.9(4) . .
N2 C1 N1 107.2(4) . .
C1 C2 S1 120.3(4) . .
C3 C2 C1 127.9(4) . .
C3 C2 S1 111.7(3) . .
C2 C3 H3 123.6 . .
C2 C3 C4 112.8(4) . .
C4 C3 H3 123.6 . .
C3 C4 C6 126.5(4) . .
C5 C4 C3 110.2(4) . .
C5 C4 C6 123.3(4) . .
C4 C5 H5 122.7 . .
C4 C5 S1 114.7(4) . .
S1 C5 H5 122.7 . .
C7 C6 C4 121.5(4) . .
C11 C6 C4 120.2(4) . .
C11 C6 C7 118.1(5) . .
C6 C7 H7 120.0 . .
C8 C7 C6 119.9(5) . .
C8 C7 H7 120.0 . .
C7 C8 H8 119.5 . .
C9 C8 C7 121.0(5) . .
C9 C8 H8 119.5 . .
C8 C9 H9 120.1 . .
C10 C9 C8 119.8(5) . .
C10 C9 H9 120.1 . .
C9 C10 H10 120.1 . .
C9 C10 C11 119.8(5) . .
C11 C10 H10 120.1 . .
C6 C11 H11 119.3 . .
C10 C11 C6 121.4(5) . .
C10 C11 H11 119.3 . .
C14 C12 C13 114.3(4) . .
C14 C12 C15 111.2(4) . .
C15 C12 C13 114.2(4) . .
N2 C12 C13 99.0(4) . .
N2 C12 C14 106.8(4) . .
N2 C12 C15 110.4(4) . .
C16 C13 C12 114.6(4) . .
C17 C13 C12 113.4(4) . .
C17 C13 C16 110.9(4) . .
N1 C13 C12 99.8(4) . .
N1 C13 C16 110.5(4) . .
N1 C13 C17 106.8(4) . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15B 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C13 C16 H16A 109.5 . .
C13 C16 H16B 109.5 . .
C13 C16 H16C 109.5 . .
H16A C16 H16B 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C13 C17 H17A 109.5 . .
C13 C17 H17B 109.5 . .
C13 C17 H17C 109.5 . .
H17A C17 H17B 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C19 C18 C21 117.1(5) . .
O3 C18 C19 128.8(5) . .
O3 C18 C21 114.0(5) . .
C18 C19 H19 120.0 . .
C20 C19 C18 120.0(5) . .
C20 C19 H19 120.0 . .
C19 C20 C22 117.8(5) . .
O4 C20 C19 128.1(5) . .
O4 C20 C22 114.0(5) . .
F1 C21 C18 115.1(5) . .
F1 C21 F2 108.0(5) . .
F1 C21 F3 108.0(5) . .
F2 C21 C18 108.7(5) . .
F3 C21 C18 110.9(5) . .
F3 C21 F2 105.7(5) . .
F4 C22 C20 114.4(5) . .
F4 C22 F5 106.0(5) . .
F5 C22 C20 110.1(5) . .
F6 C22 C20 112.4(5) . .
F6 C22 F4 106.7(5) . .
F6 C22 F5 106.8(5) . .
C24 C23 C26 117.2(5) . .
O5 C23 C24 128.8(5) . .
O5 C23 C26 113.9(4) . .
C23 C24 H24 119.4 . .
C23 C24 C25 121.1(5) . .
C25 C24 H24 119.4 . .
C24 C25 C27 114.8(5) . .
O6 C25 C24 128.9(4) . .
O6 C25 C27 116.2(4) . .
F10 C26 C23 111.2(5) . .
F10 C26 F11 106.2(4) . .
F10 C26 F12 108.4(5) . .
F11 C26 C23 110.4(5) . .
F12 C26 C23 114.1(4) . .
F12 C26 F11 106.0(5) . .
F7 C27 C25 113.1(4) . .
F7 C27 F8 108.2(4) . .
F7 C27 F9 107.0(4) . .
F8 C27 C25 110.9(4) . .
F8 C27 F9 106.6(4) . .
F9 C27 C25 110.6(4) . .
C29 C28 C31 119.8(5) . .
O7 C28 C29 127.4(5) . .
O7 C28 C31 112.8(5) . .
C28 C29 H29 119.3 . .
C28 C29 C30 121.4(5) . .
C30 C29 H29 119.3 . .
C29 C30 C32 117.4(4) . .
O8 C30 C29 128.0(5) . .
O8 C30 C32 114.6(4) . .
F13 C31 C28 110.8(4) . .
F14 C31 C28 113.5(5) . .
F14 C31 F13 106.3(5) . .
F15 C31 C28 112.4(5) . .
F15 C31 F13 106.9(5) . .
F15 C31 F14 106.6(5) . .
F16 C32 C30 114.7(5) . .
F16 C32 F17 105.3(4) . .
F17 C32 C30 110.1(4) . .
F18 C32 C30 111.9(4) . .
F18 C32 F16 107.2(5) . .
F18 C32 F17 107.2(5) . .
N3 C33 C34 125.6(4) . .
N4 C33 C34 127.6(4) . .
N4 C33 N3 106.8(4) . .
C33 C34 S2 119.2(4) . .
C35 C34 C33 129.1(5) . .
C35 C34 S2 111.5(4) . .
C34 C35 H35 123.5 . .
C34 C35 C36 113.1(4) . .
C36 C35 H35 123.5 . .
C35 C36 C38 125.8(4) . .
C37 C36 C35 111.1(4) . .
C37 C36 C38 123.0(4) . .
C36 C37 H37 123.0 . .
C36 C37 S2 114.0(4) . .
S2 C37 H37 123.0 . .
C39 C38 C36 120.4(4) . .
C43 C38 C36 120.6(4) . .
C43 C38 C39 118.9(5) . .
C38 C39 H39 120.2 . .
C40 C39 C38 119.7(5) . .
C40 C39 H39 120.2 . .
C39 C40 H40 119.6 . .
C41 C40 C39 120.9(5) . .
C41 C40 H40 119.6 . .
C40 C41 H41 120.2 . .
C40 C41 C42 119.7(5) . .
C42 C41 H41 120.2 . .
C41 C42 H42 120.1 . .
C41 C42 C43 119.9(5) . .
C43 C42 H42 120.1 . .
C38 C43 H43 119.5 . .
C42 C43 C38 120.9(5) . .
C42 C43 H43 119.5 . .
C46 C44 C45 112.9(4) . .
C47 C44 C45 114.8(4) . .
C47 C44 C46 112.4(4) . .
N3 C44 C45 99.2(3) . .
N3 C44 C46 104.5(4) . .
N3 C44 C47 111.7(4) . .
C48 C45 C44 115.8(4) . .
C48 C45 C49 111.4(4) . .
C48 C45 N4 110.7(4) . .
C49 C45 C44 112.9(4) . .
N4 C45 C44 99.1(4) . .
N4 C45 C49 105.7(4) . .
C44 C46 H46A 109.5 . .
C44 C46 H46B 109.5 . .
C44 C46 H46C 109.5 . .
H46A C46 H46B 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C44 C47 H47A 109.5 . .
C44 C47 H47B 109.5 . .
C44 C47 H47C 109.5 . .
H47A C47 H47B 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C45 C48 H48A 109.5 . .
C45 C48 H48B 109.5 . .
C45 C48 H48C 109.5 . .
H48A C48 H48B 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
C45 C49 H49A 109.5 . .
C45 C49 H49B 109.5 . .
C45 C49 H49C 109.5 . .
H49A C49 H49B 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
C51 C50 C53 119.3(5) . .
O11 C50 C51 126.5(5) . .
O11 C50 C53 114.3(5) . .
C50 C51 H51 118.7 . .
C52 C51 C50 122.5(5) . .
C52 C51 H51 118.7 . .
C51 C52 C54 117.8(5) . .
O12 C52 C51 128.3(5) . .
O12 C52 C54 113.9(5) . .
F19 C53 C50 112.2(5) . .
F19 C53 F20 108.7(5) . .
F19 C53 F21 105.7(5) . .
F20 C53 C50 114.8(5) . .
F20 C53 F21 105.4(5) . .
F21 C53 C50 109.5(5) . .
F22 C54 C52 110.6(4) . .
F22 C54 F23 107.8(5) . .
F22 C54 F24 106.1(5) . .
F23 C54 C52 114.3(5) . .
F23 C54 F24 106.1(5) . .
F24 C54 C52 111.6(5) . .
C56 C55 C58 118.1(4) . .
O14 C55 C56 127.3(5) . .
O14 C55 C58 114.6(4) . .
C55 C56 H56 118.7 . .
C55 C56 C57 122.5(5) . .
C57 C56 H56 118.7 . .
C56 C57 C59 116.9(5) . .
O13 C57 C56 127.7(5) . .
O13 C57 C59 115.3(4) . .
F25A C58 C55 106.2(5) . .
F25B C58 C55 114.9(6) . .
F25B C58 F26A 113.0(8) . .
F25B C58 F27B 107.3(7) . .
F26A C58 C55 112.3(7) . .
F26A C58 F27B 102.1(7) . .
F26B C58 C55 115.2(7) . .
F26B C58 F25A 105.4(7) . .
F26B C58 F27A 112.8(7) . .
F27A C58 C55 113.5(6) . .
F27A C58 F25A 102.3(7) . .
F27B C58 C55 106.0(5) . .
C57 C59 F30A 102.5(5) . .
F28A C59 C57 115.0(8) . .
F28A C59 F29A 100.1(7) . .
F28B C59 C57 116.1(11) . .
F28B C59 F30A 97.8(8) . .
F29A C59 C57 104.9(5) . .
F29B C59 C57 118.3(6) . .
F29B C59 F28B 117.4(10) . .
F29B C59 F30A 98.5(6) . .
F30B C59 C57 118.4(6) . .
F30B C59 F28A 113.6(8) . .
F30B C59 F29A 101.3(6) . .
C61 C60 C63 118.2(5) . .
O15 C60 C61 128.3(5) . .
O15 C60 C63 113.5(5) . .
C60 C61 H61 119.5 . .
C62 C61 C60 121.1(5) . .
C62 C61 H61 119.5 . .
C61 C62 C64 118.1(5) . .
O16 C62 C61 128.6(5) . .
O16 C62 C64 113.3(5) . .
F31A C63 C60 111.6(5) . .
F31A C63 F32A 107.6(5) . .
F31A C63 F33B 108.2(5) . .
F31B C63 C60 114.0(12) . .
F32A C63 C60 109.5(5) . .
F32B C63 C60 115.2(12) . .
F32B C63 F31B 103.9(13) . .
F32B C63 F33A 104.0(14) . .
F33A C63 C60 113.7(13) . .
F33A C63 F31B 104.7(14) . .
F33B C63 C60 113.2(5) . .
F33B C63 F32A 106.4(5) . .
F34 C64 C62 111.3(4) . .
F34 C64 F35 106.6(4) . .
F34 C64 F36 106.5(4) . .
F35 C64 C62 113.6(4) . .
F36 C64 C62 110.8(4) . .
F36 C64 F35 107.6(4) . .
O1 Tb1 O2 143.22(11) . 2_545
O3 Tb1 O1 77.96(11) . .
O3 Tb1 O2 72.81(11) . 2_545
O3 Tb1 O4 72.86(11) . .
O3 Tb1 O5 126.43(11) . .
O3 Tb1 O6 72.65(11) . .
O3 Tb1 O7 147.79(11) . .
O3 Tb1 O8 131.78(11) . .
O4 Tb1 O1 77.65(11) . .
O4 Tb1 O2 72.82(10) . 2_545
O4 Tb1 O5 130.70(11) . .
O4 Tb1 O8 131.84(11) . .
O5 Tb1 O1 144.32(11) . .
O5 Tb1 O2 72.40(11) . 2_545
O6 Tb1 O1 94.31(10) . .
O6 Tb1 O2 97.71(10) . 2_545
O6 Tb1 O4 145.49(11) . .
O6 Tb1 O5 73.17(11) . .
O6 Tb1 O8 73.74(11) . .
O7 Tb1 O1 95.59(11) . .
O7 Tb1 O2 97.36(11) . 2_545
O7 Tb1 O4 74.93(11) . .
O7 Tb1 O5 76.10(11) . .
O7 Tb1 O6 139.57(12) . .
O7 Tb1 O8 72.68(11) . .
O8 Tb1 O1 71.18(11) . .
O8 Tb1 O2 145.59(11) . 2_545
O8 Tb1 O5 73.24(11) . .
O10 Tb2 O9 137.29(10) 2_645 .
O10 Tb2 O12 70.56(10) 2_645 .
O10 Tb2 O14 73.24(11) 2_645 .
O10 Tb2 O16 149.51(10) 2_645 .
O11 Tb2 O9 74.72(11) . .
O11 Tb2 O10 76.18(11) . 2_645
O11 Tb2 O12 73.21(11) . .
O11 Tb2 O13 150.99(11) . .
O11 Tb2 O14 128.30(11) . .
O11 Tb2 O15 72.95(11) . .
O11 Tb2 O16 125.95(11) . .
O12 Tb2 O9 71.51(10) . .
O13 Tb2 O9 94.98(11) . .
O13 Tb2 O10 95.58(11) . 2_645
O13 Tb2 O12 77.81(11) . .
O13 Tb2 O14 73.11(11) . .
O13 Tb2 O15 136.06(11) . .
O13 Tb2 O16 73.95(11) . .
O14 Tb2 O9 149.07(10) . .
O14 Tb2 O12 130.36(11) . .
O15 Tb2 O9 101.58(11) . .
O15 Tb2 O10 98.95(11) . 2_645
O15 Tb2 O12 146.08(11) . .
O15 Tb2 O14 71.91(11) . .
O15 Tb2 O16 72.62(11) . .
O16 Tb2 O9 72.95(10) . .
O16 Tb2 O12 131.80(11) . .
O16 Tb2 O14 76.30(10) . .
C1 N1 C13 112.7(4) . .
O1 N1 C1 123.7(4) . .
O1 N1 C13 122.4(4) . .
C1 N2 C12 112.5(4) . .
O2 N2 C1 124.6(4) . .
O2 N2 C12 122.2(4) . .
C33 N3 C44 112.4(4) . .
O9 N3 C33 124.7(4) . .
O9 N3 C44 121.4(4) . .
C33 N4 C45 112.4(4) . .
O10 N4 C33 124.5(4) . .
O10 N4 C45 122.4(4) . .
N1 O1 Tb1 154.1(3) . .
N2 O2 Tb1 130.5(3) . 2
C18 O3 Tb1 135.2(3) . .
C20 O4 Tb1 134.7(3) . .
C23 O5 Tb1 130.7(3) . .
C25 O6 Tb1 132.1(3) . .
C28 O7 Tb1 135.2(3) . .
C30 O8 Tb1 133.9(3) . .
N3 O9 Tb2 131.6(2) . .
N4 O10 Tb2 147.8(3) . 2_655
C50 O11 Tb2 136.2(3) . .
C52 O12 Tb2 132.9(3) . .
C57 O13 Tb2 131.4(3) . .
C55 O14 Tb2 130.6(3) . .
C60 O15 Tb2 134.0(3) . .
C62 O16 Tb2 133.0(3) . .
C5 S1 C2 90.7(2) . .
C37 S2 C34 90.3(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.440(6) .
C1 N1 1.354(5) .
C1 N2 1.347(5) .
C2 C3 1.373(6) .
C2 S1 1.723(5) .
C3 H3 0.9500 .
C3 C4 1.423(6) .
C4 C5 1.366(6) .
C4 C6 1.475(6) .
C5 H5 0.9500 .
C5 S1 1.689(5) .
C6 C7 1.394(6) .
C6 C11 1.393(6) .
C7 H7 0.9500 .
C7 C8 1.391(6) .
C8 H8 0.9500 .
C8 C9 1.376(7) .
C9 H9 0.9500 .
C9 C10 1.372(8) .
C10 H10 0.9500 .
C10 C11 1.388(6) .
C11 H11 0.9500 .
C12 C13 1.570(7) .
C12 C14 1.504(7) .
C12 C15 1.520(6) .
C12 N2 1.501(5) .
C13 C16 1.521(6) .
C13 C17 1.518(7) .
C13 N1 1.501(6) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 C19 1.401(7) .
C18 C21 1.541(7) .
C18 O3 1.243(6) .
C19 H19 0.9500 .
C19 C20 1.397(6) .
C20 C22 1.538(7) .
C20 O4 1.245(6) .
C21 F1 1.313(7) .
C21 F2 1.326(6) .
C21 F3 1.323(7) .
C22 F4 1.313(6) .
C22 F5 1.321(7) .
C22 F6 1.304(7) .
C23 C24 1.381(6) .
C23 C26 1.540(7) .
C23 O5 1.254(6) .
C24 H24 0.9500 .
C24 C25 1.391(7) .
C25 C27 1.541(6) .
C25 O6 1.240(5) .
C26 F10 1.309(6) .
C26 F11 1.328(6) .
C26 F12 1.316(6) .
C27 F7 1.324(6) .
C27 F8 1.333(6) .
C27 F9 1.353(5) .
C28 C29 1.387(7) .
C28 C31 1.523(7) .
C28 O7 1.265(6) .
C29 H29 0.9500 .
C29 C30 1.391(6) .
C30 C32 1.523(7) .
C30 O8 1.242(5) .
C31 F13 1.330(6) .
C31 F14 1.329(6) .
C31 F15 1.314(6) .
C32 F16 1.333(6) .
C32 F17 1.333(6) .
C32 F18 1.311(6) .
C33 C34 1.433(6) .
C33 N3 1.349(5) .
C33 N4 1.347(6) .
C34 C35 1.372(6) .
C34 S2 1.737(5) .
C35 H35 0.9500 .
C35 C36 1.404(6) .
C36 C37 1.369(6) .
C36 C38 1.487(6) .
C37 H37 0.9500 .
C37 S2 1.697(5) .
C38 C39 1.392(6) .
C38 C43 1.385(6) .
C39 H39 0.9500 .
C39 C40 1.386(6) .
C40 H40 0.9500 .
C40 C41 1.377(7) .
C41 H41 0.9500 .
C41 C42 1.377(7) .
C42 H42 0.9500 .
C42 C43 1.384(6) .
C43 H43 0.9500 .
C44 C45 1.555(6) .
C44 C46 1.533(6) .
C44 C47 1.518(6) .
C44 N3 1.491(5) .
C45 C48 1.503(6) .
C45 C49 1.529(6) .
C45 N4 1.518(6) .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C50 C51 1.394(7) .
C50 C53 1.517(7) .
C50 O11 1.256(5) .
C51 H51 0.9500 .
C51 C52 1.390(7) .
C52 C54 1.532(7) .
C52 O12 1.248(5) .
C53 F19 1.312(6) .
C53 F20 1.327(6) .
C53 F21 1.348(7) .
C54 F22 1.315(6) .
C54 F23 1.323(6) .
C54 F24 1.325(6) .
C55 C56 1.376(6) .
C55 C58 1.544(7) .
C55 O14 1.269(5) .
C56 H56 0.9500 .
C56 C57 1.388(6) .
C57 C59 1.513(7) .
C57 O13 1.263(5) .
C58 F25A 1.406(9) .
C58 F25B 1.250(8) .
C58 F26A 1.308(11) .
C58 F26B 1.280(10) .
C58 F27A 1.295(8) .
C58 F27B 1.402(8) .
C59 F28A 1.304(10) .
C59 F28B 1.308(12) .
C59 F29A 1.487(8) .
C59 F29B 1.245(8) .
C59 F30A 1.551(9) .
C59 F30B 1.256(7) .
C60 C61 1.387(7) .
C60 C63 1.548(7) .
C60 O15 1.249(5) .
C61 H61 0.9500 .
C61 C62 1.373(7) .
C62 C64 1.542(7) .
C62 O16 1.253(5) .
C63 F31A 1.304(6) .
C63 F31B 1.350(15) .
C63 F32A 1.313(6) .
C63 F32B 1.324(15) .
C63 F33A 1.340(15) .
C63 F33B 1.312(6) .
C64 F34 1.328(6) .
C64 F35 1.335(5) .
C64 F36 1.331(6) .
Tb1 O1 2.396(3) .
Tb1 O2 2.420(3) 2_545
Tb1 O3 2.331(3) .
Tb1 O4 2.366(3) .
Tb1 O5 2.390(3) .
Tb1 O6 2.346(3) .
Tb1 O7 2.336(3) .
Tb1 O8 2.373(3) .
Tb2 O9 2.415(3) .
Tb2 O10 2.360(3) 2_645
Tb2 O11 2.330(3) .
Tb2 O12 2.396(3) .
Tb2 O13 2.348(3) .
Tb2 O14 2.372(3) .
Tb2 O15 2.357(3) .
Tb2 O16 2.365(3) .
N1 O1 1.286(5) .
N2 O2 1.294(4) .
N3 O9 1.300(4) .
N4 O10 1.291(4) .
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_4
C1 C2 C3 C4 -176.9(4) .
C1 C2 S1 C5 178.0(4) .
C1 N1 O1 Tb1 -121.8(6) .
C1 N2 O2 Tb1 -89.2(5) 2
C2 C1 N1 C13 173.2(4) .
C2 C1 N1 O1 5.7(7) .
C2 C1 N2 C12 166.1(5) .
C2 C1 N2 O2 -4.4(8) .
C2 C3 C4 C5 -1.3(6) .
C2 C3 C4 C6 -179.1(4) .
C3 C2 S1 C5 0.6(4) .
C3 C4 C5 S1 1.8(6) .
C3 C4 C6 C7 23.8(8) .
C3 C4 C6 C11 -160.5(5) .
C4 C5 S1 C2 -1.4(5) .
C4 C6 C7 C8 174.8(5) .
C4 C6 C11 C10 -174.6(5) .
C5 C4 C6 C7 -153.7(5) .
C5 C4 C6 C11 22.0(8) .
C6 C4 C5 S1 179.7(4) .
C6 C7 C8 C9 -0.5(8) .
C7 C6 C11 C10 1.3(8) .
C7 C8 C9 C10 1.7(8) .
C8 C9 C10 C11 -1.4(9) .
C9 C10 C11 C6 -0.1(8) .
C11 C6 C7 C8 -1.0(7) .
C12 C13 N1 C1 21.9(5) .
C12 C13 N1 O1 -170.4(4) .
C12 N2 O2 Tb1 101.1(5) 2
C13 C12 N2 C1 27.5(5) .
C13 C12 N2 O2 -161.7(4) .
C13 N1 O1 Tb1 71.8(8) .
C14 C12 C13 C16 -31.9(6) .
C14 C12 C13 C17 -160.5(4) .
C14 C12 C13 N1 86.2(5) .
C14 C12 N2 C1 -91.4(5) .
C14 C12 N2 O2 79.4(5) .
C15 C12 C13 C16 97.7(5) .
C15 C12 C13 C17 -30.9(6) .
C15 C12 C13 N1 -144.2(4) .
C15 C12 N2 C1 147.6(4) .
C15 C12 N2 O2 -41.5(6) .
C16 C13 N1 C1 143.0(4) .
C16 C13 N1 O1 -49.3(6) .
C17 C13 N1 C1 -96.3(5) .
C17 C13 N1 O1 71.4(5) .
C18 C19 C20 C22 -178.8(5) .
C18 C19 C20 O4 -0.4(8) .
C19 C18 C21 F1 8.9(8) .
C19 C18 C21 F2 -112.4(6) .
C19 C18 C21 F3 131.8(6) .
C19 C18 O3 Tb1 4.6(9) .
C19 C20 C22 F4 -13.6(8) .
C19 C20 C22 F5 105.6(6) .
C19 C20 C22 F6 -135.4(5) .
C19 C20 O4 Tb1 -3.9(8) .
C21 C18 C19 C20 177.7(5) .
C21 C18 O3 Tb1 -173.1(3) .
C22 C20 O4 Tb1 174.6(3) .
C23 C24 C25 C27 -179.6(5) .
C23 C24 C25 O6 0.2(9) .
C24 C23 C26 F10 126.0(5) .
C24 C23 C26 F11 -116.4(5) .
C24 C23 C26 F12 3.0(8) .
C24 C23 O5 Tb1 -16.2(8) .
C24 C25 C27 F7 -177.6(4) .
C24 C25 C27 F8 -55.8(6) .
C24 C25 C27 F9 62.3(6) .
C24 C25 O6 Tb1 18.7(8) .
C26 C23 C24 C25 179.8(5) .
C26 C23 O5 Tb1 162.9(3) .
C27 C25 O6 Tb1 -161.5(3) .
C28 C29 C30 C32 -177.5(5) .
C28 C29 C30 O8 0.7(8) .
C29 C28 C31 F13 116.0(6) .
C29 C28 C31 F14 -3.4(7) .
C29 C28 C31 F15 -124.4(5) .
C29 C28 O7 Tb1 4.0(8) .
C29 C30 C32 F16 -21.6(7) .
C29 C30 C32 F17 96.9(5) .
C29 C30 C32 F18 -144.0(5) .
C29 C30 O8 Tb1 -12.2(8) .
C31 C28 C29 C30 -175.3(5) .
C31 C28 O7 Tb1 -177.0(3) .
C32 C30 O8 Tb1 165.9(3) .
C33 C34 C35 C36 175.1(4) .
C33 C34 S2 C37 -175.7(4) .
C33 N3 O9 Tb2 -87.7(5) .
C33 N4 O10 Tb2 -115.6(5) 2_655
C34 C33 N3 C44 161.1(4) .
C34 C33 N3 O9 -5.2(7) .
C34 C33 N4 C45 177.0(4) .
C34 C33 N4 O10 6.8(7) .
C34 C35 C36 C37 -0.3(6) .
C34 C35 C36 C38 179.1(4) .
C35 C34 S2 C37 -0.6(4) .
C35 C36 C37 S2 -0.2(5) .
C35 C36 C38 C39 25.8(7) .
C35 C36 C38 C43 -156.9(5) .
C36 C37 S2 C34 0.5(4) .
C36 C38 C39 C40 175.6(4) .
C36 C38 C43 C42 -175.2(4) .
C37 C36 C38 C39 -154.9(5) .
C37 C36 C38 C43 22.4(7) .
C38 C36 C37 S2 -179.6(3) .
C38 C39 C40 C41 0.7(8) .
C39 C38 C43 C42 2.1(7) .
C39 C40 C41 C42 0.0(8) .
C40 C41 C42 C43 0.4(8) .
C41 C42 C43 C38 -1.4(8) .
C43 C38 C39 C40 -1.7(7) .
C44 C45 N4 C33 23.4(5) .
C44 C45 N4 O10 -166.2(4) .
C44 N3 O9 Tb2 107.1(4) .
C45 C44 N3 C33 29.7(5) .
C45 C44 N3 O9 -163.5(4) .
C45 N4 O10 Tb2 75.1(6) 2_655
C46 C44 C45 C48 -36.9(6) .
C46 C44 C45 C49 -167.1(4) .
C46 C44 C45 N4 81.5(4) .
C46 C44 N3 C33 -87.0(4) .
C46 C44 N3 O9 79.8(5) .
C47 C44 C45 C48 93.7(5) .
C47 C44 C45 C49 -36.5(6) .
C47 C44 C45 N4 -147.9(4) .
C47 C44 N3 C33 151.2(4) .
C47 C44 N3 O9 -42.0(6) .
C48 C45 N4 C33 145.5(4) .
C48 C45 N4 O10 -44.0(6) .
C49 C45 N4 C33 -93.7(4) .
C49 C45 N4 O10 76.8(5) .
C50 C51 C52 C54 176.9(5) .
C50 C51 C52 O12 -3.3(9) .
C51 C50 C53 F19 -135.1(5) .
C51 C50 C53 F20 -10.4(8) .
C51 C50 C53 F21 107.8(6) .
C51 C50 O11 Tb2 4.6(8) .
C51 C52 C54 F22 118.3(6) .
C51 C52 C54 F23 -3.5(7) .
C51 C52 C54 F24 -123.8(5) .
C51 C52 O12 Tb2 -1.7(8) .
C53 C50 C51 C52 -176.1(5) .
C53 C50 O11 Tb2 -177.2(3) .
C54 C52 O12 Tb2 178.1(3) .
C55 C56 C57 C59 -175.2(5) .
C55 C56 C57 O13 2.6(9) .
C56 C55 C58 F25A 78.7(8) .
C56 C55 C58 F25B 32.7(11) .
C56 C55 C58 F26A 163.7(8) .
C56 C55 C58 F26B -165.1(8) .
C56 C55 C58 F27A -32.9(10) .
C56 C55 C58 F27B -85.6(8) .
C56 C55 O14 Tb2 -22.0(7) .
C56 C57 C59 F28A -157.5(7) .
C56 C57 C59 F28B -168.3(8) .
C56 C57 C59 F29A 93.6(6) .
C56 C57 C59 F29B 43.9(9) .
C56 C57 C59 F30A -63.1(7) .
C56 C57 C59 F30B -18.5(9) .
C56 C57 O13 Tb2 18.6(8) .
C58 C55 C56 C57 -180.0(5) .
C58 C55 O14 Tb2 157.3(3) .
C59 C57 O13 Tb2 -163.5(4) .
C60 C61 C62 C64 178.7(5) .
C60 C61 C62 O16 0.8(9) .
C61 C60 C63 F31A 127.6(6) .
C61 C60 C63 F31B -178.8(15) .
C61 C60 C63 F32A -113.4(6) .
C61 C60 C63 F32B -58.8(17) .
C61 C60 C63 F33A 61.2(17) .
C61 C60 C63 F33B 5.2(8) .
C61 C60 O15 Tb2 6.9(8) .
C61 C62 C64 F34 -107.9(5) .
C61 C62 C64 F35 12.5(7) .
C61 C62 C64 F36 133.8(5) .
C61 C62 O16 Tb2 -15.3(8) .
C63 C60 C61 C62 -176.3(5) .
C63 C60 O15 Tb2 -173.2(3) .
C64 C62 O16 Tb2 166.7(3) .
N1 C1 C2 C3 165.8(5) .
N1 C1 C2 S1 -11.1(7) .
N1 C1 N2 C12 -15.0(5) .
N1 C1 N2 O2 174.4(4) .
N2 C1 C2 C3 -15.5(8) .
N2 C1 C2 S1 167.5(4) .
N2 C1 N1 C13 -5.6(5) .
N2 C1 N1 O1 -173.2(4) .
N2 C12 C13 C16 -145.0(4) .
N2 C12 C13 C17 86.4(5) .
N2 C12 C13 N1 -26.9(4) .
N3 C33 C34 C35 173.0(5) .
N3 C33 C34 S2 -12.8(6) .
N3 C33 N4 C45 -6.0(5) .
N3 C33 N4 O10 -176.2(4) .
N3 C44 C45 C48 -147.1(4) .
N3 C44 C45 C49 82.7(4) .
N3 C44 C45 N4 -28.7(4) .
N4 C33 C34 C35 -10.5(8) .
N4 C33 C34 S2 163.6(4) .
N4 C33 N3 C44 -16.0(5) .
N4 C33 N3 O9 177.7(4) .
O3 C18 C19 C20 0.1(9) .
O3 C18 C21 F1 -173.1(5) .
O3 C18 C21 F2 65.6(7) .
O3 C18 C21 F3 -50.1(7) .
O4 C20 C22 F4 167.8(5) .
O4 C20 C22 F5 -73.1(6) .
O4 C20 C22 F6 45.9(7) .
O5 C23 C24 C25 -1.2(9) .
O5 C23 C26 F10 -53.1(6) .
O5 C23 C26 F11 64.5(6) .
O5 C23 C26 F12 -176.2(5) .
O6 C25 C27 F7 2.6(6) .
O6 C25 C27 F8 124.4(5) .
O6 C25 C27 F9 -117.5(5) .
O7 C28 C29 C30 3.6(8) .
O7 C28 C31 F13 -63.0(6) .
O7 C28 C31 F14 177.6(5) .
O7 C28 C31 F15 56.5(6) .
O8 C30 C32 F16 160.0(4) .
O8 C30 C32 F17 -81.5(6) .
O8 C30 C32 F18 37.6(7) .
O11 C50 C51 C52 2.0(9) .
O11 C50 C53 F19 46.6(7) .
O11 C50 C53 F20 171.3(5) .
O11 C50 C53 F21 -70.5(6) .
O12 C52 C54 F22 -61.5(6) .
O12 C52 C54 F23 176.7(4) .
O12 C52 C54 F24 56.4(6) .
O13 C57 C59 F28A 24.4(8) .
O13 C57 C59 F28B 13.5(10) .
O13 C57 C59 F29A -84.6(6) .
O13 C57 C59 F29B -134.3(7) .
O13 C57 C59 F30A 118.8(5) .
O13 C57 C59 F30B 163.4(6) .
O14 C55 C56 C57 -0.6(8) .
O14 C55 C58 F25A -100.8(7) .
O14 C55 C58 F25B -146.7(10) .
O14 C55 C58 F26A -15.8(9) .
O14 C55 C58 F26B 15.4(10) .
O14 C55 C58 F27A 147.6(8) .
O14 C55 C58 F27B 94.9(7) .
O15 C60 C61 C62 3.6(9) .
O15 C60 C63 F31A -52.3(7) .
O15 C60 C63 F31B 1.3(16) .
O15 C60 C63 F32A 66.7(6) .
O15 C60 C63 F32B 121.3(16) .
O15 C60 C63 F33A -118.7(17) .
O15 C60 C63 F33B -174.7(5) .
O16 C62 C64 F34 70.3(6) .
O16 C62 C64 F35 -169.3(4) .
O16 C62 C64 F36 -48.0(6) .
S1 C2 C3 C4 0.3(5) .
S2 C34 C35 C36 0.6(5) .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 -0.818 0.000 379.1 36.8
2 0.000 -0.990 0.500 379.1 36.8
3 0.450 0.002 0.908 13.6 0.0
4 0.450 0.498 0.408 13.6 0.0
5 0.550 -0.002 0.092 13.6 0.0
6 0.550 0.502 0.592 13.6 0.0