First synthesis and characterization of isolable thioselenenic acid, triptycene-9-thioselenenic acid
Ishii, Akihiko; Takahashi, Takeshi; Tawata, Akira; Furukawa, Aki; Oshida, Hideaki; Nakayama, Juzo; Chemical Communications (Cambridge, United Kingdom)  (2002) 2810–2811; doi:10.1039/b207810d

data_7114415
_publ_section_title
;
 First synthesis and characterization of isolable thioselenenic acid,
 triptycene-9-thioselenenic acid
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   23
_journal_name_full
'Chemical Communications (Cambridge, United Kingdom)'
_journal_page_first              2810
_journal_page_last               2811
_journal_paper_doi               10.1039/b207810d
_journal_year                    2002
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C20 H14 S Se '
_chemical_formula_sum            'C20 H14 S Se'
_chemical_formula_weight         365.356
_chemical_name_systematic
;
Triptycene-9-thioselenenic acid
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                82.53(1)
_cell_angle_beta                 72.58(1)
_cell_angle_gamma                67.82(1)
_cell_formula_units_Z            2
_cell_length_a                   8.181(2)
_cell_length_b                   8.217(1)
_cell_length_c                   13.175(3)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    298
_cell_volume                     782.4(3)
_computing_cell_refinement       'MXC(MAC Science)'
_computing_data_collection       'MXC(MAC Science)'
_computing_data_reduction        'maXus (Mackay et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Mac Science MXC3KHF'
_diffrn_measurement_method       '\q \w scans'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.13533
_diffrn_orient_matrix_UB_12      -0.02770
_diffrn_orient_matrix_UB_13      -0.01813
_diffrn_orient_matrix_UB_21      0.00334
_diffrn_orient_matrix_UB_22      0.02878
_diffrn_orient_matrix_UB_23      -0.07654
_diffrn_orient_matrix_UB_31      -0.02237
_diffrn_orient_matrix_UB_32      0.12522
_diffrn_orient_matrix_UB_33      0.01198
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3166
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_standards_decay_%        3.873
_diffrn_standards_interval_time  1918
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.417
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
psi-scan (North, Philips & Mathews, 1968)
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0069(6)
_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   1.050
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0514P)^2^+0.4892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                2822
_reflns_number_total             2944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207810d.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        782.4(2)
_cod_original_sg_symbol_H-M      'P -1          '
_cod_original_formula_sum        'C20 H14 S Se '
_cod_database_code               7114415