#\#CIF_1.1
 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2010-06-07 at 14:18:31
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.4
#  Request file    : d:\my progs\wingx\files\archive.reqdat
#  CIF files read  : dmcn03 dreduc sadabs sortav struct
 
#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#
 
data_global
 
#------------------ AUDIT DETAILS -------------------------------------------#
 
_audit_creation_date            2010-06-07
_audit_creation_method          'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.4
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record            ?
 
#------------------ AUTHOR DETAILS -------------------------------------------#
 
# Name and address of author for correspondence
 
_publ_contact_author_name            'Farrugia, Louis J.'
# Name of author for correspondence
 
_publ_contact_author_address
;
Department of Chemistry
University of Glasgow
Glasgow
G12 8QQ, UK
;
# Address of author for correspondence
 
_publ_contact_author_email           louis@chem.gla.ac.uk
_publ_contact_author_fax             '44(0141)3304888'
_publ_contact_author_phone           '44(0141)3305137'
 
 
# Insert blank lines between references
 
_publ_section_references
;
Blessing, R. H. (1995) Acta Cryst., A51, 33-38.
 
Blessing, R. H. (1987) Cryst. Rev. 1, 3-58.
 
Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397.
 
APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s).
Bruker AXS Inc., Madison, Wisconsin, USA.
[Older versions (pre-1997) should refer to Siemens Analytical X-ray
Instruments Inc. instead of Bruker AXS.]
 
ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
 
PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
 
SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison,
Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of
Göttingen, Germany.
 
SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
 
SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla,
M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
 
WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 
;
 
#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#
 
data_compound_1a
 
_audit_creation_date                    2010-06-07T14:18:31-00:00
_audit_creation_method                  'WinGX routine CIF_UPDATE'
_audit_conform_dict_name                cif_core.dic
_audit_conform_dict_version             2.4
_audit_conform_dict_location            ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category                FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C30 H22 O8 S4, 2(C4 H8 O2 S)'
_chemical_formula_sum                   'C38 H38 O12 S6'
_chemical_formula_weight                879.04
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'I 2/a'
_symmetry_space_group_name_Hall         '-I 2ya'
_symmetry_Int_Tables_number             15
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
 
_cell_length_a                          18.3523(13)
_cell_length_b                          11.5228(8)
_cell_length_c                          18.6286(14)
_cell_angle_alpha                       90
_cell_angle_beta                        90.916(6)
_cell_angle_gamma                       90
_cell_volume                            3938.9(5)
_cell_formula_units_Z                   4
_cell_measurement_temperature           100(2)
_cell_measurement_reflns_used           9895
_cell_measurement_theta_min             2.2197
_cell_measurement_theta_max             34.8173
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.35
_exptl_crystal_size_mid                 0.2
_exptl_crystal_size_min                 0.2
_exptl_crystal_density_diffrn           1.482
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1832
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.411
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min         0.663
_exptl_absorpt_correction_T_max         0.747
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'sealed x-ray tube'
_diffrn_ambient_temperature             100(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'APEX-II CCD'
_diffrn_orient_matrix_type              'x-axis to radiation source'
_diffrn_orient_matrix_ub_11             -0.468577E-1
_diffrn_orient_matrix_ub_12             -0.248359E-1
_diffrn_orient_matrix_ub_13             -0.676418E-1
_diffrn_orient_matrix_ub_21             0.142704E-1
_diffrn_orient_matrix_ub_22             -0.831481E-1
_diffrn_orient_matrix_ub_23             0.198537E-1
_diffrn_orient_matrix_ub_31             -0.21978E-1
_diffrn_orient_matrix_ub_32             -0.103759E-2
_diffrn_orient_matrix_ub_33             0.280888E-1
_diffrn_measurement_device              'κ-geometry diffractometer'
_diffrn_measurement_device_type         'Bruker APEX-II'
_diffrn_measurement_method              'φ or ω oscillation scans'
_diffrn_reflns_av_R_equivalents         0.035
_diffrn_reflns_av_unetI/netI            0.0338
_diffrn_reflns_number                   60930
_diffrn_reflns_limit_h_min              -29
_diffrn_reflns_limit_h_max              29
_diffrn_reflns_limit_k_min              -18
_diffrn_reflns_limit_k_max              18
_diffrn_reflns_limit_l_min              -19
_diffrn_reflns_limit_l_max              29
_diffrn_reflns_theta_min                2.08
_diffrn_reflns_theta_max                34.89
_diffrn_reflns_theta_full               34.89
_diffrn_measured_fraction_theta_full
                                        0.998
_diffrn_measured_fraction_theta_max
                                        0.998
_reflns_number_total                    8583
_reflns_number_gt                       7301
_reflns_threshold_expression            >2σ(I)
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
 After data reduction, the structure was transformed from the input space 
 group of C2/c (having a beta angle of ~134 deg) to the non-standard I2/a 
 cell with a beta angle closer to 90 deg. This was done to remove many high
 correlations in the refinement.
 The data given for _diffrn_reflns_limit_h_min etc are for the original C2/c
 cell            
;
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Bruker APEX2 software'
_computing_cell_refinement              'SAINT V7.68A integration software'
_computing_data_reduction               'SORTAV (Blessing, 1995)'
_computing_structure_solution           'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
 
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 The high value for the ratio of maximum / minimum residual density is due
 the high quality and the relatively high resolution of the data. These 
 preponderance of peaks as opposed to troughs is because these are bonding 
 density peaks, which are a necessary result of the spherical atom 
 approximation for the atomic scattering factors. The strongest peaks lie
 at the centre of the covalent bonds.
;
_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)+(0.0584P)²+1.8791P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment           constr
_refine_ls_extinction_method            none
_refine_ls_number_reflns                8583
_refine_ls_number_parameters            253
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0443
_refine_ls_R_factor_gt                  0.0366
_refine_ls_wR_factor_ref                0.1056
_refine_ls_wR_factor_gt                 0.1021
_refine_ls_goodness_of_fit_ref          1.071
_refine_ls_restrained_S_all             1.071
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.857
_refine_diff_density_min                -0.284
_refine_diff_density_rms                0.092
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
loop_
    _atom_site_label
    _atom_site_type_symbol
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_occupancy
    _atom_site_symmetry_multiplicity
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_disorder_assembly
    _atom_site_disorder_group
S1 S 0.827494(12) 1.06162(2) 0.446493(12) 0.01374(5) Uani 1 1 d . . .
S2 S 0.835363(12) 0.59967(2) 0.455889(12) 0.01366(5) Uani 1 1 d . . .
O11 O 0.77411(4) 1.14569(7) 0.42371(4) 0.01724(13) Uani 1 1 d . . .
O12 O 0.87834(4) 1.01916(7) 0.39431(4) 0.02018(14) Uani 1 1 d . . .
O21 O 0.90528(4) 0.64676(7) 0.43727(5) 0.02013(14) Uani 1 1 d . . .
O22 O 0.83178(4) 0.51690(7) 0.51362(4) 0.01732(13) Uani 1 1 d . . .
C1 C 0.78137(5) 0.93514(8) 0.47906(5) 0.01269(14) Uani 1 1 d . . .
C2 C 0.81220(5) 0.82967(8) 0.45935(5) 0.01316(14) Uani 1 1 d . . .
H2 H 0.855 0.8297 0.4313 0.016 Uiso 1 1 calc R . .
C3 C 0.78183(5) 0.72414(8) 0.47982(5) 0.01205(14) Uani 1 1 d . . .
C111 C 0.87727(5) 1.11581(8) 0.52059(5) 0.01533(15) Uani 1 1 d . . .
C112 C 0.91865(7) 1.04064(10) 0.56271(7) 0.0269(2) Uani 1 1 d . . .
H112 H 0.9184 0.9596 0.5533 0.032 Uiso 1 1 calc R . .
C113 C 0.96046(7) 1.08587(12) 0.61894(8) 0.0302(3) Uani 1 1 d . . .
H113 H 0.9882 1.0354 0.649 0.036 Uiso 1 1 calc R . .
C114 C 0.96178(6) 1.20441(11) 0.63121(7) 0.0248(2) Uani 1 1 d . . .
H114 H 0.9912 1.2352 0.6691 0.03 Uiso 1 1 calc R . .
C115 C 0.92028(7) 1.27845(10) 0.58823(7) 0.0253(2) Uani 1 1 d . . .
H115 H 0.9216 1.3598 0.5966 0.03 Uiso 1 1 calc R . .
C116 C 0.87682(6) 1.23400(9) 0.53303(6) 0.02059(18) Uani 1 1 d . . .
H116 H 0.8473 1.284 0.5043 0.025 Uiso 1 1 calc R . .
C211 C 0.79646(5) 0.53921(9) 0.37751(5) 0.01578(16) Uani 1 1 d . . .
C212 C 0.76640(6) 0.42858(9) 0.37998(5) 0.01871(17) Uani 1 1 d . . .
H212 H 0.7632 0.3882 0.4243 0.022 Uiso 1 1 calc R . .
C213 C 0.74118(7) 0.37794(10) 0.31667(6) 0.0242(2) Uani 1 1 d . . .
H213 H 0.7209 0.3021 0.3173 0.029 Uiso 1 1 calc R . .
C214 C 0.74565(8) 0.43837(12) 0.25232(6) 0.0284(2) Uani 1 1 d . . .
H214 H 0.728 0.4037 0.2092 0.034 Uiso 1 1 calc R . .
C215 C 0.77573(8) 0.54906(12) 0.25039(6) 0.0301(3) Uani 1 1 d . . .
H215 H 0.7785 0.5895 0.2061 0.036 Uiso 1 1 calc R . .
C216 C 0.80177(7) 0.60062(10) 0.31341(6) 0.0231(2) Uani 1 1 d . . .
H216 H 0.8227 0.676 0.3127 0.028 Uiso 1 1 calc R . .
S3 S -0.079858(14) 0.73835(2) 0.662775(13) 0.01788(6) Uani 1 1 d . . .
O31 O -0.14866(5) 0.76585(9) 0.62825(5) 0.02625(17) Uani 1 1 d . . .
O32 O -0.05688(5) 0.80922(9) 0.72274(5) 0.02820(18) Uani 1 1 d . . .
C31 C -0.00800(7) 0.73429(11) 0.59833(7) 0.0254(2) Uani 1 1 d . . .
H31A H -0.0269 0.7549 0.5499 0.03 Uiso 1 1 calc R . .
H31B H 0.0313 0.7893 0.6119 0.03 Uiso 1 1 calc R . .
C32 C 0.02043(8) 0.60929(12) 0.59943(8) 0.0321(3) Uani 1 1 d . . .
H32A H -0.0041 0.5632 0.5612 0.038 Uiso 1 1 calc R . .
H32B H 0.0735 0.6084 0.5909 0.038 Uiso 1 1 calc R . .
C33 C 0.00441(7) 0.55741(11) 0.67319(7) 0.0283(2) Uani 1 1 d . . .
H33A H 0.0107 0.4721 0.6726 0.034 Uiso 1 1 calc R . .
H33B H 0.0374 0.5906 0.7104 0.034 Uiso 1 1 calc R . .
C34 C -0.07466(7) 0.58941(11) 0.68791(7) 0.0273(2) Uani 1 1 d . . .
H34A H -0.086 0.579 0.7393 0.033 Uiso 1 1 calc R . .
H34B H -0.1087 0.5417 0.6586 0.033 Uiso 1 1 calc R . .
 
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_23
    _atom_site_aniso_U_13
    _atom_site_aniso_U_12
S1 0.01650(10) 0.01061(10) 0.01413(9) 0.00126(7) 0.00045(7) -0.00110(7)
S2 0.01453(10) 0.01041(10) 0.01603(10) -0.00110(7) -0.00024(7) 0.00128(7)
O11 0.0212(3) 0.0135(3) 0.0170(3) 0.0034(2) -0.0028(2) 0.0011(2)
O12 0.0235(3) 0.0172(3) 0.0201(3) 0.0007(3) 0.0076(3) -0.0012(3)
O21 0.0144(3) 0.0165(3) 0.0296(4) -0.0024(3) 0.0028(3) 0.0003(2)
O22 0.0221(3) 0.0130(3) 0.0168(3) 0.0016(2) -0.0031(2) 0.0034(2)
C1 0.0154(3) 0.0101(3) 0.0125(3) 0.0003(3) -0.0007(3) -0.0002(3)
C2 0.0148(3) 0.0104(3) 0.0143(3) -0.0002(3) 0.0001(3) -0.0002(3)
C3 0.0134(3) 0.0101(3) 0.0125(3) -0.0007(3) -0.0012(3) 0.0004(3)
C111 0.0147(3) 0.0123(4) 0.0188(4) 0.0002(3) -0.0021(3) -0.0009(3)
C112 0.0325(6) 0.0151(5) 0.0327(6) -0.0016(4) -0.0152(4) 0.0038(4)
C113 0.0315(6) 0.0234(6) 0.0352(6) -0.0016(4) -0.0172(5) 0.0039(4)
C114 0.0216(5) 0.0238(5) 0.0286(5) -0.0038(4) -0.0070(4) -0.0031(4)
C115 0.0288(5) 0.0164(5) 0.0303(5) -0.0039(4) -0.0071(4) -0.0038(4)
C116 0.0237(4) 0.0129(4) 0.0250(5) -0.0005(3) -0.0053(4) -0.0004(3)
C211 0.0203(4) 0.0129(4) 0.0142(3) -0.0014(3) 0.0015(3) 0.0008(3)
C212 0.0264(5) 0.0131(4) 0.0166(4) -0.0018(3) -0.0010(3) 0.0001(3)
C213 0.0348(6) 0.0183(5) 0.0193(4) -0.0048(3) -0.0028(4) -0.0019(4)
C214 0.0426(7) 0.0265(6) 0.0162(4) -0.0045(4) -0.0028(4) -0.0006(5)
C215 0.0472(7) 0.0291(6) 0.0140(4) 0.0011(4) 0.0013(4) -0.0039(5)
C216 0.0330(5) 0.0199(5) 0.0166(4) 0.0017(3) 0.0029(4) -0.0034(4)
S3 0.01874(11) 0.01682(11) 0.01798(11) -0.00267(8) -0.00290(8) 0.00294(8)
O31 0.0224(4) 0.0303(5) 0.0258(4) -0.0027(3) -0.0077(3) 0.0058(3)
O32 0.0309(4) 0.0274(4) 0.0259(4) -0.0108(3) -0.0095(3) 0.0064(3)
C31 0.0259(5) 0.0212(5) 0.0293(5) 0.0009(4) 0.0052(4) 0.0046(4)
C32 0.0350(6) 0.0266(6) 0.0348(6) 0.0007(5) 0.0056(5) 0.0127(5)
C33 0.0310(6) 0.0213(5) 0.0325(6) 0.0017(4) -0.0043(4) 0.0077(4)
C34 0.0304(6) 0.0205(5) 0.0311(6) 0.0033(4) 0.0014(4) 0.0013(4)
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_distance
    _geom_bond_site_symmetry_2
    _geom_bond_publ_flag
S1 O11 1.4370(8) . ?
S1 O12 1.4436(8) . ?
S1 C111 1.7577(10) . ?
S1 C1 1.7959(9) . ?
S2 O22 1.4397(8) . ?
S2 O21 1.4407(8) . ?
S2 C211 1.7590(10) . ?
S2 C3 1.7986(9) . ?
C1 C2 1.3923(13) . ?
C1 C1 1.4010(18) 2_656 ?
C2 C3 1.3934(13) . ?
C2 H2 0.95 . ?
C3 C3 1.3995(18) 2_656 ?
C111 C116 1.3815(15) . ?
C111 C112 1.3867(15) . ?
C112 C113 1.3900(16) . ?
C112 H112 0.95 . ?
C113 C114 1.3850(18) . ?
C113 H113 0.95 . ?
C114 C115 1.3891(17) . ?
C114 H114 0.95 . ?
C115 C116 1.3892(15) . ?
C115 H115 0.95 . ?
C116 H116 0.95 . ?
C211 C212 1.3900(14) . ?
C211 C216 1.3927(14) . ?
C212 C213 1.3886(15) . ?
C212 H212 0.95 . ?
C213 C214 1.3898(17) . ?
C213 H213 0.95 . ?
C214 C215 1.3906(19) . ?
C214 H214 0.95 . ?
C215 C216 1.3934(17) . ?
C215 H215 0.95 . ?
C216 H216 0.95 . ?
S3 O32 1.4414(9) . ?
S3 O31 1.4431(9) . ?
S3 C34 1.7811(13) . ?
S3 C31 1.7981(12) . ?
C31 C32 1.5320(18) . ?
C31 H31A 0.99 . ?
C31 H31B 0.99 . ?
C32 C33 1.531(2) . ?
C32 H32A 0.99 . ?
C32 H32B 0.99 . ?
C33 C34 1.5263(18) . ?
C33 H33A 0.99 . ?
C33 H33B 0.99 . ?
C34 H34A 0.99 . ?
C34 H34B 0.99 . ?
 
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
O11 S1 O12 118.33(5) . . ?
O11 S1 C111 109.62(5) . . ?
O12 S1 C111 108.41(5) . . ?
O11 S1 C1 108.90(4) . . ?
O12 S1 C1 105.41(5) . . ?
C111 S1 C1 105.36(4) . . ?
O22 S2 O21 118.74(5) . . ?
O22 S2 C211 109.56(5) . . ?
O21 S2 C211 107.50(5) . . ?
O22 S2 C3 108.15(4) . . ?
O21 S2 C3 104.57(4) . . ?
C211 S2 C3 107.79(4) . . ?
C2 C1 C1 119.21(5) . 2_656 ?
C2 C1 S1 115.05(7) . . ?
C1 C1 S1 125.74(3) 2_656 . ?
C1 C2 C3 121.57(8) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C2 C3 C3 119.22(5) . 2_656 ?
C2 C3 S2 113.93(7) . . ?
C3 C3 S2 126.67(3) 2_656 . ?
C116 C111 C112 121.70(9) . . ?
C116 C111 S1 118.52(8) . . ?
C112 C111 S1 119.70(8) . . ?
C111 C112 C113 118.88(11) . . ?
C111 C112 H112 120.6 . . ?
C113 C112 H112 120.6 . . ?
C114 C113 C112 120.14(11) . . ?
C114 C113 H113 119.9 . . ?
C112 C113 H113 119.9 . . ?
C113 C114 C115 120.18(10) . . ?
C113 C114 H114 119.9 . . ?
C115 C114 H114 119.9 . . ?
C114 C115 C116 120.21(11) . . ?
C114 C115 H115 119.9 . . ?
C116 C115 H115 119.9 . . ?
C111 C116 C115 118.86(10) . . ?
C111 C116 H116 120.6 . . ?
C115 C116 H116 120.6 . . ?
C212 C211 C216 121.85(9) . . ?
C212 C211 S2 119.45(7) . . ?
C216 C211 S2 118.52(8) . . ?
C213 C212 C211 118.96(10) . . ?
C213 C212 H212 120.5 . . ?
C211 C212 H212 120.5 . . ?
C212 C213 C214 119.90(11) . . ?
C212 C213 H213 120 . . ?
C214 C213 H213 120 . . ?
C213 C214 C215 120.72(11) . . ?
C213 C214 H214 119.6 . . ?
C215 C214 H214 119.6 . . ?
C214 C215 C216 120.01(11) . . ?
C214 C215 H215 120 . . ?
C216 C215 H215 120 . . ?
C211 C216 C215 118.55(11) . . ?
C211 C216 H216 120.7 . . ?
C215 C216 H216 120.7 . . ?
O32 S3 O31 117.65(5) . . ?
O32 S3 C34 109.17(6) . . ?
O31 S3 C34 111.81(6) . . ?
O32 S3 C31 108.88(6) . . ?
O31 S3 C31 110.73(6) . . ?
C34 S3 C31 96.53(6) . . ?
C32 C31 S3 105.59(9) . . ?
C32 C31 H31A 110.6 . . ?
S3 C31 H31A 110.6 . . ?
C32 C31 H31B 110.6 . . ?
S3 C31 H31B 110.6 . . ?
H31A C31 H31B 108.8 . . ?
C33 C32 C31 107.99(10) . . ?
C33 C32 H32A 110.1 . . ?
C31 C32 H32A 110.1 . . ?
C33 C32 H32B 110.1 . . ?
C31 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
C34 C33 C32 105.29(10) . . ?
C34 C33 H33A 110.7 . . ?
C32 C33 H33A 110.7 . . ?
C34 C33 H33B 110.7 . . ?
C32 C33 H33B 110.7 . . ?
H33A C33 H33B 108.8 . . ?
C33 C34 S3 103.45(9) . . ?
C33 C34 H34A 111.1 . . ?
S3 C34 H34A 111.1 . . ?
C33 C34 H34B 111.1 . . ?
S3 C34 H34B 111.1 . . ?
H34A C34 H34B 109 . . ?
 
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
O11 S1 C1 C2 139.46(7) . . . . ?
O12 S1 C1 C2 11.53(8) . . . . ?
C111 S1 C1 C2 -103.01(7) . . . . ?
O11 S1 C1 C1 -40.11(12) . . . 2_656 ?
O12 S1 C1 C1 -168.04(11) . . . 2_656 ?
C111 S1 C1 C1 77.42(12) . . . 2_656 ?
C1 C1 C2 C3 0.50(16) 2_656 . . . ?
S1 C1 C2 C3 -179.10(7) . . . . ?
C1 C2 C3 C3 1.03(15) . . . 2_656 ?
C1 C2 C3 S2 -174.31(7) . . . . ?
O22 S2 C3 C2 141.47(7) . . . . ?
O21 S2 C3 C2 14.03(8) . . . . ?
C211 S2 C3 C2 -100.16(7) . . . . ?
O22 S2 C3 C3 -33.46(12) . . . 2_656 ?
O21 S2 C3 C3 -160.90(11) . . . 2_656 ?
C211 S2 C3 C3 84.92(11) . . . 2_656 ?
O11 S1 C111 C116 -19.28(10) . . . . ?
O12 S1 C111 C116 111.24(9) . . . . ?
C1 S1 C111 C116 -136.32(9) . . . . ?
O11 S1 C111 C112 163.93(9) . . . . ?
O12 S1 C111 C112 -65.55(10) . . . . ?
C1 S1 C111 C112 46.89(10) . . . . ?
C116 C111 C112 C113 0.19(19) . . . . ?
S1 C111 C112 C113 176.88(11) . . . . ?
C111 C112 C113 C114 -1.5(2) . . . . ?
C112 C113 C114 C115 1.2(2) . . . . ?
C113 C114 C115 C116 0.5(2) . . . . ?
C112 C111 C116 C115 1.45(17) . . . . ?
S1 C111 C116 C115 -175.28(9) . . . . ?
C114 C115 C116 C111 -1.76(18) . . . . ?
O22 S2 C211 C212 2.17(10) . . . . ?
O21 S2 C211 C212 132.49(8) . . . . ?
C3 S2 C211 C212 -115.30(8) . . . . ?
O22 S2 C211 C216 -173.00(8) . . . . ?
O21 S2 C211 C216 -42.68(10) . . . . ?
C3 S2 C211 C216 69.54(9) . . . . ?
C216 C211 C212 C213 0.16(16) . . . . ?
S2 C211 C212 C213 -174.84(9) . . . . ?
C211 C212 C213 C214 -0.58(18) . . . . ?
C212 C213 C214 C215 0.5(2) . . . . ?
C213 C214 C215 C216 0.0(2) . . . . ?
C212 C211 C216 C215 0.31(17) . . . . ?
S2 C211 C216 C215 175.36(10) . . . . ?
C214 C215 C216 C211 -0.4(2) . . . . ?
O32 S3 C31 C32 111.90(9) . . . . ?
O31 S3 C31 C32 -117.27(9) . . . . ?
C34 S3 C31 C32 -0.96(10) . . . . ?
S3 C31 C32 C33 -25.71(13) . . . . ?
C31 C32 C33 C34 46.56(14) . . . . ?
C32 C33 C34 S3 -45.01(12) . . . . ?
O32 S3 C34 C33 -85.79(9) . . . . ?
O31 S3 C34 C33 142.27(8) . . . . ?
C31 S3 C34 C33 26.83(10) . . . . ?

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#


data_compound_1b
 
_audit_creation_date                    2012-06-29T11:11:40-00:00
_audit_creation_method                  'WinGX routine CIF_UPDATE'
_audit_conform_dict_name                cif_core.dic
_audit_conform_dict_version             2.4.2
_audit_conform_dict_location            ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category                FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C30 H22 O8 S4, 2(C7 H12 O)'
_chemical_formula_sum                   'C44 H46 O10 S4'
_chemical_formula_weight                863.05
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'I 2/c'
_symmetry_space_group_name_Hall         '-I 2yc'
_symmetry_Int_Tables_number             15
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z'
 
_cell_length_a                          19.1198(6)
_cell_length_b                          11.6030(4)
_cell_length_c                          19.1943(5)
_cell_angle_alpha                       90
_cell_angle_beta                        102.023(2)
_cell_angle_gamma                       90
_cell_volume                            4164.8(2)
_cell_formula_units_Z                   4
_cell_measurement_temperature           100(2)
_cell_measurement_reflns_used           9884
_cell_measurement_theta_min             2.1697
_cell_measurement_theta_max             31.2255
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              plate
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.2
_exptl_crystal_size_mid                 0.2
_exptl_crystal_size_min                 0.05
_exptl_crystal_density_diffrn           1.376
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1816
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.287
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min         0.682
_exptl_absorpt_correction_T_max         0.746
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'sealed x-ray tube'
_diffrn_ambient_temperature             100(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'APEX-II CCD'
_diffrn_orient_matrix_type              'x-axis to radiation source'
_diffrn_measurement_device              'κ-geometry diffractometer'
_diffrn_measurement_device_type         'Bruker APEX-II'
_diffrn_measurement_method              'φ or ω oscillation scans'
_diffrn_reflns_av_R_equivalents         0.0824
_diffrn_reflns_av_unetI/netI            0.057
_diffrn_reflns_number                   71078
_diffrn_reflns_limit_h_min              -28
_diffrn_reflns_limit_h_max              28
_diffrn_reflns_limit_k_min              -12
_diffrn_reflns_limit_k_max              17
_diffrn_reflns_limit_l_min              -28
_diffrn_reflns_limit_l_max              28
_diffrn_reflns_theta_min                2.06
_diffrn_reflns_theta_max                31.96
_diffrn_reflns_theta_full               31.96
_diffrn_measured_fraction_theta_full
                                        0.998
_diffrn_measured_fraction_theta_max
                                        0.998
_reflns_number_total                    7196
_reflns_number_gt                       5660
_reflns_threshold_expression            >2σ(I)
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397

 Data were transformed from standard C2/c setting to I2/c as the beta angle
 in the standard setting was close to 130 deg. Many high correlations were
 observed in refinement with C2/c, which were absent in I2/c.
;
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Bruker APEX2 software'
_computing_cell_refinement              'SAINT V7.68A integration software'
_computing_data_reduction               'SORTAV (Blessing, 1995)'
_computing_structure_solution           'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
 
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0512P)²+1.1685P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment           constr
_refine_ls_extinction_method            none
_refine_ls_number_reflns                7196
_refine_ls_number_parameters            262
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.057
_refine_ls_R_factor_gt                  0.0396
_refine_ls_wR_factor_ref                0.1039
_refine_ls_wR_factor_gt                 0.0975
_refine_ls_goodness_of_fit_ref          1.027
_refine_ls_restrained_S_all             1.027
_refine_ls_shift/su_max                 0.002
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.592
_refine_diff_density_min                -0.41
_refine_diff_density_rms                0.074
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
loop_
    _atom_site_label
    _atom_site_type_symbol
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_occupancy
    _atom_site_symmetry_multiplicity
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_disorder_assembly
    _atom_site_disorder_group
S1 S 0.554879(16) 0.58027(2) 0.837922(15) 0.01302(7) Uani 1 1 d . . .
S2 S 0.561464(15) 1.03964(2) 0.831932(14) 0.01201(7) Uani 1 1 d . . .
O11 O 0.50130(5) 0.49156(7) 0.82528(5) 0.01732(18) Uani 1 1 d . . .
O12 O 0.57771(5) 0.62527(8) 0.90901(5) 0.01964(19) Uani 1 1 d . . .
O21 O 0.61568(5) 0.99552(8) 0.88956(5) 0.01756(18) Uani 1 1 d . . .
O22 O 0.58235(5) 1.11851(7) 0.78204(5) 0.01626(17) Uani 1 1 d . . .
C1 C 0.52255(6) 0.70410(9) 0.78381(6) 0.0121(2) Uani 1 1 d . . .
C2 C 0.54481(6) 0.80925(9) 0.81649(6) 0.0127(2) Uani 1 1 d . . .
H2 H 0.5756 0.8093 0.8623 0.015 Uiso 1 1 calc R . .
C3 C 0.52294(6) 0.91400(9) 0.78355(6) 0.0117(2) Uani 1 1 d . . .
C111 C 0.63179(7) 0.53235(10) 0.80921(6) 0.0149(2) Uani 1 1 d . . .
C112 C 0.69274(7) 0.60184(12) 0.82131(7) 0.0215(3) Uani 1 1 d . . .
H112 H 0.6918 0.6764 0.8416 0.026 Uiso 1 1 calc R . .
C113 C 0.75485(8) 0.56044(13) 0.80333(8) 0.0262(3) Uani 1 1 d . . .
H113 H 0.7966 0.607 0.8109 0.031 Uiso 1 1 calc R . .
C114 C 0.75582(7) 0.45056(13) 0.77421(8) 0.0244(3) Uani 1 1 d . . .
H114 H 0.7985 0.4221 0.7624 0.029 Uiso 1 1 calc R . .
C115 C 0.69467(7) 0.38247(12) 0.76230(7) 0.0224(3) Uani 1 1 d . . .
H115 H 0.6957 0.3078 0.7423 0.027 Uiso 1 1 calc R . .
C116 C 0.63192(7) 0.42296(11) 0.77951(7) 0.0175(2) Uani 1 1 d . . .
H116 H 0.59 0.3768 0.7711 0.021 Uiso 1 1 calc R . .
C211 C 0.49413(6) 1.10244(10) 0.86956(6) 0.0128(2) Uani 1 1 d . . .
C212 C 0.48449(7) 1.22093(11) 0.86334(7) 0.0183(2) Uani 1 1 d . . .
H212 H 0.5089 1.2648 0.8341 0.022 Uiso 1 1 calc R . .
C213 C 0.43854(8) 1.27400(11) 0.90070(8) 0.0224(3) Uani 1 1 d . . .
H213 H 0.4319 1.3551 0.8977 0.027 Uiso 1 1 calc R . .
C214 C 0.40217(8) 1.20862(12) 0.94245(7) 0.0218(3) Uani 1 1 d . . .
H214 H 0.3713 1.2455 0.9684 0.026 Uiso 1 1 calc R . .
C215 C 0.41067(8) 1.08950(11) 0.94649(7) 0.0217(3) Uani 1 1 d . . .
H215 H 0.3846 1.0451 0.974 0.026 Uiso 1 1 calc R . .
C216 C 0.45738(7) 1.03542(11) 0.91020(7) 0.0181(2) Uani 1 1 d . . .
H216 H 0.464 0.9543 0.9131 0.022 Uiso 1 1 calc R . .
O31 O 0.89480(7) 0.74526(9) 0.86313(6) 0.0312(2) Uani 1 1 d . . .
C31 C 0.87899(7) 0.79740(11) 0.91286(7) 0.0202(2) Uani 1 1 d . . .
C32 C 0.86748(10) 0.73021(12) 0.97728(8) 0.0281(3) Uani 1 1 d . . .
H32A H 0.9118 0.6863 0.996 0.034 Uiso 1 1 calc R . .
H32B H 0.8292 0.6731 0.9605 0.034 Uiso 1 1 calc R . .
C33 C 0.84794(9) 0.79587(13) 1.03945(8) 0.0283(3) Uani 1 1 d . . .
H33A H 0.8858 0.8534 1.0567 0.034 Uiso 1 1 calc R . .
H33B H 0.8475 0.7409 1.0788 0.034 Uiso 1 1 calc R . .
C34 C 0.77557(8) 0.85830(15) 1.02233(8) 0.0292(3) Uani 1 1 d . . .
H34A H 0.7404 0.8079 0.9915 0.035 Uiso 1 1 calc R . .
H34B H 0.7589 0.8703 1.0673 0.035 Uiso 1 1 calc R . .
C35 C 0.77689(7) 0.97415(13) 0.98551(7) 0.0234(3) Uani 1 1 d . . .
H35A H 0.8125 1.0242 1.0162 0.028 Uiso 1 1 calc R . .
H35B H 0.7295 1.011 0.9811 0.028 Uiso 1 1 calc R . .
C36 C 0.79483(8) 0.96840(13) 0.91188(8) 0.0250(3) Uani 1 1 d . . .
H36A H 0.7882 1.0461 0.8902 0.03 Uiso 1 1 calc R . .
H36B H 0.7602 0.9162 0.8817 0.03 Uiso 1 1 calc R . .
C37 C 0.87075(8) 0.92684(12) 0.91053(8) 0.0248(3) Uani 1 1 d . . .
H37A H 0.8843 0.9561 0.8667 0.03 Uiso 1 1 calc R . .
H37B H 0.9044 0.9605 0.9518 0.03 Uiso 1 1 calc R . .
 
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_23
    _atom_site_aniso_U_13
    _atom_site_aniso_U_12
S1 0.01572(14) 0.01010(13) 0.01382(13) 0.00165(9) 0.00441(10) 0.00226(9)
S2 0.01255(13) 0.01032(13) 0.01327(12) -0.00167(9) 0.00295(9) -0.00091(9)
O11 0.0176(4) 0.0128(4) 0.0235(4) 0.0035(3) 0.0087(3) -0.0001(3)
O12 0.0287(5) 0.0166(4) 0.0129(4) 0.0009(3) 0.0026(3) 0.0058(4)
O21 0.0161(4) 0.0172(4) 0.0173(4) -0.0026(3) -0.0015(3) 0.0004(3)
O22 0.0178(4) 0.0143(4) 0.0183(4) -0.0006(3) 0.0074(3) -0.0029(3)
C1 0.0126(5) 0.0100(5) 0.0142(5) 0.0004(4) 0.0044(4) 0.0013(4)
C2 0.0129(5) 0.0121(5) 0.0130(5) -0.0002(4) 0.0024(4) 0.0014(4)
C3 0.0123(5) 0.0099(5) 0.0130(5) -0.0011(4) 0.0032(4) -0.0001(4)
C111 0.0142(5) 0.0145(5) 0.0163(5) 0.0017(4) 0.0037(4) 0.0027(4)
C112 0.0192(6) 0.0179(6) 0.0275(6) -0.0020(5) 0.0052(5) -0.0009(5)
C113 0.0166(6) 0.0297(7) 0.0328(7) 0.0000(6) 0.0066(5) -0.0028(5)
C114 0.0169(6) 0.0306(7) 0.0271(6) 0.0011(5) 0.0077(5) 0.0062(5)
C115 0.0206(6) 0.0208(6) 0.0264(6) -0.0021(5) 0.0065(5) 0.0069(5)
C116 0.0168(6) 0.0153(5) 0.0208(6) 0.0004(4) 0.0048(4) 0.0019(4)
C211 0.0150(5) 0.0114(5) 0.0125(5) -0.0015(4) 0.0037(4) -0.0002(4)
C212 0.0228(6) 0.0124(5) 0.0222(6) 0.0003(4) 0.0105(5) 0.0003(4)
C213 0.0278(7) 0.0125(5) 0.0298(7) -0.0020(5) 0.0130(6) 0.0026(5)
C214 0.0236(6) 0.0205(6) 0.0242(6) -0.0045(5) 0.0117(5) 0.0013(5)
C215 0.0254(7) 0.0197(6) 0.0236(6) 0.0019(5) 0.0134(5) -0.0004(5)
C216 0.0225(6) 0.0126(5) 0.0216(6) 0.0020(4) 0.0099(5) -0.0004(4)
O31 0.0393(6) 0.0256(5) 0.0344(6) -0.0060(4) 0.0211(5) -0.0024(5)
C31 0.0177(6) 0.0182(6) 0.0264(6) -0.0020(5) 0.0083(5) -0.0018(5)
C32 0.0436(9) 0.0183(6) 0.0240(7) 0.0011(5) 0.0108(6) 0.0033(6)
C33 0.0368(8) 0.0280(7) 0.0207(6) 0.0030(5) 0.0077(6) 0.0056(6)
C34 0.0268(7) 0.0395(9) 0.0234(6) 0.0003(6) 0.0101(6) -0.0020(6)
C35 0.0185(6) 0.0310(7) 0.0196(6) -0.0052(5) 0.0017(5) 0.0058(5)
C36 0.0277(7) 0.0255(7) 0.0228(6) 0.0025(5) 0.0071(5) 0.0067(5)
C37 0.0279(7) 0.0167(6) 0.0343(7) 0.0019(5) 0.0170(6) -0.0013(5)
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_distance
    _geom_bond_site_symmetry_2
    _geom_bond_publ_flag
S1 O11 1.4368(9) . ?
S1 O12 1.4411(9) . ?
S1 C111 1.7644(12) . ?
S1 C1 1.8050(11) . ?
S2 O22 1.4399(9) . ?
S2 O21 1.4431(9) . ?
S2 C211 1.7599(12) . ?
S2 C3 1.8015(11) . ?
C1 C2 1.3972(16) . ?
C1 C1 1.401(2) 2_656 ?
C2 C3 1.3935(15) . ?
C2 H2 0.95 . ?
C3 C3 1.399(2) 2_656 ?
C111 C116 1.3916(17) . ?
C111 C112 1.3961(18) . ?
C112 C113 1.3896(19) . ?
C112 H112 0.95 . ?
C113 C114 1.394(2) . ?
C113 H113 0.95 . ?
C114 C115 1.390(2) . ?
C114 H114 0.95 . ?
C115 C116 1.3907(18) . ?
C115 H115 0.95 . ?
C116 H116 0.95 . ?
C211 C212 1.3890(16) . ?
C211 C216 1.3911(16) . ?
C212 C213 1.3884(17) . ?
C212 H212 0.95 . ?
C213 C214 1.3905(19) . ?
C213 H213 0.95 . ?
C214 C215 1.3919(19) . ?
C214 H214 0.95 . ?
C215 C216 1.3913(17) . ?
C215 H215 0.95 . ?
C216 H216 0.95 . ?
O31 C31 1.2201(16) . ?
C31 C37 1.5099(19) . ?
C31 C32 1.5161(19) . ?
C32 C33 1.526(2) . ?
C32 H32A 0.99 . ?
C32 H32B 0.99 . ?
C33 C34 1.535(2) . ?
C33 H33A 0.99 . ?
C33 H33B 0.99 . ?
C34 C35 1.521(2) . ?
C34 H34A 0.99 . ?
C34 H34B 0.99 . ?
C35 C36 1.5237(19) . ?
C35 H35A 0.99 . ?
C35 H35B 0.99 . ?
C36 C37 1.535(2) . ?
C36 H36A 0.99 . ?
C36 H36B 0.99 . ?
C37 H37A 0.99 . ?
C37 H37B 0.99 . ?
 
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
O11 S1 O12 118.96(6) . . ?
O11 S1 C111 109.44(6) . . ?
O12 S1 C111 107.58(6) . . ?
O11 S1 C1 109.05(5) . . ?
O12 S1 C1 104.86(5) . . ?
C111 S1 C1 106.19(5) . . ?
O22 S2 O21 118.74(6) . . ?
O22 S2 C211 109.74(5) . . ?
O21 S2 C211 107.59(5) . . ?
O22 S2 C3 108.17(5) . . ?
O21 S2 C3 105.03(5) . . ?
C211 S2 C3 106.92(5) . . ?
C2 C1 C1 119.16(7) . 2_656 ?
C2 C1 S1 113.63(8) . . ?
C1 C1 S1 127.17(4) 2_656 . ?
C3 C2 C1 121.55(11) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C3 119.28(7) . 2_656 ?
C2 C3 S2 114.84(9) . . ?
C3 C3 S2 125.82(4) 2_656 . ?
C116 C111 C112 121.48(11) . . ?
C116 C111 S1 119.22(9) . . ?
C112 C111 S1 119.15(9) . . ?
C113 C112 C111 119.07(12) . . ?
C113 C112 H112 120.5 . . ?
C111 C112 H112 120.5 . . ?
C112 C113 C114 119.95(13) . . ?
C112 C113 H113 120 . . ?
C114 C113 H113 120 . . ?
C115 C114 C113 120.33(12) . . ?
C115 C114 H114 119.8 . . ?
C113 C114 H114 119.8 . . ?
C114 C115 C116 120.44(13) . . ?
C114 C115 H115 119.8 . . ?
C116 C115 H115 119.8 . . ?
C115 C116 C111 118.73(12) . . ?
C115 C116 H116 120.6 . . ?
C111 C116 H116 120.6 . . ?
C212 C211 C216 121.87(11) . . ?
C212 C211 S2 118.02(9) . . ?
C216 C211 S2 119.79(9) . . ?
C213 C212 C211 118.78(11) . . ?
C213 C212 H212 120.6 . . ?
C211 C212 H212 120.6 . . ?
C212 C213 C214 120.13(12) . . ?
C212 C213 H213 119.9 . . ?
C214 C213 H213 119.9 . . ?
C213 C214 C215 120.48(12) . . ?
C213 C214 H214 119.8 . . ?
C215 C214 H214 119.8 . . ?
C216 C215 C214 119.98(12) . . ?
C216 C215 H215 120 . . ?
C214 C215 H215 120 . . ?
C211 C216 C215 118.71(11) . . ?
C211 C216 H216 120.6 . . ?
C215 C216 H216 120.6 . . ?
O31 C31 C37 120.76(13) . . ?
O31 C31 C32 119.00(12) . . ?
C37 C31 C32 120.25(12) . . ?
C31 C32 C33 118.80(12) . . ?
C31 C32 H32A 107.6 . . ?
C33 C32 H32A 107.6 . . ?
C31 C32 H32B 107.6 . . ?
C33 C32 H32B 107.6 . . ?
H32A C32 H32B 107 . . ?
C32 C33 C34 115.12(13) . . ?
C32 C33 H33A 108.5 . . ?
C34 C33 H33A 108.5 . . ?
C32 C33 H33B 108.5 . . ?
C34 C33 H33B 108.5 . . ?
H33A C33 H33B 107.5 . . ?
C35 C34 C33 114.51(12) . . ?
C35 C34 H34A 108.6 . . ?
C33 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
C33 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C34 C35 C36 114.89(12) . . ?
C34 C35 H35A 108.5 . . ?
C36 C35 H35A 108.5 . . ?
C34 C35 H35B 108.5 . . ?
C36 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
C35 C36 C37 115.21(12) . . ?
C35 C36 H36A 108.5 . . ?
C37 C36 H36A 108.5 . . ?
C35 C36 H36B 108.5 . . ?
C37 C36 H36B 108.5 . . ?
H36A C36 H36B 107.5 . . ?
C31 C37 C36 113.91(12) . . ?
C31 C37 H37A 108.8 . . ?
C36 C37 H37A 108.8 . . ?
C31 C37 H37B 108.8 . . ?
C36 C37 H37B 108.8 . . ?
H37A C37 H37B 107.7 . . ?
 
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
O11 S1 C1 C2 145.12(9) . . . . ?
O12 S1 C1 C2 16.69(10) . . . . ?
C111 S1 C1 C2 -97.04(9) . . . . ?
O11 S1 C1 C1 -32.76(15) . . . 2_656 ?
O12 S1 C1 C1 -161.19(14) . . . 2_656 ?
C111 S1 C1 C1 85.08(15) . . . 2_656 ?
C1 C1 C2 C3 0.3(2) 2_656 . . . ?
S1 C1 C2 C3 -177.77(9) . . . . ?
C1 C2 C3 C3 0.6(2) . . . 2_656 ?
C1 C2 C3 S2 -176.57(9) . . . . ?
O22 S2 C3 C2 136.61(9) . . . . ?
O21 S2 C3 C2 8.87(10) . . . . ?
C211 S2 C3 C2 -105.27(9) . . . . ?
O22 S2 C3 C3 -40.37(15) . . . 2_656 ?
O21 S2 C3 C3 -168.11(13) . . . 2_656 ?
C211 S2 C3 C3 77.75(14) . . . 2_656 ?
O11 S1 C111 C116 0.33(12) . . . . ?
O12 S1 C111 C116 130.90(10) . . . . ?
C1 S1 C111 C116 -117.25(10) . . . . ?
O11 S1 C111 C112 -175.28(10) . . . . ?
O12 S1 C111 C112 -44.71(12) . . . . ?
C1 S1 C111 C112 67.14(11) . . . . ?
C116 C111 C112 C113 -0.1(2) . . . . ?
S1 C111 C112 C113 175.41(11) . . . . ?
C111 C112 C113 C114 -0.5(2) . . . . ?
C112 C113 C114 C115 0.7(2) . . . . ?
C113 C114 C115 C116 -0.2(2) . . . . ?
C114 C115 C116 C111 -0.4(2) . . . . ?
C112 C111 C116 C115 0.58(19) . . . . ?
S1 C111 C116 C115 -174.93(10) . . . . ?
O22 S2 C211 C212 -16.97(12) . . . . ?
O21 S2 C211 C212 113.55(10) . . . . ?
C3 S2 C211 C212 -134.05(10) . . . . ?
O22 S2 C211 C216 169.37(10) . . . . ?
O21 S2 C211 C216 -60.11(11) . . . . ?
C3 S2 C211 C216 52.28(11) . . . . ?
C216 C211 C212 C213 2.1(2) . . . . ?
S2 C211 C212 C213 -171.42(11) . . . . ?
C211 C212 C213 C214 -1.1(2) . . . . ?
C212 C213 C214 C215 -0.9(2) . . . . ?
C213 C214 C215 C216 1.8(2) . . . . ?
C212 C211 C216 C215 -1.1(2) . . . . ?
S2 C211 C216 C215 172.28(10) . . . . ?
C214 C215 C216 C211 -0.8(2) . . . . ?
O31 C31 C32 C33 179.80(15) . . . . ?
C37 C31 C32 C33 -0.3(2) . . . . ?
C31 C32 C33 C34 64.3(2) . . . . ?
C32 C33 C34 C35 -81.01(17) . . . . ?
C33 C34 C35 C36 63.85(17) . . . . ?
C34 C35 C36 C37 -65.39(17) . . . . ?
O31 C31 C37 C36 116.55(15) . . . . ?
C32 C31 C37 C36 -63.30(19) . . . . ?
C35 C36 C37 C31 82.06(17) . . . . ?
 
# END of CIF

#==============================================================================
# PLATON/CHECK-(280612) versus check.def version of 280612  for entry: compound
# Data From: archive.cif - Data Type: CIF       Bond Precision   C-C = 0.0016 A
#                                                                  Temp = 100 K
#
# UCL 18.3523(13)  11.5228(8) 18.6286(14)           90    90.916(6)          90
# WaveLength 0.71073    Volume Reported     3938.9(5)  Calculated     3938.9(5)
# SpaceGroup from Symmetry I 2/a         Hall: -I 2ya
#                 Reported I 2/a               -I 2ya
# MoietyFormula C30 H22 O8 S4, 2(C4 H8 O2 S)
#      Reported C30 H22 O8 S4, 2(C4 H8 O2 S)
#    SumFormula C38 H38 O12 S6
#      Reported C38 H38 O12 S6
# Mr        =    879.10[Calc],    879.04[Rep]
# Dx,gcm-3  =     1.482[Calc],     1.482[Rep]
# Z         =         4[Calc],         4[Rep]
# Mu (mm-1) =     0.411[Calc],     0.411[Rep]
# F000      =    1832.0[Calc],    1832.0[Rep]  or F000' =   1835.84[Calc]
# Reported   T Limits: Tmin=0.663              Tmax=0.747  AbsCorr=MULTI-SCAN
# Calculated T Limits: Tmin=0.906 Tmin'=0.866  Tmax=0.921
# Reported   Hmax= 29, Kmax= 18, Lmax= 29, Nref=  8583        , Th(max)= 34.890
# Calculated Hmax= 29, Kmax= 18, Lmax= 29, Nref=  8598        , Ratio  =  0.998
# Reported   Rho(min) = -0.28, Rho(max) =  0.86 e/Ang**3 (From CIF)
# w=1/[sigma**2(Fo**2)+(0.0584P)**2+  1.8791P], P=(Fo**2+2*Fc**2)/3
# R= 0.0366(  7301), wR2= 0.1056(  8583), S = 1.071, Npar= 253
#==============================================================================
For Documentation: http://www.platonsoft.nl/CIF-VALIDATION.pdf
#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.02
#==============================================================================
005_ALERT_5_G No _iucr_refine_instructions_details in CIF ....          ?
128_ALERT_4_G Alternate Setting of Space-group C2/c    .......      I2/a
#==============================================================================
 
               ALERT_Level and ALERT_Type Summary
               ==================================
  1 ALERT_Level_C = Check. Ensure it is Not caused by an Omission or Oversight
  2 ALERT_Level_G = General Info/Check that it is not Something Unexpected
 
  1 ALERT_Type_2 Indicator that the Structure Model may be Wrong or Deficient.
  1 ALERT_Type_4 Improvement, Methodology, Query or Suggestion.
  1 ALERT_Type_5 Informative Message, Check.
#==============================================================================
#==============================================================================
# PLATON/CHECK-(280612) versus check.def version of 280612  for entry: compound
# Data From: archive.cif - Data Type: CIF       Bond Precision   C-C = 0.0019 A
#                                                                  Temp = 100 K
#
# UCL  19.1198(6)  11.6030(4)  19.1943(5)           90   102.023(2)          90
# WaveLength 0.71073    Volume Reported     4164.8(2)  Calculated     4164.8(2)
# SpaceGroup from Symmetry I 2/c         Hall: -I 2yc
#                 Reported I 2/c               -I 2yc
# MoietyFormula C30 H22 O8 S4, 2(C7 H12 O)
#      Reported C30 H22 O8 S4, 2(C7 H12 O)
#    SumFormula C44 H46 O10 S4
#      Reported C44 H46 O10 S4
# Mr        =    863.09[Calc],    863.05[Rep]
# Dx,gcm-3  =     1.377[Calc],     1.376[Rep]
# Z         =         4[Calc],         4[Rep]
# Mu (mm-1) =     0.287[Calc],     0.287[Rep]
# F000      =    1816.0[Calc],    1816.0[Rep]  or F000' =   1818.82[Calc]
# Reported   T Limits: Tmin=0.682              Tmax=0.746  AbsCorr=MULTI-SCAN
# Calculated T Limits: Tmin=0.944 Tmin'=0.944  Tmax=0.986
# Reported   Hmax= 28, Kmax= 17, Lmax= 28, Nref=  7196        , Th(max)= 31.960
# Calculated Hmax= 28, Kmax= 17, Lmax= 28, Nref=  7214        , Ratio  =  0.998
# Reported   Rho(min) = -0.41, Rho(max) =  0.59 e/Ang**3 (From CIF)
# w=1/[sigma**2(Fo**2)+(0.0512P)**2+  1.1685P], P=(Fo**2+2*Fc**2)/3
# R= 0.0396(  5660), wR2= 0.1039(  7196), S = 1.027, Npar= 262
#==============================================================================
For Documentation: http://www.platonsoft.nl/CIF-VALIDATION.pdf
#==============================================================================
>>> The Following Model ALERTS were generated                 - (Acta-Mode) <<<
#==============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
005_ALERT_5_G No _iucr_refine_instructions_details in CIF ....          ?
128_ALERT_4_G Alternate Setting of Space-group C2/c    .......      I2/c
#==============================================================================
 
#==============================================================================
!! Congratulations !! : No (A,B,C) ALERT Conditions were Detected
#==============================================================================
 
Explanation and Advice for the Reported ALERTS
===============================================================================
 
===============================================================================
ALERT_005 Type_5 Informative Message, Check.
===============================================================================
 
 No 'refinement details' record was found. Acta Cryst. requires the
 inclusion of the last shelxl.res file (in case of a SHELXL or XL refinement)
 in the CIF embedded between records with semicolons in position 1, preceded
 by an '_iucr_refine_instructions_details' record.
 
===============================================================================
ALERT_094 Type_2 Indicator that the Structure Model may be Wrong or Deficient.
===============================================================================
 
 The ratio of the maximum and minimum residual density excursions is
 unusual. This might indicate unaccounted for twinning or missing atoms
 (e.g. associated with disordered solvent).
 
===============================================================================
ALERT_128 Type_4 Improvement, Methodology, Query or Suggestion.
===============================================================================
 
 The reported monoclinic space-group is in a non-standard setting.
 Transformation to the conventional setting is indicated unless there
 is a good (scientific) reason not to do so.
 

