Electrochemical oxidative coupling of 1,4-bis(1,4-dithiafulven-6-yl)benzene cyclophanes
Lorcy, Dominique; Guérin, David; Boubekeur, Kamal; Carlier, Roger; Hascoat, Philippe; Tallec, André; Robert, Albert; Journal of the Chemical Society, Perkin Transactions 1  (2000) 2719–; doi:10.1039/b002596h

data_7213345
_publ_section_title
;
 Electrochemical oxidative coupling of
 1,4-bis(1,4-dithiafulven-6-yl)benzene cyclophanes
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2719
_journal_paper_doi               10.1039/b002596h
_journal_year                    2000
_chemical_formula_moiety         'C28 H36 S6'
_chemical_formula_sum            'C28 H36 S6'
_chemical_formula_weight         564.95
_chemical_name_common
;
1,4-(bis 1,4-dithiafulven-6-yl)benzene cyclophane
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.29(3)
_cell_angle_beta                 89.88(3)
_cell_angle_gamma                72.94(3)
_cell_formula_units_Z            4
_cell_length_a                   10.510(2)
_cell_length_b                   13.225(3)
_cell_length_c                   22.293(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      1.65
_cell_volume                     2960.9(12)
_computing_cell_refinement       'SELECT (Stoe IPDS)'
_computing_data_collection       'EXPOSE (Stoe IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Rotation, \D\f=2\%'
_diffrn_radiation_detector       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.1306
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17225
_diffrn_reflns_reduction_process 'INTEGRATE (Stoe IPDS)'
_diffrn_reflns_theta_full        23.62
_diffrn_reflns_theta_max         23.62
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needdle
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.1430
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                3147
_reflns_number_total             7734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002596hsup1.cif
_cod_data_source_block           ph80i2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2960.8(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213345