# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Badjic_TN_ClosedAcetone
_database_code_depnum_ccdc_archive 'CCDC 1939474'
loop_
_audit_author_name
_audit_author_address
'Curtis Moore'
;The Ohio State University
United States of America
;
_audit_update_record             
;
2019-07-09 deposited with the CCDC.	2019-09-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H15 Br3 O3, C3 H6 O'
_chemical_formula_sum            'C27 H21 Br3 O4'
_chemical_formula_weight         649.17
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 '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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   11.7759(6)
_cell_length_b                   8.8470(4)
_cell_length_c                   23.5375(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.994(2)
_cell_angle_gamma                90
_cell_volume                     2451.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.334
_cell_measurement_theta_min      2.880
_shelx_estimated_absorpt_T_max   0.710
_shelx_estimated_absorpt_T_min   0.489
_exptl_absorpt_coefficient_mu    4.968
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0595 before and 0.0464 after correction. The Ratio of minimum to maximum transmission is 0.6781. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'Redish Orange'
_exptl_crystal_colour_modifier   Redish
_exptl_crystal_colour_primary    Orange
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.074
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30295
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_min         2.880
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Curved-Graphite, Bruker TRIUMPH'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4125
_reflns_number_total             5015
_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       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5015
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0285
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²+2.8084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0690
_refine_special_details          ?
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C5(H5), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16),
 C20(H20), C21(H21), C23(H23)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C1S(H1SA,H1SB,H1SC), C3S(H3SA,H3SB,H3SC)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.69022(3) 1.06201(4) 0.91751(2) 0.04235(9) Uani 1 1 d . . . . .
Br2 Br -0.04603(3) 0.34949(4) 0.93379(2) 0.05296(10) Uani 1 1 d . . . . .
Br3 Br 0.27924(3) 1.11980(4) 0.50562(2) 0.04906(10) Uani 1 1 d . . . . .
O1 O 0.28542(16) 0.6718(2) 0.86303(7) 0.0348(4) Uani 1 1 d . . . . .
O2 O 0.34524(15) 0.96465(19) 0.75327(7) 0.0280(4) Uani 1 1 d . . . . .
O3 O 0.15750(18) 0.4934(2) 0.70755(8) 0.0418(5) Uani 1 1 d . . . . .
H3 H 0.113480 0.464730 0.681232 0.063 Uiso 1 1 calc GR . . . .
C1 C 0.3791(2) 0.7619(3) 0.87231(11) 0.0288(5) Uani 1 1 d . . . . .
C2 C 0.4134(2) 0.7771(3) 0.92898(11) 0.0326(6) Uani 1 1 d . . . . .
H2 H 0.373517 0.726302 0.958048 0.039 Uiso 1 1 calc R . . . .
C3 C 0.5054(2) 0.8662(3) 0.94243(11) 0.0323(6) Uani 1 1 d . . . . .
H3A H 0.529115 0.878934 0.980918 0.039 Uiso 1 1 calc R . . . .
C4 C 0.5634(2) 0.9376(3) 0.89919(11) 0.0317(6) Uani 1 1 d . . . . .
C5 C 0.5304(2) 0.9211(3) 0.84299(11) 0.0301(6) Uani 1 1 d . . . . .
H5 H 0.572027 0.969621 0.813953 0.036 Uiso 1 1 calc R . . . .
C6 C 0.4359(2) 0.8331(3) 0.82903(10) 0.0265(5) Uani 1 1 d . . . . .
C7 C 0.3960(2) 0.8168(3) 0.76807(10) 0.0275(5) Uani 1 1 d . . . . .
C8 C 0.3048(2) 0.6988(3) 0.76323(10) 0.0289(5) Uani 1 1 d . . . . .
H8 H 0.282517 0.665948 0.726265 0.035 Uiso 1 1 calc R . . . .
C9 C 0.2532(2) 0.6371(3) 0.80749(11) 0.0295(6) Uani 1 1 d . . . . .
C10 C 0.1569(2) 0.5302(3) 0.80790(11) 0.0312(6) Uani 1 1 d . . . . .
C11 C 0.1101(2) 0.4635(3) 0.75829(12) 0.0360(6) Uani 1 1 d . . . . .
C12 C 0.0172(3) 0.3672(3) 0.76219(14) 0.0428(7) Uani 1 1 d . . . . .
H12 H -0.013293 0.322122 0.728612 0.051 Uiso 1 1 calc R . . . .
C13 C -0.0314(3) 0.3359(3) 0.81328(15) 0.0457(8) Uani 1 1 d . . . . .
H13 H -0.096104 0.272135 0.815124 0.055 Uiso 1 1 calc R . . . .
C14 C 0.0154(2) 0.3987(3) 0.86226(13) 0.0391(7) Uani 1 1 d . . . . .
C15 C 0.1072(2) 0.4940(3) 0.85995(12) 0.0352(6) Uani 1 1 d . . . . .
H15 H 0.137633 0.536130 0.894089 0.042 Uiso 1 1 calc R . . . .
C16 C 0.4926(2) 0.7833(3) 0.72897(10) 0.0286(5) Uani 1 1 d . . . . .
H16 H 0.553599 0.722530 0.742767 0.034 Uiso 1 1 calc R . . . .
C17 C 0.4964(2) 0.8349(3) 0.67598(11) 0.0306(6) Uani 1 1 d . . . . .
C18 C 0.4051(2) 0.9354(3) 0.65607(11) 0.0289(5) Uani 1 1 d . . . . .
C19 C 0.3320(2) 0.9966(3) 0.69603(10) 0.0271(5) Uani 1 1 d . . . . .
C20 C 0.2481(2) 1.0994(3) 0.68075(11) 0.0321(6) Uani 1 1 d . . . . .
H20 H 0.201120 1.142571 0.708861 0.039 Uiso 1 1 calc R . . . .
C21 C 0.2333(2) 1.1389(3) 0.62384(12) 0.0364(6) Uani 1 1 d . . . . .
H21 H 0.176150 1.209089 0.612561 0.044 Uiso 1 1 calc R . . . .
C22 C 0.3027(3) 1.0745(3) 0.58432(11) 0.0355(6) Uani 1 1 d . . . . .
C23 C 0.3887(2) 0.9761(3) 0.59905(11) 0.0333(6) Uani 1 1 d . . . . .
H23 H 0.436691 0.935984 0.570719 0.040 Uiso 1 1 calc R . . . .
C24 C 0.5911(2) 0.7942(3) 0.63692(12) 0.0388(7) Uani 1 1 d . . . . .
H24A H 0.560543 0.736368 0.604618 0.058 Uiso 1 1 calc GR . . . .
H24B H 0.647578 0.733024 0.657582 0.058 Uiso 1 1 calc GR . . . .
H24C H 0.627091 0.886755 0.623069 0.058 Uiso 1 1 calc GR . . . .
O1S O 0.02021(19) 0.4085(3) 0.61929(10) 0.0548(6) Uani 1 1 d . . . . .
C1S C -0.1478(3) 0.5399(4) 0.63987(18) 0.0620(10) Uani 1 1 d . . . . .
H1SA H -0.214890 0.479557 0.648924 0.093 Uiso 1 1 calc GR . . . .
H1SB H -0.171532 0.632242 0.619995 0.093 Uiso 1 1 calc GR . . . .
H1SC H -0.106977 0.566695 0.675080 0.093 Uiso 1 1 calc GR . . . .
C2S C -0.0721(3) 0.4508(4) 0.60298(13) 0.0441(7) Uani 1 1 d . . . . .
C3S C -0.1136(4) 0.4130(7) 0.54488(16) 0.0986(19) Uani 1 1 d . . . . .
H3SA H -0.133380 0.506166 0.524493 0.148 Uiso 1 1 calc GR . . . .
H3SB H -0.180988 0.348355 0.547257 0.148 Uiso 1 1 calc GR . . . .
H3SC H -0.053994 0.359348 0.524483 0.148 Uiso 1 1 calc GR . . . .


_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 C4 1.899(3) . ?
Br2 C14 1.895(3) . ?
Br3 C22 1.911(3) . ?
O1 C1 1.375(3) . ?
O1 C9 1.390(3) . ?
O2 C7 1.478(3) . ?
O2 C19 1.383(3) . ?
O3 H3 0.8400 . ?
O3 C11 1.353(3) . ?
C1 C2 1.394(3) . ?
C1 C6 1.380(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.372(4) . ?
C3 H3A 0.9500 . ?
C3 C4 1.387(4) . ?
C4 C5 1.380(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(4) . ?
C6 C7 1.509(3) . ?
C7 C8 1.501(4) . ?
C7 C16 1.505(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.332(4) . ?
C9 C10 1.477(4) . ?
C10 C11 1.411(4) . ?
C10 C15 1.403(4) . ?
C11 C12 1.391(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.369(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(4) . ?
C14 C15 1.373(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.330(4) . ?
C17 C18 1.466(4) . ?
C17 C24 1.501(4) . ?
C18 C19 1.395(4) . ?
C18 C23 1.400(4) . ?
C19 C20 1.386(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.392(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.373(4) . ?
C22 C23 1.376(4) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O1S C2S 1.206(4) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C1S C2S 1.482(5) . ?
C2S C3S 1.483(5) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 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
C1 O1 C9 118.9(2) . . ?
C19 O2 C7 116.67(18) . . ?
C11 O3 H3 109.5 . . ?
O1 C1 C2 115.3(2) . . ?
O1 C1 C6 123.0(2) . . ?
C6 C1 C2 121.7(2) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 H3A 120.4 . . ?
C2 C3 C4 119.2(2) . . ?
C4 C3 H3A 120.4 . . ?
C3 C4 Br1 119.49(19) . . ?
C5 C4 Br1 119.1(2) . . ?
C5 C4 C3 121.5(2) . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.7(2) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 118.5(2) . . ?
C1 C6 C7 120.8(2) . . ?
C5 C6 C7 120.8(2) . . ?
O2 C7 C6 104.91(19) . . ?
O2 C7 C8 108.2(2) . . ?
O2 C7 C16 109.7(2) . . ?
C8 C7 C6 110.4(2) . . ?
C8 C7 C16 111.4(2) . . ?
C16 C7 C6 112.0(2) . . ?
C7 C8 H8 117.9 . . ?
C9 C8 C7 124.2(2) . . ?
C9 C8 H8 117.9 . . ?
O1 C9 C10 109.4(2) . . ?
C8 C9 O1 121.6(2) . . ?
C8 C9 C10 128.9(2) . . ?
C11 C10 C9 123.4(2) . . ?
C15 C10 C9 118.9(2) . . ?
C15 C10 C11 117.7(3) . . ?
O3 C11 C10 119.2(2) . . ?
O3 C11 C12 121.0(3) . . ?
C12 C11 C10 119.8(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.5(3) . . ?
C13 C12 H12 119.2 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 119.0(3) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 Br2 119.7(2) . . ?
C15 C14 Br2 119.3(2) . . ?
C15 C14 C13 121.0(3) . . ?
C10 C15 H15 119.5 . . ?
C14 C15 C10 121.0(3) . . ?
C14 C15 H15 119.5 . . ?
C7 C16 H16 118.5 . . ?
C17 C16 C7 123.0(2) . . ?
C17 C16 H16 118.5 . . ?
C16 C17 C18 118.1(2) . . ?
C16 C17 C24 122.0(3) . . ?
C18 C17 C24 119.9(2) . . ?
C19 C18 C17 118.5(2) . . ?
C19 C18 C23 118.1(2) . . ?
C23 C18 C17 123.4(2) . . ?
O2 C19 C18 121.1(2) . . ?
O2 C19 C20 117.1(2) . . ?
C20 C19 C18 121.7(2) . . ?
C19 C20 H20 120.3 . . ?
C19 C20 C21 119.4(3) . . ?
C21 C20 H20 120.3 . . ?
C20 C21 H21 120.6 . . ?
C22 C21 C20 118.8(3) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 Br3 119.5(2) . . ?
C21 C22 C23 122.4(2) . . ?
C23 C22 Br3 118.1(2) . . ?
C18 C23 H23 120.2 . . ?
C22 C23 C18 119.5(3) . . ?
C22 C23 H23 120.2 . . ?
C17 C24 H24A 109.5 . . ?
C17 C24 H24B 109.5 . . ?
C17 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
O1S C2S C1S 121.7(3) . . ?
O1S C2S C3S 120.3(3) . . ?
C1S C2S C3S 117.9(3) . . ?
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O1S 0.84 1.88 2.716(3) 176.4 . yes
C8 H8 O3 0.95 2.16 2.820(3) 125.4 . yes

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Badjic_TN_2BrHCl
_database_code_depnum_ccdc_archive 'CCDC 1939475'
loop_
_audit_author_name
_audit_author_address
'Curtis Moore'
;The Ohio State University
United States of America
;
_audit_update_record             
;
2019-07-09 deposited with the CCDC.	2019-09-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H11 Br2 O2, Cl'
_chemical_formula_sum            'C16 H11 Br2 Cl O2'
_chemical_formula_weight         430.52
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_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                   8.6085(8)
_cell_length_b                   9.1123(8)
_cell_length_c                   10.0471(10)
_cell_angle_alpha                74.183(3)
_cell_angle_beta                 80.293(3)
_cell_angle_gamma                85.184(3)
_cell_volume                     746.83(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7330
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.338
_cell_measurement_theta_min      2.960
_shelx_estimated_absorpt_T_max   0.638
_shelx_estimated_absorpt_T_min   0.483
_exptl_absorpt_coefficient_mu    5.606
_exptl_absorpt_correction_T_max  0.093175
_exptl_absorpt_correction_T_min  0.060453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 45512 reflections, Rint = 0.0428
 (27152 with I > 3sig(I), Rint = 0.0341)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'Light Yellow'
_exptl_crystal_colour_modifier   Light
_exptl_crystal_colour_primary    Yellow
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             420
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.088
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            45442
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         3.276
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Photon II MoTRIUMPH'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Curved-Graphite, Bruker TRIUMPH'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2644
_reflns_number_total             3058
_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       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0217
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0226P)²+0.3723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0491
_refine_special_details          ?
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C8(H8), C12(H12), C13(H13), C15(H15)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 1.31600(3) 0.08333(3) 0.96279(2) 0.02122(7) Uani 1 1 d . . . . .
Br2 Br 0.46482(3) 0.15643(3) 0.26752(3) 0.02762(8) Uani 1 1 d . . . . .
O1 O 0.74398(17) 0.19661(17) 0.67777(16) 0.0182(3) Uani 1 1 d . . . . .
O2 O 0.32800(18) 0.45517(18) 0.74105(17) 0.0214(3) Uani 1 1 d . . . . .
H2 H 0.250181 0.516658 0.728466 0.032 Uiso 1 1 calc GR . . . .
C1 C 0.8735(3) 0.1755(2) 0.7437(2) 0.0175(5) Uani 1 1 d . . . . .
C2 C 0.9837(3) 0.0639(3) 0.7152(2) 0.0206(5) Uani 1 1 d . . . . .
H2A H 0.968955 0.007592 0.651691 0.025 Uiso 1 1 calc R . . . .
C3 C 1.1146(3) 0.0368(3) 0.7810(2) 0.0206(5) Uani 1 1 d . . . . .
H3 H 1.191779 -0.039496 0.763966 0.025 Uiso 1 1 calc R . . . .
C4 C 1.1339(3) 0.1221(2) 0.8735(2) 0.0190(5) Uani 1 1 d . . . . .
C5 C 1.0240(3) 0.2314(2) 0.9036(2) 0.0185(5) Uani 1 1 d . . . . .
H5 H 1.039232 0.286874 0.967608 0.022 Uiso 1 1 calc R . . . .
C6 C 0.8888(3) 0.2596(2) 0.8378(2) 0.0181(5) Uani 1 1 d . . . . .
C7 C 0.7629(3) 0.3662(2) 0.8646(2) 0.0188(5) Uani 1 1 d . . . . .
C8 C 0.6340(3) 0.3785(2) 0.7979(2) 0.0190(5) Uani 1 1 d . . . . .
H8 H 0.547911 0.445487 0.817865 0.023 Uiso 1 1 calc R . . . .
C9 C 0.6257(3) 0.2951(2) 0.7015(2) 0.0181(5) Uani 1 1 d . . . . .
C10 C 0.5033(3) 0.3043(2) 0.6171(2) 0.0186(5) Uani 1 1 d . . . . .
C11 C 0.3568(3) 0.3844(2) 0.6389(2) 0.0191(5) Uani 1 1 d . . . . .
C12 C 0.2439(3) 0.3853(3) 0.5537(2) 0.0206(5) Uani 1 1 d . . . . .
H12 H 0.144464 0.436383 0.569876 0.025 Uiso 1 1 calc R . . . .
C13 C 0.2729(3) 0.3144(3) 0.4473(2) 0.0223(5) Uani 1 1 d . . . . .
H13 H 0.194528 0.315078 0.390962 0.027 Uiso 1 1 calc R . . . .
C14 C 0.4195(3) 0.2414(3) 0.4237(2) 0.0210(5) Uani 1 1 d . . . . .
C15 C 0.5323(3) 0.2335(2) 0.5061(2) 0.0203(5) Uani 1 1 d . . . . .
H15 H 0.630257 0.180393 0.488891 0.024 Uiso 1 1 calc R . . . .
C16 C 0.7731(3) 0.4621(3) 0.9604(3) 0.0251(5) Uani 1 1 d . . . . .
H16A H 0.859239 0.532410 0.920517 0.038 Uiso 1 1 calc GR . . . .
H16B H 0.793356 0.396590 1.051360 0.038 Uiso 1 1 calc GR . . . .
H16C H 0.673407 0.520735 0.972787 0.038 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.07306(7) 0.68813(7) 0.70085(7) 0.02713(14) Uani 1 1 d . . . . .


_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 C4 1.896(2) . ?
Br2 C14 1.902(2) . ?
O1 C1 1.365(3) . ?
O1 C9 1.334(3) . ?
O2 C11 1.334(3) . ?
C1 C2 1.386(3) . ?
C1 C6 1.397(3) . ?
C2 C3 1.373(3) . ?
C3 C4 1.401(3) . ?
C4 C5 1.374(3) . ?
C5 C6 1.405(3) . ?
C6 C7 1.435(3) . ?
C7 C8 1.372(3) . ?
C7 C16 1.483(3) . ?
C8 C9 1.398(3) . ?
C9 C10 1.444(3) . ?
C10 C11 1.418(3) . ?
C10 C15 1.412(3) . ?
C11 C12 1.397(3) . ?
C12 C13 1.372(3) . ?
C13 C14 1.391(3) . ?
C14 C15 1.364(3) . ?

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
C9 O1 C1 122.13(18) . . ?
O1 C1 C2 116.2(2) . . ?
O1 C1 C6 120.80(19) . . ?
C2 C1 C6 122.9(2) . . ?
C3 C2 C1 118.3(2) . . ?
C2 C3 C4 119.7(2) . . ?
C3 C4 Br1 119.01(16) . . ?
C5 C4 Br1 118.71(17) . . ?
C5 C4 C3 122.3(2) . . ?
C4 C5 C6 118.7(2) . . ?
C1 C6 C5 118.1(2) . . ?
C1 C6 C7 117.9(2) . . ?
C5 C6 C7 124.0(2) . . ?
C6 C7 C16 120.8(2) . . ?
C8 C7 C6 118.3(2) . . ?
C8 C7 C16 120.9(2) . . ?
C7 C8 C9 121.8(2) . . ?
O1 C9 C8 119.0(2) . . ?
O1 C9 C10 113.25(19) . . ?
C8 C9 C10 127.7(2) . . ?
C11 C10 C9 122.8(2) . . ?
C15 C10 C9 118.5(2) . . ?
C15 C10 C11 118.7(2) . . ?
O2 C11 C10 119.8(2) . . ?
O2 C11 C12 121.2(2) . . ?
C12 C11 C10 119.0(2) . . ?
C13 C12 C11 121.7(2) . . ?
C12 C13 C14 118.7(2) . . ?
C13 C14 Br2 118.47(18) . . ?
C15 C14 Br2 119.45(17) . . ?
C15 C14 C13 122.0(2) . . ?
C14 C15 C10 119.9(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 Cl1 0.84 2.09 2.9215(16) 173.3 . yes
C8 H8 O2 0.95 2.15 2.781(3) 122.9 . yes

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Badjic_TN_OpenClosed
_database_code_depnum_ccdc_archive 'CCDC 1939476'
loop_
_audit_author_name
_audit_author_address
'Curtis Moore'
;The Ohio State University
United States of America
;
_audit_update_record             
;
2019-07-09 deposited with the CCDC.	2019-09-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H15 Br3 O3, C24 H16 Br3 O3, C H3 O3 S'
_chemical_formula_sum            'C49 H34 Br6 O9 S'
_chemical_formula_weight         1278.28
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 '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'

_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                   11.4092(9)
_cell_length_b                   14.1314(10)
_cell_length_c                   15.9669(12)
_cell_angle_alpha                109.501(2)
_cell_angle_beta                 99.298(3)
_cell_angle_gamma                101.718(2)
_cell_volume                     2301.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.370
_cell_measurement_theta_min      2.780
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.604
_exptl_absorpt_coefficient_mu    5.336
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0724 before and 0.0495 after correction. The Ratio of minimum to maximum transmission is 0.6416. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_colour_modifier   Dark
_exptl_crystal_colour_primary    Red
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.017
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62357
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.391
_diffrn_reflns_theta_min         2.780
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Curved-Graphite, Bruker TRIUMPH'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7396
_reflns_number_total             9395
_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       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         9395
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0386
_refine_ls_restrained_S_all      1.020
_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)+(0.0486P)²+5.8926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1028
_refine_special_details          ?
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C5(H5), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16),
 C20(H20), C21(H21), C23(H23), C2'(H2'A), C3'(H3'A), C5'(H5'), C8'(H8'),
 C12'(H12'), C13'(H13'), C15'(H15'), C16'(H16'), C20'(H20'), C21'(H21'),
 C23'(H23')
2.b Idealised Me refined as rotating group:
 C24(H24D,H24E,H24F), C24'(H24A,H24B,H24C), C1A(H1AA,H1AB,H1AC)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O2'(H2'), O3'(H3')
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 1.25311(5) 0.94516(4) 1.20886(4) 0.04480(14) Uani 1 1 d . . . . .
Br2 Br 0.39814(5) 0.33611(4) 0.92119(4) 0.04752(15) Uani 1 1 d . . . . .
Br3 Br 1.42658(5) 1.03383(4) 0.87119(4) 0.04673(15) Uani 1 1 d . . . . .
O1 O 0.8404(3) 0.5619(2) 0.9740(2) 0.0335(7) Uani 1 1 d . . . . .
O2 O 1.0160(3) 0.6705(2) 0.8392(2) 0.0301(7) Uani 1 1 d . . . . .
O3 O 0.8012(3) 0.3161(2) 0.7202(2) 0.0287(7) Uani 1 1 d . . . . .
H3 H 0.773365 0.264984 0.669871 0.043 Uiso 1 1 calc GR . . . .
C1 C 0.9416(4) 0.6450(3) 1.0258(3) 0.0264(9) Uani 1 1 d . . . . .
C2 C 0.9338(4) 0.7033(4) 1.1129(3) 0.0328(10) Uani 1 1 d . . . . .
H2 H 0.864071 0.682117 1.134532 0.039 Uiso 1 1 calc R . . . .
C3 C 1.0269(4) 0.7916(4) 1.1677(3) 0.0328(10) Uani 1 1 d . . . . .
H3A H 1.021691 0.832768 1.226959 0.039 Uiso 1 1 calc R . . . .
C4 C 1.1282(4) 0.8195(3) 1.1352(3) 0.0311(10) Uani 1 1 d . . . . .
C5 C 1.1405(4) 0.7590(3) 1.0516(3) 0.0306(10) Uani 1 1 d . . . . .
H5 H 1.214303 0.776728 1.033083 0.037 Uiso 1 1 calc R . . . .
C6 C 1.0437(4) 0.6710(3) 0.9933(3) 0.0269(9) Uani 1 1 d . . . . .
C7 C 1.0456(4) 0.6093(3) 0.8962(3) 0.0282(9) Uani 1 1 d . . . . .
C8 C 0.9409(4) 0.5119(3) 0.8549(3) 0.0300(10) Uani 1 1 d . . . . .
H8 H 0.942762 0.459462 0.799725 0.036 Uiso 1 1 calc R . . . .
C9 C 0.8459(4) 0.4944(3) 0.8903(3) 0.0260(9) Uani 1 1 d . . . . .
C10 C 0.7321(4) 0.4059(3) 0.8503(3) 0.0267(9) Uani 1 1 d . . . . .
C11 C 0.7131(4) 0.3207(3) 0.7691(3) 0.0263(9) Uani 1 1 d . . . . .
C12 C 0.6049(4) 0.2390(3) 0.7373(3) 0.0311(10) Uani 1 1 d . . . . .
H12 H 0.594824 0.179887 0.683257 0.037 Uiso 1 1 calc R . . . .
C13 C 0.5125(4) 0.2427(3) 0.7830(3) 0.0327(10) Uani 1 1 d . . . . .
H13 H 0.439042 0.186593 0.760858 0.039 Uiso 1 1 calc R . . . .
C14 C 0.5277(4) 0.3280(4) 0.8606(3) 0.0328(10) Uani 1 1 d . . . . .
C15 C 0.6357(4) 0.4085(3) 0.8956(3) 0.0315(10) Uani 1 1 d . . . . .
H15 H 0.645205 0.466092 0.950689 0.038 Uiso 1 1 calc R . . . .
C16 C 1.1679(4) 0.5876(3) 0.8870(3) 0.0297(9) Uani 1 1 d . . . . .
H16 H 1.182143 0.525805 0.892607 0.036 Uiso 1 1 calc R . . . .
C17 C 1.2569(4) 0.6518(3) 0.8714(3) 0.0303(10) Uani 1 1 d . . . . .
C18 C 1.2332(4) 0.7461(3) 0.8611(3) 0.0295(9) Uani 1 1 d . . . . .
C19 C 1.1106(4) 0.7524(3) 0.8463(3) 0.0285(9) Uani 1 1 d . . . . .
C20 C 1.0818(4) 0.8378(4) 0.8347(3) 0.0324(10) Uani 1 1 d . . . . .
H20 H 0.998143 0.839495 0.822738 0.039 Uiso 1 1 calc R . . . .
C21 C 1.1754(5) 0.9217(4) 0.8405(3) 0.0354(11) Uani 1 1 d . . . . .
H21 H 1.156415 0.980919 0.832283 0.042 Uiso 1 1 calc R . . . .
C22 C 1.2960(4) 0.9174(4) 0.8583(3) 0.0339(10) Uani 1 1 d . . . . .
C23 C 1.3266(5) 0.8313(4) 0.8677(3) 0.0345(10) Uani 1 1 d . . . . .
H23 H 1.410447 0.829874 0.878486 0.041 Uiso 1 1 calc R . . . .
C24 C 1.3805(5) 0.6310(4) 0.8648(4) 0.0405(12) Uani 1 1 d . . . . .
H24D H 1.399152 0.635576 0.808292 0.061 Uiso 1 1 calc GR . . . .
H24E H 1.377554 0.560998 0.864177 0.061 Uiso 1 1 calc GR . . . .
H24F H 1.444853 0.683043 0.917837 0.061 Uiso 1 1 calc GR . . . .
Br1' Br -0.12886(4) 0.66158(3) 0.35228(3) 0.02628(10) Uani 1 1 d . . . . .
Br2' Br -0.18000(4) -0.11786(3) 0.32712(3) 0.02726(11) Uani 1 1 d . . . . .
Br3' Br 0.17337(5) 0.15935(4) 0.02908(4) 0.04644(14) Uani 1 1 d . . . . .
O1' O -0.0214(2) 0.28074(19) 0.39536(18) 0.0181(5) Uani 1 1 d . . . . .
O2' O 0.5267(3) 0.3736(2) 0.4027(2) 0.0291(7) Uani 1 1 d . . . . .
H2' H 0.553826 0.330518 0.420090 0.044 Uiso 1 1 calc GR . . . .
O3' O 0.3078(2) 0.2117(2) 0.4630(2) 0.0257(6) Uani 1 1 d . . . . .
H3' H 0.365112 0.186130 0.476418 0.039 Uiso 1 1 calc GR . . . .
C1' C -0.0406(4) 0.3702(3) 0.3870(3) 0.0194(8) Uani 1 1 d . . . . .
C2' C -0.1603(4) 0.3787(3) 0.3824(3) 0.0223(8) Uani 1 1 d . . . . .
H2'A H -0.223131 0.325430 0.385663 0.027 Uiso 1 1 calc R . . . .
C3' C -0.1856(4) 0.4663(3) 0.3729(3) 0.0228(8) Uani 1 1 d . . . . .
H3'A H -0.266697 0.474328 0.369352 0.027 Uiso 1 1 calc R . . . .
C4' C -0.0904(4) 0.5435(3) 0.3686(3) 0.0211(8) Uani 1 1 d . . . . .
C5' C 0.0281(4) 0.5364(3) 0.3744(3) 0.0195(8) Uani 1 1 d . . . . .
H5' H 0.090589 0.590552 0.371945 0.023 Uiso 1 1 calc R . . . .
C6' C 0.0559(3) 0.4468(3) 0.3842(3) 0.0182(8) Uani 1 1 d . . . . .
C7' C 0.1755(4) 0.4285(3) 0.3876(3) 0.0187(8) Uani 1 1 d . . . . .
C8' C 0.1890(4) 0.3369(3) 0.3978(3) 0.0206(8) Uani 1 1 d . . . . .
H8' H 0.268143 0.324411 0.403203 0.025 Uiso 1 1 calc R . . . .
C9' C 0.0906(3) 0.2638(3) 0.4003(3) 0.0185(8) Uani 1 1 d . . . . .
C10' C 0.0903(4) 0.1627(3) 0.4050(3) 0.0187(8) Uani 1 1 d . . . . .
C11' C 0.1991(4) 0.1382(3) 0.4346(3) 0.0195(8) Uani 1 1 d . . . . .
C12' C 0.1916(4) 0.0385(3) 0.4355(3) 0.0205(8) Uani 1 1 d . . . . .
H12' H 0.264857 0.022255 0.456452 0.025 Uiso 1 1 calc R . . . .
C13' C 0.0803(4) -0.0363(3) 0.4066(3) 0.0210(8) Uani 1 1 d . . . . .
H13' H 0.076529 -0.103669 0.407581 0.025 Uiso 1 1 calc R . . . .
C14' C -0.0276(3) -0.0125(3) 0.3756(3) 0.0191(8) Uani 1 1 d . . . . .
C15' C -0.0231(4) 0.0852(3) 0.3757(3) 0.0198(8) Uani 1 1 d . . . . .
H15' H -0.097362 0.100761 0.355657 0.024 Uiso 1 1 calc R . . . .
C16' C 0.2806(4) 0.5051(3) 0.3849(3) 0.0213(8) Uani 1 1 d . . . . .
H16' H 0.283371 0.576663 0.412367 0.026 Uiso 1 1 calc R . . . .
C17' C 0.3730(4) 0.4835(3) 0.3472(3) 0.0222(8) Uani 1 1 d . . . . .
C18' C 0.3705(4) 0.3758(3) 0.2882(3) 0.0214(8) Uani 1 1 d . . . . .
C19' C 0.4506(4) 0.3233(3) 0.3175(3) 0.0233(8) Uani 1 1 d . . . . .
C20' C 0.4473(4) 0.2235(3) 0.2603(3) 0.0287(9) Uani 1 1 d . . . . .
H20' H 0.501353 0.188027 0.280397 0.034 Uiso 1 1 calc R . . . .
C21' C 0.3662(4) 0.1755(3) 0.1747(3) 0.0321(10) Uani 1 1 d . . . . .
H21' H 0.364883 0.107491 0.135764 0.038 Uiso 1 1 calc R . . . .
C22' C 0.2869(4) 0.2265(3) 0.1459(3) 0.0306(10) Uani 1 1 d . . . . .
C23' C 0.2878(4) 0.3257(3) 0.2019(3) 0.0268(9) Uani 1 1 d . . . . .
H23' H 0.231951 0.359648 0.181564 0.032 Uiso 1 1 calc R . . . .
C24' C 0.4817(4) 0.5684(3) 0.3555(4) 0.0313(10) Uani 1 1 d . . . . .
H24A H 0.556522 0.561930 0.390420 0.047 Uiso 1 1 calc GR . . . .
H24B H 0.468803 0.636497 0.387392 0.047 Uiso 1 1 calc GR . . . .
H24C H 0.491059 0.562637 0.294193 0.047 Uiso 1 1 calc GR . . . .
S1A S 0.61247(8) 0.15503(7) 0.48216(7) 0.0189(2) Uani 1 1 d . . . . .
O1A O 0.7158(2) 0.1604(2) 0.5516(2) 0.0241(6) Uani 1 1 d . . . . .
O2A O 0.6383(3) 0.2406(2) 0.4501(2) 0.0270(6) Uani 1 1 d . . . . .
O3A O 0.4970(2) 0.1453(2) 0.5113(2) 0.0264(6) Uani 1 1 d . . . . .
C1A C 0.5907(4) 0.0392(3) 0.3880(3) 0.0293(9) Uani 1 1 d . . . . .
H1AA H 0.571983 -0.020489 0.406561 0.044 Uiso 1 1 calc GR . . . .
H1AB H 0.666139 0.041327 0.365910 0.044 Uiso 1 1 calc GR . . . .
H1AC H 0.521806 0.032117 0.338789 0.044 Uiso 1 1 calc GR . . . .


_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 C4 1.898(4) . ?
Br2 C14 1.895(4) . ?
Br3 C22 1.910(4) . ?
O1 C1 1.375(5) . ?
O1 C9 1.378(5) . ?
O2 C7 1.495(5) . ?
O2 C19 1.372(5) . ?
O3 H3 0.8400 . ?
O3 C11 1.367(5) . ?
C1 C2 1.388(6) . ?
C1 C6 1.381(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.372(6) . ?
C3 H3A 0.9500 . ?
C3 C4 1.380(6) . ?
C4 C5 1.372(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.404(6) . ?
C6 C7 1.511(6) . ?
C7 C8 1.492(6) . ?
C7 C16 1.507(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.319(6) . ?
C9 C10 1.481(6) . ?
C10 C11 1.393(6) . ?
C10 C15 1.411(6) . ?
C11 C12 1.394(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.376(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.367(7) . ?
C14 C15 1.382(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.333(6) . ?
C17 C18 1.467(6) . ?
C17 C24 1.509(6) . ?
C18 C19 1.407(6) . ?
C18 C23 1.398(6) . ?
C19 C20 1.374(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.391(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.376(7) . ?
C22 C23 1.380(7) . ?
C23 H23 0.9500 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?
Br1' C4' 1.896(4) . ?
Br2' C14' 1.893(4) . ?
Br3' C22' 1.896(5) . ?
O1' C1' 1.371(4) . ?
O1' C9' 1.342(4) . ?
O2' H2' 0.8400 . ?
O2' C19' 1.354(5) . ?
O3' H3' 0.8400 . ?
O3' C11' 1.343(5) . ?
C1' C2' 1.387(5) . ?
C1' C6' 1.397(5) . ?
C2' H2'A 0.9500 . ?
C2' C3' 1.376(5) . ?
C3' H3'A 0.9500 . ?
C3' C4' 1.404(6) . ?
C4' C5' 1.366(5) . ?
C5' H5' 0.9500 . ?
C5' C6' 1.418(5) . ?
C6' C7' 1.436(5) . ?
C7' C8' 1.393(5) . ?
C7' C16' 1.460(5) . ?
C8' H8' 0.9500 . ?
C8' C9' 1.378(5) . ?
C9' C10' 1.455(5) . ?
C10' C11' 1.406(5) . ?
C10' C15' 1.407(5) . ?
C11' C12' 1.399(5) . ?
C12' H12' 0.9500 . ?
C12' C13' 1.372(5) . ?
C13' H13' 0.9500 . ?
C13' C14' 1.399(5) . ?
C14' C15' 1.371(5) . ?
C15' H15' 0.9500 . ?
C16' H16' 0.9500 . ?
C16' C17' 1.334(6) . ?
C17' C18' 1.490(5) . ?
C17' C24' 1.495(5) . ?
C18' C19' 1.404(5) . ?
C18' C23' 1.396(6) . ?
C19' C20' 1.390(6) . ?
C20' H20' 0.9500 . ?
C20' C21' 1.379(7) . ?
C21' H21' 0.9500 . ?
C21' C22' 1.379(6) . ?
C22' C23' 1.386(6) . ?
C23' H23' 0.9500 . ?
C24' H24A 0.9800 . ?
C24' H24B 0.9800 . ?
C24' H24C 0.9800 . ?
S1A O1A 1.452(3) . ?
S1A O2A 1.459(3) . ?
S1A O3A 1.462(3) . ?
S1A C1A 1.753(4) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 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
C1 O1 C9 118.9(3) . . ?
C19 O2 C7 116.2(3) . . ?
C11 O3 H3 109.5 . . ?
O1 C1 C2 115.5(4) . . ?
O1 C1 C6 122.7(4) . . ?
C6 C1 C2 121.7(4) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3A 120.6 . . ?
C2 C3 C4 118.9(4) . . ?
C4 C3 H3A 120.6 . . ?
C3 C4 Br1 118.7(3) . . ?
C5 C4 Br1 119.5(3) . . ?
C5 C4 C3 121.8(4) . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 117.8(4) . . ?
C1 C6 C7 120.1(4) . . ?
C5 C6 C7 122.0(4) . . ?
O2 C7 C6 107.7(3) . . ?
O2 C7 C16 108.7(3) . . ?
C8 C7 O2 103.2(3) . . ?
C8 C7 C6 110.5(4) . . ?
C8 C7 C16 112.2(4) . . ?
C16 C7 C6 113.9(4) . . ?
C7 C8 H8 118.0 . . ?
C9 C8 C7 124.0(4) . . ?
C9 C8 H8 118.0 . . ?
O1 C9 C10 109.9(4) . . ?
C8 C9 O1 122.0(4) . . ?
C8 C9 C10 128.1(4) . . ?
C11 C10 C9 123.9(4) . . ?
C11 C10 C15 117.6(4) . . ?
C15 C10 C9 118.5(4) . . ?
O3 C11 C10 120.2(4) . . ?
O3 C11 C12 119.4(4) . . ?
C10 C11 C12 120.4(4) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.0(4) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.2(4) . . ?
C14 C13 H13 120.4 . . ?
C13 C14 Br2 119.4(3) . . ?
C13 C14 C15 121.2(4) . . ?
C15 C14 Br2 119.4(4) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 C10 120.5(4) . . ?
C14 C15 H15 119.7 . . ?
C7 C16 H16 118.7 . . ?
C17 C16 C7 122.6(4) . . ?
C17 C16 H16 118.7 . . ?
C16 C17 C18 118.3(4) . . ?
C16 C17 C24 122.2(4) . . ?
C18 C17 C24 119.5(4) . . ?
C19 C18 C17 118.4(4) . . ?
C23 C18 C17 123.4(4) . . ?
C23 C18 C19 118.2(4) . . ?
O2 C19 C18 120.2(4) . . ?
O2 C19 C20 118.5(4) . . ?
C20 C19 C18 121.3(4) . . ?
C19 C20 H20 120.0 . . ?
C19 C20 C21 119.9(4) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 120.6 . . ?
C22 C21 C20 118.9(4) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 Br3 119.7(4) . . ?
C21 C22 C23 122.1(4) . . ?
C23 C22 Br3 118.2(4) . . ?
C18 C23 H23 120.3 . . ?
C22 C23 C18 119.5(5) . . ?
C22 C23 H23 120.3 . . ?
C17 C24 H24D 109.5 . . ?
C17 C24 H24E 109.5 . . ?
C17 C24 H24F 109.5 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
C9' O1' C1' 120.9(3) . . ?
C19' O2' H2' 109.5 . . ?
C11' O3' H3' 109.5 . . ?
O1' C1' C2' 115.6(3) . . ?
O1' C1' C6' 121.0(3) . . ?
C2' C1' C6' 123.4(3) . . ?
C1' C2' H2'A 120.9 . . ?
C3' C2' C1' 118.3(4) . . ?
C3' C2' H2'A 120.9 . . ?
C2' C3' H3'A 120.3 . . ?
C2' C3' C4' 119.3(4) . . ?
C4' C3' H3'A 120.3 . . ?
C3' C4' Br1' 118.4(3) . . ?
C5' C4' Br1' 118.8(3) . . ?
C5' C4' C3' 122.8(3) . . ?
C4' C5' H5' 120.6 . . ?
C4' C5' C6' 118.7(3) . . ?
C6' C5' H5' 120.6 . . ?
C1' C6' C5' 117.5(3) . . ?
C1' C6' C7' 118.5(3) . . ?
C5' C6' C7' 124.0(3) . . ?
C6' C7' C16' 121.4(3) . . ?
C8' C7' C6' 117.4(3) . . ?
C8' C7' C16' 121.1(3) . . ?
C7' C8' H8' 119.1 . . ?
C9' C8' C7' 121.7(4) . . ?
C9' C8' H8' 119.1 . . ?
O1' C9' C8' 120.4(3) . . ?
O1' C9' C10' 112.4(3) . . ?
C8' C9' C10' 127.2(3) . . ?
C11' C10' C9' 122.7(3) . . ?
C11' C10' C15' 118.8(3) . . ?
C15' C10' C9' 118.5(3) . . ?
O3' C11' C10' 119.3(3) . . ?
O3' C11' C12' 121.4(3) . . ?
C12' C11' C10' 119.3(3) . . ?
C11' C12' H12' 119.4 . . ?
C13' C12' C11' 121.2(4) . . ?
C13' C12' H12' 119.4 . . ?
C12' C13' H13' 120.3 . . ?
C12' C13' C14' 119.4(3) . . ?
C14' C13' H13' 120.3 . . ?
C13' C14' Br2' 119.8(3) . . ?
C15' C14' Br2' 119.5(3) . . ?
C15' C14' C13' 120.6(4) . . ?
C10' C15' H15' 119.7 . . ?
C14' C15' C10' 120.7(4) . . ?
C14' C15' H15' 119.7 . . ?
C7' C16' H16' 117.1 . . ?
C17' C16' C7' 125.8(4) . . ?
C17' C16' H16' 117.1 . . ?
C16' C17' C18' 123.0(3) . . ?
C16' C17' C24' 121.2(4) . . ?
C18' C17' C24' 115.6(3) . . ?
C19' C18' C17' 121.3(4) . . ?
C23' C18' C17' 119.7(3) . . ?
C23' C18' C19' 119.0(4) . . ?
O2' C19' C18' 116.9(4) . . ?
O2' C19' C20' 123.2(4) . . ?
C20' C19' C18' 119.9(4) . . ?
C19' C20' H20' 119.7 . . ?
C21' C20' C19' 120.5(4) . . ?
C21' C20' H20' 119.7 . . ?
C20' C21' H21' 120.1 . . ?
C22' C21' C20' 119.8(4) . . ?
C22' C21' H21' 120.1 . . ?
C21' C22' Br3' 119.7(3) . . ?
C21' C22' C23' 120.8(4) . . ?
C23' C22' Br3' 119.5(3) . . ?
C18' C23' H23' 120.0 . . ?
C22' C23' C18' 120.0(4) . . ?
C22' C23' H23' 120.0 . . ?
C17' C24' H24A 109.5 . . ?
C17' C24' H24B 109.5 . . ?
C17' C24' H24C 109.5 . . ?
H24A C24' H24B 109.5 . . ?
H24A C24' H24C 109.5 . . ?
H24B C24' H24C 109.5 . . ?
O1A S1A O2A 112.53(17) . . ?
O1A S1A O3A 112.35(17) . . ?
O1A S1A C1A 106.28(19) . . ?
O2A S1A O3A 112.12(16) . . ?
O2A S1A C1A 107.0(2) . . ?
O3A S1A C1A 106.1(2) . . ?
S1A C1A H1AA 109.5 . . ?
S1A C1A H1AB 109.5 . . ?
S1A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O1A 0.84 1.88 2.714(4) 174.1 . yes
C8 H8 O3 0.95 2.15 2.820(5) 126.6 . yes
O2' H2' O2A 0.84 1.88 2.709(4) 169.8 . yes
O3' H3' O3A 0.84 1.79 2.627(4) 174.1 . yes

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT910_Badjic_TN_OpenClosed 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: Reflections Block by Beamstop
;
# end Validation Reply Form
