data_global

loop_
_publ_author_name
'Manabu Hoshino'
'Shunsuke Nozawa'
'Tokushi Sato'
'Ayana Tomita'
'Shin-ichi Adachi'
'Shin-ya Koshihara'

_publ_contact_author_name        'Manabu Hoshino'
_publ_contact_author_address     
;
Department of Chemistry and Materials Science
Tokyo Institute of Technology 
Oh-okayama
Meguro-ku
Tokyo
152-8551
JAPAN
;

_publ_contact_author_email       mhoshino@chem.titech.ac.jp

_publ_requested_journal          'RSC Adv.'
 
data_off150ps 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2130(1) 
_cell_length_b                    7.5860(1) 
_cell_length_c                    14.4840(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1270(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.499(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.911 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.654 
_exptl_absorpt_correction_type   multi-scan 
_exptl_absorpt_correction_T_min   0.91526 
_exptl_absorpt_correction_T_max   0.92451 
_exptl_absorpt_process_details   'PLATON-MULABS was used (A.L.Spek, 2008)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46254 
_diffrn_reflns_av_R_equivalents   0.0326 
_diffrn_reflns_av_sigmaI/netI     0.0278 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.55 
_reflns_number_total              11103 
_reflns_number_gt                 10174 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0280P)²+0.0948P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.42(16) 
_refine_ls_number_reflns          11103 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0229 
_refine_ls_R_factor_gt            0.0206 
_refine_ls_wR_factor_ref          0.0587 
_refine_ls_wR_factor_gt           0.0578 
_refine_ls_goodness_of_fit_ref    1.082 
_refine_ls_restrained_S_all       1.082 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
S4 S 0.39005(10) 0.23665(10) 0.01869(5) 0.00722(2) Uani 1 1 d . . . 
S5 S 0.44696(10) 0.44163(10) -0.14741(5) 0.00659(2) Uani 1 1 d . . . 
S11 S 0.62062(10) 0.76381(10) -0.01358(5) 0.00722(2) Uani 1 1 d . . . 
S12 S 0.56303(10) 0.55834(10) 0.15292(5) 0.00659(2) Uani 1 1 d . . . 
C1 C 0.3137(4) 0.1414(4) -0.0910(2) 0.00820(6) Uani 1 1 d . . . 
H6 H 0.2540 0.0294 -0.0969 0.010 Uiso 1 1 calc R . . 
C2 C 0.4672(4) 0.4326(4) -0.0262(2) 0.00689(5) Uani 1 1 d . . . 
C3 C 0.3435(4) 0.2336(4) -0.1656(2) 0.00804(8) Uani 1 1 d . . . 
H7 H 0.3095 0.1875 -0.2269 0.010 Uiso 1 1 calc R . . 
C8 C 0.6934(4) 0.8579(4) 0.0957(2) 0.00820(6) Uani 1 1 d . . . 
H13 H 0.7461 0.9729 0.1018 0.010 Uiso 1 1 calc R . . 
C9 C 0.5424(4) 0.5674(4) 0.0305(2) 0.00689(5) Uani 1 1 d . . . 
C10 C 0.6722(4) 0.7613(4) 0.1713(2) 0.00804(8) Uani 1 1 d . . . 
H14 H 0.7157 0.8032 0.2327 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08194(9) 0.44968(11) -0.21517(4) 0.00890(2) Uani 1 1 d . . . 
Cl20 Cl -0.16400(10) 0.14246(9) -0.07915(5) 0.00797(2) Uani 1 1 d . . . 
Cl25 Cl 0.09202(9) 0.54987(11) 0.22039(4) 0.00890(2) Uani 1 1 d . . . 
Cl26 Cl 0.17519(10) 0.85767(9) 0.08460(5) 0.00797(2) Uani 1 1 d . . . 
O18 O 0.0944(4) 0.7526(3) -0.1119(2) 0.00980(5) Uani 1 1 d . . . 
O24 O -0.0856(4) 0.2471(3) 0.1174(2) 0.00980(5) Uani 1 1 d . . . 
C15 C 0.0512(4) 0.6374(3) -0.0594(2) 0.00620(5) Uani 1 1 d . . . 
C16 C -0.0366(4) 0.4715(4) -0.0962(2) 0.00613(5) Uani 1 1 d . . . 
C17 C -0.0755(4) 0.3401(4) -0.0390(2) 0.00578(5) Uani 1 1 d . . . 
C21 C -0.0382(4) 0.3590(3) 0.0657(2) 0.00620(5) Uani 1 1 d . . . 
C22 C 0.0505(4) 0.5290(4) 0.1017(2) 0.00613(5) Uani 1 1 d . . . 
C23 C 0.0850(4) 0.6589(4) 0.0423(2) 0.00578(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C2 1.749(3) . ? 
S4 C1 1.752(3) . ? 
S5 C2 1.739(3) . ? 
S5 C3 1.748(3) . ? 
S11 C8 1.740(3) . ? 
S11 C9 1.749(3) . ? 
S12 C10 1.731(3) . ? 
S12 C9 1.757(3) . ? 
S12 Cl26 3.6171(11) . ? 
S12 Cl25 3.6817(11) . ? 
C1 C3 1.333(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3684(7) . ? 
C2 C15 3.345(4) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.346(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.710(3) . ? 
Cl19 S5 3.6840(11) 1_455 ? 
Cl20 C17 1.696(3) . ? 
Cl20 S11 3.4691(11) 1_445 ? 
Cl20 S5 3.6225(11) 1_455 ? 
Cl25 C22 1.706(3) . ? 
Cl26 C23 1.716(3) . ? 
Cl26 S4 3.4711(11) 1_565 ? 
O18 C15 1.230(4) . ? 
O24 C21 1.217(4) . ? 
C15 C23 1.464(4) . ? 
C15 C16 1.471(4) . ? 
C16 C17 1.354(4) . ? 
C17 C21 1.503(4) . ? 
C21 C22 1.496(4) . ? 
C21 C9 3.379(4) 1_455 ? 
C22 C23 1.356(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 S4 C1 94.95(15) . . ? 
C2 S5 C3 94.71(15) . . ? 
C8 S11 C9 94.91(15) . . ? 
C10 S12 C9 94.81(15) . . ? 
C10 S12 Cl26 78.27(11) . . ? 
C9 S12 Cl26 76.21(11) . . ? 
C10 S12 Cl25 113.03(10) . . ? 
C9 S12 Cl25 109.55(11) . . ? 
Cl26 S12 Cl25 51.49(2) . . ? 
C3 C1 S4 116.8(2) . . ? 
C3 C1 H6 121.6 . . ? 
S4 C1 H6 121.6 . . ? 
C9 C2 S5 122.58(10) . . ? 
C9 C2 S4 122.06(11) . . ? 
S5 C2 S4 115.35(16) . . ? 
C9 C2 C15 90.03(8) . . ? 
S5 C2 C15 84.67(12) . . ? 
S4 C2 C15 96.72(13) . . ? 
C1 C3 S5 118.1(3) . . ? 
C1 C3 H7 120.9 . . ? 
S5 C3 H7 120.9 . . ? 
C10 C8 S11 117.4(2) . . ? 
C10 C8 H13 121.3 . . ? 
S11 C8 H13 121.3 . . ? 
C2 C9 S11 122.49(11) . . ? 
C2 C9 S12 122.61(10) . . ? 
S11 C9 S12 114.89(16) . . ? 
C8 C10 S12 117.8(3) . . ? 
C8 C10 H14 121.1 . . ? 
S12 C10 H14 121.1 . . ? 
C16 Cl19 S5 76.72(10) . 1_455 ? 
C17 Cl20 S11 143.00(10) . 1_445 ? 
C17 Cl20 S5 76.87(10) . 1_455 ? 
S11 Cl20 S5 103.43(3) 1_445 1_455 ? 
C22 Cl25 S12 75.88(10) . . ? 
C23 Cl26 S4 142.19(10) . 1_565 ? 
C23 Cl26 S12 77.23(10) . . ? 
S4 Cl26 S12 103.62(3) 1_565 . ? 
O18 C15 C23 121.7(3) . . ? 
O18 C15 C16 121.3(3) . . ? 
C23 C15 C16 117.0(2) . . ? 
O18 C15 C2 96.3(2) . . ? 
C23 C15 C2 84.53(17) . . ? 
C16 C15 C2 88.81(18) . . ? 
C17 C16 C15 121.8(3) . . ? 
C17 C16 Cl19 121.4(2) . . ? 
C15 C16 Cl19 116.8(2) . . ? 
C16 C17 C21 121.7(3) . . ? 
C16 C17 Cl20 122.9(2) . . ? 
C21 C17 Cl20 115.3(2) . . ? 
O24 C21 C22 122.3(3) . . ? 
O24 C21 C17 122.1(3) . . ? 
C22 C21 C17 115.6(2) . . ? 
O24 C21 C9 95.0(2) . 1_455 ? 
C22 C21 C9 88.40(18) . 1_455 ? 
C17 C21 C9 83.10(17) . 1_455 ? 
C23 C22 C21 121.1(3) . . ? 
C23 C22 Cl25 123.4(2) . . ? 
C21 C22 Cl25 115.4(2) . . ? 
C22 C23 C15 122.6(3) . . ? 
C22 C23 Cl26 120.6(2) . . ? 
C15 C23 Cl26 116.8(2) . . ? 
 
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 
C2 S4 C1 C3 3.0(3) . . . . ? 
C3 S5 C2 C9 -179.72(12) . . . . ? 
C3 S5 C2 S4 1.8(2) . . . . ? 
C3 S5 C2 C15 -93.10(13) . . . . ? 
C1 S4 C2 C9 178.80(13) . . . . ? 
C1 S4 C2 S5 -2.7(2) . . . . ? 
C1 S4 C2 C15 84.53(14) . . . . ? 
S4 C1 C3 S5 -2.2(4) . . . . ? 
C2 S5 C3 C1 0.2(3) . . . . ? 
C9 S11 C8 C10 0.8(3) . . . . ? 
S5 C2 C9 S11 1.49(8) . . . . ? 
S4 C2 C9 S11 179.9(2) . . . . ? 
C15 C2 C9 S11 -82.20(14) . . . . ? 
S5 C2 C9 S12 -180.0(3) . . . . ? 
S4 C2 C9 S12 -1.62(8) . . . . ? 
C15 C2 C9 S12 96.33(16) . . . . ? 
C8 S11 C9 C2 -179.35(13) . . . . ? 
C8 S11 C9 S12 2.0(2) . . . . ? 
C10 S12 C9 C2 177.94(13) . . . . ? 
Cl26 S12 C9 C2 -105.40(9) . . . . ? 
Cl25 S12 C9 C2 -65.54(10) . . . . ? 
C10 S12 C9 S11 -3.4(2) . . . . ? 
Cl26 S12 C9 S11 73.23(16) . . . . ? 
Cl25 S12 C9 S11 113.09(15) . . . . ? 
S11 C8 C10 S12 -3.5(4) . . . . ? 
C9 S12 C10 C8 4.1(3) . . . . ? 
Cl26 S12 C10 C8 -70.7(2) . . . . ? 
Cl25 S12 C10 C8 -109.5(2) . . . . ? 
C10 S12 Cl25 C22 112.08(17) . . . . ? 
C9 S12 Cl25 C22 7.75(14) . . . . ? 
Cl26 S12 Cl25 C22 60.45(10) . . . . ? 
C10 S12 Cl26 C23 166.62(15) . . . . ? 
C9 S12 Cl26 C23 68.62(13) . . . . ? 
Cl25 S12 Cl26 C23 -60.85(10) . . . . ? 
C10 S12 Cl26 S4 25.49(12) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.51(10) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.01(3) . . . 1_565 ? 
C9 C2 C15 O18 73.99(19) . . . . ? 
S5 C2 C15 O18 -48.7(2) . . . . ? 
S4 C2 C15 O18 -163.7(2) . . . . ? 
C9 C2 C15 C23 -47.34(16) . . . . ? 
S5 C2 C15 C23 -170.07(18) . . . . ? 
S4 C2 C15 C23 74.97(19) . . . . ? 
C9 C2 C15 C16 -164.62(16) . . . . ? 
S5 C2 C15 C16 72.64(18) . . . . ? 
S4 C2 C15 C16 -42.32(19) . . . . ? 
O18 C15 C16 C17 176.4(3) . . . . ? 
C23 C15 C16 C17 -3.4(4) . . . . ? 
C2 C15 C16 C17 79.8(3) . . . . ? 
O18 C15 C16 Cl19 -2.0(4) . . . . ? 
C23 C15 C16 Cl19 178.2(2) . . . . ? 
C2 C15 C16 Cl19 -98.57(19) . . . . ? 
S5 Cl19 C16 C17 65.4(2) 1_455 . . . ? 
S5 Cl19 C16 C15 -116.2(2) 1_455 . . . ? 
C15 C16 C17 C21 2.4(4) . . . . ? 
Cl19 C16 C17 C21 -179.3(2) . . . . ? 
C15 C16 C17 Cl20 -176.1(2) . . . . ? 
Cl19 C16 C17 Cl20 2.2(4) . . . . ? 
S11 Cl20 C17 C16 -165.11(18) 1_445 . . . ? 
S5 Cl20 C17 C16 -70.1(2) 1_455 . . . ? 
S11 Cl20 C17 C21 16.3(3) 1_445 . . . ? 
S5 Cl20 C17 C21 111.3(2) 1_455 . . . ? 
C16 C17 C21 O24 174.4(3) . . . . ? 
Cl20 C17 C21 O24 -7.0(4) . . . . ? 
C16 C17 C21 C22 -2.1(4) . . . . ? 
Cl20 C17 C21 C22 176.5(2) . . . . ? 
C16 C17 C21 C9 82.8(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -98.58(18) . . . 1_455 ? 
O24 C21 C22 C23 -173.4(3) . . . . ? 
C17 C21 C22 C23 3.1(4) . . . . ? 
C9 C21 C22 C23 -78.5(3) 1_455 . . . ? 
O24 C21 C22 Cl25 3.5(4) . . . . ? 
C17 C21 C22 Cl25 179.9(2) . . . . ? 
C9 C21 C22 Cl25 98.32(19) 1_455 . . . ? 
S12 Cl25 C22 C23 -67.0(2) . . . . ? 
S12 Cl25 C22 C21 116.3(2) . . . . ? 
C21 C22 C23 C15 -4.4(4) . . . . ? 
Cl25 C22 C23 C15 179.0(2) . . . . ? 
C21 C22 C23 Cl26 176.5(2) . . . . ? 
Cl25 C22 C23 Cl26 0.0(4) . . . . ? 
O18 C15 C23 C22 -175.4(3) . . . . ? 
C16 C15 C23 C22 4.5(4) . . . . ? 
C2 C15 C23 C22 -81.4(3) . . . . ? 
O18 C15 C23 Cl26 3.7(4) . . . . ? 
C16 C15 C23 Cl26 -176.4(2) . . . . ? 
C2 C15 C23 Cl26 97.71(19) . . . . ? 
S4 Cl26 C23 C22 164.55(18) 1_565 . . . ? 
S12 Cl26 C23 C22 68.7(2) . . . . ? 
S4 Cl26 C23 C15 -14.5(3) 1_565 . . . ? 
S12 Cl26 C23 C15 -110.4(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.39 3.338(4) 178.2 1_545 
C8 H13 O24  0.95 2.40 3.346(4) 173.2 1_665 
C10 H14 O18  0.95 2.58 3.278(4) 131.0 2_565 
C3 H7 O24  0.95 2.54 3.267(4) 133.6 2_554 
 
_diffrn_measured_fraction_theta_max    0.902 
_diffrn_reflns_theta_full              33.55 
_diffrn_measured_fraction_theta_full   0.902 
_refine_diff_density_max    0.701 
_refine_diff_density_min   -0.487 
_refine_diff_density_rms    0.076 

#==END

 
data_on150ps 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2140(1) 
_cell_length_b                    7.5870(1) 
_cell_length_c                    14.4850(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1310(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.756(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.910 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.654 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91612 
_exptl_absorpt_correction_T_max   0.92618 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46260 
_diffrn_reflns_av_R_equivalents   0.0330 
_diffrn_reflns_av_sigmaI/netI     0.0281 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.56 
_reflns_number_total              11104 
_reflns_number_gt                 10153 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0288P)²+0.0854P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.50(17) 
_refine_ls_number_reflns          11104 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0232 
_refine_ls_R_factor_gt            0.0209 
_refine_ls_wR_factor_ref          0.0593 
_refine_ls_wR_factor_gt           0.0583 
_refine_ls_goodness_of_fit_ref    1.081 
_refine_ls_restrained_S_all       1.081 
_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 
S4 S 0.39004(10) 0.23665(11) 0.01871(5) 0.00745(2) Uani 1 1 d . . . 
S5 S 0.44700(10) 0.44163(10) -0.14746(5) 0.00685(2) Uani 1 1 d . . . 
S11 S 0.62054(10) 0.76376(11) -0.01355(5) 0.00745(2) Uani 1 1 d . . . 
S12 S 0.56313(10) 0.55832(10) 0.15285(5) 0.00685(2) Uani 1 1 d . . . 
C1 C 0.3143(5) 0.1416(4) -0.0906(2) 0.00857(5) Uani 1 1 d . . . 
H6 H 0.2546 0.0296 -0.0966 0.010 Uiso 1 1 calc R . . 
C2 C 0.4674(4) 0.4330(4) -0.0260(2) 0.00709(5) Uani 1 1 d . . . 
C3 C 0.3443(4) 0.2337(5) -0.1651(2) 0.00829(8) Uani 1 1 d . . . 
H7 H 0.3105 0.1873 -0.2264 0.010 Uiso 1 1 calc R . . 
C8 C 0.6938(5) 0.8580(4) 0.0961(2) 0.00857(5) Uani 1 1 d . . . 
H13 H 0.7464 0.9730 0.1022 0.010 Uiso 1 1 calc R . . 
C9 C 0.5426(4) 0.5676(4) 0.0307(2) 0.00709(5) Uani 1 1 d . . . 
C10 C 0.6729(4) 0.7612(5) 0.1718(2) 0.00829(8) Uani 1 1 d . . . 
H14 H 0.7167 0.8027 0.2332 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08194(9) 0.44967(11) -0.21526(5) 0.00922(2) Uani 1 1 d . . . 
Cl20 Cl -0.16409(10) 0.14245(10) -0.07910(5) 0.00827(2) Uani 1 1 d . . . 
Cl25 Cl 0.09208(9) 0.54977(11) 0.22030(5) 0.00922(2) Uani 1 1 d . . . 
Cl26 Cl 0.17502(10) 0.85762(10) 0.08466(5) 0.00827(2) Uani 1 1 d . . . 
O18 O 0.0944(4) 0.7527(3) -0.1115(2) 0.01006(5) Uani 1 1 d . . . 
O24 O -0.0853(4) 0.2472(3) 0.1177(2) 0.01006(5) Uani 1 1 d . . . 
C15 C 0.0508(4) 0.6378(4) -0.0596(2) 0.00641(5) Uani 1 1 d . . . 
C16 C -0.0364(4) 0.4716(4) -0.0961(2) 0.00633(5) Uani 1 1 d . . . 
C17 C -0.0757(4) 0.3404(4) -0.0390(2) 0.00593(5) Uani 1 1 d . . . 
C21 C -0.0383(4) 0.3594(4) 0.0654(2) 0.00641(5) Uani 1 1 d . . . 
C22 C 0.0506(4) 0.5291(4) 0.1018(2) 0.00633(5) Uani 1 1 d . . . 
C23 C 0.0847(4) 0.6592(4) 0.0424(2) 0.00593(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C1 1.746(3) . ? 
S4 C2 1.751(3) . ? 
S5 C2 1.743(3) . ? 
S5 C3 1.745(3) . ? 
S11 C8 1.745(3) . ? 
S11 C9 1.748(3) . ? 
S12 C10 1.733(3) . ? 
S12 C9 1.754(3) . ? 
S12 Cl26 3.6185(11) . ? 
S12 Cl25 3.6823(11) . ? 
C1 C3 1.333(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3681(7) . ? 
C2 C15 3.349(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.347(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.713(3) . ? 
Cl19 S5 3.6845(11) 1_455 ? 
Cl20 C17 1.698(3) . ? 
Cl20 S11 3.4696(11) 1_445 ? 
Cl20 S5 3.6225(11) 1_455 ? 
Cl25 C22 1.702(3) . ? 
Cl26 C23 1.714(3) . ? 
Cl26 S4 3.4725(11) 1_565 ? 
O18 C15 1.224(4) . ? 
O24 C21 1.222(4) . ? 
C15 C23 1.467(4) . ? 
C15 C16 1.470(4) . ? 
C16 C17 1.353(4) . ? 
C17 C21 1.500(4) . ? 
C21 C22 1.496(4) . ? 
C21 C9 3.377(5) 1_455 ? 
C22 C23 1.357(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C1 S4 C2 95.06(16) . . ? 
C2 S5 C3 94.58(15) . . ? 
C8 S11 C9 94.80(16) . . ? 
C10 S12 C9 94.99(15) . . ? 
C10 S12 Cl26 78.47(11) . . ? 
C9 S12 Cl26 76.21(11) . . ? 
C10 S12 Cl25 113.06(10) . . ? 
C9 S12 Cl25 109.56(11) . . ? 
Cl26 S12 Cl25 51.45(2) . . ? 
C3 C1 S4 116.7(3) . . ? 
C3 C1 H6 121.6 . . ? 
S4 C1 H6 121.6 . . ? 
C9 C2 S5 122.69(10) . . ? 
C9 C2 S4 122.16(11) . . ? 
S5 C2 S4 115.14(16) . . ? 
C9 C2 C15 90.12(8) . . ? 
S5 C2 C15 84.62(12) . . ? 
S4 C2 C15 96.73(14) . . ? 
C1 C3 S5 118.4(2) . . ? 
C1 C3 H7 120.8 . . ? 
S5 C3 H7 120.8 . . ? 
C10 C8 S11 117.4(3) . . ? 
C10 C8 H13 121.3 . . ? 
S11 C8 H13 121.3 . . ? 
C2 C9 S11 122.37(11) . . ? 
C2 C9 S12 122.54(10) . . ? 
S11 C9 S12 115.07(16) . . ? 
C8 C10 S12 117.6(2) . . ? 
C8 C10 H14 121.2 . . ? 
S12 C10 H14 121.2 . . ? 
C16 Cl19 S5 76.73(10) . 1_455 ? 
C17 Cl20 S11 143.02(10) . 1_445 ? 
C17 Cl20 S5 76.80(10) . 1_455 ? 
S11 Cl20 S5 103.45(3) 1_445 1_455 ? 
C22 Cl25 S12 75.88(10) . . ? 
C23 Cl26 S4 142.19(10) . 1_565 ? 
C23 Cl26 S12 77.29(10) . . ? 
S4 Cl26 S12 103.58(3) 1_565 . ? 
O18 C15 C23 121.4(3) . . ? 
O18 C15 C16 121.8(3) . . ? 
C23 C15 C16 116.8(2) . . ? 
O18 C15 C2 96.2(2) . . ? 
C23 C15 C2 84.43(18) . . ? 
C16 C15 C2 88.70(18) . . ? 
C17 C16 C15 122.0(3) . . ? 
C17 C16 Cl19 121.3(2) . . ? 
C15 C16 Cl19 116.7(2) . . ? 
C16 C17 C21 121.6(3) . . ? 
C16 C17 Cl20 123.0(2) . . ? 
C21 C17 Cl20 115.3(2) . . ? 
O24 C21 C22 121.8(3) . . ? 
O24 C21 C17 122.3(3) . . ? 
C22 C21 C17 115.8(2) . . ? 
O24 C21 C9 95.1(2) . 1_455 ? 
C22 C21 C9 88.49(18) . 1_455 ? 
C17 C21 C9 83.17(17) . 1_455 ? 
C23 C22 C21 120.9(3) . . ? 
C23 C22 Cl25 123.5(2) . . ? 
C21 C22 Cl25 115.5(2) . . ? 
C22 C23 C15 122.7(3) . . ? 
C22 C23 Cl26 120.6(2) . . ? 
C15 C23 Cl26 116.7(2) . . ? 
 
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 
C2 S4 C1 C3 3.0(3) . . . . ? 
C3 S5 C2 C9 -179.87(12) . . . . ? 
C3 S5 C2 S4 1.7(2) . . . . ? 
C3 S5 C2 C15 -93.19(13) . . . . ? 
C1 S4 C2 C9 178.91(13) . . . . ? 
C1 S4 C2 S5 -2.7(2) . . . . ? 
C1 S4 C2 C15 84.51(14) . . . . ? 
S4 C1 C3 S5 -2.3(4) . . . . ? 
C2 S5 C3 C1 0.4(3) . . . . ? 
C9 S11 C8 C10 0.9(3) . . . . ? 
S5 C2 C9 S11 1.58(8) . . . . ? 
S4 C2 C9 S11 179.9(3) . . . . ? 
C15 C2 C9 S11 -82.10(14) . . . . ? 
S5 C2 C9 S12 -179.9(3) . . . . ? 
S4 C2 C9 S12 -1.64(8) . . . . ? 
C15 C2 C9 S12 96.39(16) . . . . ? 
C8 S11 C9 C2 -179.32(13) . . . . ? 
C8 S11 C9 S12 2.1(2) . . . . ? 
C10 S12 C9 C2 177.83(13) . . . . ? 
Cl26 S12 C9 C2 -105.35(9) . . . . ? 
Cl25 S12 C9 C2 -65.54(10) . . . . ? 
C10 S12 C9 S11 -3.6(2) . . . . ? 
Cl26 S12 C9 S11 73.25(16) . . . . ? 
Cl25 S12 C9 S11 113.06(16) . . . . ? 
S11 C8 C10 S12 -3.6(3) . . . . ? 
C9 S12 C10 C8 4.3(3) . . . . ? 
Cl26 S12 C10 C8 -70.5(2) . . . . ? 
Cl25 S12 C10 C8 -109.4(2) . . . . ? 
C10 S12 Cl25 C22 112.37(17) . . . . ? 
C9 S12 Cl25 C22 7.80(15) . . . . ? 
Cl26 S12 Cl25 C22 60.45(11) . . . . ? 
C10 S12 Cl26 C23 166.85(16) . . . . ? 
C9 S12 Cl26 C23 68.72(14) . . . . ? 
Cl25 S12 Cl26 C23 -60.81(11) . . . . ? 
C10 S12 Cl26 S4 25.71(11) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.42(10) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.05(3) . . . 1_565 ? 
C9 C2 C15 O18 73.70(19) . . . . ? 
S5 C2 C15 O18 -49.1(2) . . . . ? 
S4 C2 C15 O18 -163.9(2) . . . . ? 
C9 C2 C15 C23 -47.40(16) . . . . ? 
S5 C2 C15 C23 -170.23(18) . . . . ? 
S4 C2 C15 C23 75.03(19) . . . . ? 
C9 C2 C15 C16 -164.48(16) . . . . ? 
S5 C2 C15 C16 72.69(19) . . . . ? 
S4 C2 C15 C16 -42.1(2) . . . . ? 
O18 C15 C16 C17 176.4(3) . . . . ? 
C23 C15 C16 C17 -3.1(4) . . . . ? 
C2 C15 C16 C17 80.0(3) . . . . ? 
O18 C15 C16 Cl19 -2.3(4) . . . . ? 
C23 C15 C16 Cl19 178.2(2) . . . . ? 
C2 C15 C16 Cl19 -98.7(2) . . . . ? 
S5 Cl19 C16 C17 65.3(2) 1_455 . . . ? 
S5 Cl19 C16 C15 -116.0(2) 1_455 . . . ? 
C15 C16 C17 C21 2.1(4) . . . . ? 
Cl19 C16 C17 C21 -179.3(2) . . . . ? 
C15 C16 C17 Cl20 -176.2(2) . . . . ? 
Cl19 C16 C17 Cl20 2.5(4) . . . . ? 
S11 Cl20 C17 C16 -165.22(19) 1_445 . . . ? 
S5 Cl20 C17 C16 -70.3(3) 1_455 . . . ? 
S11 Cl20 C17 C21 16.4(3) 1_445 . . . ? 
S5 Cl20 C17 C21 111.4(2) 1_455 . . . ? 
C16 C17 C21 O24 174.7(3) . . . . ? 
Cl20 C17 C21 O24 -7.0(4) . . . . ? 
C16 C17 C21 C22 -2.0(4) . . . . ? 
Cl20 C17 C21 C22 176.4(2) . . . . ? 
C16 C17 C21 C9 83.0(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -98.65(19) . . . 1_455 ? 
O24 C21 C22 C23 -173.4(3) . . . . ? 
C17 C21 C22 C23 3.3(4) . . . . ? 
C9 C21 C22 C23 -78.4(3) 1_455 . . . ? 
O24 C21 C22 Cl25 3.2(4) . . . . ? 
C17 C21 C22 Cl25 179.9(2) . . . . ? 
C9 C21 C22 Cl25 98.19(19) 1_455 . . . ? 
S12 Cl25 C22 C23 -67.1(3) . . . . ? 
S12 Cl25 C22 C21 116.4(2) . . . . ? 
C21 C22 C23 C15 -4.7(4) . . . . ? 
Cl25 C22 C23 C15 179.0(2) . . . . ? 
C21 C22 C23 Cl26 176.5(2) . . . . ? 
Cl25 C22 C23 Cl26 0.2(4) . . . . ? 
O18 C15 C23 C22 -175.1(3) . . . . ? 
C16 C15 C23 C22 4.5(4) . . . . ? 
C2 C15 C23 C22 -81.2(3) . . . . ? 
O18 C15 C23 Cl26 3.8(4) . . . . ? 
C16 C15 C23 Cl26 -176.7(2) . . . . ? 
C2 C15 C23 Cl26 97.63(19) . . . . ? 
S4 Cl26 C23 C22 164.40(18) 1_565 . . . ? 
S12 Cl26 C23 C22 68.6(2) . . . . ? 
S4 Cl26 C23 C15 -14.5(3) 1_565 . . . ? 
S12 Cl26 C23 C15 -110.3(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.39 3.340(4) 178.1 1_545 
C8 H13 O24  0.95 2.40 3.347(4) 173.2 1_665 
C10 H14 O18  0.95 2.58 3.280(4) 130.9 2_565 
C3 H7 O24  0.95 2.54 3.268(4) 133.6 2_554 
 
_diffrn_measured_fraction_theta_max    0.902 
_diffrn_reflns_theta_full              33.56 
_diffrn_measured_fraction_theta_full   0.902 
_refine_diff_density_max    0.721 
_refine_diff_density_min   -0.413 
_refine_diff_density_rms    0.075 

#==END

 
data_off500ps 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2130(1) 
_cell_length_b                    7.5860(1) 
_cell_length_c                    14.4840(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1250(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.503(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.911 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.654 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91462 
_exptl_absorpt_correction_T_max   0.92637 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46232 
_diffrn_reflns_av_R_equivalents   0.0329 
_diffrn_reflns_av_sigmaI/netI     0.0283 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.54 
_reflns_number_total              11099 
_reflns_number_gt                 10113 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0297P)²+0.0653P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.50(17) 
_refine_ls_number_reflns          11099 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0235 
_refine_ls_R_factor_gt            0.0210 
_refine_ls_wR_factor_ref          0.0603 
_refine_ls_wR_factor_gt           0.0593 
_refine_ls_goodness_of_fit_ref    1.097 
_refine_ls_restrained_S_all       1.097 
_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 
S4 S 0.39008(11) 0.23677(10) 0.01868(5) 0.00722(2) Uani 1 1 d . . . 
S5 S 0.44691(10) 0.44157(10) -0.14739(5) 0.00661(2) Uani 1 1 d . . . 
S11 S 0.62067(10) 0.76391(10) -0.01359(5) 0.00722(2) Uani 1 1 d . . . 
S12 S 0.56299(10) 0.55828(10) 0.15295(5) 0.00661(2) Uani 1 1 d . . . 
C1 C 0.3145(5) 0.1411(4) -0.0908(2) 0.00832(5) Uani 1 1 d . . . 
H6 H 0.2559 0.0287 -0.0967 0.010 Uiso 1 1 calc R . . 
C2 C 0.4671(4) 0.4324(4) -0.0261(2) 0.00693(5) Uani 1 1 d . . . 
C3 C 0.3433(4) 0.2336(4) -0.1654(2) 0.00808(8) Uani 1 1 d . . . 
H7 H 0.3084 0.1878 -0.2267 0.010 Uiso 1 1 calc R . . 
C8 C 0.6940(5) 0.8577(4) 0.0959(3) 0.00832(5) Uani 1 1 d . . . 
H13 H 0.7475 0.9724 0.1020 0.010 Uiso 1 1 calc R . . 
C9 C 0.5422(4) 0.5670(4) 0.0307(2) 0.00693(5) Uani 1 1 d . . . 
C10 C 0.6720(4) 0.7613(4) 0.1715(2) 0.00808(8) Uani 1 1 d . . . 
H14 H 0.7148 0.8034 0.2330 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08194(9) 0.44963(11) -0.21529(5) 0.00890(2) Uani 1 1 d . . . 
Cl20 Cl -0.16399(10) 0.14253(10) -0.07912(5) 0.00798(2) Uani 1 1 d . . . 
Cl25 Cl 0.09201(9) 0.54984(11) 0.22028(5) 0.00890(2) Uani 1 1 d . . . 
Cl26 Cl 0.17520(10) 0.85772(10) 0.08462(5) 0.00798(2) Uani 1 1 d . . . 
O18 O 0.0945(4) 0.7529(3) -0.1118(2) 0.00976(5) Uani 1 1 d . . . 
O24 O -0.0855(4) 0.2474(3) 0.1174(2) 0.00976(5) Uani 1 1 d . . . 
C15 C 0.0504(4) 0.6379(4) -0.0593(2) 0.00622(5) Uani 1 1 d . . . 
C16 C -0.0361(4) 0.4719(4) -0.0960(2) 0.00606(6) Uani 1 1 d . . . 
C17 C -0.0756(4) 0.3397(4) -0.0387(2) 0.00576(5) Uani 1 1 d . . . 
C21 C -0.0388(4) 0.3595(4) 0.0658(2) 0.00622(5) Uani 1 1 d . . . 
C22 C 0.0510(4) 0.5294(4) 0.1019(2) 0.00606(6) Uani 1 1 d . . . 
C23 C 0.0850(4) 0.6586(4) 0.0426(2) 0.00576(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C2 1.745(3) . ? 
S4 C1 1.750(3) . ? 
S5 C2 1.741(3) . ? 
S5 C3 1.747(3) . ? 
S11 C8 1.742(3) . ? 
S11 C9 1.754(3) . ? 
S12 C10 1.731(3) . ? 
S12 C9 1.755(3) . ? 
S12 Cl26 3.6174(11) . ? 
S12 Cl25 3.6807(11) . ? 
C1 C3 1.332(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3675(7) . ? 
C2 C15 3.352(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.348(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.715(3) . ? 
Cl19 S5 3.6852(11) 1_455 ? 
Cl20 C17 1.693(3) . ? 
Cl20 S11 3.4685(11) 1_445 ? 
Cl20 S5 3.6222(11) 1_455 ? 
Cl25 C22 1.700(3) . ? 
Cl26 C23 1.718(3) . ? 
Cl26 S4 3.4717(11) 1_565 ? 
O18 C15 1.232(4) . ? 
O24 C21 1.215(4) . ? 
C15 C23 1.466(4) . ? 
C15 C16 1.467(4) . ? 
C16 C17 1.360(4) . ? 
C17 C21 1.502(4) . ? 
C21 C22 1.499(4) . ? 
C21 C9 3.374(5) 1_455 ? 
C22 C23 1.351(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 S4 C1 95.04(15) . . ? 
C2 S5 C3 94.58(15) . . ? 
C8 S11 C9 94.84(15) . . ? 
C10 S12 C9 95.01(15) . . ? 
C10 S12 Cl26 78.23(12) . . ? 
C9 S12 Cl26 76.20(11) . . ? 
C10 S12 Cl25 112.94(11) . . ? 
C9 S12 Cl25 109.47(11) . . ? 
Cl26 S12 Cl25 51.48(2) . . ? 
C3 C1 S4 116.7(3) . . ? 
C3 C1 H6 121.6 . . ? 
S4 C1 H6 121.6 . . ? 
C9 C2 S5 122.59(10) . . ? 
C9 C2 S4 122.04(11) . . ? 
S5 C2 S4 115.34(16) . . ? 
C9 C2 C15 89.98(8) . . ? 
S5 C2 C15 84.67(13) . . ? 
S4 C2 C15 96.77(13) . . ? 
C1 C3 S5 118.2(3) . . ? 
C1 C3 H7 120.9 . . ? 
S5 C3 H7 120.9 . . ? 
C10 C8 S11 117.4(3) . . ? 
C10 C8 H13 121.3 . . ? 
S11 C8 H13 121.3 . . ? 
C2 C9 S11 122.41(11) . . ? 
C2 C9 S12 122.74(10) . . ? 
S11 C9 S12 114.84(16) . . ? 
C8 C10 S12 117.8(3) . . ? 
C8 C10 H14 121.1 . . ? 
S12 C10 H14 121.1 . . ? 
C16 Cl19 S5 76.79(10) . 1_455 ? 
C17 Cl20 S11 142.87(11) . 1_445 ? 
C17 Cl20 S5 76.94(11) . 1_455 ? 
S11 Cl20 S5 103.42(3) 1_445 1_455 ? 
C22 Cl25 S12 75.81(10) . . ? 
C23 Cl26 S4 142.33(11) . 1_565 ? 
C23 Cl26 S12 77.15(11) . . ? 
S4 Cl26 S12 103.64(3) 1_565 . ? 
O18 C15 C23 121.8(3) . . ? 
O18 C15 C16 121.4(3) . . ? 
C23 C15 C16 116.8(2) . . ? 
O18 C15 C2 96.0(2) . . ? 
C23 C15 C2 84.24(18) . . ? 
C16 C15 C2 88.45(18) . . ? 
C17 C16 C15 122.0(3) . . ? 
C17 C16 Cl19 121.1(2) . . ? 
C15 C16 Cl19 116.9(2) . . ? 
C16 C17 C21 121.3(3) . . ? 
C16 C17 Cl20 123.0(2) . . ? 
C21 C17 Cl20 115.7(2) . . ? 
O24 C21 C22 122.2(3) . . ? 
O24 C21 C17 121.9(3) . . ? 
C22 C21 C17 115.8(2) . . ? 
O24 C21 C9 95.2(2) . 1_455 ? 
C22 C21 C9 88.77(18) . 1_455 ? 
C17 C21 C9 83.33(17) . 1_455 ? 
C23 C22 C21 120.9(3) . . ? 
C23 C22 Cl25 123.7(2) . . ? 
C21 C22 Cl25 115.3(2) . . ? 
C22 C23 C15 123.0(3) . . ? 
C22 C23 Cl26 120.6(2) . . ? 
C15 C23 Cl26 116.4(2) . . ? 
 
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 
C2 S4 C1 C3 2.5(3) . . . . ? 
C3 S5 C2 C9 -179.64(13) . . . . ? 
C3 S5 C2 S4 1.9(2) . . . . ? 
C3 S5 C2 C15 -93.08(13) . . . . ? 
C1 S4 C2 C9 178.98(13) . . . . ? 
C1 S4 C2 S5 -2.6(2) . . . . ? 
C1 S4 C2 C15 84.74(14) . . . . ? 
S4 C1 C3 S5 -1.6(4) . . . . ? 
C2 S5 C3 C1 -0.2(3) . . . . ? 
C9 S11 C8 C10 0.5(3) . . . . ? 
S5 C2 C9 S11 1.44(8) . . . . ? 
S4 C2 C9 S11 179.8(3) . . . . ? 
C15 C2 C9 S11 -82.22(14) . . . . ? 
S5 C2 C9 S12 -179.9(3) . . . . ? 
S4 C2 C9 S12 -1.58(8) . . . . ? 
C15 C2 C9 S12 96.40(16) . . . . ? 
C8 S11 C9 C2 -179.17(13) . . . . ? 
C8 S11 C9 S12 2.1(2) . . . . ? 
C10 S12 C9 C2 177.96(13) . . . . ? 
Cl26 S12 C9 C2 -105.48(9) . . . . ? 
Cl25 S12 C9 C2 -65.56(11) . . . . ? 
C10 S12 C9 S11 -3.3(2) . . . . ? 
Cl26 S12 C9 S11 73.24(16) . . . . ? 
Cl25 S12 C9 S11 113.16(16) . . . . ? 
S11 C8 C10 S12 -3.0(4) . . . . ? 
C9 S12 C10 C8 3.8(3) . . . . ? 
Cl26 S12 C10 C8 -71.0(3) . . . . ? 
Cl25 S12 C10 C8 -109.8(3) . . . . ? 
C10 S12 Cl25 C22 112.08(18) . . . . ? 
C9 S12 Cl25 C22 7.59(15) . . . . ? 
Cl26 S12 Cl25 C22 60.39(11) . . . . ? 
C10 S12 Cl26 C23 166.88(16) . . . . ? 
C9 S12 Cl26 C23 68.67(14) . . . . ? 
Cl25 S12 Cl26 C23 -60.68(11) . . . . ? 
C10 S12 Cl26 S4 25.62(12) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.60(10) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.05(3) . . . 1_565 ? 
C9 C2 C15 O18 74.0(2) . . . . ? 
S5 C2 C15 O18 -48.7(2) . . . . ? 
S4 C2 C15 O18 -163.7(2) . . . . ? 
C9 C2 C15 C23 -47.44(16) . . . . ? 
S5 C2 C15 C23 -170.19(18) . . . . ? 
S4 C2 C15 C23 74.86(19) . . . . ? 
C9 C2 C15 C16 -164.59(16) . . . . ? 
S5 C2 C15 C16 72.65(18) . . . . ? 
S4 C2 C15 C16 -42.3(2) . . . . ? 
O18 C15 C16 C17 176.2(3) . . . . ? 
C23 C15 C16 C17 -2.7(4) . . . . ? 
C2 C15 C16 C17 80.1(3) . . . . ? 
O18 C15 C16 Cl19 -2.7(4) . . . . ? 
C23 C15 C16 Cl19 178.5(2) . . . . ? 
C2 C15 C16 Cl19 -98.8(2) . . . . ? 
S5 Cl19 C16 C17 65.3(2) 1_455 . . . ? 
S5 Cl19 C16 C15 -115.8(2) 1_455 . . . ? 
C15 C16 C17 C21 2.2(4) . . . . ? 
Cl19 C16 C17 C21 -179.0(2) . . . . ? 
C15 C16 C17 Cl20 -176.4(2) . . . . ? 
Cl19 C16 C17 Cl20 2.4(4) . . . . ? 
S11 Cl20 C17 C16 -165.26(18) 1_445 . . . ? 
S5 Cl20 C17 C16 -70.2(3) 1_455 . . . ? 
S11 Cl20 C17 C21 16.0(3) 1_445 . . . ? 
S5 Cl20 C17 C21 111.1(2) 1_455 . . . ? 
C16 C17 C21 O24 174.8(3) . . . . ? 
Cl20 C17 C21 O24 -6.5(4) . . . . ? 
C16 C17 C21 C22 -2.6(4) . . . . ? 
Cl20 C17 C21 C22 176.2(2) . . . . ? 
C16 C17 C21 C9 82.8(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -98.42(19) . . . 1_455 ? 
O24 C21 C22 C23 -173.6(3) . . . . ? 
C17 C21 C22 C23 3.7(4) . . . . ? 
C9 C21 C22 C23 -78.3(3) 1_455 . . . ? 
O24 C21 C22 Cl25 2.7(4) . . . . ? 
C17 C21 C22 Cl25 -179.9(2) . . . . ? 
C9 C21 C22 Cl25 98.09(19) 1_455 . . . ? 
S12 Cl25 C22 C23 -67.1(3) . . . . ? 
S12 Cl25 C22 C21 116.6(2) . . . . ? 
C21 C22 C23 C15 -4.6(4) . . . . ? 
Cl25 C22 C23 C15 179.4(2) . . . . ? 
C21 C22 C23 Cl26 176.2(2) . . . . ? 
Cl25 C22 C23 Cl26 0.1(4) . . . . ? 
O18 C15 C23 C22 -174.9(3) . . . . ? 
C16 C15 C23 C22 3.9(4) . . . . ? 
C2 C15 C23 C22 -81.4(3) . . . . ? 
O18 C15 C23 Cl26 4.4(4) . . . . ? 
C16 C15 C23 Cl26 -176.8(2) . . . . ? 
C2 C15 C23 Cl26 97.9(2) . . . . ? 
S4 Cl26 C23 C22 164.41(18) 1_565 . . . ? 
S12 Cl26 C23 C22 68.7(2) . . . . ? 
S4 Cl26 C23 C15 -14.9(3) 1_565 . . . ? 
S12 Cl26 C23 C15 -110.7(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.39 3.336(4) 177.3 1_545 
C8 H13 O24  0.95 2.40 3.348(4) 173.9 1_665 
C10 H14 O18  0.95 2.57 3.275(5) 131.2 2_565 
C3 H7 O24  0.95 2.54 3.270(5) 133.4 2_554 
 
_diffrn_measured_fraction_theta_max    0.904 
_diffrn_reflns_theta_full              33.54 
_diffrn_measured_fraction_theta_full   0.904 
_refine_diff_density_max    0.723 
_refine_diff_density_min   -0.457 
_refine_diff_density_rms    0.077 

#==END

 
data_on500ps 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2140(1) 
_cell_length_b                    7.5870(1) 
_cell_length_c                    14.4850(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1300(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.758(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.910 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.654 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91520 
_exptl_absorpt_correction_T_max   0.92500 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46185 
_diffrn_reflns_av_R_equivalents   0.0342 
_diffrn_reflns_av_sigmaI/netI     0.0286 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.55 
_reflns_number_total              11111 
_reflns_number_gt                 10090 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0277P)²+0.0855P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.45(17) 
_refine_ls_number_reflns          11111 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0237 
_refine_ls_R_factor_gt            0.0209 
_refine_ls_wR_factor_ref          0.0595 
_refine_ls_wR_factor_gt           0.0584 
_refine_ls_goodness_of_fit_ref    1.089 
_refine_ls_restrained_S_all       1.089 
_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 
S4 S 0.39015(11) 0.23607(11) 0.01883(5) 0.00743(2) Uani 1 1 d . . . 
S5 S 0.44711(11) 0.44155(10) -0.14746(5) 0.00682(2) Uani 1 1 d . . . 
S11 S 0.62065(11) 0.76319(11) -0.01344(5) 0.00743(2) Uani 1 1 d . . . 
S12 S 0.56322(11) 0.55823(10) 0.15285(5) 0.00682(2) Uani 1 1 d . . . 
C1 C 0.3155(5) 0.1416(4) -0.0899(2) 0.00851(6) Uani 1 1 d . . . 
H6 H 0.2575 0.0289 -0.0960 0.010 Uiso 1 1 calc R . . 
C2 C 0.4677(5) 0.4317(4) -0.0259(2) 0.00705(5) Uani 1 1 d . . . 
C3 C 0.3442(4) 0.2365(4) -0.1653(2) 0.00838(7) Uani 1 1 d . . . 
H7 H 0.3085 0.1913 -0.2267 0.010 Uiso 1 1 calc R . . 
C8 C 0.6951(5) 0.8582(4) 0.0968(2) 0.00851(6) Uani 1 1 d . . . 
H13 H 0.7492 0.9726 0.1027 0.010 Uiso 1 1 calc R . . 
C9 C 0.5428(5) 0.5663(4) 0.0308(2) 0.00705(5) Uani 1 1 d . . . 
C10 C 0.6728(4) 0.7641(4) 0.1715(2) 0.00838(7) Uani 1 1 d . . . 
H14 H 0.7148 0.8068 0.2329 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08167(10) 0.44967(11) -0.21540(4) 0.00920(2) Uani 1 1 d . . . 
Cl20 Cl -0.16460(10) 0.14233(10) -0.07907(5) 0.00826(2) Uani 1 1 d . . . 
Cl25 Cl 0.09235(10) 0.54976(11) 0.22014(4) 0.00920(2) Uani 1 1 d . . . 
Cl26 Cl 0.17451(10) 0.85745(10) 0.08467(5) 0.00826(2) Uani 1 1 d . . . 
O18 O 0.0930(4) 0.7545(3) -0.1119(2) 0.00993(6) Uani 1 1 d . . . 
O24 O -0.0867(4) 0.2490(3) 0.1173(2) 0.00993(6) Uani 1 1 d . . . 
C15 C 0.0503(4) 0.6397(4) -0.0596(2) 0.00646(5) Uani 1 1 d . . . 
C16 C -0.0367(4) 0.4717(4) -0.0959(2) 0.00633(5) Uani 1 1 d . . . 
C17 C -0.0745(4) 0.3419(4) -0.0386(2) 0.00590(5) Uani 1 1 d . . . 
C21 C -0.0389(4) 0.3613(4) 0.0654(2) 0.00646(5) Uani 1 1 d . . . 
C22 C 0.0504(4) 0.5292(4) 0.1020(2) 0.00633(5) Uani 1 1 d . . . 
C23 C 0.0859(4) 0.6606(4) 0.0427(2) 0.00590(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C1 1.736(3) . ? 
S4 C2 1.747(3) . ? 
S5 C3 1.726(3) . ? 
S5 C2 1.745(3) . ? 
S11 C9 1.753(3) . ? 
S11 C8 1.756(3) . ? 
S12 C9 1.751(3) . ? 
S12 C10 1.752(3) . ? 
S12 Cl26 3.6213(12) . ? 
S12 Cl25 3.6802(11) . ? 
C1 C3 1.351(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3678(7) . ? 
C2 C15 3.366(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.328(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.718(3) . ? 
Cl19 S5 3.6864(11) 1_455 ? 
Cl20 C17 1.714(3) . ? 
Cl20 S11 3.4707(11) 1_445 ? 
Cl20 S5 3.6195(12) 1_455 ? 
Cl25 C22 1.697(3) . ? 
Cl26 C23 1.699(3) . ? 
Cl26 S4 3.4717(11) 1_565 ? 
O18 C15 1.226(3) . ? 
O24 C21 1.221(3) . ? 
C15 C23 1.471(5) . ? 
C15 C16 1.480(4) . ? 
C16 C17 1.343(4) . ? 
C17 C21 1.496(4) . ? 
C21 C22 1.487(4) . ? 
C21 C9 3.361(5) 1_455 ? 
C22 C23 1.367(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C1 S4 C2 94.92(16) . . ? 
C3 S5 C2 94.49(15) . . ? 
C9 S11 C8 94.98(15) . . ? 
C9 S12 C10 95.07(15) . . ? 
C9 S12 Cl26 76.43(11) . . ? 
C10 S12 Cl26 78.12(11) . . ? 
C9 S12 Cl25 109.55(12) . . ? 
C10 S12 Cl25 112.80(11) . . ? 
Cl26 S12 Cl25 51.38(2) . . ? 
C3 C1 S4 116.6(2) . . ? 
C3 C1 H6 121.7 . . ? 
S4 C1 H6 121.7 . . ? 
C9 C2 S5 122.46(11) . . ? 
C9 C2 S4 122.07(11) . . ? 
S5 C2 S4 115.46(17) . . ? 
C9 C2 C15 89.82(8) . . ? 
S5 C2 C15 84.41(13) . . ? 
S4 C2 C15 96.90(14) . . ? 
C1 C3 S5 118.5(3) . . ? 
C1 C3 H7 120.8 . . ? 
S5 C3 H7 120.8 . . ? 
C10 C8 S11 117.5(2) . . ? 
C10 C8 H13 121.3 . . ? 
S11 C8 H13 121.3 . . ? 
C2 C9 S12 122.84(11) . . ? 
C2 C9 S11 122.40(11) . . ? 
S12 C9 S11 114.74(17) . . ? 
C8 C10 S12 117.6(3) . . ? 
C8 C10 H14 121.2 . . ? 
S12 C10 H14 121.2 . . ? 
C16 Cl19 S5 76.55(11) . 1_455 ? 
C17 Cl20 S11 143.16(10) . 1_445 ? 
C17 Cl20 S5 76.98(11) . 1_455 ? 
S11 Cl20 S5 103.60(3) 1_445 1_455 ? 
C22 Cl25 S12 76.05(11) . . ? 
C23 Cl26 S4 142.05(10) . 1_565 ? 
C23 Cl26 S12 77.16(11) . . ? 
S4 Cl26 S12 103.43(3) 1_565 . ? 
O18 C15 C23 121.6(3) . . ? 
O18 C15 C16 121.8(3) . . ? 
C23 C15 C16 116.6(2) . . ? 
O18 C15 C2 96.6(2) . . ? 
C23 C15 C2 84.01(18) . . ? 
C16 C15 C2 88.10(18) . . ? 
C17 C16 C15 121.9(3) . . ? 
C17 C16 Cl19 121.7(2) . . ? 
C15 C16 Cl19 116.3(2) . . ? 
C16 C17 C21 122.0(3) . . ? 
C16 C17 Cl20 122.7(2) . . ? 
C21 C17 Cl20 115.3(2) . . ? 
O24 C21 C22 121.8(3) . . ? 
O24 C21 C17 122.1(3) . . ? 
C22 C21 C17 116.0(2) . . ? 
O24 C21 C9 94.6(2) . 1_455 ? 
C22 C21 C9 89.13(18) . 1_455 ? 
C17 C21 C9 83.62(18) . 1_455 ? 
C23 C22 C21 121.0(3) . . ? 
C23 C22 Cl25 123.1(2) . . ? 
C21 C22 Cl25 115.8(2) . . ? 
C22 C23 C15 122.3(3) . . ? 
C22 C23 Cl26 120.9(2) . . ? 
C15 C23 Cl26 116.8(2) . . ? 
 
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 
C2 S4 C1 C3 2.0(3) . . . . ? 
C3 S5 C2 C9 -179.39(13) . . . . ? 
C3 S5 C2 S4 1.8(2) . . . . ? 
C3 S5 C2 C15 -93.18(12) . . . . ? 
C1 S4 C2 C9 178.93(13) . . . . ? 
C1 S4 C2 S5 -2.3(2) . . . . ? 
C1 S4 C2 C15 84.80(14) . . . . ? 
S4 C1 C3 S5 -1.1(4) . . . . ? 
C2 S5 C3 C1 -0.4(3) . . . . ? 
C9 S11 C8 C10 0.0(3) . . . . ? 
S5 C2 C9 S12 179.7(3) . . . . ? 
S4 C2 C9 S12 -1.59(8) . . . . ? 
C15 C2 C9 S12 96.44(17) . . . . ? 
S5 C2 C9 S11 1.41(9) . . . . ? 
S4 C2 C9 S11 -179.9(3) . . . . ? 
C15 C2 C9 S11 -81.85(14) . . . . ? 
C10 S12 C9 C2 178.22(13) . . . . ? 
Cl26 S12 C9 C2 -105.31(10) . . . . ? 
Cl25 S12 C9 C2 -65.41(11) . . . . ? 
C10 S12 C9 S11 -3.4(2) . . . . ? 
Cl26 S12 C9 S11 73.09(17) . . . . ? 
Cl25 S12 C9 S11 113.00(17) . . . . ? 
C8 S11 C9 C2 -179.18(13) . . . . ? 
C8 S11 C9 S12 2.4(2) . . . . ? 
S11 C8 C10 S12 -2.4(4) . . . . ? 
C9 S12 C10 C8 3.5(3) . . . . ? 
Cl26 S12 C10 C8 -71.5(3) . . . . ? 
Cl25 S12 C10 C8 -110.2(3) . . . . ? 
C9 S12 Cl25 C22 7.45(16) . . . . ? 
C10 S12 Cl25 C22 111.99(18) . . . . ? 
Cl26 S12 Cl25 C22 60.41(12) . . . . ? 
C9 S12 Cl26 C23 68.36(14) . . . . ? 
C10 S12 Cl26 C23 166.62(15) . . . . ? 
Cl25 S12 Cl26 C23 -60.94(10) . . . . ? 
C9 S12 Cl26 S4 -72.64(11) . . . 1_565 ? 
C10 S12 Cl26 S4 25.62(12) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.06(3) . . . 1_565 ? 
C9 C2 C15 O18 74.0(2) . . . . ? 
S5 C2 C15 O18 -48.6(2) . . . . ? 
S4 C2 C15 O18 -163.7(2) . . . . ? 
C9 C2 C15 C23 -47.24(16) . . . . ? 
S5 C2 C15 C23 -169.9(2) . . . . ? 
S4 C2 C15 C23 75.07(19) . . . . ? 
C9 C2 C15 C16 -164.20(16) . . . . ? 
S5 C2 C15 C16 73.15(19) . . . . ? 
S4 C2 C15 C16 -41.9(2) . . . . ? 
O18 C15 C16 C17 176.4(3) . . . . ? 
C23 C15 C16 C17 -2.6(4) . . . . ? 
C2 C15 C16 C17 79.7(3) . . . . ? 
O18 C15 C16 Cl19 -2.1(4) . . . . ? 
C23 C15 C16 Cl19 178.9(2) . . . . ? 
C2 C15 C16 Cl19 -98.8(2) . . . . ? 
S5 Cl19 C16 C17 65.7(3) 1_455 . . . ? 
S5 Cl19 C16 C15 -115.8(2) 1_455 . . . ? 
C15 C16 C17 C21 2.7(4) . . . . ? 
Cl19 C16 C17 C21 -178.9(2) . . . . ? 
C15 C16 C17 Cl20 -176.8(2) . . . . ? 
Cl19 C16 C17 Cl20 1.7(4) . . . . ? 
S11 Cl20 C17 C16 -165.17(19) 1_445 . . . ? 
S5 Cl20 C17 C16 -69.8(3) 1_455 . . . ? 
S11 Cl20 C17 C21 15.3(3) 1_445 . . . ? 
S5 Cl20 C17 C21 110.7(2) 1_455 . . . ? 
C16 C17 C21 O24 174.1(3) . . . . ? 
Cl20 C17 C21 O24 -6.4(4) . . . . ? 
C16 C17 C21 C22 -3.2(4) . . . . ? 
Cl20 C17 C21 C22 176.3(2) . . . . ? 
C16 C17 C21 C9 82.7(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -97.81(19) . . . 1_455 ? 
O24 C21 C22 C23 -173.4(3) . . . . ? 
C17 C21 C22 C23 3.9(4) . . . . ? 
C9 C21 C22 C23 -78.5(3) 1_455 . . . ? 
O24 C21 C22 Cl25 3.2(4) . . . . ? 
C17 C21 C22 Cl25 -179.4(2) . . . . ? 
C9 C21 C22 Cl25 98.1(2) 1_455 . . . ? 
S12 Cl25 C22 C23 -66.8(3) . . . . ? 
S12 Cl25 C22 C21 116.6(2) . . . . ? 
C21 C22 C23 C15 -4.2(4) . . . . ? 
Cl25 C22 C23 C15 179.4(2) . . . . ? 
C21 C22 C23 Cl26 175.9(2) . . . . ? 
Cl25 C22 C23 Cl26 -0.5(4) . . . . ? 
O18 C15 C23 C22 -175.6(3) . . . . ? 
C16 C15 C23 C22 3.4(4) . . . . ? 
C2 C15 C23 C22 -81.5(3) . . . . ? 
O18 C15 C23 Cl26 4.3(4) . . . . ? 
C16 C15 C23 Cl26 -176.7(2) . . . . ? 
C2 C15 C23 Cl26 98.4(2) . . . . ? 
S4 Cl26 C23 C22 164.41(18) 1_565 . . . ? 
S12 Cl26 C23 C22 69.0(2) . . . . ? 
S4 Cl26 C23 C15 -15.5(4) 1_565 . . . ? 
S12 Cl26 C23 C15 -111.0(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.39 3.338(4) 176.4 1_545 
C8 H13 O24  0.95 2.40 3.348(4) 174.7 1_665 
C10 H14 O18  0.95 2.58 3.281(4) 130.7 2_565 
C3 H7 O24  0.95 2.53 3.267(4) 134.1 2_554 
 
_diffrn_measured_fraction_theta_max    0.903 
_diffrn_reflns_theta_full              33.55 
_diffrn_measured_fraction_theta_full   0.903 
_refine_diff_density_max    0.737 
_refine_diff_density_min   -0.443 
_refine_diff_density_rms    0.076 

#==END

 
data_off800ps 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2120(1) 
_cell_length_b                    7.5860(1) 
_cell_length_c                    14.4830(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1270(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.336(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.911 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.655 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91465 
_exptl_absorpt_correction_T_max   0.92695 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46021 
_diffrn_reflns_av_R_equivalents   0.0323 
_diffrn_reflns_av_sigmaI/netI     0.0285 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.57 
_reflns_number_total              11112 
_reflns_number_gt                 10069 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0284P)²+0.0853P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.48(17) 
_refine_ls_number_reflns          11112 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0235 
_refine_ls_R_factor_gt            0.0207 
_refine_ls_wR_factor_ref          0.0595 
_refine_ls_wR_factor_gt           0.0583 
_refine_ls_goodness_of_fit_ref    1.081 
_refine_ls_restrained_S_all       1.081 
_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 
S4 S 0.39011(10) 0.23684(11) 0.01871(5) 0.00719(2) Uani 1 1 d . . . 
S5 S 0.44690(10) 0.44149(10) -0.14743(5) 0.00658(2) Uani 1 1 d . . . 
S11 S 0.62069(10) 0.76396(11) -0.01355(5) 0.00719(2) Uani 1 1 d . . . 
S12 S 0.56297(10) 0.55821(10) 0.15289(5) 0.00658(2) Uani 1 1 d . . . 
C1 C 0.3140(5) 0.1411(4) -0.0908(3) 0.00825(6) Uani 1 1 d . . . 
H6 H 0.2543 0.0292 -0.0968 0.010 Uiso 1 1 calc R . . 
C2 C 0.4675(4) 0.4323(4) -0.0261(2) 0.00690(5) Uani 1 1 d . . . 
C3 C 0.3443(4) 0.2336(5) -0.1649(2) 0.00795(9) Uani 1 1 d . . . 
H7 H 0.3106 0.1874 -0.2262 0.010 Uiso 1 1 calc R . . 
C8 C 0.6935(5) 0.8577(4) 0.0959(3) 0.00825(6) Uani 1 1 d . . . 
H13 H 0.7461 0.9727 0.1019 0.010 Uiso 1 1 calc R . . 
C9 C 0.5426(4) 0.5670(4) 0.0306(2) 0.00690(5) Uani 1 1 d . . . 
C10 C 0.6728(4) 0.7612(5) 0.1720(2) 0.00795(9) Uani 1 1 d . . . 
H14 H 0.7167 0.8028 0.2335 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08185(10) 0.44966(10) -0.21530(4) 0.00888(2) Uani 1 1 d . . . 
Cl20 Cl -0.16418(10) 0.14254(10) -0.07915(5) 0.00796(2) Uani 1 1 d . . . 
Cl25 Cl 0.09209(10) 0.54988(10) 0.22028(4) 0.00888(2) Uani 1 1 d . . . 
Cl26 Cl 0.17501(10) 0.85773(10) 0.08459(5) 0.00796(2) Uani 1 1 d . . . 
O18 O 0.0943(4) 0.7528(3) -0.1118(2) 0.00978(5) Uani 1 1 d . . . 
O24 O -0.0858(4) 0.2473(3) 0.1175(2) 0.00978(5) Uani 1 1 d . . . 
C15 C 0.0509(4) 0.6380(3) -0.0595(2) 0.00624(5) Uani 1 1 d . . . 
C16 C -0.0365(4) 0.4717(4) -0.0956(2) 0.00603(6) Uani 1 1 d . . . 
C17 C -0.0748(4) 0.3400(4) -0.0387(2) 0.00570(5) Uani 1 1 d . . . 
C21 C -0.0383(4) 0.3596(3) 0.0655(2) 0.00624(5) Uani 1 1 d . . . 
C22 C 0.0506(4) 0.5292(4) 0.1024(2) 0.00603(6) Uani 1 1 d . . . 
C23 C 0.0858(4) 0.6588(4) 0.0427(2) 0.00570(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C2 1.745(3) . ? 
S4 C1 1.751(3) . ? 
S5 C2 1.741(3) . ? 
S5 C3 1.743(3) . ? 
S11 C8 1.741(3) . ? 
S11 C9 1.753(3) . ? 
S12 C10 1.734(3) . ? 
S12 C9 1.755(3) . ? 
S12 Cl26 3.6182(11) . ? 
S12 Cl25 3.6797(11) . ? 
C1 C3 1.329(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3679(7) . ? 
C2 C15 3.352(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.351(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.721(3) . ? 
Cl19 S5 3.6852(11) 1_455 ? 
Cl20 C17 1.698(3) . ? 
Cl20 S11 3.4677(11) 1_445 ? 
Cl20 S5 3.6205(11) 1_455 ? 
Cl25 C22 1.694(3) . ? 
Cl26 C23 1.713(3) . ? 
Cl26 S4 3.4724(11) 1_565 ? 
O18 C15 1.226(4) . ? 
O24 C21 1.221(4) . ? 
C15 C16 1.469(4) . ? 
C15 C23 1.470(4) . ? 
C16 C17 1.351(4) . ? 
C17 C21 1.498(4) . ? 
C21 C22 1.498(4) . ? 
C21 C9 3.373(5) 1_455 ? 
C22 C23 1.360(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 S4 C1 95.08(15) . . ? 
C2 S5 C3 94.40(15) . . ? 
C8 S11 C9 94.80(15) . . ? 
C10 S12 C9 95.18(15) . . ? 
C10 S12 Cl26 78.46(11) . . ? 
C9 S12 Cl26 76.29(11) . . ? 
C10 S12 Cl25 112.99(10) . . ? 
C9 S12 Cl25 109.59(11) . . ? 
Cl26 S12 Cl25 51.47(2) . . ? 
C3 C1 S4 116.4(2) . . ? 
C3 C1 H6 121.8 . . ? 
S4 C1 H6 121.8 . . ? 
C9 C2 S5 122.58(11) . . ? 
C9 C2 S4 122.07(11) . . ? 
S5 C2 S4 115.34(17) . . ? 
C9 C2 C15 89.97(8) . . ? 
S5 C2 C15 84.52(13) . . ? 
S4 C2 C15 96.72(14) . . ? 
C1 C3 S5 118.7(2) . . ? 
C1 C3 H7 120.6 . . ? 
S5 C3 H7 120.6 . . ? 
C10 C8 S11 117.7(2) . . ? 
C10 C8 H13 121.1 . . ? 
S11 C8 H13 121.1 . . ? 
C2 C9 S11 122.47(11) . . ? 
C2 C9 S12 122.64(11) . . ? 
S11 C9 S12 114.87(17) . . ? 
C8 C10 S12 117.2(2) . . ? 
C8 C10 H14 121.4 . . ? 
S12 C10 H14 121.4 . . ? 
C16 Cl19 S5 76.64(11) . 1_455 ? 
C17 Cl20 S11 142.94(11) . 1_445 ? 
C17 Cl20 S5 77.11(11) . 1_455 ? 
S11 Cl20 S5 103.46(3) 1_445 1_455 ? 
C22 Cl25 S12 75.95(11) . . ? 
C23 Cl26 S4 142.28(11) . 1_565 ? 
C23 Cl26 S12 76.97(11) . . ? 
S4 Cl26 S12 103.62(3) 1_565 . ? 
O18 C15 C16 121.8(3) . . ? 
O18 C15 C23 121.7(3) . . ? 
C16 C15 C23 116.4(2) . . ? 
O18 C15 C2 96.3(2) . . ? 
C16 C15 C2 88.60(18) . . ? 
C23 C15 C2 84.15(18) . . ? 
C17 C16 C15 122.4(3) . . ? 
C17 C16 Cl19 121.2(2) . . ? 
C15 C16 Cl19 116.4(2) . . ? 
C16 C17 C21 121.4(3) . . ? 
C16 C17 Cl20 123.0(2) . . ? 
C21 C17 Cl20 115.5(2) . . ? 
O24 C21 C22 121.7(3) . . ? 
O24 C21 C17 122.0(3) . . ? 
C22 C21 C17 116.2(2) . . ? 
O24 C21 C9 94.9(2) . 1_455 ? 
C22 C21 C9 88.59(18) . 1_455 ? 
C17 C21 C9 83.42(17) . 1_455 ? 
C23 C22 C21 120.5(3) . . ? 
C23 C22 Cl25 123.6(2) . . ? 
C21 C22 Cl25 115.8(2) . . ? 
C22 C23 C15 122.9(3) . . ? 
C22 C23 Cl26 120.6(2) . . ? 
C15 C23 Cl26 116.5(2) . . ? 
 
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 
C2 S4 C1 C3 2.9(3) . . . . ? 
C3 S5 C2 C9 -179.75(13) . . . . ? 
C3 S5 C2 S4 1.5(2) . . . . ? 
C3 S5 C2 C15 -93.31(12) . . . . ? 
C1 S4 C2 C9 178.79(13) . . . . ? 
C1 S4 C2 S5 -2.5(2) . . . . ? 
C1 S4 C2 C15 84.60(14) . . . . ? 
S4 C1 C3 S5 -2.3(4) . . . . ? 
C2 S5 C3 C1 0.5(3) . . . . ? 
C9 S11 C8 C10 0.8(3) . . . . ? 
S5 C2 C9 S11 1.42(8) . . . . ? 
S4 C2 C9 S11 -180.0(3) . . . . ? 
C15 C2 C9 S11 -82.04(14) . . . . ? 
S5 C2 C9 S12 179.8(3) . . . . ? 
S4 C2 C9 S12 -1.55(8) . . . . ? 
C15 C2 C9 S12 96.37(16) . . . . ? 
C8 S11 C9 C2 -179.31(13) . . . . ? 
C8 S11 C9 S12 2.2(2) . . . . ? 
C10 S12 C9 C2 177.81(13) . . . . ? 
Cl26 S12 C9 C2 -105.41(9) . . . . ? 
Cl25 S12 C9 C2 -65.53(11) . . . . ? 
C10 S12 C9 S11 -3.7(2) . . . . ? 
Cl26 S12 C9 S11 73.11(16) . . . . ? 
Cl25 S12 C9 S11 112.99(16) . . . . ? 
S11 C8 C10 S12 -3.7(4) . . . . ? 
C9 S12 C10 C8 4.4(3) . . . . ? 
Cl26 S12 C10 C8 -70.5(2) . . . . ? 
Cl25 S12 C10 C8 -109.5(2) . . . . ? 
C10 S12 Cl25 C22 112.47(17) . . . . ? 
C9 S12 Cl25 C22 7.69(14) . . . . ? 
Cl26 S12 Cl25 C22 60.46(10) . . . . ? 
C10 S12 Cl26 C23 166.99(16) . . . . ? 
C9 S12 Cl26 C23 68.67(15) . . . . ? 
Cl25 S12 Cl26 C23 -60.78(11) . . . . ? 
C10 S12 Cl26 S4 25.79(11) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.53(11) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.02(3) . . . 1_565 ? 
C9 C2 C15 O18 73.93(19) . . . . ? 
S5 C2 C15 O18 -48.8(2) . . . . ? 
S4 C2 C15 O18 -163.8(2) . . . . ? 
C9 C2 C15 C16 -164.18(17) . . . . ? 
S5 C2 C15 C16 73.1(2) . . . . ? 
S4 C2 C15 C16 -41.9(2) . . . . ? 
C9 C2 C15 C23 -47.42(15) . . . . ? 
S5 C2 C15 C23 -170.17(19) . . . . ? 
S4 C2 C15 C23 74.89(18) . . . . ? 
O18 C15 C16 C17 176.0(3) . . . . ? 
C23 C15 C16 C17 -3.3(4) . . . . ? 
C2 C15 C16 C17 79.5(3) . . . . ? 
O18 C15 C16 Cl19 -2.1(4) . . . . ? 
C23 C15 C16 Cl19 178.6(2) . . . . ? 
C2 C15 C16 Cl19 -98.6(2) . . . . ? 
S5 Cl19 C16 C17 65.7(2) 1_455 . . . ? 
S5 Cl19 C16 C15 -116.1(2) 1_455 . . . ? 
C15 C16 C17 C21 3.0(4) . . . . ? 
Cl19 C16 C17 C21 -179.0(2) . . . . ? 
C15 C16 C17 Cl20 -176.4(2) . . . . ? 
Cl19 C16 C17 Cl20 1.6(4) . . . . ? 
S11 Cl20 C17 C16 -165.03(19) 1_445 . . . ? 
S5 Cl20 C17 C16 -69.7(3) 1_455 . . . ? 
S11 Cl20 C17 C21 15.6(3) 1_445 . . . ? 
S5 Cl20 C17 C21 110.9(2) 1_455 . . . ? 
C16 C17 C21 O24 174.1(3) . . . . ? 
Cl20 C17 C21 O24 -6.5(4) . . . . ? 
C16 C17 C21 C22 -2.7(4) . . . . ? 
Cl20 C17 C21 C22 176.7(2) . . . . ? 
C16 C17 C21 C9 82.4(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -98.15(19) . . . 1_455 ? 
O24 C21 C22 C23 -173.7(3) . . . . ? 
C17 C21 C22 C23 3.1(4) . . . . ? 
C9 C21 C22 C23 -78.8(3) 1_455 . . . ? 
O24 C21 C22 Cl25 3.4(4) . . . . ? 
C17 C21 C22 Cl25 -179.8(2) . . . . ? 
C9 C21 C22 Cl25 98.28(19) 1_455 . . . ? 
S12 Cl25 C22 C23 -66.7(3) . . . . ? 
S12 Cl25 C22 C21 116.3(2) . . . . ? 
C21 C22 C23 C15 -3.8(4) . . . . ? 
Cl25 C22 C23 C15 179.3(2) . . . . ? 
C21 C22 C23 Cl26 176.2(2) . . . . ? 
Cl25 C22 C23 Cl26 -0.6(4) . . . . ? 
O18 C15 C23 C22 -175.5(3) . . . . ? 
C16 C15 C23 C22 3.7(4) . . . . ? 
C2 C15 C23 C22 -81.8(3) . . . . ? 
O18 C15 C23 Cl26 4.4(4) . . . . ? 
C16 C15 C23 Cl26 -176.3(2) . . . . ? 
C2 C15 C23 Cl26 98.17(19) . . . . ? 
S4 Cl26 C23 C22 164.62(18) 1_565 . . . ? 
S12 Cl26 C23 C22 69.1(2) . . . . ? 
S4 Cl26 C23 C15 -15.3(3) 1_565 . . . ? 
S12 Cl26 C23 C15 -110.8(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.39 3.336(4) 178.0 1_545 
C8 H13 O24  0.95 2.40 3.348(4) 173.3 1_665 
C10 H14 O18  0.95 2.57 3.271(4) 130.8 2_565 
C3 H7 O24  0.95 2.54 3.273(4) 133.8 2_554 
 
_diffrn_measured_fraction_theta_max    0.902 
_diffrn_reflns_theta_full              33.57 
_diffrn_measured_fraction_theta_full   0.902 
_refine_diff_density_max    0.736 
_refine_diff_density_min   -0.484 
_refine_diff_density_rms    0.078 

#==END
 
 
data_on800ps 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2140(1) 
_cell_length_b                    7.5870(1) 
_cell_length_c                    14.4850(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1300(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.758(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.910 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.654 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91518 
_exptl_absorpt_correction_T_max   0.92474 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46028 
_diffrn_reflns_av_R_equivalents   0.0326 
_diffrn_reflns_av_sigmaI/netI     0.0283 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.55 
_reflns_number_total              11101 
_reflns_number_gt                 10065 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0278P)²+0.0726P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.59(17) 
_refine_ls_number_reflns          11101 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0233 
_refine_ls_R_factor_gt            0.0207 
_refine_ls_wR_factor_ref          0.0583 
_refine_ls_wR_factor_gt           0.0573 
_refine_ls_goodness_of_fit_ref    1.078 
_refine_ls_restrained_S_all       1.078 
_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 
S4 S 0.39024(11) 0.23679(11) 0.01875(5) 0.00741(2) Uani 1 1 d . . . 
S5 S 0.44706(11) 0.44158(10) -0.14742(5) 0.00682(2) Uani 1 1 d . . . 
S11 S 0.62072(11) 0.76391(10) -0.01350(5) 0.00741(2) Uani 1 1 d . . . 
S12 S 0.56320(11) 0.55825(10) 0.15288(5) 0.00682(2) Uani 1 1 d . . . 
C1 C 0.3166(5) 0.1407(4) -0.0894(2) 0.00843(7) Uani 1 1 d . . . 
H6 H 0.2595 0.0275 -0.0946 0.010 Uiso 1 1 calc R . . 
C2 C 0.4682(5) 0.4322(4) -0.0262(2) 0.00704(5) Uani 1 1 d . . . 
C3 C 0.3435(5) 0.2335(4) -0.1661(3) 0.00828(8) Uani 1 1 d . . . 
H7 H 0.3078 0.1875 -0.2273 0.010 Uiso 1 1 calc R . . 
C8 C 0.6962(5) 0.8572(4) 0.0973(2) 0.00843(7) Uani 1 1 d . . . 
H13 H 0.7514 0.9711 0.1041 0.010 Uiso 1 1 calc R . . 
C9 C 0.5434(5) 0.5668(4) 0.0305(2) 0.00704(5) Uani 1 1 d . . . 
C10 C 0.6722(5) 0.7610(4) 0.1708(3) 0.00828(8) Uani 1 1 d . . . 
H14 H 0.7143 0.8028 0.2323 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08168(10) 0.44970(11) -0.21509(5) 0.00919(2) Uani 1 1 d . . . 
Cl20 Cl -0.16455(11) 0.14252(10) -0.07933(5) 0.00823(2) Uani 1 1 d . . . 
Cl25 Cl 0.09235(10) 0.54982(11) 0.22046(5) 0.00919(2) Uani 1 1 d . . . 
Cl26 Cl 0.17456(11) 0.85762(10) 0.08441(5) 0.00823(2) Uani 1 1 d . . . 
O18 O 0.0930(4) 0.7526(3) -0.1124(2) 0.00994(6) Uani 1 1 d . . . 
O24 O -0.0868(4) 0.2472(3) 0.1168(2) 0.00994(6) Uani 1 1 d . . . 
C15 C 0.0498(5) 0.6385(4) -0.0597(2) 0.00645(5) Uani 1 1 d . . . 
C16 C -0.0379(5) 0.4722(4) -0.0965(2) 0.00630(5) Uani 1 1 d . . . 
C17 C -0.0740(4) 0.3399(4) -0.0376(2) 0.00597(5) Uani 1 1 d . . . 
C21 C -0.0392(5) 0.3600(4) 0.0653(2) 0.00645(5) Uani 1 1 d . . . 
C22 C 0.0492(5) 0.5296(4) 0.1015(2) 0.00630(5) Uani 1 1 d . . . 
C23 C 0.0864(4) 0.6587(4) 0.0437(2) 0.00597(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C1 1.733(3) . ? 
S4 C2 1.748(3) . ? 
S5 C2 1.740(3) . ? 
S5 C3 1.749(4) . ? 
S11 C9 1.751(3) . ? 
S11 C8 1.760(3) . ? 
S12 C10 1.729(4) . ? 
S12 C9 1.756(3) . ? 
S12 Cl26 3.6223(12) . ? 
S12 Cl25 3.6817(12) . ? 
C1 C3 1.355(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3675(7) . ? 
C2 C15 3.366(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.324(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.705(3) . ? 
Cl19 S5 3.6850(12) 1_455 ? 
Cl20 C17 1.706(3) . ? 
Cl20 S11 3.4683(11) 1_445 ? 
Cl20 S5 3.6186(12) 1_455 ? 
Cl25 C22 1.709(3) . ? 
Cl26 C23 1.706(3) . ? 
Cl26 S4 3.4743(11) 1_565 ? 
O18 C15 1.227(4) . ? 
O24 C21 1.219(4) . ? 
C15 C16 1.473(4) . ? 
C15 C23 1.488(4) . ? 
C16 C17 1.369(4) . ? 
C17 C21 1.480(4) . ? 
C21 C22 1.493(4) . ? 
C21 C9 3.362(5) 1_455 ? 
C22 C23 1.342(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C1 S4 C2 95.23(17) . . ? 
C2 S5 C3 94.93(16) . . ? 
C9 S11 C8 94.68(16) . . ? 
C10 S12 C9 94.62(16) . . ? 
C10 S12 Cl26 78.28(12) . . ? 
C9 S12 Cl26 76.41(12) . . ? 
C10 S12 Cl25 113.12(11) . . ? 
C9 S12 Cl25 109.76(12) . . ? 
Cl26 S12 Cl25 51.47(2) . . ? 
C3 C1 S4 117.4(3) . . ? 
C3 C1 H6 121.3 . . ? 
S4 C1 H6 121.3 . . ? 
C9 C2 S5 122.59(11) . . ? 
C9 C2 S4 122.02(12) . . ? 
S5 C2 S4 115.38(18) . . ? 
C9 C2 C15 90.02(8) . . ? 
S5 C2 C15 84.39(13) . . ? 
S4 C2 C15 96.54(14) . . ? 
C1 C3 S5 117.1(3) . . ? 
C1 C3 H7 121.5 . . ? 
S5 C3 H7 121.5 . . ? 
C10 C8 S11 116.8(3) . . ? 
C10 C8 H13 121.6 . . ? 
S11 C8 H13 121.6 . . ? 
C2 C9 S11 122.53(12) . . ? 
C2 C9 S12 122.65(11) . . ? 
S11 C9 S12 114.80(18) . . ? 
C8 C10 S12 119.0(3) . . ? 
C8 C10 H14 120.5 . . ? 
S12 C10 H14 120.5 . . ? 
C16 Cl19 S5 76.42(11) . 1_455 ? 
C17 Cl20 S11 142.42(11) . 1_445 ? 
C17 Cl20 S5 77.44(10) . 1_455 ? 
S11 Cl20 S5 103.53(3) 1_445 1_455 ? 
C22 Cl25 S12 76.20(11) . . ? 
C23 Cl26 S4 142.81(11) . 1_565 ? 
C23 Cl26 S12 76.69(10) . . ? 
S4 Cl26 S12 103.50(3) 1_565 . ? 
O18 C15 C16 121.1(3) . . ? 
O18 C15 C23 122.1(3) . . ? 
C16 C15 C23 116.7(3) . . ? 
O18 C15 C2 96.2(2) . . ? 
C16 C15 C2 88.72(19) . . ? 
C23 C15 C2 83.73(18) . . ? 
C17 C16 C15 121.1(3) . . ? 
C17 C16 Cl19 122.1(2) . . ? 
C15 C16 Cl19 116.8(2) . . ? 
C16 C17 C21 122.2(3) . . ? 
C16 C17 Cl20 121.6(3) . . ? 
C21 C17 Cl20 116.2(2) . . ? 
O24 C21 C17 121.6(3) . . ? 
O24 C21 C22 122.5(3) . . ? 
C17 C21 C22 115.9(2) . . ? 
O24 C21 C9 95.0(2) . 1_455 ? 
C17 C21 C9 83.82(18) . 1_455 ? 
C22 C21 C9 88.46(19) . 1_455 ? 
C23 C22 C21 121.8(3) . . ? 
C23 C22 Cl25 122.7(3) . . ? 
C21 C22 Cl25 115.5(2) . . ? 
C22 C23 C15 122.1(3) . . ? 
C22 C23 Cl26 122.1(3) . . ? 
C15 C23 Cl26 115.8(2) . . ? 
 
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 
C2 S4 C1 C3 1.6(3) . . . . ? 
C3 S5 C2 C9 -179.59(14) . . . . ? 
C3 S5 C2 S4 1.4(2) . . . . ? 
C3 S5 C2 C15 -93.16(14) . . . . ? 
C1 S4 C2 C9 179.23(14) . . . . ? 
C1 S4 C2 S5 -1.8(2) . . . . ? 
C1 S4 C2 C15 85.09(15) . . . . ? 
S4 C1 C3 S5 -0.8(4) . . . . ? 
C2 S5 C3 C1 -0.4(3) . . . . ? 
C9 S11 C8 C10 -0.5(3) . . . . ? 
S5 C2 C9 S11 1.51(8) . . . . ? 
S4 C2 C9 S11 -179.6(3) . . . . ? 
C15 C2 C9 S11 -81.84(15) . . . . ? 
S5 C2 C9 S12 179.5(3) . . . . ? 
S4 C2 C9 S12 -1.59(8) . . . . ? 
C15 C2 C9 S12 96.14(17) . . . . ? 
C8 S11 C9 C2 -178.93(14) . . . . ? 
C8 S11 C9 S12 2.9(2) . . . . ? 
C10 S12 C9 C2 178.04(14) . . . . ? 
Cl26 S12 C9 C2 -105.21(10) . . . . ? 
Cl25 S12 C9 C2 -65.37(11) . . . . ? 
C10 S12 C9 S11 -3.8(2) . . . . ? 
Cl26 S12 C9 S11 72.92(18) . . . . ? 
Cl25 S12 C9 S11 112.76(17) . . . . ? 
S11 C8 C10 S12 -2.2(4) . . . . ? 
C9 S12 C10 C8 3.7(3) . . . . ? 
Cl26 S12 C10 C8 -71.4(3) . . . . ? 
Cl25 S12 C10 C8 -110.1(3) . . . . ? 
C10 S12 Cl25 C22 111.72(18) . . . . ? 
C9 S12 Cl25 C22 7.45(16) . . . . ? 
Cl26 S12 Cl25 C22 60.21(11) . . . . ? 
C10 S12 Cl26 C23 166.93(16) . . . . ? 
C9 S12 Cl26 C23 69.19(15) . . . . ? 
Cl25 S12 Cl26 C23 -60.39(11) . . . . ? 
C10 S12 Cl26 S4 25.21(12) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.53(11) . . . 1_565 ? 
Cl25 S12 Cl26 S4 157.89(3) . . . 1_565 ? 
C9 C2 C15 O18 74.3(2) . . . . ? 
S5 C2 C15 O18 -48.5(2) . . . . ? 
S4 C2 C15 O18 -163.4(2) . . . . ? 
C9 C2 C15 C16 -164.55(17) . . . . ? 
S5 C2 C15 C16 72.7(2) . . . . ? 
S4 C2 C15 C16 -42.3(2) . . . . ? 
C9 C2 C15 C23 -47.48(16) . . . . ? 
S5 C2 C15 C23 -170.24(19) . . . . ? 
S4 C2 C15 C23 74.8(2) . . . . ? 
O18 C15 C16 C17 175.4(3) . . . . ? 
C23 C15 C16 C17 -3.4(4) . . . . ? 
C2 C15 C16 C17 78.9(3) . . . . ? 
O18 C15 C16 Cl19 -1.8(4) . . . . ? 
C23 C15 C16 Cl19 179.5(2) . . . . ? 
C2 C15 C16 Cl19 -98.2(2) . . . . ? 
S5 Cl19 C16 C17 66.5(3) 1_455 . . . ? 
S5 Cl19 C16 C15 -116.4(3) 1_455 . . . ? 
C15 C16 C17 C21 4.1(4) . . . . ? 
Cl19 C16 C17 C21 -178.9(2) . . . . ? 
C15 C16 C17 Cl20 -176.7(2) . . . . ? 
Cl19 C16 C17 Cl20 0.3(4) . . . . ? 
S11 Cl20 C17 C16 -164.79(19) 1_445 . . . ? 
S5 Cl20 C17 C16 -68.8(3) 1_455 . . . ? 
S11 Cl20 C17 C21 14.5(3) 1_445 . . . ? 
S5 Cl20 C17 C21 110.5(2) 1_455 . . . ? 
C16 C17 C21 O24 173.6(3) . . . . ? 
Cl20 C17 C21 O24 -5.7(4) . . . . ? 
C16 C17 C21 C22 -3.7(4) . . . . ? 
Cl20 C17 C21 C22 177.0(2) . . . . ? 
C16 C17 C21 C9 81.5(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -97.77(19) . . . 1_455 ? 
O24 C21 C22 C23 -174.3(3) . . . . ? 
C17 C21 C22 C23 3.0(4) . . . . ? 
C9 C21 C22 C23 -79.3(3) 1_455 . . . ? 
O24 C21 C22 Cl25 3.8(4) . . . . ? 
C17 C21 C22 Cl25 -178.9(2) . . . . ? 
C9 C21 C22 Cl25 98.7(2) 1_455 . . . ? 
S12 Cl25 C22 C23 -65.9(3) . . . . ? 
S12 Cl25 C22 C21 116.1(2) . . . . ? 
C21 C22 C23 C15 -2.7(4) . . . . ? 
Cl25 C22 C23 C15 179.4(2) . . . . ? 
C21 C22 C23 Cl26 176.1(2) . . . . ? 
Cl25 C22 C23 Cl26 -1.8(4) . . . . ? 
O18 C15 C23 C22 -176.0(3) . . . . ? 
C16 C15 C23 C22 2.8(4) . . . . ? 
C2 C15 C23 C22 -82.6(3) . . . . ? 
O18 C15 C23 Cl26 5.1(4) . . . . ? 
C16 C15 C23 Cl26 -176.1(2) . . . . ? 
C2 C15 C23 Cl26 98.52(19) . . . . ? 
S4 Cl26 C23 C22 164.8(2) 1_565 . . . ? 
S12 Cl26 C23 C22 69.9(3) . . . . ? 
S4 Cl26 C23 C15 -16.4(4) 1_565 . . . ? 
S12 Cl26 C23 C15 -111.2(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.40 3.348(4) 175.6 1_545 
C8 H13 O24  0.95 2.39 3.338(4) 175.2 1_665 
C10 H14 O18  0.95 2.57 3.282(4) 131.6 2_565 
C3 H7 O24  0.95 2.54 3.267(4) 133.0 2_554 
 
_diffrn_measured_fraction_theta_max    0.903 
_diffrn_reflns_theta_full              33.55 
_diffrn_measured_fraction_theta_full   0.903 
_refine_diff_density_max    0.698 
_refine_diff_density_min   -0.513 
_refine_diff_density_rms    0.076 

#==END

 
data_off1ns 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2120(1) 
_cell_length_b                    7.5860(1) 
_cell_length_c                    14.4830(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1270(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.336(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.911 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.655 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91817 
_exptl_absorpt_correction_T_max   0.92510 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46099 
_diffrn_reflns_av_R_equivalents   0.0316 
_diffrn_reflns_av_sigmaI/netI     0.0281 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.55 
_reflns_number_total              11084 
_reflns_number_gt                 10074 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0269P)²+0.0803P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.35(17) 
_refine_ls_number_reflns          11084 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0232 
_refine_ls_R_factor_gt            0.0204 
_refine_ls_wR_factor_ref          0.0581 
_refine_ls_wR_factor_gt           0.0570 
_refine_ls_goodness_of_fit_ref    1.087 
_refine_ls_restrained_S_all       1.087 
_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 
S4 S 0.39000(11) 0.23672(11) 0.01872(5) 0.00721(2) Uani 1 1 d . . . 
S5 S 0.44696(10) 0.44167(11) -0.14739(5) 0.00658(2) Uani 1 1 d . . . 
S11 S 0.62057(11) 0.76385(11) -0.01356(5) 0.00721(2) Uani 1 1 d . . . 
S12 S 0.56303(10) 0.55840(10) 0.15293(5) 0.00658(2) Uani 1 1 d . . . 
C1 C 0.3136(5) 0.1418(4) -0.0911(3) 0.00825(6) Uani 1 1 d . . . 
H6 H 0.2535 0.0300 -0.0972 0.010 Uiso 1 1 calc R . . 
C2 C 0.4670(5) 0.4326(4) -0.0261(2) 0.00688(5) Uani 1 1 d . . . 
C3 C 0.3438(5) 0.2333(4) -0.1651(3) 0.00801(9) Uani 1 1 d . . . 
H7 H 0.3103 0.1868 -0.2264 0.010 Uiso 1 1 calc R . . 
C8 C 0.6933(5) 0.8584(4) 0.0955(3) 0.00825(6) Uani 1 1 d . . . 
H13 H 0.7456 0.9736 0.1016 0.010 Uiso 1 1 calc R . . 
C9 C 0.5421(5) 0.5674(4) 0.0306(2) 0.00688(5) Uani 1 1 d . . . 
C10 C 0.6724(5) 0.7609(4) 0.1717(3) 0.00801(9) Uani 1 1 d . . . 
H14 H 0.7162 0.8025 0.2331 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08181(10) 0.44969(11) -0.21524(5) 0.00890(2) Uani 1 1 d . . . 
Cl20 Cl -0.16413(11) 0.14244(10) -0.07916(5) 0.00797(2) Uani 1 1 d . . . 
Cl25 Cl 0.09216(10) 0.54991(11) 0.22033(5) 0.00890(2) Uani 1 1 d . . . 
Cl26 Cl 0.17507(11) 0.85765(10) 0.08459(5) 0.00797(2) Uani 1 1 d . . . 
O18 O 0.0949(4) 0.7526(3) -0.1117(2) 0.00977(5) Uani 1 1 d . . . 
O24 O -0.0851(4) 0.2470(3) 0.1176(2) 0.00977(5) Uani 1 1 d . . . 
C15 C 0.0509(5) 0.6379(4) -0.0593(2) 0.00619(5) Uani 1 1 d . . . 
C16 C -0.0367(4) 0.4716(4) -0.0962(2) 0.00608(5) Uani 1 1 d . . . 
C17 C -0.0753(4) 0.3401(4) -0.0388(2) 0.00573(5) Uani 1 1 d . . . 
C21 C -0.0383(5) 0.3593(4) 0.0658(2) 0.00619(5) Uani 1 1 d . . . 
C22 C 0.0503(4) 0.5293(4) 0.1018(2) 0.00608(5) Uani 1 1 d . . . 
C23 C 0.0852(4) 0.6588(4) 0.0425(2) 0.00573(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C2 1.747(3) . ? 
S4 C1 1.753(4) . ? 
S5 C2 1.741(3) . ? 
S5 C3 1.749(3) . ? 
S11 C8 1.739(4) . ? 
S11 C9 1.751(3) . ? 
S12 C10 1.729(3) . ? 
S12 C9 1.755(3) . ? 
S12 Cl26 3.6171(12) . ? 
S12 Cl25 3.6798(11) . ? 
C1 C3 1.324(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3684(7) . ? 
C2 C15 3.347(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.356(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.711(3) . ? 
Cl19 S5 3.6849(11) 1_455 ? 
Cl20 C17 1.697(3) . ? 
Cl20 S11 3.4684(12) 1_445 ? 
Cl20 S5 3.6217(12) 1_455 ? 
Cl25 C22 1.703(3) . ? 
Cl26 C23 1.715(3) . ? 
Cl26 S4 3.4715(12) 1_565 ? 
O18 C15 1.229(4) . ? 
O24 C21 1.218(4) . ? 
C15 C23 1.465(4) . ? 
C15 C16 1.472(4) . ? 
C16 C17 1.355(4) . ? 
C17 C21 1.503(4) . ? 
C21 C22 1.495(4) . ? 
C21 C9 3.379(5) 1_455 ? 
C22 C23 1.354(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 S4 C1 94.88(16) . . ? 
C2 S5 C3 94.47(16) . . ? 
C8 S11 C9 95.01(16) . . ? 
C10 S12 C9 95.05(16) . . ? 
C10 S12 Cl26 78.40(12) . . ? 
C9 S12 Cl26 76.13(12) . . ? 
C10 S12 Cl25 113.02(11) . . ? 
C9 S12 Cl25 109.45(12) . . ? 
Cl26 S12 Cl25 51.48(2) . . ? 
C3 C1 S4 116.8(3) . . ? 
C3 C1 H6 121.6 . . ? 
S4 C1 H6 121.6 . . ? 
C9 C2 S5 122.54(11) . . ? 
C9 C2 S4 122.10(11) . . ? 
S5 C2 S4 115.34(17) . . ? 
C9 C2 C15 89.95(8) . . ? 
S5 C2 C15 84.70(13) . . ? 
S4 C2 C15 96.81(14) . . ? 
C1 C3 S5 118.4(3) . . ? 
C1 C3 H7 120.8 . . ? 
S5 C3 H7 120.8 . . ? 
C10 C8 S11 117.2(3) . . ? 
C10 C8 H13 121.4 . . ? 
S11 C8 H13 121.4 . . ? 
C2 C9 S11 122.45(11) . . ? 
C2 C9 S12 122.64(11) . . ? 
S11 C9 S12 114.89(17) . . ? 
C8 C10 S12 117.7(3) . . ? 
C8 C10 H14 121.2 . . ? 
S12 C10 H14 121.2 . . ? 
C16 Cl19 S5 76.64(11) . 1_455 ? 
C17 Cl20 S11 142.96(11) . 1_445 ? 
C17 Cl20 S5 76.92(11) . 1_455 ? 
S11 Cl20 S5 103.46(3) 1_445 1_455 ? 
C22 Cl25 S12 75.97(11) . . ? 
C23 Cl26 S4 142.28(11) . 1_565 ? 
C23 Cl26 S12 77.15(11) . . ? 
S4 Cl26 S12 103.61(3) 1_565 . ? 
O18 C15 C23 121.7(3) . . ? 
O18 C15 C16 121.4(3) . . ? 
C23 C15 C16 116.9(3) . . ? 
O18 C15 C2 96.0(2) . . ? 
C23 C15 C2 84.33(19) . . ? 
C16 C15 C2 88.68(19) . . ? 
C17 C16 C15 121.7(3) . . ? 
C17 C16 Cl19 121.4(2) . . ? 
C15 C16 Cl19 116.8(2) . . ? 
C16 C17 C21 121.7(3) . . ? 
C16 C17 Cl20 122.9(2) . . ? 
C21 C17 Cl20 115.4(2) . . ? 
O24 C21 C22 122.2(3) . . ? 
O24 C21 C17 122.1(3) . . ? 
C22 C21 C17 115.7(3) . . ? 
O24 C21 C9 95.2(2) . 1_455 ? 
C22 C21 C9 88.45(19) . 1_455 ? 
C17 C21 C9 83.21(18) . 1_455 ? 
C23 C22 C21 121.1(3) . . ? 
C23 C22 Cl25 123.4(2) . . ? 
C21 C22 Cl25 115.4(2) . . ? 
C22 C23 C15 122.7(3) . . ? 
C22 C23 Cl26 120.7(2) . . ? 
C15 C23 Cl26 116.5(2) . . ? 
 
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 
C2 S4 C1 C3 3.2(3) . . . . ? 
C3 S5 C2 C9 -179.78(13) . . . . ? 
C3 S5 C2 S4 1.8(2) . . . . ? 
C3 S5 C2 C15 -93.23(13) . . . . ? 
C1 S4 C2 C9 178.74(14) . . . . ? 
C1 S4 C2 S5 -2.8(2) . . . . ? 
C1 S4 C2 C15 84.50(15) . . . . ? 
S4 C1 C3 S5 -2.6(4) . . . . ? 
C2 S5 C3 C1 0.4(3) . . . . ? 
C9 S11 C8 C10 1.1(3) . . . . ? 
S5 C2 C9 S11 1.41(9) . . . . ? 
S4 C2 C9 S11 179.7(3) . . . . ? 
C15 C2 C9 S11 -82.27(15) . . . . ? 
S5 C2 C9 S12 -179.8(3) . . . . ? 
S4 C2 C9 S12 -1.52(8) . . . . ? 
C15 C2 C9 S12 96.50(17) . . . . ? 
C8 S11 C9 C2 -179.31(14) . . . . ? 
C8 S11 C9 S12 1.8(2) . . . . ? 
C10 S12 C9 C2 177.77(13) . . . . ? 
Cl26 S12 C9 C2 -105.51(10) . . . . ? 
Cl25 S12 C9 C2 -65.64(11) . . . . ? 
C10 S12 C9 S11 -3.4(2) . . . . ? 
Cl26 S12 C9 S11 73.35(17) . . . . ? 
Cl25 S12 C9 S11 113.22(17) . . . . ? 
S11 C8 C10 S12 -3.8(4) . . . . ? 
C9 S12 C10 C8 4.3(3) . . . . ? 
Cl26 S12 C10 C8 -70.5(2) . . . . ? 
Cl25 S12 C10 C8 -109.4(2) . . . . ? 
C10 S12 Cl25 C22 112.27(18) . . . . ? 
C9 S12 Cl25 C22 7.71(15) . . . . ? 
Cl26 S12 Cl25 C22 60.40(11) . . . . ? 
C10 S12 Cl26 C23 166.87(17) . . . . ? 
C9 S12 Cl26 C23 68.64(15) . . . . ? 
Cl25 S12 Cl26 C23 -60.78(11) . . . . ? 
C10 S12 Cl26 S4 25.65(13) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.58(11) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.00(3) . . . 1_565 ? 
C9 C2 C15 O18 74.0(2) . . . . ? 
S5 C2 C15 O18 -48.7(2) . . . . ? 
S4 C2 C15 O18 -163.7(2) . . . . ? 
C9 C2 C15 C23 -47.44(17) . . . . ? 
S5 C2 C15 C23 -170.14(19) . . . . ? 
S4 C2 C15 C23 74.9(2) . . . . ? 
C9 C2 C15 C16 -164.64(17) . . . . ? 
S5 C2 C15 C16 72.66(19) . . . . ? 
S4 C2 C15 C16 -42.3(2) . . . . ? 
O18 C15 C16 C17 175.9(3) . . . . ? 
C23 C15 C16 C17 -3.2(4) . . . . ? 
C2 C15 C16 C17 79.7(3) . . . . ? 
O18 C15 C16 Cl19 -2.4(4) . . . . ? 
C23 C15 C16 Cl19 178.5(2) . . . . ? 
C2 C15 C16 Cl19 -98.6(2) . . . . ? 
S5 Cl19 C16 C17 65.6(3) 1_455 . . . ? 
S5 Cl19 C16 C15 -116.1(3) 1_455 . . . ? 
C15 C16 C17 C21 2.6(4) . . . . ? 
Cl19 C16 C17 C21 -179.2(3) . . . . ? 
C15 C16 C17 Cl20 -176.2(3) . . . . ? 
Cl19 C16 C17 Cl20 2.0(4) . . . . ? 
S11 Cl20 C17 C16 -165.1(2) 1_445 . . . ? 
S5 Cl20 C17 C16 -70.0(3) 1_455 . . . ? 
S11 Cl20 C17 C21 16.1(4) 1_445 . . . ? 
S5 Cl20 C17 C21 111.2(2) 1_455 . . . ? 
C16 C17 C21 O24 174.6(3) . . . . ? 
Cl20 C17 C21 O24 -6.5(4) . . . . ? 
C16 C17 C21 C22 -2.3(4) . . . . ? 
Cl20 C17 C21 C22 176.6(2) . . . . ? 
C16 C17 C21 C9 82.7(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -98.4(2) . . . 1_455 ? 
O24 C21 C22 C23 -173.8(3) . . . . ? 
C17 C21 C22 C23 3.1(4) . . . . ? 
C9 C21 C22 C23 -78.7(3) 1_455 . . . ? 
O24 C21 C22 Cl25 3.2(4) . . . . ? 
C17 C21 C22 Cl25 -179.9(2) . . . . ? 
C9 C21 C22 Cl25 98.4(2) 1_455 . . . ? 
S12 Cl25 C22 C23 -66.8(3) . . . . ? 
S12 Cl25 C22 C21 116.3(2) . . . . ? 
C21 C22 C23 C15 -4.1(4) . . . . ? 
Cl25 C22 C23 C15 179.1(3) . . . . ? 
C21 C22 C23 Cl26 176.4(2) . . . . ? 
Cl25 C22 C23 Cl26 -0.4(4) . . . . ? 
O18 C15 C23 C22 -175.1(3) . . . . ? 
C16 C15 C23 C22 4.0(4) . . . . ? 
C2 C15 C23 C22 -81.6(3) . . . . ? 
O18 C15 C23 Cl26 4.4(4) . . . . ? 
C16 C15 C23 Cl26 -176.5(2) . . . . ? 
C2 C15 C23 Cl26 97.9(2) . . . . ? 
S4 Cl26 C23 C22 164.61(19) 1_565 . . . ? 
S12 Cl26 C23 C22 68.9(3) . . . . ? 
S4 Cl26 C23 C15 -14.9(4) 1_565 . . . ? 
S12 Cl26 C23 C15 -110.6(3) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.39 3.338(4) 178.5 1_545 
C8 H13 O24  0.95 2.40 3.344(4) 172.9 1_665 
C10 H14 O18  0.95 2.57 3.275(5) 131.0 2_565 
C3 H7 O24  0.95 2.54 3.271(5) 133.6 2_554 
 
_diffrn_measured_fraction_theta_max    0.902 
_diffrn_reflns_theta_full              33.55 
_diffrn_measured_fraction_theta_full   0.902 
_refine_diff_density_max    0.668 
_refine_diff_density_min   -0.450 
_refine_diff_density_rms    0.075 

#==END

 
data_on1ns 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2140(1) 
_cell_length_b                    7.5870(1) 
_cell_length_c                    14.4850(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1320(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      782.753(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.910 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.654 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91699 
_exptl_absorpt_correction_T_max   0.92480 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46004 
_diffrn_reflns_av_R_equivalents   0.0327 
_diffrn_reflns_av_sigmaI/netI     0.0285 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.56 
_reflns_number_total              11106 
_reflns_number_gt                 10088 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0269P)²+0.0907P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.52(17) 
_refine_ls_number_reflns          11106 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0236 
_refine_ls_R_factor_gt            0.0207 
_refine_ls_wR_factor_ref          0.0587 
_refine_ls_wR_factor_gt           0.0576 
_refine_ls_goodness_of_fit_ref    1.081 
_refine_ls_restrained_S_all       1.081 
_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 
S4 S 0.39014(10) 0.23655(11) 0.01870(5) 0.00744(2) Uani 1 1 d . . . 
S5 S 0.44693(10) 0.44160(11) -0.14743(5) 0.00685(2) Uani 1 1 d . . . 
S11 S 0.62063(10) 0.76365(11) -0.01356(5) 0.00744(2) Uani 1 1 d . . . 
S12 S 0.56309(10) 0.55828(11) 0.15287(5) 0.00685(2) Uani 1 1 d . . . 
C1 C 0.3140(5) 0.1416(4) -0.0907(3) 0.00858(6) Uani 1 1 d . . . 
H6 H 0.2540 0.0298 -0.0967 0.010 Uiso 1 1 calc R . . 
C2 C 0.4673(5) 0.4328(4) -0.0263(2) 0.00704(5) Uani 1 1 d . . . 
C3 C 0.3439(4) 0.2333(5) -0.1653(2) 0.00827(9) Uani 1 1 d . . . 
H7 H 0.3102 0.1869 -0.2266 0.010 Uiso 1 1 calc R . . 
C8 C 0.6935(5) 0.8580(4) 0.0960(3) 0.00858(6) Uani 1 1 d . . . 
H13 H 0.7459 0.9731 0.1021 0.010 Uiso 1 1 calc R . . 
C9 C 0.5425(5) 0.5675(4) 0.0305(2) 0.00704(5) Uani 1 1 d . . . 
C10 C 0.6725(4) 0.7610(5) 0.1715(2) 0.00827(9) Uani 1 1 d . . . 
H14 H 0.7162 0.8025 0.2330 0.010 Uiso 1 1 calc R . . 
Cl19 Cl -0.08200(10) 0.44967(12) -0.21526(5) 0.00923(2) Uani 1 1 d . . . 
Cl20 Cl -0.16402(10) 0.14250(10) -0.07910(5) 0.00828(2) Uani 1 1 d . . . 
Cl25 Cl 0.09204(10) 0.54976(12) 0.22029(5) 0.00923(2) Uani 1 1 d . . . 
Cl26 Cl 0.17509(10) 0.85761(10) 0.08466(5) 0.00828(2) Uani 1 1 d . . . 
O18 O 0.0945(4) 0.7527(3) -0.1115(2) 0.01009(5) Uani 1 1 d . . . 
O24 O -0.0852(4) 0.2472(3) 0.1177(2) 0.01009(5) Uani 1 1 d . . . 
C15 C 0.0505(5) 0.6380(4) -0.0592(2) 0.00641(5) Uani 1 1 d . . . 
C16 C -0.0363(4) 0.4716(4) -0.0962(2) 0.00628(5) Uani 1 1 d . . . 
C17 C -0.0755(4) 0.3405(4) -0.0389(2) 0.00594(5) Uani 1 1 d . . . 
C21 C -0.0385(4) 0.3596(4) 0.0658(2) 0.00641(5) Uani 1 1 d . . . 
C22 C 0.0507(4) 0.5290(4) 0.1018(2) 0.00628(5) Uani 1 1 d . . . 
C23 C 0.0849(4) 0.6591(4) 0.0424(2) 0.00594(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C1 1.749(4) . ? 
S4 C2 1.752(3) . ? 
S5 C2 1.739(3) . ? 
S5 C3 1.748(3) . ? 
S11 C8 1.744(4) . ? 
S11 C9 1.747(3) . ? 
S12 C10 1.730(3) . ? 
S12 C9 1.757(3) . ? 
S12 Cl26 3.6181(11) . ? 
S12 Cl25 3.6821(11) . ? 
C1 C3 1.331(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3682(7) . ? 
C2 C15 3.352(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.348(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.712(3) . ? 
Cl19 S5 3.6847(11) 1_455 ? 
Cl20 C17 1.698(3) . ? 
Cl20 S11 3.4705(11) 1_445 ? 
Cl20 S5 3.6228(11) 1_455 ? 
Cl25 C22 1.703(3) . ? 
Cl26 C23 1.714(3) . ? 
Cl26 S4 3.4721(11) 1_565 ? 
O18 C15 1.228(4) . ? 
O24 C21 1.220(4) . ? 
C15 C23 1.463(4) . ? 
C15 C16 1.472(4) . ? 
C16 C17 1.353(4) . ? 
C17 C21 1.505(4) . ? 
C21 C22 1.494(4) . ? 
C21 C9 3.376(5) 1_455 ? 
C22 C23 1.357(4) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C1 S4 C2 94.92(16) . . ? 
C2 S5 C3 94.63(15) . . ? 
C8 S11 C9 94.92(16) . . ? 
C10 S12 C9 94.92(15) . . ? 
C10 S12 Cl26 78.38(12) . . ? 
C9 S12 Cl26 76.20(11) . . ? 
C10 S12 Cl25 113.04(11) . . ? 
C9 S12 Cl25 109.54(11) . . ? 
Cl26 S12 Cl25 51.46(2) . . ? 
C3 C1 S4 116.9(3) . . ? 
C3 C1 H6 121.6 . . ? 
S4 C1 H6 121.6 . . ? 
C9 C2 S5 122.68(11) . . ? 
C9 C2 S4 122.04(11) . . ? 
S5 C2 S4 115.27(17) . . ? 
C9 C2 C15 89.98(8) . . ? 
S5 C2 C15 84.73(13) . . ? 
S4 C2 C15 96.71(14) . . ? 
C1 C3 S5 118.2(3) . . ? 
C1 C3 H7 120.9 . . ? 
S5 C3 H7 120.9 . . ? 
C10 C8 S11 117.3(3) . . ? 
C10 C8 H13 121.4 . . ? 
S11 C8 H13 121.4 . . ? 
C2 C9 S11 122.45(11) . . ? 
C2 C9 S12 122.59(11) . . ? 
S11 C9 S12 114.94(17) . . ? 
C8 C10 S12 117.8(3) . . ? 
C8 C10 H14 121.1 . . ? 
S12 C10 H14 121.1 . . ? 
C16 Cl19 S5 76.77(11) . 1_455 ? 
C17 Cl20 S11 143.04(11) . 1_445 ? 
C17 Cl20 S5 76.84(11) . 1_455 ? 
S11 Cl20 S5 103.45(3) 1_445 1_455 ? 
C22 Cl25 S12 75.84(11) . . ? 
C23 Cl26 S4 142.19(11) . 1_565 ? 
C23 Cl26 S12 77.25(11) . . ? 
S4 Cl26 S12 103.58(3) 1_565 . ? 
O18 C15 C23 121.6(3) . . ? 
O18 C15 C16 121.4(3) . . ? 
C23 C15 C16 117.0(3) . . ? 
O18 C15 C2 95.9(2) . . ? 
C23 C15 C2 84.40(18) . . ? 
C16 C15 C2 88.50(19) . . ? 
C17 C16 C15 121.7(3) . . ? 
C17 C16 Cl19 121.4(2) . . ? 
C15 C16 Cl19 116.9(2) . . ? 
C16 C17 C21 121.7(3) . . ? 
C16 C17 Cl20 122.9(2) . . ? 
C21 C17 Cl20 115.3(2) . . ? 
O24 C21 C22 122.2(3) . . ? 
O24 C21 C17 122.1(3) . . ? 
C22 C21 C17 115.6(2) . . ? 
O24 C21 C9 95.3(2) . 1_455 ? 
C22 C21 C9 88.67(18) . 1_455 ? 
C17 C21 C9 83.16(18) . 1_455 ? 
C23 C22 C21 121.1(3) . . ? 
C23 C22 Cl25 123.4(3) . . ? 
C21 C22 Cl25 115.4(2) . . ? 
C22 C23 C15 122.6(3) . . ? 
C22 C23 Cl26 120.7(2) . . ? 
C15 C23 Cl26 116.7(2) . . ? 
 
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 
C2 S4 C1 C3 3.1(3) . . . . ? 
C3 S5 C2 C9 -179.78(13) . . . . ? 
C3 S5 C2 S4 1.7(2) . . . . ? 
C3 S5 C2 C15 -93.20(14) . . . . ? 
C1 S4 C2 C9 178.77(13) . . . . ? 
C1 S4 C2 S5 -2.7(2) . . . . ? 
C1 S4 C2 C15 84.57(15) . . . . ? 
S4 C1 C3 S5 -2.5(4) . . . . ? 
C2 S5 C3 C1 0.4(3) . . . . ? 
C9 S11 C8 C10 1.0(3) . . . . ? 
S5 C2 C9 S11 1.42(9) . . . . ? 
S4 C2 C9 S11 179.8(3) . . . . ? 
C15 C2 C9 S11 -82.30(14) . . . . ? 
S5 C2 C9 S12 -180.0(3) . . . . ? 
S4 C2 C9 S12 -1.58(8) . . . . ? 
C15 C2 C9 S12 96.32(17) . . . . ? 
C8 S11 C9 C2 -179.34(13) . . . . ? 
C8 S11 C9 S12 1.9(2) . . . . ? 
C10 S12 C9 C2 177.83(13) . . . . ? 
Cl26 S12 C9 C2 -105.43(9) . . . . ? 
Cl25 S12 C9 C2 -65.60(11) . . . . ? 
C10 S12 C9 S11 -3.5(2) . . . . ? 
Cl26 S12 C9 S11 73.29(17) . . . . ? 
Cl25 S12 C9 S11 113.12(16) . . . . ? 
S11 C8 C10 S12 -3.7(4) . . . . ? 
C9 S12 C10 C8 4.3(3) . . . . ? 
Cl26 S12 C10 C8 -70.5(3) . . . . ? 
Cl25 S12 C10 C8 -109.4(2) . . . . ? 
C10 S12 Cl25 C22 112.27(19) . . . . ? 
C9 S12 Cl25 C22 7.81(16) . . . . ? 
Cl26 S12 Cl25 C22 60.49(12) . . . . ? 
C10 S12 Cl26 C23 166.77(16) . . . . ? 
C9 S12 Cl26 C23 68.69(14) . . . . ? 
Cl25 S12 Cl26 C23 -60.80(11) . . . . ? 
C10 S12 Cl26 S4 25.64(12) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.45(11) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.06(3) . . . 1_565 ? 
C9 C2 C15 O18 73.9(2) . . . . ? 
S5 C2 C15 O18 -48.9(2) . . . . ? 
S4 C2 C15 O18 -163.8(2) . . . . ? 
C9 C2 C15 C23 -47.33(17) . . . . ? 
S5 C2 C15 C23 -170.16(19) . . . . ? 
S4 C2 C15 C23 75.0(2) . . . . ? 
C9 C2 C15 C16 -164.68(16) . . . . ? 
S5 C2 C15 C16 72.48(19) . . . . ? 
S4 C2 C15 C16 -42.4(2) . . . . ? 
O18 C15 C16 C17 176.2(3) . . . . ? 
C23 C15 C16 C17 -2.7(4) . . . . ? 
C2 C15 C16 C17 80.2(3) . . . . ? 
O18 C15 C16 Cl19 -2.7(4) . . . . ? 
C23 C15 C16 Cl19 178.3(2) . . . . ? 
C2 C15 C16 Cl19 -98.7(2) . . . . ? 
S5 Cl19 C16 C17 65.3(3) 1_455 . . . ? 
S5 Cl19 C16 C15 -115.8(2) 1_455 . . . ? 
C15 C16 C17 C21 2.0(4) . . . . ? 
Cl19 C16 C17 C21 -179.1(2) . . . . ? 
C15 C16 C17 Cl20 -176.4(2) . . . . ? 
Cl19 C16 C17 Cl20 2.5(4) . . . . ? 
S11 Cl20 C17 C16 -165.2(2) 1_445 . . . ? 
S5 Cl20 C17 C16 -70.3(3) 1_455 . . . ? 
S11 Cl20 C17 C21 16.2(3) 1_445 . . . ? 
S5 Cl20 C17 C21 111.2(2) 1_455 . . . ? 
C16 C17 C21 O24 174.8(3) . . . . ? 
Cl20 C17 C21 O24 -6.6(4) . . . . ? 
C16 C17 C21 C22 -2.3(4) . . . . ? 
Cl20 C17 C21 C22 176.2(2) . . . . ? 
C16 C17 C21 C9 82.9(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -98.6(2) . . . 1_455 ? 
O24 C21 C22 C23 -173.5(3) . . . . ? 
C17 C21 C22 C23 3.6(4) . . . . ? 
C9 C21 C22 C23 -78.2(3) 1_455 . . . ? 
O24 C21 C22 Cl25 2.8(4) . . . . ? 
C17 C21 C22 Cl25 179.9(2) . . . . ? 
C9 C21 C22 Cl25 98.2(2) 1_455 . . . ? 
S12 Cl25 C22 C23 -67.2(3) . . . . ? 
S12 Cl25 C22 C21 116.6(2) . . . . ? 
C21 C22 C23 C15 -4.7(4) . . . . ? 
Cl25 C22 C23 C15 179.3(2) . . . . ? 
C21 C22 C23 Cl26 176.3(2) . . . . ? 
Cl25 C22 C23 Cl26 0.2(4) . . . . ? 
O18 C15 C23 C22 -174.8(3) . . . . ? 
C16 C15 C23 C22 4.1(4) . . . . ? 
C2 C15 C23 C22 -81.3(3) . . . . ? 
O18 C15 C23 Cl26 4.3(4) . . . . ? 
C16 C15 C23 Cl26 -176.8(2) . . . . ? 
C2 C15 C23 Cl26 97.8(2) . . . . ? 
S4 Cl26 C23 C22 164.36(19) 1_565 . . . ? 
S12 Cl26 C23 C22 68.6(3) . . . . ? 
S4 Cl26 C23 C15 -14.7(4) 1_565 . . . ? 
S12 Cl26 C23 C15 -110.5(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.39 3.339(4) 178.3 1_545 
C8 H13 O24  0.95 2.40 3.347(4) 173.0 1_665 
C10 H14 O18  0.95 2.58 3.281(4) 131.0 2_565 
C3 H7 O24  0.95 2.54 3.267(4) 133.5 2_554 
 
_diffrn_measured_fraction_theta_max    0.902 
_diffrn_reflns_theta_full              33.56 
_diffrn_measured_fraction_theta_full   0.902 
_refine_diff_density_max    0.701 
_refine_diff_density_min   -0.505 
_refine_diff_density_rms    0.076 

#==END

 
data_Heated 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 'C6 H4 S4, C6 O2 Cl4'
_chemical_formula_sum 
 'C12 H4 Cl4 O2 S4' 
_chemical_formula_weight          450.19 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0003   0.0009 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.0836   0.0987 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'O'  'O'   0.0028   0.0036 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 'S'  'S'   0.0688   0.0765 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4 and Sasaki (1989)' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    'P n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, z+1/2' 

# These symmetry equivalent positions were chosen instead of
# 'x,y,z' and 'x+1/2, -y, z+1/2' for corresponding to the previous
# work reported by Garcia et al. (Faraday Discuss., 2007, 135, 217-235)
 
_cell_length_a                    7.2220(1) 
_cell_length_b                    7.5910(1) 
_cell_length_c                    14.4930(1) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.1370(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      784.457(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             black 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.906 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.653 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.91552 
_exptl_absorpt_correction_T_max   0.92702 
_exptl_absorpt_process_details    'PLATON-MULABS was used (A.L.Spek, 2008)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.56366 
_diffrn_radiation_type            synchrotron 
_diffrn_source_type              'PF-AR NW14A undulator beamline'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MarCCD 165 with MarDTB'  
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             46042 
_diffrn_reflns_av_R_equivalents   0.0324 
_diffrn_reflns_av_sigmaI/netI     0.0291 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        28 
_diffrn_reflns_theta_min          3.77 
_diffrn_reflns_theta_max          33.55 
_reflns_number_total              11130 
_reflns_number_gt                 10029 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'marccd software (Doyle, 2006)'
_computing_cell_refinement       'Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1998)'  
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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)+(0.0273P)²+0.0721P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.47(18) 
_refine_ls_number_reflns          11130 
_refine_ls_number_parameters      133 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0246 
_refine_ls_R_factor_gt            0.0213 
_refine_ls_wR_factor_ref          0.0600 
_refine_ls_wR_factor_gt           0.0588 
_refine_ls_goodness_of_fit_ref    1.089 
_refine_ls_restrained_S_all       1.089 
_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 
S4 S 0.39016(11) 0.23684(12) 0.01875(6) 0.00813(2) Uani 1 1 d . . . 
S5 S 0.44680(11) 0.44144(11) -0.14747(5) 0.00759(2) Uani 1 1 d . . . 
S11 S 0.62050(11) 0.76386(12) -0.01346(6) 0.00813(2) Uani 1 1 d . . . 
S12 S 0.56311(11) 0.55790(11) 0.15281(5) 0.00759(2) Uani 1 1 d . . . 
C1 C 0.3140(5) 0.1419(5) -0.0907(3) 0.00931(6) Uani 1 1 d . . . 
H6 H 0.2542 0.0301 -0.0968 0.011 Uiso 1 1 calc R . . 
C2 C 0.4673(5) 0.4324(4) -0.0258(2) 0.00758(5) Uani 1 1 d . . . 
C3 C 0.3442(5) 0.2345(5) -0.1651(3) 0.00905(8) Uani 1 1 d . . . 
H7 H 0.3103 0.1884 -0.2263 0.011 Uiso 1 1 calc R . . 
C8 C 0.6933(5) 0.8581(5) 0.0961(3) 0.00931(6) Uani 1 1 d . . . 
H13 H 0.7455 0.9732 0.1021 0.011 Uiso 1 1 calc R . . 
C9 C 0.5425(5) 0.5668(4) 0.0310(2) 0.00758(5) Uani 1 1 d . . . 
C10 C 0.6728(5) 0.7619(5) 0.1718(3) 0.00905(8) Uani 1 1 d . . . 
H14 H 0.7165 0.8036 0.2332 0.011 Uiso 1 1 calc R . . 
Cl19 Cl -0.08190(11) 0.44985(11) -0.21530(5) 0.01018(2) Uani 1 1 d . . . 
Cl20 Cl -0.16408(11) 0.14283(11) -0.07912(6) 0.00915(2) Uani 1 1 d . . . 
Cl25 Cl 0.09232(11) 0.54959(11) 0.22015(5) 0.01018(2) Uani 1 1 d . . . 
Cl26 Cl 0.17479(11) 0.85774(11) 0.08467(6) 0.00915(2) Uani 1 1 d . . . 
O18 O 0.0936(4) 0.7530(4) -0.1116(2) 0.01089(5) Uani 1 1 d . . . 
O24 O -0.0856(4) 0.2474(3) 0.1174(2) 0.01089(5) Uani 1 1 d . . . 
C15 C 0.0507(5) 0.6382(4) -0.0593(2) 0.00704(5) Uani 1 1 d . . . 
C16 C -0.0365(5) 0.4716(4) -0.0954(2) 0.00681(6) Uani 1 1 d . . . 
C17 C -0.0743(5) 0.3402(4) -0.0387(2) 0.00655(5) Uani 1 1 d . . . 
C21 C -0.0381(5) 0.3597(4) 0.0656(2) 0.00704(5) Uani 1 1 d . . . 
C22 C 0.0506(5) 0.5291(4) 0.1025(2) 0.00681(6) Uani 1 1 d . . . 
C23 C 0.0861(5) 0.6589(4) 0.0428(2) 0.00655(5) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
S4 C2 1.745(3) . ? 
S4 C1 1.749(4) . ? 
S5 C3 1.738(4) . ? 
S5 C2 1.748(4) . ? 
S11 C8 1.745(4) . ? 
S11 C9 1.756(3) . ? 
S12 C10 1.741(4) . ? 
S12 C9 1.749(4) . ? 
S12 Cl26 3.6251(12) . ? 
S12 Cl25 3.6838(13) . ? 
C1 C3 1.334(5) . ? 
C1 H6 0.9500 . ? 
C2 C9 1.3681(7) . ? 
C2 C15 3.356(5) . ? 
C3 H7 0.9500 . ? 
C8 C10 1.346(5) . ? 
C8 H13 0.9500 . ? 
C10 H14 0.9500 . ? 
Cl19 C16 1.724(3) . ? 
Cl19 S5 3.6903(13) 1_455 ? 
Cl20 C17 1.699(3) . ? 
Cl20 S11 3.4745(13) 1_445 ? 
Cl20 S5 3.6239(12) 1_455 ? 
Cl25 C22 1.691(3) . ? 
Cl26 C23 1.713(3) . ? 
Cl26 S4 3.4764(13) 1_565 ? 
O18 C15 1.227(4) . ? 
O24 C21 1.220(4) . ? 
C15 C23 1.470(5) . ? 
C15 C16 1.471(5) . ? 
C16 C17 1.348(5) . ? 
C17 C21 1.500(5) . ? 
C21 C22 1.497(4) . ? 
C21 C9 3.379(5) 1_455 ? 
C22 C23 1.363(5) . ? 
 
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 S4 C1 95.06(17) . . ? 
C3 S5 C2 94.48(17) . . ? 
C8 S11 C9 94.78(17) . . ? 
C10 S12 C9 95.09(17) . . ? 
C10 S12 Cl26 78.32(12) . . ? 
C9 S12 Cl26 76.26(12) . . ? 
C10 S12 Cl25 112.91(12) . . ? 
C9 S12 Cl25 109.49(12) . . ? 
Cl26 S12 Cl25 51.41(2) . . ? 
C3 C1 S4 116.6(3) . . ? 
C3 C1 H6 121.7 . . ? 
S4 C1 H6 121.7 . . ? 
C9 C2 S4 122.12(12) . . ? 
C9 C2 S5 122.65(12) . . ? 
S4 C2 S5 115.21(18) . . ? 
C9 C2 C15 90.05(8) . . ? 
S4 C2 C15 96.78(15) . . ? 
S5 C2 C15 84.55(14) . . ? 
C1 C3 S5 118.6(3) . . ? 
C1 C3 H7 120.7 . . ? 
S5 C3 H7 120.7 . . ? 
C10 C8 S11 117.6(3) . . ? 
C10 C8 H13 121.2 . . ? 
S11 C8 H13 121.2 . . ? 
C2 C9 S12 122.70(12) . . ? 
C2 C9 S11 122.30(12) . . ? 
S12 C9 S11 114.98(18) . . ? 
C8 C10 S12 117.4(3) . . ? 
C8 C10 H14 121.3 . . ? 
S12 C10 H14 121.3 . . ? 
C16 Cl19 S5 76.66(12) . 1_455 ? 
C17 Cl20 S11 142.99(12) . 1_445 ? 
C17 Cl20 S5 77.27(11) . 1_455 ? 
S11 Cl20 S5 103.37(3) 1_445 1_455 ? 
C22 Cl25 S12 76.04(12) . . ? 
C23 Cl26 S4 142.23(12) . 1_565 ? 
C23 Cl26 S12 76.86(11) . . ? 
S4 Cl26 S12 103.54(3) 1_565 . ? 
O18 C15 C23 121.7(3) . . ? 
O18 C15 C16 121.8(3) . . ? 
C23 C15 C16 116.5(3) . . ? 
O18 C15 C2 96.4(2) . . ? 
C23 C15 C2 83.99(19) . . ? 
C16 C15 C2 88.6(2) . . ? 
C17 C16 C15 122.4(3) . . ? 
C17 C16 Cl19 121.3(3) . . ? 
C15 C16 Cl19 116.3(2) . . ? 
C16 C17 C21 121.5(3) . . ? 
C16 C17 Cl20 123.1(3) . . ? 
C21 C17 Cl20 115.5(2) . . ? 
O24 C21 C22 121.7(3) . . ? 
O24 C21 C17 122.0(3) . . ? 
C22 C21 C17 116.2(3) . . ? 
O24 C21 C9 94.8(2) . 1_455 ? 
C22 C21 C9 88.6(2) . 1_455 ? 
C17 C21 C9 83.54(19) . 1_455 ? 
C23 C22 C21 120.5(3) . . ? 
C23 C22 Cl25 123.5(3) . . ? 
C21 C22 Cl25 115.9(2) . . ? 
C22 C23 C15 122.8(3) . . ? 
C22 C23 Cl26 120.6(3) . . ? 
C15 C23 Cl26 116.5(2) . . ? 
 
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 
C2 S4 C1 C3 3.0(3) . . . . ? 
C1 S4 C2 C9 178.79(14) . . . . ? 
C1 S4 C2 S5 -2.7(2) . . . . ? 
C1 S4 C2 C15 84.46(16) . . . . ? 
C3 S5 C2 C9 -179.75(14) . . . . ? 
C3 S5 C2 S4 1.7(2) . . . . ? 
C3 S5 C2 C15 -93.20(13) . . . . ? 
S4 C1 C3 S5 -2.3(4) . . . . ? 
C2 S5 C3 C1 0.3(3) . . . . ? 
C9 S11 C8 C10 0.9(3) . . . . ? 
S4 C2 C9 S12 -1.58(9) . . . . ? 
S5 C2 C9 S12 -180.0(3) . . . . ? 
C15 C2 C9 S12 96.46(19) . . . . ? 
S4 C2 C9 S11 179.9(3) . . . . ? 
S5 C2 C9 S11 1.55(9) . . . . ? 
C15 C2 C9 S11 -82.01(15) . . . . ? 
C10 S12 C9 C2 177.96(14) . . . . ? 
Cl26 S12 C9 C2 -105.40(10) . . . . ? 
Cl25 S12 C9 C2 -65.54(12) . . . . ? 
C10 S12 C9 S11 -3.5(2) . . . . ? 
Cl26 S12 C9 S11 73.18(18) . . . . ? 
Cl25 S12 C9 S11 113.03(17) . . . . ? 
C8 S11 C9 C2 -179.43(15) . . . . ? 
C8 S11 C9 S12 2.0(2) . . . . ? 
S11 C8 C10 S12 -3.6(4) . . . . ? 
C9 S12 C10 C8 4.2(3) . . . . ? 
Cl26 S12 C10 C8 -70.6(3) . . . . ? 
Cl25 S12 C10 C8 -109.4(3) . . . . ? 
C10 S12 Cl25 C22 112.29(19) . . . . ? 
C9 S12 Cl25 C22 7.71(16) . . . . ? 
Cl26 S12 Cl25 C22 60.49(12) . . . . ? 
C10 S12 Cl26 C23 166.89(17) . . . . ? 
C9 S12 Cl26 C23 68.62(16) . . . . ? 
Cl25 S12 Cl26 C23 -60.77(12) . . . . ? 
C10 S12 Cl26 S4 25.75(13) . . . 1_565 ? 
C9 S12 Cl26 S4 -72.52(12) . . . 1_565 ? 
Cl25 S12 Cl26 S4 158.09(3) . . . 1_565 ? 
C9 C2 C15 O18 74.0(2) . . . . ? 
S4 C2 C15 O18 -163.6(2) . . . . ? 
S5 C2 C15 O18 -48.8(2) . . . . ? 
C9 C2 C15 C23 -47.31(17) . . . . ? 
S4 C2 C15 C23 75.1(2) . . . . ? 
S5 C2 C15 C23 -170.1(2) . . . . ? 
C9 C2 C15 C16 -164.14(19) . . . . ? 
S4 C2 C15 C16 -41.8(2) . . . . ? 
S5 C2 C15 C16 73.0(2) . . . . ? 
O18 C15 C16 C17 176.1(3) . . . . ? 
C23 C15 C16 C17 -3.2(5) . . . . ? 
C2 C15 C16 C17 79.4(3) . . . . ? 
O18 C15 C16 Cl19 -2.0(5) . . . . ? 
C23 C15 C16 Cl19 178.8(2) . . . . ? 
C2 C15 C16 Cl19 -98.7(2) . . . . ? 
S5 Cl19 C16 C17 65.8(3) 1_455 . . . ? 
S5 Cl19 C16 C15 -116.1(3) 1_455 . . . ? 
C15 C16 C17 C21 3.1(5) . . . . ? 
Cl19 C16 C17 C21 -178.9(3) . . . . ? 
C15 C16 C17 Cl20 -176.6(3) . . . . ? 
Cl19 C16 C17 Cl20 1.4(4) . . . . ? 
S11 Cl20 C17 C16 -164.9(2) 1_445 . . . ? 
S5 Cl20 C17 C16 -69.5(3) 1_455 . . . ? 
S11 Cl20 C17 C21 15.4(4) 1_445 . . . ? 
S5 Cl20 C17 C21 110.8(3) 1_455 . . . ? 
C16 C17 C21 O24 174.0(3) . . . . ? 
Cl20 C17 C21 O24 -6.3(4) . . . . ? 
C16 C17 C21 C22 -2.9(4) . . . . ? 
Cl20 C17 C21 C22 176.8(2) . . . . ? 
C16 C17 C21 C9 82.4(3) . . . 1_455 ? 
Cl20 C17 C21 C9 -97.9(2) . . . 1_455 ? 
O24 C21 C22 C23 -173.8(3) . . . . ? 
C17 C21 C22 C23 3.0(4) . . . . ? 
C9 C21 C22 C23 -79.1(3) 1_455 . . . ? 
O24 C21 C22 Cl25 3.5(5) . . . . ? 
C17 C21 C22 Cl25 -179.6(2) . . . . ? 
C9 C21 C22 Cl25 98.3(2) 1_455 . . . ? 
S12 Cl25 C22 C23 -66.5(3) . . . . ? 
S12 Cl25 C22 C21 116.2(3) . . . . ? 
C21 C22 C23 C15 -3.5(4) . . . . ? 
Cl25 C22 C23 C15 179.4(3) . . . . ? 
C21 C22 C23 Cl26 176.1(3) . . . . ? 
Cl25 C22 C23 Cl26 -1.0(4) . . . . ? 
O18 C15 C23 C22 -175.8(3) . . . . ? 
C16 C15 C23 C22 3.4(4) . . . . ? 
C2 C15 C23 C22 -82.0(3) . . . . ? 
O18 C15 C23 Cl26 4.5(4) . . . . ? 
C16 C15 C23 Cl26 -176.3(3) . . . . ? 
C2 C15 C23 Cl26 98.4(2) . . . . ? 
S4 Cl26 C23 C22 164.6(2) 1_565 . . . ? 
S12 Cl26 C23 C22 69.4(3) . . . . ? 
S4 Cl26 C23 C15 -15.8(4) 1_565 . . . ? 
S12 Cl26 C23 C15 -111.0(3) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C1 H6 O18  0.95 2.40 3.345(5) 178.0 1_545 
C8 H13 O24  0.95 2.40 3.350(5) 173.0 1_665 
C10 H14 O18  0.95 2.58 3.280(5) 130.7 2_565 
C3 H7 O24  0.95 2.54 3.275(5) 133.9 2_554 
 
_diffrn_measured_fraction_theta_max    0.903 
_diffrn_reflns_theta_full              33.55 
_diffrn_measured_fraction_theta_full   0.903 
_refine_diff_density_max    0.793 
_refine_diff_density_min   -0.390 
_refine_diff_density_rms    0.075 

#==END
