#------------------------------------------------------------------------------
#$Date: 2024-12-06 22:38:47 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296695 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160143.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_7160143
loop_
_publ_author_name
'Varak, Pooja'
'Ravikanth, Mangalampalli'
_publ_section_title
;
 Pyrrolizinofluorene-embedded dithiacalixcorrole(1.0.1.1)s.
;
_journal_issue                   40
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              8125
_journal_page_last               8132
_journal_paper_doi               10.1039/d4ob01276c
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C57 H40 N2 O2 S3'
_chemical_formula_sum            'C57 H40 N2 O2 S3'
_chemical_formula_weight         881.09
_chemical_name_common            Calixcorrole
_chemical_name_systematic
'Pyrrolizinofluorene-Embedded Dithiacalixcorrole'
_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
_audit_creation_date             2024-06-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-25 deposited with the CCDC.	2024-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.139(5)
_cell_angle_beta                 90.991(6)
_cell_angle_gamma                94.836(5)
_cell_formula_units_Z            2
_cell_length_a                   11.9857(9)
_cell_length_b                   13.2787(8)
_cell_length_c                   13.8288(10)
_cell_measurement_reflns_used    4299
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.0940
_cell_measurement_theta_min      1.9790
_cell_volume                     2157.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -10.27 349.73   2.00   10.00  72.69 -18.16  31.50    --   180
  2  ω    -76.17   5.83   2.00   10.00    --  -18.16  89.85  18.34   41
  3  ω    -76.17   5.83   2.00   10.00    --  -18.16  89.85-137.66   41
  4  ω   -122.88  23.12   2.00   10.00    --  -18.16 -59.25-135.92   73
  5  ω    -76.17   5.83   2.00   10.00    --  -18.16  89.85 171.34   41
  6  ω   -122.88  23.12   2.00   10.00    --  -18.16 -59.25  71.08   73
  7  φ   -349.73  10.27   2.00   10.00  31.11 -18.16 -31.50    --   180
  8  ω    -76.17   5.83   2.00   10.00    --  -18.16  89.85  69.33   41
  9  ω    -76.17   5.83   2.00   10.00    --  -18.16  89.85 -32.66   41
 10  ω   -122.88  23.12   2.00   10.00    --  -18.16 -59.25 -84.92   73
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1502
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61621
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.564
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.361
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1221P)²+3.1222P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4906
_reflns_number_total             7602
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ob01276c2.cif
_cod_data_source_block           mr_pv_flu_autored
_cod_depositor_comments          'Adding full bibliography for 7160143.cif.'
_cod_database_code               7160143
_shelx_shelxl_version_number     2018/3
_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   0.981
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C33(H33), C8(H8), C28(H28)
1.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C6(H6), C1(H1), C2(H2A), C16(H16), C45(H45), C50(H50), C49(H49),
 C46(H46), C35(H35), C22(H22), C13(H13), C21(H21), C31(H31), C10(H10), C41(H41),
  C12(H12), C25(H25), C30(H30), C26(H26), C57(H57), C11(H11), C43(H43),
 C56(H56), C52(H52), C53(H53), C39(H39), C42(H42), C36(H36), C37(H37), C40(H40)
1.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C55(H55A,H55B,H55C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
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 0.09504(10) 0.84791(8) 0.34833(8) 0.0319(3) Uani 1 1 d . . . . .
S2 S 0.16935(11) 0.62356(9) 0.24289(9) 0.0380(3) Uani 1 1 d . . . . .
S3 S 0.80302(12) 0.59531(13) 0.27966(11) 0.0563(4) Uani 1 1 d . . . . .
O1 O -0.1199(3) 1.3964(2) 0.4740(3) 0.0458(9) Uani 1 1 d . . . . .
O2 O -0.0865(4) 0.0804(3) 0.0841(3) 0.0686(13) Uani 1 1 d . . . . .
N1 N 0.2937(3) 0.9778(3) 0.5098(3) 0.0293(9) Uani 1 1 d . . . . .
N2 N 0.4059(3) 0.5107(3) 0.2280(3) 0.0402(10) Uani 1 1 d . . . . .
H2 H 0.425509 0.541717 0.178860 0.048 Uiso 1 1 calc R U . . .
C1 C 0.2068(4) 1.1047(3) 0.6045(3) 0.0304(10) Uani 1 1 d . . . . .
H1 H 0.162228 1.160152 0.624311 0.036 Uiso 1 1 calc R U . . .
C2 C 0.2747(4) 1.0661(3) 0.6652(3) 0.0314(11) Uani 1 1 d . . . . .
H2A H 0.283278 1.087819 0.734322 0.038 Uiso 1 1 calc R U . . .
C3 C 0.3318(4) 0.9863(3) 0.6070(3) 0.0290(10) Uani 1 1 d . . . . .
C4 C 0.4107(4) 0.9179(3) 0.6138(3) 0.0329(11) Uani 1 1 d . . . . .
C5 C 0.4253(4) 0.8663(3) 0.5142(3) 0.0307(10) Uani 1 1 d . . . . .
C6 C 0.5004(4) 0.7954(3) 0.4731(3) 0.0295(10) Uani 1 1 d . . . . .
H6 H 0.551574 0.769503 0.513830 0.035 Uiso 1 1 calc R U . . .
C7 C 0.4975(4) 0.7645(3) 0.3724(3) 0.0315(11) Uani 1 1 d . . . . .
C8 C 0.5747(4) 0.6967(3) 0.3102(3) 0.0324(11) Uani 1 1 d . . . . .
H8 H 0.652473 0.731194 0.320906 0.039 Uiso 1 1 calc R U . . .
C9 C 0.5359(4) 0.7021(3) 0.2067(4) 0.0349(11) Uani 1 1 d . . . . .
C10 C 0.5746(4) 0.6549(4) 0.1170(4) 0.0410(12) Uani 1 1 d . . . . .
H10 H 0.638353 0.616622 0.114582 0.049 Uiso 1 1 calc R U . . .
C11 C 0.5176(5) 0.6651(4) 0.0308(4) 0.0479(14) Uani 1 1 d . . . . .
H11 H 0.541848 0.631887 -0.030826 0.057 Uiso 1 1 calc R U . . .
C12 C 0.4265(5) 0.7226(4) 0.0337(4) 0.0465(13) Uani 1 1 d . . . . .
H12 H 0.388802 0.728299 -0.025811 0.056 Uiso 1 1 calc R U . . .
C13 C 0.3896(4) 0.7722(4) 0.1228(4) 0.0406(12) Uani 1 1 d . . . . .
H13 H 0.327191 0.812060 0.124664 0.049 Uiso 1 1 calc R U . . .
C14 C 0.4458(4) 0.7624(4) 0.2094(3) 0.0339(11) Uani 1 1 d . . . . .
C15 C 0.4255(4) 0.8050(3) 0.3110(3) 0.0316(11) Uani 1 1 d . . . . .
C16 C 0.3542(4) 0.8794(3) 0.3485(3) 0.0289(10) Uani 1 1 d . . . . .
H16 H 0.308315 0.909272 0.306536 0.035 Uiso 1 1 calc R U . . .
C17 C 0.3535(4) 0.9075(3) 0.4496(3) 0.0287(10) Uani 1 1 d . . . . .
C18 C 0.2118(4) 1.0490(3) 0.5043(3) 0.0288(10) Uani 1 1 d . . . . .
C19 C 0.1404(4) 1.0565(3) 0.4284(3) 0.0311(10) Uani 1 1 d . . . . .
C20 C 0.1193(4) 0.9768(3) 0.3407(3) 0.0327(11) Uani 1 1 d . . . . .
C21 C 0.1186(5) 0.9881(4) 0.2436(4) 0.0447(13) Uani 1 1 d . . . . .
H21 H 0.125481 1.053154 0.223612 0.054 Uiso 1 1 calc R U . . .
C22 C 0.1069(5) 0.8942(4) 0.1766(4) 0.0415(13) Uani 1 1 d . . . . .
H22 H 0.106641 0.889561 0.107298 0.050 Uiso 1 1 calc R U . . .
C23 C 0.0957(4) 0.8099(3) 0.2226(3) 0.0318(11) Uani 1 1 d . . . . .
C24 C 0.1034(4) 0.7033(3) 0.1780(4) 0.0327(11) Uani 1 1 d . . . . .
C25 C 0.0830(4) 0.6555(4) 0.0839(4) 0.0409(12) Uani 1 1 d . . . . .
H25 H 0.045772 0.685580 0.036377 0.049 Uiso 1 1 calc R U . . .
C26 C 0.1218(5) 0.5569(4) 0.0625(4) 0.0433(13) Uani 1 1 d . . . . .
H26 H 0.114736 0.514983 -0.000802 0.052 Uiso 1 1 calc R U . . .
C27 C 0.1693(4) 0.5285(3) 0.1402(4) 0.0362(11) Uani 1 1 d . . . . .
C28 C 0.2290(4) 0.4310(3) 0.1420(3) 0.0346(11) Uani 1 1 d . . . . .
H28 H 0.274236 0.420355 0.081510 0.042 Uiso 1 1 calc R U . . .
C29 C 0.3108(4) 0.4462(3) 0.2282(4) 0.0354(11) Uani 1 1 d . . . . .
C30 C 0.3128(4) 0.4135(4) 0.3164(4) 0.0474(14) Uani 1 1 d . . . . .
H30 H 0.256944 0.368724 0.338760 0.057 Uiso 1 1 calc R U . . .
C31 C 0.4137(5) 0.4583(4) 0.3691(4) 0.0435(13) Uani 1 1 d . . . . .
H31 H 0.438438 0.445826 0.431213 0.052 Uiso 1 1 calc R U . . .
C32 C 0.4671(4) 0.5209(3) 0.3155(3) 0.0325(11) Uani 1 1 d . . . . .
C33 C 0.5773(4) 0.5852(3) 0.3327(3) 0.0324(11) Uani 1 1 d . . . . .
H33 H 0.597262 0.592691 0.404248 0.039 Uiso 1 1 calc R U . . .
C34 C 0.6710(4) 0.5330(4) 0.2775(4) 0.0382(12) Uani 1 1 d . . . . .
C35 C 0.6636(4) 0.4350(4) 0.2179(4) 0.0420(12) Uani 1 1 d . . . . .
H35 H 0.598198 0.388403 0.205510 0.050 Uiso 1 1 calc R U . . .
C36 C 0.7722(5) 0.4177(5) 0.1790(5) 0.0655(18) Uani 1 1 d . . . . .
H36 H 0.785918 0.355899 0.136487 0.079 Uiso 1 1 calc R U . . .
C37 C 0.8523(5) 0.4936(5) 0.2060(5) 0.0686(19) Uani 1 1 d . . . . .
H37 H 0.927799 0.491154 0.186560 0.082 Uiso 1 1 calc R U . . .
C38 C 0.4668(4) 0.9028(3) 0.7051(3) 0.0311(11) Uani 1 1 d . . . . .
C39 C 0.5026(5) 0.8098(4) 0.7163(4) 0.0547(15) Uani 1 1 d . . . . .
H39 H 0.490084 0.752835 0.664044 0.066 Uiso 1 1 calc R U . . .
C40 C 0.5568(6) 0.7973(5) 0.8025(4) 0.0654(18) Uani 1 1 d . . . . .
H40 H 0.582187 0.732504 0.807613 0.079 Uiso 1 1 calc R U . . .
C41 C 0.5739(5) 0.8773(4) 0.8801(4) 0.0459(13) Uani 1 1 d . . . . .
H41 H 0.612704 0.869279 0.938360 0.055 Uiso 1 1 calc R U . . .
C42 C 0.5334(5) 0.9701(5) 0.8716(4) 0.0580(16) Uani 1 1 d . . . . .
H42 H 0.541434 1.025527 0.925777 0.070 Uiso 1 1 calc R U . . .
C43 C 0.4819(5) 0.9828(4) 0.7861(4) 0.0486(14) Uani 1 1 d . . . . .
H43 H 0.455814 1.047456 0.781564 0.058 Uiso 1 1 calc R U . . .
C44 C 0.0733(4) 1.1459(3) 0.4344(3) 0.0312(11) Uani 1 1 d . . . . .
C45 C 0.1189(4) 1.2473(3) 0.4704(3) 0.0348(11) Uani 1 1 d . . . . .
H45 H 0.196502 1.259801 0.487900 0.042 Uiso 1 1 calc R U . . .
C46 C 0.0530(4) 1.3289(3) 0.4807(4) 0.0369(12) Uani 1 1 d . . . . .
H46 H 0.085854 1.396731 0.503697 0.044 Uiso 1 1 calc R U . . .
C47 C -0.0610(4) 1.3121(3) 0.4576(3) 0.0335(11) Uani 1 1 d . . . . .
C48 C -0.2388(5) 1.3802(4) 0.4628(5) 0.0561(15) Uani 1 1 d . . . . .
H48A H -0.259531 1.347304 0.395007 0.084 Uiso 1 1 calc R U . . .
H48B H -0.271069 1.446402 0.477553 0.084 Uiso 1 1 calc R U . . .
H48C H -0.267563 1.335867 0.508019 0.084 Uiso 1 1 calc R U . . .
C49 C -0.1075(4) 1.2135(3) 0.4194(3) 0.0324(11) Uani 1 1 d . . . . .
H49 H -0.185066 1.201460 0.401588 0.039 Uiso 1 1 calc R U . . .
C50 C -0.0395(4) 1.1326(3) 0.4073(3) 0.0321(11) Uani 1 1 d . . . . .
H50 H -0.071646 1.065682 0.379373 0.039 Uiso 1 1 calc R U . . .
C51 C 0.1479(4) 0.3354(3) 0.1360(4) 0.0358(11) Uani 1 1 d . . . . .
C52 C 0.0611(5) 0.3292(4) 0.1971(4) 0.0469(13) Uani 1 1 d . . . . .
H52 H 0.054515 0.383963 0.250530 0.056 Uiso 1 1 calc R U . . .
C53 C -0.0186(5) 0.2447(4) 0.1836(4) 0.0530(15) Uani 1 1 d . . . . .
H53 H -0.078703 0.241847 0.227284 0.064 Uiso 1 1 calc R U . . .
C54 C -0.0091(5) 0.1658(4) 0.1067(4) 0.0505(15) Uani 1 1 d . . . . .
C55 C -0.1885(7) 0.0813(6) 0.1401(6) 0.102(3) Uani 1 1 d . . . . .
H55A H -0.237886 0.019153 0.115183 0.153 Uiso 1 1 calc R U . . .
H55B H -0.227027 0.142021 0.133021 0.153 Uiso 1 1 calc R U . . .
H55C H -0.169281 0.083423 0.209586 0.153 Uiso 1 1 calc R U . . .
C56 C 0.0802(5) 0.1673(4) 0.0438(4) 0.0512(15) Uani 1 1 d . . . . .
H56 H 0.088368 0.110822 -0.007438 0.061 Uiso 1 1 calc R U . . .
C57 C 0.1564(5) 0.2526(4) 0.0575(4) 0.0470(13) Uani 1 1 d . . . . .
H57 H 0.215864 0.255877 0.013367 0.056 Uiso 1 1 calc R U . . .
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'
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'
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
C23 S1 C20 92.7(2) . . ?
C27 S2 C24 91.9(2) . . ?
C37 S3 C34 92.1(3) . . ?
C47 O1 C48 117.5(4) . . ?
C54 O2 C55 117.1(5) . . ?
C3 N1 C18 109.7(4) . . ?
C17 N1 C3 109.2(4) . . ?
C17 N1 C18 140.9(4) . . ?
C29 N2 H2 124.5 . . ?
C29 N2 C32 110.9(4) . . ?
C32 N2 H2 124.5 . . ?
C2 C1 H1 124.9 . . ?
C2 C1 C18 110.2(4) . . ?
C18 C1 H1 124.9 . . ?
C1 C2 H2A 125.8 . . ?
C1 C2 C3 108.3(4) . . ?
C3 C2 H2A 125.8 . . ?
N1 C3 C2 107.2(4) . . ?
C4 C3 N1 110.5(4) . . ?
C4 C3 C2 142.3(4) . . ?
C3 C4 C5 105.7(4) . . ?
C3 C4 C38 125.8(4) . . ?
C5 C4 C38 128.5(4) . . ?
C6 C5 C4 132.4(4) . . ?
C6 C5 C17 119.0(4) . . ?
C17 C5 C4 108.4(4) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 C5 118.3(4) . . ?
C7 C6 H6 120.9 . . ?
C6 C7 C8 128.5(4) . . ?
C6 C7 C15 121.6(4) . . ?
C15 C7 C8 109.5(4) . . ?
C7 C8 H8 107.8 . . ?
C7 C8 C33 115.8(4) . . ?
C9 C8 C7 102.5(4) . . ?
C9 C8 H8 107.8 . . ?
C9 C8 C33 114.8(4) . . ?
C33 C8 H8 107.8 . . ?
C10 C9 C8 129.7(5) . . ?
C10 C9 C14 120.3(5) . . ?
C14 C9 C8 109.9(4) . . ?
C9 C10 H10 120.8 . . ?
C9 C10 C11 118.5(5) . . ?
C11 C10 H10 120.8 . . ?
C10 C11 H11 119.5 . . ?
C12 C11 C10 121.0(5) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.7(5) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 120.6 . . ?
C12 C13 C14 118.8(5) . . ?
C14 C13 H13 120.6 . . ?
C9 C14 C15 109.0(4) . . ?
C13 C14 C9 120.6(4) . . ?
C13 C14 C15 130.4(5) . . ?
C7 C15 C14 108.9(4) . . ?
C16 C15 C7 121.8(4) . . ?
C16 C15 C14 129.1(4) . . ?
C15 C16 H16 121.6 . . ?
C17 C16 C15 116.8(4) . . ?
C17 C16 H16 121.6 . . ?
N1 C17 C5 106.1(4) . . ?
C16 C17 N1 131.4(4) . . ?
C16 C17 C5 122.5(4) . . ?
N1 C18 C1 104.5(4) . . ?
C19 C18 N1 129.7(4) . . ?
C19 C18 C1 125.1(4) . . ?
C18 C19 C20 123.8(4) . . ?
C18 C19 C44 120.1(4) . . ?
C20 C19 C44 115.9(4) . . ?
C19 C20 S1 121.9(3) . . ?
C21 C20 S1 109.8(3) . . ?
C21 C20 C19 128.3(4) . . ?
C20 C21 H21 123.1 . . ?
C20 C21 C22 113.8(4) . . ?
C22 C21 H21 123.1 . . ?
C21 C22 H22 123.6 . . ?
C23 C22 C21 112.8(4) . . ?
C23 C22 H22 123.6 . . ?
C22 C23 S1 110.6(3) . . ?
C22 C23 C24 127.0(4) . . ?
C24 C23 S1 121.5(3) . . ?
C23 C24 S2 119.4(3) . . ?
C25 C24 S2 109.7(4) . . ?
C25 C24 C23 129.9(4) . . ?
C24 C25 H25 123.0 . . ?
C24 C25 C26 114.0(5) . . ?
C26 C25 H25 123.0 . . ?
C25 C26 H26 123.4 . . ?
C27 C26 C25 113.2(5) . . ?
C27 C26 H26 123.4 . . ?
C26 C27 S2 111.2(4) . . ?
C26 C27 C28 127.3(4) . . ?
C28 C27 S2 121.2(4) . . ?
C27 C28 H28 106.6 . . ?
C29 C28 C27 110.8(4) . . ?
C29 C28 H28 106.6 . . ?
C29 C28 C51 113.1(4) . . ?
C51 C28 C27 112.8(4) . . ?
C51 C28 H28 106.6 . . ?
N2 C29 C28 118.9(4) . . ?
C30 C29 N2 106.0(4) . . ?
C30 C29 C28 135.0(4) . . ?
C29 C30 H30 126.0 . . ?
C29 C30 C31 108.1(4) . . ?
C31 C30 H30 126.0 . . ?
C30 C31 H31 126.0 . . ?
C32 C31 C30 107.9(5) . . ?
C32 C31 H31 126.0 . . ?
N2 C32 C33 121.4(4) . . ?
C31 C32 N2 106.9(4) . . ?
C31 C32 C33 131.5(5) . . ?
C8 C33 H33 106.6 . . ?
C32 C33 C8 114.6(4) . . ?
C32 C33 H33 106.6 . . ?
C32 C33 C34 112.2(4) . . ?
C34 C33 C8 109.7(4) . . ?
C34 C33 H33 106.6 . . ?
C33 C34 S3 120.6(4) . . ?
C35 C34 S3 112.1(4) . . ?
C35 C34 C33 127.2(4) . . ?
C34 C35 H35 125.9 . . ?
C34 C35 C36 108.1(5) . . ?
C36 C35 H35 125.9 . . ?
C35 C36 H36 122.0 . . ?
C37 C36 C35 115.9(6) . . ?
C37 C36 H36 122.0 . . ?
S3 C37 H37 124.2 . . ?
C36 C37 S3 111.7(5) . . ?
C36 C37 H37 124.2 . . ?
C39 C38 C4 122.2(4) . . ?
C39 C38 C43 117.0(5) . . ?
C43 C38 C4 120.7(4) . . ?
C38 C39 H39 119.3 . . ?
C38 C39 C40 121.5(5) . . ?
C40 C39 H39 119.3 . . ?
C39 C40 H40 119.6 . . ?
C41 C40 C39 120.7(6) . . ?
C41 C40 H40 119.6 . . ?
C40 C41 H41 120.8 . . ?
C40 C41 C42 118.5(5) . . ?
C42 C41 H41 120.8 . . ?
C41 C42 H42 119.7 . . ?
C43 C42 C41 120.6(5) . . ?
C43 C42 H42 119.7 . . ?
C38 C43 H43 119.2 . . ?
C42 C43 C38 121.6(5) . . ?
C42 C43 H43 119.2 . . ?
C45 C44 C19 122.4(4) . . ?
C50 C44 C19 120.7(4) . . ?
C50 C44 C45 116.8(4) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 C44 121.3(5) . . ?
C46 C45 H45 119.3 . . ?
C45 C46 H46 119.9 . . ?
C45 C46 C47 120.3(4) . . ?
C47 C46 H46 119.9 . . ?
O1 C47 C46 116.2(4) . . ?
O1 C47 C49 124.2(5) . . ?
C46 C47 C49 119.6(4) . . ?
O1 C48 H48A 109.5 . . ?
O1 C48 H48B 109.5 . . ?
O1 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49 120.3 . . ?
C47 C49 C50 119.3(5) . . ?
C50 C49 H49 120.3 . . ?
C44 C50 C49 122.5(4) . . ?
C44 C50 H50 118.8 . . ?
C49 C50 H50 118.8 . . ?
C52 C51 C28 123.1(4) . . ?
C52 C51 C57 118.0(5) . . ?
C57 C51 C28 118.7(5) . . ?
C51 C52 H52 119.1 . . ?
C51 C52 C53 121.8(5) . . ?
C53 C52 H52 119.1 . . ?
C52 C53 H53 120.5 . . ?
C54 C53 C52 119.1(5) . . ?
C54 C53 H53 120.5 . . ?
O2 C54 C56 115.1(5) . . ?
C53 C54 O2 123.7(6) . . ?
C53 C54 C56 121.2(5) . . ?
O2 C55 H55A 109.5 . . ?
O2 C55 H55B 109.5 . . ?
O2 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56 120.8 . . ?
C57 C56 C54 118.5(5) . . ?
C57 C56 H56 120.8 . . ?
C51 C57 H57 119.3 . . ?
C56 C57 C51 121.4(5) . . ?
C56 C57 H57 119.3 . . ?
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 C20 1.734(5) . ?
S1 C23 1.723(5) . ?
S2 C24 1.732(5) . ?
S2 C27 1.726(5) . ?
S3 C34 1.720(5) . ?
S3 C37 1.697(6) . ?
O1 C47 1.361(5) . ?
O1 C48 1.425(6) . ?
O2 C54 1.390(6) . ?
O2 C55 1.458(9) . ?
N1 C3 1.395(6) . ?
N1 C17 1.393(6) . ?
N1 C18 1.429(6) . ?
N2 H2 0.8800 . ?
N2 C29 1.367(6) . ?
N2 C32 1.385(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.352(6) . ?
C1 C18 1.456(6) . ?
C2 H2A 0.9500 . ?
C3 C2 1.442(6) . ?
C3 C4 1.378(7) . ?
C4 C38 1.472(6) . ?
C5 C4 1.447(6) . ?
C5 C17 1.435(6) . ?
C6 C5 1.411(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.380(6) . ?
C7 C8 1.517(6) . ?
C7 C15 1.402(7) . ?
C8 H8 1.0000 . ?
C8 C9 1.513(7) . ?
C9 C10 1.393(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.397(7) . ?
C11 H11 0.9500 . ?
C12 C11 1.381(8) . ?
C12 H12 0.9500 . ?
C13 C12 1.389(7) . ?
C13 H13 0.9500 . ?
C14 C9 1.396(7) . ?
C14 C13 1.395(7) . ?
C15 C14 1.453(6) . ?
C16 C15 1.398(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(6) . ?
C18 C19 1.366(6) . ?
C19 C20 1.465(6) . ?
C20 C21 1.376(7) . ?
C21 H21 0.9500 . ?
C22 C21 1.411(7) . ?
C22 H22 0.9500 . ?
C23 C22 1.380(7) . ?
C23 C24 1.453(6) . ?
C24 C25 1.352(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.409(7) . ?
C26 H26 0.9500 . ?
C27 C26 1.333(7) . ?
C28 C27 1.535(6) . ?
C28 H28 1.0000 . ?
C28 C29 1.504(7) . ?
C29 C30 1.366(7) . ?
C30 H30 0.9500 . ?
C31 C30 1.429(7) . ?
C31 H31 0.9500 . ?
C32 C31 1.339(7) . ?
C33 C8 1.568(6) . ?
C33 C32 1.504(6) . ?
C33 H33 1.0000 . ?
C33 C34 1.516(6) . ?
C35 C34 1.407(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.439(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.330(9) . ?
C37 H37 0.9500 . ?
C38 C39 1.374(7) . ?
C38 C43 1.399(7) . ?
C39 H39 0.9500 . ?
C39 C40 1.389(8) . ?
C40 H40 0.9500 . ?
C41 C40 1.370(8) . ?
C41 H41 0.9500 . ?
C41 C42 1.385(8) . ?
C42 H42 0.9500 . ?
C43 C42 1.368(8) . ?
C43 H43 0.9500 . ?
C44 C19 1.480(6) . ?
C44 C45 1.411(6) . ?
C44 C50 1.385(7) . ?
C45 H45 0.9500 . ?
C45 C46 1.383(7) . ?
C46 H46 0.9500 . ?
C47 C46 1.388(7) . ?
C47 C49 1.389(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49 0.9500 . ?
C50 C49 1.392(6) . ?
C50 H50 0.9500 . ?
C51 C28 1.521(6) . ?
C51 C52 1.358(7) . ?
C51 C57 1.414(7) . ?
C52 H52 0.9500 . ?
C52 C53 1.396(7) . ?
C53 H53 0.9500 . ?
C54 C53 1.369(8) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C54 1.391(8) . ?
C56 H56 0.9500 . ?
C57 C56 1.377(7) . ?
C57 H57 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C20 C21 C22 -4.2(6) . . . . ?
S1 C23 C22 C21 2.1(6) . . . . ?
S1 C23 C24 S2 -27.1(6) . . . . ?
S1 C23 C24 C25 165.1(4) . . . . ?
S2 C24 C25 C26 -1.4(6) . . . . ?
S2 C27 C26 C25 -0.7(6) . . . . ?
O1 C47 C46 C45 177.3(4) . . . . ?
O1 C47 C49 C50 -178.9(4) . . . . ?
O2 C54 C53 C52 -177.0(5) . . . . ?
N1 C3 C2 C1 -1.1(5) . . . . ?
N1 C3 C4 C5 2.1(5) . . . . ?
N1 C3 C4 C38 -178.0(4) . . . . ?
N1 C18 C19 C20 12.5(7) . . . . ?
N1 C18 C19 C44 -171.4(4) . . . . ?
N2 C29 C30 C31 -1.4(6) . . . . ?
N2 C32 C31 C30 -4.0(6) . . . . ?
C1 C18 C19 C20 -156.9(4) . . . . ?
C1 C18 C19 C44 19.2(7) . . . . ?
C2 C1 C18 N1 -3.2(5) . . . . ?
C2 C1 C18 C19 168.4(4) . . . . ?
C2 C3 C4 C5 -176.6(6) . . . . ?
C2 C3 C4 C38 3.3(9) . . . . ?
C3 N1 C17 C5 4.3(5) . . . . ?
C3 N1 C17 C16 -173.6(4) . . . . ?
C3 N1 C18 C1 2.5(4) . . . . ?
C3 N1 C18 C19 -168.6(4) . . . . ?
C3 C4 C38 C39 150.0(5) . . . . ?
C3 C4 C38 C43 -27.5(7) . . . . ?
C4 C3 C2 C1 177.6(6) . . . . ?
C4 C5 C17 N1 -3.0(5) . . . . ?
C4 C5 C17 C16 175.1(4) . . . . ?
C4 C38 C39 C40 179.1(5) . . . . ?
C4 C38 C43 C42 179.7(5) . . . . ?
C5 C4 C38 C39 -30.1(8) . . . . ?
C5 C4 C38 C43 152.4(5) . . . . ?
C5 C6 C7 C8 174.6(4) . . . . ?
C5 C6 C7 C15 2.5(6) . . . . ?
C6 C5 C4 C3 173.8(5) . . . . ?
C6 C5 C4 C38 -6.1(8) . . . . ?
C6 C5 C17 N1 -177.3(4) . . . . ?
C6 C5 C17 C16 0.8(6) . . . . ?
C6 C7 C8 C9 -173.9(4) . . . . ?
C6 C7 C8 C33 60.3(6) . . . . ?
C6 C7 C15 C14 176.9(4) . . . . ?
C6 C7 C15 C16 0.8(7) . . . . ?
C7 C6 C5 C4 -176.0(4) . . . . ?
C7 C6 C5 C17 -3.3(6) . . . . ?
C7 C8 C9 C10 -179.6(5) . . . . ?
C7 C8 C9 C14 -1.8(5) . . . . ?
C7 C15 C14 C9 -4.7(5) . . . . ?
C7 C15 C14 C13 174.0(5) . . . . ?
C8 C7 C15 C14 3.5(5) . . . . ?
C8 C7 C15 C16 -172.5(4) . . . . ?
C8 C9 C10 C11 174.4(5) . . . . ?
C8 C33 C32 N2 50.8(6) . . . . ?
C8 C33 C32 C31 -135.8(5) . . . . ?
C8 C33 C34 S3 47.4(5) . . . . ?
C8 C33 C34 C35 -130.2(5) . . . . ?
C9 C10 C11 C12 1.6(8) . . . . ?
C9 C14 C13 C12 -1.4(7) . . . . ?
C13 C12 C11 C10 0.2(8) . . . . ?
C13 C14 C9 C8 -174.9(4) . . . . ?
C13 C14 C9 C10 3.2(7) . . . . ?
C14 C9 C10 C11 -3.2(7) . . . . ?
C14 C13 C12 C11 -0.3(8) . . . . ?
C15 C7 C8 C9 -1.1(5) . . . . ?
C15 C7 C8 C33 -126.9(4) . . . . ?
C15 C14 C9 C8 3.9(5) . . . . ?
C15 C14 C9 C10 -178.0(4) . . . . ?
C15 C14 C13 C12 -179.9(5) . . . . ?
C15 C16 C17 N1 180.0(4) . . . . ?
C15 C16 C17 C5 2.5(6) . . . . ?
C16 C15 C14 C9 171.0(4) . . . . ?
C16 C15 C14 C13 -10.4(8) . . . . ?
C17 N1 C3 C2 175.0(3) . . . . ?
C17 N1 C3 C4 -4.1(5) . . . . ?
C17 N1 C18 C1 -171.5(5) . . . . ?
C17 N1 C18 C19 17.4(8) . . . . ?
C17 C5 C4 C3 0.6(5) . . . . ?
C17 C5 C4 C38 -179.4(4) . . . . ?
C17 C16 C15 C7 -3.3(6) . . . . ?
C17 C16 C15 C14 -178.5(4) . . . . ?
C18 N1 C3 C2 -1.0(5) . . . . ?
C18 N1 C3 C4 179.8(4) . . . . ?
C18 N1 C17 C5 178.4(5) . . . . ?
C18 N1 C17 C16 0.5(9) . . . . ?
C18 C1 C2 C3 2.7(5) . . . . ?
C18 C19 C20 S1 45.5(6) . . . . ?
C18 C19 C20 C21 -132.3(6) . . . . ?
C19 C20 C21 C22 173.8(5) . . . . ?
C19 C44 C45 C46 -176.2(4) . . . . ?
C19 C44 C50 C49 174.6(4) . . . . ?
C20 S1 C23 C22 -3.8(4) . . . . ?
C20 S1 C23 C24 166.2(4) . . . . ?
C22 C23 C24 S2 141.1(5) . . . . ?
C22 C23 C24 C25 -26.6(9) . . . . ?
C23 S1 C20 C19 -173.6(4) . . . . ?
C23 S1 C20 C21 4.6(4) . . . . ?
C23 C22 C21 C20 1.5(7) . . . . ?
C23 C24 C25 C26 167.2(5) . . . . ?
C24 S2 C27 C26 -0.1(4) . . . . ?
C24 S2 C27 C28 174.2(4) . . . . ?
C24 C23 C22 C21 -167.3(5) . . . . ?
C24 C25 C26 C27 1.4(7) . . . . ?
C27 S2 C24 C23 -169.1(4) . . . . ?
C27 S2 C24 C25 0.9(4) . . . . ?
C27 C28 C29 N2 -70.0(5) . . . . ?
C27 C28 C29 C30 105.8(6) . . . . ?
C28 C27 C26 C25 -174.5(5) . . . . ?
C28 C29 C30 C31 -177.6(5) . . . . ?
C28 C51 C52 C53 173.3(5) . . . . ?
C28 C51 C57 C56 -175.0(5) . . . . ?
C29 N2 C32 C31 3.2(6) . . . . ?
C29 N2 C32 C33 178.1(4) . . . . ?
C29 C28 C27 S2 -17.2(6) . . . . ?
C29 C28 C27 C26 156.1(5) . . . . ?
C32 N2 C29 C28 175.8(4) . . . . ?
C32 N2 C29 C30 -1.1(5) . . . . ?
C32 C31 C30 C29 3.4(6) . . . . ?
C32 C33 C8 C7 62.0(5) . . . . ?
C32 C33 C8 C9 -57.2(5) . . . . ?
C32 C33 C34 S3 175.9(3) . . . . ?
C32 C33 C34 C35 -1.6(7) . . . . ?
C33 C8 C9 C10 -53.2(7) . . . . ?
C33 C8 C9 C14 124.6(4) . . . . ?
C33 C32 C31 C30 -178.0(5) . . . . ?
C34 S3 C37 C36 1.7(6) . . . . ?
C34 C33 C8 C7 -170.8(4) . . . . ?
C34 C33 C8 C9 70.0(5) . . . . ?
C34 C33 C32 N2 -75.1(5) . . . . ?
C34 C33 C32 C31 98.2(6) . . . . ?
C34 C35 C36 C37 0.1(8) . . . . ?
C35 C36 C37 S3 -1.4(8) . . . . ?
C36 C35 C34 S3 1.2(6) . . . . ?
C36 C35 C34 C33 179.0(5) . . . . ?
C37 S3 C34 C33 -179.6(4) . . . . ?
C37 S3 C34 C35 -1.7(4) . . . . ?
C38 C39 C40 C41 1.5(10) . . . . ?
C38 C43 C42 C41 1.0(9) . . . . ?
C39 C38 C43 C42 2.1(8) . . . . ?
C40 C41 C42 C43 -2.9(9) . . . . ?
C42 C41 C40 C39 1.7(10) . . . . ?
C43 C38 C39 C40 -3.3(9) . . . . ?
C44 C19 C20 S1 -130.7(4) . . . . ?
C44 C19 C20 C21 51.5(7) . . . . ?
C44 C45 C46 C47 1.4(7) . . . . ?
C44 C50 C49 C47 1.7(7) . . . . ?
C45 C44 C19 C18 43.2(6) . . . . ?
C45 C44 C19 C20 -140.5(5) . . . . ?
C45 C44 C50 C49 -3.5(7) . . . . ?
C46 C47 C49 C50 1.7(7) . . . . ?
C48 O1 C47 C46 -172.4(4) . . . . ?
C48 O1 C47 C49 8.2(7) . . . . ?
C49 C47 C46 C45 -3.2(7) . . . . ?
C50 C44 C19 C18 -134.9(5) . . . . ?
C50 C44 C19 C20 41.5(6) . . . . ?
C50 C44 C45 C46 1.9(7) . . . . ?
C51 C28 C27 S2 110.6(4) . . . . ?
C51 C28 C27 C26 -76.1(6) . . . . ?
C51 C28 C29 N2 162.3(4) . . . . ?
C51 C28 C29 C30 -21.9(8) . . . . ?
C51 C52 C53 C54 0.0(9) . . . . ?
C51 C57 C56 C54 2.7(8) . . . . ?
C52 C51 C28 C27 -52.4(6) . . . . ?
C52 C51 C28 C29 74.3(6) . . . . ?
C52 C51 C57 C56 -0.9(8) . . . . ?
C55 O2 C54 C53 6.5(9) . . . . ?
C55 O2 C54 C56 -172.5(6) . . . . ?
C56 C54 C53 C52 1.9(9) . . . . ?
C57 C51 C28 C27 121.4(5) . . . . ?
C57 C51 C28 C29 -111.9(5) . . . . ?
C57 C51 C52 C53 -0.5(8) . . . . ?
C57 C56 C54 O2 175.8(5) . . . . ?
C57 C56 C54 C53 -3.2(8) . . . . ?
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
_smtbx_masks_void_content
1 0.159 0.195 0.833 17.2 1.1 ?
2 0.841 0.805 0.167 17.2 1.2 ?
