# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 997379'
_audit_update_record             
;
2014-04-15 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
2,3-dimethyl 4-(4-methoxyphenyl)-2-(4-methylphenyl)
-1-oxo-1,2-dihydronapthalene-2,3-dicarboxylate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H24 O6'
_chemical_formula_sum            'C28 H24 O6'
_chemical_formula_weight         456.47

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5256(2)
_cell_length_b                   10.2095(3)
_cell_length_c                   15.6299(4)
_cell_angle_alpha                93.9900(10)
_cell_angle_beta                 94.6790(10)
_cell_angle_gamma                101.089(2)
_cell_volume                     1170.06(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4611
_cell_measurement_theta_min      1.31
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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 Axs Kappa APEXII CCD diffractometer'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23872
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4611
_reflns_number_gt                3600
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (BRUKER, 2008)'
_computing_cell_refinement       APEX2
_computing_data_reduction        'SAINT (BRUKER, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 2012)'
_computing_publication_material  
'SHELXL-97 (Sheldrick, 2008) and  PLATON  (Spek, 2009)'

_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)+(0.0727P)²+0.1453P] 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         4611
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1209
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_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
C1 C 1.04018(18) 0.02693(13) 0.34058(8) 0.0383(3) Uani 1 1 d . . .
C2 C 1.0229(2) 0.13517(15) 0.39599(10) 0.0477(4) Uani 1 1 d . . .
H2 H 0.9373 0.1863 0.3808 0.057 Uiso 1 1 calc R . .
C3 C 1.1304(2) 0.16817(16) 0.47320(10) 0.0547(4) Uani 1 1 d . . .
H3 H 1.1161 0.2407 0.5096 0.066 Uiso 1 1 calc R . .
C4 C 1.2578(2) 0.09481(17) 0.49648(11) 0.0585(4) Uani 1 1 d . . .
H4 H 1.3299 0.1172 0.5486 0.070 Uiso 1 1 calc R . .
C5 C 1.2792(2) -0.01205(17) 0.44261(11) 0.0550(4) Uani 1 1 d . . .
H5 H 1.3666 -0.0614 0.4582 0.066 Uiso 1 1 calc R . .
C6 C 1.17129(18) -0.04674(14) 0.36527(9) 0.0415(3) Uani 1 1 d . . .
C7 C 1.1959(2) -0.16143(15) 0.30795(10) 0.0443(3) Uani 1 1 d . . .
C8 C 1.03031(19) -0.22890(13) 0.24592(9) 0.0394(3) Uani 1 1 d . . .
C9 C 0.92933(19) -0.12498(13) 0.21158(8) 0.0384(3) Uani 1 1 d . . .
C10 C 0.92855(18) -0.00896(13) 0.25741(8) 0.0370(3) Uani 1 1 d . . .
C11 C 0.8042(2) 0.08104(13) 0.23095(8) 0.0400(3) Uani 1 1 d . . .
C12 C 0.6189(2) 0.03662(16) 0.23131(11) 0.0518(4) Uani 1 1 d . . .
H12 H 0.5749 -0.0497 0.2458 0.062 Uiso 1 1 calc R . .
C13 C 0.4983(2) 0.11752(18) 0.21063(12) 0.0590(4) Uani 1 1 d . . .
H13 H 0.3742 0.0860 0.2118 0.071 Uiso 1 1 calc R . .
C14 C 0.5605(2) 0.24497(16) 0.18812(10) 0.0506(4) Uani 1 1 d . . .
C15 C 0.7448(2) 0.29123(15) 0.18676(10) 0.0519(4) Uani 1 1 d . . .
H15 H 0.7880 0.3769 0.1711 0.062 Uiso 1 1 calc R . .
C16 C 0.8649(2) 0.20944(14) 0.20887(10) 0.0476(4) Uani 1 1 d . . .
H16 H 0.9892 0.2417 0.2089 0.057 Uiso 1 1 calc R . .
C17 C 0.4756(4) 0.43503(19) 0.12850(14) 0.0817(7) Uani 1 1 d . . .
H17A H 0.5667 0.4979 0.1649 0.123 Uiso 1 1 calc R . .
H17B H 0.3697 0.4731 0.1177 0.123 Uiso 1 1 calc R . .
H17C H 0.5225 0.4149 0.0749 0.123 Uiso 1 1 calc R . .
C18 C 0.91531(19) -0.32871(13) 0.29922(8) 0.0381(3) Uani 1 1 d . . .
C19 C 0.9957(2) -0.41952(15) 0.34216(10) 0.0493(4) Uani 1 1 d . . .
H19 H 1.1195 -0.4171 0.3405 0.059 Uiso 1 1 calc R . .
C20 C 0.8952(3) -0.51328(16) 0.38732(10) 0.0571(4) Uani 1 1 d . . .
H20 H 0.9528 -0.5726 0.4162 0.068 Uiso 1 1 calc R . .
C21 C 0.7110(3) -0.52141(15) 0.39078(10) 0.0570(4) Uani 1 1 d . . .
C22 C 0.6324(2) -0.42849(16) 0.35013(10) 0.0534(4) Uani 1 1 d . . .
H22 H 0.5090 -0.4302 0.3529 0.064 Uiso 1 1 calc R . .
C23 C 0.7324(2) -0.33248(15) 0.30520(9) 0.0432(3) Uani 1 1 d . . .
H23 H 0.6760 -0.2702 0.2789 0.052 Uiso 1 1 calc R . .
C24 C 0.6001(4) -0.6312(2) 0.43494(16) 0.0923(7) Uani 1 1 d . . .
H24A H 0.4829 -0.6107 0.4425 0.138 Uiso 1 1 calc R . .
H24B H 0.6617 -0.6383 0.4902 0.138 Uiso 1 1 calc R . .
H24C H 0.5852 -0.7147 0.4003 0.138 Uiso 1 1 calc R . .
C25 C 1.0998(2) -0.30580(16) 0.17182(10) 0.0519(4) Uani 1 1 d . . .
C26 C 1.2396(4) -0.2783(3) 0.04363(16) 0.1069(9) Uani 1 1 d . . .
H26A H 1.3530 -0.3042 0.0598 0.160 Uiso 1 1 calc R . .
H26B H 1.2573 -0.2141 0.0016 0.160 Uiso 1 1 calc R . .
H26C H 1.1518 -0.3559 0.0196 0.160 Uiso 1 1 calc R . .
C27 C 0.8253(2) -0.16462(14) 0.12555(9) 0.0456(4) Uani 1 1 d . . .
C28 C 0.7520(3) -0.0989(2) -0.01143(12) 0.0830(7) Uani 1 1 d . . .
H28A H 0.7794 -0.1808 -0.0357 0.125 Uiso 1 1 calc R . .
H28B H 0.7931 -0.0279 -0.0467 0.125 Uiso 1 1 calc R . .
H28C H 0.6230 -0.1094 -0.0091 0.125 Uiso 1 1 calc R . .
O1 O 1.33433(15) -0.20590(12) 0.31243(9) 0.0627(3) Uani 1 1 d . . .
O2 O 0.42859(19) 0.31624(13) 0.16967(9) 0.0733(4) Uani 1 1 d . . .
O3 O 1.0895(2) -0.42337(12) 0.16241(9) 0.0762(4) Uani 1 1 d . . .
O4 O 1.17485(18) -0.21965(12) 0.11867(8) 0.0677(4) Uani 1 1 d . . .
O5 O 0.7425(2) -0.27618(12) 0.10393(8) 0.0718(4) Uani 1 1 d . . .
O6 O 0.84264(17) -0.06655(11) 0.07423(7) 0.0585(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 1.389(2) . ?
C1 C6 1.397(2) . ?
C1 C10 1.4721(19) . ?
C2 C3 1.380(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.384(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.474(2) . ?
C7 O1 1.2127(18) . ?
C7 C8 1.532(2) . ?
C8 C9 1.5212(19) . ?
C8 C25 1.537(2) . ?
C8 C18 1.5421(19) . ?
C9 C10 1.3422(19) . ?
C9 C27 1.488(2) . ?
C10 C11 1.4870(19) . ?
C11 C12 1.382(2) . ?
C11 C16 1.380(2) . ?
C12 C13 1.374(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(2) . ?
C13 H13 0.9300 . ?
C14 O2 1.3631(19) . ?
C14 C15 1.379(3) . ?
C15 C16 1.384(2) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 O2 1.411(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C23 1.381(2) . ?
C18 C19 1.383(2) . ?
C19 C20 1.374(2) . ?
C19 H19 0.9300 . ?
C20 C21 1.379(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.375(2) . ?
C21 C24 1.507(2) . ?
C22 C23 1.385(2) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O3 1.1859(19) . ?
C25 O4 1.330(2) . ?
C26 O4 1.442(2) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 O5 1.1997(18) . ?
C27 O6 1.3197(18) . ?
C28 O6 1.439(2) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?

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 117.77(13) . . ?
C2 C1 C10 122.03(13) . . ?
C6 C1 C10 120.19(12) . . ?
C3 C2 C1 121.14(15) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C4 C3 C2 120.33(15) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.81(14) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 120.40(15) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 120.54(14) . . ?
C5 C6 C7 119.85(14) . . ?
C1 C6 C7 119.61(12) . . ?
O1 C7 C6 122.68(14) . . ?
O1 C7 C8 121.18(13) . . ?
C6 C7 C8 115.99(12) . . ?
C9 C8 C7 110.64(11) . . ?
C9 C8 C25 110.61(12) . . ?
C7 C8 C25 107.51(12) . . ?
C9 C8 C18 113.33(11) . . ?
C7 C8 C18 104.74(11) . . ?
C25 C8 C18 109.72(11) . . ?
C10 C9 C27 122.87(13) . . ?
C10 C9 C8 122.15(12) . . ?
C27 C9 C8 114.92(11) . . ?
C9 C10 C1 120.25(13) . . ?
C9 C10 C11 121.90(12) . . ?
C1 C10 C11 117.61(11) . . ?
C12 C11 C16 117.92(13) . . ?
C12 C11 C10 118.83(12) . . ?
C16 C11 C10 123.20(13) . . ?
C13 C12 C11 121.24(15) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.26(16) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
O2 C14 C13 115.02(16) . . ?
O2 C14 C15 125.42(15) . . ?
C13 C14 C15 119.55(14) . . ?
C14 C15 C16 119.62(14) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C11 C16 C15 121.39(15) . . ?
C11 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 118.01(13) . . ?
C23 C18 C8 122.41(12) . . ?
C19 C18 C8 119.58(13) . . ?
C20 C19 C18 120.95(16) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 121.48(16) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 117.44(15) . . ?
C22 C21 C24 121.72(19) . . ?
C20 C21 C24 120.81(18) . . ?
C21 C22 C23 121.68(16) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C18 C23 C22 120.37(14) . . ?
C18 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C25 O4 124.47(14) . . ?
O3 C25 C8 126.15(15) . . ?
O4 C25 C8 109.38(13) . . ?
O4 C26 H26A 109.5 . . ?
O4 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O4 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O5 C27 O6 123.73(14) . . ?
O5 C27 C9 123.19(14) . . ?
O6 C27 C9 112.98(12) . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C14 O2 C17 118.29(16) . . ?
C25 O4 C26 115.62(15) . . ?
C27 O6 C28 116.23(13) . . ?

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
C6 C1 C2 C3 -0.6(2) . . . . ?
C10 C1 C2 C3 -179.19(14) . . . . ?
C1 C2 C3 C4 0.4(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
C4 C5 C6 C1 0.5(2) . . . . ?
C4 C5 C6 C7 179.84(15) . . . . ?
C2 C1 C6 C5 0.1(2) . . . . ?
C10 C1 C6 C5 178.76(13) . . . . ?
C2 C1 C6 C7 -179.26(13) . . . . ?
C10 C1 C6 C7 -0.6(2) . . . . ?
C5 C6 C7 O1 -20.2(2) . . . . ?
C1 C6 C7 O1 159.14(14) . . . . ?
C5 C6 C7 C8 155.46(14) . . . . ?
C1 C6 C7 C8 -25.17(19) . . . . ?
O1 C7 C8 C9 -146.06(14) . . . . ?
C6 C7 C8 C9 38.17(16) . . . . ?
O1 C7 C8 C25 -25.18(19) . . . . ?
C6 C7 C8 C25 159.05(12) . . . . ?
O1 C7 C8 C18 91.49(16) . . . . ?
C6 C7 C8 C18 -84.28(14) . . . . ?
C7 C8 C9 C10 -29.43(18) . . . . ?
C25 C8 C9 C10 -148.44(13) . . . . ?
C18 C8 C9 C10 87.86(16) . . . . ?
C7 C8 C9 C27 153.25(12) . . . . ?
C25 C8 C9 C27 34.23(16) . . . . ?
C18 C8 C9 C27 -89.46(14) . . . . ?
C27 C9 C10 C1 -177.52(12) . . . . ?
C8 C9 C10 C1 5.4(2) . . . . ?
C27 C9 C10 C11 8.3(2) . . . . ?
C8 C9 C10 C11 -168.85(12) . . . . ?
C2 C1 C10 C9 -170.04(13) . . . . ?
C6 C1 C10 C9 11.4(2) . . . . ?
C2 C1 C10 C11 4.4(2) . . . . ?
C6 C1 C10 C11 -174.17(12) . . . . ?
C9 C10 C11 C12 65.29(18) . . . . ?
C1 C10 C11 C12 -109.07(15) . . . . ?
C9 C10 C11 C16 -117.16(16) . . . . ?
C1 C10 C11 C16 68.48(17) . . . . ?
C16 C11 C12 C13 -0.2(2) . . . . ?
C10 C11 C12 C13 177.50(14) . . . . ?
C11 C12 C13 C14 0.7(3) . . . . ?
C12 C13 C14 O2 -179.46(15) . . . . ?
C12 C13 C14 C15 -0.2(3) . . . . ?
O2 C14 C15 C16 178.48(14) . . . . ?
C13 C14 C15 C16 -0.6(2) . . . . ?
C12 C11 C16 C15 -0.7(2) . . . . ?
C10 C11 C16 C15 -178.30(13) . . . . ?
C14 C15 C16 C11 1.1(2) . . . . ?
C9 C8 C18 C23 7.76(18) . . . . ?
C7 C8 C18 C23 128.44(13) . . . . ?
C25 C8 C18 C23 -116.42(14) . . . . ?
C9 C8 C18 C19 -173.04(12) . . . . ?
C7 C8 C18 C19 -52.35(15) . . . . ?
C25 C8 C18 C19 62.78(17) . . . . ?
C23 C18 C19 C20 1.9(2) . . . . ?
C8 C18 C19 C20 -177.35(13) . . . . ?
C18 C19 C20 C21 0.7(2) . . . . ?
C19 C20 C21 C22 -2.6(2) . . . . ?
C19 C20 C21 C24 175.37(16) . . . . ?
C20 C21 C22 C23 1.8(2) . . . . ?
C24 C21 C22 C23 -176.10(16) . . . . ?
C19 C18 C23 C22 -2.6(2) . . . . ?
C8 C18 C23 C22 176.60(12) . . . . ?
C21 C22 C23 C18 0.8(2) . . . . ?
C9 C8 C25 O3 -135.18(19) . . . . ?
C7 C8 C25 O3 103.9(2) . . . . ?
C18 C8 C25 O3 -9.4(2) . . . . ?
C9 C8 C25 O4 44.85(17) . . . . ?
C7 C8 C25 O4 -76.04(16) . . . . ?
C18 C8 C25 O4 170.60(13) . . . . ?
C10 C9 C27 O5 -138.50(17) . . . . ?
C8 C9 C27 O5 38.8(2) . . . . ?
C10 C9 C27 O6 45.2(2) . . . . ?
C8 C9 C27 O6 -137.52(13) . . . . ?
C13 C14 O2 C17 -166.52(16) . . . . ?
C15 C14 O2 C17 14.3(2) . . . . ?
O3 C25 O4 C26 2.6(3) . . . . ?
C8 C25 O4 C26 -177.48(18) . . . . ?
O5 C27 O6 C28 1.2(3) . . . . ?
C9 C27 O6 C28 177.52(16) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1438209'
_audit_update_record             
;
2015-11-23 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'ethyl 4-oxo-3-phenyl-1-(thiophen-2-yl)-3-(thiophen-3-yl)-3,4-dihydronaphthalene-2-carboxylate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H20 O3 S2'
_chemical_formula_sum            'C27 H20 O3 S2'
_chemical_formula_weight         456.55

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'
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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   12.1263(11)
_cell_length_b                   11.8009(11)
_cell_length_c                   16.0657(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.181(2)
_cell_angle_gamma                90.00
_cell_volume                     2262.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4111
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      25.39

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_type   multi_scan
_exptl_absorpt_correction_T_min  0.9373
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_process_details   'SADABS (Bruker, 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 KappaApexII CCD Diffractometer'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29905
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.39
_reflns_number_total             4111
_reflns_number_gt                2686
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0338P)²+2.9594P] 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         4111
_refine_ls_number_parameters     364
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1475
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_iucr_refine_instruction_details 
;
TITL G6 in P2(1)/c
CELL  0.71073  12.1263  11.8009  16.0657   90.000  100.181   90.000
ZERR     4.00   0.0011   0.0011   0.0013    0.000    0.002    0.000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    O    S
UNIT  108  80   12   8
MERG   2
DFIX 1.70 0.01 C18 S2 C18 S2'
DFIX 1.70 0.01 C21 S2 C21' S2'
DFIX 1.50 0.01 C19 C20 C19' C20'
DFIX 1.40 0.01 C18 C19 C18 C19'
DFIX 1.40 0.01 C20 C21 C20' C21'
DFIX 1.70 0.01 C11 S1 C11 S1'
DFIX 1.70 0.01 C14 S1 C14' S1'
DFIX 1.50 0.01 C12 C13 C12' C13'
DFIX 1.40 0.01 C11 C12 C11 C12'
DFIX 1.40 0.01 C13 C14 C13' C14'
SIMU 0.01 S1  > C14
SIMU 0.01 S1' > C14'
DELU 0.01 S1  > C14
DELU 0.01 S1' > C14'
SIMU 0.01 S2  > C21
SIMU 0.01 S2' > C21'
DELU 0.01 S2  > C21
DELU 0.01 S2' > C21'
FMAP   2
PLAN   20
SIZE     0.15   0.25   0.25
BOND $H
ACTA
CONF
L.S.   8
TEMP    23.00
WGHT    0.033800    2.959400
FVAR       0.19265   0.47119   0.63264
C7    1    0.614704    0.755389    0.119482    11.00000    0.04780    0.04441 =
         0.03707   -0.00125    0.00817   -0.00160
C6    1    0.574477    0.743964    0.027827    11.00000    0.03502    0.04647 =
         0.03765   -0.00699    0.00871    0.00023
C5    1    0.495266    0.661425   -0.001311    11.00000    0.04899    0.05725 =
         0.05061   -0.00753    0.01230   -0.00943
AFIX  43
H5    2    0.468628    0.614243    0.037066    11.00000   -1.20000
AFIX   0
C4    1    0.455975    0.649044   -0.086597    11.00000    0.05132    0.06840 =
         0.05749   -0.01678    0.00201   -0.01450
AFIX  43
H4    2    0.403399    0.593352   -0.105932    11.00000   -1.20000
AFIX   0
C3    1    0.495031    0.719616   -0.142978    11.00000    0.05457    0.07295 =
         0.04157   -0.01383   -0.00121   -0.00375
AFIX  43
H3    2    0.468668    0.711124   -0.200610    11.00000   -1.20000
AFIX   0
C2    1    0.572491    0.802550   -0.115384    11.00000    0.04645    0.05889 =
         0.03810   -0.00052    0.00586    0.00128
AFIX  43
H2    2    0.597577    0.849845   -0.154425    11.00000   -1.20000
AFIX   0
C1    1    0.613759    0.816324   -0.029286    11.00000    0.02956    0.04491 =
         0.03568   -0.00342    0.00414    0.00587
C10   1    0.694838    0.906186    0.002818    11.00000    0.02966    0.04252 =
         0.03386   -0.00040    0.00684    0.00478
C9    1    0.744353    0.908907    0.084326    11.00000    0.03119    0.04150 =
         0.03779   -0.00040    0.00638    0.00097
C8    1    0.727375    0.817139    0.147614    11.00000    0.03855    0.04465 =
         0.03144   -0.00258    0.00388   -0.00073
C22   1    0.730742    0.870035    0.235355    11.00000    0.04284    0.04990 =
         0.03568   -0.00385    0.01000   -0.00683
C23   1    0.806250    0.836270    0.309670    11.00000    0.04353    0.05968 =
         0.03572   -0.00800    0.00557   -0.00768
AFIX  43
H23   2    0.856903    0.777432    0.308241    11.00000   -1.20000
AFIX   0
C24   1    0.801635    0.893330    0.383060    11.00000    0.07543    0.10731 =
         0.04612   -0.00511    0.00236   -0.02231
AFIX  43
H24   2    0.850662    0.872433    0.431894    11.00000   -1.20000
AFIX   0
C25   1    0.729646    0.977808    0.387505    11.00000    0.08285    0.09996 =
         0.06712   -0.03287    0.02654   -0.02419
AFIX  43
H25   2    0.729738    1.014296    0.438826    11.00000   -1.20000
AFIX   0
C26   1    0.656971    1.010699    0.318509    11.00000    0.08108    0.06547 =
         0.08052   -0.01907    0.03756   -0.00845
AFIX  43
H26   2    0.606483    1.068917    0.322514    11.00000   -1.20000
AFIX   0
C27   1    0.657263    0.958862    0.242858    11.00000    0.05803    0.06227 =
         0.04906   -0.00528    0.01727    0.00182
AFIX  43
H27   2    0.607591    0.983102    0.195339    11.00000   -1.20000
AFIX   0
C15   1    0.824645    1.001324    0.117792    11.00000    0.04444    0.05324 =
         0.03706    0.00156    0.00669   -0.00405
C16   1    0.844201    1.200466    0.138542    11.00000    0.10266    0.05982 =
         0.08879   -0.01842   -0.00293   -0.02134
AFIX  23
H16A  2    0.801518    1.254207    0.165735    11.00000   -1.20000
H16B  2    0.908758    1.177130    0.179580    11.00000   -1.20000
AFIX   0
C17   1    0.881212    1.253980    0.067960    11.00000    0.17239    0.09699 =
         0.10683   -0.01441    0.04109   -0.06590
AFIX 137
H17A  2    0.929473    1.203246    0.044459    11.00000   -1.50000
H17B  2    0.921444    1.322051    0.086638    11.00000   -1.50000
H17C  2    0.817438    1.272384    0.025641    11.00000   -1.50000
AFIX   0
C11   1    0.722762    0.991878   -0.057041    11.00000    0.03687    0.04619 =
         0.03828    0.00210    0.00410    0.00059
PART    1
S1'   4    0.851703    0.993133   -0.082686    21.00000    0.05500    0.07001 =
         0.04283    0.00811    0.01636   -0.00584
C12'  1    0.654144    1.080472   -0.090549    21.00000    0.07803    0.07356 =
         0.06518    0.02353    0.00322   -0.00784
AFIX  43
H12'  2    0.582369    1.092428   -0.079375    21.00000   -1.20000
AFIX   0
C13'  1    0.708551    1.154277   -0.146478    21.00000    0.07893    0.06570 =
         0.05642    0.01342   -0.00386   -0.00775
AFIX  43
H13'  2    0.678233    1.217385   -0.176883    21.00000   -1.20000
AFIX   0
C14'  1    0.812759    1.109035   -0.143374    21.00000    0.06356    0.06759 =
         0.03271    0.01280    0.01020   -0.01722
AFIX  43
H14'  2    0.862346    1.141635   -0.174446    21.00000   -1.20000
AFIX   0
PART    2
S1    4    0.630765    1.092514   -0.101795   -21.00000    0.05766    0.07091 =
         0.08007    0.02657    0.00301    0.01603
C12   1    0.822215    1.002598   -0.085794   -21.00000    0.06804    0.06543 =
         0.07853    0.01063    0.00315   -0.00369
AFIX  43
H12   2    0.880685    0.951676   -0.069931   -21.00000   -1.20000
AFIX   0
C13   1    0.832527    1.098719   -0.143179   -21.00000    0.05326    0.06534 =
         0.06548    0.00368    0.00592   -0.00182
AFIX  43
H13   2    0.894223    1.120737   -0.166389   -21.00000   -1.20000
AFIX   0
C14   1    0.729561    1.146430   -0.153331   -21.00000    0.05032    0.06363 =
         0.06341    0.01626    0.00220    0.00515
AFIX  43
H14   2    0.712937    1.208885   -0.188622   -21.00000   -1.20000
AFIX   0
PART    0
C18   1    0.813046    0.723140    0.146200    11.00000    0.05049    0.04773 =
         0.03405   -0.00200    0.00139    0.00947
PART    1
S2    4    0.805764    0.595707    0.192864    31.00000    0.10290    0.05374 =
         0.07836    0.01626    0.01201    0.01343
C19   1    0.907449    0.738064    0.109684    31.00000    0.06693    0.05659 =
         0.06843   -0.00974    0.00458    0.04755
AFIX  43
H19   2    0.926685    0.802984    0.082708    31.00000   -1.20000
AFIX   0
C20   1    0.972416    0.629800    0.121973    31.00000    0.05930    0.06462 =
         0.07438   -0.01923    0.00105    0.04201
AFIX  43
H20   2    1.037698    0.619020    0.100086    31.00000   -1.20000
AFIX   0
C21   1    0.929487    0.546755    0.167851    31.00000    0.08995    0.05860 =
         0.07036   -0.00903   -0.02207    0.03858
AFIX  43
H21   2    0.961900    0.476521    0.182648    31.00000   -1.20000
AFIX   0
PART    2
S2'   4    0.923993    0.724513    0.099922   -31.00000    0.06430    0.08374 =
         0.10772   -0.02685    0.02949    0.00966
C19'  1    0.794647    0.620836    0.185284   -31.00000    0.11291    0.09007 =
         0.12596   -0.01352    0.01777    0.07383
AFIX  43
H19'  2    0.735751    0.601586    0.212591   -31.00000   -1.20000
AFIX   0
C20'  1    0.892730    0.549474    0.172622   -31.00000    0.10500    0.07403 =
         0.11308   -0.00842    0.00623    0.07258
AFIX  43
H20'  2    0.900377    0.476634    0.194995   -31.00000   -1.20000
AFIX   0
C21'  1    0.972714    0.591060    0.127650   -31.00000    0.10136    0.08413 =
         0.10722   -0.02045    0.00477    0.06096
AFIX  43
H21'  2    1.036459    0.555257    0.115742   -31.00000   -1.20000
AFIX   0
PART    0
O1    3    0.565710    0.713466    0.171420    11.00000    0.07056    0.07876 =
         0.04157    0.00018    0.01774   -0.02468
O2    3    0.920263    0.985788    0.148607    11.00000    0.04433    0.07469 =
         0.08112   -0.01159   -0.00923   -0.00786
O3    3    0.774792    1.101887    0.110814    11.00000    0.06560    0.04582 =
         0.07095   -0.00550    0.00028   -0.00453
HKLF    4
 
REM  G6 in P2(1)/c
REM R1 =  0.0608 for   2686 Fo > 4sig(Fo)  and  0.1019 for all   4111 data
REM    364 parameters refined using    100 restraints
 
END
;

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
C7 C 0.6147(3) 0.7554(3) 0.11948(19) 0.0430(7) Uani 1 1 d . . .
C6 C 0.5745(2) 0.7440(3) 0.02783(18) 0.0394(7) Uani 1 1 d . . .
C5 C 0.4953(3) 0.6614(3) -0.0013(2) 0.0519(8) Uani 1 1 d . . .
H5 H 0.4686 0.6142 0.0371 0.062 Uiso 1 1 calc R . .
C4 C 0.4560(3) 0.6490(3) -0.0866(2) 0.0600(10) Uani 1 1 d . . .
H4 H 0.4034 0.5934 -0.1059 0.072 Uiso 1 1 calc R . .
C3 C 0.4950(3) 0.7196(3) -0.1430(2) 0.0575(9) Uani 1 1 d . . .
H3 H 0.4687 0.7111 -0.2006 0.069 Uiso 1 1 calc R . .
C2 C 0.5725(3) 0.8026(3) -0.11538(19) 0.0480(8) Uani 1 1 d . . .
H2 H 0.5976 0.8498 -0.1544 0.058 Uiso 1 1 calc R . .
C1 C 0.6138(2) 0.8163(3) -0.02929(18) 0.0369(7) Uani 1 1 d . . .
C10 C 0.6948(2) 0.9062(2) 0.00282(17) 0.0352(7) Uani 1 1 d . A .
C9 C 0.7444(2) 0.9089(3) 0.08433(18) 0.0368(7) Uani 1 1 d . . .
C8 C 0.7274(2) 0.8171(3) 0.14761(17) 0.0385(7) Uani 1 1 d . B .
C22 C 0.7307(3) 0.8700(3) 0.23535(18) 0.0424(7) Uani 1 1 d . . .
C23 C 0.8062(3) 0.8363(3) 0.30967(19) 0.0465(8) Uani 1 1 d . . .
H23 H 0.8569 0.7774 0.3082 0.056 Uiso 1 1 calc R . .
C24 C 0.8016(4) 0.8933(4) 0.3831(2) 0.0773(13) Uani 1 1 d . . .
H24 H 0.8507 0.8724 0.4319 0.093 Uiso 1 1 calc R . .
C25 C 0.7296(4) 0.9778(4) 0.3875(3) 0.0817(14) Uani 1 1 d . . .
H25 H 0.7297 1.0143 0.4388 0.098 Uiso 1 1 calc R . .
C26 C 0.6570(4) 1.0107(4) 0.3185(3) 0.0729(12) Uani 1 1 d . . .
H26 H 0.6065 1.0689 0.3225 0.087 Uiso 1 1 calc R . .
C27 C 0.6573(3) 0.9589(3) 0.2429(2) 0.0555(9) Uani 1 1 d . . .
H27 H 0.6076 0.9831 0.1953 0.067 Uiso 1 1 calc R . .
C15 C 0.8246(3) 1.0013(3) 0.11779(19) 0.0450(8) Uani 1 1 d . . .
C16 C 0.8442(4) 1.2005(4) 0.1385(3) 0.0862(14) Uani 1 1 d . . .
H16A H 0.8015 1.2542 0.1657 0.103 Uiso 1 1 calc R . .
H16B H 0.9088 1.1771 0.1796 0.103 Uiso 1 1 calc R . .
C17 C 0.8812(6) 1.2540(5) 0.0680(4) 0.123(2) Uani 1 1 d . . .
H17A H 0.9295 1.2032 0.0445 0.185 Uiso 1 1 calc R . .
H17B H 0.9214 1.3221 0.0866 0.185 Uiso 1 1 calc R . .
H17C H 0.8174 1.2724 0.0256 0.185 Uiso 1 1 calc R . .
C11 C 0.7228(2) 0.9919(3) -0.05704(19) 0.0408(7) Uani 1 1 d D . .
S1' S 0.8517(4) 0.9931(5) -0.0827(3) 0.0550(9) Uani 0.471(4) 1 d PDU A 1
C12' C 0.6541(15) 1.0805(16) -0.0905(16) 0.073(5) Uani 0.471(4) 1 d PDU A 1
H12' H 0.5824 1.0924 -0.0794 0.088 Uiso 0.471(4) 1 calc PR A 1
C13' C 0.7086(15) 1.154(2) -0.1465(17) 0.069(4) Uani 0.471(4) 1 d PDU A 1
H13' H 0.6782 1.2174 -0.1769 0.083 Uiso 0.471(4) 1 calc PR A 1
C14' C 0.8128(17) 1.1090(17) -0.1434(15) 0.054(3) Uani 0.471(4) 1 d PDU A 1
H14' H 0.8623 1.1416 -0.1744 0.065 Uiso 0.471(4) 1 calc PR A 1
S1 S 0.6308(4) 1.0925(5) -0.1018(4) 0.0707(12) Uani 0.529(4) 1 d PDU A 2
C12 C 0.8222(10) 1.0026(18) -0.0858(12) 0.072(5) Uani 0.529(4) 1 d PDU A 2
H12 H 0.8807 0.9517 -0.0699 0.086 Uiso 0.529(4) 1 calc PR A 2
C13 C 0.8325(16) 1.0987(17) -0.1432(16) 0.062(3) Uani 0.529(4) 1 d PDU A 2
H13 H 0.8942 1.1207 -0.1664 0.074 Uiso 0.529(4) 1 calc PR A 2
C14 C 0.7296(12) 1.1464(19) -0.1533(15) 0.060(3) Uani 0.529(4) 1 d PDU A 2
H14 H 0.7129 1.2089 -0.1886 0.072 Uiso 0.529(4) 1 calc PR A 2
C18 C 0.8130(3) 0.7231(3) 0.14620(19) 0.0448(8) Uani 1 1 d D . .
S2 S 0.8058(3) 0.5957(2) 0.1929(2) 0.0788(10) Uani 0.633(5) 1 d PDU B 1
C19 C 0.9074(11) 0.7381(13) 0.1097(12) 0.065(4) Uani 0.633(5) 1 d PDU B 1
H19 H 0.9267 0.8030 0.0827 0.078 Uiso 0.633(5) 1 calc PR B 1
C20 C 0.9724(10) 0.6298(8) 0.1220(8) 0.067(2) Uani 0.633(5) 1 d PDU B 1
H20 H 1.0377 0.6190 0.1001 0.081 Uiso 0.633(5) 1 calc PR B 1
C21 C 0.9295(7) 0.5468(11) 0.1679(8) 0.077(2) Uani 0.633(5) 1 d PDU B 1
H21 H 0.9619 0.4765 0.1826 0.093 Uiso 0.633(5) 1 calc PR B 1
S2' S 0.9240(7) 0.7245(7) 0.0999(7) 0.084(2) Uani 0.367(5) 1 d PDU B 2
C19' C 0.795(2) 0.6208(14) 0.1853(19) 0.110(7) Uani 0.367(5) 1 d PDU B 2
H19' H 0.7358 0.6016 0.2126 0.132 Uiso 0.367(5) 1 calc PR B 2
C20' C 0.8927(18) 0.549(3) 0.1726(18) 0.099(5) Uani 0.367(5) 1 d PDU B 2
H20' H 0.9004 0.4766 0.1950 0.119 Uiso 0.367(5) 1 calc PR B 2
C21' C 0.973(2) 0.5911(13) 0.1276(19) 0.099(6) Uani 0.367(5) 1 d PDU B 2
H21' H 1.0365 0.5553 0.1157 0.119 Uiso 0.367(5) 1 calc PR B 2
O1 O 0.5657(2) 0.7135(2) 0.17142(14) 0.0627(7) Uani 1 1 d . . .
O2 O 0.9203(2) 0.9858(2) 0.14861(17) 0.0692(8) Uani 1 1 d . . .
O3 O 0.7748(2) 1.1019(2) 0.11081(16) 0.0622(7) 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
C7 O1 1.212(4) . ?
C7 C6 1.473(4) . ?
C7 C8 1.544(4) . ?
C6 C5 1.390(4) . ?
C6 C1 1.397(4) . ?
C5 C4 1.377(5) . ?
C5 H5 0.9300 . ?
C4 C3 1.375(5) . ?
C4 H4 0.9300 . ?
C3 C2 1.375(5) . ?
C3 H3 0.9300 . ?
C2 C1 1.395(4) . ?
C2 H2 0.9300 . ?
C1 C10 1.476(4) . ?
C10 C9 1.341(4) . ?
C10 C11 1.476(4) . ?
C9 C15 1.497(4) . ?
C9 C8 1.524(4) . ?
C8 C18 1.523(4) . ?
C8 C22 1.536(4) . ?
C22 C27 1.395(5) . ?
C22 C23 1.427(4) . ?
C23 C24 1.368(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.335(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.346(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.361(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C15 O2 1.192(4) . ?
C15 O3 1.328(4) . ?
C16 C17 1.437(6) . ?
C16 O3 1.459(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C11 C12 1.371(9) . ?
C11 C12' 1.385(9) . ?
C11 S1' 1.686(4) . ?
C11 S1 1.700(4) . ?
S1' C14' 1.698(9) . ?
C12' C13' 1.487(10) . ?
C12' H12' 0.9300 . ?
C13' C14' 1.365(9) . ?
C13' H13' 0.9300 . ?
C14' H14' 0.9300 . ?
S1 C14 1.696(8) . ?
C12 C13 1.481(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.353(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C18 C19 1.387(9) . ?
C18 C19' 1.397(10) . ?
C18 S2' 1.648(6) . ?
C18 S2 1.690(4) . ?
S2 C21 1.720(7) . ?
C19 C20 1.496(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.382(8) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
S2' C21' 1.713(9) . ?
C19' C20' 1.500(10) . ?
C19' H19' 0.9300 . ?
C20' C21' 1.397(10) . ?
C20' H20' 0.9300 . ?
C21' H21' 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
O1 C7 C6 122.3(3) . . ?
O1 C7 C8 120.5(3) . . ?
C6 C7 C8 117.1(3) . . ?
C5 C6 C1 120.2(3) . . ?
C5 C6 C7 119.2(3) . . ?
C1 C6 C7 120.6(3) . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C2 C3 C4 120.9(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C1 C6 118.4(3) . . ?
C2 C1 C10 122.0(3) . . ?
C6 C1 C10 119.5(3) . . ?
C9 C10 C11 120.3(3) . . ?
C9 C10 C1 120.9(3) . . ?
C11 C10 C1 118.7(2) . . ?
C10 C9 C15 121.2(3) . . ?
C10 C9 C8 123.0(3) . . ?
C15 C9 C8 115.7(2) . . ?
C18 C8 C9 109.6(2) . . ?
C18 C8 C22 113.7(2) . . ?
C9 C8 C22 109.8(2) . . ?
C18 C8 C7 102.9(2) . . ?
C9 C8 C7 110.9(2) . . ?
C22 C8 C7 109.8(2) . . ?
C27 C22 C23 117.6(3) . . ?
C27 C22 C8 118.1(3) . . ?
C23 C22 C8 124.3(3) . . ?
C24 C23 C22 117.8(4) . . ?
C24 C23 H23 121.1 . . ?
C22 C23 H23 121.1 . . ?
C25 C24 C23 122.7(4) . . ?
C25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C24 C25 C26 120.7(4) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C27 120.1(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C22 121.2(4) . . ?
C26 C27 H27 119.4 . . ?
C22 C27 H27 119.4 . . ?
O2 C15 O3 124.6(3) . . ?
O2 C15 C9 124.1(3) . . ?
O3 C15 C9 111.3(3) . . ?
C17 C16 O3 110.7(4) . . ?
C17 C16 H16A 109.5 . . ?
O3 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C11 C12' 107.7(12) . . ?
C12 C11 C10 126.8(8) . . ?
C12' C11 C10 125.4(9) . . ?
C12' C11 S1' 114.7(8) . . ?
C10 C11 S1' 119.7(3) . . ?
C12 C11 S1 110.1(7) . . ?
C10 C11 S1 123.1(3) . . ?
S1' C11 S1 117.3(3) . . ?
C11 S1' C14' 88.4(8) . . ?
C11 C12' C13' 112.1(17) . . ?
C11 C12' H12' 123.9 . . ?
C13' C12' H12' 123.9 . . ?
C14' C13' C12' 105(2) . . ?
C14' C13' H13' 127.6 . . ?
C12' C13' H13' 127.6 . . ?
C13' C14' S1' 119.9(16) . . ?
C13' C14' H14' 120.1 . . ?
S1' C14' H14' 120.1 . . ?
C14 S1 C11 90.1(8) . . ?
C11 C12 C13 117.2(15) . . ?
C11 C12 H12 121.4 . . ?
C13 C12 H12 121.4 . . ?
C14 C13 C12 102.5(18) . . ?
C14 C13 H13 128.8 . . ?
C12 C13 H13 128.8 . . ?
C13 C14 S1 120.1(16) . . ?
C13 C14 H14 119.9 . . ?
S1 C14 H14 120.0 . . ?
C19 C18 C19' 120.6(10) . . ?
C19 C18 C8 122.0(6) . . ?
C19' C18 C8 117.3(9) . . ?
C19' C18 S2' 114.8(9) . . ?
C8 C18 S2' 127.8(4) . . ?
C19 C18 S2 114.4(6) . . ?
C8 C18 S2 123.5(3) . . ?
S2' C18 S2 108.6(4) . . ?
C18 S2 C21 94.5(5) . . ?
C18 C19 C20 106.9(10) . . ?
C18 C19 H19 126.6 . . ?
C20 C19 H19 126.6 . . ?
C21 C20 C19 115.9(11) . . ?
C21 C20 H20 122.0 . . ?
C19 C20 H20 122.0 . . ?
C20 C21 S2 108.2(10) . . ?
C20 C21 H21 125.9 . . ?
S2 C21 H21 125.9 . . ?
C18 S2' C21' 98.3(11) . . ?
C18 C19' C20' 103.3(18) . . ?
C18 C19' H19' 128.3 . . ?
C20' C19' H19' 128.3 . . ?
C21' C20' C19' 121(2) . . ?
C21' C20' H20' 119.6 . . ?
C19' C20' H20' 119.6 . . ?
C20' C21' S2' 103(2) . . ?
C20' C21' H21' 128.7 . . ?
S2' C21' H21' 128.7 . . ?
C15 O3 C16 117.2(3) . . ?

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
O1 C7 C6 C5 -16.1(5) . . . . ?
C8 C7 C6 C5 160.0(3) . . . . ?
O1 C7 C6 C1 162.8(3) . . . . ?
C8 C7 C6 C1 -21.1(4) . . . . ?
C1 C6 C5 C4 0.9(5) . . . . ?
C7 C6 C5 C4 179.8(3) . . . . ?
C6 C5 C4 C3 -0.5(5) . . . . ?
C5 C4 C3 C2 -0.2(6) . . . . ?
C4 C3 C2 C1 0.4(5) . . . . ?
C3 C2 C1 C6 0.0(5) . . . . ?
C3 C2 C1 C10 -178.5(3) . . . . ?
C5 C6 C1 C2 -0.7(4) . . . . ?
C7 C6 C1 C2 -179.6(3) . . . . ?
C5 C6 C1 C10 177.8(3) . . . . ?
C7 C6 C1 C10 -1.0(4) . . . . ?
C2 C1 C10 C9 -171.3(3) . . . . ?
C6 C1 C10 C9 10.3(4) . . . . ?
C2 C1 C10 C11 7.2(4) . . . . ?
C6 C1 C10 C11 -171.2(3) . . . . ?
C11 C10 C9 C15 3.0(4) . . . . ?
C1 C10 C9 C15 -178.6(3) . . . . ?
C11 C10 C9 C8 -174.3(3) . . . . ?
C1 C10 C9 C8 4.2(4) . . . . ?
C10 C9 C8 C18 88.2(3) . . . . ?
C15 C9 C8 C18 -89.2(3) . . . . ?
C10 C9 C8 C22 -146.3(3) . . . . ?
C15 C9 C8 C22 36.3(3) . . . . ?
C10 C9 C8 C7 -24.7(4) . . . . ?
C15 C9 C8 C7 157.9(3) . . . . ?
O1 C7 C8 C18 91.3(3) . . . . ?
C6 C7 C8 C18 -84.9(3) . . . . ?
O1 C7 C8 C9 -151.7(3) . . . . ?
C6 C7 C8 C9 32.1(4) . . . . ?
O1 C7 C8 C22 -30.1(4) . . . . ?
C6 C7 C8 C22 153.7(3) . . . . ?
C18 C8 C22 C27 178.5(3) . . . . ?
C9 C8 C22 C27 55.3(4) . . . . ?
C7 C8 C22 C27 -66.9(4) . . . . ?
C18 C8 C22 C23 0.1(4) . . . . ?
C9 C8 C22 C23 -123.0(3) . . . . ?
C7 C8 C22 C23 114.8(3) . . . . ?
C27 C22 C23 C24 -0.1(5) . . . . ?
C8 C22 C23 C24 178.2(3) . . . . ?
C22 C23 C24 C25 0.3(6) . . . . ?
C23 C24 C25 C26 0.2(7) . . . . ?
C24 C25 C26 C27 -0.9(7) . . . . ?
C25 C26 C27 C22 1.1(6) . . . . ?
C23 C22 C27 C26 -0.6(5) . . . . ?
C8 C22 C27 C26 -179.0(3) . . . . ?
C10 C9 C15 O2 -119.3(4) . . . . ?
C8 C9 C15 O2 58.2(4) . . . . ?
C10 C9 C15 O3 62.5(4) . . . . ?
C8 C9 C15 O3 -120.1(3) . . . . ?
C9 C10 C11 C12 69.2(13) . . . . ?
C1 C10 C11 C12 -109.3(12) . . . . ?
C9 C10 C11 C12' -106.8(15) . . . . ?
C1 C10 C11 C12' 74.7(15) . . . . ?
C9 C10 C11 S1' 67.6(4) . . . . ?
C1 C10 C11 S1' -111.0(4) . . . . ?
C9 C10 C11 S1 -111.7(4) . . . . ?
C1 C10 C11 S1 69.7(5) . . . . ?
C12 C11 S1' C14' 13(9) . . . . ?
C12' C11 S1' C14' -2.9(18) . . . . ?
C10 C11 S1' C14' -177.9(10) . . . . ?
S1 C11 S1' C14' 1.5(11) . . . . ?
C12 C11 C12' C13' 1(3) . . . . ?
C10 C11 C12' C13' 177.9(17) . . . . ?
S1' C11 C12' C13' 3(3) . . . . ?
S1 C11 C12' C13' -121(16) . . . . ?
C11 C12' C13' C14' -2(3) . . . . ?
C12' C13' C14' S1' 0(3) . . . . ?
C11 S1' C14' C13' 2(2) . . . . ?
C12 C11 S1 C14 -1.9(16) . . . . ?
C12' C11 S1 C14 58(14) . . . . ?
C10 C11 S1 C14 178.9(10) . . . . ?
S1' C11 S1 C14 -0.4(12) . . . . ?
C12' C11 C12 C13 -1(3) . . . . ?
C10 C11 C12 C13 -177.5(17) . . . . ?
S1' C11 C12 C13 -166(11) . . . . ?
S1 C11 C12 C13 3(3) . . . . ?
C11 C12 C13 C14 -3(3) . . . . ?
C12 C13 C14 S1 2(3) . . . . ?
C11 S1 C14 C13 0(2) . . . . ?
C9 C8 C18 C19 15.8(11) . . . . ?
C22 C8 C18 C19 -107.5(11) . . . . ?
C7 C8 C18 C19 133.8(11) . . . . ?
C9 C8 C18 C19' -165.8(16) . . . . ?
C22 C8 C18 C19' 70.9(16) . . . . ?
C7 C8 C18 C19' -47.8(16) . . . . ?
C9 C8 C18 S2' 11.2(6) . . . . ?
C22 C8 C18 S2' -112.1(6) . . . . ?
C7 C8 C18 S2' 129.2(6) . . . . ?
C9 C8 C18 S2 -167.7(3) . . . . ?
C22 C8 C18 S2 69.1(4) . . . . ?
C7 C8 C18 S2 -49.7(3) . . . . ?
C19 C18 S2 C21 -0.4(11) . . . . ?
C19' C18 S2 C21 168(14) . . . . ?
C8 C18 S2 C21 -177.2(5) . . . . ?
S2' C18 S2 C21 3.8(6) . . . . ?
C19' C18 C19 C20 0(2) . . . . ?
C8 C18 C19 C20 178.7(8) . . . . ?
S2' C18 C19 C20 -33(9) . . . . ?
S2 C18 C19 C20 1.9(16) . . . . ?
C18 C19 C20 C21 -3.1(19) . . . . ?
C19 C20 C21 S2 2.8(15) . . . . ?
C18 S2 C21 C20 -1.4(9) . . . . ?
C19 C18 S2' C21' 146(10) . . . . ?
C19' C18 S2' C21' -3(2) . . . . ?
C8 C18 S2' C21' -179.9(11) . . . . ?
S2 C18 S2' C21' -0.9(12) . . . . ?
C19 C18 C19' C20' -1(3) . . . . ?
C8 C18 C19' C20' -179.8(15) . . . . ?
S2' C18 C19' C20' 3(3) . . . . ?
S2 C18 C19' C20' -14(12) . . . . ?
C18 C19' C20' C21' -2(4) . . . . ?
C19' C20' C21' S2' 0(4) . . . . ?
C18 S2' C21' C20' 1(2) . . . . ?
O2 C15 O3 C16 3.7(5) . . . . ?
C9 C15 O3 C16 -178.1(3) . . . . ?
C17 C16 O3 C15 96.7(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.39
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.047
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_final
_database_code_depnum_ccdc_archive 'CCDC 1438503'
_audit_update_record             
;
2015-11-24 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'2,3-dimethyl 1-oxo-2(pyren-4-yl)-4-(thiophen-2-yl)-1,2-dihydronaphthalene-2,3-dicarboxylate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H22 O5 S'
_chemical_formula_sum            'C34 H22 O5 S'
_chemical_formula_weight         542.58

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'
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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.9268(10)
_cell_length_b                   18.9670(14)
_cell_length_c                   12.2628(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.030(2)
_cell_angle_gamma                90.00
_cell_volume                     2537.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4457
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   multi_scan
_exptl_absorpt_correction_T_min  0.9580
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_process_details   'SADABS (Bruker, 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 Kappa ApexII CCD Diffractometer'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21576
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4457
_reflns_number_gt                3341
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0388P)²+1.1902P] 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         4457
_refine_ls_number_parameters     409
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_iucr_refine_instruction_details 
;
TITL GOP1 in P2(1)/n
CELL  0.71073  10.9268  18.9670  12.2628   90.000   93.030   90.000
ZERR     4.00   0.0010   0.0014   0.0009    0.000    0.002    0.000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    O    S
UNIT  136  88   20   4
MERG   2
OMIT -2 50
SADI 0.01 C11 C12 C11' C12'
SADI 0.01 C12 C13 C12' C13'
SADI 0.01 C13 C14 C13' C14'
DFIX 1.71 0.01 C14 S1 C14' S1'
DFIX 1.71 0.01 C11 S1 C11' S1'
SIMU 0.02 S1 > C14'
DELU 0.02 S1 > C14
DELU 0.02 S1' > C14'
FMAP   2
PLAN   20
SIZE     0.20   0.25   0.25
ACTA
BOND   $H
CONF
L.S.   12
TEMP    23.00
WGHT    0.038800    1.190200
FVAR       0.14479   0.69063
C1    1    0.968280    0.110668    0.901640    11.00000    0.03794    0.03184 =
         0.02682    0.00451    0.00686    0.00018
C2    1    1.070800    0.117140    0.973699    11.00000    0.04011    0.04791 =
         0.03666   -0.00004    0.00282    0.00046
AFIX  43
H2    2    1.139574    0.089502    0.963555    11.00000   -1.20000
AFIX   0
C3    1    1.071557    0.163903    1.059663    11.00000    0.05171    0.05497 =
         0.03601   -0.00168   -0.00262   -0.00841
AFIX  43
H3    2    1.139905    0.166425    1.108024    11.00000   -1.20000
AFIX   0
C4    1    0.973055    0.206717    1.074869    11.00000    0.06718    0.04602 =
         0.03628   -0.00811    0.00431   -0.00520
AFIX  43
H4    2    0.973837    0.237446    1.134000    11.00000   -1.20000
AFIX   0
C5    1    0.873127    0.204013    1.002307    11.00000    0.05764    0.03862 =
         0.03963   -0.00506    0.00803    0.00691
AFIX  43
H5    2    0.807671    0.234530    1.010681    11.00000   -1.20000
AFIX   0
C6    1    0.868825    0.156029    0.916305    11.00000    0.04358    0.03113 =
         0.03101    0.00086    0.00557    0.00201
C7    1    0.762641    0.155499    0.837930    11.00000    0.04191    0.03635 =
         0.03528    0.00097    0.00850    0.00933
C8    1    0.738437    0.086946    0.772122    11.00000    0.03183    0.03460 =
         0.03024    0.00181    0.00586    0.00469
C9    1    0.855838    0.045103    0.754987    11.00000    0.03520    0.02874 =
         0.02556    0.00490    0.00699    0.00423
C10   1    0.961607    0.058053    0.812659    11.00000    0.03307    0.02999 =
         0.02641    0.00452    0.00638    0.00289
C15   1    0.658963    0.044755    0.849909    11.00000    0.03698    0.04586 =
         0.03531    0.00356    0.00800    0.00588
C16   1    0.609106   -0.066276    0.918145    11.00000    0.05916    0.05648 =
         0.06465    0.01451    0.01996   -0.01050
AFIX 137
H16A  2    0.623729   -0.049692    0.991644    11.00000   -1.50000
H16B  2    0.634884   -0.114520    0.913491    11.00000   -1.50000
H16C  2    0.523231   -0.062938    0.897879    11.00000   -1.50000
AFIX   0
C17   1    0.846157   -0.013562    0.672626    11.00000    0.03464    0.03714 =
         0.03480   -0.00136    0.00565    0.00431
C18   1    0.908742   -0.129594    0.635952    11.00000    0.07838    0.04020 =
         0.07468   -0.01834    0.01181    0.01041
AFIX 137
H18A  2    0.831829   -0.140221    0.598055    11.00000   -1.50000
H18B  2    0.938700   -0.170765    0.674279    11.00000   -1.50000
H18C  2    0.966899   -0.115229    0.584312    11.00000   -1.50000
AFIX   0
C19   1    0.664770    0.103263    0.665002    11.00000    0.03150    0.03026 =
         0.03446    0.00093    0.00242    0.00464
C20   1    0.550016    0.074428    0.642389    11.00000    0.03458    0.03689 =
         0.04882    0.00529    0.00490   -0.00145
AFIX  43
H20   2    0.515983    0.045665    0.694221    11.00000   -1.20000
AFIX   0
C21   1    0.484718    0.087116    0.545247    11.00000    0.02786    0.03972 =
         0.05657   -0.00088   -0.00377   -0.00315
AFIX  43
H21   2    0.408492    0.066044    0.532227    11.00000   -1.20000
AFIX   0
C22   1    0.530647    0.130697    0.466699    11.00000    0.02978    0.03103 =
         0.04350   -0.00293   -0.00368    0.00268
C23   1    0.464342    0.145896    0.365247    11.00000    0.03461    0.04800 =
         0.05306   -0.00512   -0.01376    0.00059
AFIX  43
H23   2    0.389750    0.123609    0.349163    11.00000   -1.20000
AFIX   0
C24   1    0.507235    0.191140    0.293766    11.00000    0.04876    0.05010 =
         0.04058   -0.00016   -0.01589    0.00823
AFIX  43
H24   2    0.460594    0.200563    0.229789    11.00000   -1.20000
AFIX   0
C25   1    0.622625    0.225753    0.312024    11.00000    0.04113    0.03847 =
         0.03463   -0.00143   -0.00487    0.00903
C26   1    0.668809    0.274330    0.239836    11.00000    0.05783    0.05527 =
         0.03445    0.00911   -0.00269    0.01111
AFIX  43
H26   2    0.622873    0.285500    0.176171    11.00000   -1.20000
AFIX   0
C27   1    0.780619    0.306243    0.260207    11.00000    0.05582    0.05330 =
         0.04373    0.01479    0.00984    0.00388
AFIX  43
H27   2    0.808528    0.338991    0.210833    11.00000   -1.20000
AFIX   0
C28   1    0.851687    0.290253    0.352869    11.00000    0.03935    0.04538 =
         0.04320    0.00277    0.00641   -0.00028
AFIX  43
H28   2    0.927926    0.311455    0.365074    11.00000   -1.20000
AFIX   0
C29   1    0.809348    0.242050    0.428911    11.00000    0.03440    0.03226 =
         0.03316    0.00029    0.00318    0.00484
C30   1    0.878088    0.224449    0.527085    11.00000    0.02832    0.03942 =
         0.04167   -0.00204   -0.00071   -0.00364
AFIX  43
H30   2    0.955726    0.243808    0.539827    11.00000   -1.20000
AFIX   0
C31   1    0.834059    0.180654    0.601932    11.00000    0.03301    0.03655 =
         0.03336    0.00136   -0.00529    0.00004
AFIX  43
H31   2    0.881795    0.171201    0.665283    11.00000   -1.20000
AFIX   0
C32   1    0.715885    0.148079    0.587167    11.00000    0.02973    0.02699 =
         0.03327   -0.00114    0.00017    0.00351
C33   1    0.647201    0.162426    0.487838    11.00000    0.02984    0.02714 =
         0.03409   -0.00363   -0.00271    0.00563
C34   1    0.693786    0.209662    0.409346    11.00000    0.03340    0.02901 =
         0.03156   -0.00333    0.00020    0.00648
O1    3    0.691955    0.204587    0.827535    11.00000    0.06295    0.04570 =
         0.06334   -0.00936   -0.00828    0.02593
O2    3    0.589429    0.071614    0.908955    11.00000    0.09103    0.06207 =
         0.08760    0.00725    0.06162    0.01525
O3    3    0.677680   -0.023569    0.844888    11.00000    0.05432    0.03865 =
         0.05661    0.00744    0.02493    0.00068
O4    3    0.800192   -0.008238    0.582329    11.00000    0.08685    0.06561 =
         0.04059   -0.01602   -0.01605    0.02923
O5    3    0.891927   -0.073398    0.712827    11.00000    0.05907    0.02978 =
         0.04490   -0.00164    0.00693    0.00498
PART    1
S1    4    1.123234    0.028835    0.654816    21.00000    0.04679    0.04388 =
         0.04181   -0.00491    0.02110    0.00023
C11   1    1.076335    0.020256    0.784565    21.00000    0.02723    0.03512 =
         0.03701   -0.00187    0.01037    0.00667
C12   1    1.146706   -0.025473    0.844306    21.00000    0.05374    0.06907 =
         0.06758   -0.00311    0.01019    0.00439
AFIX  43
H12   2    1.132584   -0.036546    0.916445    21.00000   -1.20000
AFIX   0
C13   1    1.244538   -0.055340    0.787315    21.00000    0.04082    0.04884 =
         0.07857    0.00292    0.00315    0.01214
AFIX  43
H13   2    1.301551   -0.087750    0.815792    21.00000   -1.20000
AFIX   0
C14   1    1.240671   -0.029033    0.686262    21.00000    0.04508    0.05030 =
         0.06819   -0.00938    0.02645    0.00987
AFIX  43
H14   2    1.297938   -0.041265    0.636072    21.00000   -1.20000
AFIX   0
PART    2
S1'   4    1.157783   -0.032253    0.868531   -21.00000    0.04540    0.04933 =
         0.05834    0.00601   -0.00099    0.01573
C11'  1    1.071316    0.023607    0.785282   -21.00000    0.04573    0.02858 =
         0.03111    0.00819   -0.00732   -0.00754
C12'  1    1.131453    0.026641    0.691894   -21.00000    0.08494    0.05667 =
         0.05195    0.00495    0.00192    0.00758
AFIX  43
H12'  2    1.106839    0.060671    0.640719   -21.00000   -1.20000
AFIX   0
C13'  1    1.229765   -0.018581    0.666415   -21.00000    0.05147    0.05632 =
         0.05096    0.00779    0.00675   -0.00977
AFIX  43
H13'  2    1.267579   -0.025257    0.601019   -21.00000   -1.20000
AFIX   0
C14'  1    1.251836   -0.048630    0.763913   -21.00000    0.04339    0.05852 =
         0.06173    0.00196    0.00308    0.01571
AFIX  43
H14'  2    1.318640   -0.078628    0.775141   -21.00000   -1.20000
HKLF    4
 
REM  GOP1 in P2(1)/n
REM R1 =  0.0387 for   3341 Fo > 4sig(Fo)  and  0.0611 for all   4457 data
REM    409 parameters refined using    147 restraints
 
END
;

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 0.96828(18) 0.11067(10) 0.90164(15) 0.0320(4) Uani 1 1 d . A .
C2 C 1.0708(2) 0.11714(11) 0.97370(16) 0.0415(5) Uani 1 1 d . . .
H2 H 1.1396 0.0895 0.9636 0.050 Uiso 1 1 calc R . .
C3 C 1.0716(2) 0.16390(12) 1.05966(17) 0.0477(6) Uani 1 1 d . . .
H3 H 1.1399 0.1664 1.1080 0.057 Uiso 1 1 calc R . .
C4 C 0.9731(2) 0.20672(12) 1.07487(17) 0.0498(6) Uani 1 1 d . . .
H4 H 0.9738 0.2374 1.1340 0.060 Uiso 1 1 calc R . .
C5 C 0.8731(2) 0.20401(11) 1.00231(17) 0.0451(5) Uani 1 1 d . . .
H5 H 0.8077 0.2345 1.0107 0.054 Uiso 1 1 calc R . .
C6 C 0.86883(19) 0.15603(10) 0.91630(15) 0.0351(5) Uani 1 1 d . . .
C7 C 0.76264(19) 0.15550(11) 0.83793(16) 0.0376(5) Uani 1 1 d . . .
C8 C 0.73844(17) 0.08695(10) 0.77212(15) 0.0321(4) Uani 1 1 d . . .
C9 C 0.85584(18) 0.04510(9) 0.75499(14) 0.0296(4) Uani 1 1 d . A .
C10 C 0.96161(18) 0.05805(9) 0.81266(14) 0.0297(4) Uani 1 1 d . . .
C15 C 0.65896(19) 0.04476(11) 0.84991(16) 0.0392(5) Uani 1 1 d . . .
C16 C 0.6091(2) -0.06628(13) 0.9181(2) 0.0595(7) Uani 1 1 d . . .
H16A H 0.6237 -0.0497 0.9916 0.089 Uiso 1 1 calc R . .
H16B H 0.6349 -0.1145 0.9135 0.089 Uiso 1 1 calc R . .
H16C H 0.5232 -0.0629 0.8979 0.089 Uiso 1 1 calc R . .
C17 C 0.84616(18) -0.01356(10) 0.67263(16) 0.0354(5) Uani 1 1 d . . .
C18 C 0.9087(3) -0.12959(12) 0.6360(2) 0.0641(7) Uani 1 1 d . . .
H18A H 0.8318 -0.1402 0.5981 0.096 Uiso 1 1 calc R A .
H18B H 0.9387 -0.1708 0.6743 0.096 Uiso 1 1 calc R . .
H18C H 0.9669 -0.1152 0.5843 0.096 Uiso 1 1 calc R . .
C19 C 0.66477(17) 0.10326(10) 0.66500(15) 0.0320(4) Uani 1 1 d . . .
C20 C 0.55002(18) 0.07443(11) 0.64239(17) 0.0400(5) Uani 1 1 d . . .
H20 H 0.5160 0.0457 0.6942 0.048 Uiso 1 1 calc R . .
C21 C 0.48472(19) 0.08712(11) 0.54525(18) 0.0416(5) Uani 1 1 d . . .
H21 H 0.4085 0.0660 0.5322 0.050 Uiso 1 1 calc R . .
C22 C 0.53065(18) 0.13070(10) 0.46670(16) 0.0350(5) Uani 1 1 d . . .
C23 C 0.4643(2) 0.14590(12) 0.36525(18) 0.0458(5) Uani 1 1 d . . .
H23 H 0.3898 0.1236 0.3492 0.055 Uiso 1 1 calc R . .
C24 C 0.5072(2) 0.19114(12) 0.29377(18) 0.0471(6) Uani 1 1 d . . .
H24 H 0.4606 0.2006 0.2298 0.057 Uiso 1 1 calc R . .
C25 C 0.62262(19) 0.22575(10) 0.31202(16) 0.0383(5) Uani 1 1 d . . .
C26 C 0.6688(2) 0.27433(12) 0.23984(17) 0.0494(6) Uani 1 1 d . . .
H26 H 0.6229 0.2855 0.1762 0.059 Uiso 1 1 calc R . .
C27 C 0.7806(2) 0.30624(12) 0.26021(18) 0.0507(6) Uani 1 1 d . . .
H27 H 0.8085 0.3390 0.2108 0.061 Uiso 1 1 calc R . .
C28 C 0.8517(2) 0.29025(11) 0.35287(17) 0.0425(5) Uani 1 1 d . . .
H28 H 0.9279 0.3115 0.3651 0.051 Uiso 1 1 calc R . .
C29 C 0.80935(18) 0.24205(10) 0.42891(15) 0.0332(4) Uani 1 1 d . . .
C30 C 0.87809(18) 0.22445(10) 0.52708(16) 0.0366(5) Uani 1 1 d . . .
H30 H 0.9557 0.2438 0.5398 0.044 Uiso 1 1 calc R . .
C31 C 0.83406(18) 0.18065(10) 0.60193(16) 0.0346(5) Uani 1 1 d . . .
H31 H 0.8818 0.1712 0.6653 0.041 Uiso 1 1 calc R . .
C32 C 0.71588(17) 0.14808(9) 0.58717(15) 0.0301(4) Uani 1 1 d . . .
C33 C 0.64720(17) 0.16243(9) 0.48784(15) 0.0305(4) Uani 1 1 d . . .
C34 C 0.69379(17) 0.20966(10) 0.40935(15) 0.0314(4) Uani 1 1 d . . .
O1 O 0.69195(15) 0.20459(8) 0.82754(13) 0.0577(5) Uani 1 1 d . . .
O2 O 0.58943(18) 0.07161(9) 0.90895(16) 0.0782(6) Uani 1 1 d . . .
O3 O 0.67768(14) -0.02357(7) 0.84489(12) 0.0491(4) Uani 1 1 d . . .
O4 O 0.80019(18) -0.00824(9) 0.58233(13) 0.0650(5) Uani 1 1 d . A .
O5 O 0.89193(14) -0.07340(7) 0.71283(11) 0.0444(4) Uani 1 1 d . A .
S1 S 1.12323(15) 0.02883(10) 0.65482(12) 0.0435(4) Uani 0.691(3) 1 d PDU A 1
C11 C 1.0763(11) 0.0203(8) 0.7846(7) 0.033(2) Uani 0.691(3) 1 d PDU A 1
C12 C 1.1467(13) -0.0255(7) 0.8443(10) 0.063(3) Uani 0.691(3) 1 d PDU A 1
H12 H 1.1326 -0.0365 0.9164 0.076 Uiso 0.691(3) 1 calc PR A 1
C13 C 1.2445(14) -0.0553(8) 0.7873(9) 0.0561(18) Uani 0.691(3) 1 d PDU A 1
H13 H 1.3016 -0.0877 0.8158 0.067 Uiso 0.691(3) 1 calc PR A 1
C14 C 1.2407(10) -0.0290(6) 0.6863(9) 0.054(2) Uani 0.691(3) 1 d PDU A 1
H14 H 1.2979 -0.0413 0.6361 0.064 Uiso 0.691(3) 1 calc PR A 1
S1' S 1.1578(8) -0.0323(4) 0.8685(6) 0.0512(11) Uani 0.309(3) 1 d PDU A 2
C11' C 1.071(2) 0.0236(17) 0.7853(15) 0.035(5) Uani 0.309(3) 1 d PDU A 2
C12' C 1.1315(17) 0.0266(11) 0.6919(11) 0.065(4) Uani 0.309(3) 1 d PDU A 2
H12' H 1.1068 0.0607 0.6407 0.077 Uiso 0.309(3) 1 calc PR A 2
C13' C 1.230(2) -0.0186(15) 0.666(2) 0.053(3) Uani 0.309(3) 1 d PDU A 2
H13' H 1.2676 -0.0253 0.6010 0.063 Uiso 0.309(3) 1 calc PR A 2
C14' C 1.252(3) -0.049(2) 0.7639(19) 0.055(4) Uani 0.309(3) 1 d PDU A 2
H14' H 1.3186 -0.0786 0.7751 0.065 Uiso 0.309(3) 1 calc PR A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.395(3) . ?
C1 C6 1.405(3) . ?
C1 C10 1.478(3) . ?
C2 C3 1.377(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.467(3) . ?
C7 O1 1.212(2) . ?
C7 C8 1.546(3) . ?
C8 C9 1.532(3) . ?
C8 C19 1.535(3) . ?
C8 C15 1.547(3) . ?
C9 C10 1.345(3) . ?
C9 C17 1.503(3) . ?
C10 C11' 1.421(16) . ?
C10 C11 1.500(6) . ?
C15 O2 1.191(2) . ?
C15 O3 1.314(2) . ?
C16 O3 1.448(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O4 1.196(2) . ?
C17 O5 1.325(2) . ?
C18 O5 1.441(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.383(3) . ?
C19 C32 1.415(3) . ?
C20 C21 1.377(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.383(3) . ?
C21 H21 0.9300 . ?
C22 C33 1.420(3) . ?
C22 C23 1.435(3) . ?
C23 C24 1.330(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.429(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(3) . ?
C25 C34 1.423(3) . ?
C26 C27 1.374(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.376(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.402(3) . ?
C28 H28 0.9300 . ?
C29 C34 1.413(3) . ?
C29 C30 1.425(3) . ?
C30 C31 1.346(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.434(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.423(3) . ?
C33 C34 1.428(3) . ?
S1 C11 1.705(6) . ?
S1 C14 1.717(6) . ?
C11 C12 1.349(10) . ?
C12 C13 1.425(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.334(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
S1' C14' 1.714(10) . ?
S1' C11' 1.719(10) . ?
C11' C12' 1.351(13) . ?
C12' C13' 1.422(14) . ?
C12' H12' 0.9300 . ?
C13' C14' 1.335(9) . ?
C13' H13' 0.9300 . ?
C14' H14' 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
C2 C1 C6 117.75(18) . . ?
C2 C1 C10 122.26(18) . . ?
C6 C1 C10 119.98(18) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C4 C3 C2 120.9(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.6(2) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 120.6(2) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 120.13(19) . . ?
C5 C6 C7 119.65(18) . . ?
C1 C6 C7 120.15(17) . . ?
O1 C7 C6 122.76(19) . . ?
O1 C7 C8 120.05(19) . . ?
C6 C7 C8 117.09(16) . . ?
C9 C8 C19 113.07(15) . . ?
C9 C8 C7 112.70(16) . . ?
C19 C8 C7 110.16(15) . . ?
C9 C8 C15 108.54(15) . . ?
C19 C8 C15 110.24(16) . . ?
C7 C8 C15 101.50(15) . . ?
C10 C9 C17 121.10(17) . . ?
C10 C9 C8 122.38(17) . . ?
C17 C9 C8 116.49(17) . . ?
C9 C10 C11' 120.3(15) . . ?
C9 C10 C1 121.27(17) . . ?
C11' C10 C1 118.4(15) . . ?
C9 C10 C11 119.8(7) . . ?
C1 C10 C11 118.9(7) . . ?
O2 C15 O3 123.79(19) . . ?
O2 C15 C8 123.40(19) . . ?
O3 C15 C8 112.80(16) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 O5 123.28(19) . . ?
O4 C17 C9 124.83(18) . . ?
O5 C17 C9 111.87(17) . . ?
O5 C18 H18A 109.5 . . ?
O5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C32 119.24(18) . . ?
C20 C19 C8 121.38(17) . . ?
C32 C19 C8 119.37(17) . . ?
C21 C20 C19 121.83(19) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C20 C21 C22 121.08(19) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C21 C22 C33 118.75(18) . . ?
C21 C22 C23 122.57(19) . . ?
C33 C22 C23 118.67(18) . . ?
C24 C23 C22 121.4(2) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 122.2(2) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C26 C25 C34 118.4(2) . . ?
C26 C25 C24 123.47(19) . . ?
C34 C25 C24 118.14(19) . . ?
C27 C26 C25 121.7(2) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 120.7(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C29 120.1(2) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C34 119.60(18) . . ?
C28 C29 C30 122.49(19) . . ?
C34 C29 C30 117.91(17) . . ?
C31 C30 C29 121.98(18) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C30 C31 C32 122.13(18) . . ?
C30 C31 H31 118.9 . . ?
C32 C31 H31 118.9 . . ?
C19 C32 C33 118.90(17) . . ?
C19 C32 C31 123.95(17) . . ?
C33 C32 C31 117.15(17) . . ?
C22 C33 C32 120.17(17) . . ?
C22 C33 C34 119.40(17) . . ?
C32 C33 C34 120.41(17) . . ?
C29 C34 C25 119.54(18) . . ?
C29 C34 C33 120.35(17) . . ?
C25 C34 C33 120.09(18) . . ?
C15 O3 C16 115.84(16) . . ?
C17 O5 C18 116.67(17) . . ?
C11 S1 C14 89.3(4) . . ?
C12 C11 C10 129.9(8) . . ?
C12 C11 S1 112.2(7) . . ?
C10 C11 S1 117.7(4) . . ?
C11 C12 C13 114.2(11) . . ?
C11 C12 H12 122.9 . . ?
C13 C12 H12 122.9 . . ?
C14 C13 C12 108.6(12) . . ?
C14 C13 H13 125.7 . . ?
C12 C13 H13 125.7 . . ?
C13 C14 S1 115.7(9) . . ?
C13 C14 H14 122.1 . . ?
S1 C14 H14 122.1 . . ?
C14' S1' C11' 90.0(13) . . ?
C12' C11' C10 129.4(12) . . ?
C12' C11' S1' 104.6(12) . . ?
C10 C11' S1' 126.0(10) . . ?
C11' C12' C13' 124.6(19) . . ?
C11' C12' H12' 117.7 . . ?
C13' C12' H12' 117.7 . . ?
C14' C13' C12' 99(3) . . ?
C14' C13' H13' 130.3 . . ?
C12' C13' H13' 130.3 . . ?
C13' C14' S1' 120(2) . . ?
C13' C14' H14' 119.8 . . ?
S1' C14' H14' 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
C6 C1 C2 C3 3.4(3) . . . . ?
C10 C1 C2 C3 -176.23(18) . . . . ?
C1 C2 C3 C4 -1.9(3) . . . . ?
C2 C3 C4 C5 -1.3(3) . . . . ?
C3 C4 C5 C6 2.8(3) . . . . ?
C4 C5 C6 C1 -1.3(3) . . . . ?
C4 C5 C6 C7 -178.23(19) . . . . ?
C2 C1 C6 C5 -1.8(3) . . . . ?
C10 C1 C6 C5 177.80(17) . . . . ?
C2 C1 C6 C7 175.15(18) . . . . ?
C10 C1 C6 C7 -5.3(3) . . . . ?
C5 C6 C7 O1 18.2(3) . . . . ?
C1 C6 C7 O1 -158.8(2) . . . . ?
C5 C6 C7 C8 -158.18(18) . . . . ?
C1 C6 C7 C8 24.9(3) . . . . ?
O1 C7 C8 C9 154.97(18) . . . . ?
C6 C7 C8 C9 -28.6(2) . . . . ?
O1 C7 C8 C19 27.7(2) . . . . ?
C6 C7 C8 C19 -155.90(16) . . . . ?
O1 C7 C8 C15 -89.1(2) . . . . ?
C6 C7 C8 C15 87.31(19) . . . . ?
C19 C8 C9 C10 140.56(18) . . . . ?
C7 C8 C9 C10 14.8(2) . . . . ?
C15 C8 C9 C10 -96.8(2) . . . . ?
C19 C8 C9 C17 -41.6(2) . . . . ?
C7 C8 C9 C17 -167.36(15) . . . . ?
C15 C8 C9 C17 81.03(19) . . . . ?
C17 C9 C10 C11' 9.6(11) . . . . ?
C8 C9 C10 C11' -172.7(11) . . . . ?
C17 C9 C10 C1 -173.57(16) . . . . ?
C8 C9 C10 C1 4.2(3) . . . . ?
C17 C9 C10 C11 8.3(5) . . . . ?
C8 C9 C10 C11 -174.0(5) . . . . ?
C2 C1 C10 C9 169.54(18) . . . . ?
C6 C1 C10 C9 -10.0(3) . . . . ?
C2 C1 C10 C11' -13.6(10) . . . . ?
C6 C1 C10 C11' 166.8(10) . . . . ?
C2 C1 C10 C11 -12.3(5) . . . . ?
C6 C1 C10 C11 168.1(5) . . . . ?
C9 C8 C15 O2 151.4(2) . . . . ?
C19 C8 C15 O2 -84.2(3) . . . . ?
C7 C8 C15 O2 32.5(3) . . . . ?
C9 C8 C15 O3 -27.7(2) . . . . ?
C19 C8 C15 O3 96.7(2) . . . . ?
C7 C8 C15 O3 -146.59(18) . . . . ?
C10 C9 C17 O4 -133.5(2) . . . . ?
C8 C9 C17 O4 48.7(3) . . . . ?
C10 C9 C17 O5 48.3(2) . . . . ?
C8 C9 C17 O5 -129.54(17) . . . . ?
C9 C8 C19 C20 114.1(2) . . . . ?
C7 C8 C19 C20 -118.8(2) . . . . ?
C15 C8 C19 C20 -7.6(2) . . . . ?
C9 C8 C19 C32 -65.2(2) . . . . ?
C7 C8 C19 C32 61.9(2) . . . . ?
C15 C8 C19 C32 173.14(16) . . . . ?
C32 C19 C20 C21 1.1(3) . . . . ?
C8 C19 C20 C21 -178.11(18) . . . . ?
C19 C20 C21 C22 -1.3(3) . . . . ?
C20 C21 C22 C33 0.0(3) . . . . ?
C20 C21 C22 C23 -179.07(19) . . . . ?
C21 C22 C23 C24 176.0(2) . . . . ?
C33 C22 C23 C24 -3.1(3) . . . . ?
C22 C23 C24 C25 1.7(3) . . . . ?
C23 C24 C25 C26 -178.7(2) . . . . ?
C23 C24 C25 C34 1.2(3) . . . . ?
C34 C25 C26 C27 0.4(3) . . . . ?
C24 C25 C26 C27 -179.7(2) . . . . ?
C25 C26 C27 C28 0.9(3) . . . . ?
C26 C27 C28 C29 -1.3(3) . . . . ?
C27 C28 C29 C34 0.5(3) . . . . ?
C27 C28 C29 C30 -178.90(19) . . . . ?
C28 C29 C30 C31 176.80(19) . . . . ?
C34 C29 C30 C31 -2.6(3) . . . . ?
C29 C30 C31 C32 0.9(3) . . . . ?
C20 C19 C32 C33 0.3(3) . . . . ?
C8 C19 C32 C33 179.54(16) . . . . ?
C20 C19 C32 C31 -179.84(18) . . . . ?
C8 C19 C32 C31 -0.6(3) . . . . ?
C30 C31 C32 C19 -178.23(18) . . . . ?
C30 C31 C32 C33 1.7(3) . . . . ?
C21 C22 C33 C32 1.4(3) . . . . ?
C23 C22 C33 C32 -179.49(17) . . . . ?
C21 C22 C33 C34 -177.63(17) . . . . ?
C23 C22 C33 C34 1.5(3) . . . . ?
C19 C32 C33 C22 -1.5(3) . . . . ?
C31 C32 C33 C22 178.59(17) . . . . ?
C19 C32 C33 C34 177.47(17) . . . . ?
C31 C32 C33 C34 -2.4(3) . . . . ?
C28 C29 C34 C25 0.8(3) . . . . ?
C30 C29 C34 C25 -179.81(17) . . . . ?
C28 C29 C34 C33 -177.67(17) . . . . ?
C30 C29 C34 C33 1.7(3) . . . . ?
C26 C25 C34 C29 -1.2(3) . . . . ?
C24 C25 C34 C29 178.87(18) . . . . ?
C26 C25 C34 C33 177.24(18) . . . . ?
C24 C25 C34 C33 -2.7(3) . . . . ?
C22 C33 C34 C29 179.74(17) . . . . ?
C32 C33 C34 C29 0.8(3) . . . . ?
C22 C33 C34 C25 1.3(3) . . . . ?
C32 C33 C34 C25 -177.70(17) . . . . ?
O2 C15 O3 C16 -1.0(3) . . . . ?
C8 C15 O3 C16 178.12(18) . . . . ?
O4 C17 O5 C18 13.0(3) . . . . ?
C9 C17 O5 C18 -168.71(18) . . . . ?
C9 C10 C11 C12 -116.6(17) . . . . ?
C11' C10 C11 C12 131(81) . . . . ?
C1 C10 C11 C12 65(2) . . . . ?
C9 C10 C11 S1 57.6(13) . . . . ?
C11' C10 C11 S1 -54(78) . . . . ?
C1 C10 C11 S1 -120.6(9) . . . . ?
C14 S1 C11 C12 -1.3(14) . . . . ?
C14 S1 C11 C10 -176.5(13) . . . . ?
C10 C11 C12 C13 175.3(16) . . . . ?
S1 C11 C12 C13 1(2) . . . . ?
C11 C12 C13 C14 0(2) . . . . ?
C12 C13 C14 S1 -1.2(18) . . . . ?
C11 S1 C14 C13 1.5(13) . . . . ?
C9 C10 C11' C12' 62(4) . . . . ?
C1 C10 C11' C12' -115(3) . . . . ?
C11 C10 C11' C12' 131(82) . . . . ?
C9 C10 C11' S1' -119(2) . . . . ?
C1 C10 C11' S1' 65(3) . . . . ?
C11 C10 C11' S1' -50(76) . . . . ?
C14' S1' C11' C12' -5(3) . . . . ?
C14' S1' C11' C10 176(3) . . . . ?
C10 C11' C12' C13' -169(3) . . . . ?
S1' C11' C12' C13' 11(4) . . . . ?
C11' C12' C13' C14' -11(4) . . . . ?
C12' C13' C14' S1' 6(4) . . . . ?
C11' S1' C14' C13' -1(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.037
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1450132'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
2,3-dimethyl4-(naphthalen-1-yl)-1-oxo-2-phenyl-1,2-dihydronaphthalene-2,3-dicarboxylate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H22 O5'
_chemical_formula_sum            'C30 H22 O5'
_chemical_formula_weight         462.48

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   16.2811(9)
_cell_length_b                   10.0247(5)
_cell_length_c                   15.5040(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.902(2)
_cell_angle_gamma                90.00
_cell_volume                     2347.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4122
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9738
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_process_details   'SADABS (Bruker, 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  'Kappa ApexII CCD Diffractometer'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25692
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4122
_reflns_number_gt                3262
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0706P)²+0.3170P] 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         4122
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1192
_refine_ls_wR_factor_gt          0.1070
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_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 0.16810(10) 0.79300(15) 0.08703(10) 0.0381(4) Uani 1 1 d . . .
C2 C 0.15819(10) 0.64702(14) 0.07613(10) 0.0364(3) Uani 1 1 d . . .
C3 C 0.10938(11) 0.59202(17) -0.00964(11) 0.0481(4) Uani 1 1 d . . .
H3 H 0.0855 0.6469 -0.0614 0.058 Uiso 1 1 calc R . .
C4 C 0.09604(13) 0.45625(18) -0.01856(12) 0.0551(5) Uani 1 1 d . . .
H4 H 0.0629 0.4193 -0.0761 0.066 Uiso 1 1 calc R . .
C5 C 0.13226(12) 0.37531(17) 0.05851(12) 0.0518(4) Uani 1 1 d . . .
H5 H 0.1224 0.2838 0.0529 0.062 Uiso 1 1 calc R . .
C6 C 0.18295(11) 0.42900(15) 0.14373(11) 0.0409(4) Uani 1 1 d . . .
H6 H 0.2079 0.3730 0.1947 0.049 Uiso 1 1 calc R . .
C7 C 0.19714(9) 0.56571(14) 0.15443(10) 0.0329(3) Uani 1 1 d . . .
C8 C 0.25385(9) 0.62674(13) 0.24366(9) 0.0314(3) Uani 1 1 d . . .
C9 C 0.24868(9) 0.75887(14) 0.25757(10) 0.0325(3) Uani 1 1 d . . .
C10 C 0.17985(9) 0.84532(14) 0.18459(10) 0.0342(3) Uani 1 1 d . . .
C11 C 0.31149(10) 0.53719(14) 0.31924(10) 0.0351(3) Uani 1 1 d . . .
C12 C 0.38377(10) 0.46701(14) 0.30968(11) 0.0385(4) Uani 1 1 d . . .
C13 C 0.40609(11) 0.47718(16) 0.23040(13) 0.0474(4) Uani 1 1 d . . .
H13 H 0.3725 0.5317 0.1814 0.057 Uiso 1 1 calc R . .
C14 C 0.47591(13) 0.40870(19) 0.22422(17) 0.0665(6) Uani 1 1 d . . .
H14 H 0.4887 0.4152 0.1707 0.080 Uiso 1 1 calc R . .
C15 C 0.52846(14) 0.3286(2) 0.2979(2) 0.0784(7) Uani 1 1 d . . .
H15 H 0.5764 0.2830 0.2934 0.094 Uiso 1 1 calc R . .
C16 C 0.51020(13) 0.31711(19) 0.37514(19) 0.0726(7) Uani 1 1 d . . .
H16 H 0.5461 0.2639 0.4237 0.087 Uiso 1 1 calc R . .
C17 C 0.43703(11) 0.38464(16) 0.38425(13) 0.0513(4) Uani 1 1 d . . .
C18 C 0.41625(14) 0.37321(19) 0.46430(14) 0.0659(6) Uani 1 1 d . . .
H18 H 0.4509 0.3193 0.5132 0.079 Uiso 1 1 calc R . .
C19 C 0.34646(15) 0.4397(2) 0.47101(13) 0.0636(5) Uani 1 1 d . . .
H19 H 0.3333 0.4307 0.5242 0.076 Uiso 1 1 calc R . .
C20 C 0.29386(12) 0.52230(16) 0.39806(11) 0.0459(4) Uani 1 1 d . . .
H20 H 0.2462 0.5675 0.4036 0.055 Uiso 1 1 calc R . .
C21 C 0.08688(9) 0.83404(14) 0.18891(10) 0.0349(3) Uani 1 1 d . . .
C22 C 0.01590(11) 0.89851(16) 0.12212(12) 0.0467(4) Uani 1 1 d . . .
H22 H 0.0255 0.9502 0.0770 0.056 Uiso 1 1 calc R . .
C23 C -0.06846(11) 0.88684(18) 0.12188(13) 0.0535(4) Uani 1 1 d . . .
H23 H -0.1151 0.9318 0.0773 0.064 Uiso 1 1 calc R . .
C24 C -0.08400(11) 0.80933(19) 0.18702(12) 0.0530(4) Uani 1 1 d . . .
H24 H -0.1411 0.8008 0.1864 0.064 Uiso 1 1 calc R . .
C25 C -0.01457(11) 0.74406(18) 0.25348(12) 0.0505(4) Uani 1 1 d . . .
H25 H -0.0248 0.6914 0.2978 0.061 Uiso 1 1 calc R . .
C26 C 0.07010(10) 0.75662(16) 0.25435(10) 0.0412(4) Uani 1 1 d . . .
H26 H 0.1166 0.7124 0.2996 0.049 Uiso 1 1 calc R . .
C27 C 0.30751(11) 0.82461(15) 0.34507(10) 0.0385(4) Uani 1 1 d . . .
C28 C 0.31288(16) 0.9993(2) 0.44990(16) 0.0809(7) Uani 1 1 d . . .
H28A H 0.3620 1.0386 0.4391 0.121 Uiso 1 1 calc R . .
H28B H 0.3345 0.9448 0.5047 0.121 Uiso 1 1 calc R . .
H28C H 0.2758 1.0685 0.4583 0.121 Uiso 1 1 calc R . .
C29 C 0.21036(11) 0.99078(15) 0.18912(11) 0.0402(4) Uani 1 1 d . . .
C30 C 0.33376(13) 1.12616(17) 0.20682(16) 0.0634(5) Uani 1 1 d . . .
H30A H 0.3000 1.1772 0.1528 0.095 Uiso 1 1 calc R . .
H30B H 0.3938 1.1185 0.2106 0.095 Uiso 1 1 calc R . .
H30C H 0.3328 1.1701 0.2615 0.095 Uiso 1 1 calc R . .
O1 O 0.16230(10) 0.86806(12) 0.02391(8) 0.0600(4) Uani 1 1 d . . .
O2 O 0.38451(8) 0.80178(12) 0.38594(8) 0.0537(3) Uani 1 1 d . . .
O3 O 0.26227(8) 0.91803(12) 0.37103(8) 0.0529(3) Uani 1 1 d . . .
O4 O 0.16556(8) 1.08759(11) 0.18169(10) 0.0598(4) Uani 1 1 d . . .
O5 O 0.29551(7) 0.99458(10) 0.20016(8) 0.0473(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 O1 1.2100(17) . ?
C1 C2 1.475(2) . ?
C1 C10 1.544(2) . ?
C2 C3 1.384(2) . ?
C2 C7 1.402(2) . ?
C3 C4 1.377(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.389(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.479(2) . ?
C8 C9 1.3496(19) . ?
C8 C11 1.4964(19) . ?
C9 C27 1.491(2) . ?
C9 C10 1.5301(19) . ?
C10 C29 1.534(2) . ?
C10 C21 1.544(2) . ?
C11 C20 1.364(2) . ?
C11 C12 1.425(2) . ?
C12 C13 1.409(2) . ?
C12 C17 1.422(2) . ?
C13 C14 1.362(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.397(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.342(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.422(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.408(3) . ?
C18 C19 1.355(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.405(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C26 1.383(2) . ?
C21 C22 1.390(2) . ?
C22 C23 1.377(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.370(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.378(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(2) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O2 1.1970(18) . ?
C27 O3 1.3427(19) . ?
C28 O3 1.444(2) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 O4 1.1934(18) . ?
C29 O5 1.3325(19) . ?
C30 O5 1.4458(19) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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
O1 C1 C2 123.51(14) . . ?
O1 C1 C10 121.66(14) . . ?
C2 C1 C10 114.68(12) . . ?
C3 C2 C7 120.83(14) . . ?
C3 C2 C1 120.29(14) . . ?
C7 C2 C1 118.87(13) . . ?
C4 C3 C2 120.18(15) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.56(16) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 120.60(15) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 120.85(14) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C2 117.95(13) . . ?
C6 C7 C8 122.53(13) . . ?
C2 C7 C8 119.49(13) . . ?
C9 C8 C7 120.07(13) . . ?
C9 C8 C11 121.46(13) . . ?
C7 C8 C11 118.33(12) . . ?
C8 C9 C27 121.47(13) . . ?
C8 C9 C10 120.65(13) . . ?
C27 C9 C10 117.85(12) . . ?
C9 C10 C29 111.68(12) . . ?
C9 C10 C1 108.73(11) . . ?
C29 C10 C1 106.71(11) . . ?
C9 C10 C21 112.69(11) . . ?
C29 C10 C21 111.94(11) . . ?
C1 C10 C21 104.62(11) . . ?
C20 C11 C12 119.80(14) . . ?
C20 C11 C8 119.15(13) . . ?
C12 C11 C8 121.04(13) . . ?
C13 C12 C17 118.27(15) . . ?
C13 C12 C11 123.11(14) . . ?
C17 C12 C11 118.60(15) . . ?
C14 C13 C12 121.23(18) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 120.3(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 120.47(19) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 121.34(19) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C18 C17 C12 119.33(16) . . ?
C18 C17 C16 122.32(18) . . ?
C12 C17 C16 118.35(19) . . ?
C19 C18 C17 120.80(17) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.33(18) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C11 C20 C19 121.12(17) . . ?
C11 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C26 C21 C22 118.07(14) . . ?
C26 C21 C10 122.55(13) . . ?
C22 C21 C10 119.31(13) . . ?
C23 C22 C21 120.91(15) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C22 120.28(16) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.66(16) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C25 C26 120.14(16) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 120.94(15) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 H26 119.5 . . ?
O2 C27 O3 123.92(14) . . ?
O2 C27 C9 125.99(14) . . ?
O3 C27 C9 110.06(13) . . ?
O3 C28 H28A 109.5 . . ?
O3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O4 C29 O5 123.93(14) . . ?
O4 C29 C10 126.37(14) . . ?
O5 C29 C10 109.68(12) . . ?
O5 C30 H30A 109.5 . . ?
O5 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O5 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 O3 C28 116.34(14) . . ?
C29 O5 C30 115.79(13) . . ?

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
O1 C1 C2 C3 -25.2(2) . . . . ?
C10 C1 C2 C3 150.51(14) . . . . ?
O1 C1 C2 C7 156.37(15) . . . . ?
C10 C1 C2 C7 -27.94(19) . . . . ?
C7 C2 C3 C4 2.1(2) . . . . ?
C1 C2 C3 C4 -176.34(15) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C3 C4 C5 C6 -1.2(3) . . . . ?
C4 C5 C6 C7 1.4(3) . . . . ?
C5 C6 C7 C2 0.2(2) . . . . ?
C5 C6 C7 C8 -177.57(14) . . . . ?
C3 C2 C7 C6 -1.9(2) . . . . ?
C1 C2 C7 C6 176.53(13) . . . . ?
C3 C2 C7 C8 175.92(13) . . . . ?
C1 C2 C7 C8 -5.6(2) . . . . ?
C6 C7 C8 C9 -163.65(14) . . . . ?
C2 C7 C8 C9 18.63(19) . . . . ?
C6 C7 C8 C11 12.1(2) . . . . ?
C2 C7 C8 C11 -165.60(13) . . . . ?
C7 C8 C9 C27 -177.39(12) . . . . ?
C11 C8 C9 C27 7.0(2) . . . . ?
C7 C8 C9 C10 4.44(19) . . . . ?
C11 C8 C9 C10 -171.20(12) . . . . ?
C8 C9 C10 C29 -153.22(13) . . . . ?
C27 C9 C10 C29 28.54(17) . . . . ?
C8 C9 C10 C1 -35.74(17) . . . . ?
C27 C9 C10 C1 146.02(12) . . . . ?
C8 C9 C10 C21 79.77(16) . . . . ?
C27 C9 C10 C21 -98.47(14) . . . . ?
O1 C1 C10 C9 -137.75(15) . . . . ?
C2 C1 C10 C9 46.48(16) . . . . ?
O1 C1 C10 C29 -17.15(19) . . . . ?
C2 C1 C10 C29 167.07(12) . . . . ?
O1 C1 C10 C21 101.63(17) . . . . ?
C2 C1 C10 C21 -74.14(15) . . . . ?
C9 C8 C11 C20 63.14(19) . . . . ?
C7 C8 C11 C20 -112.57(15) . . . . ?
C9 C8 C11 C12 -117.28(15) . . . . ?
C7 C8 C11 C12 67.01(18) . . . . ?
C20 C11 C12 C13 179.95(15) . . . . ?
C8 C11 C12 C13 0.4(2) . . . . ?
C20 C11 C12 C17 -1.2(2) . . . . ?
C8 C11 C12 C17 179.19(13) . . . . ?
C17 C12 C13 C14 1.0(2) . . . . ?
C11 C12 C13 C14 179.78(15) . . . . ?
C12 C13 C14 C15 -1.5(3) . . . . ?
C13 C14 C15 C16 0.7(3) . . . . ?
C14 C15 C16 C17 0.4(3) . . . . ?
C13 C12 C17 C18 179.80(15) . . . . ?
C11 C12 C17 C18 0.9(2) . . . . ?
C13 C12 C17 C16 0.2(2) . . . . ?
C11 C12 C17 C16 -178.67(15) . . . . ?
C15 C16 C17 C18 179.51(19) . . . . ?
C15 C16 C17 C12 -0.9(3) . . . . ?
C12 C17 C18 C19 -0.1(3) . . . . ?
C16 C17 C18 C19 179.48(18) . . . . ?
C17 C18 C19 C20 -0.4(3) . . . . ?
C12 C11 C20 C19 0.7(2) . . . . ?
C8 C11 C20 C19 -179.70(15) . . . . ?
C18 C19 C20 C11 0.1(3) . . . . ?
C9 C10 C21 C26 1.91(19) . . . . ?
C29 C10 C21 C26 -124.97(15) . . . . ?
C1 C10 C21 C26 119.85(14) . . . . ?
C9 C10 C21 C22 -174.90(13) . . . . ?
C29 C10 C21 C22 58.23(18) . . . . ?
C1 C10 C21 C22 -56.95(16) . . . . ?
C26 C21 C22 C23 0.8(2) . . . . ?
C10 C21 C22 C23 177.71(15) . . . . ?
C21 C22 C23 C24 -1.0(3) . . . . ?
C22 C23 C24 C25 0.7(3) . . . . ?
C23 C24 C25 C26 -0.1(3) . . . . ?
C24 C25 C26 C21 -0.2(3) . . . . ?
C22 C21 C26 C25 -0.2(2) . . . . ?
C10 C21 C26 C25 -177.01(14) . . . . ?
C8 C9 C27 O2 40.4(2) . . . . ?
C10 C9 C27 O2 -141.34(15) . . . . ?
C8 C9 C27 O3 -141.53(14) . . . . ?
C10 C9 C27 O3 36.70(17) . . . . ?
C9 C10 C29 O4 -139.09(17) . . . . ?
C1 C10 C29 O4 102.22(18) . . . . ?
C21 C10 C29 O4 -11.7(2) . . . . ?
C9 C10 C29 O5 42.71(16) . . . . ?
C1 C10 C29 O5 -75.98(15) . . . . ?
C21 C10 C29 O5 170.12(12) . . . . ?
O2 C27 O3 C28 3.9(2) . . . . ?
C9 C27 O3 C28 -174.18(15) . . . . ?
O4 C29 O5 C30 2.5(2) . . . . ?
C10 C29 O5 C30 -179.22(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.035
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1450133'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
2,3-dimethyl4-(5-hexylthiophen-2-yl)-1-oxo-2-phenyl-1,2-dihydronaphthalene-2,3-dicarboxylate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 O5 S'
_chemical_formula_sum            'C30 H30 O5 S'
_chemical_formula_weight         502.60

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'
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           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4725(4)
_cell_length_b                   12.9073(7)
_cell_length_c                   14.9503(8)
_cell_angle_alpha                105.607(2)
_cell_angle_beta                 103.985(4)
_cell_angle_gamma                100.951(5)
_cell_volume                     1296.49(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5097
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   'SADABS (Bruker, 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  'Kappa ApexII CCD Diffractometer'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26878
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5097
_reflns_number_gt                4006
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0918P)²+0.2678P] 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         5097
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1409
_refine_ls_wR_factor_gt          0.1208
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_iucr_refine_instruction_details 
;
TITL G11 in P-1
CELL  0.71073   7.4725  12.9073  14.9503  105.607  103.985  100.951
ZERR     2.00   0.0004   0.0007   0.0008    0.002    0.002    0.002
LATT   1
SFAC  C    H    O    S
UNIT  60   60   10   2
MERG   2
OMIT    -2.00  52.00
OMIT  0  1  0
OMIT  0  0  1
OMIT  0 -1  1
EQIV $1 -x+1, -y+1, -z
HTAB C18 O5_$1
EQIV $2 x+1, y, z
HTAB C22 O1_$2
FMAP   2
PLAN   20
ACTA
BOND   $H
CONF
L.S.  10
WGHT    0.091800    0.267800
FVAR       0.15554
C1    1    0.578020    0.728243    0.367370    11.00000    0.03486    0.04724 =
         0.04080    0.02115    0.01590    0.01704
C2    1    0.685748    0.841428    0.378429    11.00000    0.03807    0.03943 =
         0.04291    0.01725    0.01636    0.01783
C3    1    0.663100    0.933890    0.442874    11.00000    0.05445    0.04908 =
         0.05707    0.01864    0.02794    0.02721
AFIX  43
H3    2    0.577968    0.924304    0.478122    11.00000   -1.20000
AFIX   0
C4    1    0.765977    1.039964    0.455044    11.00000    0.06993    0.04301 =
         0.05870    0.01153    0.02298    0.02725
AFIX  43
H4    2    0.751659    1.101804    0.499022    11.00000   -1.20000
AFIX   0
C5    1    0.889905    1.054097    0.401948    11.00000    0.06061    0.03522 =
         0.05894    0.01489    0.01497    0.01264
AFIX  43
H5    2    0.959988    1.125676    0.410438    11.00000   -1.20000
AFIX   0
C6    1    0.911032    0.962483    0.335943    11.00000    0.04836    0.03869 =
         0.04954    0.01699    0.01858    0.01035
AFIX  43
H6    2    0.993452    0.973186    0.299532    11.00000   -1.20000
AFIX   0
C7    1    0.810316    0.854526    0.323451    11.00000    0.03809    0.03521 =
         0.03807    0.01499    0.01146    0.01237
C8    1    0.828559    0.754878    0.253397    11.00000    0.03355    0.03575 =
         0.03547    0.01499    0.01214    0.01111
C9    1    0.755789    0.651763    0.254768    11.00000    0.03356    0.03662 =
         0.03356    0.01514    0.01213    0.01274
C10   1    0.670782    0.634121    0.334158    11.00000    0.03136    0.03480 =
         0.03796    0.01626    0.01389    0.00980
C11   1    0.821995    0.639341    0.426721    11.00000    0.03427    0.02930 =
         0.03608    0.01351    0.01282    0.00908
C12   1    1.012289    0.647866    0.431762    11.00000    0.03641    0.03754 =
         0.03924    0.01460    0.01540    0.01134
AFIX  43
H12   2    1.052416    0.653208    0.378534    11.00000   -1.20000
AFIX   0
C13   1    1.142761    0.648494    0.515164    11.00000    0.03521    0.04422 =
         0.04931    0.01577    0.00938    0.01219
AFIX  43
H13   2    1.269923    0.654133    0.517633    11.00000   -1.20000
AFIX   0
C14   1    1.085917    0.640855    0.594297    11.00000    0.05173    0.04317 =
         0.04035    0.01605    0.00401    0.01057
AFIX  43
H14   2    1.173374    0.639674    0.649827    11.00000   -1.20000
AFIX   0
C15   1    0.898498    0.634948    0.590937    11.00000    0.05918    0.05386 =
         0.03898    0.02087    0.01956    0.01421
AFIX  43
H15   2    0.860211    0.631500    0.645056    11.00000   -1.20000
AFIX   0
C16   1    0.766963    0.634094    0.508113    11.00000    0.04147    0.04855 =
         0.04308    0.01973    0.01987    0.01488
AFIX  43
H16   2    0.640653    0.629983    0.506706    11.00000   -1.20000
AFIX   0
C17   1    0.764221    0.547705    0.184828    11.00000    0.04121    0.03601 =
         0.03850    0.01550    0.01447    0.01258
C18   1    0.715156    0.446197    0.021382    11.00000    0.09694    0.05686 =
         0.03909    0.00968    0.01998    0.03281
AFIX 137
H18A  2    0.841987    0.436474    0.032845    11.00000   -1.50000
H18B  2    0.670916    0.451182   -0.042781    11.00000   -1.50000
H18C  2    0.630288    0.383527    0.026304    11.00000   -1.50000
AFIX   0
C19   1    0.511608    0.523476    0.295545    11.00000    0.03472    0.04437 =
         0.04358    0.01750    0.01343    0.00752
C20   1    0.237325    0.413178    0.164470    11.00000    0.05690    0.07497 =
         0.06813    0.02385   -0.00634   -0.01759
AFIX 137
H20A  2    0.281653    0.350639    0.173919    11.00000   -1.50000
H20B  2    0.186435    0.400398    0.095821    11.00000   -1.50000
H20C  2    0.138933    0.421857    0.194676    11.00000   -1.50000
AFIX   0
C21   1    0.942688    0.772925    0.188191    11.00000    0.04178    0.03600 =
         0.03866    0.01496    0.01605    0.01008
C22   1    1.117861    0.756683    0.194094    11.00000    0.04599    0.05894 =
         0.04781    0.02731    0.02106    0.02132
AFIX  43
H22   2    1.182326    0.729002    0.239831    11.00000   -1.20000
AFIX   0
C23   1    1.193060    0.786268    0.123247    11.00000    0.04819    0.06214 =
         0.05502    0.02497    0.02922    0.02033
AFIX  43
H23   2    1.312666    0.780218    0.118404    11.00000   -1.20000
AFIX   0
C24   1    1.076361    0.823865    0.063611    11.00000    0.05009    0.03990 =
         0.04457    0.01576    0.02404    0.01244
C25   1    1.106809    0.865370   -0.018000    11.00000    0.06753    0.05397 =
         0.05544    0.02855    0.03364    0.01966
AFIX  23
H25A  2    0.989337    0.835205   -0.072576    11.00000   -1.20000
H25B  2    1.132702    0.946154    0.004056    11.00000   -1.20000
AFIX   0
C26   1    1.267992    0.834499   -0.053008    11.00000    0.07071    0.05891 =
         0.05824    0.03023    0.03771    0.02541
AFIX  23
H26A  2    1.239970    0.753640   -0.076876    11.00000   -1.20000
H26B  2    1.384481    0.862538    0.002113    11.00000   -1.20000
AFIX   0
C27   1    1.303932    0.878730   -0.132714    11.00000    0.06810    0.05565 =
         0.05577    0.02715    0.03316    0.01843
AFIX  23
H27A  2    1.328582    0.959434   -0.109893    11.00000   -1.20000
H27B  2    1.189472    0.848598   -0.189022    11.00000   -1.20000
AFIX   0
C28   1    1.471305    0.849086   -0.163604    11.00000    0.05881    0.06291 =
         0.05196    0.02523    0.02428    0.01611
AFIX  23
H28A  2    1.585220    0.879030   -0.107003    11.00000   -1.20000
H28B  2    1.446245    0.768352   -0.186088    11.00000   -1.20000
AFIX   0
C29   1    1.511091    0.892024   -0.242987    11.00000    0.06464    0.06544 =
         0.05828    0.02656    0.02801    0.00951
AFIX  23
H29A  2    1.396045    0.863789   -0.298936    11.00000   -1.20000
H29B  2    1.539746    0.972929   -0.219818    11.00000   -1.20000
AFIX   0
C30   1    1.673883    0.859855   -0.275537    11.00000    0.08596    0.12518 =
         0.09621    0.05365    0.06069    0.02989
AFIX 137
H30A  2    1.790816    0.892779   -0.222070    11.00000   -1.50000
H30B  2    1.685842    0.886292   -0.328582    11.00000   -1.50000
H30C  2    1.648986    0.779945   -0.296755    11.00000   -1.50000
AFIX   0
O1    3    0.430138    0.709785    0.387486    11.00000    0.04278    0.06459 =
         0.07811    0.03486    0.03642    0.02443
O2    3    0.798652    0.469765    0.207968    11.00000    0.09153    0.04432 =
         0.04728    0.02116    0.02335    0.03262
O3    3    0.718573    0.547401    0.093112    11.00000    0.07491    0.04045 =
         0.03431    0.01292    0.01574    0.02146
O4    3    0.490418    0.456869    0.335753    11.00000    0.05254    0.05201 =
         0.06234    0.03111    0.01202   -0.00242
O5    3    0.395420    0.513562    0.208146    11.00000    0.04208    0.05659 =
         0.04910    0.02107    0.00287   -0.00280
S1    4    0.868823    0.824153    0.094578    11.00000    0.05131    0.05806 =
         0.05088    0.03186    0.02524    0.02316
HKLF    4
 
REM  G11 in P-1
REM R1 =  0.0398 for   4006 Fo > 4sig(Fo)  and  0.0552 for all   5097 data
REM    328 parameters refined using      0 restraints
 
END
;

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 0.5780(2) 0.72824(15) 0.36737(12) 0.0379(4) Uani 1 1 d . . .
C2 C 0.6857(2) 0.84143(14) 0.37843(13) 0.0376(4) Uani 1 1 d . . .
C3 C 0.6631(3) 0.93389(16) 0.44287(15) 0.0494(5) Uani 1 1 d . . .
H3 H 0.5780 0.9243 0.4781 0.059 Uiso 1 1 calc R . .
C4 C 0.7660(3) 1.03996(17) 0.45504(16) 0.0560(5) Uani 1 1 d . . .
H4 H 0.7517 1.1018 0.4990 0.067 Uiso 1 1 calc R . .
C5 C 0.8899(3) 1.05410(16) 0.40195(15) 0.0525(5) Uani 1 1 d . . .
H5 H 0.9600 1.1257 0.4104 0.063 Uiso 1 1 calc R . .
C6 C 0.9110(3) 0.96248(15) 0.33594(14) 0.0446(4) Uani 1 1 d . . .
H6 H 0.9935 0.9732 0.2995 0.054 Uiso 1 1 calc R . .
C7 C 0.8103(2) 0.85453(14) 0.32345(12) 0.0362(4) Uani 1 1 d . . .
C8 C 0.8286(2) 0.75488(13) 0.25340(12) 0.0337(3) Uani 1 1 d . . .
C9 C 0.7558(2) 0.65176(13) 0.25477(11) 0.0330(3) Uani 1 1 d . . .
C10 C 0.6708(2) 0.63412(13) 0.33416(12) 0.0331(3) Uani 1 1 d . . .
C11 C 0.8220(2) 0.63934(13) 0.42672(11) 0.0322(3) Uani 1 1 d . . .
C12 C 1.0123(2) 0.64787(14) 0.43176(12) 0.0365(4) Uani 1 1 d . . .
H12 H 1.0524 0.6532 0.3785 0.044 Uiso 1 1 calc R . .
C13 C 1.1428(3) 0.64849(15) 0.51516(14) 0.0433(4) Uani 1 1 d . . .
H13 H 1.2699 0.6541 0.5176 0.052 Uiso 1 1 calc R . .
C14 C 1.0859(3) 0.64085(15) 0.59430(13) 0.0469(4) Uani 1 1 d . . .
H14 H 1.1734 0.6397 0.6498 0.056 Uiso 1 1 calc R . .
C15 C 0.8985(3) 0.63495(17) 0.59094(14) 0.0489(5) Uani 1 1 d . . .
H15 H 0.8602 0.6315 0.6451 0.059 Uiso 1 1 calc R . .
C16 C 0.7670(3) 0.63409(15) 0.50811(13) 0.0417(4) Uani 1 1 d . . .
H16 H 0.6407 0.6300 0.5067 0.050 Uiso 1 1 calc R . .
C17 C 0.7642(2) 0.54771(14) 0.18483(12) 0.0372(4) Uani 1 1 d . . .
C18 C 0.7152(4) 0.44620(19) 0.02138(15) 0.0641(6) Uani 1 1 d . . .
H18A H 0.8420 0.4365 0.0328 0.096 Uiso 1 1 calc R . .
H18B H 0.6709 0.4512 -0.0428 0.096 Uiso 1 1 calc R . .
H18C H 0.6303 0.3835 0.0263 0.096 Uiso 1 1 calc R . .
C19 C 0.5116(2) 0.52348(15) 0.29554(13) 0.0405(4) Uani 1 1 d . . .
C20 C 0.2373(3) 0.4132(2) 0.16447(19) 0.0767(8) Uani 1 1 d . . .
H20A H 0.2817 0.3506 0.1739 0.115 Uiso 1 1 calc R . .
H20B H 0.1864 0.4004 0.0958 0.115 Uiso 1 1 calc R . .
H20C H 0.1389 0.4219 0.1947 0.115 Uiso 1 1 calc R . .
C21 C 0.9427(2) 0.77292(14) 0.18819(12) 0.0377(4) Uani 1 1 d . . .
C22 C 1.1179(3) 0.75668(17) 0.19409(14) 0.0466(4) Uani 1 1 d . . .
H22 H 1.1823 0.7290 0.2398 0.056 Uiso 1 1 calc R . .
C23 C 1.1931(3) 0.78627(18) 0.12325(15) 0.0507(5) Uani 1 1 d . . .
H23 H 1.3127 0.7802 0.1184 0.061 Uiso 1 1 calc R . .
C24 C 1.0764(3) 0.82387(15) 0.06361(13) 0.0427(4) Uani 1 1 d . . .
C25 C 1.1068(3) 0.86537(18) -0.01800(16) 0.0536(5) Uani 1 1 d . . .
H25A H 0.9893 0.8352 -0.0726 0.064 Uiso 1 1 calc R . .
H25B H 1.1327 0.9462 0.0041 0.064 Uiso 1 1 calc R . .
C26 C 1.2680(3) 0.83450(18) -0.05301(16) 0.0558(5) Uani 1 1 d . . .
H26A H 1.2400 0.7536 -0.0769 0.067 Uiso 1 1 calc R . .
H26B H 1.3845 0.8625 0.0021 0.067 Uiso 1 1 calc R . .
C27 C 1.3039(3) 0.87873(18) -0.13271(16) 0.0551(5) Uani 1 1 d . . .
H27A H 1.3286 0.9594 -0.1099 0.066 Uiso 1 1 calc R . .
H27B H 1.1895 0.8486 -0.1890 0.066 Uiso 1 1 calc R . .
C28 C 1.4713(3) 0.84909(19) -0.16360(16) 0.0553(5) Uani 1 1 d . . .
H28A H 1.5852 0.8790 -0.1070 0.066 Uiso 1 1 calc R . .
H28B H 1.4462 0.7684 -0.1861 0.066 Uiso 1 1 calc R . .
C29 C 1.5111(3) 0.8920(2) -0.24299(17) 0.0610(6) Uani 1 1 d . . .
H29A H 1.3960 0.8638 -0.2989 0.073 Uiso 1 1 calc R . .
H29B H 1.5397 0.9729 -0.2198 0.073 Uiso 1 1 calc R . .
C30 C 1.6739(4) 0.8599(3) -0.2755(2) 0.0926(9) Uani 1 1 d . . .
H30A H 1.7908 0.8928 -0.2221 0.139 Uiso 1 1 calc R . .
H30B H 1.6858 0.8863 -0.3286 0.139 Uiso 1 1 calc R . .
H30C H 1.6490 0.7799 -0.2968 0.139 Uiso 1 1 calc R . .
O1 O 0.43014(18) 0.70978(12) 0.38749(11) 0.0547(4) Uani 1 1 d . . .
O2 O 0.7987(2) 0.46977(11) 0.20797(10) 0.0574(4) Uani 1 1 d . . .
O3 O 0.7186(2) 0.54740(10) 0.09311(9) 0.0492(3) Uani 1 1 d . . .
O4 O 0.4904(2) 0.45687(12) 0.33575(11) 0.0566(4) Uani 1 1 d . . .
O5 O 0.39542(18) 0.51356(12) 0.20815(10) 0.0530(4) Uani 1 1 d . . .
S1 S 0.86882(7) 0.82415(4) 0.09458(4) 0.04751(16) 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 O1 1.211(2) . ?
C1 C2 1.473(2) . ?
C1 C10 1.538(2) . ?
C2 C3 1.385(3) . ?
C2 C7 1.398(2) . ?
C3 C4 1.377(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.384(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.392(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.477(2) . ?
C8 C9 1.346(2) . ?
C8 C21 1.477(2) . ?
C9 C17 1.486(2) . ?
C9 C10 1.523(2) . ?
C10 C11 1.537(2) . ?
C10 C19 1.538(2) . ?
C11 C12 1.387(2) . ?
C11 C16 1.389(2) . ?
C12 C13 1.382(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.371(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.378(3) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 O2 1.200(2) . ?
C17 O3 1.329(2) . ?
C18 O3 1.441(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 O4 1.182(2) . ?
C19 O5 1.341(2) . ?
C20 O5 1.446(2) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.350(3) . ?
C21 S1 1.7216(17) . ?
C22 C23 1.417(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.345(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.506(2) . ?
C24 S1 1.7227(18) . ?
C25 C26 1.503(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.510(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.513(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.505(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.503(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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
O1 C1 C2 122.82(16) . . ?
O1 C1 C10 121.24(16) . . ?
C2 C1 C10 115.85(13) . . ?
C3 C2 C7 120.52(16) . . ?
C3 C2 C1 119.96(16) . . ?
C7 C2 C1 119.52(15) . . ?
C4 C3 C2 120.36(18) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 119.76(18) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.42(18) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 120.73(17) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C2 118.19(16) . . ?
C6 C7 C8 122.23(15) . . ?
C2 C7 C8 119.58(15) . . ?
C9 C8 C21 121.43(14) . . ?
C9 C8 C7 120.59(14) . . ?
C21 C8 C7 117.78(14) . . ?
C8 C9 C17 123.49(14) . . ?
C8 C9 C10 121.59(14) . . ?
C17 C9 C10 114.77(13) . . ?
C9 C10 C11 113.10(12) . . ?
C9 C10 C1 109.64(13) . . ?
C11 C10 C1 105.49(13) . . ?
C9 C10 C19 111.14(13) . . ?
C11 C10 C19 110.29(13) . . ?
C1 C10 C19 106.84(13) . . ?
C12 C11 C16 118.48(15) . . ?
C12 C11 C10 122.27(14) . . ?
C16 C11 C10 119.24(14) . . ?
C13 C12 C11 120.59(16) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.41(17) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 119.50(17) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 120.62(17) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 120.38(16) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
O2 C17 O3 123.48(16) . . ?
O2 C17 C9 123.51(15) . . ?
O3 C17 C9 112.89(14) . . ?
O3 C18 H18A 109.5 . . ?
O3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O4 C19 O5 124.12(16) . . ?
O4 C19 C10 126.43(16) . . ?
O5 C19 C10 109.45(14) . . ?
O5 C20 H20A 109.5 . . ?
O5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C8 126.54(16) . . ?
C22 C21 S1 110.42(13) . . ?
C8 C21 S1 123.00(13) . . ?
C21 C22 C23 112.88(17) . . ?
C21 C22 H22 123.6 . . ?
C23 C22 H22 123.6 . . ?
C24 C23 C22 114.13(17) . . ?
C24 C23 H23 122.9 . . ?
C22 C23 H23 122.9 . . ?
C23 C24 C25 129.83(17) . . ?
C23 C24 S1 109.91(13) . . ?
C25 C24 S1 120.24(15) . . ?
C26 C25 C24 114.06(17) . . ?
C26 C25 H25A 108.7 . . ?
C24 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C24 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C25 C26 C27 114.55(18) . . ?
C25 C26 H26A 108.6 . . ?
C27 C26 H26A 108.6 . . ?
C25 C26 H26B 108.6 . . ?
C27 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C26 C27 C28 112.92(18) . . ?
C26 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
C26 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C29 C28 C27 114.27(19) . . ?
C29 C28 H28A 108.7 . . ?
C27 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C30 C29 C28 114.2(2) . . ?
C30 C29 H29A 108.7 . . ?
C28 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C28 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C17 O3 C18 115.33(14) . . ?
C19 O5 C20 114.84(16) . . ?
C21 S1 C24 92.67(9) . . ?

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
O1 C1 C2 C3 23.0(3) . . . . ?
C10 C1 C2 C3 -153.45(16) . . . . ?
O1 C1 C2 C7 -156.92(18) . . . . ?
C10 C1 C2 C7 26.6(2) . . . . ?
C7 C2 C3 C4 -1.3(3) . . . . ?
C1 C2 C3 C4 178.77(18) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C4 C5 C6 C7 -1.2(3) . . . . ?
C5 C6 C7 C2 0.8(3) . . . . ?
C5 C6 C7 C8 179.70(17) . . . . ?
C3 C2 C7 C6 0.4(3) . . . . ?
C1 C2 C7 C6 -179.61(16) . . . . ?
C3 C2 C7 C8 -178.49(16) . . . . ?
C1 C2 C7 C8 1.5(2) . . . . ?
C6 C7 C8 C9 168.58(16) . . . . ?
C2 C7 C8 C9 -12.5(2) . . . . ?
C6 C7 C8 C21 -6.3(2) . . . . ?
C2 C7 C8 C21 172.56(15) . . . . ?
C21 C8 C9 C17 -7.0(2) . . . . ?
C7 C8 C9 C17 178.29(15) . . . . ?
C21 C8 C9 C10 168.39(15) . . . . ?
C7 C8 C9 C10 -6.3(2) . . . . ?
C8 C9 C10 C11 -85.16(18) . . . . ?
C17 C9 C10 C11 90.60(17) . . . . ?
C8 C9 C10 C1 32.3(2) . . . . ?
C17 C9 C10 C1 -151.98(14) . . . . ?
C8 C9 C10 C19 150.16(16) . . . . ?
C17 C9 C10 C19 -34.09(18) . . . . ?
O1 C1 C10 C9 142.13(17) . . . . ?
C2 C1 C10 C9 -41.33(19) . . . . ?
O1 C1 C10 C11 -95.79(19) . . . . ?
C2 C1 C10 C11 80.76(16) . . . . ?
O1 C1 C10 C19 21.6(2) . . . . ?
C2 C1 C10 C19 -161.87(14) . . . . ?
C9 C10 C11 C12 -6.2(2) . . . . ?
C1 C10 C11 C12 -125.99(16) . . . . ?
C19 C10 C11 C12 118.99(16) . . . . ?
C9 C10 C11 C16 174.60(14) . . . . ?
C1 C10 C11 C16 54.77(18) . . . . ?
C19 C10 C11 C16 -60.25(19) . . . . ?
C16 C11 C12 C13 1.5(2) . . . . ?
C10 C11 C12 C13 -177.77(15) . . . . ?
C11 C12 C13 C14 -0.1(3) . . . . ?
C12 C13 C14 C15 -1.4(3) . . . . ?
C13 C14 C15 C16 1.5(3) . . . . ?
C14 C15 C16 C11 -0.1(3) . . . . ?
C12 C11 C16 C15 -1.4(3) . . . . ?
C10 C11 C16 C15 177.89(16) . . . . ?
C8 C9 C17 O2 139.04(19) . . . . ?
C10 C9 C17 O2 -36.6(2) . . . . ?
C8 C9 C17 O3 -44.7(2) . . . . ?
C10 C9 C17 O3 139.66(15) . . . . ?
C9 C10 C19 O4 135.44(19) . . . . ?
C11 C10 C19 O4 9.2(2) . . . . ?
C1 C10 C19 O4 -105.0(2) . . . . ?
C9 C10 C19 O5 -45.47(18) . . . . ?
C11 C10 C19 O5 -171.72(13) . . . . ?
C1 C10 C19 O5 74.11(17) . . . . ?
C9 C8 C21 C22 -67.3(3) . . . . ?
C7 C8 C21 C22 107.6(2) . . . . ?
C9 C8 C21 S1 115.25(17) . . . . ?
C7 C8 C21 S1 -69.88(19) . . . . ?
C8 C21 C22 C23 -177.36(17) . . . . ?
S1 C21 C22 C23 0.3(2) . . . . ?
C21 C22 C23 C24 -0.4(3) . . . . ?
C22 C23 C24 C25 178.37(19) . . . . ?
C22 C23 C24 S1 0.3(2) . . . . ?
C23 C24 C25 C26 16.4(3) . . . . ?
S1 C24 C25 C26 -165.73(16) . . . . ?
C24 C25 C26 C27 -178.19(18) . . . . ?
C25 C26 C27 C28 178.12(19) . . . . ?
C26 C27 C28 C29 -179.97(19) . . . . ?
C27 C28 C29 C30 -178.4(2) . . . . ?
O2 C17 O3 C18 -0.8(3) . . . . ?
C9 C17 O3 C18 -177.08(17) . . . . ?
O4 C19 O5 C20 0.0(3) . . . . ?
C10 C19 O5 C20 -179.14(18) . . . . ?
C22 C21 S1 C24 -0.15(15) . . . . ?
C8 C21 S1 C24 177.65(15) . . . . ?
C23 C24 S1 C21 -0.09(16) . . . . ?
C25 C24 S1 C21 -178.37(16) . . . . ?

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
C18 H18B O5 0.96 2.58 3.533(3) 170.9 2_665
C22 H22 O1 0.93 2.62 3.520(2) 163.4 1_655

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.042
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
