Photochemical synthesis and structural properties of high membered thiohelicenes
Caronna, Tullio; Sinisi, Roberta; Malpezzi, Luciana; Meille, Stefano V.; Mele, Andrea; Catellani, Marinella; Chemical Communications  (2000) 1139–; doi:10.1039/b002581j

data_7115113
_publ_section_title
;
 Photochemical synthesis and structural properties of high membered
 thiohelicenes
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1139
_journal_paper_doi               10.1039/b002581j
_journal_year                    2000
_chemical_formula_moiety         'C28 H12 S5'
_chemical_formula_sum            'C28 H12 S5'
_chemical_formula_weight         508.68
_chemical_name_common            '[9]-thiohelicene'
_chemical_name_systematic
;
 [9]-thiohelicene
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6550(10)
_cell_length_b                   10.6560(10)
_cell_length_c                   13.9760(10)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      12.6
_cell_volume                     2147.7(3)
_computing_cell_refinement       'xscans (Siemens, 1994)'
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'Xscans (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al.1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.452
_diffrn_measured_fraction_theta_max 0.452
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3662
_diffrn_reflns_theta_full        67.92
_diffrn_reflns_theta_max         67.92
_diffrn_reflns_theta_min         5.16
_diffrn_standards_decay_%        <0.3
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.098
_exptl_absorpt_correction_T_max  0.7131
_exptl_absorpt_correction_T_min  0.1648
_exptl_absorpt_correction_type   'empirical via \y-scan'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0021(2)
_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   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         1875
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          2.639
_refine_ls_shift/su_mean         0.110
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+1.5730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                1760
_reflns_number_total             1875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002581j.txt
_cod_data_source_block           heli9
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+1.5730P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+1.5730P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7115113