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_7216959
_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 O2 S2 '
_chemical_formula_sum            'C33 H42 O2 S2'
_chemical_formula_weight         534.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Mon Jun 11 15:26:42 2001'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90.878(4)
_cell_angle_beta                 116.678(2)
_cell_angle_gamma                83.190(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7609(6)
_cell_length_b                   18.671(2)
_cell_length_c                   9.1231(5)
_cell_measurement_reflns_used    7088
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     1473.8(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9276
_diffrn_measured_fraction_theta_max 0.9276
_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  0.045
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12179
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3397
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.0092
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                3397
_reflns_number_total             6256
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            b106154m.txt
_cod_data_source_block           dithia[3.3.1]MCP
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C33 H42 O2 S2 '
_cod_database_code               7216959