 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C28 H26 O4 S6'
_chemical_formula_sum
 'C28 H26 O4 S6'
_chemical_formula_weight          618.85
 
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    C2/c
_symmetry_space_group_name_hall   '-C 2yc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    15.509(3)
_cell_length_b                    8.0208(16)
_cell_length_c                    22.583(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.60(3)
_cell_angle_gamma                 90.00
_cell_volume                      2790.6(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     13016
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.45
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.473
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1288
_exptl_absorpt_coefficient_mu     0.525
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7982
_exptl_absorpt_correction_T_max   0.9023
_exptl_absorpt_process_details    'SORTAV (R.H.Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_decay_%         'negligible'
_diffrn_reflns_number             13072
_diffrn_reflns_av_R_equivalents   0.0938
_diffrn_reflns_av_sigmaI/netI     0.0574
_diffrn_reflns_limit_h_min        -20
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -29
_diffrn_reflns_limit_l_max        29
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          27.34
_reflns_number_total              3113
_reflns_number_gt                 2511
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Watkin, Pearce 1995)'
_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 > 2σ(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)+(0.0764P)²+10.4492P] 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          3113
_refine_ls_number_parameters      174
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0812
_refine_ls_R_factor_gt            0.0654
_refine_ls_wR_factor_ref          0.1752
_refine_ls_wR_factor_gt           0.1649
_refine_ls_goodness_of_fit_ref    1.075
_refine_ls_restrained_S_all       1.075
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.0574(2) -0.2414(4) 0.05943(15) 0.0286(7) Uani 1 1 d . . .
C2 C 0.1195(2) -0.3512(4) 0.04001(15) 0.0286(7) Uani 1 1 d . . .
C3 C 0.1138(2) -0.4004(4) -0.01940(15) 0.0313(8) Uani 1 1 d . . .
H3 H 0.1565 -0.4724 -0.0323 0.038 Uiso 1 1 calc R . .
C4 C 0.0455(2) -0.3445(4) -0.06010(15) 0.0297(7) Uani 1 1 d . . .
C5 C -0.0182(2) -0.2409(4) -0.04202(16) 0.0321(8) Uani 1 1 d . . .
H5 H -0.0655 -0.2048 -0.0695 0.039 Uiso 1 1 calc R . .
C6 C -0.0112(2) -0.1910(5) 0.01750(15) 0.0319(8) Uani 1 1 d . . .
H6 H -0.0546 -0.1200 0.0301 0.038 Uiso 1 1 calc R . .
C7 C 0.2527(3) -0.5014(6) 0.06327(17) 0.0434(10) Uani 1 1 d . . .
H7A H 0.2314 -0.6111 0.0492 0.065 Uiso 1 1 calc R . .
H7B H 0.2986 -0.5154 0.0965 0.065 Uiso 1 1 calc R . .
H7C H 0.2759 -0.4419 0.0307 0.065 Uiso 1 1 calc R . .
C8 C -0.0223(3) -0.3511(6) -0.16098(16) 0.0458(10) Uani 1 1 d . . .
H8A H -0.0780 -0.3833 -0.1477 0.069 Uiso 1 1 calc R . .
H8B H -0.0158 -0.4058 -0.1990 0.069 Uiso 1 1 calc R . .
H8C H -0.0206 -0.2299 -0.1661 0.069 Uiso 1 1 calc R . .
C9 C 0.0621(2) -0.1816(4) 0.12182(14) 0.0266(7) Uani 1 1 d . . .
C10 C 0.0216(2) -0.1059(4) 0.22275(14) 0.0255(7) Uani 1 1 d . . .
C11 C 0.1056(2) -0.0609(4) 0.21517(14) 0.0244(7) Uani 1 1 d . . .
C12 C 0.1292(2) -0.1040(4) 0.15739(15) 0.0267(7) Uani 1 1 d . . .
C13 C 0.2752(2) 0.0439(6) 0.24747(19) 0.0419(9) Uani 1 1 d . . .
H13A H 0.3140 0.1217 0.2719 0.050 Uiso 1 1 calc R . .
H13B H 0.2984 -0.0702 0.2546 0.050 Uiso 1 1 calc R . .
C14 C 0.2763(3) 0.0870(6) 0.1825(2) 0.0509(12) Uani 1 1 d . . .
H14A H 0.3370 0.1075 0.1751 0.061 Uiso 1 1 calc R . .
H14B H 0.2435 0.1918 0.1740 0.061 Uiso 1 1 calc R . .
O1 O 0.18204(17) -0.4066(3) 0.08301(10) 0.0350(6) Uani 1 1 d . . .
O2 O 0.04703(18) -0.4015(3) -0.11726(11) 0.0371(6) Uani 1 1 d . . .
S1 S -0.02819(6) -0.20195(12) 0.15906(4) 0.0304(2) Uani 1 1 d . . .
S2 S 0.16842(6) 0.05437(12) 0.27136(4) 0.0336(3) Uani 1 1 d . . .
S3 S 0.23053(6) -0.07210(14) 0.13162(4) 0.0392(3) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C6 1.400(5) . ?
C1 C2 1.412(5) . ?
C1 C9 1.482(4) . ?
C2 O1 1.366(4) . ?
C2 C3 1.392(5) . ?
C3 C4 1.394(5) . ?
C3 H3 0.9500 . ?
C4 O2 1.372(4) . ?
C4 C5 1.389(5) . ?
C5 C6 1.394(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O1 1.445(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 O2 1.432(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C12 1.386(5) . ?
C9 S1 1.723(3) . ?
C10 C11 1.380(5) . ?
C10 C10 1.468(6) 2 ?
C10 S1 1.733(3) . ?
C11 C12 1.437(4) . ?
C11 S2 1.770(3) . ?
C12 S3 1.757(3) . ?
C13 C14 1.509(6) . ?
C13 S2 1.802(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 S3 1.807(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
 
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
C6 C1 C2 117.6(3) . . ?
C6 C1 C9 120.0(3) . . ?
C2 C1 C9 122.4(3) . . ?
O1 C2 C3 123.7(3) . . ?
O1 C2 C1 115.9(3) . . ?
C3 C2 C1 120.4(3) . . ?
C2 C3 C4 120.3(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
O2 C4 C5 124.5(3) . . ?
O2 C4 C3 114.8(3) . . ?
C5 C4 C3 120.7(3) . . ?
C4 C5 C6 118.4(3) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C5 C6 C1 122.6(3) . . ?
C5 C6 H6 118.7 . . ?
C1 C6 H6 118.7 . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C9 C1 130.4(3) . . ?
C12 C9 S1 110.9(2) . . ?
C1 C9 S1 118.6(3) . . ?
C11 C10 C10 129.2(4) . 2 ?
C11 C10 S1 110.5(2) . . ?
C10 C10 S1 119.5(3) 2 . ?
C10 C11 C12 113.1(3) . . ?
C10 C11 S2 119.8(2) . . ?
C12 C11 S2 126.9(3) . . ?
C9 C12 C11 112.4(3) . . ?
C9 C12 S3 120.9(3) . . ?
C11 C12 S3 126.6(3) . . ?
C14 C13 S2 113.2(3) . . ?
C14 C13 H13A 108.9 . . ?
S2 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
S2 C13 H13B 108.9 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 S3 114.2(3) . . ?
C13 C14 H14A 108.7 . . ?
S3 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
S3 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C2 O1 C7 117.0(3) . . ?
C4 O2 C8 117.5(3) . . ?
C9 S1 C10 93.03(16) . . ?
C11 S2 C13 102.15(17) . . ?
C12 S3 C14 101.12(18) . . ?
 
_diffrn_measured_fraction_theta_max    0.983
_diffrn_reflns_theta_full              27.34
_diffrn_measured_fraction_theta_full   0.983
_refine_diff_density_max    0.699
_refine_diff_density_min   -0.382
_refine_diff_density_rms    0.096
