# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_km-nsp-1
_database_code_depnum_ccdc_archive 'CCDC 1454211'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        3a
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H13 N O2 S2'
_chemical_formula_weight         339.41

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.1398(3)
_cell_length_b                   12.3213(4)
_cell_length_c                   16.5028(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.686(2)
_cell_angle_gamma                90.00
_cell_volume                     1614.71(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4102
_cell_measurement_theta_min      0.916
_cell_measurement_theta_max      0.945

_exptl_crystal_description       blocks
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17602
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         28.56
_reflns_number_total             4102
_reflns_number_gt                2391
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0374P)²+0.9635P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0024(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4102
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1115
_refine_ls_wR_factor_gt          0.1000
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.0086(2) 0.71004(15) 0.27849(12) 0.0525(5) Uani 1 1 d . . .
O1 O -0.0683(2) 0.81638(14) 0.26704(12) 0.0675(5) Uani 1 1 d . . .
H1 H -0.1120 0.8334 0.3055 0.101 Uiso 1 1 calc R . .
O2 O 0.2254(2) 0.39286(13) 0.11929(10) 0.0606(5) Uani 1 1 d . . .
S1 S 0.07684(9) 0.78058(5) 0.13821(4) 0.0590(2) Uani 1 1 d . . .
S2 S 0.18920(9) 0.71008(5) -0.01240(4) 0.0600(2) Uani 1 1 d . . .
C1 C 0.7881(4) 0.5518(3) 0.4560(2) 0.1039(12) Uani 1 1 d . . .
H1A H 0.7873 0.4895 0.4908 0.156 Uiso 1 1 calc R . .
H1B H 0.8043 0.6161 0.4896 0.156 Uiso 1 1 calc R . .
H1C H 0.8782 0.5451 0.4272 0.156 Uiso 1 1 calc R . .
C2 C 0.6217(3) 0.5592(2) 0.39334(17) 0.0663(7) Uani 1 1 d . . .
C3 C 0.5839(3) 0.6478(2) 0.34218(16) 0.0586(7) Uani 1 1 d . . .
H3 H 0.6609 0.7045 0.3471 0.070 Uiso 1 1 calc R . .
C4 C 0.4339(3) 0.65473(19) 0.28345(15) 0.0504(6) Uani 1 1 d . . .
H4 H 0.4125 0.7152 0.2490 0.060 Uiso 1 1 calc R . .
C5 C 0.3155(3) 0.57255(18) 0.27547(13) 0.0432(5) Uani 1 1 d . . .
C6 C 0.3527(4) 0.4837(2) 0.32741(17) 0.0743(8) Uani 1 1 d . . .
H6 H 0.2752 0.4274 0.3235 0.089 Uiso 1 1 calc R . .
C7 C 0.5043(4) 0.4774(3) 0.38531(19) 0.0900(10) Uani 1 1 d . . .
H7 H 0.5270 0.4167 0.4194 0.108 Uiso 1 1 calc R . .
C8 C 0.1495(3) 0.58051(17) 0.21063(12) 0.0415(5) Uani 1 1 d . . .
H8 H 0.0750 0.5205 0.2179 0.050 Uiso 1 1 calc R . .
C9 C 0.0645(3) 0.68740(18) 0.21837(14) 0.0462(5) Uani 1 1 d . . .
C10 C 0.1556(3) 0.67695(18) 0.08397(13) 0.0465(5) Uani 1 1 d . . .
C11 C 0.1776(3) 0.57986(17) 0.12238(12) 0.0397(5) Uani 1 1 d . . .
C12 C 0.2207(3) 0.48183(18) 0.08379(13) 0.0427(5) Uani 1 1 d . . .
C13 C 0.2578(3) 0.48854(18) -0.00008(13) 0.0421(5) Uani 1 1 d . . .
C14 C 0.3036(3) 0.3927(2) -0.03559(15) 0.0532(6) Uani 1 1 d . . .
H14 H 0.3090 0.3277 -0.0065 0.064 Uiso 1 1 calc R . .
C15 C 0.3407(3) 0.3943(2) -0.11323(16) 0.0632(7) Uani 1 1 d . . .
H15 H 0.3701 0.3303 -0.1363 0.076 Uiso 1 1 calc R . .
C16 C 0.3343(3) 0.4905(3) -0.15694(16) 0.0665(7) Uani 1 1 d . . .
H16 H 0.3602 0.4908 -0.2091 0.080 Uiso 1 1 calc R . .
C17 C 0.2903(3) 0.5848(2) -0.12400(14) 0.0593(7) Uani 1 1 d . . .
H17 H 0.2868 0.6493 -0.1536 0.071 Uiso 1 1 calc R . .
C18 C 0.2502(3) 0.58482(19) -0.04563(13) 0.0460(5) 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
N1 C9 1.294(3) . ?
N1 O1 1.396(2) . ?
O2 C12 1.240(3) . ?
S1 C10 1.759(2) . ?
S1 C9 1.771(2) . ?
S2 C10 1.721(2) . ?
S2 C18 1.746(2) . ?
C1 C2 1.516(4) . ?
C2 C3 1.373(4) . ?
C2 C7 1.375(4) . ?
C3 C4 1.385(3) . ?
C4 C5 1.384(3) . ?
C5 C6 1.383(3) . ?
C5 C8 1.531(3) . ?
C6 C7 1.387(4) . ?
C8 C9 1.506(3) . ?
C8 C11 1.523(3) . ?
C10 C11 1.347(3) . ?
C11 C12 1.444(3) . ?
C12 C13 1.483(3) . ?
C13 C18 1.398(3) . ?
C13 C14 1.405(3) . ?
C14 C15 1.379(3) . ?
C15 C16 1.382(4) . ?
C16 C17 1.365(4) . ?
C17 C18 1.402(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 N1 O1 107.67(19) . . ?
C10 S1 C9 89.79(10) . . ?
C10 S2 C18 101.21(11) . . ?
C3 C2 C7 117.8(2) . . ?
C3 C2 C1 120.9(3) . . ?
C7 C2 C1 121.3(3) . . ?
C2 C3 C4 121.6(2) . . ?
C5 C4 C3 120.7(2) . . ?
C4 C5 C6 117.8(2) . . ?
C4 C5 C8 120.6(2) . . ?
C6 C5 C8 121.6(2) . . ?
C5 C6 C7 120.8(3) . . ?
C2 C7 C6 121.3(3) . . ?
C9 C8 C11 104.70(17) . . ?
C9 C8 C5 110.36(17) . . ?
C11 C8 C5 111.91(17) . . ?
N1 C9 C8 123.4(2) . . ?
N1 C9 S1 122.94(18) . . ?
C8 C9 S1 113.65(15) . . ?
C11 C10 S2 127.87(17) . . ?
C11 C10 S1 115.50(17) . . ?
S2 C10 S1 116.60(13) . . ?
C10 C11 C12 123.71(19) . . ?
C10 C11 C8 114.40(19) . . ?
C12 C11 C8 121.88(18) . . ?
O2 C12 C11 121.09(19) . . ?
O2 C12 C13 119.9(2) . . ?
C11 C12 C13 118.96(19) . . ?
C18 C13 C14 118.3(2) . . ?
C18 C13 C12 123.7(2) . . ?
C14 C13 C12 118.0(2) . . ?
C15 C14 C13 120.5(2) . . ?
C14 C15 C16 120.4(2) . . ?
C17 C16 C15 120.4(2) . . ?
C16 C17 C18 120.2(2) . . ?
C17 C18 C13 120.3(2) . . ?
C17 C18 S2 115.44(18) . . ?
C13 C18 S2 124.29(16) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        28.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.044
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: EtOH'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_exp_2302
_database_code_depnum_ccdc_archive 'CCDC 1454213'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        5a
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H9 N O2 S2'
_chemical_formula_weight         323.37

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.3128(3)
_cell_length_b                   18.0467(9)
_cell_length_c                   12.6157(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.132(4)
_cell_angle_gamma                90.00
_cell_volume                     1429.03(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3698
_cell_measurement_theta_min      0.900
_cell_measurement_theta_max      0.936

_exptl_crystal_description       blocks
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6216
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         28.70
_reflns_number_total             3698
_reflns_number_gt                2306
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0203P)²+0.8107P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0026(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3698
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0869
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 1.0007(4) 0.34637(13) 0.27378(19) 0.0493(6) Uani 1 1 d . . .
O1 O 0.2589(3) 0.44990(12) 0.08165(16) 0.0616(6) Uani 1 1 d . . .
O2 O 1.1510(3) 0.35707(14) 0.34491(18) 0.0686(7) Uani 1 1 d . . .
S1 S 0.48115(11) 0.56508(4) 0.38575(5) 0.0453(2) Uani 1 1 d . . .
S2 S 0.83396(10) 0.45906(4) 0.38175(5) 0.0413(2) Uani 1 1 d . . .
C1 C 0.2472(4) 0.57999(14) 0.30044(19) 0.0350(6) Uani 1 1 d . . .
C2 C 0.1192(4) 0.63828(15) 0.3304(2) 0.0469(7) Uani 1 1 d . . .
H2 H 0.1623 0.6665 0.3905 0.056 Uiso 1 1 calc R . .
C3 C -0.0704(5) 0.65347(16) 0.2702(3) 0.0531(8) Uani 1 1 d . . .
H3 H -0.1548 0.6923 0.2898 0.064 Uiso 1 1 calc R . .
C4 C -0.1376(4) 0.61149(16) 0.1805(2) 0.0477(7) Uani 1 1 d . . .
H4 H -0.2678 0.6212 0.1413 0.057 Uiso 1 1 calc R . .
C5 C -0.0094(4) 0.55541(15) 0.1503(2) 0.0390(6) Uani 1 1 d . . .
H5 H -0.0535 0.5279 0.0897 0.047 Uiso 1 1 calc R . .
C6 C 0.1856(4) 0.53884(13) 0.20874(19) 0.0325(5) Uani 1 1 d . . .
C7 C 0.3149(4) 0.47860(14) 0.1676(2) 0.0350(6) Uani 1 1 d . . .
C8 C 0.5125(4) 0.45508(13) 0.23221(18) 0.0300(5) Uani 1 1 d . . .
C9 C 0.5913(4) 0.49145(14) 0.32538(19) 0.0340(6) Uani 1 1 d . . .
C10 C 0.8338(4) 0.39513(14) 0.27835(19) 0.0354(6) Uani 1 1 d . . .
C11 C 0.6541(4) 0.39807(13) 0.20528(19) 0.0311(5) Uani 1 1 d . . .
C12 C 0.6198(4) 0.34624(13) 0.11376(19) 0.0326(6) Uani 1 1 d . . .
C13 C 0.4364(4) 0.30244(14) 0.1006(2) 0.0375(6) Uani 1 1 d . . .
H13 H 0.3351 0.3067 0.1486 0.045 Uiso 1 1 calc R . .
C14 C 0.4043(4) 0.25299(15) 0.0173(2) 0.0430(7) Uani 1 1 d . . .
H14 H 0.2827 0.2236 0.0100 0.052 Uiso 1 1 calc R . .
C15 C 0.5526(4) 0.24685(15) -0.0558(2) 0.0455(7) Uani 1 1 d . . .
H15 H 0.5296 0.2140 -0.1126 0.055 Uiso 1 1 calc R . .
C16 C 0.7341(4) 0.28969(16) -0.0438(2) 0.0474(7) Uani 1 1 d . . .
H16 H 0.8336 0.2857 -0.0929 0.057 Uiso 1 1 calc R . .
C17 C 0.7697(4) 0.33876(15) 0.0411(2) 0.0404(6) Uani 1 1 d . . .
H17 H 0.8941 0.3667 0.0494 0.048 Uiso 1 1 calc R . .


_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
N1 O2 1.249(3) . ?
N1 C10 1.379(3) . ?
O1 C7 1.219(3) . ?
S1 C9 1.715(3) . ?
S1 C1 1.753(3) . ?
S2 C9 1.721(2) . ?
S2 C10 1.741(3) . ?
C1 C6 1.395(3) . ?
C1 C2 1.403(3) . ?
C2 C3 1.375(4) . ?
C3 C4 1.390(4) . ?
C4 C5 1.374(4) . ?
C5 C6 1.398(3) . ?
C6 C7 1.486(3) . ?
C7 C8 1.478(3) . ?
C8 C9 1.391(3) . ?
C8 C11 1.428(3) . ?
C10 C11 1.384(3) . ?
C11 C12 1.484(3) . ?
C12 C13 1.397(3) . ?
C12 C17 1.393(3) . ?
C13 C14 1.378(3) . ?
C14 C15 1.387(3) . ?
C15 C16 1.377(4) . ?
C16 C17 1.389(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
O2 N1 C10 113.4(2) . . ?
C9 S1 C1 101.60(12) . . ?
C9 S2 C10 89.22(12) . . ?
C6 C1 C2 120.3(2) . . ?
C6 C1 S1 124.72(19) . . ?
C2 C1 S1 114.9(2) . . ?
C3 C2 C1 119.6(3) . . ?
C2 C3 C4 120.8(3) . . ?
C5 C4 C3 119.3(3) . . ?
C4 C5 C6 121.5(3) . . ?
C1 C6 C5 118.4(2) . . ?
C1 C6 C7 124.4(2) . . ?
C5 C6 C7 117.3(2) . . ?
O1 C7 C8 121.1(2) . . ?
O1 C7 C6 120.2(2) . . ?
C8 C7 C6 118.7(2) . . ?
C9 C8 C11 111.4(2) . . ?
C9 C8 C7 122.4(2) . . ?
C11 C8 C7 126.1(2) . . ?
C8 C9 S1 128.00(19) . . ?
C8 C9 S2 114.26(19) . . ?
S1 C9 S2 117.69(14) . . ?
N1 C10 C11 124.9(2) . . ?
N1 C10 S2 120.99(19) . . ?
C11 C10 S2 114.10(18) . . ?
C10 C11 C8 111.0(2) . . ?
C10 C11 C12 122.4(2) . . ?
C8 C11 C12 126.6(2) . . ?
C13 C12 C17 118.7(2) . . ?
C13 C12 C11 120.0(2) . . ?
C17 C12 C11 121.3(2) . . ?
C14 C13 C12 120.6(2) . . ?
C13 C14 C15 120.3(2) . . ?
C16 C15 C14 119.7(3) . . ?
C15 C16 C17 120.4(2) . . ?
C16 C17 C12 120.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.055
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_karuna1
_database_code_depnum_ccdc_archive 'CCDC 1454212'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        4f
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H10 Br N O S2'
_chemical_formula_weight         388.28

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.1202(5)
_cell_length_b                   12.7017(3)
_cell_length_c                   14.3420(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.1330(10)
_cell_angle_gamma                90.00
_cell_volume                     3035.51(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7634
_cell_measurement_theta_min      0.419
_cell_measurement_theta_max      0.579

_exptl_crystal_description       blocks
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552.0
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40271
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         28.42
_reflns_number_total             7634
_reflns_number_gt                3719
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0591P)²+5.2880P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7634
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1386
_refine_ls_wR_factor_gt          0.1141
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5373(2) 0.4911(3) 0.7223(3) 0.0573(12) Uani 1 1 d . . .
H1A H 0.4880 0.4760 0.6860 0.069 Uiso 1 1 calc R . .
H1B H 0.5518 0.5557 0.7354 0.069 Uiso 1 1 calc R . .
N2 N 0.0442(2) 0.2011(3) 0.2017(3) 0.0586(12) Uani 1 1 d . . .
H2A H -0.0055 0.2171 0.1690 0.070 Uiso 1 1 calc R . .
H2B H 0.0597 0.1369 0.2034 0.070 Uiso 1 1 calc R . .
O1 O 0.61005(19) 0.0748(2) 0.7600(3) 0.0571(9) Uani 1 1 d . . .
O2 O 0.1091(2) 0.6120(3) 0.3035(3) 0.0632(10) Uani 1 1 d . . .
S1 S 0.82212(7) 0.28720(10) 0.90092(10) 0.0495(3) Uani 1 1 d . . .
S2 S 0.69348(7) 0.44683(9) 0.82389(9) 0.0455(3) Uani 1 1 d . . .
S3 S 0.32610(7) 0.40314(10) 0.41091(11) 0.0578(4) Uani 1 1 d . . .
S4 S 0.20038(7) 0.24474(9) 0.30718(11) 0.0524(3) Uani 1 1 d . . .
Br1 Br 0.38985(3) 0.07119(4) 0.43641(4) 0.0629(2) Uani 1 1 d . . .
Br2 Br -0.11585(4) 0.63643(6) -0.02393(5) 0.0847(3) Uani 1 1 d . . .
C18 C 0.3201(3) 0.5382(4) 0.4293(4) 0.0484(12) Uani 1 1 d . . .
C19 C 0.3936(3) 0.5857(5) 0.4885(4) 0.0584(14) Uani 1 1 d . . .
H19 H 0.4403 0.5457 0.5145 0.070 Uiso 1 1 calc R . .
C20 C 0.3959(4) 0.6917(5) 0.5077(4) 0.0675(16) Uani 1 1 d . . .
H20 H 0.4441 0.7230 0.5491 0.081 Uiso 1 1 calc R . .
C21 C 0.3271(3) 0.7525(4) 0.4660(4) 0.0594(14) Uani 1 1 d . . .
H21 H 0.3296 0.8250 0.4758 0.071 Uiso 1 1 calc R . .
C22 C 0.2557(3) 0.7053(4) 0.4104(4) 0.0560(13) Uani 1 1 d . . .
H22 H 0.2095 0.7462 0.3851 0.067 Uiso 1 1 calc R . .
C23 C 0.2498(3) 0.5970(4) 0.3902(3) 0.0445(11) Uani 1 1 d . . .
C25 C 0.1614(3) 0.4407(3) 0.3099(3) 0.0406(11) Uani 1 1 d . . .
C26 C 0.2266(3) 0.3752(4) 0.3409(4) 0.0448(11) Uani 1 1 d . . .
C27 C 0.0869(3) 0.3842(4) 0.2580(3) 0.0420(11) Uani 1 1 d . . .
C24 C 0.1686(3) 0.5537(4) 0.3313(4) 0.0478(12) Uani 1 1 d . . .
C29 C 0.0046(3) 0.4294(4) 0.2096(3) 0.0416(11) Uani 1 1 d . . .
C30 C -0.0145(3) 0.5024(4) 0.1300(3) 0.0465(12) Uani 1 1 d . . .
H30 H 0.0250 0.5266 0.1090 0.056 Uiso 1 1 calc R . .
C31 C -0.0921(3) 0.5375(4) 0.0836(4) 0.0495(12) Uani 1 1 d . . .
C32 C -0.1519(3) 0.5054(4) 0.1125(4) 0.0498(12) Uani 1 1 d . . .
H32 H -0.2042 0.5298 0.0791 0.060 Uiso 1 1 calc R . .
C33 C -0.1331(3) 0.4363(4) 0.1918(4) 0.0513(13) Uani 1 1 d . . .
H33 H -0.1728 0.4148 0.2136 0.062 Uiso 1 1 calc R . .
C28 C 0.0990(3) 0.2785(4) 0.2514(4) 0.0459(12) Uani 1 1 d . . .
C1 C 0.8181(3) 0.1500(3) 0.9076(3) 0.0411(11) Uani 1 1 d . . .
C2 C 0.8906(3) 0.0998(4) 0.9652(4) 0.0523(13) Uani 1 1 d . . .
H2 H 0.9371 0.1393 0.9957 0.063 Uiso 1 1 calc R . .
C3 C 0.8928(3) -0.0070(4) 0.9767(4) 0.0610(15) Uani 1 1 d . . .
H3 H 0.9409 -0.0399 1.0158 0.073 Uiso 1 1 calc R . .
C4 C 0.8242(3) -0.0666(4) 0.9306(5) 0.0669(16) Uani 1 1 d . . .
H4 H 0.8261 -0.1393 0.9388 0.080 Uiso 1 1 calc R . .
C7 C 0.6680(3) 0.1351(3) 0.7993(3) 0.0389(10) Uani 1 1 d . . .
C10 C 0.5825(2) 0.3049(3) 0.7471(3) 0.0387(10) Uani 1 1 d . . .
C8 C 0.6584(2) 0.2492(3) 0.7918(3) 0.0359(10) Uani 1 1 d . . .
C9 C 0.7220(3) 0.3162(3) 0.8344(3) 0.0387(10) Uani 1 1 d . . .
C11 C 0.5927(3) 0.4122(4) 0.7590(3) 0.0422(11) Uani 1 1 d . . .
C12 C 0.5022(2) 0.2585(3) 0.6914(3) 0.0382(10) Uani 1 1 d . . .
C13 C 0.4856(3) 0.1957(3) 0.6060(3) 0.0399(10) Uani 1 1 d . . .
H13 H 0.5264 0.1799 0.5843 0.048 Uiso 1 1 calc R . .
C14 C 0.4094(3) 0.1567(3) 0.5531(4) 0.0447(12) Uani 1 1 d . . .
C15 C 0.3470(3) 0.1776(4) 0.5823(4) 0.0478(12) Uani 1 1 d . . .
H15 H 0.2958 0.1513 0.5456 0.057 Uiso 1 1 calc R . .
C16 C 0.3627(3) 0.2392(4) 0.6679(4) 0.0510(13) Uani 1 1 d . . .
H16 H 0.3216 0.2542 0.6893 0.061 Uiso 1 1 calc R . .
C17 C 0.4393(3) 0.2788(4) 0.7223(4) 0.0468(12) Uani 1 1 d . . .
H17 H 0.4489 0.3192 0.7799 0.056 Uiso 1 1 calc R . .
C34 C -0.0555(3) 0.3978(4) 0.2401(4) 0.0502(12) Uani 1 1 d . . .
H34 H -0.0439 0.3504 0.2934 0.060 Uiso 1 1 calc R . .
C6 C 0.7480(2) 0.0908(3) 0.8595(3) 0.0372(10) Uani 1 1 d . . .
C5 C 0.7537(3) -0.0184(4) 0.8730(4) 0.0536(13) Uani 1 1 d . . .
H5 H 0.7081 -0.0593 0.8418 0.064 Uiso 1 1 calc R . .


_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
N1 C11 1.369(6) . ?
N2 C28 1.379(6) . ?
O1 C7 1.242(5) . ?
O2 C24 1.237(6) . ?
S1 C9 1.725(4) . ?
S1 C1 1.748(5) . ?
S2 C9 1.727(4) . ?
S2 C11 1.749(4) . ?
S3 C26 1.721(5) . ?
S3 C18 1.746(5) . ?
S4 C26 1.739(5) . ?
S4 C28 1.745(5) . ?
Br1 C14 1.908(5) . ?
Br2 C31 1.903(5) . ?
C18 C23 1.391(7) . ?
C18 C19 1.404(7) . ?
C19 C20 1.372(8) . ?
C20 C21 1.388(8) . ?
C21 C22 1.363(7) . ?
C22 C23 1.401(7) . ?
C23 C24 1.485(7) . ?
C25 C26 1.369(6) . ?
C25 C27 1.450(6) . ?
C25 C24 1.463(6) . ?
C27 C28 1.370(6) . ?
C27 C29 1.490(6) . ?
C29 C34 1.383(7) . ?
C29 C30 1.404(6) . ?
C30 C31 1.373(6) . ?
C31 C32 1.366(7) . ?
C32 C33 1.370(7) . ?
C33 C34 1.390(7) . ?
C1 C2 1.400(6) . ?
C1 C6 1.402(6) . ?
C2 C3 1.365(7) . ?
C3 C4 1.383(8) . ?
C4 C5 1.363(7) . ?
C7 C8 1.458(6) . ?
C7 C6 1.477(6) . ?
C10 C11 1.377(6) . ?
C10 C8 1.452(6) . ?
C10 C12 1.480(6) . ?
C8 C9 1.370(6) . ?
C12 C13 1.392(6) . ?
C12 C17 1.398(6) . ?
C13 C14 1.380(6) . ?
C14 C15 1.376(7) . ?
C15 C16 1.388(7) . ?
C16 C17 1.392(6) . ?
C6 C5 1.398(6) . ?

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 S1 C1 100.7(2) . . ?
C9 S2 C11 91.1(2) . . ?
C26 S3 C18 100.2(2) . . ?
C26 S4 C28 91.0(2) . . ?
C23 C18 C19 121.0(5) . . ?
C23 C18 S3 124.6(4) . . ?
C19 C18 S3 114.4(4) . . ?
C20 C19 C18 119.3(5) . . ?
C19 C20 C21 120.6(5) . . ?
C22 C21 C20 119.5(5) . . ?
C21 C22 C23 122.1(5) . . ?
C18 C23 C22 117.4(5) . . ?
C18 C23 C24 125.2(4) . . ?
C22 C23 C24 117.4(4) . . ?
C26 C25 C27 112.2(4) . . ?
C26 C25 C24 122.2(4) . . ?
C27 C25 C24 125.6(4) . . ?
C25 C26 S3 129.6(4) . . ?
C25 C26 S4 112.4(3) . . ?
S3 C26 S4 117.9(3) . . ?
C28 C27 C25 112.2(4) . . ?
C28 C27 C29 120.2(4) . . ?
C25 C27 C29 127.4(4) . . ?
O2 C24 C25 121.7(4) . . ?
O2 C24 C23 120.3(4) . . ?
C25 C24 C23 118.0(4) . . ?
C34 C29 C30 118.4(4) . . ?
C34 C29 C27 120.6(4) . . ?
C30 C29 C27 121.0(4) . . ?
C31 C30 C29 119.2(5) . . ?
C32 C31 C30 122.7(5) . . ?
C32 C31 Br2 119.3(4) . . ?
C30 C31 Br2 118.0(4) . . ?
C31 C32 C33 118.4(4) . . ?
C32 C33 C34 120.8(5) . . ?
C27 C28 N2 129.2(4) . . ?
C27 C28 S4 112.1(3) . . ?
N2 C28 S4 118.5(4) . . ?
C2 C1 C6 120.3(4) . . ?
C2 C1 S1 115.9(4) . . ?
C6 C1 S1 123.9(3) . . ?
C3 C2 C1 120.0(5) . . ?
C2 C3 C4 120.5(5) . . ?
C5 C4 C3 119.7(5) . . ?
O1 C7 C8 121.6(4) . . ?
O1 C7 C6 119.5(4) . . ?
C8 C7 C6 118.9(4) . . ?
C11 C10 C8 111.7(4) . . ?
C11 C10 C12 121.1(4) . . ?
C8 C10 C12 127.1(4) . . ?
C9 C8 C10 112.3(4) . . ?
C9 C8 C7 122.0(4) . . ?
C10 C8 C7 125.6(4) . . ?
C8 C9 S1 129.2(3) . . ?
C8 C9 S2 112.8(3) . . ?
S1 C9 S2 117.9(2) . . ?
N1 C11 C10 129.4(4) . . ?
N1 C11 S2 118.4(3) . . ?
C10 C11 S2 112.1(3) . . ?
C13 C12 C17 117.6(4) . . ?
C13 C12 C10 121.9(4) . . ?
C17 C12 C10 120.5(4) . . ?
C14 C13 C12 120.8(4) . . ?
C15 C14 C13 121.8(5) . . ?
C15 C14 Br1 119.0(3) . . ?
C13 C14 Br1 119.2(4) . . ?
C14 C15 C16 118.1(4) . . ?
C15 C16 C17 120.8(5) . . ?
C16 C17 C12 120.9(5) . . ?
C29 C34 C33 120.6(5) . . ?
C5 C6 C1 117.4(4) . . ?
C5 C6 C7 117.5(4) . . ?
C1 C6 C7 125.0(4) . . ?
C4 C5 C6 122.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.42
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.081
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: EtOH'
_chemical_properties_physical    Moisture-sensitive
