#------------------------------------------------------------------------------
#$Date: 2020-11-29 02:09:34 +0200 (Sun, 29 Nov 2020) $
#$Revision: 259279 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/89/4038935.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_4038935
loop_
_publ_author_name
'Hempe, Matthias'
'Harrison, Alastair K.'
'Ward, Jonathan S.'
'Batsanov, Andrei S.'
'Fox, Mark A.'
'Dias, Fernando B.'
'Bryce, Martin R.'
_publ_section_title
;
 Cyclophane Molecules Exhibiting Thermally Activated Delayed Fluorescence:
 Linking Donor Units to Influence Molecular Conformation
;
_journal_name_full               'The Journal of Organic Chemistry'
_journal_paper_doi               10.1021/acs.joc.0c02174
_journal_year                    2020
_chemical_formula_moiety         'C46 H28 N2 O6 S3, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C47.5 H31 Cl3 N2 O6 S3'
_chemical_formula_weight         928.27
_chemical_melting_point          601
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                93.0414(17)
_cell_angle_beta                 92.2764(15)
_cell_angle_gamma                105.0333(16)
_cell_formula_units_Z            2
_cell_length_a                   7.3272(2)
_cell_length_b                   13.9943(5)
_cell_length_c                   21.5754(8)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    120
_cell_measurement_theta_max      75.47
_cell_measurement_theta_min      3.75
_cell_volume                     2130.31(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 multi-CPU (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23375
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         75.589
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.764
_exptl_absorpt_correction_T_max  0.9298
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS-2014/5 (Krause et al., 2015) was used for absorption correction. wR2(int) was 
 0.0669 before and 0.0535 after correction. The Ratio of minimum to maximum 
 transmission is 0.6583. The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00050(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         7777
_refine_ls_number_restraints     529
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0610P)²+3.8840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5978
_reflns_number_total             7777
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            2a.cif
_cod_data_source_block           2a_16s448
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C47.50 H31 Cl3 N2 O6 S3'
_cod_database_code               4038935
_shelx_shelxl_version_number     2016/6
_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   0.886
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O5B-C45B \\sim O5-C45
 with sigma of 0.02
 O6-C45 \\sim O6B-C45B
 with sigma of 0.02
 O5-C46 \\sim O5B-C46B
 with sigma of 0.02
 C28-C27 \\sim C28B-C27B
 with sigma of 0.02
 C29B-C28B \\sim C29-C28
 with sigma of 0.02
 C30-C29 \\sim C30B-C29B
 with sigma of 0.02
 S3B-C26B \\sim S3-C26
 with sigma of 0.02
 C27-C26 \\sim C27B-C26B
 with sigma of 0.02
 O3-C37 \\sim O3B-C37
 with sigma of 0.02
 C35B-C34B \\sim C35-C34
 with sigma of 0.02
 C36-C35 \\sim C36-C35B
 with sigma of 0.02
 C34-C33 \\sim C34B-C33B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O6) = Uanis(O6B)
Uanis(C42B) = Uanis(C42)
Uanis(S3) = Uanis(S3B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C45, O6, O5, C41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(S3B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(H36A)=Sof(H37C)=Sof(H37D)=
 Sof(C25B)=Sof(C26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=
 Sof(C30B)=Sof(H30B)=Sof(C32B)=Sof(C33B)=Sof(H33B)=Sof(C34B)=Sof(H34B)=
 Sof(C35B)=Sof(H35B)=Sof(C38B)=Sof(C41B)=Sof(C40B)=Sof(H40B)=Sof(C39B)=
 Sof(C44B)=Sof(H44B)=Sof(C43B)=Sof(H43B)=Sof(C42B)=Sof(H42B)=Sof(C45B)=
 Sof(C46B)=Sof(H46C)=Sof(H46D)=1-FVAR(1)
 Sof(S3)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(H36)=Sof(H37A)=Sof(H37B)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(C30)=Sof(H30)=
 Sof(C32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C38)=
 Sof(C41)=Sof(C40)=Sof(H40)=Sof(C39)=Sof(C44)=Sof(H44)=Sof(C43)=Sof(H43)=
 Sof(C42)=Sof(H42)=Sof(C45)=Sof(C46)=Sof(H46A)=Sof(H46B)=FVAR(1)
 Fixed Sof: Cl1(0.8) Cl2(0.67) Cl5(0.45) Cl6(0.45) Cl4(0.23) Cl3(0.15)
 Cl7(0.07) Cl8(0.1) C4S(0.45) H4SA(0.45) H4SB(0.45) C1S(0.67) H1SA(0.67)
 H1SB(0.67) C3S(0.08) H3SA(0.08) H3SB(0.08) C2S(0.15) H2SA(0.15) H2SB(0.15)
 Cl9(0.08)
6.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C37(H37C,H37D), C46(H46A,H46B), C46B(H46C,H46D), C4S(H4SA,
 H4SB), C1S(H1SA,H1SB), C2S(H2SA,H2SB)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C15(H15), C16(H16),
 C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C36(H36), C36(H36A),
 C27(H27), C28(H28), C30(H30), C33(H33), C34(H34), C35(H35), C40(H40), C44(H44),
  C43(H43), C42(H42), C27B(H27B), C28B(H28B), C30B(H30B), C33B(H33B),
 C34B(H34B), C35B(H35B), C40B(H40B), C44B(H44B), C43B(H43B), C42B(H42B)
6.c Fitted hexagon refined as free rotating group:
 C41(C40,C39,C44,C43,C42), C41B(C40B,C39B,C44B,C43B,C42B)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.72286(10) 0.66374(6) 0.40286(4) 0.0327(2) Uani 1 1 d . U . . .
S2 S -0.40605(10) 0.25144(7) 0.28520(4) 0.0353(2) Uani 1 1 d . U . . .
S3 S 0.0053(3) 1.04184(18) 0.25779(11) 0.0350(4) Uani 0.729(4) 1 d D U P A 1
S3B S 0.0542(8) 1.0471(6) 0.2456(3) 0.0350(4) Uani 0.271(4) 1 d D U P A 2
O1 O 0.8735(3) 0.65080(17) 0.36561(15) 0.0484(7) Uani 1 1 d . U . . .
O2 O 0.7623(3) 0.68164(18) 0.46866(14) 0.0468(7) Uani 1 1 d . U . . .
O3 O 0.2833(7) 0.3789(4) 0.0912(2) 0.0452(12) Uani 0.729(4) 1 d D U P A 1
O4 O 0.4300(6) 0.5038(3) 0.15993(18) 0.0529(11) Uani 0.729(4) 1 d . U P A 1
O5 O 0.5722(6) 0.8409(4) 0.08954(18) 0.0485(10) Uani 0.729(4) 1 d D U P A 1
O6 O 0.4341(10) 0.8767(4) 0.0033(3) 0.0695(14) Uani 0.729(4) 1 d D U P A 1
O3B O 0.3254(19) 0.4100(10) 0.1085(6) 0.038(4) Uiso 0.271(4) 1 d D U P A 2
O4B O 0.1753(13) 0.3260(7) 0.0248(4) 0.043(3) Uiso 0.271(4) 1 d . U P A 2
O5B O 0.5394(15) 0.7810(10) 0.0933(5) 0.047(3) Uiso 0.271(4) 1 d D U P A 2
O6B O 0.480(3) 0.8498(13) 0.0033(10) 0.0695(14) Uani 0.271(4) 1 d D U P A 2
N1 N -0.0087(3) 0.37171(18) 0.33255(13) 0.0268(6) Uani 1 1 d . U . . .
N2 N 0.2964(3) 0.93483(18) 0.30558(12) 0.0231(5) Uani 1 1 d . U . . .
C1 C 0.5149(4) 0.5672(2) 0.38593(16) 0.0268(7) Uani 1 1 d . U . . .
C2 C 0.4897(4) 0.4683(2) 0.39759(17) 0.0317(8) Uani 1 1 d . U . . .
H2 H 0.588545 0.445683 0.416606 0.038 Uiso 1 1 calc R . . . .
C3 C 0.3140(4) 0.4035(2) 0.38034(17) 0.0329(8) Uani 1 1 d . U . . .
H3 H 0.291254 0.335092 0.387515 0.039 Uiso 1 1 calc R . . . .
C4 C 0.1717(4) 0.4388(2) 0.35260(16) 0.0279(7) Uani 1 1 d . U . . .
C5 C 0.1976(4) 0.5381(2) 0.34203(15) 0.0247(7) Uani 1 1 d . U . . .
H5 H 0.098375 0.561028 0.323520 0.030 Uiso 1 1 calc R . . . .
C6 C 0.3731(4) 0.6036(2) 0.35925(15) 0.0234(6) Uani 1 1 d . U . . .
C7 C 0.4328(4) 0.7120(2) 0.35285(15) 0.0228(6) Uani 1 1 d . U . . .
C8 C 0.3254(4) 0.7720(2) 0.33004(14) 0.0223(6) Uani 1 1 d . U . . .
H8 H 0.197325 0.744567 0.315549 0.027 Uiso 1 1 calc R . . . .
C9 C 0.4089(4) 0.8729(2) 0.32884(14) 0.0222(6) Uani 1 1 d . U . . .
C10 C 0.5974(4) 0.9142(2) 0.34972(15) 0.0262(7) Uani 1 1 d . U . . .
H10 H 0.651577 0.983475 0.348364 0.031 Uiso 1 1 calc R . . . .
C11 C 0.7055(4) 0.8547(2) 0.37236(16) 0.0286(7) Uani 1 1 d . U . . .
H11 H 0.834062 0.881736 0.386399 0.034 Uiso 1 1 calc R . . . .
C12 C 0.6197(4) 0.7543(2) 0.37385(16) 0.0263(7) Uani 1 1 d . U . . .
C13 C -0.0221(4) 0.3243(2) 0.27259(16) 0.0272(7) Uani 1 1 d . U . . .
C14 C -0.1952(4) 0.2653(2) 0.24609(16) 0.0294(7) Uani 1 1 d . U . . .
C15 C -0.2063(5) 0.2203(3) 0.18679(17) 0.0370(8) Uani 1 1 d . U . . .
H15 H -0.323942 0.178928 0.170051 0.044 Uiso 1 1 calc R . . . .
C16 C -0.0487(5) 0.2346(3) 0.15150(18) 0.0405(8) Uani 1 1 d . U . . .
H16 H -0.058318 0.204270 0.110630 0.049 Uiso 1 1 calc R . . . .
C17 C 0.1237(5) 0.2940(3) 0.17664(18) 0.0376(8) Uani 1 1 d . U . . .
C18 C 0.1366(4) 0.3373(2) 0.23655(17) 0.0323(7) Uani 1 1 d . U . . .
H18 H 0.255624 0.376637 0.253554 0.039 Uiso 1 1 calc R . . . .
C19 C -0.1314(4) 0.3319(2) 0.37925(16) 0.0246(7) Uani 1 1 d . U . . .
C20 C -0.3135(4) 0.2695(2) 0.36257(15) 0.0245(6) Uani 1 1 d . U . . .
C21 C -0.4308(4) 0.2270(2) 0.40855(17) 0.0303(7) Uani 1 1 d . U . . .
H21 H -0.550062 0.182050 0.396916 0.036 Uiso 1 1 calc R . . . .
C22 C -0.3764(4) 0.2491(3) 0.47061(18) 0.0369(8) Uani 1 1 d . U . . .
H22 H -0.458202 0.220496 0.501622 0.044 Uiso 1 1 calc R . . . .
C23 C -0.2013(4) 0.3134(3) 0.48729(18) 0.0370(8) Uani 1 1 d . U . . .
H23 H -0.163625 0.329859 0.529995 0.044 Uiso 1 1 calc R . . . .
C24 C -0.0801(4) 0.3540(2) 0.44195(16) 0.0315(7) Uani 1 1 d . U . . .
H24 H 0.039999 0.397723 0.454171 0.038 Uiso 1 1 calc R . . . .
C31 C 0.2234(4) 0.9899(2) 0.35048(15) 0.0231(6) Uani 1 1 d . U . . .
C36 C 0.2623(4) 0.9864(2) 0.41367(15) 0.0257(7) Uani 1 1 d D U . . .
H36 H 0.337349 0.944166 0.426487 0.031 Uiso 0.729(4) 1 calc R . P A 1
H36A H 0.338614 0.947624 0.430556 0.031 Uiso 0.271(4) 1 calc R . P A 2
C37 C 0.2969(6) 0.3120(3) 0.1388(2) 0.0483(10) Uani 1 1 d D U . . .
H37A H 0.411565 0.340869 0.166312 0.058 Uiso 0.729(4) 1 calc R . P A 1
H37B H 0.308212 0.248321 0.119290 0.058 Uiso 0.729(4) 1 calc R . P A 1
H37C H 0.281496 0.257403 0.106323 0.058 Uiso 0.271(4) 1 calc R . P A 2
H37D H 0.409624 0.313400 0.166047 0.058 Uiso 0.271(4) 1 calc R . P A 2
C25 C 0.3165(12) 0.9673(6) 0.2457(4) 0.0246(19) Uani 0.729(4) 1 d . U P A 1
C26 C 0.1944(12) 1.0182(6) 0.2178(3) 0.0325(15) Uani 0.729(4) 1 d D U P A 1
C27 C 0.2166(11) 1.0463(5) 0.1572(3) 0.0437(15) Uani 0.729(4) 1 d D U P A 1
H27 H 0.133613 1.080774 0.139405 0.052 Uiso 0.729(4) 1 calc R . P A 1
C28 C 0.3570(11) 1.0251(5) 0.1223(3) 0.0483(16) Uani 0.729(4) 1 d D U P A 1
H28 H 0.370474 1.045558 0.081031 0.058 Uiso 0.729(4) 1 calc R . P A 1
C29 C 0.4778(9) 0.9742(5) 0.1472(3) 0.0359(13) Uani 0.729(4) 1 d D U P A 1
C30 C 0.4556(8) 0.9462(5) 0.2083(3) 0.0274(14) Uani 0.729(4) 1 d D U P A 1
H30 H 0.538740 0.911218 0.225323 0.033 Uiso 0.729(4) 1 calc R . P A 1
C32 C 0.1036(13) 1.0491(7) 0.3358(5) 0.0225(17) Uani 0.729(4) 1 d . U P A 1
C33 C 0.0388(9) 1.1072(5) 0.3802(4) 0.0210(15) Uani 0.729(4) 1 d D U P A 1
H33 H -0.038294 1.148559 0.367440 0.025 Uiso 0.729(4) 1 calc R . P A 1
C34 C 0.0869(10) 1.1045(5) 0.4424(4) 0.0242(15) Uani 0.729(4) 1 d D U P A 1
H34 H 0.045698 1.144648 0.472839 0.029 Uiso 0.729(4) 1 calc R . P A 1
C35 C 0.1968(17) 1.0419(7) 0.4596(5) 0.026(2) Uani 0.729(4) 1 d D U P A 1
H35 H 0.227358 1.036787 0.502296 0.031 Uiso 0.729(4) 1 calc R . P A 1
C38 C 0.3557(7) 0.4724(5) 0.1098(2) 0.0373(12) Uani 0.729(4) 1 d . U P A 1
C41 C 0.3999(6) 0.7062(2) 0.02547(19) 0.0418(13) Uani 0.729(4) 1 d . U P A 1
C40 C 0.4127(5) 0.6414(3) 0.07109(13) 0.0389(12) Uani 0.729(4) 1 d G U P A 1
H40 H 0.472376 0.666424 0.110668 0.047 Uiso 0.729(4) 1 calc R . P A 1
C39 C 0.3380(5) 0.5399(3) 0.05881(16) 0.0385(13) Uani 0.729(4) 1 d G U P A 1
C44 C 0.2506(5) 0.5032(2) 0.00091(19) 0.0448(15) Uani 0.729(4) 1 d G U P A 1
H44 H 0.199620 0.433846 -0.007487 0.054 Uiso 0.729(4) 1 calc R . P A 1
C43 C 0.2379(6) 0.5680(4) -0.04472(14) 0.0575(18) Uani 0.729(4) 1 d G U P A 1
H43 H 0.178180 0.542972 -0.084298 0.069 Uiso 0.729(4) 1 calc R . P A 1
C42 C 0.3125(7) 0.6695(3) -0.03244(17) 0.0589(13) Uani 0.729(4) 1 d G U P A 1
H42 H 0.303838 0.713825 -0.063626 0.071 Uiso 0.729(4) 1 calc R . P A 1
C45 C 0.4742(9) 0.8193(6) 0.0392(3) 0.0463(13) Uani 0.729(4) 1 d D U P A 1
C46 C 0.6300(8) 0.9457(4) 0.1106(2) 0.0446(13) Uani 0.729(4) 1 d D U P A 1
H46A H 0.655085 0.986472 0.074231 0.053 Uiso 0.729(4) 1 calc R . P A 1
H46B H 0.748564 0.959364 0.137083 0.053 Uiso 0.729(4) 1 calc R . P A 1
C25B C 0.345(4) 0.9555(18) 0.2389(12) 0.020(5) Uiso 0.271(4) 1 d . U P A 2
C26B C 0.240(3) 1.014(2) 0.2122(11) 0.033(6) Uiso 0.271(4) 1 d D U P A 2
C27B C 0.288(3) 1.0418(17) 0.1532(11) 0.055(7) Uiso 0.271(4) 1 d D U P A 2
H27B H 0.233134 1.088025 0.133869 0.066 Uiso 0.271(4) 1 calc R . P A 2
C28B C 0.414(3) 1.0023(17) 0.1233(11) 0.054(6) Uiso 0.271(4) 1 d D U P A 2
H28B H 0.439351 1.018557 0.081740 0.065 Uiso 0.271(4) 1 calc R . P A 2
C29B C 0.508(3) 0.9400(15) 0.1502(8) 0.046(5) Uiso 0.271(4) 1 d D U P A 2
C30B C 0.477(2) 0.9194(13) 0.2126(7) 0.024(5) Uiso 0.271(4) 1 d D U P A 2
H30B H 0.546700 0.882045 0.234637 0.029 Uiso 0.271(4) 1 calc R . P A 2
C32B C 0.105(4) 1.048(2) 0.3208(10) 0.019(6) Uiso 0.271(4) 1 d . U P A 2
C33B C 0.043(3) 1.103(2) 0.3616(9) 0.024(5) Uiso 0.271(4) 1 d D U P A 2
H33B H -0.025093 1.146501 0.345778 0.029 Uiso 0.271(4) 1 calc R . P A 2
C34B C 0.068(3) 1.1042(19) 0.4249(11) 0.027(6) Uiso 0.271(4) 1 d D U P A 2
H34B H 0.012496 1.143777 0.451331 0.032 Uiso 0.271(4) 1 calc R . P A 2
C35B C 0.176(5) 1.046(3) 0.4495(12) 0.035(9) Uiso 0.271(4) 1 d D U P A 2
H35B H 0.193356 1.047712 0.493425 0.042 Uiso 0.271(4) 1 calc R . P A 2
C38B C 0.2502(16) 0.4041(9) 0.0497(6) 0.026(3) Uiso 0.271(4) 1 d . U P A 2
C41B C 0.381(2) 0.6753(7) 0.0184(6) 0.056(5) Uiso 0.271(4) 1 d . U P A 2
C40B C 0.3655(18) 0.5903(9) 0.0505(5) 0.039(4) Uiso 0.271(4) 1 d G U P A 2
H40B H 0.419378 0.595282 0.091735 0.046 Uiso 0.271(4) 1 calc R . P A 2
C39B C 0.2714(18) 0.4981(7) 0.0224(6) 0.035(4) Uiso 0.271(4) 1 d G U P A 2
C44B C 0.1926(17) 0.4908(7) -0.0379(6) 0.056(4) Uiso 0.271(4) 1 d G U P A 2
H44B H 0.128302 0.427752 -0.057152 0.067 Uiso 0.271(4) 1 calc R . P A 2
C43B C 0.208(2) 0.5758(9) -0.0701(5) 0.060(5) Uiso 0.271(4) 1 d G U P A 2
H43B H 0.153896 0.570784 -0.111267 0.072 Uiso 0.271(4) 1 calc R . P A 2
C42B C 0.302(2) 0.6680(7) -0.0419(6) 0.0589(13) Uani 0.271(4) 1 d G U P A 2
H42B H 0.312230 0.726067 -0.063882 0.071 Uiso 0.271(4) 1 calc R . P A 2
C45B C 0.465(3) 0.7772(16) 0.0354(7) 0.048(5) Uiso 0.271(4) 1 d D U P A 2
C46B C 0.642(3) 0.8857(15) 0.1158(11) 0.073(6) Uiso 0.271(4) 1 d D U P A 2
H46C H 0.693522 0.923179 0.079962 0.087 Uiso 0.271(4) 1 calc R . P A 2
H46D H 0.750079 0.884386 0.144631 0.087 Uiso 0.271(4) 1 calc R . P A 2
Cl1 Cl 1.0525(3) 0.6210(2) 0.18545(9) 0.0906(6) Uani 0.8 1 d D U P . .
Cl2 Cl 0.8628(3) 0.77807(15) 0.21798(10) 0.0697(5) Uani 0.67 1 d . U P B 1
Cl5 Cl 0.9987(8) 0.9810(5) 0.0099(2) 0.0852(15) Uani 0.45 1 d . U P C 1
Cl6 Cl 0.9003(4) 0.7723(3) 0.01112(18) 0.1119(15) Uani 0.45 1 d . U P C 1
Cl4 Cl 0.6808(9) 0.5071(5) 0.2423(4) 0.092(2) Uani 0.23 1 d D U P D 2
Cl3 Cl 0.7465(18) 0.7200(8) 0.2417(5) 0.087(3) Uani 0.15 1 d . U P D 2
Cl7 Cl 1.008(2) 0.7980(14) 0.0900(8) 0.059(4) Uiso 0.07 1 d . U P E 2
Cl8 Cl 1.018(2) 0.7436(12) 0.1016(7) 0.077(4) Uiso 0.1 1 d . U P F 3
C4S C 1.0275(17) 0.8797(9) 0.0489(6) 0.073(3) Uiso 0.45 1 d . U P C 1
H4SA H 1.163097 0.880534 0.051614 0.088 Uiso 0.45 1 calc R . P C 1
H4SB H 0.985158 0.884086 0.091709 0.088 Uiso 0.45 1 calc R . P C 1
C1S C 0.8384(10) 0.6492(6) 0.2027(4) 0.076(2) Uani 0.67 1 d . U P B 1
H1SA H 0.787825 0.613812 0.239428 0.091 Uiso 0.67 1 calc R . P B 1
H1SB H 0.745100 0.624458 0.167225 0.091 Uiso 0.67 1 calc R . P B 1
C3S C 0.874(5) 0.541(4) 0.208(3) 0.068(16) Uiso 0.08 1 d D U P D 2
H3SA H 0.942774 0.497328 0.227761 0.082 Uiso 0.08 1 calc R . P D 2
H3SB H 0.828460 0.505278 0.166700 0.082 Uiso 0.08 1 calc R . P D 2
C2S C 0.630(4) 0.609(2) 0.2129(14) 0.053(7) Uiso 0.15 1 d . U P D 2
H2SA H 0.649368 0.605978 0.167751 0.063 Uiso 0.15 1 calc R . P D 2
H2SB H 0.493703 0.602788 0.217542 0.063 Uiso 0.15 1 calc R . P D 2
Cl9 Cl 1.057(2) 0.6586(12) 0.1584(8) 0.055(4) Uiso 0.08 1 d . U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 -1.00 0.0580
1.00 -1.00 1.00 0.0770
0.00 1.00 -1.00 0.0260
0.00 -1.00 1.00 0.0410
0.00 -1.00 0.00 0.0450
0.00 0.00 1.00 0.0120
0.00 0.00 -1.00 0.0060
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 S1 C1 111.39(15) . . ?
O1 S1 C12 111.02(16) . . ?
O2 S1 O1 117.67(16) . . ?
O2 S1 C1 110.85(16) . . ?
O2 S1 C12 110.19(15) . . ?
C12 S1 C1 93.02(14) . . ?
C20 S2 C14 99.91(15) . . ?
C26 S3 C32 99.1(4) . . ?
C32B S3B C26B 103.4(14) . . ?
C38 O3 C37 113.0(5) . . ?
C45 O5 C46 116.3(5) . . ?
C38B O3B C37 115.5(11) . . ?
C45B O5B C46B 111.3(16) . . ?
C13 N1 C4 116.6(2) . . ?
C13 N1 C19 122.0(2) . . ?
C19 N1 C4 117.4(3) . . ?
C9 N2 C25B 108.5(9) . . ?
C31 N2 C9 116.5(2) . . ?
C31 N2 C25B 130.4(9) . . ?
C25 N2 C9 120.5(4) . . ?
C25 N2 C31 118.9(4) . . ?
C2 C1 S1 126.3(2) . . ?
C2 C1 C6 123.0(3) . . ?
C6 C1 S1 110.6(2) . . ?
C1 C2 C3 117.4(3) . . ?
C4 C3 C2 120.1(3) . . ?
C3 C4 N1 120.6(3) . . ?
C5 C4 N1 117.5(3) . . ?
C5 C4 C3 122.0(3) . . ?
C4 C5 C6 118.3(3) . . ?
C1 C6 C5 119.2(3) . . ?
C1 C6 C7 112.9(3) . . ?
C5 C6 C7 127.9(3) . . ?
C8 C7 C6 127.9(3) . . ?
C8 C7 C12 119.4(3) . . ?
C12 C7 C6 112.7(3) . . ?
C7 C8 C9 118.6(3) . . ?
C8 C9 N2 118.3(2) . . ?
C8 C9 C10 121.4(3) . . ?
C10 C9 N2 120.3(3) . . ?
C11 C10 C9 120.3(3) . . ?
C10 C11 C12 117.7(3) . . ?
C7 C12 S1 110.7(2) . . ?
C11 C12 S1 126.6(2) . . ?
C11 C12 C7 122.7(3) . . ?
C14 C13 N1 121.4(3) . . ?
C14 C13 C18 117.7(3) . . ?
C18 C13 N1 120.9(3) . . ?
C13 C14 S2 121.2(3) . . ?
C15 C14 S2 118.1(2) . . ?
C15 C14 C13 120.6(3) . . ?
C16 C15 C14 121.1(3) . . ?
C15 C16 C17 119.2(4) . . ?
C16 C17 C37 120.2(4) . . ?
C18 C17 C16 120.0(3) . . ?
C18 C17 C37 119.8(3) . . ?
C17 C18 C13 121.5(3) . . ?
C20 C19 N1 120.1(3) . . ?
C24 C19 N1 121.8(3) . . ?
C24 C19 C20 118.0(3) . . ?
C19 C20 S2 121.7(2) . . ?
C21 C20 S2 118.1(2) . . ?
C21 C20 C19 120.0(3) . . ?
C22 C21 C20 121.0(3) . . ?
C21 C22 C23 119.3(3) . . ?
C22 C23 C24 120.5(3) . . ?
C19 C24 C23 121.2(3) . . ?
N2 C31 C32B 111.2(9) . . ?
C36 C31 N2 121.7(3) . . ?
C36 C31 C32 114.6(5) . . ?
C36 C31 C32B 127.1(9) . . ?
C32 C31 N2 123.6(5) . . ?
C31 C36 C35 123.5(6) . . ?
C31 C36 C35B 112.1(12) . . ?
O3 C37 C17 110.1(3) . . ?
C17 C37 O3B 110.1(6) . . ?
N2 C25 C26 122.8(7) . . ?
N2 C25 C30 120.9(7) . . ?
C30 C25 C26 116.2(7) . . ?
C25 C26 S3 120.6(5) . . ?
C27 C26 S3 118.7(6) . . ?
C27 C26 C25 120.6(8) . . ?
C28 C27 C26 121.3(6) . . ?
C29 C28 C27 120.2(5) . . ?
C28 C29 C30 118.5(5) . . ?
C28 C29 C46 122.7(6) . . ?
C30 C29 C46 118.8(6) . . ?
C29 C30 C25 123.3(6) . . ?
C31 C32 S3 119.2(6) . . ?
C31 C32 C33 123.4(7) . . ?
C33 C32 S3 117.0(7) . . ?
C34 C33 C32 120.0(7) . . ?
C33 C34 C35 118.7(8) . . ?
C34 C35 C36 119.7(9) . . ?
O3 C38 C39 111.3(4) . . ?
O4 C38 O3 126.6(6) . . ?
O4 C38 C39 122.1(5) . . ?
C40 C41 C42 120.0 . . ?
C40 C41 C45 120.7(3) . . ?
C42 C41 C45 119.3(3) . . ?
C41 C40 C39 120.0 . . ?
C40 C39 C38 118.1(3) . . ?
C44 C39 C38 121.9(3) . . ?
C44 C39 C40 120.0 . . ?
C39 C44 C43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C43 C42 C41 120.0 . . ?
O5 C45 C41 112.0(5) . . ?
O6 C45 O5 127.5(7) . . ?
O6 C45 C41 120.5(6) . . ?
O5 C46 C29 110.9(4) . . ?
C26B C25B N2 112.5(19) . . ?
C30B C25B N2 120.2(18) . . ?
C30B C25B C26B 127(2) . . ?
C25B C26B S3B 124.9(19) . . ?
C27B C26B S3B 119.5(17) . . ?
C27B C26B C25B 115.5(19) . . ?
C28B C27B C26B 119(2) . . ?
C27B C28B C29B 123(2) . . ?
C28B C29B C30B 118.4(19) . . ?
C28B C29B C46B 125.2(18) . . ?
C30B C29B C46B 116.3(18) . . ?
C25B C30B C29B 115.9(19) . . ?
C31 C32B S3B 126.1(18) . . ?
C33B C32B S3B 122(2) . . ?
C33B C32B C31 112(2) . . ?
C32B C33B C34B 126(3) . . ?
C33B C34B C35B 119(3) . . ?
C34B C35B C36 124(2) . . ?
O3B C38B C39B 115.0(11) . . ?
O4B C38B O3B 119.7(13) . . ?
O4B C38B C39B 125.3(13) . . ?
C40B C41B C42B 120.0 . . ?
C40B C41B C45B 132.0(10) . . ?
C42B C41B C45B 108.0(10) . . ?
C41B C40B C39B 120.0 . . ?
C40B C39B C38B 125.7(10) . . ?
C40B C39B C44B 120.0 . . ?
C44B C39B C38B 114.3(10) . . ?
C43B C44B C39B 120.0 . . ?
C44B C43B C42B 120.0 . . ?
C43B C42B C41B 120.0 . . ?
O5B C45B C41B 106.1(14) . . ?
O6B C45B O5B 125(2) . . ?
O6B C45B C41B 128.8(16) . . ?
O5B C46B C29B 111.6(15) . . ?
Cl5 Cl5 C4S 167.7(12) 2_775 . ?
C3S Cl4 C2S 85(3) . . ?
Cl6 C4S Cl5 110.5(7) . . ?
Cl1 C1S Cl2 113.4(4) . . ?
Cl1 C3S Cl4 154(5) . . ?
Cl3 C2S Cl4 119.3(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.434(3) . ?
S1 O2 1.433(3) . ?
S1 C1 1.765(3) . ?
S1 C12 1.764(3) . ?
S2 C14 1.761(3) . ?
S2 C20 1.757(3) . ?
S3 C26 1.753(8) . ?
S3 C32 1.791(10) . ?
S3B C26B 1.723(15) . ?
S3B C32B 1.65(2) . ?
O3 C37 1.443(6) . ?
O3 C38 1.311(8) . ?
O4 C38 1.199(6) . ?
O5 C45 1.256(7) . ?
O5 C46 1.460(7) . ?
O6 C45 1.225(8) . ?
O3B C37 1.519(13) . ?
O3B C38B 1.354(18) . ?
O4B C38B 1.177(14) . ?
O5B C45B 1.335(14) . ?
O5B C46B 1.508(17) . ?
O6B C45B 1.243(16) . ?
N1 C4 1.443(4) . ?
N1 C13 1.410(4) . ?
N1 C19 1.416(4) . ?
N2 C9 1.438(4) . ?
N2 C31 1.413(4) . ?
N2 C25 1.393(9) . ?
N2 C25B 1.52(3) . ?
C1 C2 1.386(4) . ?
C1 C6 1.388(4) . ?
C2 C3 1.393(4) . ?
C3 C4 1.392(4) . ?
C4 C5 1.386(4) . ?
C5 C6 1.395(4) . ?
C6 C7 1.482(4) . ?
C7 C8 1.386(4) . ?
C7 C12 1.390(4) . ?
C8 C9 1.388(4) . ?
C9 C10 1.398(4) . ?
C10 C11 1.383(4) . ?
C11 C12 1.385(4) . ?
C13 C14 1.402(4) . ?
C13 C18 1.403(4) . ?
C14 C15 1.386(5) . ?
C15 C16 1.385(5) . ?
C16 C17 1.391(5) . ?
C17 C18 1.387(5) . ?
C17 C37 1.510(5) . ?
C19 C20 1.413(4) . ?
C19 C24 1.386(5) . ?
C20 C21 1.394(4) . ?
C21 C22 1.377(5) . ?
C22 C23 1.384(5) . ?
C23 C24 1.391(5) . ?
C31 C36 1.388(4) . ?
C31 C32 1.392(11) . ?
C31 C32B 1.48(3) . ?
C36 C35 1.402(6) . ?
C36 C35B 1.393(16) . ?
C25 C26 1.415(11) . ?
C25 C30 1.405(11) . ?
C26 C27 1.389(7) . ?
C27 C28 1.383(10) . ?
C28 C29 1.382(9) . ?
C29 C30 1.399(7) . ?
C29 C46 1.513(8) . ?
C32 C33 1.400(12) . ?
C33 C34 1.379(10) . ?
C34 C35 1.389(9) . ?
C38 C39 1.511(6) . ?
C41 C40 1.3900 . ?
C41 C42 1.3900 . ?
C41 C45 1.543(8) . ?
C40 C39 1.3900 . ?
C39 C44 1.3900 . ?
C44 C43 1.3900 . ?
C43 C42 1.3900 . ?
C25B C26B 1.39(3) . ?
C25B C30B 1.34(3) . ?
C26B C27B 1.383(17) . ?
C27B C28B 1.363(18) . ?
C28B C29B 1.377(18) . ?
C29B C30B 1.405(16) . ?
C29B C46B 1.58(3) . ?
C32B C33B 1.31(3) . ?
C33B C34B 1.369(16) . ?
C34B C35B 1.380(17) . ?
C38B C39B 1.444(15) . ?
C41B C40B 1.3900 . ?
C41B C42B 1.3900 . ?
C41B C45B 1.42(2) . ?
C40B C39B 1.3900 . ?
C39B C44B 1.3900 . ?
C44B C43B 1.3900 . ?
C43B C42B 1.3900 . ?
Cl1 C1S 1.763(7) . ?
Cl1 C3S 1.598(19) . ?
Cl2 C1S 1.777(8) . ?
Cl5 Cl5 0.696(8) 2_775 ?
Cl5 C4S 1.741(13) . ?
Cl6 C4S 1.695(12) . ?
Cl4 C3S 1.599(19) . ?
Cl4 C2S 1.71(3) . ?
Cl3 C2S 1.64(3) . ?
