#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:29:40 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700009.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_7700009
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 'C64 H44 F36 N4 O16 S2 Tb2'
_chemical_formula_sum 'C64 H44 F36 N4 O16 S2 Tb2'
_chemical_formula_weight 2190.99
_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 97.913(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.1897(5)
_cell_length_b 20.9619(7)
_cell_length_c 23.0457(8)
_cell_measurement_reflns_used 12362
_cell_measurement_temperature 120(10)
_cell_measurement_theta_max 29.2117
_cell_measurement_theta_min 2.4744
_cell_volume 8225.0(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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 'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature 120(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -1.00 57.40 0.8000 98.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 37.0000 30.0000 73
#__ type_ start__ end____ width___ exp.time_
2 omega 27.00 74.20 0.8000 98.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 77.0000 30.0000 59
#__ type_ start__ end____ width___ exp.time_
3 omega -75.00 -43.80 0.8000 98.0000
omega____ theta____ kappa____ phi______ frames
- -18.8185 123.0000 -91.0000 39
#__ type_ start__ end____ width___ exp.time_
4 omega -80.00 5.60 0.8000 98.0000
omega____ theta____ kappa____ phi______ frames
- -18.8185 -37.0000 150.0000 107
;
_diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0017501000
_diffrn_orient_matrix_UB_12 -0.0247026000
_diffrn_orient_matrix_UB_13 0.0207592000
_diffrn_orient_matrix_UB_21 0.0041826000
_diffrn_orient_matrix_UB_22 0.0228788000
_diffrn_orient_matrix_UB_23 0.0229344000
_diffrn_orient_matrix_UB_31 -0.0414358000
_diffrn_orient_matrix_UB_32 0.0032486000
_diffrn_orient_matrix_UB_33 -0.0028516000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0357
_diffrn_reflns_av_unetI/netI 0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 31550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.009
_diffrn_reflns_theta_max 25.009
_diffrn_reflns_theta_min 2.479
_diffrn_source 'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 1.901
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.77716
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour 'metallic light green'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.769
_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 0.587
_refine_diff_density_min -0.653
_refine_diff_density_rms 0.102
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.012
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1293
_refine_ls_number_reflns 14485
_refine_ls_number_restraints 504
_refine_ls_restrained_S_all 1.051
_refine_ls_R_factor_all 0.0528
_refine_ls_R_factor_gt 0.0364
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+2.6543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0625
_refine_ls_wR_factor_ref 0.0681
_reflns_Friedel_coverage 0.000
_reflns_number_gt 11500
_reflns_number_total 14485
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file c9dt01704f2.cif
_cod_data_source_block p101229e
_cod_depositor_comments
'Adding full bibliography for 7700008--7700009.cif.'
_cod_database_code 7700009
_shelx_shelxl_version_number 2018/3
_chemical_oxdiff_formula C12TB1
_chemical_oxdiff_usercomment TBL3
_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 0.702
_reflns_odcompleteness_completeness 99.87
_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
F7-F8 = F8-F9 = F7-F9 = F7'-F8' = F8'-F9' = F7'-F9'
2.12 with sigma of 0.02
C38-F7 = C38-F7' = C38-F8 = C38-F8' = C38-F9 = C38-F9'
1.38 with sigma of 0.01
F10-F11 = F11-F12 = F10-F12 = F10'-F11' = F11'-F12' = F10'-F12'
2.12 with sigma of 0.02
C39-F10 = C39-F10' = C39-F11 = C39-F11' = C39-F12 = C39-F12'
1.38 with sigma of 0.01
F13-F14 = F14-F15 = F13-F15 = F13'-F14' = F14'-F15' = F13'-F15'
2.12 with sigma of 0.02
C49-F13 = C49-F14 = C49-F15 = C49-F13' = C49-F14' = C49-F15'
1.38 with sigma of 0.01
F16-F17 = F17-F18 = F16-F18 = F16'-F17' = F17'-F18' = F16'-F18'
2.12 with sigma of 0.02
C48-F16 = C48-F17 = C48-F18 = C48-F16' = C48-F17' = C48-F18'
1.38 with sigma of 0.01
F25-F26 = F26-F27 = F25-F27 = F25'-F26' = F26'-F27' = F25'-F27'
2.12 with sigma of 0.02
C54-F25 = C54-F26 = C54-F27 = C54-F25' = C54-F26' = C54-F27'
1.38 with sigma of 0.01
F28-F29 = F29-F30 = F28-F30 = F28'-F29' = F29'-F30' = F28'-F30'
2.12 with sigma of 0.02
C53-F28 = C53-F29 = C53-F30 = C53-F28' = C53-F29' = C53-F30'
1.38 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F7' \\sim F8' \\sim F9': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
F10 \\sim F11 \\sim F12 \\sim F10' \\sim F11' \\sim F12': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F13 \\sim F14 \\sim F15 \\sim F13' \\sim F14' \\sim F15': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F16 \\sim F17 \\sim F18 \\sim F16' \\sim F17' \\sim F18': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F25 \\sim F26 \\sim F27 \\sim F25' \\sim F26' \\sim F27': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
F28 \\sim F29 \\sim F30 \\sim F28' \\sim F29' \\sim F30': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F25)
\\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F29) \\sim Ueq,
Uanis(F28) \\sim Ueq, Uanis(F30) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim
Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq,
Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F16') \\sim Ueq, Uanis(F17') \\sim Ueq, Uanis(F18') \\sim Ueq,
Uanis(F25') \\sim Ueq, Uanis(F26') \\sim Ueq, Uanis(F27') \\sim Ueq,
Uanis(F29') \\sim Ueq, Uanis(F28') \\sim Ueq, Uanis(F30') \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F7') \\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F10')
\\sim Ueq, Uanis(F11') \\sim Ueq, Uanis(F12') \\sim Ueq, Uanis(F13') \\sim Ueq,
Uanis(F14') \\sim Ueq, Uanis(F15') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(1)
Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
Sof(F10')=Sof(F11')=Sof(F12')=1-FVAR(2)
Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
Sof(F13')=Sof(F14')=Sof(F15')=1-FVAR(3)
Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
Sof(F16')=Sof(F17')=Sof(F18')=1-FVAR(4)
Sof(F16)=Sof(F17)=Sof(F18)=FVAR(4)
Sof(F25')=Sof(F26')=Sof(F27')=1-FVAR(5)
Sof(F25)=Sof(F26)=Sof(F27)=FVAR(5)
Sof(F28')=Sof(F29')=Sof(F30')=1-FVAR(6)
Sof(F28)=Sof(F29)=Sof(F30)=FVAR(6)
5.a Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C20(H20),
C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C36(H36), C41(H41),
C46(H46), C51(H51), C56(H56), C61(H61)
5.b Idealised Me refined as rotating group:
C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c), C17(H17a,H17b,
H17c), C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C34(H34a,
H34b,H34c)
;
_shelx_res_file
;
TITL P101229E in P21/c #14
p101229e.res
created by SHELXL-2018/3 at 11:00:38 on 10-Jan-2019
CELL 0.71073 17.189693 20.961947 23.045665 90 97.9133 90
ZERR 4 0.000532 0.0007 0.000823 0 0.0031 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 2.12 F7 F8 F8 F9 F7 F9 F7' F8' F8' F9' F7' F9'
DFIX 1.38 0.01 C38 F7 C38 F7' C38 F8 C38 F8' C38 F9 C38 F9'
DFIX 2.12 F10 F11 F11 F12 F10 F12 F10' F11' F11' F12' F10' F12'
DFIX 1.38 0.01 C39 F10 C39 F10' C39 F11 C39 F11' C39 F12 C39 F12'
DFIX 2.12 F13 F14 F14 F15 F13 F15 F13' F14' F14' F15' F13' F15'
DFIX 1.38 0.01 C49 F13 C49 F14 C49 F15 C49 F13' C49 F14' C49 F15'
DFIX 2.12 F16 F17 F17 F18 F16 F18 F16' F17' F17' F18' F16' F18'
DFIX 1.38 0.01 C48 F16 C48 F17 C48 F18 C48 F16' C48 F17' C48 F18'
DFIX 2.12 F25 F26 F26 F27 F25 F27 F25' F26' F26' F27' F25' F27'
DFIX 1.38 0.01 C54 F25 C54 F26 C54 F27 C54 F25' C54 F26' C54 F27'
DFIX 2.12 F28 F29 F29 F30 F28 F30 F28' F29' F29' F30' F28' F30'
DFIX 1.38 0.01 C53 F28 C53 F29 C53 F30 C53 F28' C53 F29' C53 F30'
SIMU F7 F8 F9 F7' F8' F9'
SIMU F10 F11 F12 F10' F11' F12'
SIMU F13 F14 F15 F13' F14' F15'
SIMU F16 F17 F18 F16' F17' F18'
SIMU F25 F26 F27 F25' F26' F27'
SIMU F28 F29 F30 F28' F29' F30'
ISOR 0.005 0.01 F16 F17 F18 F25 F26 F27 F29 F28 F30
ISOR 0.005 0.01 F7 F8 F9 F10 F11 F12 F13 F14 F15
ISOR 0.005 0.01 F16' F17' F18' F25' F26' F27' F29' F28' F30'
ISOR 0.005 0.01 F7' F8' F9' F10' F11' F12' F13' F14' F15'
L.S. 5
PLAN 10
SIZE 0.15 0.15 0.2
TEMP -153(10)
BOND
conf
htab 2
fmap 2
acta
ABIN
OMIT -3 50.02
OMIT -20 4 7
REM
REM
REM
WGHT 0.020800 2.654300
FVAR 0.31718 0.57147 0.16525 0.46633 0.71261 0.40558 0.61420
TB1 7 1.136107 0.706605 0.758053 11.00000 0.01047 0.01446 =
0.01795 -0.00246 0.00156 -0.00027
TB2 7 0.636824 0.713449 0.773440 11.00000 0.01097 0.01399 =
0.01273 -0.00194 0.00089 0.00118
C1 1 0.379475 0.685588 0.783948 11.00000 0.01157 0.01657 =
0.01867 0.00069 0.00109 0.00462
C2 1 0.371264 0.653995 0.728641 11.00000 0.01050 0.01615 =
0.01387 -0.00219 0.00002 0.00332
C3 1 0.314529 0.611749 0.705398 11.00000 0.01338 0.01473 =
0.02056 0.00153 0.00293 0.00140
AFIX 43
H3 2 0.272189 0.598523 0.725052 11.00000 -1.20000
AFIX 0
C4 1 0.325545 0.590191 0.649744 11.00000 0.01578 0.01335 =
0.02610 0.00044 -0.00064 -0.00130
AFIX 43
H4 2 0.291322 0.560849 0.627581 11.00000 -1.20000
AFIX 0
C5 1 0.390898 0.615736 0.630325 11.00000 0.02093 0.01289 =
0.01812 -0.00279 -0.00116 -0.00005
C6 1 0.422432 0.604368 0.574960 11.00000 0.02285 0.01174 =
0.01817 -0.00116 0.00425 0.00229
C7 1 0.374951 0.580439 0.526507 11.00000 0.02738 0.01672 =
0.01902 -0.00240 -0.00005 -0.00509
AFIX 43
H7 2 0.320793 0.573343 0.528475 11.00000 -1.20000
AFIX 0
C8 1 0.404904 0.566699 0.475360 11.00000 0.04336 0.02131 =
0.01606 -0.00552 -0.00098 -0.00312
AFIX 43
H8 2 0.371639 0.549290 0.442883 11.00000 -1.20000
AFIX 0
C9 1 0.483204 0.578187 0.471213 11.00000 0.04367 0.02483 =
0.01796 0.00051 0.01058 0.00789
AFIX 43
H9 2 0.504139 0.567991 0.436294 11.00000 -1.20000
AFIX 0
C10 1 0.530503 0.604553 0.518212 11.00000 0.02761 0.03123 =
0.02776 0.00037 0.01153 0.00237
AFIX 43
H10 2 0.583740 0.614208 0.515005 11.00000 -1.20000
AFIX 0
C11 1 0.501206 0.617143 0.570144 11.00000 0.02378 0.03030 =
0.02042 -0.00791 -0.00025 -0.00290
AFIX 43
H11 2 0.534678 0.634485 0.602546 11.00000 -1.20000
AFIX 0
C12 1 0.358900 0.712496 0.880908 11.00000 0.01372 0.03354 =
0.01755 -0.00728 -0.00113 -0.00203
C13 1 0.297061 0.749363 0.908072 11.00000 0.02310 0.04111 =
0.02288 -0.01403 0.00586 0.00048
AFIX 137
H13A 2 0.274175 0.782210 0.880626 11.00000 -1.50000
H13B 2 0.321344 0.769619 0.944433 11.00000 -1.50000
H13C 2 0.255724 0.720071 0.916702 11.00000 -1.50000
AFIX 0
C14 1 0.385304 0.653678 0.917907 11.00000 0.03153 0.04613 =
0.02349 0.00145 0.00256 -0.00050
AFIX 137
H14A 2 0.340477 0.625014 0.918944 11.00000 -1.50000
H14B 2 0.405718 0.667037 0.957861 11.00000 -1.50000
H14C 2 0.426606 0.631355 0.900587 11.00000 -1.50000
AFIX 0
C15 1 0.427210 0.753289 0.863520 11.00000 0.01060 0.02520 =
0.01726 -0.01058 0.00054 0.00273
C16 1 0.402812 0.821288 0.845078 11.00000 0.02167 0.02904 =
0.02528 -0.01328 -0.00166 -0.00348
AFIX 137
H16A 2 0.355059 0.819989 0.816461 11.00000 -1.50000
H16B 2 0.445110 0.841789 0.827419 11.00000 -1.50000
H16C 2 0.392635 0.845658 0.879535 11.00000 -1.50000
AFIX 0
C17 1 0.501803 0.753532 0.907638 11.00000 0.01474 0.04476 =
0.02289 -0.01316 -0.00259 -0.00095
AFIX 137
H17A 2 0.490352 0.771384 0.944843 11.00000 -1.50000
H17B 2 0.541883 0.779606 0.892542 11.00000 -1.50000
H17C 2 0.521180 0.709763 0.913921 11.00000 -1.50000
AFIX 0
C18 1 0.876361 0.736704 0.755702 11.00000 0.01136 0.01438 =
0.01620 -0.00135 0.00230 -0.00068
C19 1 0.889229 0.766328 0.811748 11.00000 0.01351 0.01534 =
0.01448 0.00101 0.00232 -0.00102
C20 1 0.952292 0.760246 0.854831 11.00000 0.01658 0.02868 =
0.01963 -0.00867 0.00119 0.00116
AFIX 43
H20 2 0.994671 0.731702 0.852477 11.00000 -1.20000
AFIX 0
C21 1 0.947576 0.800614 0.902701 11.00000 0.01756 0.03254 =
0.01229 -0.00254 -0.00299 -0.00193
AFIX 43
H21 2 0.986045 0.801668 0.936495 11.00000 -1.20000
AFIX 0
C22 1 0.881605 0.838584 0.895838 11.00000 0.01357 0.02004 =
0.01274 -0.00175 0.00192 -0.00427
C23 1 0.856187 0.885600 0.936846 11.00000 0.02238 0.01644 =
0.01729 0.00054 0.00282 -0.00084
C24 1 0.910805 0.916220 0.977356 11.00000 0.02567 0.02338 =
0.02368 -0.00400 -0.00183 -0.00016
AFIX 43
H24 2 0.965220 0.907703 0.978134 11.00000 -1.20000
AFIX 0
C25 1 0.886144 0.959181 1.016662 11.00000 0.04597 0.03009 =
0.02208 -0.00680 -0.00263 0.00075
AFIX 43
H25 2 0.923847 0.980214 1.044143 11.00000 -1.20000
AFIX 0
C26 1 0.807586 0.971655 1.016258 11.00000 0.05393 0.02815 =
0.02780 -0.00965 0.01091 0.00943
AFIX 43
H26 2 0.791224 1.000439 1.044034 11.00000 -1.20000
AFIX 0
C27 1 0.752627 0.942663 0.975843 11.00000 0.03368 0.02706 =
0.03722 -0.00359 0.01106 0.00884
AFIX 43
H27 2 0.698440 0.952077 0.975108 11.00000 -1.20000
AFIX 0
C28 1 0.776381 0.899734 0.936227 11.00000 0.02314 0.02807 =
0.02639 -0.00404 0.00084 0.00307
AFIX 43
H28 2 0.738287 0.879657 0.908362 11.00000 -1.20000
AFIX 0
C29 1 0.894187 0.677591 0.670400 11.00000 0.01271 0.02542 =
0.01475 -0.00797 -0.00003 -0.00244
C30 1 0.952521 0.681277 0.625872 11.00000 0.01968 0.03881 =
0.02164 -0.01426 0.00482 -0.00277
AFIX 137
H30A 2 0.973147 0.724797 0.624962 11.00000 -1.50000
H30B 2 0.925785 0.669851 0.586931 11.00000 -1.50000
H30C 2 0.995940 0.651542 0.637245 11.00000 -1.50000
AFIX 0
C31 1 0.873571 0.608200 0.681648 11.00000 0.02772 0.02396 =
0.02483 -0.00512 0.00192 -0.00034
AFIX 137
H31A 2 0.853673 0.587538 0.644405 11.00000 -1.50000
H31B 2 0.833180 0.606796 0.707769 11.00000 -1.50000
H31C 2 0.920636 0.585752 0.699986 11.00000 -1.50000
AFIX 0
C32 1 0.821961 0.722151 0.656883 11.00000 0.01203 0.02262 =
0.01511 -0.00355 0.00249 -0.00193
C33 1 0.840296 0.785771 0.629909 11.00000 0.02873 0.02463 =
0.01986 -0.00032 0.00129 -0.00496
AFIX 137
H33A 2 0.794719 0.814081 0.628608 11.00000 -1.50000
H33B 2 0.852332 0.778746 0.590055 11.00000 -1.50000
H33C 2 0.885639 0.805434 0.653703 11.00000 -1.50000
AFIX 0
C34 1 0.750164 0.690736 0.623323 11.00000 0.01721 0.02391 =
0.01410 -0.00497 -0.00388 -0.00254
AFIX 137
H34A 2 0.763571 0.673095 0.586585 11.00000 -1.50000
H34B 2 0.708287 0.722448 0.614654 11.00000 -1.50000
H34C 2 0.732159 0.656328 0.647006 11.00000 -1.50000
AFIX 0
C35 1 0.594752 0.571383 0.826008 11.00000 0.01815 0.02371 =
0.02786 0.00162 0.00602 0.00241
C36 1 0.616690 0.535364 0.779885 11.00000 0.03281 0.01363 =
0.03103 -0.00383 0.01153 -0.00055
AFIX 43
H36 2 0.622592 0.490501 0.784374 11.00000 -1.20000
AFIX 0
C37 1 0.629978 0.563377 0.728016 11.00000 0.01672 0.01939 =
0.02027 -0.00798 -0.00158 0.00076
C38 1 0.648350 0.517888 0.680266 11.00000 0.05473 0.02261 =
0.02435 -0.01069 0.00584 0.00003
C39 1 0.572546 0.535745 0.878340 11.00000 0.06545 0.02666 =
0.04083 0.00267 0.02562 0.00626
C40 1 0.784600 0.631918 0.850062 11.00000 0.01606 0.01939 =
0.02294 0.00306 0.00440 0.00267
C41 1 0.773758 0.654291 0.904657 11.00000 0.02477 0.03230 =
0.01274 0.00379 -0.00236 0.01053
AFIX 43
H41 2 0.800529 0.634391 0.938719 11.00000 -1.20000
AFIX 0
C42 1 0.723622 0.706142 0.910549 11.00000 0.01717 0.02665 =
0.01749 -0.00372 0.00256 -0.00399
C43 1 0.725629 0.730515 0.973505 11.00000 0.02122 0.03304 =
0.01901 -0.00320 -0.00008 -0.00208
C44 1 0.845774 0.579430 0.846691 11.00000 0.02984 0.02730 =
0.02148 -0.00030 -0.00233 0.00815
C45 1 0.565385 0.809521 0.662130 11.00000 0.01031 0.02625 =
0.02496 0.00797 0.00104 -0.00245
C46 1 0.571910 0.866751 0.693007 11.00000 0.03122 0.01972 =
0.02992 0.00643 -0.00366 0.00018
AFIX 43
H46 2 0.555668 0.905204 0.673118 11.00000 -1.20000
AFIX 0
C47 1 0.601131 0.869069 0.751303 11.00000 0.01260 0.01773 =
0.03096 0.00056 0.00302 0.00205
C48 1 0.605719 0.932892 0.782508 11.00000 0.03322 0.02086 =
0.03566 -0.00065 -0.00166 -0.00016
C49 1 0.532825 0.811468 0.597474 11.00000 0.02502 0.03203 =
0.02574 0.00871 0.00116 0.00136
C50 1 1.106466 0.614625 0.873161 11.00000 0.01694 0.03496 =
0.03240 0.00643 0.00468 -0.00256
C51 1 1.109516 0.555601 0.846011 11.00000 0.03584 0.02603 =
0.04474 0.01494 0.01443 0.00270
AFIX 43
H51 2 1.105625 0.517714 0.868049 11.00000 -1.20000
AFIX 0
C52 1 1.118104 0.551353 0.787585 11.00000 0.01913 0.01580 =
0.05017 -0.00097 0.01001 -0.00153
C53 1 1.096689 0.615901 0.937710 11.00000 0.04369 0.03801 =
0.04092 0.01829 0.00969 0.00631
C54 1 1.117478 0.485375 0.758784 11.00000 0.05564 0.02121 =
0.07540 -0.00127 0.03302 -0.00662
C55 1 1.177946 0.701064 0.620632 11.00000 0.01656 0.02698 =
0.01979 -0.00331 0.00233 0.01027
C56 1 1.230223 0.751441 0.624416 11.00000 0.02016 0.02543 =
0.01789 0.00187 0.00544 0.00033
AFIX 43
H56 2 1.248706 0.766421 0.589884 11.00000 -1.20000
AFIX 0
C57 1 1.256123 0.780421 0.677222 11.00000 0.01264 0.01583 =
0.03013 0.00201 0.00123 0.00446
C58 1 1.313640 0.836425 0.676948 11.00000 0.02343 0.02810 =
0.03250 0.00106 0.00576 -0.00487
C59 1 1.152837 0.671181 0.560194 11.00000 0.02774 0.04455 =
0.02760 -0.00714 0.00169 -0.00516
C60 1 1.079516 0.849599 0.701299 11.00000 0.00970 0.02229 =
0.03122 0.00260 0.00565 0.00024
C61 1 1.100652 0.885603 0.752048 11.00000 0.02707 0.01470 =
0.03227 0.00261 0.00199 0.00476
AFIX 43
H61 2 1.098611 0.930842 0.749884 11.00000 -1.20000
AFIX 0
C62 1 1.124457 0.856515 0.805295 11.00000 0.01687 0.01854 =
0.03612 -0.00861 0.00431 -0.00359
C63 1 1.142498 0.898719 0.859939 11.00000 0.03408 0.02398 =
0.03915 -0.01388 0.00566 -0.00612
C64 1 1.059398 0.886188 0.643532 11.00000 0.02773 0.02468 =
0.03940 0.00400 0.00284 -0.00051
F1 3 0.714689 0.683750 1.010867 11.00000 0.04846 0.04274 =
0.01900 0.00249 0.00817 -0.01112
F2 3 0.795126 0.757179 0.992547 11.00000 0.02603 0.04015 =
0.01956 -0.00350 -0.00468 -0.00390
F3 3 0.670885 0.774781 0.977813 11.00000 0.03185 0.05145 =
0.02207 -0.01264 0.00061 0.01414
F4 3 0.870458 0.552507 0.897959 11.00000 0.06424 0.05987 =
0.03210 0.01591 0.00607 0.04509
F5 3 0.909090 0.602819 0.826224 11.00000 0.02024 0.04345 =
0.05153 -0.00094 0.00989 0.00906
F6 3 0.818024 0.533280 0.810015 11.00000 0.03613 0.02325 =
0.06019 -0.00992 -0.00319 0.01043
PART 1
F7 3 0.680496 0.464244 0.697563 21.00000 0.13024 0.03135 =
0.04999 -0.01258 0.02137 0.02560
F8 3 0.683908 0.543757 0.639370 21.00000 0.03429 0.03377 =
0.04177 -0.01529 0.01879 -0.01219
F9 3 0.574308 0.499286 0.650437 21.00000 0.06189 0.05994 =
0.04428 -0.04221 0.01561 -0.02835
PART 0
PART 2
F7' 3 0.724814 0.491931 0.699463 -21.00000 0.06243 0.04754 =
0.03006 -0.01736 0.00260 0.02887
F8' 3 0.660140 0.545357 0.630247 -21.00000 0.04407 0.02903 =
0.01834 -0.01171 0.00416 0.00014
F9' 3 0.606639 0.466852 0.670385 -21.00000 0.07351 0.03040 =
0.05845 -0.02621 0.03230 -0.02880
PART 0
PART 3
F10 3 0.640515 0.502680 0.901039 31.00000 0.05780 0.04501 =
0.03685 0.03131 0.01762 0.01578
F11 3 0.514489 0.492989 0.877173 31.00000 0.12285 0.10548 =
0.09666 0.00921 0.00806 -0.01565
F12 3 0.567129 0.573524 0.925717 31.00000 0.02205 0.02656 =
0.01555 0.00323 0.00850 0.01817
PART 0
PART 4
F10' 3 0.599117 0.476742 0.884484 -31.00000 0.12583 0.03081 =
0.07970 0.03005 0.07104 0.02865
F11' 3 0.492699 0.528298 0.871523 -31.00000 0.05907 0.05421 =
0.05971 0.00215 0.03744 -0.02446
F12' 3 0.590800 0.567409 0.927527 -31.00000 0.07822 0.06205 =
0.03505 0.01041 0.01408 -0.01077
PART 0
PART 5
F13 3 0.568878 0.767073 0.566855 41.00000 0.04230 0.04058 =
0.02277 0.00431 0.00662 0.00352
F14 3 0.457458 0.795609 0.586854 41.00000 0.02127 0.08359 =
0.02976 -0.00008 -0.00027 0.01799
F15 3 0.543675 0.866275 0.570601 41.00000 0.10242 0.05065 =
0.03461 0.02171 -0.00802 -0.00675
PART 0
PART 6
F13' 3 0.584538 0.790822 0.564656 -41.00000 0.03566 0.10851 =
0.01894 0.02179 0.01315 0.02422
F14' 3 0.469380 0.773102 0.585903 -41.00000 0.04091 0.03958 =
0.02916 0.00900 -0.01683 -0.00093
F15' 3 0.506615 0.868707 0.578696 -41.00000 0.07139 0.03355 =
0.03816 0.01357 -0.02426 0.01016
PART 0
PART 7
F16 3 0.575259 0.930092 0.834278 51.00000 0.08016 0.03001 =
0.05966 -0.01118 0.03224 0.00625
F17 3 0.679967 0.949499 0.798256 51.00000 0.03575 0.03703 =
0.07653 -0.02782 -0.00237 -0.00659
F18 3 0.567888 0.981103 0.753980 51.00000 0.06956 0.02382 =
0.06488 -0.01442 -0.02319 0.02131
PART 0
PART 8
F16' 3 0.543276 0.942769 0.808405 -51.00000 0.04689 0.04455 =
0.09290 -0.02845 0.02462 0.01176
F17' 3 0.671743 0.943187 0.818980 -51.00000 0.04102 0.02663 =
0.02651 -0.01228 -0.01737 0.01222
F18' 3 0.606443 0.980398 0.741610 -51.00000 0.08175 0.01106 =
0.04824 0.00305 -0.01129 0.00428
PART 0
F19 3 1.322897 0.856131 0.623481 11.00000 0.05157 0.04600 =
0.03648 0.01246 0.00828 -0.02513
F20 3 1.384593 0.821000 0.703954 11.00000 0.02037 0.04178 =
0.04605 0.00088 0.00174 -0.01027
F21 3 1.289419 0.886445 0.705535 11.00000 0.04080 0.02274 =
0.07402 -0.01329 0.02247 -0.01104
F22 3 1.203719 0.680690 0.523147 11.00000 0.04880 0.11413 =
0.03183 -0.03332 0.02055 -0.02840
F23 3 1.142476 0.608996 0.563069 11.00000 0.12480 0.04743 =
0.03953 -0.02257 -0.00153 -0.02047
F24 3 1.084703 0.694889 0.536074 11.00000 0.04255 0.11077 =
0.03136 -0.02330 -0.01484 0.01985
PART 9
F25 3 1.189817 0.476297 0.744084 61.00000 0.06101 0.03407 =
0.06651 -0.00898 0.03211 -0.00197
F26 3 1.104015 0.435648 0.793466 61.00000 0.04525 0.02032 =
0.08255 0.00617 0.02999 0.00195
F27 3 1.061771 0.478714 0.712082 61.00000 0.08743 0.04473 =
0.07328 -0.01748 0.03056 -0.02035
PART 0
PART 10
F25' 3 1.169264 0.480313 0.719964 -61.00000 0.06320 0.02676 =
0.07242 -0.01462 0.03366 0.00250
F26' 3 1.130429 0.437495 0.797630 -61.00000 0.08279 0.01843 =
0.10609 0.00455 0.02428 -0.00497
F27' 3 1.047137 0.476359 0.726133 -61.00000 0.06727 0.04609 =
0.07744 -0.03325 0.02751 -0.03429
PART 0
PART 11
F28 3 1.166875 0.627311 0.968867 71.00000 0.06409 0.09619 =
0.03293 0.01117 0.00001 -0.00376
F29 3 1.047575 0.661116 0.950494 71.00000 0.08852 0.06155 =
0.04353 0.00416 0.03219 0.01489
F30 3 1.070868 0.560504 0.956779 71.00000 0.07519 0.06053 =
0.04379 0.03148 0.02019 -0.01037
PART 0
PART 12
F28' 3 1.150263 0.654178 0.970273 -71.00000 0.06356 0.07033 =
0.03056 0.00063 0.00234 -0.01346
F29' 3 1.026616 0.641218 0.945084 -71.00000 0.04155 0.06314 =
0.03117 0.00272 0.01928 0.00178
F30' 3 1.102707 0.560032 0.966241 -71.00000 0.07866 0.06106 =
0.04170 0.01522 0.00927 0.00092
PART 0
F31 3 1.218134 0.897036 0.881153 11.00000 0.04112 0.04914 =
0.04991 -0.02357 -0.00706 -0.00208
F32 3 1.125269 0.959229 0.849983 11.00000 0.11118 0.02459 =
0.06645 -0.02197 -0.03159 0.02249
F33 3 1.104751 0.879385 0.902313 11.00000 0.09118 0.08823 =
0.05471 -0.04838 0.04539 -0.05285
F34 3 1.123007 0.891127 0.616858 11.00000 0.04539 0.06586 =
0.04982 0.02705 0.02155 0.01038
F35 3 1.034507 0.945075 0.650472 11.00000 0.06610 0.04017 =
0.05374 0.02305 0.01256 0.02749
F36 3 1.005695 0.856541 0.607524 11.00000 0.07679 0.06607 =
0.04717 0.03229 -0.03593 -0.04180
N1 4 0.325531 0.687540 0.821916 11.00000 0.00935 0.01831 =
0.02544 -0.00240 0.00289 -0.00033
N2 4 0.441959 0.719695 0.808611 11.00000 0.00988 0.01928 =
0.01449 -0.00297 0.00168 0.00148
N3 4 0.809348 0.737668 0.718327 11.00000 0.01451 0.01625 =
0.01584 -0.00056 0.00286 0.00287
N4 4 0.929851 0.705363 0.728263 11.00000 0.01185 0.02210 =
0.01477 -0.00213 0.00240 0.00283
O1 5 1.000156 0.691815 0.751982 11.00000 0.00679 0.02854 =
0.01763 -0.00234 -0.00068 0.00305
O2 5 1.135494 0.797805 0.815818 11.00000 0.01980 0.01741 =
0.02147 -0.00421 0.00046 0.00243
O3 5 1.077258 0.790500 0.696852 11.00000 0.01846 0.01971 =
0.02402 0.00062 0.00053 0.00100
O4 5 1.239696 0.766670 0.727449 11.00000 0.01545 0.01757 =
0.01935 -0.00177 0.00213 -0.00296
O5 5 1.145478 0.676373 0.660966 11.00000 0.01717 0.02147 =
0.02579 -0.00673 0.00511 -0.00326
O6 5 1.125329 0.595698 0.751916 11.00000 0.02064 0.01669 =
0.03390 -0.00299 0.00873 -0.00298
O7 5 1.110319 0.668579 0.851160 11.00000 0.01394 0.02128 =
0.02402 0.00277 0.00334 0.00011
O8 5 0.743693 0.761404 0.730458 11.00000 0.00944 0.02209 =
0.01756 -0.00163 0.00018 0.00265
O9 5 0.501689 0.732661 0.782259 11.00000 0.01019 0.02632 =
0.01917 -0.00312 0.00474 -0.00083
O10 5 0.750698 0.650438 0.800926 11.00000 0.01417 0.01942 =
0.01525 0.00125 0.00026 0.00358
O11 5 0.680241 0.734891 0.872455 11.00000 0.01522 0.02229 =
0.01236 -0.00233 -0.00239 0.00169
O12 5 0.625252 0.823806 0.784903 11.00000 0.01393 0.01425 =
0.02351 -0.00522 -0.00082 -0.00122
O13 5 0.583737 0.754475 0.681346 11.00000 0.01237 0.02239 =
0.01686 0.00123 0.00007 0.00229
O14 5 0.589192 0.630745 0.828495 11.00000 0.02204 0.01706 =
0.02415 -0.00230 0.00750 -0.00031
O15 5 0.628978 0.621189 0.714271 11.00000 0.02188 0.01474 =
0.01609 -0.00219 -0.00034 0.00168
O16 5 0.255043 0.664017 0.811027 11.00000 0.00947 0.02240 =
0.02206 0.00109 0.00204 -0.00220
S1 6 0.823979 0.823517 0.830442 11.00000 0.01486 0.01883 =
0.01716 -0.00437 -0.00017 0.00203
S2 6 0.438979 0.667137 0.680868 11.00000 0.01559 0.02598 =
0.01873 -0.00742 0.00395 -0.00598
HKLF 4
REM P101229E in P21/c #14
REM wR2 = 0.0681, GooF = S = 1.012, Restrained GooF = 1.051 for all data
REM R1 = 0.0364 for 11500 Fo > 4sig(Fo) and 0.0528 for all 14485 data
REM 1293 parameters refined using 504 restraints
END
WGHT 0.0208 2.6577
REM Instructions for potential hydrogen bonds
HTAB C3 O16
EQIV $1 x-1, y, z
HTAB C13 F31_$1
HTAB C13 O2_$1
HTAB C14 F11'
HTAB C17 O11
HTAB C20 O1
HTAB C20 O7
HTAB C30 O3
HTAB C30 O5
EQIV $3 x, -y+3/2, z-1/2
HTAB C33 F2_$3
HTAB C34 F8
HTAB C34 F8'
HTAB C34 O15
EQIV $4 -x+1, y+1/2, -z+3/2
HTAB C46 F11_$4
REM Highest difference peak 0.587, deepest hole -0.653, 1-sigma level 0.102
Q1 1 1.0793 0.9164 0.8644 11.00000 0.05 0.59
Q2 1 0.6116 0.9378 0.7998 11.00000 0.05 0.53
Q3 1 0.5679 0.4806 0.8597 11.00000 0.05 0.52
Q4 1 1.0969 0.6296 0.5568 11.00000 0.05 0.52
Q5 1 0.6730 0.5239 0.9190 11.00000 0.05 0.50
Q6 1 1.1821 0.8782 0.8967 11.00000 0.05 0.50
Q7 1 0.5984 0.5443 0.6302 11.00000 0.05 0.50
Q8 1 0.5995 0.8467 0.5738 11.00000 0.05 0.48
Q9 1 0.6458 0.7594 0.7455 11.00000 0.05 0.47
Q10 1 1.1564 0.6650 0.7347 11.00000 0.05 0.47
;
_shelx_res_checksum 74792
_shelx_fab_file
;
-20 0 2 1.1990 -0.9136
-20 0 4 2.7453 -0.0696
-20 0 6 -0.9343 0.2572
-20 0 8 1.4800 -0.1290
-20 1 1 1.1247 0.5129
-20 1 2 2.3597 -0.2818
-20 1 3 -3.0201 0.5654
-20 1 4 0.2388 -0.1455
-20 1 5 -1.1130 -0.3088
-20 1 6 -3.0010 -0.1448
-20 1 7 -0.3686 0.0529
-20 1 8 -2.6255 -0.0007
-20 1 9 -2.5711 0.1260
-20 2 1 -3.8469 0.4459
-20 2 2 1.4456 -0.5909
-20 2 3 -1.6607 0.4155
-20 2 4 3.5301 0.0016
-20 2 5 4.6762 0.2591
-20 2 6 1.6761 0.1620
-20 2 7 7.7341 0.0947
-20 2 8 3.2984 -0.2447
-20 3 1 -0.2721 0.1144
-20 3 2 2.6062 -0.4456
-20 3 3 -3.9456 0.3246
-20 3 4 -3.7717 -0.3209
-20 3 5 -3.9768 -0.0705
-20 3 6 -11.3347 -0.0822
-20 3 7 -4.2721 0.1537
-20 3 8 -8.9970 -0.0079
-20 4 1 -2.3153 0.1910
-20 4 2 2.5907 -0.2054
-20 4 3 1.4061 0.3042
-20 4 4 4.6525 -0.2497
-20 4 5 10.1652 0.1069
-20 4 6 4.8683 -0.1280
-20 5 3 -3.6891 0.1926
-20 5 4 -5.9599 -0.1217
-20 5 5 -4.4056 0.2425
-19 0 2 -3.4907 0.5649
-19 0 4 -0.1304 0.0448
-19 0 6 1.2696 0.1289
-19 0 8 -0.3342 0.1101
-19 0 10 0.6537 -0.1032
-19 0 12 -2.0956 -0.0486
-19 1 1 3.0206 -0.6167
-19 1 2 1.4578 -0.2331
-19 1 3 2.8490 -0.3357
-19 1 4 3.7207 -0.0780
-19 1 5 -0.8991 -0.0895
-19 1 6 3.7678 -0.0616
-19 1 7 0.1786 -0.2725
-19 1 8 1.3493 -0.1167
-19 1 9 -0.3213 0.0334
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16 11 0 -4.0905 0.1523
16 11 1 -3.1571 -0.0802
16 11 2 -4.2756 0.2729
16 11 3 -0.6662 0.0647
16 11 4 -2.0600 -0.0487
16 11 5 1.5517 -0.1397
16 11 6 1.4080 0.0126
16 11 7 2.4444 0.0836
16 11 8 2.6812 0.0248
16 12 0 5.6830 0.1378
16 12 1 3.0486 -0.2743
16 12 2 2.7846 -0.0540
16 12 3 2.2660 -0.0140
16 12 4 -0.2593 0.0604
16 12 5 -0.6674 0.0563
16 12 6 -1.0884 0.0440
16 12 7 -4.0832 -0.1423
16 13 0 -3.3518 0.1412
16 13 1 -4.3837 0.0189
16 13 2 -2.4064 0.0934
16 13 3 -0.3541 0.1035
16 13 4 -1.5767 -0.0758
16 13 5 -0.0156 0.0055
16 13 6 2.4432 0.1135
16 14 0 4.5894 -0.0515
16 14 1 3.1745 -0.1076
16 14 2 -0.3586 -0.0972
16 14 3 3.2362 0.0221
16 14 4 -1.1892 -0.0170
16 15 0 -3.5030 0.1270
16 15 1 -0.1250 0.0658
17 0 0 -2.3407 -0.8711
17 0 2 -2.2741 -0.8112
17 0 4 -1.7603 0.0097
17 0 6 0.2350 -0.0831
17 0 8 -0.2981 -0.1151
17 0 10 -0.9903 0.1408
17 1 0 0.7004 0.3763
17 1 1 1.9655 0.9668
17 1 2 -0.4952 0.0738
17 1 3 1.5822 0.2844
17 1 4 -1.1985 -0.1384
17 1 5 0.2785 0.0063
17 1 6 -0.8971 -0.1244
17 1 7 -1.0723 0.0739
17 1 8 -0.0774 0.0090
17 1 9 0.1646 -0.1453
17 1 10 0.2801 -0.0515
17 1 11 0.2833 -0.0135
17 2 0 -1.7505 -0.6854
17 2 1 0.6247 -0.4146
17 2 2 -0.4559 -0.4965
17 2 3 2.3897 0.0611
17 2 4 -0.5374 -0.0633
17 2 5 2.7335 0.1236
17 2 6 1.0706 -0.0482
17 2 7 1.6778 -0.0070
17 2 8 1.1323 0.1974
17 2 9 0.4595 -0.0397
17 2 10 -0.0174 0.1340
17 2 11 -0.1976 0.1474
17 3 0 -0.3235 0.4826
17 3 1 -0.2288 0.4589
17 3 2 -2.0807 0.0988
17 3 3 -0.0093 0.0890
17 3 4 -2.7537 -0.1951
17 3 5 0.6456 0.1026
17 3 6 -2.4819 -0.0581
17 3 7 -0.2928 -0.1170
17 3 8 -0.9471 0.0792
17 3 9 0.8273 -0.1834
17 3 10 -0.2997 0.0276
17 3 11 2.0594 0.0864
17 4 0 0.1534 -0.2062
17 4 1 0.9357 -0.1497
17 4 2 1.1039 -0.0570
17 4 3 0.8765 0.1534
17 4 4 -0.7193 -0.0500
17 4 5 0.3948 0.1441
17 4 6 -1.0778 -0.0806
17 4 7 -0.1190 -0.0454
17 4 8 -1.0639 0.1269
17 4 9 -1.1802 -0.1567
17 4 10 -2.5035 -0.1068
17 4 11 -0.5239 -0.0458
17 5 0 -0.7255 0.0202
17 5 1 -1.4590 0.0187
17 5 2 -0.3680 -0.0204
17 5 3 -0.9515 -0.0171
17 5 4 1.4083 -0.1006
17 5 5 0.2854 0.1181
17 5 6 1.8458 0.0092
17 5 7 0.0536 0.0482
17 5 8 2.1613 0.1226
17 5 9 0.2479 0.0380
17 5 10 1.8607 0.1270
17 6 0 1.1840 0.0466
17 6 1 1.0951 -0.0718
17 6 2 1.5367 -0.0151
17 6 3 -0.2325 -0.0504
17 6 4 1.4212 -0.0155
17 6 5 -2.1447 -0.0600
17 6 6 1.1976 -0.0917
17 6 7 -1.6829 -0.0719
17 6 8 1.8233 -0.0446
17 6 9 -1.3994 -0.0522
17 6 10 2.0177 0.1088
17 7 0 -0.1816 0.0461
17 7 1 -0.4576 0.0004
17 7 2 -0.9572 0.1124
17 7 3 -1.3712 -0.0062
17 7 4 0.7919 0.0949
17 7 5 -1.6649 -0.0189
17 7 6 1.4928 0.0981
17 7 7 -1.8662 0.0715
17 7 8 0.0412 0.0102
17 7 9 -2.9380 -0.0724
17 8 0 -1.3446 0.0340
17 8 1 -0.3186 -0.0014
17 8 2 -0.6851 0.0114
17 8 3 0.5532 -0.0290
17 8 4 0.9044 0.0216
17 8 5 -1.0340 -0.0668
17 8 6 0.8801 -0.0742
17 8 7 -0.0487 -0.0491
17 8 8 1.7866 -0.0889
17 8 9 1.1681 0.0116
17 9 0 2.5044 -0.1109
17 9 1 3.0482 -0.0730
17 9 2 -0.5003 -0.0198
17 9 3 0.7040 -0.0254
17 9 4 -0.9141 0.0420
17 9 5 0.1751 0.1212
17 9 6 -0.4510 0.0341
17 9 7 0.1524 0.1536
17 9 8 -1.4236 0.0526
17 10 0 -3.9903 0.0073
17 10 1 -1.5648 0.0476
17 10 2 -1.7180 0.2159
17 10 3 1.5829 -0.1596
17 10 4 -0.5595 -0.0402
17 10 5 2.0707 -0.0429
17 10 6 -1.8403 -0.0774
17 10 7 2.1153 -0.0099
17 11 0 5.4074 -0.1429
17 11 1 1.3692 -0.2714
17 11 2 1.4130 0.1330
17 11 3 -0.2273 -0.2381
17 11 4 -1.2203 0.1509
17 11 5 1.8617 -0.0339
17 11 6 -2.1805 -0.1240
17 12 0 -1.2472 0.0621
17 12 1 -5.2527 0.1717
17 12 2 1.1806 0.3291
17 12 3 -2.3932 -0.1431
17 12 4 -0.5471 0.0989
17 13 0 6.9132 -0.2965
17 13 1 -0.9642 -0.0900
17 13 2 4.6139 0.0029
18 0 0 5.9676 1.9040
18 0 2 3.5205 0.4146
18 0 4 1.3644 -0.0776
18 0 6 0.9367 0.4814
18 0 8 1.8413 -0.0419
18 1 0 0.7219 0.2707
18 1 1 -4.1741 -1.1219
18 1 2 1.5194 0.3879
18 1 3 -2.6099 0.0267
18 1 4 0.9350 0.1420
18 1 5 -1.3437 -0.2171
18 1 6 -0.0850 -0.0147
18 1 7 -2.1307 -0.1999
18 1 8 0.1824 -0.0560
18 1 9 -1.8279 0.0748
18 2 0 2.9167 1.1082
18 2 1 -1.1937 -0.6373
18 2 2 2.9169 0.2001
18 2 3 -0.8332 -0.5354
18 2 4 2.7307 -0.0214
18 2 5 0.9735 -0.1543
18 2 6 2.1611 0.1183
18 2 7 1.9671 -0.0185
18 2 8 2.7586 0.0231
18 2 9 0.1342 -0.0564
18 3 0 0.4752 0.4623
18 3 1 -1.6038 -0.2604
18 3 2 0.4810 0.6509
18 3 3 -2.9447 0.0534
18 3 4 -1.1182 0.3415
18 3 5 -2.3014 -0.0073
18 3 6 -2.8861 0.0454
18 3 7 -1.4130 0.0747
18 3 8 -2.3129 0.0516
18 3 9 -1.3366 -0.2019
18 4 0 0.0974 0.0572
18 4 1 -0.7259 -0.3581
18 4 2 1.4484 -0.0118
18 4 3 0.2833 -0.3446
18 4 4 2.2897 0.0285
18 4 5 1.4583 -0.1020
18 4 6 0.4937 -0.1129
18 4 7 1.7780 -0.0040
18 4 8 -0.3976 0.0238
18 5 0 0.6052 0.0529
18 5 1 -0.1196 0.0360
18 5 2 -0.0466 0.1058
18 5 3 -1.3443 -0.0159
18 5 4 -1.2123 0.1028
18 5 5 -0.9780 0.0219
18 5 6 -0.9069 -0.0243
18 5 7 0.9551 0.0666
18 5 8 0.2659 0.0874
18 6 0 0.5248 -0.1152
18 6 1 0.3678 0.0610
18 6 2 0.5541 -0.0325
18 6 3 2.2620 -0.0037
18 6 4 1.1802 -0.0103
18 6 5 2.7452 0.0536
18 6 6 -0.1144 0.0138
18 6 7 1.1716 0.0819
18 7 0 -0.2466 -0.0382
18 7 1 -0.7809 0.0453
18 7 2 -1.2605 -0.0943
18 7 3 -0.4814 0.0412
18 7 4 -3.9076 -0.1134
18 7 5 -0.5233 -0.0463
18 7 6 -2.9687 -0.2163
18 7 7 1.4959 -0.1534
18 8 0 0.5042 -0.0162
18 8 1 -1.0635 0.1382
18 8 2 -0.7924 -0.0348
18 8 3 1.2994 0.1340
18 8 4 -0.1767 0.0242
18 8 5 2.8891 0.2305
18 8 6 -1.0874 0.0512
18 9 0 1.8659 -0.0817
18 9 1 2.0243 0.0828
18 9 2 2.0256 -0.0609
18 9 3 1.8257 -0.0658
18 9 4 -0.6771 -0.0062
18 9 5 0.5331 -0.0145
18 10 0 -1.7507 -0.0835
18 10 1 -3.4105 -0.0395
18 10 2 -2.5995 0.0024
18 10 3 -2.0287 -0.2170
18 11 0 3.8997 0.0719
18 11 1 1.6996 0.1704
19 0 0 -0.9271 0.0678
19 0 2 -0.1859 0.9467
19 0 4 -1.6269 -0.0707
19 0 6 -2.1778 -0.2027
19 1 0 0.4083 -0.2008
19 1 1 0.5565 -0.6366
19 1 2 2.2723 -0.0430
19 1 3 0.9618 -0.5420
19 1 4 3.5657 0.0198
19 1 5 1.3940 0.2119
19 1 6 2.8681 0.0008
19 2 0 -2.2409 -0.1981
19 2 1 -1.9112 0.1580
19 2 2 -1.1051 0.4348
19 2 3 -4.1191 -0.0776
19 2 4 -0.1950 -0.0199
19 2 5 -4.3351 -0.0309
19 2 6 1.2775 -0.0477
19 3 0 1.5257 -0.1717
19 3 1 1.7267 0.0966
19 3 2 3.6112 0.0148
19 3 3 0.3834 0.0023
19 3 4 4.6165 0.0553
19 3 5 -2.4517 0.0766
19 4 0 -2.5499 -0.3627
19 4 1 -3.6563 -0.0140
19 4 2 -1.4810 -0.1176
19 4 3 -5.2809 0.0193
19 4 4 1.3148 -0.0489
19 4 5 -4.6975 0.0292
19 5 0 2.6401 0.0865
19 5 1 2.3760 0.1611
19 5 2 4.7197 -0.0075
19 5 3 0.8047 0.0482
19 5 4 5.1574 -0.0523
19 6 0 -2.1641 -0.0744
19 6 1 -1.6832 -0.1579
19 6 2 -1.2974 -0.0237
19 6 3 -3.2996 0.0185
19 6 4 0.8732 -0.0037
19 7 0 -1.6627 0.2079
19 7 1 0.5564 -0.0181
19 7 2 0.2404 0.0485
19 7 3 -0.0193 -0.0180
19 8 0 -0.5470 0.0884
19 8 1 2.6656 0.0376
20 0 0 -1.9799 0.0362
20 1 0 -2.3418 -0.3206
20 1 1 1.7950 0.1867
20 2 0 -1.8691 -0.0556
20 2 1 3.9187 0.4432
20 3 0 -4.0489 -0.5155
0 0 0 0.0 0.0
;
_shelx_fab_checksum 67712
_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
Tb1 Tb 1.13611(2) 0.70660(2) 0.75805(2) 0.01433(6) Uani 1 1 d . . . . .
Tb2 Tb 0.63682(2) 0.71345(2) 0.77344(2) 0.01263(5) Uani 1 1 d . . . . .
C1 C 0.3795(2) 0.68559(19) 0.78395(17) 0.0157(9) Uani 1 1 d . . . . .
C2 C 0.3713(2) 0.65400(18) 0.72864(16) 0.0137(9) Uani 1 1 d . . . . .
C3 C 0.3145(2) 0.61175(18) 0.70540(17) 0.0162(9) Uani 1 1 d . . . . .
H3 H 0.272189 0.598523 0.725052 0.019 Uiso 1 1 calc R . . . .
C4 C 0.3255(2) 0.59019(19) 0.64974(17) 0.0187(9) Uani 1 1 d . . . . .
H4 H 0.291322 0.560849 0.627581 0.022 Uiso 1 1 calc R . . . .
C5 C 0.3909(2) 0.61574(18) 0.63033(17) 0.0177(9) Uani 1 1 d . . . . .
C6 C 0.4224(2) 0.60437(18) 0.57496(17) 0.0175(9) Uani 1 1 d . . . . .
C7 C 0.3750(2) 0.58044(19) 0.52651(17) 0.0213(10) Uani 1 1 d . . . . .
H7 H 0.320793 0.573343 0.528475 0.026 Uiso 1 1 calc R . . . .
C8 C 0.4049(3) 0.5667(2) 0.47536(18) 0.0274(11) Uani 1 1 d . . . . .
H8 H 0.371639 0.549290 0.442883 0.033 Uiso 1 1 calc R . . . .
C9 C 0.4832(3) 0.5782(2) 0.47121(18) 0.0282(11) Uani 1 1 d . . . . .
H9 H 0.504139 0.567991 0.436294 0.034 Uiso 1 1 calc R . . . .
C10 C 0.5305(3) 0.6046(2) 0.51821(19) 0.0281(11) Uani 1 1 d . . . . .
H10 H 0.583740 0.614208 0.515005 0.034 Uiso 1 1 calc R . . . .
C11 C 0.5012(2) 0.6171(2) 0.57014(18) 0.0251(11) Uani 1 1 d . . . . .
H11 H 0.534678 0.634485 0.602546 0.030 Uiso 1 1 calc R . . . .
C12 C 0.3589(2) 0.7125(2) 0.88091(17) 0.0219(10) Uani 1 1 d . . . . .
C13 C 0.2971(2) 0.7494(2) 0.90807(18) 0.0288(11) Uani 1 1 d . . . . .
H13A H 0.274175 0.782210 0.880626 0.043 Uiso 1 1 calc GR . . . .
H13B H 0.321344 0.769619 0.944433 0.043 Uiso 1 1 calc GR . . . .
H13C H 0.255724 0.720071 0.916702 0.043 Uiso 1 1 calc GR . . . .
C14 C 0.3853(3) 0.6537(2) 0.91791(19) 0.0338(12) Uani 1 1 d . . . . .
H14A H 0.340477 0.625014 0.918944 0.051 Uiso 1 1 calc GR . . . .
H14B H 0.405718 0.667037 0.957861 0.051 Uiso 1 1 calc GR . . . .
H14C H 0.426606 0.631355 0.900587 0.051 Uiso 1 1 calc GR . . . .
C15 C 0.4272(2) 0.7533(2) 0.86352(17) 0.0178(10) Uani 1 1 d . . . . .
C16 C 0.4028(2) 0.8213(2) 0.84508(18) 0.0258(11) Uani 1 1 d . . . . .
H16A H 0.355059 0.819989 0.816461 0.039 Uiso 1 1 calc GR . . . .
H16B H 0.445110 0.841789 0.827419 0.039 Uiso 1 1 calc GR . . . .
H16C H 0.392635 0.845658 0.879535 0.039 Uiso 1 1 calc GR . . . .
C17 C 0.5018(2) 0.7535(2) 0.90764(18) 0.0280(11) Uani 1 1 d . . . . .
H17A H 0.490352 0.771384 0.944843 0.042 Uiso 1 1 calc GR . . . .
H17B H 0.541883 0.779606 0.892542 0.042 Uiso 1 1 calc GR . . . .
H17C H 0.521180 0.709763 0.913921 0.042 Uiso 1 1 calc GR . . . .
C18 C 0.8764(2) 0.73670(19) 0.75570(16) 0.0139(9) Uani 1 1 d . . . . .
C19 C 0.8892(2) 0.76633(19) 0.81175(16) 0.0144(9) Uani 1 1 d . . . . .
C20 C 0.9523(2) 0.7602(2) 0.85483(17) 0.0218(10) Uani 1 1 d . . . . .
H20 H 0.994671 0.731702 0.852477 0.026 Uiso 1 1 calc R . . . .
C21 C 0.9476(2) 0.8006(2) 0.90270(17) 0.0213(10) Uani 1 1 d . . . . .
H21 H 0.986045 0.801668 0.936495 0.026 Uiso 1 1 calc R . . . .
C22 C 0.8816(2) 0.83858(19) 0.89584(16) 0.0154(9) Uani 1 1 d . . . . .
C23 C 0.8562(2) 0.88560(19) 0.93685(17) 0.0187(9) Uani 1 1 d . . . . .
C24 C 0.9108(2) 0.9162(2) 0.97736(18) 0.0247(10) Uani 1 1 d . . . . .
H24 H 0.965220 0.907703 0.978134 0.030 Uiso 1 1 calc R . . . .
C25 C 0.8861(3) 0.9592(2) 1.01666(19) 0.0334(12) Uani 1 1 d . . . . .
H25 H 0.923847 0.980214 1.044143 0.040 Uiso 1 1 calc R . . . .
C26 C 0.8076(3) 0.9717(2) 1.0163(2) 0.0361(13) Uani 1 1 d . . . . .
H26 H 0.791224 1.000439 1.044034 0.043 Uiso 1 1 calc R . . . .
C27 C 0.7526(3) 0.9427(2) 0.9758(2) 0.0321(12) Uani 1 1 d . . . . .
H27 H 0.698440 0.952077 0.975108 0.038 Uiso 1 1 calc R . . . .
C28 C 0.7764(2) 0.8997(2) 0.93623(18) 0.0261(11) Uani 1 1 d . . . . .
H28 H 0.738287 0.879657 0.908362 0.031 Uiso 1 1 calc R . . . .
C29 C 0.8942(2) 0.6776(2) 0.67040(17) 0.0178(9) Uani 1 1 d . . . . .
C30 C 0.9525(2) 0.6813(2) 0.62587(17) 0.0265(11) Uani 1 1 d . . . . .
H30A H 0.973147 0.724797 0.624962 0.040 Uiso 1 1 calc GR . . . .
H30B H 0.925785 0.669851 0.586931 0.040 Uiso 1 1 calc GR . . . .
H30C H 0.995940 0.651542 0.637245 0.040 Uiso 1 1 calc GR . . . .
C31 C 0.8736(2) 0.60820(19) 0.68165(18) 0.0257(10) Uani 1 1 d . . . . .
H31A H 0.853673 0.587538 0.644405 0.038 Uiso 1 1 calc GR . . . .
H31B H 0.833180 0.606796 0.707769 0.038 Uiso 1 1 calc GR . . . .
H31C H 0.920636 0.585752 0.699986 0.038 Uiso 1 1 calc GR . . . .
C32 C 0.8220(2) 0.72215(19) 0.65688(16) 0.0165(9) Uani 1 1 d . . . . .
C33 C 0.8403(2) 0.78577(19) 0.62991(17) 0.0246(10) Uani 1 1 d . . . . .
H33A H 0.794719 0.814081 0.628608 0.037 Uiso 1 1 calc GR . . . .
H33B H 0.852332 0.778746 0.590055 0.037 Uiso 1 1 calc GR . . . .
H33C H 0.885639 0.805434 0.653703 0.037 Uiso 1 1 calc GR . . . .
C34 C 0.7502(2) 0.69074(19) 0.62332(16) 0.0190(10) Uani 1 1 d . . . . .
H34A H 0.763571 0.673095 0.586585 0.028 Uiso 1 1 calc GR . . . .
H34B H 0.708287 0.722448 0.614654 0.028 Uiso 1 1 calc GR . . . .
H34C H 0.732159 0.656328 0.647006 0.028 Uiso 1 1 calc GR . . . .
C35 C 0.5948(2) 0.5714(2) 0.82601(18) 0.0230(10) Uani 1 1 d . . . . .
C36 C 0.6167(2) 0.5354(2) 0.77989(18) 0.0252(11) Uani 1 1 d . . . . .
H36 H 0.622592 0.490501 0.784374 0.030 Uiso 1 1 calc R . . . .
C37 C 0.6300(2) 0.5634(2) 0.72802(17) 0.0192(10) Uani 1 1 d . . . . .
C38 C 0.6483(3) 0.5179(2) 0.68027(18) 0.0339(12) Uani 1 1 d D . . . .
C39 C 0.5725(3) 0.5357(2) 0.8783(2) 0.0426(14) Uani 1 1 d D . . . .
C40 C 0.7846(2) 0.63192(19) 0.85006(18) 0.0193(10) Uani 1 1 d . . . . .
C41 C 0.7738(2) 0.6543(2) 0.90466(17) 0.0237(10) Uani 1 1 d . . . . .
H41 H 0.800529 0.634391 0.938719 0.028 Uiso 1 1 calc R . . . .
C42 C 0.7236(2) 0.7061(2) 0.91055(17) 0.0204(10) Uani 1 1 d . . . . .
C43 C 0.7256(2) 0.7305(2) 0.97351(18) 0.0247(11) Uani 1 1 d . . . . .
C44 C 0.8458(3) 0.5794(2) 0.84669(19) 0.0268(11) Uani 1 1 d . . . . .
C45 C 0.5654(2) 0.8095(2) 0.66213(18) 0.0206(10) Uani 1 1 d . . . . .
C46 C 0.5719(2) 0.8668(2) 0.69301(19) 0.0277(11) Uani 1 1 d . . . . .
H46 H 0.555668 0.905204 0.673118 0.033 Uiso 1 1 calc R . . . .
C47 C 0.6011(2) 0.8691(2) 0.75130(19) 0.0204(10) Uani 1 1 d . . . . .
C48 C 0.6057(2) 0.9329(2) 0.78251(19) 0.0305(11) Uani 1 1 d D . . . .
C49 C 0.5328(2) 0.8115(2) 0.59747(18) 0.0278(11) Uani 1 1 d D . . . .
C50 C 1.1065(2) 0.6146(2) 0.87316(19) 0.0280(11) Uani 1 1 d . . . . .
C51 C 1.1095(3) 0.5556(2) 0.8460(2) 0.0347(12) Uani 1 1 d . . . . .
H51 H 1.105625 0.517714 0.868049 0.042 Uiso 1 1 calc R . . . .
C52 C 1.1181(2) 0.5514(2) 0.7876(2) 0.0279(11) Uani 1 1 d . . . . .
C53 C 1.0967(3) 0.6159(2) 0.9377(2) 0.0405(14) Uani 1 1 d D . . . .
C54 C 1.1175(3) 0.4854(2) 0.7588(2) 0.0485(16) Uani 1 1 d D . . . .
C55 C 1.1779(2) 0.7011(2) 0.62063(17) 0.0211(10) Uani 1 1 d . . . . .
C56 C 1.2302(2) 0.7514(2) 0.62442(17) 0.0209(10) Uani 1 1 d . . . . .
H56 H 1.248706 0.766421 0.589884 0.025 Uiso 1 1 calc R . . . .
C57 C 1.2561(2) 0.78042(19) 0.67722(18) 0.0197(10) Uani 1 1 d . . . . .
C58 C 1.3136(3) 0.8364(2) 0.6769(2) 0.0278(11) Uani 1 1 d . . . . .
C59 C 1.1528(3) 0.6712(2) 0.5602(2) 0.0335(12) Uani 1 1 d . . . . .
C60 C 1.0795(2) 0.8496(2) 0.70130(19) 0.0208(10) Uani 1 1 d . . . . .
C61 C 1.1007(2) 0.8856(2) 0.75205(19) 0.0249(10) Uani 1 1 d . . . . .
H61 H 1.098611 0.930842 0.749884 0.030 Uiso 1 1 calc R . . . .
C62 C 1.1245(2) 0.8565(2) 0.80529(19) 0.0238(10) Uani 1 1 d . . . . .
C63 C 1.1425(3) 0.8987(2) 0.8599(2) 0.0323(12) Uani 1 1 d . . . . .
C64 C 1.0594(3) 0.8862(2) 0.6435(2) 0.0308(11) Uani 1 1 d . . . . .
F1 F 0.71469(15) 0.68375(12) 1.01087(10) 0.0364(7) Uani 1 1 d . . . . .
F2 F 0.79513(13) 0.75718(12) 0.99255(10) 0.0293(6) Uani 1 1 d . . . . .
F3 F 0.67088(14) 0.77478(13) 0.97781(10) 0.0354(7) Uani 1 1 d . . . . .
F4 F 0.87046(17) 0.55251(14) 0.89796(12) 0.0521(9) Uani 1 1 d . . . . .
F5 F 0.90909(14) 0.60282(12) 0.82622(11) 0.0379(7) Uani 1 1 d . . . . .
F6 F 0.81802(15) 0.53328(12) 0.81002(12) 0.0408(7) Uani 1 1 d . . . . .
F7 F 0.6805(8) 0.4642(4) 0.6976(3) 0.070(3) Uani 0.571(15) 1 d D U P A 1
F8 F 0.6839(6) 0.5438(7) 0.6394(5) 0.035(3) Uani 0.571(15) 1 d D U P A 1
F9 F 0.5743(4) 0.4993(5) 0.6504(3) 0.055(3) Uani 0.571(15) 1 d D U P A 1
F7' F 0.7248(6) 0.4919(6) 0.6995(3) 0.047(3) Uani 0.429(15) 1 d D U P A 2
F8' F 0.6601(8) 0.5454(9) 0.6302(5) 0.030(3) Uani 0.429(15) 1 d D U P A 2
F9' F 0.6066(8) 0.4669(5) 0.6704(5) 0.052(4) Uani 0.429(15) 1 d D U P A 2
F10 F 0.6405(11) 0.5027(13) 0.9010(9) 0.046(7) Uani 0.165(13) 1 d D U P B 3
F11 F 0.5145(16) 0.4930(15) 0.8772(13) 0.109(12) Uani 0.165(13) 1 d D U P B 3
F12 F 0.5671(15) 0.5735(14) 0.9257(11) 0.021(6) Uani 0.165(13) 1 d D U P B 3
F10' F 0.5991(5) 0.4767(2) 0.8845(3) 0.073(2) Uani 0.835(13) 1 d D U P B 4
F11' F 0.4927(2) 0.5283(3) 0.87152(18) 0.0549(17) Uani 0.835(13) 1 d D U P B 4
F12' F 0.5908(4) 0.5674(4) 0.9275(3) 0.0579(19) Uani 0.835(13) 1 d D U P B 4
F13 F 0.5689(8) 0.7671(6) 0.5669(6) 0.035(3) Uani 0.47(3) 1 d D U P C 5
F14 F 0.4575(5) 0.7956(10) 0.5869(7) 0.045(4) Uani 0.47(3) 1 d D U P C 5
F15 F 0.5437(15) 0.8663(5) 0.5706(5) 0.064(4) Uani 0.47(3) 1 d D U P C 5
F13' F 0.5845(7) 0.7908(11) 0.5647(5) 0.053(3) Uani 0.53(3) 1 d D U P C 6
F14' F 0.4694(7) 0.7731(6) 0.5859(6) 0.039(3) Uani 0.53(3) 1 d D U P C 6
F15' F 0.5066(10) 0.8687(3) 0.5787(5) 0.051(3) Uani 0.53(3) 1 d D U P C 6
F16 F 0.5753(7) 0.9301(3) 0.8343(4) 0.054(2) Uani 0.71(2) 1 d D U P D 7
F17 F 0.6800(3) 0.9495(5) 0.7983(5) 0.051(2) Uani 0.71(2) 1 d D U P D 7
F18 F 0.5679(6) 0.9811(3) 0.7540(3) 0.056(2) Uani 0.71(2) 1 d D U P D 7
F16' F 0.5433(9) 0.9428(9) 0.8084(12) 0.060(6) Uani 0.29(2) 1 d D U P D 8
F17' F 0.6717(8) 0.9432(11) 0.8190(8) 0.033(4) Uani 0.29(2) 1 d D U P D 8
F18' F 0.6064(16) 0.9804(7) 0.7416(6) 0.049(5) Uani 0.29(2) 1 d D U P D 8
F19 F 1.32290(15) 0.85613(13) 0.62348(11) 0.0445(8) Uani 1 1 d . . . . .
F20 F 1.38459(14) 0.82100(12) 0.70395(11) 0.0363(7) Uani 1 1 d . . . . .
F21 F 1.28942(15) 0.88645(12) 0.70554(13) 0.0445(8) Uani 1 1 d . . . . .
F22 F 1.20372(16) 0.68069(16) 0.52315(12) 0.0635(10) Uani 1 1 d . . . . .
F23 F 1.1425(2) 0.60900(15) 0.56307(13) 0.0718(11) Uani 1 1 d . . . . .
F24 F 1.08470(16) 0.69489(17) 0.53607(12) 0.0634(10) Uani 1 1 d . . . . .
F25 F 1.1898(8) 0.4763(8) 0.7441(12) 0.052(4) Uani 0.41(4) 1 d D U P E 9
F26 F 1.1040(12) 0.4356(8) 0.7935(9) 0.047(4) Uani 0.41(4) 1 d D U P E 9
F27 F 1.0618(12) 0.4787(12) 0.7121(8) 0.067(5) Uani 0.41(4) 1 d D U P E 9
F25' F 1.1693(10) 0.4803(6) 0.7200(8) 0.052(3) Uani 0.59(4) 1 d D U P E 10
F26' F 1.1304(13) 0.4375(6) 0.7976(6) 0.068(4) Uani 0.59(4) 1 d D U P E 10
F27' F 1.0471(6) 0.4764(8) 0.7261(7) 0.062(3) Uani 0.59(4) 1 d D U P E 10
F28 F 1.1669(5) 0.6273(11) 0.9689(5) 0.065(3) Uani 0.61(4) 1 d D U P F 11
F29 F 1.0476(11) 0.6611(7) 0.9505(6) 0.062(3) Uani 0.61(4) 1 d D U P F 11
F30 F 1.0709(11) 0.5605(4) 0.9568(6) 0.059(3) Uani 0.61(4) 1 d D U P F 11
F28' F 1.1503(12) 0.6542(12) 0.9703(7) 0.055(5) Uani 0.39(4) 1 d D U P F 12
F29' F 1.0266(8) 0.6412(11) 0.9451(8) 0.044(4) Uani 0.39(4) 1 d D U P F 12
F30' F 1.1027(17) 0.5600(6) 0.9662(8) 0.060(5) Uani 0.39(4) 1 d D U P F 12
F31 F 1.21813(16) 0.89704(14) 0.88115(12) 0.0480(8) Uani 1 1 d . . . . .
F32 F 1.1253(2) 0.95923(13) 0.84998(14) 0.0715(11) Uani 1 1 d . . . . .
F33 F 1.1048(2) 0.87938(16) 0.90231(13) 0.0747(12) Uani 1 1 d . . . . .
F34 F 1.12301(16) 0.89113(14) 0.61686(12) 0.0523(9) Uani 1 1 d . . . . .
F35 F 1.03451(17) 0.94507(13) 0.65047(13) 0.0529(8) Uani 1 1 d . . . . .
F36 F 1.00570(19) 0.85654(15) 0.60752(13) 0.0675(10) Uani 1 1 d . . . . .
N1 N 0.32553(18) 0.68754(15) 0.82192(14) 0.0177(8) Uani 1 1 d . . . . .
N2 N 0.44196(17) 0.71970(15) 0.80861(13) 0.0145(7) Uani 1 1 d . . . . .
N3 N 0.80935(18) 0.73767(15) 0.71833(13) 0.0155(8) Uani 1 1 d . . . . .
N4 N 0.92985(17) 0.70536(16) 0.72826(13) 0.0162(8) Uani 1 1 d . . . . .
O1 O 1.00016(14) 0.69181(13) 0.75198(11) 0.0179(6) Uani 1 1 d . . . . .
O2 O 1.13549(15) 0.79781(13) 0.81582(11) 0.0198(7) Uani 1 1 d . . . . .
O3 O 1.07726(15) 0.79050(13) 0.69685(12) 0.0210(7) Uani 1 1 d . . . . .
O4 O 1.23970(14) 0.76667(12) 0.72745(11) 0.0175(6) Uani 1 1 d . . . . .
O5 O 1.14548(15) 0.67637(13) 0.66097(12) 0.0213(7) Uani 1 1 d . . . . .
O6 O 1.12533(15) 0.59570(13) 0.75192(12) 0.0233(7) Uani 1 1 d . . . . .
O7 O 1.11032(15) 0.66858(13) 0.85116(12) 0.0197(7) Uani 1 1 d . . . . .
O8 O 0.74369(14) 0.76140(13) 0.73046(11) 0.0165(6) Uani 1 1 d . . . . .
O9 O 0.50169(14) 0.73266(13) 0.78226(11) 0.0183(6) Uani 1 1 d . . . . .
O10 O 0.75070(14) 0.65044(12) 0.80093(11) 0.0164(6) Uani 1 1 d . . . . .
O11 O 0.68024(14) 0.73489(13) 0.87245(11) 0.0170(6) Uani 1 1 d . . . . .
O12 O 0.62525(14) 0.82381(13) 0.78490(11) 0.0175(6) Uani 1 1 d . . . . .
O13 O 0.58374(14) 0.75447(13) 0.68135(11) 0.0174(6) Uani 1 1 d . . . . .
O14 O 0.58919(15) 0.63075(13) 0.82849(12) 0.0207(7) Uani 1 1 d . . . . .
O15 O 0.62898(15) 0.62119(13) 0.71427(11) 0.0178(6) Uani 1 1 d . . . . .
O16 O 0.25504(14) 0.66402(13) 0.81103(11) 0.0180(6) Uani 1 1 d . . . . .
S1 S 0.82398(6) 0.82352(5) 0.83044(4) 0.0172(2) Uani 1 1 d . . . . .
S2 S 0.43898(6) 0.66714(5) 0.68087(4) 0.0200(2) 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
Tb1 0.01047(10) 0.01446(11) 0.01795(11) -0.00246(9) 0.00156(8) -0.00027(9)
Tb2 0.01097(10) 0.01399(11) 0.01273(10) -0.00194(8) 0.00089(7) 0.00118(9)
C1 0.012(2) 0.017(2) 0.019(2) 0.0007(18) 0.0011(17) 0.0046(19)
C2 0.0105(19) 0.016(2) 0.014(2) -0.0022(18) 0.0000(16) 0.0033(19)
C3 0.013(2) 0.015(2) 0.021(2) 0.0015(18) 0.0029(17) 0.0014(19)
C4 0.016(2) 0.013(2) 0.026(2) 0.0004(19) -0.0006(18) -0.0013(19)
C5 0.021(2) 0.013(2) 0.018(2) -0.0028(18) -0.0012(18) -0.0001(19)
C6 0.023(2) 0.012(2) 0.018(2) -0.0012(18) 0.0042(18) 0.0023(19)
C7 0.027(2) 0.017(2) 0.019(2) -0.0024(19) -0.0001(19) -0.005(2)
C8 0.043(3) 0.021(3) 0.016(2) -0.006(2) -0.001(2) -0.003(2)
C9 0.044(3) 0.025(3) 0.018(3) 0.001(2) 0.011(2) 0.008(2)
C10 0.028(3) 0.031(3) 0.028(3) 0.000(2) 0.012(2) 0.002(2)
C11 0.024(2) 0.030(3) 0.020(2) -0.008(2) -0.0002(19) -0.003(2)
C12 0.014(2) 0.034(3) 0.018(2) -0.007(2) -0.0011(17) -0.002(2)
C13 0.023(2) 0.041(3) 0.023(3) -0.014(2) 0.006(2) 0.000(2)
C14 0.032(3) 0.046(3) 0.023(3) 0.001(2) 0.003(2) -0.001(3)
C15 0.011(2) 0.025(3) 0.017(2) -0.0106(19) 0.0005(17) 0.0027(19)
C16 0.022(2) 0.029(3) 0.025(3) -0.013(2) -0.0017(19) -0.003(2)
C17 0.015(2) 0.045(3) 0.023(3) -0.013(2) -0.0026(18) -0.001(2)
C18 0.011(2) 0.014(2) 0.016(2) -0.0013(18) 0.0023(17) -0.0007(18)
C19 0.014(2) 0.015(2) 0.014(2) 0.0010(18) 0.0023(17) -0.0010(19)
C20 0.017(2) 0.029(3) 0.020(2) -0.009(2) 0.0012(18) 0.001(2)
C21 0.018(2) 0.033(3) 0.012(2) -0.003(2) -0.0030(17) -0.002(2)
C22 0.014(2) 0.020(2) 0.013(2) -0.0017(18) 0.0019(17) -0.0043(19)
C23 0.022(2) 0.016(2) 0.017(2) 0.0005(18) 0.0028(18) -0.001(2)
C24 0.026(2) 0.023(3) 0.024(3) -0.004(2) -0.002(2) 0.000(2)
C25 0.046(3) 0.030(3) 0.022(3) -0.007(2) -0.003(2) 0.001(3)
C26 0.054(3) 0.028(3) 0.028(3) -0.010(2) 0.011(3) 0.009(3)
C27 0.034(3) 0.027(3) 0.037(3) -0.004(2) 0.011(2) 0.009(2)
C28 0.023(2) 0.028(3) 0.026(3) -0.004(2) 0.001(2) 0.003(2)
C29 0.013(2) 0.025(2) 0.015(2) -0.0080(19) 0.0000(17) -0.002(2)
C30 0.020(2) 0.039(3) 0.022(2) -0.014(2) 0.0048(19) -0.003(2)
C31 0.028(2) 0.024(3) 0.025(3) -0.005(2) 0.002(2) 0.000(2)
C32 0.012(2) 0.023(2) 0.015(2) -0.0036(18) 0.0025(16) -0.0019(19)
C33 0.029(2) 0.025(3) 0.020(2) 0.000(2) 0.0013(19) -0.005(2)
C34 0.017(2) 0.024(2) 0.014(2) -0.0050(19) -0.0039(17) -0.003(2)
C35 0.018(2) 0.024(3) 0.028(3) 0.002(2) 0.0060(19) 0.002(2)
C36 0.033(3) 0.014(2) 0.031(3) -0.004(2) 0.012(2) -0.001(2)
C37 0.017(2) 0.019(3) 0.020(2) -0.008(2) -0.0016(18) 0.001(2)
C38 0.055(4) 0.023(3) 0.024(3) -0.011(2) 0.006(3) 0.000(3)
C39 0.065(4) 0.027(3) 0.041(3) 0.003(3) 0.026(3) 0.006(3)
C40 0.016(2) 0.019(2) 0.023(2) 0.003(2) 0.0044(18) 0.003(2)
C41 0.025(2) 0.032(3) 0.013(2) 0.004(2) -0.0024(18) 0.011(2)
C42 0.017(2) 0.027(3) 0.017(2) -0.004(2) 0.0026(18) -0.004(2)
C43 0.021(2) 0.033(3) 0.019(2) -0.003(2) -0.0001(19) -0.002(2)
C44 0.030(3) 0.027(3) 0.021(3) 0.000(2) -0.002(2) 0.008(2)
C45 0.010(2) 0.026(3) 0.025(3) 0.008(2) 0.0010(18) -0.002(2)
C46 0.031(3) 0.020(3) 0.030(3) 0.006(2) -0.004(2) 0.000(2)
C47 0.013(2) 0.018(2) 0.031(3) 0.001(2) 0.0030(19) 0.002(2)
C48 0.033(3) 0.021(3) 0.036(3) -0.001(2) -0.002(2) 0.000(2)
C49 0.025(3) 0.032(3) 0.026(3) 0.009(2) 0.001(2) 0.001(2)
C50 0.017(2) 0.035(3) 0.032(3) 0.006(2) 0.005(2) -0.003(2)
C51 0.036(3) 0.026(3) 0.045(3) 0.015(2) 0.014(2) 0.003(2)
C52 0.019(2) 0.016(3) 0.050(3) -0.001(2) 0.010(2) -0.002(2)
C53 0.044(3) 0.038(3) 0.041(3) 0.018(3) 0.010(3) 0.006(3)
C54 0.056(4) 0.021(3) 0.075(5) -0.001(3) 0.033(4) -0.007(3)
C55 0.017(2) 0.027(3) 0.020(2) -0.003(2) 0.0023(18) 0.010(2)
C56 0.020(2) 0.025(3) 0.018(2) 0.002(2) 0.0054(18) 0.000(2)
C57 0.013(2) 0.016(2) 0.030(3) 0.002(2) 0.0012(18) 0.0045(19)
C58 0.023(2) 0.028(3) 0.032(3) 0.001(2) 0.006(2) -0.005(2)
C59 0.028(3) 0.045(3) 0.028(3) -0.007(2) 0.002(2) -0.005(3)
C60 0.010(2) 0.022(3) 0.031(3) 0.003(2) 0.0057(19) 0.000(2)
C61 0.027(2) 0.015(2) 0.032(3) 0.003(2) 0.002(2) 0.005(2)
C62 0.017(2) 0.019(3) 0.036(3) -0.009(2) 0.004(2) -0.004(2)
C63 0.034(3) 0.024(3) 0.039(3) -0.014(2) 0.006(2) -0.006(2)
C64 0.028(3) 0.025(3) 0.039(3) 0.004(2) 0.003(2) -0.001(2)
F1 0.0485(17) 0.0427(17) 0.0190(14) 0.0025(13) 0.0082(12) -0.0111(15)
F2 0.0260(14) 0.0402(16) 0.0196(14) -0.0035(12) -0.0047(11) -0.0039(13)
F3 0.0318(14) 0.0514(18) 0.0221(14) -0.0126(13) 0.0006(11) 0.0141(14)
F4 0.064(2) 0.060(2) 0.0321(17) 0.0159(15) 0.0061(15) 0.0451(17)
F5 0.0202(13) 0.0434(18) 0.0515(18) -0.0009(14) 0.0099(13) 0.0091(13)
F6 0.0361(16) 0.0232(15) 0.060(2) -0.0099(14) -0.0032(14) 0.0104(13)
F7 0.130(8) 0.031(4) 0.050(4) -0.013(3) 0.021(5) 0.026(5)
F8 0.034(5) 0.034(4) 0.042(5) -0.015(4) 0.019(4) -0.012(4)
F9 0.062(4) 0.060(5) 0.044(4) -0.042(4) 0.016(3) -0.028(4)
F7' 0.062(6) 0.048(6) 0.030(4) -0.017(4) 0.003(4) 0.029(5)
F8' 0.044(7) 0.029(5) 0.018(4) -0.012(4) 0.004(4) 0.000(5)
F9' 0.074(7) 0.030(5) 0.058(6) -0.026(5) 0.032(5) -0.029(5)
F10 0.058(10) 0.045(10) 0.037(9) 0.031(7) 0.018(7) 0.016(8)
F11 0.123(15) 0.105(15) 0.097(14) 0.009(9) 0.008(9) -0.016(10)
F12 0.022(9) 0.027(9) 0.016(9) 0.003(7) 0.009(6) 0.018(7)
F10' 0.126(5) 0.031(3) 0.080(4) 0.030(2) 0.071(4) 0.029(3)
F11' 0.059(3) 0.054(3) 0.060(3) 0.002(2) 0.037(2) -0.024(2)
F12' 0.078(5) 0.062(4) 0.035(3) 0.010(3) 0.014(3) -0.011(3)
F13 0.042(5) 0.041(5) 0.023(4) 0.004(4) 0.007(3) 0.004(4)
F14 0.021(4) 0.084(8) 0.030(4) 0.000(6) 0.000(3) 0.018(5)
F15 0.102(9) 0.051(5) 0.035(4) 0.022(4) -0.008(5) -0.007(5)
F13' 0.036(5) 0.109(8) 0.019(3) 0.022(5) 0.013(3) 0.024(5)
F14' 0.041(5) 0.040(5) 0.029(4) 0.009(4) -0.017(4) -0.001(4)
F15' 0.071(7) 0.034(4) 0.038(5) 0.014(3) -0.024(4) 0.010(4)
F16 0.080(5) 0.030(3) 0.060(4) -0.011(3) 0.032(4) 0.006(3)
F17 0.036(3) 0.037(4) 0.077(5) -0.028(4) -0.002(3) -0.007(2)
F18 0.070(5) 0.024(3) 0.065(4) -0.014(2) -0.023(3) 0.021(3)
F16' 0.047(7) 0.045(8) 0.093(10) -0.028(7) 0.025(7) 0.012(6)
F17' 0.041(7) 0.027(7) 0.027(7) -0.012(6) -0.017(5) 0.012(6)
F18' 0.082(10) 0.011(6) 0.048(7) 0.003(5) -0.011(6) 0.004(6)
F19 0.0516(18) 0.0460(19) 0.0365(17) 0.0125(14) 0.0083(14) -0.0251(15)
F20 0.0204(14) 0.0418(17) 0.0461(17) 0.0009(14) 0.0017(13) -0.0103(13)
F21 0.0408(17) 0.0227(16) 0.074(2) -0.0133(15) 0.0225(16) -0.0110(13)
F22 0.0488(18) 0.114(3) 0.0318(17) -0.0333(18) 0.0206(15) -0.0284(19)
F23 0.125(3) 0.047(2) 0.040(2) -0.0226(17) -0.002(2) -0.020(2)
F24 0.0426(18) 0.111(3) 0.0314(17) -0.0233(18) -0.0148(14) 0.0198(19)
F25 0.061(6) 0.034(5) 0.067(9) -0.009(6) 0.032(6) -0.002(5)
F26 0.045(7) 0.020(6) 0.083(7) 0.006(5) 0.030(5) 0.002(5)
F27 0.087(8) 0.045(6) 0.073(8) -0.017(6) 0.031(7) -0.020(6)
F25' 0.063(5) 0.027(4) 0.072(7) -0.015(4) 0.034(5) 0.003(4)
F26' 0.083(8) 0.018(4) 0.106(6) 0.005(4) 0.024(5) -0.005(5)
F27' 0.067(5) 0.046(5) 0.077(6) -0.033(5) 0.028(5) -0.034(4)
F28 0.064(4) 0.096(8) 0.033(4) 0.011(5) 0.000(3) -0.004(5)
F29 0.089(6) 0.062(5) 0.044(4) 0.004(4) 0.032(5) 0.015(5)
F30 0.075(7) 0.061(5) 0.044(5) 0.031(3) 0.020(5) -0.010(4)
F28' 0.064(7) 0.070(8) 0.031(5) 0.001(6) 0.002(5) -0.013(6)
F29' 0.042(6) 0.063(8) 0.031(5) 0.003(6) 0.019(4) 0.002(5)
F30' 0.079(9) 0.061(7) 0.042(6) 0.015(5) 0.009(6) 0.001(6)
F31 0.0411(17) 0.049(2) 0.0499(19) -0.0236(16) -0.0071(14) -0.0021(16)
F32 0.111(3) 0.0246(18) 0.066(2) -0.0220(16) -0.032(2) 0.0225(19)
F33 0.091(3) 0.088(3) 0.055(2) -0.0484(19) 0.045(2) -0.053(2)
F34 0.0454(18) 0.066(2) 0.0498(19) 0.0270(16) 0.0215(15) 0.0104(16)
F35 0.066(2) 0.0402(19) 0.054(2) 0.0231(15) 0.0126(17) 0.0275(17)
F36 0.077(2) 0.066(2) 0.047(2) 0.0323(18) -0.0359(16) -0.042(2)
N1 0.0094(17) 0.018(2) 0.025(2) -0.0024(16) 0.0029(15) -0.0003(16)
N2 0.0099(16) 0.0193(19) 0.0145(18) -0.0030(15) 0.0017(14) 0.0015(16)
N3 0.0145(18) 0.0163(19) 0.0158(19) -0.0006(15) 0.0029(14) 0.0029(16)
N4 0.0119(17) 0.022(2) 0.0148(18) -0.0021(16) 0.0024(14) 0.0028(16)
O1 0.0068(13) 0.0285(17) 0.0176(15) -0.0023(13) -0.0007(11) 0.0030(13)
O2 0.0198(15) 0.0174(17) 0.0215(16) -0.0042(13) 0.0005(12) 0.0024(14)
O3 0.0185(15) 0.0197(17) 0.0240(16) 0.0006(14) 0.0005(12) 0.0010(14)
O4 0.0154(14) 0.0176(16) 0.0193(16) -0.0018(13) 0.0021(12) -0.0030(13)
O5 0.0172(15) 0.0215(17) 0.0258(17) -0.0067(14) 0.0051(13) -0.0033(13)
O6 0.0206(16) 0.0167(17) 0.0339(18) -0.0030(14) 0.0087(14) -0.0030(14)
O7 0.0139(14) 0.0213(17) 0.0240(17) 0.0028(14) 0.0033(12) 0.0001(13)
O8 0.0094(14) 0.0221(16) 0.0176(15) -0.0016(13) 0.0002(11) 0.0026(13)
O9 0.0102(14) 0.0263(17) 0.0192(15) -0.0031(13) 0.0047(12) -0.0008(13)
O10 0.0142(14) 0.0194(16) 0.0152(15) 0.0012(13) 0.0003(12) 0.0036(13)
O11 0.0152(14) 0.0223(16) 0.0124(15) -0.0023(13) -0.0024(12) 0.0017(13)
O12 0.0139(14) 0.0142(16) 0.0235(16) -0.0052(13) -0.0008(12) -0.0012(13)
O13 0.0124(14) 0.0224(17) 0.0169(15) 0.0012(13) 0.0001(12) 0.0023(13)
O14 0.0220(16) 0.0171(17) 0.0241(17) -0.0023(13) 0.0075(13) -0.0003(14)
O15 0.0219(15) 0.0147(16) 0.0161(15) -0.0022(12) -0.0003(12) 0.0017(14)
O16 0.0095(14) 0.0224(17) 0.0221(16) 0.0011(13) 0.0020(12) -0.0022(13)
S1 0.0149(5) 0.0188(6) 0.0172(5) -0.0044(5) -0.0002(4) 0.0020(5)
S2 0.0156(5) 0.0260(6) 0.0187(6) -0.0074(5) 0.0040(4) -0.0060(5)
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_3
O1 Tb1 O3 74.00(9) .
O1 Tb1 O4 146.94(9) .
O1 Tb1 O5 96.08(9) .
O1 Tb1 O7 72.68(9) .
O1 Tb1 O16 138.84(9) 1_655
O2 Tb1 O1 93.43(9) .
O2 Tb1 O3 72.46(9) .
O2 Tb1 O4 78.26(9) .
O2 Tb1 O5 140.41(9) .
O2 Tb1 O6 147.65(9) .
O2 Tb1 O7 75.19(9) .
O2 Tb1 O16 94.87(9) 1_655
O3 Tb1 O16 146.52(9) 1_655
O4 Tb1 O3 72.98(9) .
O4 Tb1 O7 133.32(9) .
O4 Tb1 O16 74.14(9) 1_655
O5 Tb1 O3 73.49(9) .
O5 Tb1 O4 72.96(9) .
O5 Tb1 O7 144.15(10) .
O5 Tb1 O16 102.60(9) 1_655
O6 Tb1 O1 78.14(9) .
O6 Tb1 O3 132.32(10) .
O6 Tb1 O4 124.64(8) .
O6 Tb1 O5 71.90(9) .
O6 Tb1 O7 72.48(9) .
O6 Tb1 O16 73.49(9) 1_655
O7 Tb1 O3 131.32(9) .
O7 Tb1 O16 70.72(8) 1_655
O9 Tb2 O8 139.85(9) .
O10 Tb2 O8 72.31(8) .
O10 Tb2 O9 147.68(9) .
O11 Tb2 O8 99.25(9) .
O11 Tb2 O9 93.88(8) .
O11 Tb2 O10 72.94(9) .
O11 Tb2 O13 147.06(9) .
O11 Tb2 O14 72.85(9) .
O11 Tb2 O15 134.81(9) .
O12 Tb2 O8 73.56(8) .
O12 Tb2 O9 74.07(9) .
O12 Tb2 O10 126.85(9) .
O12 Tb2 O11 73.81(9) .
O12 Tb2 O13 73.28(9) .
O12 Tb2 O14 128.63(8) .
O12 Tb2 O15 151.23(9) .
O13 Tb2 O8 72.63(9) .
O13 Tb2 O9 75.81(8) .
O13 Tb2 O10 130.30(8) .
O13 Tb2 O14 129.25(9) .
O13 Tb2 O15 78.12(9) .
O14 Tb2 O8 149.69(9) .
O14 Tb2 O9 70.45(9) .
O14 Tb2 O10 77.42(9) .
O15 Tb2 O8 95.17(8) .
O15 Tb2 O9 102.01(9) .
O15 Tb2 O10 71.19(9) .
O15 Tb2 O14 73.27(9) .
N1 C1 C2 126.6(4) .
N2 C1 C2 126.7(3) .
N2 C1 N1 106.7(3) .
C1 C2 S2 120.1(3) .
C3 C2 C1 128.8(3) .
C3 C2 S2 111.0(3) .
C2 C3 C4 112.9(3) .
C5 C4 C3 113.2(4) .
C4 C5 C6 129.4(4) .
C4 C5 S2 111.3(3) .
C6 C5 S2 119.3(3) .
C7 C6 C5 120.8(3) .
C7 C6 C11 118.4(3) .
C11 C6 C5 120.9(4) .
C8 C7 C6 121.1(4) .
C7 C8 C9 120.2(4) .
C10 C9 C8 119.3(4) .
C9 C10 C11 120.7(4) .
C10 C11 C6 120.2(4) .
C13 C12 C14 110.5(3) .
C13 C12 C15 115.1(4) .
C14 C12 C15 114.3(3) .
N1 C12 C13 110.5(3) .
N1 C12 C14 105.8(3) .
N1 C12 C15 99.6(3) .
C16 C15 C12 113.4(3) .
C17 C15 C12 115.3(3) .
C17 C15 C16 110.8(3) .
N2 C15 C12 100.4(3) .
N2 C15 C16 106.0(3) .
N2 C15 C17 109.9(3) .
N3 C18 C19 126.1(3) .
N3 C18 N4 106.6(3) .
N4 C18 C19 127.2(4) .
C18 C19 S1 120.1(3) .
C20 C19 C18 128.7(4) .
C20 C19 S1 111.0(3) .
C19 C20 C21 112.8(4) .
C22 C21 C20 113.2(4) .
C21 C22 C23 128.7(4) .
C21 C22 S1 111.2(3) .
C23 C22 S1 120.0(3) .
C24 C23 C22 120.6(4) .
C24 C23 C28 118.7(4) .
C28 C23 C22 120.8(4) .
C25 C24 C23 120.1(4) .
C26 C25 C24 120.6(4) .
C27 C26 C25 120.3(4) .
C26 C27 C28 119.8(4) .
C27 C28 C23 120.6(4) .
C30 C29 C32 114.5(3) .
C31 C29 C30 110.5(3) .
C31 C29 C32 114.2(3) .
N4 C29 C30 110.4(3) .
N4 C29 C31 107.1(3) .
N4 C29 C32 99.3(3) .
C33 C32 C29 113.9(3) .
C34 C32 C29 114.5(3) .
C34 C32 C33 111.9(3) .
N3 C32 C29 99.0(3) .
N3 C32 C33 105.1(3) .
N3 C32 C34 111.3(3) .
C36 C35 C39 117.7(4) .
O14 C35 C36 127.1(4) .
O14 C35 C39 115.2(4) .
C37 C36 C35 121.6(4) .
C36 C37 C38 115.8(4) .
O15 C37 C36 129.3(4) .
O15 C37 C38 114.9(3) .
F7 C38 C37 116.4(4) .
F7 C38 F8 111.1(7) .
F7 C38 F9 103.2(5) .
F8 C38 C37 115.1(8) .
F8 C38 F9 104.0(6) .
F9 C38 C37 105.2(4) .
F7' C38 C37 106.7(5) .
F8' C38 C37 115.3(9) .
F8' C38 F7' 100.9(7) .
F9' C38 C37 118.8(5) .
F9' C38 F7' 101.7(6) .
F9' C38 F8' 110.7(9) .
F10 C39 C35 104.7(10) .
F11 C39 C35 125.7(14) .
F11 C39 F10 105.0(12) .
F11 C39 F12 105.8(14) .
F12 C39 C35 113.9(16) .
F12 C39 F10 97.7(11) .
F10' C39 C35 115.3(4) .
F10' C39 F11' 103.4(5) .
F11' C39 C35 108.9(4) .
F12' C39 C35 112.5(5) .
F12' C39 F10' 110.1(6) .
F12' C39 F11' 105.9(5) .
C41 C40 C44 118.1(4) .
O10 C40 C41 127.6(4) .
O10 C40 C44 114.3(3) .
C40 C41 C42 120.9(4) .
C41 C42 C43 114.5(4) .
O11 C42 C41 129.1(4) .
O11 C42 C43 116.4(4) .
F1 C43 C42 112.2(4) .
F1 C43 F2 107.1(3) .
F2 C43 C42 110.6(3) .
F3 C43 C42 112.2(4) .
F3 C43 F1 107.4(3) .
F3 C43 F2 107.0(3) .
F4 C44 C40 113.5(3) .
F4 C44 F5 107.1(4) .
F4 C44 F6 107.4(4) .
F5 C44 C40 110.6(4) .
F6 C44 C40 111.5(4) .
F6 C44 F5 106.3(3) .
C46 C45 C49 118.1(4) .
O13 C45 C46 127.7(4) .
O13 C45 C49 114.2(4) .
C47 C46 C45 121.7(4) .
C46 C47 C48 119.0(4) .
O12 C47 C46 128.5(4) .
O12 C47 C48 112.5(4) .
F16 C48 C47 112.0(4) .
F17 C48 C47 110.3(5) .
F17 C48 F16 104.0(5) .
F17 C48 F18 108.9(6) .
F18 C48 C47 116.6(4) .
F18 C48 F16 104.2(4) .
F16' C48 C47 111.2(7) .
F16' C48 F17' 111.4(10) .
F16' C48 F18' 106.4(8) .
F17' C48 C47 115.2(10) .
F17' C48 F18' 103.2(9) .
F18' C48 C47 108.6(8) .
F13 C49 C45 110.9(7) .
F14 C49 C45 113.1(8) .
F14 C49 F13 103.6(8) .
F14 C49 F15 109.0(8) .
F15 C49 C45 115.1(7) .
F15 C49 F13 104.2(7) .
F13' C49 C45 111.6(6) .
F13' C49 F14' 106.3(8) .
F13' C49 F15' 109.5(6) .
F14' C49 C45 110.9(7) .
F15' C49 C45 113.9(6) .
F15' C49 F14' 104.1(6) .
C51 C50 C53 118.2(4) .
O7 C50 C51 128.1(4) .
O7 C50 C53 113.7(4) .
C52 C51 C50 120.9(4) .
C51 C52 C54 119.1(4) .
O6 C52 C51 128.6(4) .
O6 C52 C54 112.3(4) .
F28 C53 C50 108.4(6) .
F28 C53 F30 107.1(7) .
F29 C53 C50 112.9(7) .
F29 C53 F28 107.9(7) .
F29 C53 F30 107.2(7) .
F30 C53 C50 113.1(6) .
F28' C53 C50 113.0(8) .
F29' C53 C50 110.6(9) .
F29' C53 F28' 104.2(9) .
F30' C53 C50 117.0(9) .
F30' C53 F28' 104.1(9) .
F30' C53 F29' 107.0(9) .
F25 C54 C52 106.5(9) .
F25 C54 F26 106.2(9) .
F26 C54 C52 115.5(11) .
F27 C54 C52 113.7(12) .
F27 C54 F25 111.4(9) .
F27 C54 F26 103.4(11) .
F25' C54 C52 113.1(6) .
F26' C54 C52 113.3(8) .
F26' C54 F25' 108.6(8) .
F26' C54 F27' 108.7(8) .
F27' C54 C52 108.7(8) .
F27' C54 F25' 104.0(7) .
C56 C55 C59 118.0(4) .
O5 C55 C56 128.2(4) .
O5 C55 C59 113.9(4) .
C57 C56 C55 121.4(4) .
C56 C57 C58 117.6(4) .
O4 C57 C56 128.6(4) .
O4 C57 C58 113.8(4) .
F19 C58 C57 113.6(4) .
F19 C58 F20 106.9(3) .
F19 C58 F21 107.4(4) .
F20 C58 C57 111.2(4) .
F20 C58 F21 106.7(4) .
F21 C58 C57 110.7(3) .
F22 C59 C55 113.4(4) .
F22 C59 F24 107.4(4) .
F23 C59 C55 112.4(4) .
F23 C59 F22 106.7(4) .
F23 C59 F24 105.9(4) .
F24 C59 C55 110.5(4) .
C61 C60 C64 117.3(4) .
O3 C60 C61 127.5(4) .
O3 C60 C64 115.2(4) .
C62 C61 C60 121.1(4) .
C61 C62 C63 118.4(4) .
O2 C62 C61 128.2(4) .
O2 C62 C63 113.3(4) .
F31 C63 C62 111.4(4) .
F32 C63 C62 113.4(4) .
F32 C63 F31 106.0(4) .
F33 C63 C62 111.6(4) .
F33 C63 F31 106.2(4) .
F33 C63 F32 107.8(4) .
F34 C64 C60 109.8(4) .
F35 C64 C60 113.5(4) .
F35 C64 F34 106.5(4) .
F36 C64 C60 111.6(4) .
F36 C64 F34 107.3(4) .
F36 C64 F35 107.9(4) .
C1 N1 C12 112.7(3) .
O16 N1 C1 124.3(3) .
O16 N1 C12 122.6(3) .
C1 N2 C15 112.8(3) .
O9 N2 C1 123.5(3) .
O9 N2 C15 122.4(3) .
C18 N3 C32 112.4(3) .
O8 N3 C18 124.3(3) .
O8 N3 C32 122.0(3) .
C18 N4 C29 112.4(3) .
O1 N4 C18 124.5(3) .
O1 N4 C29 122.3(3) .
N4 O1 Tb1 150.1(2) .
C62 O2 Tb1 134.6(3) .
C60 O3 Tb1 132.7(3) .
C57 O4 Tb1 131.9(3) .
C55 O5 Tb1 133.4(3) .
C52 O6 Tb1 135.2(3) .
C50 O7 Tb1 134.1(3) .
N3 O8 Tb2 131.3(2) .
N2 O9 Tb2 148.0(2) .
C40 O10 Tb2 132.3(2) .
C42 O11 Tb2 133.0(3) .
C47 O12 Tb2 134.6(3) .
C45 O13 Tb2 134.3(3) .
C35 O14 Tb2 132.2(2) .
C37 O15 Tb2 130.5(2) .
N1 O16 Tb1 131.4(2) 1_455
C22 S1 C19 91.75(19) .
C5 S2 C2 91.64(18) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.342(2) .
Tb1 O2 2.330(3) .
Tb1 O3 2.390(3) .
Tb1 O4 2.366(2) .
Tb1 O5 2.352(3) .
Tb1 O6 2.335(3) .
Tb1 O7 2.387(3) .
Tb1 O16 2.404(3) 1_655
Tb2 O8 2.422(2) .
Tb2 O9 2.394(2) .
Tb2 O10 2.374(3) .
Tb2 O11 2.345(3) .
Tb2 O12 2.340(3) .
Tb2 O13 2.354(3) .
Tb2 O14 2.360(3) .
Tb2 O15 2.359(3) .
C1 C2 1.426(5) .
C1 N1 1.360(4) .
C1 N2 1.349(5) .
C2 C3 1.371(5) .
C2 S2 1.731(3) .
C3 C4 1.397(5) .
C4 C5 1.374(5) .
C5 C6 1.473(5) .
C5 S2 1.713(4) .
C6 C7 1.383(5) .
C6 C11 1.400(5) .
C7 C8 1.380(5) .
C8 C9 1.384(6) .
C9 C10 1.377(6) .
C10 C11 1.386(5) .
C12 C13 1.517(5) .
C12 C14 1.532(6) .
C12 C15 1.549(5) .
C12 N1 1.495(5) .
C15 C16 1.529(6) .
C15 C17 1.523(5) .
C15 N2 1.500(4) .
C18 C19 1.423(5) .
C18 N3 1.340(5) .
C18 N4 1.355(4) .
C19 C20 1.371(5) .
C19 S1 1.736(4) .
C20 C21 1.402(5) .
C21 C22 1.377(5) .
C22 C23 1.473(5) .
C22 S1 1.715(4) .
C23 C24 1.387(6) .
C23 C28 1.402(5) .
C24 C25 1.385(5) .
C25 C26 1.374(6) .
C26 C27 1.374(6) .
C27 C28 1.383(5) .
C29 C30 1.532(5) .
C29 C31 1.528(5) .
C29 C32 1.551(5) .
C29 N4 1.506(5) .
C32 C33 1.523(5) .
C32 C34 1.514(5) .
C32 N3 1.497(4) .
C35 C36 1.397(5) .
C35 C39 1.512(6) .
C35 O14 1.250(5) .
C36 C37 1.379(5) .
C37 C38 1.522(5) .
C37 O15 1.252(5) .
C38 F7 1.292(6) .
C38 F8 1.309(7) .
C38 F9 1.415(6) .
C38 F7' 1.435(7) .
C38 F8' 1.329(8) .
C38 F9' 1.291(7) .
C39 F10 1.397(9) .
C39 F11 1.339(10) .
C39 F12 1.362(10) .
C39 F10' 1.319(5) .
C39 F11' 1.369(6) .
C39 F12' 1.314(6) .
C40 C41 1.379(5) .
C40 C44 1.531(6) .
C40 O10 1.261(5) .
C41 C42 1.405(5) .
C42 C43 1.534(5) .
C42 O11 1.229(5) .
C43 F1 1.335(5) .
C43 F2 1.337(5) .
C43 F3 1.335(5) .
C44 F4 1.325(5) .
C44 F5 1.337(5) .
C44 F6 1.329(5) .
C45 C46 1.391(6) .
C45 C49 1.518(6) .
C45 O13 1.260(5) .
C46 C47 1.369(6) .
C47 C48 1.516(6) .
C47 O12 1.258(5) .
C48 F16 1.369(6) .
C48 F17 1.324(6) .
C48 F18 1.326(6) .
C48 F16' 1.314(8) .
C48 F17' 1.334(9) .
C48 F18' 1.372(8) .
C49 F13 1.367(8) .
C49 F14 1.327(8) .
C49 F15 1.330(8) .
C49 F13' 1.317(7) .
C49 F14' 1.352(7) .
C49 F15' 1.333(7) .
C50 C51 1.391(6) .
C50 C53 1.520(6) .
C50 O7 1.245(5) .
C51 C52 1.377(6) .
C52 C54 1.533(6) .
C52 O6 1.258(5) .
C53 F28 1.338(7) .
C53 F29 1.329(7) .
C53 F30 1.339(7) .
C53 F28' 1.366(8) .
C53 F29' 1.348(8) .
C53 F30' 1.340(8) .
C54 F25 1.347(8) .
C54 F26 1.353(9) .
C54 F27 1.346(9) .
C54 F25' 1.350(7) .
C54 F26' 1.343(8) .
C54 F27' 1.347(8) .
C55 C56 1.382(6) .
C55 C59 1.534(6) .
C55 O5 1.259(4) .
C56 C57 1.378(5) .
C57 C58 1.535(6) .
C57 O4 1.262(4) .
C58 F19 1.330(5) .
C58 F20 1.331(5) .
C58 F21 1.335(5) .
C59 F22 1.319(5) .
C59 F23 1.319(5) .
C59 F24 1.322(5) .
C60 C61 1.397(6) .
C60 C64 1.534(6) .
C60 O3 1.243(5) .
C61 C62 1.381(6) .
C62 C63 1.535(6) .
C62 O2 1.264(5) .
C63 F31 1.325(5) .
C63 F32 1.315(5) .
C63 F33 1.309(5) .
C64 F34 1.330(5) .
C64 F35 1.323(5) .
C64 F36 1.310(5) .
N1 O16 1.300(4) .
N2 O9 1.292(3) .
N3 O8 1.299(4) .
N4 O1 1.288(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 -179.8(4) .
C1 C2 S2 C5 179.7(3) .
C1 N1 O16 Tb1 -82.4(4) 1_455
C1 N2 O9 Tb2 -107.5(5) .
C2 C1 N1 C12 167.7(4) .
C2 C1 N1 O16 -5.1(6) .
C2 C1 N2 C15 172.8(4) .
C2 C1 N2 O9 5.9(6) .
C2 C3 C4 C5 0.2(5) .
C3 C2 S2 C5 -0.2(3) .
C3 C4 C5 C6 179.2(4) .
C3 C4 C5 S2 -0.3(5) .
C4 C5 C6 C7 20.9(7) .
C4 C5 C6 C11 -158.7(4) .
C4 C5 S2 C2 0.3(3) .
C5 C6 C7 C8 -176.8(4) .
C5 C6 C11 C10 178.2(4) .
C6 C5 S2 C2 -179.3(3) .
C6 C7 C8 C9 -1.6(7) .
C7 C6 C11 C10 -1.4(6) .
C7 C8 C9 C10 -1.2(7) .
C8 C9 C10 C11 2.7(7) .
C9 C10 C11 C6 -1.4(7) .
C11 C6 C7 C8 2.9(6) .
C12 C15 N2 C1 21.9(4) .
C12 C15 N2 O9 -171.1(3) .
C12 N1 O16 Tb1 105.4(4) 1_455
C13 C12 C15 C16 -31.3(5) .
C13 C12 C15 C17 98.0(4) .
C13 C12 C15 N2 -143.9(3) .
C13 C12 N1 C1 146.9(4) .
C13 C12 N1 O16 -40.1(5) .
C14 C12 C15 C16 -160.9(3) .
C14 C12 C15 C17 -31.5(5) .
C14 C12 C15 N2 86.5(4) .
C14 C12 N1 C1 -93.4(4) .
C14 C12 N1 O16 79.5(4) .
C15 C12 N1 C1 25.3(4) .
C15 C12 N1 O16 -161.7(3) .
C15 N2 O9 Tb2 86.8(5) .
C16 C15 N2 C1 -96.4(4) .
C16 C15 N2 O9 70.7(4) .
C17 C15 N2 C1 143.8(4) .
C17 C15 N2 O9 -49.1(5) .
C18 C19 C20 C21 175.3(4) .
C18 C19 S1 C22 -175.2(3) .
C18 N3 O8 Tb2 -89.3(4) .
C18 N4 O1 Tb1 -111.8(5) .
C19 C18 N3 C32 160.5(4) .
C19 C18 N3 O8 -6.5(6) .
C19 C18 N4 C29 177.4(4) .
C19 C18 N4 O1 7.6(6) .
C19 C20 C21 C22 -1.2(5) .
C20 C19 S1 C22 -0.2(3) .
C20 C21 C22 C23 178.8(4) .
C20 C21 C22 S1 1.1(4) .
C21 C22 C23 C24 27.0(6) .
C21 C22 C23 C28 -152.2(4) .
C21 C22 S1 C19 -0.5(3) .
C22 C23 C24 C25 -178.4(4) .
C22 C23 C28 C27 178.3(4) .
C23 C22 S1 C19 -178.5(3) .
C23 C24 C25 C26 0.4(7) .
C24 C23 C28 C27 -1.0(6) .
C24 C25 C26 C27 -1.5(7) .
C25 C26 C27 C28 1.4(7) .
C26 C27 C28 C23 -0.1(7) .
C28 C23 C24 C25 0.8(6) .
C29 C32 N3 C18 29.9(4) .
C29 C32 N3 O8 -162.8(3) .
C29 N4 O1 Tb1 79.4(6) .
C30 C29 C32 C33 -35.6(5) .
C30 C29 C32 C34 94.9(4) .
C30 C29 C32 N3 -146.6(3) .
C30 C29 N4 C18 144.3(3) .
C30 C29 N4 O1 -45.6(5) .
C31 C29 C32 C33 -164.4(3) .
C31 C29 C32 C34 -33.9(4) .
C31 C29 C32 N3 84.6(4) .
C31 C29 N4 C18 -95.4(4) .
C31 C29 N4 O1 74.7(4) .
C32 C29 N4 C18 23.6(4) .
C32 C29 N4 O1 -166.3(3) .
C32 N3 O8 Tb2 104.9(3) .
C33 C32 N3 C18 -88.0(4) .
C33 C32 N3 O8 79.4(4) .
C34 C32 N3 C18 150.7(3) .
C34 C32 N3 O8 -41.9(5) .
C35 C36 C37 C38 -176.2(4) .
C35 C36 C37 O15 3.6(7) .
C36 C35 C39 F10 62.1(14) .
C36 C35 C39 F11 -59(2) .
C36 C35 C39 F12 167.7(12) .
C36 C35 C39 F10' 20.8(8) .
C36 C35 C39 F11' -94.9(5) .
C36 C35 C39 F12' 148.1(6) .
C36 C35 O14 Tb2 -16.1(7) .
C36 C37 C38 F7 -27.1(9) .
C36 C37 C38 F8 -159.8(7) .
C36 C37 C38 F9 86.3(6) .
C36 C37 C38 F7' -69.6(7) .
C36 C37 C38 F8' 179.2(8) .
C36 C37 C38 F9' 44.3(10) .
C36 C37 O15 Tb2 17.8(6) .
C38 C37 O15 Tb2 -162.3(3) .
C39 C35 C36 C37 173.2(4) .
C39 C35 O14 Tb2 165.9(3) .
C40 C41 C42 C43 -172.8(4) .
C40 C41 C42 O11 5.6(7) .
C41 C40 C44 F4 12.8(6) .
C41 C40 C44 F5 -107.6(4) .
C41 C40 C44 F6 134.3(4) .
C41 C40 O10 Tb2 -14.7(6) .
C41 C42 C43 F1 -51.9(5) .
C41 C42 C43 F2 67.7(5) .
C41 C42 C43 F3 -172.9(3) .
C41 C42 O11 Tb2 12.3(6) .
C43 C42 O11 Tb2 -169.3(2) .
C44 C40 C41 C42 174.4(4) .
C44 C40 O10 Tb2 166.7(2) .
C45 C46 C47 C48 -179.2(4) .
C45 C46 C47 O12 -0.2(7) .
C46 C45 C49 F13 144.7(8) .
C46 C45 C49 F14 -99.4(11) .
C46 C45 C49 F15 26.8(13) .
C46 C45 C49 F13' 118.4(12) .
C46 C45 C49 F14' -123.3(9) .
C46 C45 C49 F15' -6.2(10) .
C46 C45 O13 Tb2 -0.1(6) .
C46 C47 C48 F16 131.7(7) .
C46 C47 C48 F17 -112.9(7) .
C46 C47 C48 F18 11.9(8) .
C46 C47 C48 F16' 94.5(15) .
C46 C47 C48 F17' -137.5(11) .
C46 C47 C48 F18' -22.4(13) .
C46 C47 O12 Tb2 0.1(6) .
C48 C47 O12 Tb2 179.2(2) .
C49 C45 C46 C47 -179.6(4) .
C49 C45 O13 Tb2 179.7(2) .
C50 C51 C52 C54 -177.3(4) .
C50 C51 C52 O6 1.2(8) .
C51 C50 C53 F28 101.3(11) .
C51 C50 C53 F29 -139.2(12) .
C51 C50 C53 F30 -17.3(11) .
C51 C50 C53 F28' 130.0(14) .
C51 C50 C53 F29' -113.6(13) .
C51 C50 C53 F30' 9.1(15) .
C51 C50 O7 Tb1 -6.8(7) .
C51 C52 C54 F25 -114.2(13) .
C51 C52 C54 F26 3.4(12) .
C51 C52 C54 F27 122.8(13) .
C51 C52 C54 F25' -141.8(11) .
C51 C52 C54 F26' -17.7(12) .
C51 C52 C54 F27' 103.3(10) .
C51 C52 O6 Tb1 4.1(7) .
C53 C50 C51 C52 179.8(4) .
C53 C50 O7 Tb1 173.7(3) .
C54 C52 O6 Tb1 -177.4(3) .
C55 C56 C57 C58 -179.5(4) .
C55 C56 C57 O4 1.5(7) .
C56 C55 C59 F22 23.3(6) .
C56 C55 C59 F23 144.5(4) .
C56 C55 C59 F24 -97.3(5) .
C56 C55 O5 Tb1 10.9(6) .
C56 C57 C58 F19 9.1(6) .
C56 C57 C58 F20 -111.5(4) .
C56 C57 C58 F21 130.0(4) .
C56 C57 O4 Tb1 -18.4(6) .
C58 C57 O4 Tb1 162.6(3) .
C59 C55 C56 C57 -179.4(4) .
C59 C55 O5 Tb1 -167.2(3) .
C60 C61 C62 C63 -176.7(4) .
C60 C61 C62 O2 4.9(7) .
C61 C60 C64 F34 93.7(5) .
C61 C60 C64 F35 -25.3(5) .
C61 C60 C64 F36 -147.5(4) .
C61 C60 O3 Tb1 -19.3(6) .
C61 C62 C63 F31 -113.1(5) .
C61 C62 C63 F32 6.4(6) .
C61 C62 C63 F33 128.4(4) .
C61 C62 O2 Tb1 6.9(7) .
C63 C62 O2 Tb1 -171.6(2) .
C64 C60 C61 C62 -175.9(4) .
C64 C60 O3 Tb1 158.3(3) .
N1 C1 C2 C3 -10.6(7) .
N1 C1 C2 S2 169.5(3) .
N1 C1 N2 C15 -6.8(5) .
N1 C1 N2 O9 -173.7(3) .
N1 C12 C15 C16 86.9(4) .
N1 C12 C15 C17 -143.8(3) .
N1 C12 C15 N2 -25.7(4) .
N2 C1 C2 C3 169.9(4) .
N2 C1 C2 S2 -10.0(6) .
N2 C1 N1 C12 -12.7(5) .
N2 C1 N1 O16 174.5(3) .
N3 C18 C19 C20 170.6(4) .
N3 C18 C19 S1 -15.3(6) .
N3 C18 N4 C29 -6.0(4) .
N3 C18 N4 O1 -175.8(3) .
N4 C18 C19 C20 -13.5(7) .
N4 C18 C19 S1 160.7(3) .
N4 C18 N3 C32 -16.1(4) .
N4 C18 N3 O8 176.9(3) .
N4 C29 C32 C33 82.1(4) .
N4 C29 C32 C34 -147.5(3) .
N4 C29 C32 N3 -29.0(3) .
O2 C62 C63 F31 65.5(5) .
O2 C62 C63 F32 -175.0(4) .
O2 C62 C63 F33 -53.0(5) .
O3 C60 C61 C62 1.7(7) .
O3 C60 C64 F34 -84.2(5) .
O3 C60 C64 F35 156.8(4) .
O3 C60 C64 F36 34.6(5) .
O4 C57 C58 F19 -171.7(3) .
O4 C57 C58 F20 67.7(5) .
O4 C57 C58 F21 -50.8(5) .
O5 C55 C56 C57 2.5(7) .
O5 C55 C59 F22 -158.3(4) .
O5 C55 C59 F23 -37.1(5) .
O5 C55 C59 F24 81.0(5) .
O6 C52 C54 F25 67.1(13) .
O6 C52 C54 F26 -175.3(11) .
O6 C52 C54 F27 -55.9(13) .
O6 C52 C54 F25' 39.5(12) .
O6 C52 C54 F26' 163.6(11) .
O6 C52 C54 F27' -75.4(9) .
O7 C50 C51 C52 0.3(8) .
O7 C50 C53 F28 -79.0(11) .
O7 C50 C53 F29 40.4(12) .
O7 C50 C53 F30 162.4(10) .
O7 C50 C53 F28' -50.4(15) .
O7 C50 C53 F29' 66.0(13) .
O7 C50 C53 F30' -171.3(14) .
O10 C40 C41 C42 -4.1(7) .
O10 C40 C44 F4 -168.5(4) .
O10 C40 C44 F5 71.1(5) .
O10 C40 C44 F6 -47.0(5) .
O11 C42 C43 F1 129.5(4) .
O11 C42 C43 F2 -110.9(4) .
O11 C42 C43 F3 8.4(5) .
O12 C47 C48 F16 -47.5(7) .
O12 C47 C48 F17 67.9(7) .
O12 C47 C48 F18 -167.3(7) .
O12 C47 C48 F16' -84.8(15) .
O12 C47 C48 F17' 43.3(12) .
O12 C47 C48 F18' 158.4(13) .
O13 C45 C46 C47 0.2(7) .
O13 C45 C49 F13 -35.1(9) .
O13 C45 C49 F14 80.8(11) .
O13 C45 C49 F15 -153.0(13) .
O13 C45 C49 F13' -61.4(12) .
O13 C45 C49 F14' 56.9(9) .
O13 C45 C49 F15' 174.0(10) .
O14 C35 C36 C37 -4.7(7) .
O14 C35 C39 F10 -119.7(13) .
O14 C35 C39 F11 119(2) .
O14 C35 C39 F12 -14.2(13) .
O14 C35 C39 F10' -161.1(6) .
O14 C35 C39 F11' 83.2(5) .
O14 C35 C39 F12' -33.8(7) .
O15 C37 C38 F7 153.0(8) .
O15 C37 C38 F8 20.3(8) .
O15 C37 C38 F9 -93.5(6) .
O15 C37 C38 F7' 110.5(7) .
O15 C37 C38 F8' -0.6(9) .
O15 C37 C38 F9' -135.5(9) .
S1 C19 C20 C21 0.8(4) .
S1 C22 C23 C24 -155.4(3) .
S1 C22 C23 C28 25.4(5) .
S2 C2 C3 C4 0.0(5) .
S2 C5 C6 C7 -159.6(3) .
S2 C5 C6 C11 20.8(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 0.500 0.000 0.500 296.6 6.7
2 0.500 0.500 0.000 296.6 6.7