Synthesis and X-ray structures of new concave π-prismand hydrocarbon [2.2.1]m,p,p- and [2.2.1]p,p,p-cyclophanes
Lahtinen, Tanja; Wegelius, Elina; Rissanen, Kari; New Journal of Chemistry 25 (2001) 905–; doi:10.1039/b102725p

data_7051141
_publ_section_title
;
 Synthesis and X-ray structures of new concave \p-prismand hydrocarbon
 [2.2.1]m,p,p- and [2.2.1]p,p,p-cyclophanes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              905
_journal_paper_doi               10.1039/b102725p
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C23 H22 S2'
_chemical_formula_weight         362.53
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.0448(31)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9684(7)
_cell_length_b                   10.2645(6)
_cell_length_c                   16.6081(10)
_cell_measurement_temperature    173.0(1)
_cell_volume                     1869.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8351
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9448
_exptl_absorpt_correction_type   'not used'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+1.6238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                2601
_reflns_number_total             3234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102725p.txt
_cod_data_source_block           12
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7051141