Thiacyclophane Cages and Related Bi- and Tripodal Molecules via Transient Polysulfenic Acids
Maria Chiara Aversa; Anna Barattucci; Paola Bonaccorsi; Cristina Faggi; Teresa Papalia; Journal of Organic Chemistry 72 (2007) 4486–4496; doi:10.1021/jo070449b

data_4022952
_publ_section_title
;
 Thiacyclophane Cages and Related Bi- and Tripodal Molecules
 via Transient Polysulfenic Acids
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4486
_journal_page_last               4496
_journal_paper_doi               10.1021/jo070449b
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C19 H17 Cl3 O2 S2'
_chemical_formula_weight         447.80
_chemical_name_systematic
;
 Meso-1,12-dimethylene-2,11-dithia[3.3]metacyclophane 2,11-dioxide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Thu Jan 26 17:38:21 2006'
;
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p20 beta (release 16-09-2005 CrysAlis171 .NET)
(compiled Sep 16 2005,17:54:02)
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 92.810(6)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   10.787(1)
_cell_length_b                   13.238(1)
_cell_length_c                   14.494(1)
_cell_measurement_temperature    298(2)
_cell_volume                     2067.2(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p20 beta (release 16-09-2005 CrysAlis171 .NET)
(compiled Sep 16 2005,17:54:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p20 beta (release 16-09-2005 CrysAlis171 .NET)
(compiled Sep 16 2005,17:54:02)
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p20 beta (release 16-09-2005 CrysAlis171 .NET)
(compiled Sep 16 2005,17:54:02)
;
_computing_molecular_graphics    Ortep3
_computing_publication_material  Ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir2002(J.Applied Crystallography,2003)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   -7.26   89.74   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.7362   70.0000    0.0000    0.0000    0.0000 97

  2 omega   -7.26   89.74   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.7362   70.0000  120.0000    0.0000    0.0000 97

  3 omega   -7.26   89.74   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.7362   70.0000  240.0000    0.0000    0.0000 97

  4 omega  -49.06   47.94   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.7362  -70.0000    0.0000    0.0000    0.0000 97

  5 omega  -49.06   47.94   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.7362  -70.0000  120.0000    0.0000    0.0000 97

  6 omega  -49.06   47.94   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.7362  -70.0000  240.0000    0.0000    0.0000 97
;
_diffrn_measurement_device_type  'Xcalibur3 MoK\a (Oxford Diffraction)'
_diffrn_measurement_method       'omega scan'
_diffrn_orient_matrix_UB_11      -0.0013734561
_diffrn_orient_matrix_UB_12      0.0356785181
_diffrn_orient_matrix_UB_13      0.0364385159
_diffrn_orient_matrix_UB_21      0.0312629908
_diffrn_orient_matrix_UB_22      -0.0348138269
_diffrn_orient_matrix_UB_23      0.0301922064
_diffrn_orient_matrix_UB_31      0.0579216751
_diffrn_orient_matrix_UB_32      0.0196398796
_diffrn_orient_matrix_UB_33      -0.0127028973
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-Ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15017
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  1.1402
_exptl_absorpt_correction_T_min  0.8487
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p20 beta (release 16-09-2005 CrysAlis171 .NET)
(compiled Sep 16 2005,17:54:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       rhombohedric
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0035(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+1.2651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                2189
_reflns_number_total             2749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070449bsi20070305_035911.cif
_cod_data_source_block           xcalibur
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4022952