data_23dub_ao01
_audit_creation_date               2023-06-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number       '2018/3'
loop_
  _audit_author_name
  _audit_author_email
  _audit_author_address
 'Oezcelik, A.' ani.oezcelik@fau.de
;
OC1-Dube
DCP
;
 'F.H., P.G.' ? ?

_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C22 H21 Br O4 S'
_chemical_formula_sum              'C22 H21 Br O4 S'
_chemical_formula_weight           461.36
_chemical_melting_point            ?
_chemical_oxdiff_formula           C22H21BrO4S
_chemical_oxdiff_usercomment       PKB-141A
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'
 'Br' 'Br' -0.6763 1.2805
 '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'

_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.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     6.5649(4)
_cell_length_b                     9.4961(4)
_cell_length_c                     16.7764(7)
_cell_angle_alpha                  86.705(4)
_cell_angle_beta                   88.092(4)
_cell_angle_gamma                  74.891(5)
_cell_volume                       1007.85(9)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      7822
_cell_measurement_temperature      153(1)
_cell_measurement_theta_max        70.9990
_cell_measurement_theta_min        4.8040
_shelx_estimated_absorpt_T_max     0.732
_shelx_estimated_absorpt_T_min     0.424
_exptl_absorpt_coefficient_mu      3.964
_exptl_absorpt_correction_T_max    1.000
_exptl_absorpt_correction_T_min    0.417
_exptl_absorpt_correction_type     gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light red'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      red
_exptl_crystal_density_diffrn      1.520
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               472
loop_
  _exptl_crystal_face_index_h
  _exptl_crystal_face_index_k
  _exptl_crystal_face_index_l
  _exptl_crystal_face_perp_dist
 -1 -3 -10 0.0355
 1 3 10 0.0355
 -4 -2 0 0.1283
 4 2 0 0.1283
 -1 -6 1 0.0431
 1 6 -1 0.0431
 -2 -1 9 0.0616
 2 1 -9 0.0616

_exptl_crystal_recrystallization_method 
 'The material was recrystallised from a mixture of DCM and pentane  by solvent layering'
_exptl_crystal_size_max            0.261
_exptl_crystal_size_mid            0.093
_exptl_crystal_size_min            0.084
loop_
  _exptl_oxdiff_crystal_face_indexfrac_h
  _exptl_oxdiff_crystal_face_indexfrac_k
  _exptl_oxdiff_crystal_face_indexfrac_l
  _exptl_oxdiff_crystal_face_x
  _exptl_oxdiff_crystal_face_y
  _exptl_oxdiff_crystal_face_z
 -0.5211 -2.9159 -9.8726 -0.3545 0.4167 -0.8371
 0.5211 2.9159 9.8726 0.3545 -0.4167 0.8371
 -4.2500 -1.8898 0.2086 -0.5763 0.6724 0.4645
 4.2500 1.8898 -0.2086 0.5763 -0.6724 -0.4645
 -0.5949 -6.0153 1.4045 -0.9116 -0.3781 -0.1611
 0.5949 6.0153 -1.4045 0.9116 0.3781 0.1611
 -2.0720 -1.4741 9.1733 -0.4491 -0.1880 0.8735
 2.0720 1.4741 -9.1733 0.4491 0.1880 -0.8735

_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0363
_diffrn_reflns_av_unetI/netI       0.0254
_diffrn_reflns_Laue_measured_fraction_full  0.998
_diffrn_reflns_Laue_measured_fraction_max  0.980
_diffrn_reflns_limit_h_max         8
_diffrn_reflns_limit_h_min         -7
_diffrn_reflns_limit_k_max         11
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         20
_diffrn_reflns_limit_l_min         -20
_diffrn_reflns_number              16048
_diffrn_reflns_point_group_measured_fraction_full  0.998
_diffrn_reflns_point_group_measured_fraction_max  0.980
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           71.571
_diffrn_reflns_theta_min           2.639
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        153(1)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.6144
_diffrn_detector_type              Atlas
_diffrn_measured_fraction_theta_full  0.998
_diffrn_measured_fraction_theta_max  0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     -4.00  22.00   1.00    1.00    --   34.00  91.00  65.22   26
  2  ω      3.00  28.00   1.00    1.00    --   38.00  85.00 -80.90   25
  3  ω    -65.00  34.00   1.00    1.00    --  -42.18  77.00  90.00   99
  4  ω   -110.00 -83.00   1.00    1.00    --  -42.18 -38.00  60.00   27
  5  ω    -53.00 -25.00   1.00    1.00    --  -42.18 -38.00  60.00   28
  6  ω    -82.00 -54.00   1.00    1.00    --  -42.18 -38.00  60.00   28
  7  ω     28.00  98.00   1.00    1.00    --   42.18-125.00 -90.00   70
  8  ω     13.00  42.00   1.00    1.00    --   46.00  81.00-147.97   29
  9  ω     16.00  42.00   1.00    1.00    --   50.00  81.00 167.70   26
 10  ω     16.00  42.00   1.00    1.00    --   50.00  81.00  16.35   26
 11  ω     16.00  41.00   1.00    1.00    --   50.00  82.00 105.02   25
 12  ω     16.00  41.00   1.00    1.00    --   50.00  81.00-116.46   25
 13  ω     16.00  41.00   1.00    1.00    --   50.00  81.00 -56.53   25
 14  ω     26.00  95.00   1.00    1.00    --   54.00  61.00  -1.25   69
 15  ω     64.00 123.00   1.00    1.00    --   58.00  71.00 -98.57   59
 16  ω     27.00  54.00   1.00    1.00    --   58.00  71.00 -98.57   27
 17  ω     66.00 121.00   1.00    1.00    --   62.00  70.00 137.58   55
 18  ω     32.00  59.00   1.00    1.00    --   62.00  70.00 137.58   27
 19  ω     36.00  65.00   1.00    1.00    --   66.00  70.00-167.08   29
 20  ω     36.00 138.00   1.00    1.00    --   66.00  69.00  -4.76  102
 21  ω    116.00 143.00   1.00    1.00    --   70.00  70.00  43.57   27
 22  ω     39.00  80.00   1.00    1.00    --   70.00  70.00  43.57   41
 23  ω     40.00  71.00   1.00    1.00    --   70.00  70.00 -61.27   31
 24  ω     48.00  78.00   1.00    3.21    --   78.00  64.00 -74.30   30
 25  ω    117.00 155.00   1.00    3.21    --   82.00  69.00 136.12   38
 26  ω     51.00  77.00   1.00    3.21    --   82.00  69.00 136.12   26
 27  ω     97.00 124.00   1.00    3.21    --   82.00  70.00  86.71   27
 28  ω     51.00  84.00   1.00    3.21    --   82.00  70.00  86.71   33
 29  ω     53.00  78.00   1.00    3.21    --   82.00  65.00-143.03   25
 30  ω     60.00  93.00   1.00    3.21    --   90.00  69.00-124.72   33
 31  ω    109.00 168.00   1.00    3.21    --   98.00  67.00  55.56   59
 32  ω     68.00  94.00   1.00    3.21    --   98.00  67.00  55.56   26
 33  ω     30.00 113.00   1.00    3.21    --  102.55-125.00  60.00   83
 34  ω     73.00 156.00   1.00    3.21    --  102.55  61.00 -30.00   83
 35  ω     98.00 175.00   1.00    3.21    --  102.55 125.00 -90.00   77
 36  ω     78.00 105.00   1.00    3.21    --  102.55  61.00-120.00   27
 37  ω    134.00 161.00   1.00    3.21    --  102.55  61.00  90.00   27
 38  ω     40.00 129.00   1.00    3.21    --  102.55 -61.00-150.00   89
 39  ω    150.00 175.00   1.00    3.21    --  102.55  61.00-180.00   25
 40  ω    122.00 149.00   1.00    3.21    --  102.55  61.00 -90.00   27
 41  ω     73.00 105.00   1.00    3.21    --  102.55  61.00 -90.00   32
 42  ω    113.00 140.00   1.00    3.21    --  102.55  61.00-180.00   27
 43  ω     83.00 113.00   1.00    3.21    --  102.55-125.00   0.00   30
 44  ω     73.00 106.00   1.00    3.21    --  102.55  61.00-180.00   33
 45  ω    124.00 172.00   1.00    3.21    --  102.55  61.00   0.00   48
 46  ω     26.00 103.00   1.00    3.21    --  102.55 -94.00-150.00   77
 47  ω     74.00 111.00   1.00    3.21    --  102.55  61.00   0.00   37
 48  ω     73.00 117.00   1.00    3.21    --  102.55  61.00 -60.00   44
 49  ω     76.00 168.00   1.00    3.21    --  102.55  61.00-150.00   92
 50  ω     74.00 104.00   1.00    3.21    --  102.55  61.00  90.00   30
 51  ω     47.00 110.00   1.00    3.21    --  102.55-118.00 124.42   63
 52  ω     79.00 175.00   1.00    3.21    --  102.55  61.00 120.00   96
 53  ω     61.00  88.00   1.00    3.21    --  102.55 -61.00   0.00   27
 54  ω    116.00 175.00   1.00    3.21    --  102.55  61.00-120.00   59
 55  ω     73.00 136.00   1.00    3.21    --  102.55  61.00 150.00   63
 56  ω     78.00 158.00   1.00    3.21    --  102.55  61.00  30.00   80
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0719105000
_diffrn_orient_matrix_UB_12        0.1421354000
_diffrn_orient_matrix_UB_13        -0.0098708000
_diffrn_orient_matrix_UB_21        -0.1917136000
_diffrn_orient_matrix_UB_22        0.0695333000
_diffrn_orient_matrix_UB_23        -0.0526290000
_diffrn_orient_matrix_UB_31        -0.1310674000
_diffrn_orient_matrix_UB_32        0.0572076000
_diffrn_orient_matrix_UB_33        0.0748086000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Cu K\a'
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  3269
_reflns_number_total               3848
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_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      'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max           0.680
_refine_diff_density_min           -1.206
_refine_diff_density_rms           0.062
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.039
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       272
_refine_ls_number_reflns           3848
_refine_ls_number_restraints       2
_refine_ls_R_factor_all            0.0519
_refine_ls_R_factor_gt             0.0434
_refine_ls_restrained_S_all        1.039
_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)+(0.0484P)²+1.1092P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1041
_refine_ls_wR_factor_ref           0.1109
_refine_special_details           
 'Disorder of O2-C30 : O2a-C30a = 51 : 49% occupation'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O2-C25 \\sim O2A-C25
 with sigma of 0.02
 O2A-C30 \\sim O2-C30A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30A) = Uanis(C30)
4. Others
 Sof(O2)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(O2A)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C26(H26), C27(H27)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C),
 C30A(H30D,H30E,H30F)
5.e Idealised tetrahedral OH refined as rotating group:
 O25(H25)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
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
 Br1 Br 0.37930(6) 0.15166(6) 0.90279(2) 0.07361(18) Uani 1 1 d . . . . .
 S18 S 0.32618(11) 0.23512(7) 1.09414(4) 0.03804(18) Uani 1 1 d . . . . .
 O1 O 0.2066(3) 0.63098(19) 1.16435(11) 0.0338(4) Uani 1 1 d . . . . .
 O3 O 0.1133(5) 0.0980(2) 1.21496(16) 0.0627(7) Uani 1 1 d . . . . .
 O25 O 0.4553(3) 0.53963(19) 1.28718(11) 0.0333(4) Uani 1 1 d . . . . .
 H25 H 0.370317 0.591384 1.254170 0.050 Uiso 1 1 calc R U . . .
 C3 C -0.0062(4) 0.5427(3) 1.33149(17) 0.0396(6) Uani 1 1 d . . . . .
 H3A H 0.011748 0.637639 1.311087 0.059 Uiso 1 1 calc R U . . .
 H3B H -0.124152 0.557770 1.370168 0.059 Uiso 1 1 calc R U . . .
 H3C H -0.035840 0.488813 1.287081 0.059 Uiso 1 1 calc R U . . .
 C4 C 0.2437(5) 0.5366(4) 1.44155(19) 0.0488(7) Uani 1 1 d . . . . .
 H4A H 0.356066 0.471615 1.473337 0.073 Uiso 1 1 calc R U . . .
 H4B H 0.116655 0.568217 1.475106 0.073 Uiso 1 1 calc R U . . .
 H4C H 0.289910 0.622242 1.421059 0.073 Uiso 1 1 calc R U . . .
 C5 C 0.1950(4) 0.4558(3) 1.37205(15) 0.0307(5) Uani 1 1 d . . . . .
 H5 H 0.168513 0.362206 1.394571 0.037 Uiso 1 1 calc R U . . .
 C10 C 0.2930(4) 0.3695(3) 1.01686(16) 0.0370(6) Uani 1 1 d . . . . .
 C11 C 0.2965(4) 0.3673(3) 1.16736(15) 0.0287(5) Uani 1 1 d . . . . .
 C12 C 0.2459(4) 0.5178(3) 1.12909(15) 0.0283(5) Uani 1 1 d . . . . .
 C13 C 0.2462(4) 0.5116(3) 1.04194(15) 0.0332(6) Uani 1 1 d . . . . .
 C14 C 0.2073(4) 0.6309(4) 0.98696(17) 0.0425(7) Uani 1 1 d . . . . .
 H14 H 0.174768 0.727869 1.004269 0.051 Uiso 1 1 calc R U . . .
 C15 C 0.2174(5) 0.6041(5) 0.90607(19) 0.0542(9) Uani 1 1 d . . . . .
 H15 H 0.189921 0.683853 0.867641 0.065 Uiso 1 1 calc R U . . .
 C16 C 0.2668(5) 0.4630(5) 0.88090(19) 0.0571(10) Uani 1 1 d . . . . .
 H16 H 0.274209 0.446806 0.825404 0.068 Uiso 1 1 calc R U . . .
 C17 C 0.3057(5) 0.3451(4) 0.93573(18) 0.0488(8) Uani 1 1 d . . . . .
 C21 C 0.3330(4) 0.3270(3) 1.24551(15) 0.0298(5) Uani 1 1 d . . . . .
 C22 C 0.3852(4) 0.4155(3) 1.31247(15) 0.0290(5) Uani 1 1 d . . . . .
 C23 C 0.5752(5) 0.3007(3) 1.35098(18) 0.0432(7) Uani 1 1 d . . . . .
 H23A H 0.709718 0.304205 1.323522 0.052 Uiso 1 1 calc R U . . .
 H23B H 0.585076 0.316404 1.408396 0.052 Uiso 1 1 calc R U . . .
 C24 C 0.5230(5) 0.1594(3) 1.33931(19) 0.0482(8) Uani 1 1 d . . . . .
 C25 C 0.5967(7) 0.0243(4) 1.3804(2) 0.0709(13) Uani 1 1 d D . . . .
 C26 C 0.5145(9) -0.0902(4) 1.3614(3) 0.093(2) Uani 1 1 d . . . . .
 H26 H 0.566794 -0.183887 1.387163 0.112 Uiso 1 1 calc R U . . .
 C27 C 0.3579(9) -0.0699(4) 1.3056(3) 0.0849(17) Uani 1 1 d . . . . .
 H27 H 0.302226 -0.149627 1.294953 0.102 Uiso 1 1 calc R U . . .
 C28 C 0.2796(7) 0.0640(3) 1.2647(2) 0.0585(10) Uani 1 1 d . . . . .
 C29 C 0.3750(5) 0.1765(3) 1.27970(17) 0.0409(7) Uani 1 1 d . . . . .
 C31 C 0.0126(9) -0.0143(5) 1.1984(4) 0.0999(19) Uani 1 1 d . . . . .
 H31A H -0.095587 0.023304 1.158077 0.150 Uiso 1 1 calc R U . . .
 H31B H -0.053401 -0.044264 1.247454 0.150 Uiso 1 1 calc R U . . .
 H31C H 0.118050 -0.098571 1.178221 0.150 Uiso 1 1 calc R U . . .
 O2A O 0.762(3) 0.022(2) 1.4304(12) 0.083(5) Uani 0.484(12) 1 d D . P A 1
 C30 C 0.861(2) -0.0966(13) 1.4885(7) 0.062(2) Uani 0.484(12) 1 d D . P A 1
 H30A H 0.957080 -0.175822 1.460199 0.093 Uiso 0.484(12) 1 calc R U P A 1
 H30B H 0.751957 -0.133723 1.517069 0.093 Uiso 0.484(12) 1 calc R U P A 1
 H30C H 0.941315 -0.059024 1.526721 0.093 Uiso 0.484(12) 1 calc R U P A 1
 O2 O 0.728(3) 0.0185(19) 1.4444(11) 0.080(5) Uani 0.516(12) 1 d D . P A 2
 C30A C 0.7840(19) -0.1356(12) 1.4740(7) 0.062(2) Uani 0.516(12) 1 d D . P A
 2
 H30D H 0.861131 -0.196816 1.432005 0.093 Uiso 0.516(12) 1 calc R U P A 2
 H30E H 0.655215 -0.165425 1.488805 0.093 Uiso 0.516(12) 1 calc R U P A 2
 H30F H 0.873204 -0.146925 1.520853 0.093 Uiso 0.516(12) 1 calc R U P A 2


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 Br1 C17 1.884(4) . ?
 S18 C10 1.744(3) . ?
 S18 C11 1.776(2) . ?
 O1 C12 1.221(3) . ?
 O3 C28 1.356(5) . ?
 O3 C31 1.438(4) . ?
 O25 H25 0.8400 . ?
 O25 C22 1.412(3) . ?
 C3 H3A 0.9800 . ?
 C3 H3B 0.9800 . ?
 C3 H3C 0.9800 . ?
 C3 C5 1.522(4) . ?
 C4 H4A 0.9800 . ?
 C4 H4B 0.9800 . ?
 C4 H4C 0.9800 . ?
 C4 C5 1.519(4) . ?
 C5 H5 1.0000 . ?
 C5 C22 1.555(4) . ?
 C10 C13 1.391(4) . ?
 C10 C17 1.390(4) . ?
 C11 C12 1.492(3) . ?
 C11 C21 1.356(4) . ?
 C12 C13 1.466(4) . ?
 C13 C14 1.394(4) . ?
 C14 H14 0.9500 . ?
 C14 C15 1.391(5) . ?
 C15 H15 0.9500 . ?
 C15 C16 1.381(6) . ?
 C16 H16 0.9500 . ?
 C16 C17 1.383(5) . ?
 C21 C22 1.539(4) . ?
 C21 C29 1.469(3) . ?
 C22 C23 1.557(3) . ?
 C23 H23A 0.9900 . ?
 C23 H23B 0.9900 . ?
 C23 C24 1.494(5) . ?
 C24 C25 1.397(4) . ?
 C24 C29 1.390(5) . ?
 C25 C26 1.390(8) . ?
 C25 O2A 1.388(13) . ?
 C25 O2 1.388(12) . ?
 C26 H26 0.9500 . ?
 C26 C27 1.382(8) . ?
 C27 H27 0.9500 . ?
 C27 C28 1.392(6) . ?
 C28 C29 1.410(5) . ?
 C31 H31A 0.9800 . ?
 C31 H31B 0.9800 . ?
 C31 H31C 0.9800 . ?
 O2A C30 1.475(11) . ?
 C30 H30A 0.9800 . ?
 C30 H30B 0.9800 . ?
 C30 H30C 0.9800 . ?
 O2 C30A 1.473(12) . ?
 C30A H30D 0.9800 . ?
 C30A H30E 0.9800 . ?
 C30A H30F 0.9800 . ?

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
 C10 S18 C11 91.65(13) . . ?
 C28 O3 C31 118.6(4) . . ?
 C22 O25 H25 109.5 . . ?
 H3A C3 H3B 109.5 . . ?
 H3A C3 H3C 109.5 . . ?
 H3B C3 H3C 109.5 . . ?
 C5 C3 H3A 109.5 . . ?
 C5 C3 H3B 109.5 . . ?
 C5 C3 H3C 109.5 . . ?
 H4A C4 H4B 109.5 . . ?
 H4A C4 H4C 109.5 . . ?
 H4B C4 H4C 109.5 . . ?
 C5 C4 H4A 109.5 . . ?
 C5 C4 H4B 109.5 . . ?
 C5 C4 H4C 109.5 . . ?
 C3 C5 H5 107.3 . . ?
 C3 C5 C22 112.4(2) . . ?
 C4 C5 C3 110.5(2) . . ?
 C4 C5 H5 107.3 . . ?
 C4 C5 C22 111.7(2) . . ?
 C22 C5 H5 107.3 . . ?
 C13 C10 S18 114.5(2) . . ?
 C17 C10 S18 125.8(3) . . ?
 C17 C10 C13 119.7(3) . . ?
 C12 C11 S18 110.62(18) . . ?
 C21 C11 S18 121.30(19) . . ?
 C21 C11 C12 127.9(2) . . ?
 O1 C12 C11 125.6(2) . . ?
 O1 C12 C13 124.1(2) . . ?
 C13 C12 C11 110.3(2) . . ?
 C10 C13 C12 112.8(2) . . ?
 C10 C13 C14 121.0(3) . . ?
 C14 C13 C12 126.2(3) . . ?
 C13 C14 H14 120.9 . . ?
 C15 C14 C13 118.3(3) . . ?
 C15 C14 H14 120.9 . . ?
 C14 C15 H15 119.6 . . ?
 C16 C15 C14 120.9(3) . . ?
 C16 C15 H15 119.6 . . ?
 C15 C16 H16 119.7 . . ?
 C15 C16 C17 120.6(3) . . ?
 C17 C16 H16 119.7 . . ?
 C10 C17 Br1 119.2(3) . . ?
 C16 C17 Br1 121.4(2) . . ?
 C16 C17 C10 119.5(3) . . ?
 C11 C21 C22 129.0(2) . . ?
 C11 C21 C29 125.1(2) . . ?
 C29 C21 C22 104.8(2) . . ?
 O25 C22 C5 111.2(2) . . ?
 O25 C22 C21 115.8(2) . . ?
 O25 C22 C23 107.8(2) . . ?
 C5 C22 C23 111.4(2) . . ?
 C21 C22 C5 109.9(2) . . ?
 C21 C22 C23 100.3(2) . . ?
 C22 C23 H23A 111.2 . . ?
 C22 C23 H23B 111.2 . . ?
 H23A C23 H23B 109.1 . . ?
 C24 C23 C22 102.9(2) . . ?
 C24 C23 H23A 111.2 . . ?
 C24 C23 H23B 111.2 . . ?
 C25 C24 C23 129.1(4) . . ?
 C29 C24 C23 110.5(2) . . ?
 C29 C24 C25 120.4(4) . . ?
 C26 C25 C24 118.3(4) . . ?
 O2A C25 C24 112.5(8) . . ?
 O2A C25 C26 128.9(8) . . ?
 O2 C25 C24 117.3(8) . . ?
 O2 C25 C26 123.9(7) . . ?
 C25 C26 H26 119.5 . . ?
 C27 C26 C25 121.0(3) . . ?
 C27 C26 H26 119.5 . . ?
 C26 C27 H27 119.1 . . ?
 C26 C27 C28 121.8(4) . . ?
 C28 C27 H27 119.1 . . ?
 O3 C28 C27 125.9(4) . . ?
 O3 C28 C29 117.2(3) . . ?
 C27 C28 C29 116.8(4) . . ?
 C24 C29 C21 108.3(3) . . ?
 C24 C29 C28 121.3(3) . . ?
 C28 C29 C21 130.2(3) . . ?
 O3 C31 H31A 109.5 . . ?
 O3 C31 H31B 109.5 . . ?
 O3 C31 H31C 109.5 . . ?
 H31A C31 H31B 109.5 . . ?
 H31A C31 H31C 109.5 . . ?
 H31B C31 H31C 109.5 . . ?
 C25 O2A C30 126.8(14) . . ?
 O2A C30 H30A 109.5 . . ?
 O2A C30 H30B 109.5 . . ?
 O2A C30 H30C 109.5 . . ?
 H30A C30 H30B 109.5 . . ?
 H30A C30 H30C 109.5 . . ?
 H30B C30 H30C 109.5 . . ?
 C25 O2 C30A 105.1(11) . . ?
 O2 C30A H30D 109.5 . . ?
 O2 C30A H30E 109.5 . . ?
 O2 C30A H30F 109.5 . . ?
 H30D C30A H30E 109.5 . . ?
 H30D C30A H30F 109.5 . . ?
 H30E C30A H30F 109.5 . . ?

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
 S18 C10 C13 C12 3.1(3) . . . . ?
 S18 C10 C13 C14 -177.5(2) . . . . ?
 S18 C10 C17 Br1 -3.6(3) . . . . ?
 S18 C10 C17 C16 177.3(2) . . . . ?
 S18 C11 C12 O1 176.2(2) . . . . ?
 S18 C11 C12 C13 -2.9(2) . . . . ?
 S18 C11 C21 C22 158.6(2) . . . . ?
 S18 C11 C21 C29 -7.4(4) . . . . ?
 O1 C12 C13 C10 -179.1(2) . . . . ?
 O1 C12 C13 C14 1.5(4) . . . . ?
 O3 C28 C29 C21 -4.7(5) . . . . ?
 O3 C28 C29 C24 169.5(3) . . . . ?
 O25 C22 C23 C24 -153.9(2) . . . . ?
 C3 C5 C22 O25 71.6(3) . . . . ?
 C3 C5 C22 C21 -58.0(3) . . . . ?
 C3 C5 C22 C23 -168.2(2) . . . . ?
 C4 C5 C22 O25 -53.4(3) . . . . ?
 C4 C5 C22 C21 177.1(2) . . . . ?
 C4 C5 C22 C23 66.9(3) . . . . ?
 C5 C22 C23 C24 83.9(3) . . . . ?
 C10 S18 C11 C12 3.87(18) . . . . ?
 C10 S18 C11 C21 -171.8(2) . . . . ?
 C10 C13 C14 C15 -0.3(4) . . . . ?
 C11 S18 C10 C13 -4.1(2) . . . . ?
 C11 S18 C10 C17 177.1(2) . . . . ?
 C11 C12 C13 C10 0.0(3) . . . . ?
 C11 C12 C13 C14 -179.4(2) . . . . ?
 C11 C21 C22 O25 -17.2(4) . . . . ?
 C11 C21 C22 C5 109.8(3) . . . . ?
 C11 C21 C22 C23 -132.8(3) . . . . ?
 C11 C21 C29 C24 143.4(3) . . . . ?
 C11 C21 C29 C28 -41.9(5) . . . . ?
 C12 C11 C21 C22 -16.2(4) . . . . ?
 C12 C11 C21 C29 177.8(3) . . . . ?
 C12 C13 C14 C15 179.1(2) . . . . ?
 C13 C10 C17 Br1 177.70(19) . . . . ?
 C13 C10 C17 C16 -1.5(4) . . . . ?
 C13 C14 C15 C16 -0.7(4) . . . . ?
 C14 C15 C16 C17 0.6(4) . . . . ?
 C15 C16 C17 Br1 -178.6(2) . . . . ?
 C15 C16 C17 C10 0.5(4) . . . . ?
 C17 C10 C13 C12 -178.1(2) . . . . ?
 C17 C10 C13 C14 1.4(4) . . . . ?
 C21 C11 C12 O1 -8.5(4) . . . . ?
 C21 C11 C12 C13 172.4(2) . . . . ?
 C21 C22 C23 C24 -32.4(3) . . . . ?
 C22 C21 C29 C24 -25.5(3) . . . . ?
 C22 C21 C29 C28 149.3(3) . . . . ?
 C22 C23 C24 C25 -159.0(3) . . . . ?
 C22 C23 C24 C29 19.1(3) . . . . ?
 C23 C24 C25 C26 176.3(3) . . . . ?
 C23 C24 C25 O2A -9.7(13) . . . . ?
 C23 C24 C25 O2 4.2(13) . . . . ?
 C23 C24 C29 C21 3.7(3) . . . . ?
 C23 C24 C29 C28 -171.6(3) . . . . ?
 C24 C25 C26 C27 -2.5(6) . . . . ?
 C24 C25 O2A C30 173.0(18) . . . . ?
 C24 C25 O2 C30A -178.5(9) . . . . ?
 C25 C24 C29 C21 -178.0(3) . . . . ?
 C25 C24 C29 C28 6.6(5) . . . . ?
 C25 C26 C27 C28 1.7(6) . . . . ?
 C26 C25 O2A C30 -14(3) . . . . ?
 C26 C25 O2 C30A 10(2) . . . . ?
 C26 C27 C28 O3 -173.3(3) . . . . ?
 C26 C27 C28 C29 3.2(5) . . . . ?
 C27 C28 C29 C21 178.5(3) . . . . ?
 C27 C28 C29 C24 -7.3(4) . . . . ?
 C29 C21 C22 O25 151.0(2) . . . . ?
 C29 C21 C22 C5 -82.0(2) . . . . ?
 C29 C21 C22 C23 35.4(3) . . . . ?
 C29 C24 C25 C26 -1.6(5) . . . . ?
 C29 C24 C25 O2A 172.5(13) . . . . ?
 C29 C24 C25 O2 -173.7(12) . . . . ?
 C31 O3 C28 C27 -3.6(5) . . . . ?
 C31 O3 C28 C29 179.9(3) . . . . ?
 O2A C25 C26 C27 -175.4(15) . . . . ?
 O2 C25 C26 C27 169.0(13) . . . . ?

_olex2_date_sample_data_collection  2023-06-12
_olex2_diffrn_ambient_temperature_device  'Oxford Instruments Cryojet'
_olex2_exptl_crystal_mounting_method 
 'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id  PKB-141a
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.354
_oxdiff_exptl_absorpt_empirical_full_min  0.771
