# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_ljh003
_database_code_depnum_ccdc_archive 'CCDC 1063383'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H25 N O2 S'
_chemical_formula_sum            'C31 H25 N O2 S'
_chemical_formula_weight         475.58

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   P2(1)/c
_symmetry_space_group_name_Hall  -P2ybc

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                   13.100(2)
_cell_length_b                   16.350(3)
_cell_length_c                   13.048(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.404(2)
_cell_angle_gamma                90.00
_cell_volume                     2481.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4206
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      27.36

_exptl_crystal_description       LUMP
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      1.273
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_process_details   'SHELXS-97 (Sheldrick, 2008)'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13901
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5355
_reflns_number_gt                3589
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0342P)²+1.3963P] 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       0.0092(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5355
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1190
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_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
S1 S 1.03802(6) 0.24960(4) 1.19197(5) 0.0512(2) Uani 1 1 d . . .
O1 O 1.15775(16) 0.23688(13) 1.26578(15) 0.0751(6) Uani 1 1 d . . .
C1 C 0.9612(2) 0.16474(15) 1.20070(19) 0.0491(6) Uani 1 1 d . . .
N1 N 1.02253(16) 0.25012(12) 1.05705(15) 0.0441(5) Uani 1 1 d . . .
O2 O 0.98316(17) 0.32167(10) 1.20430(14) 0.0598(5) Uani 1 1 d . . .
C2 C 1.0168(3) 0.09050(17) 1.2427(2) 0.0629(8) Uani 1 1 d . . .
H2 H 1.0966 0.0874 1.2767 0.075 Uiso 1 1 calc R . .
C3 C 0.9530(3) 0.02230(18) 1.2335(2) 0.0700(9) Uani 1 1 d . . .
H3 H 0.9904 -0.0272 1.2622 0.084 Uiso 1 1 calc R . .
C4 C 0.8344(3) 0.02494(17) 1.1827(2) 0.0650(8) Uani 1 1 d . . .
C5 C 0.7801(3) 0.10051(17) 1.1455(2) 0.0611(7) Uani 1 1 d . . .
H5 H 0.7005 0.1039 1.1142 0.073 Uiso 1 1 calc R . .
C6 C 0.8429(2) 0.17024(15) 1.1545(2) 0.0514(6) Uani 1 1 d . . .
H6 H 0.8062 0.2204 1.1297 0.062 Uiso 1 1 calc R . .
C7 C 0.7630(4) -0.05119(19) 1.1650(3) 0.0973(12) Uani 1 1 d . . .
H7A H 0.6830 -0.0369 1.1287 0.146 Uiso 1 1 calc R . .
H7B H 0.7831 -0.0763 1.2384 0.146 Uiso 1 1 calc R . .
H7C H 0.7775 -0.0888 1.1168 0.146 Uiso 1 1 calc R . .
C8 C 1.0669(2) 0.17400(15) 1.0260(2) 0.0526(6) Uani 1 1 d . . .
H8A H 1.1204 0.1455 1.0952 0.063 Uiso 1 1 calc R . .
H8B H 1.1061 0.1878 0.9808 0.063 Uiso 1 1 calc R . .
C9 C 0.96149(19) 0.12053(15) 0.95548(19) 0.0462(6) Uani 1 1 d . . .
H9A H 0.9677 0.0934 0.8924 0.055 Uiso 1 1 calc R . .
H9B H 0.9504 0.0798 1.0035 0.055 Uiso 1 1 calc R . .
C10 C 0.86633(19) 0.18277(13) 0.91171(17) 0.0380(5) Uani 1 1 d . . .
C11 C 0.75086(19) 0.17236(13) 0.82719(17) 0.0383(5) Uani 1 1 d . . .
C12 C 0.67739(19) 0.23855(14) 0.79969(17) 0.0389(5) Uani 1 1 d . . .
C13 C 0.71842(19) 0.31653(14) 0.85243(17) 0.0397(5) Uani 1 1 d . . .
C14 C 0.6455(2) 0.38621(15) 0.8229(2) 0.0496(6) Uani 1 1 d . . .
H14 H 0.5682 0.3807 0.7705 0.059 Uiso 1 1 calc R . .
C15 C 0.6865(2) 0.46052(16) 0.8696(2) 0.0579(7) Uani 1 1 d . . .
H15 H 0.6368 0.5050 0.8498 0.069 Uiso 1 1 calc R . .
C16 C 0.8030(3) 0.47112(16) 0.9473(2) 0.0580(7) Uani 1 1 d . . .
H16 H 0.8307 0.5229 0.9764 0.070 Uiso 1 1 calc R . .
C17 C 0.8756(2) 0.40610(14) 0.9803(2) 0.0491(6) Uani 1 1 d . . .
H17 H 0.9527 0.4136 1.0325 0.059 Uiso 1 1 calc R . .
C18 C 0.83535(19) 0.32676(13) 0.93617(17) 0.0392(5) Uani 1 1 d . . .
C19 C 0.90429(18) 0.25593(13) 0.96709(17) 0.0373(5) Uani 1 1 d . . .
C20 C 0.5528(2) 0.22913(14) 0.71464(19) 0.0432(5) Uani 1 1 d . . .
C21 C 0.4737(2) 0.20534(18) 0.7502(2) 0.0633(7) Uani 1 1 d . . .
H21 H 0.4977 0.1947 0.8279 0.076 Uiso 1 1 calc R . .
C22 C 0.3581(2) 0.1969(2) 0.6715(3) 0.0776(9) Uani 1 1 d . . .
H22 H 0.3054 0.1812 0.6970 0.093 Uiso 1 1 calc R . .
C23 C 0.3218(2) 0.21143(18) 0.5570(3) 0.0706(9) Uani 1 1 d . . .
H23 H 0.2448 0.2044 0.5042 0.085 Uiso 1 1 calc R . .
C24 C 0.3987(3) 0.2363(2) 0.5203(2) 0.0732(9) Uani 1 1 d . . .
H24 H 0.3740 0.2476 0.4426 0.088 Uiso 1 1 calc R . .
C25 C 0.5134(2) 0.24476(18) 0.5984(2) 0.0625(7) Uani 1 1 d . . .
H25 H 0.5652 0.2613 0.5723 0.075 Uiso 1 1 calc R . .
C26 C 0.71156(19) 0.08874(14) 0.77812(19) 0.0414(5) Uani 1 1 d . . .
C27 C 0.6978(2) 0.02923(16) 0.8454(2) 0.0566(7) Uani 1 1 d . . .
H27 H 0.7126 0.0421 0.9204 0.068 Uiso 1 1 calc R . .
C28 C 0.6626(2) -0.04893(17) 0.8047(3) 0.0640(8) Uani 1 1 d . . .
H28 H 0.6541 -0.0880 0.8520 0.077 Uiso 1 1 calc R . .
C29 C 0.6404(3) -0.06873(18) 0.6955(3) 0.0686(8) Uani 1 1 d . . .
H29 H 0.6161 -0.1212 0.6674 0.082 Uiso 1 1 calc R . .
C30 C 0.6540(3) -0.0111(2) 0.6271(3) 0.0796(10) Uani 1 1 d . . .
H30 H 0.6390 -0.0247 0.5523 0.095 Uiso 1 1 calc R . .
C31 C 0.6898(3) 0.06740(17) 0.6679(2) 0.0655(8) Uani 1 1 d . . .
H31 H 0.6993 0.1059 0.6205 0.079 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
S1 O2 1.4274(18) . ?
S1 O1 1.4284(19) . ?
S1 N1 1.6768(19) . ?
S1 C1 1.748(3) . ?
C1 C6 1.383(3) . ?
C1 C2 1.392(3) . ?
N1 C19 1.453(3) . ?
N1 C8 1.506(3) . ?
C2 C3 1.365(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(4) . ?
C4 C7 1.509(4) . ?
C5 C6 1.379(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.533(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.503(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C19 1.367(3) . ?
C10 C11 1.413(3) . ?
C11 C12 1.381(3) . ?
C11 C26 1.497(3) . ?
C12 C13 1.431(3) . ?
C12 C20 1.501(3) . ?
C13 C14 1.421(3) . ?
C13 C18 1.424(3) . ?
C14 C15 1.355(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.401(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.358(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.419(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.409(3) . ?
C20 C21 1.372(3) . ?
C20 C25 1.383(3) . ?
C21 C22 1.391(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.364(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.362(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.380(4) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C31 1.376(3) . ?
C26 C27 1.377(3) . ?
C27 C28 1.379(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.356(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.364(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.387(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?

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 S1 O1 119.85(12) . . ?
O2 S1 N1 106.88(10) . . ?
O1 S1 N1 105.86(11) . . ?
O2 S1 C1 108.24(12) . . ?
O1 S1 C1 109.08(13) . . ?
N1 S1 C1 106.10(10) . . ?
C6 C1 C2 120.5(3) . . ?
C6 C1 S1 118.88(19) . . ?
C2 C1 S1 120.3(2) . . ?
C19 N1 C8 103.70(17) . . ?
C19 N1 S1 114.66(15) . . ?
C8 N1 S1 113.77(15) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 121.6(3) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 C7 121.9(3) . . ?
C5 C4 C7 119.8(3) . . ?
C6 C5 C4 120.9(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C1 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C1 C6 H6 120.4 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C9 106.25(18) . . ?
N1 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
N1 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
C10 C9 C8 101.69(19) . . ?
C10 C9 H9A 111.4 . . ?
C8 C9 H9A 111.4 . . ?
C10 C9 H9B 111.4 . . ?
C8 C9 H9B 111.4 . . ?
H9A C9 H9B 109.3 . . ?
C19 C10 C11 121.1(2) . . ?
C19 C10 C9 110.80(19) . . ?
C11 C10 C9 128.1(2) . . ?
C12 C11 C10 118.4(2) . . ?
C12 C11 C26 122.9(2) . . ?
C10 C11 C26 118.53(19) . . ?
C11 C12 C13 120.7(2) . . ?
C11 C12 C20 120.2(2) . . ?
C13 C12 C20 119.14(19) . . ?
C14 C13 C18 117.7(2) . . ?
C14 C13 C12 121.8(2) . . ?
C18 C13 C12 120.5(2) . . ?
C15 C14 C13 121.3(2) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 120.7(2) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 120.2(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.8(2) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C19 C18 C17 124.5(2) . . ?
C19 C18 C13 116.40(19) . . ?
C17 C18 C13 119.1(2) . . ?
C10 C19 C18 122.6(2) . . ?
C10 C19 N1 111.27(19) . . ?
C18 C19 N1 126.12(19) . . ?
C21 C20 C25 117.7(2) . . ?
C21 C20 C12 120.9(2) . . ?
C25 C20 C12 121.5(2) . . ?
C20 C21 C22 120.9(3) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 119.7(3) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.0(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 121.4(3) . . ?
C24 C25 H25 119.3 . . ?
C20 C25 H25 119.3 . . ?
C31 C26 C27 117.5(2) . . ?
C31 C26 C11 122.9(2) . . ?
C27 C26 C11 119.5(2) . . ?
C26 C27 C28 121.8(2) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C29 C28 C27 119.9(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 119.6(3) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C29 C30 C31 120.8(3) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C26 C31 C30 120.4(3) . . ?
C26 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?

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
O2 S1 C1 C6 35.5(2) . . . . ?
O1 S1 C1 C6 167.49(19) . . . . ?
N1 S1 C1 C6 -78.9(2) . . . . ?
O2 S1 C1 C2 -151.01(19) . . . . ?
O1 S1 C1 C2 -19.1(2) . . . . ?
N1 S1 C1 C2 94.6(2) . . . . ?
O2 S1 N1 C19 -55.81(18) . . . . ?
O1 S1 N1 C19 175.37(16) . . . . ?
C1 S1 N1 C19 59.54(18) . . . . ?
O2 S1 N1 C8 -174.95(15) . . . . ?
O1 S1 N1 C8 56.23(18) . . . . ?
C1 S1 N1 C8 -59.60(18) . . . . ?
C6 C1 C2 C3 2.6(4) . . . . ?
S1 C1 C2 C3 -170.7(2) . . . . ?
C1 C2 C3 C4 0.5(4) . . . . ?
C2 C3 C4 C5 -3.2(4) . . . . ?
C2 C3 C4 C7 175.8(3) . . . . ?
C3 C4 C5 C6 2.8(4) . . . . ?
C7 C4 C5 C6 -176.2(2) . . . . ?
C4 C5 C6 C1 0.2(4) . . . . ?
C2 C1 C6 C5 -3.0(4) . . . . ?
S1 C1 C6 C5 170.46(18) . . . . ?
C19 N1 C8 C9 -25.1(2) . . . . ?
S1 N1 C8 C9 100.15(19) . . . . ?
N1 C8 C9 C10 22.4(2) . . . . ?
C8 C9 C10 C19 -11.7(2) . . . . ?
C8 C9 C10 C11 169.4(2) . . . . ?
C19 C10 C11 C12 1.4(3) . . . . ?
C9 C10 C11 C12 -179.8(2) . . . . ?
C19 C10 C11 C26 -174.0(2) . . . . ?
C9 C10 C11 C26 4.7(3) . . . . ?
C10 C11 C12 C13 2.3(3) . . . . ?
C26 C11 C12 C13 177.6(2) . . . . ?
C10 C11 C12 C20 -177.04(19) . . . . ?
C26 C11 C12 C20 -1.8(3) . . . . ?
C11 C12 C13 C14 177.9(2) . . . . ?
C20 C12 C13 C14 -2.7(3) . . . . ?
C11 C12 C13 C18 -1.4(3) . . . . ?
C20 C12 C13 C18 177.99(19) . . . . ?
C18 C13 C14 C15 2.3(3) . . . . ?
C12 C13 C14 C15 -177.0(2) . . . . ?
C13 C14 C15 C16 1.1(4) . . . . ?
C14 C15 C16 C17 -2.6(4) . . . . ?
C15 C16 C17 C18 0.6(4) . . . . ?
C16 C17 C18 C19 -179.0(2) . . . . ?
C16 C17 C18 C13 2.8(3) . . . . ?
C14 C13 C18 C19 177.50(19) . . . . ?
C12 C13 C18 C19 -3.2(3) . . . . ?
C14 C13 C18 C17 -4.2(3) . . . . ?
C12 C13 C18 C17 175.2(2) . . . . ?
C11 C10 C19 C18 -6.4(3) . . . . ?
C9 C10 C19 C18 174.66(19) . . . . ?
C11 C10 C19 N1 174.92(18) . . . . ?
C9 C10 C19 N1 -4.0(3) . . . . ?
C17 C18 C19 C10 -171.2(2) . . . . ?
C13 C18 C19 C10 7.1(3) . . . . ?
C17 C18 C19 N1 7.3(3) . . . . ?
C13 C18 C19 N1 -174.44(19) . . . . ?
C8 N1 C19 C10 18.3(2) . . . . ?
S1 N1 C19 C10 -106.31(19) . . . . ?
C8 N1 C19 C18 -160.3(2) . . . . ?
S1 N1 C19 C18 75.1(2) . . . . ?
C11 C12 C20 C21 88.2(3) . . . . ?
C13 C12 C20 C21 -91.2(3) . . . . ?
C11 C12 C20 C25 -92.4(3) . . . . ?
C13 C12 C20 C25 88.2(3) . . . . ?
C25 C20 C21 C22 0.4(4) . . . . ?
C12 C20 C21 C22 179.8(3) . . . . ?
C20 C21 C22 C23 0.6(5) . . . . ?
C21 C22 C23 C24 -1.6(5) . . . . ?
C22 C23 C24 C25 1.6(5) . . . . ?
C23 C24 C25 C20 -0.5(5) . . . . ?
C21 C20 C25 C24 -0.4(4) . . . . ?
C12 C20 C25 C24 -179.8(2) . . . . ?
C12 C11 C26 C31 77.5(3) . . . . ?
C10 C11 C26 C31 -107.2(3) . . . . ?
C12 C11 C26 C27 -103.6(3) . . . . ?
C10 C11 C26 C27 71.7(3) . . . . ?
C31 C26 C27 C28 -0.6(4) . . . . ?
C11 C26 C27 C28 -179.5(2) . . . . ?
C26 C27 C28 C29 -0.1(4) . . . . ?
C27 C28 C29 C30 0.5(5) . . . . ?
C28 C29 C30 C31 -0.2(5) . . . . ?
C27 C26 C31 C30 0.9(4) . . . . ?
C11 C26 C31 C30 179.8(3) . . . . ?
C29 C30 C31 C26 -0.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.040
####################################################################### 
# 
# 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_pr1150122
_database_code_depnum_ccdc_archive 'CCDC 1063384'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H23 N O2 S'
_chemical_formula_sum            'C26 H23 N O2 S'
_chemical_formula_weight         413.51

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           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   9.311(2)
_cell_length_b                   10.003(2)
_cell_length_c                   23.556(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2193.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8845
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      26.29

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   sadabs

_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            19007
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         27.54
_reflns_number_total             4998
_reflns_number_gt                3730
_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)+(0.1253P)²+0.4411P] 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       0.082(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(13)
_refine_ls_number_reflns         4998
_refine_ls_number_parameters     274
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0723
_refine_ls_wR_factor_ref         0.2045
_refine_ls_wR_factor_gt          0.1876
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.084
_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
C1 C 0.7579(4) 1.0724(3) 0.05274(15) 0.0589(9) Uani 1 1 d . . .
H1 H 0.8018 1.0132 0.0777 0.071 Uiso 1 1 calc R . .
C2 C 0.7250(4) 1.0334(4) -0.00110(17) 0.0658(10) Uani 1 1 d . . .
H2 H 0.7482 0.9472 -0.0127 0.079 Uiso 1 1 calc R . .
C3 C 0.6582(4) 1.1185(4) -0.03897(17) 0.0664(10) Uani 1 1 d . . .
C4 C 0.6216(6) 1.0733(6) -0.0978(2) 0.0954(16) Uani 1 1 d . . .
H4A H 0.5195 1.0775 -0.1031 0.143 Uiso 1 1 calc R . .
H4B H 0.6538 0.9830 -0.1031 0.143 Uiso 1 1 calc R . .
H4C H 0.6680 1.1305 -0.1249 0.143 Uiso 1 1 calc R . .
C5 C 0.6274(5) 1.2470(5) -0.02074(18) 0.0772(12) Uani 1 1 d . . .
H5 H 0.5839 1.3067 -0.0457 0.093 Uiso 1 1 calc R . .
C6 C 0.6596(5) 1.2880(4) 0.03313(18) 0.0689(10) Uani 1 1 d . . .
H6 H 0.6371 1.3743 0.0448 0.083 Uiso 1 1 calc R . .
C7 C 0.7251(3) 1.2010(3) 0.06979(15) 0.0519(7) Uani 1 1 d . . .
C8 C 0.4856(4) 1.2490(4) 0.16691(17) 0.0640(9) Uani 1 1 d . . .
H8A H 0.4970 1.3300 0.1447 0.077 Uiso 1 1 calc R . .
H8B H 0.4353 1.2707 0.2018 0.077 Uiso 1 1 calc R . .
C9 C 0.4031(4) 1.1436(3) 0.13321(17) 0.0590(8) Uani 1 1 d . . .
H9A H 0.3030 1.1404 0.1446 0.071 Uiso 1 1 calc R . .
H9B H 0.4087 1.1606 0.0927 0.071 Uiso 1 1 calc R . .
C10 C 0.4798(3) 1.0175(3) 0.14881(13) 0.0474(7) Uani 1 1 d . . .
C11 C 0.6042(4) 1.0443(3) 0.17641(13) 0.0485(7) Uani 1 1 d . . .
C12 C 0.6922(3) 0.9428(4) 0.19957(14) 0.0505(7) Uani 1 1 d . . .
C13 C 0.8126(4) 0.9656(4) 0.23423(15) 0.0619(9) Uani 1 1 d . . .
H13 H 0.8385 1.0528 0.2432 0.074 Uiso 1 1 calc R . .
C14 C 0.8917(5) 0.8620(5) 0.25490(16) 0.0751(12) Uani 1 1 d . . .
H14 H 0.9701 0.8788 0.2783 0.090 Uiso 1 1 calc R . .
C15 C 0.8557(4) 0.7322(5) 0.24111(18) 0.0773(12) Uani 1 1 d . . .
H15 H 0.9127 0.6626 0.2544 0.093 Uiso 1 1 calc R . .
C16 C 0.7387(4) 0.7034(4) 0.20850(16) 0.0663(9) Uani 1 1 d . . .
H16 H 0.7166 0.6149 0.2000 0.080 Uiso 1 1 calc R . .
C17 C 0.6503(3) 0.8082(3) 0.18747(13) 0.0511(8) Uani 1 1 d . . .
C18 C 0.5214(3) 0.7813(3) 0.15636(14) 0.0504(8) Uani 1 1 d . . .
C19 C 0.4801(5) 0.6365(4) 0.1450(2) 0.0743(12) Uani 1 1 d . . .
H19A H 0.4562 0.5934 0.1801 0.111 Uiso 1 1 calc R . .
H19B H 0.5594 0.5908 0.1276 0.111 Uiso 1 1 calc R . .
H19C H 0.3987 0.6339 0.1200 0.111 Uiso 1 1 calc R . .
C20 C 0.4371(3) 0.8847(3) 0.13733(14) 0.0459(7) Uani 1 1 d . . .
C21 C 0.3015(5) 0.8639(5) 0.1055(2) 0.0794(7) Uani 1 1 d U . .
C22 C 0.3021(5) 0.8782(5) 0.0475(2) 0.0814(7) Uani 1 1 d U . .
H22 H 0.3864 0.9008 0.0286 0.098 Uiso 1 1 calc R . .
C23 C 0.1751(5) 0.8585(5) 0.0170(2) 0.0851(7) Uani 1 1 d U . .
H23 H 0.1739 0.8672 -0.0223 0.102 Uiso 1 1 calc R . .
C24 C 0.0520(5) 0.8260(5) 0.0461(3) 0.0876(7) Uani 1 1 d U . .
H24 H -0.0319 0.8093 0.0259 0.105 Uiso 1 1 calc R . .
C25 C 0.0500(5) 0.8180(5) 0.1015(2) 0.0876(7) Uani 1 1 d U . .
H25 H -0.0362 0.8015 0.1201 0.105 Uiso 1 1 calc R . .
C26 C 0.1742(5) 0.8338(5) 0.1326(2) 0.0842(7) Uani 1 1 d U . .
H26 H 0.1722 0.8241 0.1718 0.101 Uiso 1 1 calc R . .
N1 N 0.6298(3) 1.1875(3) 0.17976(13) 0.0568(7) Uani 1 1 d . . .
O1 O 0.7542(4) 1.3897(3) 0.14420(14) 0.0831(9) Uani 1 1 d . . .
O2 O 0.8905(3) 1.1797(3) 0.15671(12) 0.0722(7) Uani 1 1 d . . .
S1 S 0.76285(9) 1.24711(9) 0.14003(4) 0.0602(3) 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
C1 C2 1.362(5) . ?
C1 C7 1.382(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(6) . ?
C2 H2 0.9300 . ?
C3 C5 1.385(7) . ?
C3 C4 1.497(7) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.369(5) . ?
C6 H6 0.9300 . ?
C7 S1 1.753(4) . ?
C8 N1 1.507(5) . ?
C8 C9 1.527(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.496(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.355(4) . ?
C10 C20 1.413(4) . ?
C11 C12 1.414(5) . ?
C11 N1 1.454(4) . ?
C12 C13 1.405(5) . ?
C12 C17 1.430(5) . ?
C13 C14 1.361(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.380(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.364(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.422(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.432(5) . ?
C18 C20 1.374(4) . ?
C18 C19 1.523(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.482(5) . ?
C21 C22 1.375(7) . ?
C21 C26 1.379(7) . ?
C22 C23 1.397(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.374(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.307(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.378(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
N1 S1 1.663(3) . ?
O1 S1 1.432(3) . ?
O2 S1 1.422(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
C2 C1 C7 119.2(3) . . ?
C2 C1 H1 120.4 . . ?
C7 C1 H1 120.4 . . ?
C1 C2 C3 121.8(4) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 H2 119.1 . . ?
C2 C3 C5 117.7(4) . . ?
C2 C3 C4 121.0(4) . . ?
C5 C3 C4 121.3(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C3 121.4(4) . . ?
C6 C5 H5 119.3 . . ?
C3 C5 H5 119.3 . . ?
C5 C6 C7 119.5(4) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C1 120.4(3) . . ?
C6 C7 S1 121.2(3) . . ?
C1 C7 S1 118.3(3) . . ?
N1 C8 C9 105.8(3) . . ?
N1 C8 H8A 110.6 . . ?
C9 C8 H8A 110.6 . . ?
N1 C8 H8B 110.6 . . ?
C9 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
C10 C9 C8 102.3(3) . . ?
C10 C9 H9A 111.3 . . ?
C8 C9 H9A 111.3 . . ?
C10 C9 H9B 111.3 . . ?
C8 C9 H9B 111.3 . . ?
H9A C9 H9B 109.2 . . ?
C11 C10 C20 121.2(3) . . ?
C11 C10 C9 111.0(3) . . ?
C20 C10 C9 127.7(3) . . ?
C10 C11 C12 122.6(3) . . ?
C10 C11 N1 111.2(3) . . ?
C12 C11 N1 126.3(3) . . ?
C13 C12 C11 124.7(3) . . ?
C13 C12 C17 119.1(3) . . ?
C11 C12 C17 116.2(3) . . ?
C14 C13 C12 121.1(4) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 120.0(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 121.7(4) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 120.1(4) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C12 117.9(3) . . ?
C16 C17 C18 121.7(3) . . ?
C12 C17 C18 120.5(3) . . ?
C20 C18 C17 120.3(3) . . ?
C20 C18 C19 120.9(3) . . ?
C17 C18 C19 118.7(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 C10 119.0(3) . . ?
C18 C20 C21 123.1(3) . . ?
C10 C20 C21 117.9(3) . . ?
C22 C21 C26 119.0(4) . . ?
C22 C21 C20 119.0(4) . . ?
C26 C21 C20 122.0(5) . . ?
C21 C22 C23 119.5(5) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 118.9(5) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C25 C24 C23 121.6(5) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 120.8(5) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 120.1(5) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C11 N1 C8 104.2(3) . . ?
C11 N1 S1 116.4(2) . . ?
C8 N1 S1 113.9(2) . . ?
O2 S1 O1 120.01(18) . . ?
O2 S1 N1 107.30(16) . . ?
O1 S1 N1 106.06(17) . . ?
O2 S1 C7 107.69(17) . . ?
O1 S1 C7 108.38(19) . . ?
N1 S1 C7 106.70(15) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.207
####################################################################### 
# 
# 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_gly150416
_database_code_depnum_ccdc_archive 'CCDC 1063386'
_audit_update_record             
;
2015-05-05 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Br2 N2 O4 S2'
_chemical_formula_sum            'C34 H30 Br2 N2 O4 S2'
_chemical_formula_weight         754.54

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'
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           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   9.5442(15)
_cell_length_b                   15.093(3)
_cell_length_c                   45.323(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6528.8(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9980
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      23.84

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3056
_exptl_absorpt_coefficient_mu    2.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_process_details   sadabs

_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_reflns_number            42133
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_theta_min         0.90
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6171
_reflns_number_gt                3480
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0857P)²+3.8940P] 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         6171
_refine_ls_number_parameters     399
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.0717
_refine_ls_wR_factor_ref         0.1782
_refine_ls_wR_factor_gt          0.1563
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
Br1 Br -0.02766(7) -0.11177(6) 0.048309(13) 0.0812(3) Uani 1 1 d . . .
Br2 Br 0.72377(9) 0.07358(8) 0.001431(15) 0.1163(5) Uani 1 1 d . . .
C1 C 0.2729(4) -0.0692(3) 0.11308(10) 0.0279(11) Uani 1 1 d . . .
C2 C 0.1988(5) -0.0710(4) 0.08630(10) 0.0378(13) Uani 1 1 d . . .
H2A H 0.2415 -0.0509 0.0691 0.045 Uiso 1 1 calc R . .
C3 C 0.0646(5) -0.1022(4) 0.08534(11) 0.0443(14) Uani 1 1 d . . .
C4 C -0.0065(5) -0.1307(4) 0.11065(10) 0.0393(13) Uani 1 1 d . . .
H4 H -0.0972 -0.1529 0.1094 0.047 Uiso 1 1 calc R . .
C5 C 0.0598(5) -0.1251(3) 0.13688(11) 0.0352(13) Uani 1 1 d . . .
H5 H 0.0121 -0.1413 0.1539 0.042 Uiso 1 1 calc R . .
C6 C 0.1999(4) -0.0954(3) 0.13914(9) 0.0255(11) Uani 1 1 d . . .
C7 C 0.2795(5) -0.0946(3) 0.16558(10) 0.0262(11) Uani 1 1 d . . .
C8 C 0.4208(5) -0.0804(3) 0.16585(10) 0.0290(11) Uani 1 1 d . . .
C9 C 0.4787(5) -0.0963(4) 0.19611(10) 0.0377(13) Uani 1 1 d . . .
H9A H 0.5019 -0.0411 0.2059 0.045 Uiso 1 1 calc R . .
H9B H 0.5611 -0.1338 0.1955 0.045 Uiso 1 1 calc R . .
C10 C 0.3570(5) -0.1427(4) 0.21125(10) 0.0395(13) Uani 1 1 d . . .
H10A H 0.3691 -0.2065 0.2106 0.047 Uiso 1 1 calc R . .
H10B H 0.3501 -0.1244 0.2317 0.047 Uiso 1 1 calc R . .
C11 C 0.2432(5) 0.0534(4) 0.21478(11) 0.0418(14) Uani 1 1 d . . .
C12 C 0.3166(6) 0.0686(4) 0.24064(11) 0.0508(16) Uani 1 1 d . . .
H12 H 0.2957 0.0358 0.2575 0.061 Uiso 1 1 calc R . .
C13 C 0.4209(7) 0.1322(4) 0.24161(14) 0.0601(18) Uani 1 1 d . . .
H13 H 0.4670 0.1431 0.2593 0.072 Uiso 1 1 calc R . .
C14 C 0.4574(6) 0.1795(4) 0.21693(14) 0.0526(16) Uani 1 1 d . . .
C15 C 0.5822(8) 0.2421(5) 0.21729(15) 0.079(2) Uani 1 1 d . . .
H15A H 0.5904 0.2707 0.1984 0.119 Uiso 1 1 calc R . .
H15B H 0.6661 0.2091 0.2213 0.119 Uiso 1 1 calc R . .
H15C H 0.5690 0.2860 0.2324 0.119 Uiso 1 1 calc R . .
C16 C 0.3802(6) 0.1664(4) 0.19173(12) 0.0510(15) Uani 1 1 d . . .
H16 H 0.4002 0.2004 0.1751 0.061 Uiso 1 1 calc R . .
C17 C 0.2735(6) 0.1046(4) 0.19021(11) 0.0419(14) Uani 1 1 d . . .
H17 H 0.2227 0.0974 0.1729 0.050 Uiso 1 1 calc R . .
C18 C 0.5049(6) 0.0712(5) 0.08015(13) 0.0538(16) Uani 1 1 d . . .
H18 H 0.4702 0.1135 0.0931 0.065 Uiso 1 1 calc R . .
C19 C 0.5726(7) 0.0980(5) 0.05439(16) 0.071(2) Uani 1 1 d . . .
H19 H 0.5826 0.1579 0.0502 0.085 Uiso 1 1 calc R . .
C20 C 0.6238(6) 0.0359(6) 0.03549(13) 0.067(2) Uani 1 1 d . . .
C21 C 0.6078(6) -0.0523(6) 0.04109(12) 0.0634(19) Uani 1 1 d . . .
H21 H 0.6406 -0.0948 0.0279 0.076 Uiso 1 1 calc R . .
C22 C 0.5421(6) -0.0765(4) 0.06663(12) 0.0515(15) Uani 1 1 d . . .
H22 H 0.5329 -0.1366 0.0708 0.062 Uiso 1 1 calc R . .
C23 C 0.4890(4) -0.0165(4) 0.08646(10) 0.0354(13) Uani 1 1 d . . .
C24 C 0.4189(4) -0.0461(3) 0.11416(9) 0.0269(11) Uani 1 1 d . . .
C25 C 0.4934(4) -0.0543(3) 0.14005(10) 0.0295(11) Uani 1 1 d . . .
C26 C 0.6481(5) -0.0320(3) 0.14210(10) 0.0348(12) Uani 1 1 d . . .
H26A H 0.6900 -0.0350 0.1226 0.042 Uiso 1 1 calc R . .
H26B H 0.6948 -0.0750 0.1546 0.042 Uiso 1 1 calc R . .
C27 C 0.6677(5) 0.0606(4) 0.15478(13) 0.0480(15) Uani 1 1 d . . .
H27A H 0.6180 0.1030 0.1426 0.058 Uiso 1 1 calc R . .
H27B H 0.6275 0.0629 0.1744 0.058 Uiso 1 1 calc R . .
C28 C 0.9694(6) 0.1765(4) 0.11710(15) 0.0583(17) Uani 1 1 d . . .
C29 C 0.9094(9) 0.1426(6) 0.0923(2) 0.103(3) Uani 1 1 d . . .
H29 H 0.8184 0.1207 0.0931 0.124 Uiso 1 1 calc R . .
C30 C 0.9816(10) 0.1406(6) 0.0662(2) 0.106(3) Uani 1 1 d . . .
H30 H 0.9388 0.1159 0.0497 0.127 Uiso 1 1 calc R . .
C31 C 1.1147(9) 0.1737(5) 0.0635(2) 0.088(2) Uani 1 1 d . . .
C32 C 1.1920(11) 0.1732(7) 0.0346(2) 0.135(4) Uani 1 1 d . . .
H32A H 1.1278 0.1859 0.0189 0.202 Uiso 1 1 calc R . .
H32B H 1.2333 0.1159 0.0315 0.202 Uiso 1 1 calc R . .
H32C H 1.2643 0.2174 0.0350 0.202 Uiso 1 1 calc R . .
C33 C 1.1751(8) 0.2077(5) 0.0894(2) 0.083(2) Uani 1 1 d . . .
H33 H 1.2655 0.2306 0.0886 0.099 Uiso 1 1 calc R . .
C34 C 1.1033(6) 0.2081(4) 0.11596(18) 0.0682(19) Uani 1 1 d . . .
H34 H 1.1461 0.2298 0.1329 0.082 Uiso 1 1 calc R . .
N1 N 0.2275(4) -0.1155(3) 0.19432(8) 0.0324(10) Uani 1 1 d . . .
N2 N 0.8169(5) 0.0855(3) 0.15629(11) 0.0593(14) Uani 1 1 d . . .
H2B H 0.8768 0.0451 0.1608 0.071 Uiso 1 1 calc R . .
O1 O 0.1012(4) -0.0711(3) 0.23987(7) 0.0598(11) Uani 1 1 d . . .
O2 O 0.0199(3) -0.0167(3) 0.19129(8) 0.0506(10) Uani 1 1 d . . .
O3 O 0.7544(4) 0.2386(3) 0.14462(11) 0.0808(14) Uani 1 1 d . . .
O4 O 0.9707(4) 0.2062(3) 0.17249(10) 0.0718(13) Uani 1 1 d . . .
S1 S 0.13232(13) -0.03796(9) 0.21122(3) 0.0413(4) Uani 1 1 d . . .
S2 S 0.87327(15) 0.18317(10) 0.14992(4) 0.0576(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
Br1 C3 1.901(5) . ?
Br2 C20 1.901(6) . ?
C1 C2 1.405(6) . ?
C1 C6 1.427(6) . ?
C1 C24 1.437(6) . ?
C2 C3 1.365(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.401(7) . ?
C4 C5 1.349(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.414(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.419(6) . ?
C7 C8 1.366(6) . ?
C7 N1 1.429(6) . ?
C8 C25 1.415(6) . ?
C8 C9 1.498(6) . ?
C9 C10 1.520(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N1 1.511(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.385(7) . ?
C11 C17 1.386(7) . ?
C11 S1 1.745(6) . ?
C12 C13 1.383(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.372(9) . ?
C13 H13 0.9300 . ?
C14 C16 1.373(7) . ?
C14 C15 1.521(9) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.383(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C23 1.362(8) . ?
C18 C19 1.394(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.360(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.365(10) . ?
C21 C22 1.366(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.373(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.491(6) . ?
C24 C25 1.377(6) . ?
C25 C26 1.517(6) . ?
C26 C27 1.523(7) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N2 1.474(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.361(9) . ?
C28 C34 1.365(8) . ?
C28 S2 1.751(7) . ?
C29 C30 1.368(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.370(11) . ?
C30 H30 0.9300 . ?
C31 C33 1.402(11) . ?
C31 C32 1.505(12) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.386(10) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
N1 S1 1.668(4) . ?
N2 S2 1.596(5) . ?
N2 H2B 0.8600 . ?
O1 S1 1.423(4) . ?
O2 S1 1.439(3) . ?
O3 S2 1.430(4) . ?
O4 S2 1.425(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
C2 C1 C6 117.6(4) . . ?
C2 C1 C24 121.5(4) . . ?
C6 C1 C24 120.8(4) . . ?
C3 C2 C1 120.4(4) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C4 122.3(4) . . ?
C2 C3 Br1 119.3(4) . . ?
C4 C3 Br1 118.4(3) . . ?
C5 C4 C3 118.4(4) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 121.8(4) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C7 124.8(4) . . ?
C5 C6 C1 119.3(4) . . ?
C7 C6 C1 115.8(4) . . ?
C8 C7 C6 122.5(4) . . ?
C8 C7 N1 111.7(4) . . ?
C6 C7 N1 125.6(4) . . ?
C7 C8 C25 121.3(4) . . ?
C7 C8 C9 110.3(4) . . ?
C25 C8 C9 128.4(4) . . ?
C8 C9 C10 101.9(4) . . ?
C8 C9 H9A 111.4 . . ?
C10 C9 H9A 111.4 . . ?
C8 C9 H9B 111.4 . . ?
C10 C9 H9B 111.4 . . ?
H9A C9 H9B 109.3 . . ?
N1 C10 C9 105.6(4) . . ?
N1 C10 H10A 110.6 . . ?
C9 C10 H10A 110.6 . . ?
N1 C10 H10B 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
C12 C11 C17 118.8(6) . . ?
C12 C11 S1 121.1(4) . . ?
C17 C11 S1 119.5(4) . . ?
C13 C12 C11 120.4(5) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 121.2(5) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C16 117.8(6) . . ?
C13 C14 C15 120.9(5) . . ?
C16 C14 C15 121.2(6) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 C17 122.2(6) . . ?
C14 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C16 C17 C11 119.4(5) . . ?
C16 C17 H17 120.3 . . ?
C11 C17 H17 120.3 . . ?
C23 C18 C19 120.6(6) . . ?
C23 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 119.6(7) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 121.0(6) . . ?
C19 C20 Br2 119.1(6) . . ?
C21 C20 Br2 119.9(6) . . ?
C20 C21 C22 118.0(6) . . ?
C20 C21 H21 121.0 . . ?
C22 C21 H21 121.0 . . ?
C21 C22 C23 123.2(6) . . ?
C21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
C18 C23 C22 117.5(5) . . ?
C18 C23 C24 121.2(5) . . ?
C22 C23 C24 121.3(5) . . ?
C25 C24 C1 120.5(4) . . ?
C25 C24 C23 120.8(4) . . ?
C1 C24 C23 118.6(4) . . ?
C24 C25 C8 118.4(4) . . ?
C24 C25 C26 122.3(4) . . ?
C8 C25 C26 119.2(4) . . ?
C25 C26 C27 110.2(4) . . ?
C25 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
N2 C27 C26 111.7(4) . . ?
N2 C27 H27A 109.3 . . ?
C26 C27 H27A 109.3 . . ?
N2 C27 H27B 109.3 . . ?
C26 C27 H27B 109.3 . . ?
H27A C27 H27B 107.9 . . ?
C29 C28 C34 119.6(7) . . ?
C29 C28 S2 120.2(6) . . ?
C34 C28 S2 120.2(5) . . ?
C28 C29 C30 120.6(7) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C31 122.4(8) . . ?
C29 C30 H30 118.8 . . ?
C31 C30 H30 118.8 . . ?
C30 C31 C33 116.1(8) . . ?
C30 C31 C32 122.0(9) . . ?
C33 C31 C32 121.8(8) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C31 121.6(7) . . ?
C34 C33 H33 119.2 . . ?
C31 C33 H33 119.2 . . ?
C28 C34 C33 119.6(7) . . ?
C28 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C7 N1 C10 103.9(3) . . ?
C7 N1 S1 116.9(3) . . ?
C10 N1 S1 113.8(3) . . ?
C27 N2 S2 123.5(4) . . ?
C27 N2 H2B 118.2 . . ?
S2 N2 H2B 118.2 . . ?
O1 S1 O2 119.7(2) . . ?
O1 S1 N1 106.7(2) . . ?
O2 S1 N1 105.9(2) . . ?
O1 S1 C11 108.6(2) . . ?
O2 S1 C11 109.5(2) . . ?
N1 S1 C11 105.4(2) . . ?
O4 S2 O3 119.7(3) . . ?
O4 S2 N2 108.4(3) . . ?
O3 S2 N2 107.7(3) . . ?
O4 S2 C28 106.4(3) . . ?
O3 S2 C28 107.9(3) . . ?
N2 S2 C28 106.1(3) . . ?

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
N2 H2B O2 0.86 2.15 2.941(6) 151.8 1_655

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         0.987
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.103
