data_17b
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
17b
;
_chemical_name_common             '17b'
_chemical_melting_point           '426'
_chemical_formula_moiety          'C19 H14 O5 S4'
_chemical_formula_sum             'C19 H14 O5 S4'
_chemical_formula_weight          450.58
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'C 2/c'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    12.696(9)
_cell_length_b                    17.151(12)
_cell_length_c                    10.238(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  114.694(5)
_cell_angle_gamma                 90.00
_cell_volume                      2025(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     'multi-scan'
_cell_measurement_theta_min       2.13
_cell_measurement_theta_max       26.49
 
_exptl_crystal_description        block
_exptl_crystal_colour             wihte
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.478
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              932
_exptl_absorpt_coefficient_mu     0.502
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.867
_exptl_absorpt_correction_T_max   0.942
_exptl_absorpt_process_details    
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
 
_exptl_special_details
;
the white block single crystals were obtained by slowly
evaporation of solvent dichloromethane
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             6363
_diffrn_reflns_av_R_equivalents   0.0271
_diffrn_reflns_av_sigmaI/netI     0.0325
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          2.13
_diffrn_reflns_theta_max          26.49
_reflns_number_total              2085
_reflns_number_gt                 1419
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT A'
_computing_structure_solution     'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1999)'
 
_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)+(0.0387P)²+1.8816P] 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_number_reflns          2085
_refine_ls_number_parameters      128
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0718
_refine_ls_R_factor_gt            0.0426
_refine_ls_wR_factor_ref          0.1073
_refine_ls_wR_factor_gt           0.0916
_refine_ls_goodness_of_fit_ref    1.018
_refine_ls_restrained_S_all       1.018
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000

 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.5000 -0.1842(3) 0.7500 0.0877(15) Uani 1 2 d S . .
C2 C 0.4579(2) -0.03756(13) 0.6828(3) 0.0474(6) Uani 1 1 d . . .
C3 C 0.2732(2) 0.06296(15) 0.5818(3) 0.0498(6) Uani 1 1 d . . .
C4 C 0.1976(2) 0.11838(15) 0.4910(3) 0.0536(6) Uani 1 1 d . . .
C5 C 0.0931(2) 0.13232(18) 0.4996(3) 0.0711(8) Uani 1 1 d . . .
C6 C 0.0636(3) 0.0932(2) 0.5961(4) 0.0827(10) Uani 1 1 d . . .
C7 C 0.1376(3) 0.03865(18) 0.6845(4) 0.0747(9) Uani 1 1 d . . .
C8 C 0.2417(2) 0.02360(16) 0.6784(3) 0.0591(7) Uani 1 1 d . . .
C9 C 0.2295(3) 0.16380(16) 0.3903(3) 0.0572(7) Uani 1 1 d . . .
C10 C 0.1687(3) 0.2570(2) 0.2041(3) 0.0888(11) Uani 1 1 d . . .
H5 H 0.0421 0.1689 0.4387 0.085 Uiso 1 1 calc R . .
H6 H -0.0064 0.1037 0.6014 0.099 Uiso 1 1 calc R . .
H7 H 0.1173 0.0115 0.7492 0.090 Uiso 1 1 calc R . .
H8 H 0.2916 -0.0134 0.7397 0.071 Uiso 1 1 calc R . .
H10A H 0.1028 0.2894 0.1521 0.133 Uiso 1 1 calc R . .
H10B H 0.1817 0.2225 0.1383 0.133 Uiso 1 1 calc R . .
H10C H 0.2360 0.2890 0.2518 0.133 Uiso 1 1 calc R . .
O1 O 0.5000 -0.25399(19) 0.7500 0.1347(17) Uani 1 2 d S . .
O2 O 0.3194(2) 0.15816(14) 0.3811(3) 0.0962(8) Uani 1 1 d . . .
O3 O 0.14728(18) 0.21178(13) 0.3091(2) 0.0826(7) Uani 1 1 d . . .
S1 S 0.40760(7) -0.12703(5) 0.60425(9) 0.0758(3) Uani 1 1 d . . .
S2 S 0.40900(6) 0.04568(4) 0.57546(8) 0.0595(2) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.197(5) . ?
C1 S1 1.761(3) . ?
C2 S1 1.727(3) . ?
C2 C2 1.344(5) 2_656 ?
C1 S1 1.761(3) 2_656 ?
C2 S2 1.750(3) . ?
S2 C3 1.777(3) . ?
C3 C4 1.394(3) . ?
C4 C5 1.386(4) . ?
C5 C6 1.370(4) . ?
C6 C7 1.366(4) . ?
C7 C8 1.373(4) . ?
C8 C3 1.388(3) . ?
C4 C9 1.477(4) . ?
C9 O2 1.189(3) . ?
C9 O3 1.316(3) . ?
C10 O3 1.441(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 S1 123.83(12) . . ?
O1 C1 S1 123.83(12) . 2_656 ?
S1 C1 S1 112.3(2) 2_656 . ?
C2 S1 C1 96.56(16) . . ?
C2 C2 S1 117.27(9) 2_656 . ?
C2 C2 S2 124.39(9) 2_656 . ?
S1 C2 S2 117.86(15) . . ?
C2 S2 C3 102.03(12) . . ?
S2 C3 C4 119.87(19) . . ?
S2 C3 C8 121.2(2) . . ?
C3 C4 C5 119.1(3) . . ?
C4 C5 C6 121.2(3) . . ?
C5 C6 C7 119.6(3) . . ?
C6 C7 C8 120.5(3) . . ?
C7 C8 C3 120.7(3) . . ?
C8 C3 C4 118.9(2) . . ?
C3 C4 C9 120.8(2) . . ?
C5 C4 C9 120.1(3) . . ?
O2 C9 C4 124.4(3) . . ?
O3 C9 C4 113.2(3) . . ?
O2 C9 O3 122.4(3) . . ?
C9 O3 C10 117.4(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C3 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
O3 C10 H10A 109.5 . . ?
O3 C10 H10B 109.5 . . ?
O3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              26.49
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    0.220
_refine_diff_density_min   -0.283
_refine_diff_density_rms    0.044



#==============================================================================

#     End of CIF

#==============================================================================






data_24b
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
24b
;
_chemical_name_common             '24b'
_chemical_melting_point           '381'
_chemical_formula_moiety          'C15 H8 N2 O5 S4'
_chemical_formula_sum             'C15 H8 N2 O5 S4'
_chemical_formula_weight          424.19
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P -1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    11.066(12)
_cell_length_b                    11.928(13)
_cell_length_c                    13.426(14)
_cell_angle_alpha                 78.033(10)
_cell_angle_beta                  89.127(10)
_cell_angle_gamma                 86.984(9)
_cell_volume                      1731(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     13065
_cell_measurement_theta_min       2.40
_cell_measurement_theta_max       26.46
 
_exptl_crystal_description        block
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.629
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              864
_exptl_absorpt_coefficient_mu     0.579
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.966
_exptl_absorpt_correction_T_max   0.971
_exptl_absorpt_process_details    
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

 
_exptl_special_details
;
the yellow block single crystals were obtained by slowly
evaporation of solvent dichloromethane
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_reflns_number             13065
_diffrn_reflns_av_R_equivalents   0.0368
_diffrn_reflns_av_sigmaI/netI     0.0685
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          2.40
_diffrn_reflns_theta_max          26.46
_reflns_number_total              6901
_reflns_number_gt                 4080
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT A'
_computing_structure_solution     'SIR2004 (Giacovazzo et al, 2004)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1999)'
 
_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)+(0.0736P)²+1.1177P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          6901
_refine_ls_number_parameters      424
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1165
_refine_ls_R_factor_gt            0.0653
_refine_ls_wR_factor_ref          0.1770
_refine_ls_wR_factor_gt           0.1516
_refine_ls_goodness_of_fit_ref    1.036
_refine_ls_restrained_S_all       1.036
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.5428(3) 0.1794(3) 0.8906(2) 0.0451(8) Uani 1 1 d . . .
C2 C 0.5190(3) -0.0230(3) 0.8456(2) 0.0382(8) Uani 1 1 d . . .
C3 C 0.4049(3) 0.0189(2) 0.8558(2) 0.0366(8) Uani 1 1 d . . .
C4 C 0.6712(3) -0.1416(3) 0.7405(2) 0.0400(8) Uani 1 1 d . . .
C5 C 0.7797(3) -0.2077(3) 0.7466(2) 0.0435(8) Uani 1 1 d . . .
C6 C 0.8724(3) -0.1827(3) 0.6778(3) 0.0654(11) Uani 1 1 d . . .
C7 C 0.8564(5) -0.0916(4) 0.5972(3) 0.0856(15) Uani 1 1 d . . .
C8 C 0.7487(5) -0.0285(3) 0.5855(3) 0.0806(14) Uani 1 1 d . . .
C9 C 0.6569(4) -0.0527(3) 0.6568(3) 0.0619(11) Uani 1 1 d . . .
C10 C 0.1788(3) 0.0320(3) 0.7750(2) 0.0376(8) Uani 1 1 d . . .
C11 C 0.0543(3) 0.0342(3) 0.7882(2) 0.0413(8) Uani 1 1 d . . .
C12 C -0.0234(3) 0.1101(3) 0.7238(3) 0.0556(10) Uani 1 1 d . . .
C13 C 0.0235(4) 0.1848(3) 0.6435(3) 0.0601(10) Uani 1 1 d . . .
C14 C 0.1468(4) 0.1838(3) 0.6277(3) 0.0572(10) Uani 1 1 d . . .
C15 C 0.2240(3) 0.1087(3) 0.6926(2) 0.0498(9) Uani 1 1 d . . .
H6 H 0.9448 -0.2267 0.6857 0.078 Uiso 1 1 calc R . .
H7 H 0.9187 -0.0728 0.5505 0.103 Uiso 1 1 calc R . .
H8 H 0.7371 0.0312 0.5292 0.097 Uiso 1 1 calc R . .
H9 H 0.5846 -0.0085 0.6482 0.074 Uiso 1 1 calc R . .
H12 H -0.1065 0.1100 0.7352 0.067 Uiso 1 1 calc R . .
H13 H -0.0274 0.2361 0.5995 0.072 Uiso 1 1 calc R . .
H14 H 0.1786 0.2345 0.5726 0.069 Uiso 1 1 calc R . .
H15 H 0.3070 0.1097 0.6809 0.060 Uiso 1 1 calc R . .
N1 N 0.7984(3) -0.3093(3) 0.8274(2) 0.0559(8) Uani 1 1 d . . .
N2 N -0.0006(3) -0.0465(3) 0.8711(2) 0.0573(8) Uani 1 1 d . . .
O1 O 0.5826(2) 0.2648(2) 0.91013(19) 0.0669(7) Uani 1 1 d . . .
O2 O 0.9012(3) -0.3431(2) 0.8530(2) 0.0999(10) Uani 1 1 d . . .
O3 O 0.7090(3) -0.3598(2) 0.86150(19) 0.0723(8) Uani 1 1 d . . .
O4 O 0.0539(2) -0.1383(2) 0.90226(19) 0.0676(7) Uani 1 1 d . . .
O5 O -0.0969(2) -0.0197(3) 0.9058(2) 0.1160(13) Uani 1 1 d . . .
S1 S 0.63607(7) 0.06379(7) 0.86392(7) 0.0480(2) Uani 1 1 d . . .
S2 S 0.38740(7) 0.15486(7) 0.88648(7) 0.0484(2) Uani 1 1 d . . .
S3 S 0.55721(8) -0.16541(7) 0.83635(7) 0.0483(2) Uani 1 1 d . . .
S4 S 0.27707(7) -0.06299(7) 0.86177(6) 0.0453(2) Uani 1 1 d . . .
C16 C 0.5356(3) 0.2730(3) 0.6127(2) 0.0430(8) Uani 1 1 d . . .
C17 C 0.6716(3) 0.4430(3) 0.6266(2) 0.0378(8) Uani 1 1 d . . .
C18 C 0.5582(3) 0.4833(2) 0.6394(2) 0.0357(7) Uani 1 1 d . . .
C19 C 0.8902(3) 0.4510(3) 0.7147(2) 0.0396(8) Uani 1 1 d . . .
C20 C 1.0153(3) 0.4570(3) 0.7150(3) 0.0450(9) Uani 1 1 d . . .
C21 C 1.0866(3) 0.3938(3) 0.7924(3) 0.0608(10) Uani 1 1 d . . .
C22 C 1.0336(4) 0.3238(3) 0.8730(3) 0.0714(12) Uani 1 1 d . . .
C23 C 0.9085(4) 0.3163(3) 0.8762(3) 0.0633(11) Uani 1 1 d . . .
C24 C 0.8387(3) 0.3793(3) 0.7982(2) 0.0488(9) Uani 1 1 d . . .
C25 C 0.4179(3) 0.6052(3) 0.7511(2) 0.0373(8) Uani 1 1 d . . .
C26 C 0.3115(3) 0.6710(3) 0.7553(2) 0.0407(8) Uani 1 1 d . . .
C27 C 0.2332(3) 0.6491(3) 0.8367(3) 0.0572(10) Uani 1 1 d . . .
C28 C 0.2608(4) 0.5598(3) 0.9174(3) 0.0631(11) Uani 1 1 d . . .
C29 C 0.3675(3) 0.4952(3) 0.9159(2) 0.0552(10) Uani 1 1 d . . .
C30 C 0.4451(3) 0.5169(3) 0.8339(2) 0.0468(9) Uani 1 1 d . . .
H21 H 1.1702 0.3989 0.7897 0.073 Uiso 1 1 calc R . .
H22 H 1.0810 0.2813 0.9255 0.086 Uiso 1 1 calc R . .
H23 H 0.8721 0.2687 0.9308 0.076 Uiso 1 1 calc R . .
H24 H 0.7551 0.3741 0.8012 0.059 Uiso 1 1 calc R . .
H27 H 0.1621 0.6941 0.8372 0.069 Uiso 1 1 calc R . .
H28 H 0.2079 0.5434 0.9724 0.076 Uiso 1 1 calc R . .
H29 H 0.3873 0.4361 0.9711 0.066 Uiso 1 1 calc R . .
H30 H 0.5165 0.4721 0.8340 0.056 Uiso 1 1 calc R . .
N3 N 1.0763(3) 0.5339(3) 0.6328(2) 0.0515(8) Uani 1 1 d . . .
N4 N 0.2810(3) 0.7688(2) 0.6727(2) 0.0515(8) Uani 1 1 d . . .
O6 O 0.4966(2) 0.1829(2) 0.60487(18) 0.0603(7) Uani 1 1 d . . .
O7 O 1.1865(2) 0.5209(2) 0.62445(19) 0.0790(8) Uani 1 1 d . . .
O8 O 1.0151(2) 0.6086(2) 0.57633(19) 0.0665(7) Uani 1 1 d . . .
O9 O 0.3644(2) 0.8163(2) 0.62219(19) 0.0651(7) Uani 1 1 d . . .
O10 O 0.1747(2) 0.8008(2) 0.6592(2) 0.0821(9) Uani 1 1 d . . .
S5 S 0.69032(7) 0.30409(7) 0.60324(7) 0.0497(2) Uani 1 1 d . . .
S6 S 0.44172(7) 0.39068(7) 0.63366(6) 0.0456(2) Uani 1 1 d . . .
S7 S 0.79851(7) 0.52791(7) 0.61290(6) 0.0457(2) Uani 1 1 d . . .
S8 S 0.51685(7) 0.62671(7) 0.64369(6) 0.0449(2) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.210(4) . ?
C1 S1 1.772(4) . ?
C1 S2 1.763(4) . ?
C2 C3 1.349(4) . ?
C2 S1 1.751(3) . ?
C3 S2 1.755(3) . ?
C2 S3 1.757(3) . ?
C3 S4 1.753(3) . ?
C4 S3 1.779(3) . ?
C4 C5 1.395(4) . ?
C5 C6 1.372(4) . ?
C6 C7 1.371(5) . ?
C7 C8 1.369(6) . ?
C8 C9 1.386(5) . ?
C4 C9 1.380(4) . ?
C5 N1 1.458(4) . ?
N1 O2 1.216(3) . ?
N1 O3 1.219(3) . ?
C10 S4 1.784(3) . ?
C10 C11 1.385(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.363(5) . ?
C13 C14 1.377(5) . ?
C14 C15 1.382(4) . ?
C10 C15 1.387(4) . ?
C11 N2 1.461(4) . ?
N2 O4 1.219(3) . ?
N2 O5 1.210(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O6 1.203(4) . ?
C16 S5 1.768(4) . ?
C16 S6 1.769(4) . ?
C17 C18 1.341(4) . ?
C17 S5 1.751(3) . ?
C18 S6 1.754(3) . ?
C17 S7 1.760(3) . ?
C19 S7 1.779(3) . ?
C19 C20 1.390(4) . ?
C20 C21 1.381(4) . ?
C21 C22 1.367(5) . ?
C22 C23 1.391(5) . ?
C23 C24 1.376(4) . ?
C19 C24 1.395(4) . ?
C20 N3 1.462(4) . ?
N3 O7 1.228(3) . ?
N3 O8 1.225(3) . ?
C18 S8 1.760(3) . ?
C25 S8 1.781(3) . ?
C25 C26 1.387(4) . ?
C26 C27 1.374(4) . ?
C27 C28 1.378(5) . ?
C28 C29 1.378(5) . ?
C29 C30 1.376(4) . ?
C25 C30 1.388(4) . ?
C26 N4 1.463(4) . ?
N4 O9 1.228(3) . ?
N4 O10 1.222(3) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 S1 123.1(3) . . ?
O1 C1 S2 124.4(3) . . ?
S1 C1 S2 112.6(2) . . ?
C1 S1 C2 96.79(17) . . ?
C3 C2 S1 116.8(2) . . ?
C2 C3 S2 117.1(2) . . ?
C1 S2 C3 96.70(15) . . ?
C3 C2 S3 124.2(2) . . ?
S1 C2 S3 118.10(18) . . ?
C2 S3 C4 99.94(15) . . ?
S3 C4 C5 122.8(3) . . ?
S3 C4 C9 120.5(3) . . ?
C4 C5 C6 122.8(3) . . ?
C5 C6 C7 118.9(4) . . ?
C6 C7 C8 120.1(4) . . ?
C7 C8 C9 120.5(4) . . ?
C8 C9 C4 121.0(4) . . ?
C9 C4 C5 116.6(3) . . ?
C4 C5 N1 120.4(3) . . ?
C6 C5 N1 116.8(3) . . ?
C5 N1 O2 119.1(3) . . ?
C5 N1 O3 117.2(3) . . ?
O2 N1 O3 123.5(3) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C4 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C2 C3 S4 123.7(2) . . ?
S2 C3 S4 118.18(17) . . ?
C3 S4 C10 100.85(16) . . ?
S4 C10 C11 121.6(3) . . ?
S4 C10 C15 121.3(3) . . ?
C10 C11 C12 122.5(3) . . ?
C11 C12 C13 119.2(3) . . ?
C12 C13 C14 119.6(3) . . ?
C13 C14 C15 121.0(3) . . ?
C14 C15 C10 120.6(3) . . ?
C15 C10 C11 117.0(3) . . ?
C10 C11 N2 120.4(3) . . ?
C12 C11 N2 117.1(3) . . ?
C11 N2 O4 117.7(3) . . ?
C11 N2 O5 119.1(3) . . ?
O4 N2 O5 123.2(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
O6 C16 S5 124.7(3) . . ?
O6 C16 S6 122.9(3) . . ?
S5 C16 S6 112.4(2) . . ?
C16 S5 C17 96.57(15) . . ?
S5 C17 C18 117.3(2) . . ?
C17 C18 S6 116.9(2) . . ?
C18 S6 C16 96.64(17) . . ?
S5 C17 S7 118.09(17) . . ?
C18 C17 S7 123.8(3) . . ?
C17 S7 C19 100.66(15) . . ?
S7 C19 C20 122.5(3) . . ?
S7 C19 C24 120.8(3) . . ?
C19 C20 C21 122.4(3) . . ?
C20 C21 C22 119.6(4) . . ?
C21 C22 C23 119.8(4) . . ?
C22 C23 C24 119.8(4) . . ?
C23 C24 C19 121.7(3) . . ?
C24 C19 C20 116.6(3) . . ?
C19 C20 N3 120.3(3) . . ?
C21 C20 N3 117.3(3) . . ?
C20 N3 O7 118.3(3) . . ?
C20 N3 O8 118.4(3) . . ?
O7 N3 O8 123.3(3) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C19 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
S6 C18 S8 117.71(17) . . ?
C17 C18 S8 124.7(2) . . ?
C18 S8 C25 100.11(14) . . ?
S8 C25 C26 123.0(2) . . ?
S8 C25 C30 119.4(2) . . ?
C25 C26 C27 122.1(3) . . ?
C26 C27 C28 119.5(3) . . ?
C27 C28 C29 119.4(3) . . ?
C28 C29 C30 120.8(3) . . ?
C29 C30 C25 120.6(3) . . ?
C30 C25 C26 117.5(3) . . ?
C25 C26 N4 120.1(3) . . ?
C27 C26 N4 117.8(3) . . ?
O26 N4 O9 117.9(3) . . ?
C26 N4 O10 118.6(3) . . ?
O9 N4 O10 123.5(3) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C25 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
_diffrn_measured_fraction_theta_max    0.967
_diffrn_reflns_theta_full              26.46
_diffrn_measured_fraction_theta_full   0.967
_refine_diff_density_max    0.292
_refine_diff_density_min   -0.290
_refine_diff_density_rms    0.054





#==============================================================================

#     End of CIF

#==============================================================================

 
 
data_34a
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
34a
;
_chemical_name_common             '34a'
_chemical_melting_point           '562'
_chemical_formula_moiety          'C11 H6 O2 S5'
_chemical_formula_sum             'C11 H6 O2 S5'
_chemical_formula_weight          330.49
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    'P m n b'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y+1/2, z+1/2'
 'x+1/2, -y, -z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, y-1/2, -z-1/2'
 '-x-1/2, y, z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    10.892(3)
_cell_length_b                    8.0130(19)
_cell_length_c                    14.444(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1260.6(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     8219
_cell_measurement_theta_min       2.34
_cell_measurement_theta_max       26.38
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'yellow'
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.741
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              672
_exptl_absorpt_coefficient_mu     0.906
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.913
_exptl_absorpt_correction_T_max   0.956
_exptl_absorpt_process_details    
;CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
 
_exptl_special_details
;
The yellow block single crystals were obtained by slowly
evaporation of solvent dichloromethane
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             8219
_diffrn_reflns_av_R_equivalents   0.0349
_diffrn_reflns_av_sigmaI/netI     0.0260
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.34
_diffrn_reflns_theta_max          26.39
_reflns_number_total              1356
_reflns_number_gt                 1093
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT A'  
_computing_structure_solution     'SIR2004 (Giacovazzo et al, 2004)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1999)'
 
_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)+(0.0296P)²+1.5112P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.034(2)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1356
_refine_ls_number_parameters      95
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0466
_refine_ls_R_factor_gt            0.0346
_refine_ls_wR_factor_ref          0.0919
_refine_ls_wR_factor_gt           0.0814
_refine_ls_goodness_of_fit_ref    1.046
_refine_ls_restrained_S_all       1.046
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.2500 0.3996(5) 0.4944(2) 0.0583(12) Uani 1 2 d S . .
C2 C 0.1886(3) 0.2700(3) 0.33718(15) 0.0432(6) Uani 1 1 d . . .
C3 C 0.1860(2) 0.2771(3) 0.15108(14) 0.0341(5) Uani 1 1 d . . .
C4 C 0.1231(2) 0.3333(3) 0.07388(15) 0.0384(6) Uani 1 1 d . . .
C5 C 0.1862(2) 0.3815(3) -0.00446(15) 0.0361(5) Uani 1 1 d . . .
C61 C 0.1948(8) 0.4315(10) -0.1638(5) 0.0509(18) Uani 0.50 1 d P . 1
C62 C 0.1859(9) 0.5151(9) -0.1477(5) 0.0537(19) Uani 0.50 1 d P . 2
H1 H 0.0378 0.3387 0.0748 0.046 Uiso 1 1 calc R . .
H61A H 0.1699 0.3362 -0.2007 0.061 Uiso 0.50 1 calc PR . 1
H61B H 0.1699 0.5300 -0.1981 0.061 Uiso 0.50 1 calc PR . 1
H62A H 0.1598 0.6307 -0.1445 0.064 Uiso 0.50 1 calc PR . 2
H62B H 0.1598 0.4731 -0.2075 0.064 Uiso 0.50 1 calc PR . 2
O1 O 0.11935(16) 0.4280(3) -0.08063(11) 0.0505(5) Uani 1 1 d . . .
S1 S 0.2500 0.47538(17) 0.60045(7) 0.0881(6) Uani 1 2 d S . .
S2 S 0.11773(8) 0.35574(10) 0.43364(4) 0.0577(3) Uani 1 1 d . . .
S3 S 0.10016(7) 0.19691(10) 0.24486(4) 0.0501(3) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 S1 1.648(4) . ?
C1 S2 1.722(2) . ?
C1 S2 1.723(2) 7_655 ?
C2 S2 1.735(2) . ?
C2 C2 1.337(6) 7_655 ?
C2 S3 1.746(3) . ?
C3 S3 1.767(2) . ?
C3 C3 1.394(5) 7_655 ?
C3 C4 1.384(3) . ?
C4 C5 1.379(3) . ?
C5 C5 1.390(5) 7_655 ?
C5 O1 1.371(3) . ?
O1 C62 1.396(9) . ?
O1 C61 1.456(8) . ?
C61 C61 1.203(17) 7_655 ?
C62 C62 1.397(19) 7_655 ?
C4 H1 0.9300 . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
 
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
S1 C1 S2 123.24(10) . . ?
S1 C1 S2 123.28(10) . 7_655 ?
S2 C1 S2 113.5(2) . 7_655 ?
C1 S2 C2 96.72(14) . . ?
C2 C2 S2 116.46(10) 7_655 . ?
S2 C2 S3 120.03(17) . . ?
C2 C2 S3 123.47(9) 7_655 . ?
C2 S3 C3 99.87(11) . . ?
C3 C3 S3 121.96(8) 7_655 . ?
S3 C3 C4 118.30(19) . . ?
C4 C3 C3 119.66(14) . 7_655 ?
C3 C4 C5 120.4(2) . . ?
C4 C5 C5 119.91(14) . 7_655 ?
C4 C5 O1 118.0(2) . . ?
O1 C5 C5 122.05(12) . 7_655 ?
C5 O1 C61 111.6(3) . . ?
C5 O1 C62 114.6(4) . . ?
C61 O1 C62 29.0(3) . . ?
O1 C61 C61 124.4(3) 7_655 . ?
O1 C62 C62 121.3(4) . 7_655 ?
C3 C4 H1 119.8 . . ?
C5 C4 H1 119.8 . . ?
C61 C61 H61A 106.2 7_655 . ?
C61 C61 H61B 106.2 7_655 . ?
C62 C62 H62A 107.0 7_655 . ?
C62 C62 H62B 107.0 7_655 . ?
H61A C61 H61B 106.4 . . ?
H62A C62 H62B 106.7 . . ?
O1 C61 H61A 106.2 . . ?
O1 C61 H61B 106.2 . . ?
O1 C62 H62A 107.0 . . ?
O1 C62 H62B 107.0 . . ?

 
_diffrn_measured_fraction_theta_max    0.999
_diffrn_reflns_theta_full              26.39
_diffrn_measured_fraction_theta_full   0.999
_refine_diff_density_max    0.437
_refine_diff_density_min   -0.375
_refine_diff_density_rms    0.056





#==============================================================================

#     End of CIF

#==============================================================================

 
data_35a
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
35a
;
_chemical_name_common             '35a'
_chemical_melting_point           '480'
_chemical_formula_moiety          'C9 H6 S6'
_chemical_formula_sum             'C9 H6 S6'
_chemical_formula_weight          306.53
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    'P b c a'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 '-x-1/2, y-1/2, z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    11.411(3)
_cell_length_b                    11.3850(17)
_cell_length_c                    19.507(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2534.2(8)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     2427
_cell_measurement_theta_min       3.13
_cell_measurement_theta_max       26.32
 
_exptl_crystal_description        block
_exptl_crystal_colour             'brown'
_exptl_crystal_size_max           0.5
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.607
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1248
_exptl_absorpt_coefficient_mu     1.041
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.65813
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
 
_exptl_special_details
;
the brown block single crystals were obtained by slowly
evaporation of solvent dichloromethane
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  16.0733
_diffrn_reflns_number             6833
_diffrn_reflns_av_R_equivalents   0.0362
_diffrn_reflns_av_sigmaI/netI     0.0503
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          3.30
_diffrn_reflns_theta_max          28.35
_reflns_number_total              2770
_reflns_number_gt                 2146
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Aligent superNova'
_computing_cell_refinement        'CrysAlisPro, Agilent Technologies'
_computing_data_reduction         'CrysAlisPro, Agilent Technologies'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1999)'
 
_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)+(0.0281P)²+3.0482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2770
_refine_ls_number_parameters      138
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0586
_refine_ls_R_factor_gt            0.0402
_refine_ls_wR_factor_ref          0.1085
_refine_ls_wR_factor_gt           0.0814
_refine_ls_goodness_of_fit_ref    1.095
_refine_ls_restrained_S_all       1.095
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.3494(3) 0.2119(3) 0.49272(17) 0.0361(8) Uani 1 1 d . . .
C2 C 0.3676(3) 0.0230(3) 0.56978(17) 0.0374(8) Uani 1 1 d . . .
C3 C 0.4594(3) 0.0932(3) 0.59007(17) 0.0370(8) Uani 1 1 d . . .
C4 C 0.3665(3) -0.0890(3) 0.69277(17) 0.0340(7) Uani 1 1 d . . .
C5 C 0.4618(3) -0.0113(3) 0.71516(16) 0.0319(7) Uani 1 1 d . . .
C6 C 0.3023(3) -0.1376(3) 0.74627(18) 0.0361(8) Uani 1 1 d . . .
C7 C 0.4691(3) -0.0010(3) 0.78569(17) 0.0355(7) Uani 1 1 d . . .
C8 C 0.1986(3) -0.2233(3) 0.7438(2) 0.0459(9) Uani 1 1 d . . .
C9 C 0.5576(3) 0.0695(3) 0.8281(2) 0.0489(9) Uani 1 1 d . . .
H8A H 0.1649 -0.2226 0.6987 0.069 Uiso 1 1 calc R . .
H8B H 0.1406 -0.1998 0.7767 0.069 Uiso 1 1 calc R . .
H8C H 0.2255 -0.3011 0.7544 0.069 Uiso 1 1 calc R . .
H9A H 0.6304 0.0275 0.8303 0.073 Uiso 1 1 calc R . .
H9B H 0.5275 0.0808 0.8736 0.073 Uiso 1 1 calc R . .
H9C H 0.5703 0.1446 0.8069 0.073 Uiso 1 1 calc R . .
S1 S 0.30813(9) 0.31148(8) 0.43477(5) 0.0478(3) Uani 1 1 d . . .
S2 S 0.27268(9) 0.07912(7) 0.50542(5) 0.0416(2) Uani 1 1 d . . .
S3 S 0.47015(8) 0.23032(8) 0.54836(5) 0.0418(2) Uani 1 1 d . . .
S4 S 0.33904(9) -0.11991(7) 0.60410(5) 0.0437(3) Uani 1 1 d . . .
S5 S 0.56239(8) 0.05726(9) 0.65652(5) 0.0444(2) Uani 1 1 d . . .
S6 S 0.36131(8) -0.08954(8) 0.82478(4) 0.0400(2) 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
S1 C1 1.669(3) . ?
S3 C1 1.767(4) . ?
S2 C1 1.764(3) . ?
S2 C2 1.777(4) . ?
S3 C3 1.765(3) . ?
C3 C2 1.376(5) . ?
S4 C2 1.789(3) . ?
S5 C3 1.797(4) . ?
S4 C4 1.793(3) . ?
S5 C5 1.798(3) . ?
C5 C4 1.468(4) . ?
C6 C4 1.390(5) . ?
C7 C5 1.383(4) . ?
S6 C6 1.760(4) . ?
S6 C7 1.764(4) . ?
C6 C8 1.534(5) . ?
C7 C9 1.532(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
S1 C1 S2 122.5(2) . . ?
S1 C1 S3 123.7(2) . . ?
S2 C1 S3 113.73(18) . . ?
C1 S2 C2 96.04(16) . . ?
C1 S3 C3 97.11(16) . . ?
C3 C2 S2 117.3(3) . . ?
C2 C3 S3 115.8(3) . . ?
C3 C2 S4 124.0(3) . . ?
C2 C3 S5 125.0(3) . . ?
S2 C2 S4 118.7(2) . . ?
S3 C3 S5 119.2(2) . . ? 
C2 S4 C4 98.66(15) . . ?
C3 S5 C5 98.06(15) . . ?
C4 C5 S5 123.0(2) . . ?
C5 C4 S4 122.3(2) . . ?
C6 C4 S4 123.6(3) . . ?
C7 C5 S5 123.9(3) . . ?
C6 C4 C5 114.0(3) . . ?
C7 C5 C4 113.1(3) . . ?
C4 C6 S6 109.1(2) . . ?
C5 C7 S6 109.8(3) . . ?
C6 S6 C7 93.93(16) . . ?
C4 C6 C8 129.5(3) . . ?
C5 C7 C9 128.4(3) . . ?
C8 C6 S6 121.4(3) . . ?
C9 C7 S6 121.7(3) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_diffrn_measured_fraction_theta_max    0.877
_diffrn_reflns_theta_full              28.35
_diffrn_measured_fraction_theta_full   0.877
_refine_diff_density_max    0.435
_refine_diff_density_min   -0.409
_refine_diff_density_rms    0.093




#==============================================================================

#     End of CIF

#==============================================================================

