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_7051144
_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            'C24 H22 Ag F3 O3 S'
_chemical_formula_weight         555.35
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7142(6)
_cell_length_b                   13.7436(5)
_cell_length_c                   13.8602(6)
_cell_measurement_temperature    173.0(1)
_cell_volume                     2231.43(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12265
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_correction_T_min  0.8589
_exptl_absorpt_correction_type   'SORTAV, not used'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0000P)^2^+0.6248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                3322
_reflns_number_total             3938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102725p.txt
_cod_data_source_block           17
_cod_database_code               7051144