data_vg_401_0m
_audit_creation_date               2019-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      'Department of Chemistry, university of Delhi, Delhi 110007'
_audit_contact_author_email        ashokenzyme@gmail.com
_audit_contact_author_name         'Ashok K. Prasad'
_audit_contact_author_phone        00-91-11-27662486
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H.
 (2015). Acta Cryst. A71, 59-75.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C33 H32 O9 S2'
_chemical_formula_sum              'C33 H32 O9 S2'
_chemical_formula_weight           636.70
_chemical_absolute_configuration   syn
_chemical_melting_point            ?
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'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             5
_space_group_name_H-M_alt          'C 1 2 1'
_space_group_name_Hall             'C 2y'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'

_cell_length_a                     33.185(5)
_cell_length_b                     5.9809(9)
_cell_length_c                     16.116(3)
_cell_angle_alpha                  90
_cell_angle_beta                   109.647(3)
_cell_angle_gamma                  90
_cell_volume                       3012.5(8)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      5366
_cell_measurement_temperature      100
_cell_measurement_theta_max        25.186
_cell_measurement_theta_min        2.162
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      0.233
_exptl_absorpt_correction_T_max    0.954
_exptl_absorpt_correction_T_min    0.946
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light white'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      white
_exptl_crystal_density_diffrn      1.404
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         needle
_exptl_crystal_F_000               1336
_exptl_crystal_size_max            0.3
_exptl_crystal_size_mid            0.2
_exptl_crystal_size_min            0.2
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0676
_diffrn_reflns_av_unetI/netI       0.0542
_diffrn_reflns_Laue_measured_fraction_full  0.994
_diffrn_reflns_Laue_measured_fraction_max  0.994
_diffrn_reflns_limit_h_max         39
_diffrn_reflns_limit_h_min         -39
_diffrn_reflns_limit_k_max         7
_diffrn_reflns_limit_k_min         -7
_diffrn_reflns_limit_l_max         19
_diffrn_reflns_limit_l_min         -19
_diffrn_reflns_number              18011
_diffrn_reflns_point_group_measured_fraction_full  0.991
_diffrn_reflns_point_group_measured_fraction_max  0.991
_diffrn_reflns_theta_full          25.186
_diffrn_reflns_theta_max           25.186
_diffrn_reflns_theta_min           2.162
_diffrn_ambient_temperature        100
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.994
_diffrn_measured_fraction_theta_max  0.994
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         ?
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     ?
_reflns_Friedel_coverage           0.806
_reflns_Friedel_fraction_full      0.988
_reflns_Friedel_fraction_max       0.988
_reflns_number_gt                  4876
_reflns_number_total               5366
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'SAINT V8.30C (?, 2016)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT V8.30C (?, 2016)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max           0.224
_refine_diff_density_min           -0.326
_refine_diff_density_rms           0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 1977 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     -0.01(4)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     0.991
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       400
_refine_ls_number_reflns           5366
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0369
_refine_ls_R_factor_gt             0.0317
_refine_ls_restrained_S_all        0.990
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0342P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0689
_refine_ls_wR_factor_ref           0.0709
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C16(H16A,H16B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C15(H15), C8(H8), C5(H5), C28(H28), C24(H24), C13(H13),
 C22(H22), C31(H31), C29(H29), C14(H14), C25(H25), C21(H21), C32(H32)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       iterative
_atom_sites_solution_secondary     ?
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_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 S1 S 0.36846(2) 0.44058(13) 0.15295(4) 0.01663(18) Uani 1 1 d . . . . .
 S2 S 0.28174(2) 0.90737(14) 0.34394(4) 0.0217(2) Uani 1 1 d . . . . .
 O3 O 0.38859(6) 0.6759(3) 0.45944(11) 0.0179(5) Uani 1 1 d . . . . .
 O1 O 0.50565(6) 0.0415(4) 0.75432(11) 0.0219(5) Uani 1 1 d . . . . .
 O2 O 0.50736(6) -0.1430(4) 0.63461(12) 0.0227(5) Uani 1 1 d . . . . .
 O6 O 0.38489(6) 0.5295(4) 0.08906(11) 0.0227(5) Uani 1 1 d . . . . .
 O5 O 0.37109(6) 0.2055(3) 0.17140(13) 0.0213(5) Uani 1 1 d . . . . .
 O7 O 0.31626(6) 0.7813(4) 0.31290(12) 0.0191(5) Uani 1 1 d . . . . .
 O9 O 0.24297(6) 0.7883(4) 0.30153(12) 0.0293(6) Uani 1 1 d . . . . .
 O4 O 0.39446(6) 0.5706(3) 0.24044(11) 0.0167(5) Uani 1 1 d . . . . .
 O8 O 0.28443(7) 1.1411(4) 0.32906(14) 0.0317(6) Uani 1 1 d . . . . .
 C11 C 0.42511(9) 0.1615(5) 0.78370(19) 0.0203(7) Uani 1 1 d . . . . .
 H11 H 0.417282 0.027451 0.753310 0.024 Uiso 1 1 calc R . . . .
 C9 C 0.43882(8) 0.3276(5) 0.65132(17) 0.0152(6) Uani 1 1 d . . . . .
 C4 C 0.45952(9) 0.1667(5) 0.61571(17) 0.0155(6) Uani 1 1 d . . . . .
 C10 C 0.43943(8) 0.3385(5) 0.74449(17) 0.0148(6) Uani 1 1 d . . . . .
 C12 C 0.42241(10) 0.1827(6) 0.86704(19) 0.0257(7) Uani 1 1 d . . . . .
 H12 H 0.412351 0.063943 0.891824 0.031 Uiso 1 1 calc R . . . .
 C15 C 0.45134(9) 0.5372(6) 0.79205(17) 0.0218(7) Uani 1 1 d . . . . .
 H15 H 0.460748 0.657711 0.766985 0.026 Uiso 1 1 calc R . . . .
 C3 C 0.49245(8) 0.0032(5) 0.66728(17) 0.0165(6) Uani 1 1 d . . . . .
 C23 C 0.32148(9) 0.7809(6) 0.63783(18) 0.0194(7) Uani 1 1 d . . . . .
 C8 C 0.41505(8) 0.4923(5) 0.59482(17) 0.0168(7) Uani 1 1 d . . . . .
 H8 H 0.400835 0.598966 0.616648 0.020 Uiso 1 1 calc R . . . .
 C5 C 0.45388(8) 0.1732(5) 0.52591(17) 0.0157(6) Uani 1 1 d . . . . .
 H5 H 0.466123 0.060757 0.502389 0.019 Uiso 1 1 calc R . . . .
 C17 C 0.39052(9) 0.5026(5) 0.32450(16) 0.0155(6) Uani 1 1 d . . . . .
 H17 H 0.363314 0.425403 0.315262 0.019 Uiso 1 1 calc R . . . .
 C20 C 0.29812(9) 0.8590(5) 0.45802(17) 0.0165(7) Uani 1 1 d . . . . .
 C27 C 0.31525(8) 0.5276(5) 0.13150(16) 0.0169(6) Uani 1 1 d . . . . .
 C2 C 0.54085(9) -0.0963(6) 0.80903(16) 0.0200(7) Uani 1 1 d . . . . .
 H2A H 0.566107 -0.074742 0.792465 0.024 Uiso 1 1 calc R . . . .
 H2B H 0.533050 -0.253247 0.802157 0.024 Uiso 1 1 calc R . . . .
 C28 C 0.28714(9) 0.3866(5) 0.15329(16) 0.0180(7) Uani 1 1 d . . . . .
 H28 H 0.296158 0.246727 0.177667 0.022 Uiso 1 1 calc R . . . .
 C6 C 0.43083(8) 0.3400(5) 0.47018(17) 0.0151(6) Uani 1 1 d . . . . .
 C30 C 0.23191(10) 0.6660(6) 0.10257(18) 0.0220(7) Uani 1 1 d . . . . .
 C24 C 0.30244(9) 0.6136(5) 0.57690(18) 0.0207(7) Uani 1 1 d . . . . .
 H24 H 0.297693 0.473765 0.597135 0.025 Uiso 1 1 calc R . . . .
 C13 C 0.43467(10) 0.3808(6) 0.91409(19) 0.0303(8) Uani 1 1 d . . . . .
 H13 H 0.433038 0.394642 0.970350 0.036 Uiso 1 1 calc R . . . .
 C7 C 0.41198(8) 0.5018(5) 0.50694(16) 0.0154(6) Uani 1 1 d . . . . .
 C22 C 0.32897(9) 0.9862(5) 0.60626(18) 0.0224(7) Uani 1 1 d . . . . .
 H22 H 0.341843 1.099077 0.646032 0.027 Uiso 1 1 calc R . . . .
 C31 C 0.26067(9) 0.8042(5) 0.08075(17) 0.0216(7) Uani 1 1 d . . . . .
 H31 H 0.251642 0.943890 0.056201 0.026 Uiso 1 1 calc R . . . .
 C26 C 0.33341(10) 0.7359(6) 0.73539(18) 0.0304(8) Uani 1 1 d . . . . .
 H26A H 0.310738 0.654745 0.746290 0.046 Uiso 1 1 calc GR . . . .
 H26B H 0.337844 0.875243 0.766756 0.046 Uiso 1 1 calc GR . . . .
 H26C H 0.359235 0.649126 0.755114 0.046 Uiso 1 1 calc GR . . . .
 C29 C 0.24563(9) 0.4563(6) 0.13840(17) 0.0225(7) Uani 1 1 d . . . . .
 H29 H 0.226612 0.361918 0.152491 0.027 Uiso 1 1 calc R . . . .
 C14 C 0.44926(10) 0.5565(6) 0.87647(19) 0.0285(8) Uani 1 1 d . . . . .
 H14 H 0.457760 0.688770 0.907821 0.034 Uiso 1 1 calc R . . . .
 C16 C 0.42785(9) 0.3553(5) 0.37403(17) 0.0165(6) Uani 1 1 d . . . . .
 H16A H 0.454155 0.417314 0.370067 0.020 Uiso 1 1 calc R . . . .
 H16B H 0.423967 0.207143 0.348047 0.020 Uiso 1 1 calc R . . . .
 C19 C 0.35801(9) 0.8874(5) 0.33172(17) 0.0183(7) Uani 1 1 d . . . . .
 H19A H 0.360346 1.014505 0.370432 0.022 Uiso 1 1 calc R . . . .
 H19B H 0.361206 0.940612 0.277425 0.022 Uiso 1 1 calc R . . . .
 C25 C 0.29049(9) 0.6507(5) 0.48729(18) 0.0197(7) Uani 1 1 d . . . . .
 H25 H 0.277585 0.538105 0.447399 0.024 Uiso 1 1 calc R . . . .
 C21 C 0.31773(9) 1.0276(6) 0.51656(18) 0.0223(7) Uani 1 1 d . . . . .
 H21 H 0.323243 1.165832 0.496198 0.027 Uiso 1 1 calc R . . . .
 C32 C 0.30262(9) 0.7372(5) 0.09496(17) 0.0190(7) Uani 1 1 d . . . . .
 H32 H 0.321671 0.830350 0.080397 0.023 Uiso 1 1 calc R . . . .
 C18 C 0.39247(9) 0.7204(5) 0.37493(17) 0.0165(7) Uani 1 1 d . . . . .
 H18 H 0.420308 0.790816 0.384137 0.020 Uiso 1 1 calc R . . . .
 C1 C 0.54940(10) -0.0231(6) 0.90284(18) 0.0322(9) Uani 1 1 d . . . . .
 H1A H 0.555894 0.133802 0.908074 0.048 Uiso 1 1 calc GR . . . .
 H1B H 0.573219 -0.105500 0.941200 0.048 Uiso 1 1 calc GR . . . .
 H1C H 0.524523 -0.050816 0.919019 0.048 Uiso 1 1 calc GR . . . .
 C33 C 0.18664(10) 0.7422(6) 0.0885(2) 0.0314(8) Uani 1 1 d . . . . .
 H33A H 0.183286 0.894442 0.068465 0.047 Uiso 1 1 calc GR . . . .
 H33B H 0.180978 0.731737 0.142998 0.047 Uiso 1 1 calc GR . . . .
 H33C H 0.166917 0.648806 0.045108 0.047 Uiso 1 1 calc GR . . . .


_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 O6 1.420(2) . ?
 S1 O5 1.433(2) . ?
 S1 O4 1.5872(19) . ?
 S1 C27 1.760(3) . ?
 S2 O7 1.586(2) . ?
 S2 O9 1.428(2) . ?
 S2 O8 1.426(2) . ?
 S2 C20 1.757(3) . ?
 O3 C7 1.369(3) . ?
 O3 C18 1.435(3) . ?
 O1 C3 1.341(3) . ?
 O1 C2 1.459(3) . ?
 O2 C3 1.209(3) . ?
 O7 C19 1.460(3) . ?
 O4 C17 1.462(3) . ?
 C11 C10 1.396(4) . ?
 C11 C12 1.382(4) . ?
 C9 C4 1.412(4) . ?
 C9 C10 1.496(4) . ?
 C9 C8 1.392(4) . ?
 C4 C3 1.493(4) . ?
 C4 C5 1.396(4) . ?
 C10 C15 1.397(4) . ?
 C12 C13 1.392(5) . ?
 C15 C14 1.390(4) . ?
 C23 C24 1.396(4) . ?
 C23 C22 1.383(4) . ?
 C23 C26 1.511(4) . ?
 C8 C7 1.386(4) . ?
 C5 C6 1.387(4) . ?
 C17 C16 1.511(4) . ?
 C17 C18 1.525(4) . ?
 C20 C25 1.385(4) . ?
 C20 C21 1.385(4) . ?
 C27 C28 1.387(4) . ?
 C27 C32 1.389(4) . ?
 C2 C1 1.507(4) . ?
 C28 C29 1.381(4) . ?
 C6 C7 1.389(4) . ?
 C6 C16 1.522(4) . ?
 C30 C31 1.394(4) . ?
 C30 C29 1.392(4) . ?
 C30 C33 1.512(4) . ?
 C24 C25 1.381(4) . ?
 C13 C14 1.380(5) . ?
 C22 C21 1.388(4) . ?
 C31 C32 1.391(4) . ?
 C19 C18 1.502(4) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O6 S1 O5 120.42(13) . . ?
 O6 S1 O4 103.53(11) . . ?
 O6 S1 C27 110.55(12) . . ?
 O5 S1 O4 108.61(11) . . ?
 O5 S1 C27 108.52(14) . . ?
 O4 S1 C27 103.85(12) . . ?
 O7 S2 C20 104.45(12) . . ?
 O9 S2 O7 104.02(13) . . ?
 O9 S2 C20 109.31(13) . . ?
 O8 S2 O7 108.67(13) . . ?
 O8 S2 O9 120.36(15) . . ?
 O8 S2 C20 108.82(14) . . ?
 C7 O3 C18 117.2(2) . . ?
 C3 O1 C2 116.7(2) . . ?
 C19 O7 S2 117.62(18) . . ?
 C17 O4 S1 119.72(17) . . ?
 C12 C11 C10 120.9(3) . . ?
 C4 C9 C10 126.4(2) . . ?
 C8 C9 C4 117.6(2) . . ?
 C8 C9 C10 116.0(2) . . ?
 C9 C4 C3 125.8(2) . . ?
 C5 C4 C9 119.2(3) . . ?
 C5 C4 C3 114.4(3) . . ?
 C11 C10 C9 122.0(3) . . ?
 C11 C10 C15 118.3(3) . . ?
 C15 C10 C9 119.6(3) . . ?
 C11 C12 C13 120.3(3) . . ?
 C14 C15 C10 120.6(3) . . ?
 O1 C3 C4 113.0(3) . . ?
 O2 C3 O1 122.8(3) . . ?
 O2 C3 C4 124.1(2) . . ?
 C24 C23 C26 120.2(3) . . ?
 C22 C23 C24 118.2(2) . . ?
 C22 C23 C26 121.6(3) . . ?
 C7 C8 C9 121.9(3) . . ?
 C6 C5 C4 122.9(3) . . ?
 O4 C17 C16 109.8(2) . . ?
 O4 C17 C18 104.8(2) . . ?
 C16 C17 C18 109.6(2) . . ?
 C25 C20 S2 118.5(2) . . ?
 C21 C20 S2 120.1(2) . . ?
 C21 C20 C25 121.4(3) . . ?
 C28 C27 S1 119.1(2) . . ?
 C28 C27 C32 121.5(3) . . ?
 C32 C27 S1 119.4(2) . . ?
 O1 C2 C1 106.5(2) . . ?
 C29 C28 C27 119.3(3) . . ?
 C5 C6 C7 117.0(2) . . ?
 C5 C6 C16 122.4(3) . . ?
 C7 C6 C16 120.5(2) . . ?
 C31 C30 C33 120.9(3) . . ?
 C29 C30 C31 118.9(3) . . ?
 C29 C30 C33 120.3(3) . . ?
 C25 C24 C23 121.6(3) . . ?
 C14 C13 C12 119.4(3) . . ?
 O3 C7 C8 115.8(2) . . ?
 O3 C7 C6 122.9(2) . . ?
 C8 C7 C6 121.2(3) . . ?
 C23 C22 C21 121.5(3) . . ?
 C32 C31 C30 121.3(3) . . ?
 C28 C29 C30 120.8(3) . . ?
 C13 C14 C15 120.5(3) . . ?
 C17 C16 C6 109.5(2) . . ?
 O7 C19 C18 109.2(2) . . ?
 C24 C25 C20 118.7(3) . . ?
 C20 C21 C22 118.7(3) . . ?
 C27 C32 C31 118.2(3) . . ?
 O3 C18 C17 110.3(2) . . ?
 O3 C18 C19 105.4(2) . . ?
 C19 C18 C17 115.6(2) . . ?


_olex2_submission_special_instructions  'No special instructions were received'
