Preparation and structural properties of dithia[3.3.1]metacyclophanes
Moriguchi, Tetsuji; Inoue, Megumi; Yasutake, Mikio; Sinmyozu, Teruo; Sakata, Kazunori; Tsuge, Akihiko; Journal of the Chemical Society, Perkin Transactions 2  (2001) 2084–; doi:10.1039/b106154m

data_7216962
_publ_section_title
;
 Preparation and structural properties of dithia[3.3.1]metacyclophanes
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              2084
_journal_paper_doi               10.1039/b106154m
_journal_year                    2001
_chemical_formula_moiety         'C33 H42 O3 S2 '
_chemical_formula_sum            'C33 H42 O3 S2'
_chemical_formula_weight         550.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Fri Feb 23 17:05:15 2001'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 94.727(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.497(2)
_cell_length_b                   16.640(3)
_cell_length_c                   15.500(2)
_cell_measurement_reflns_used    12684
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.5
_cell_volume                     2955.2(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13622
_diffrn_reflns_theta_max         27.48
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.37
_refine_ls_extinction_coef       0.0000
_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   0.845
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     343
_refine_ls_number_reflns         1914
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0922P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2359
_reflns_number_gt                1914
_reflns_number_total             6093
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b106154m.txt
_cod_data_source_block           '[1.3.3]OH'
_cod_original_cell_volume        2955.2(7)
_cod_original_formula_sum        'C33 H42 O3 S2 '
_cod_database_code               7216962