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_7216957
_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_analytical     'C33 H41 N O4 S2 '
_chemical_formula_moiety         'C33 H41 N O4 S2 '
_chemical_formula_sum            'C33 H41 N O4 S2'
_chemical_formula_weight         579.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Mon Mar 15 02:49:46 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 114.97(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.169(4)
_cell_length_b                   12.719(7)
_cell_length_c                   17.684(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    103.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     3093(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      103.2
_diffrn_detector_area_resol_mean 0.010000
_diffrn_measurement_device_type  'Rigaku RAXIS-IV'
_diffrn_measurement_method       'Imaging Plate'
_diffrn_radiation_detector       'Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.011
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6686
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         55.10
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1240.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.674
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     525
_refine_ls_number_reflns         6076
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.1270
_refine_ls_shift/su_mean         0.0070
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                6076
_reflns_number_total             6686
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b106154m.txt
_cod_data_source_block           Nitrodithia[1.3.3]MCPLowTemp
_cod_original_cell_volume        3092.6599
_cod_original_sg_symbol_H-M      'P 21/c       '
_cod_original_formula_sum        'C33 H41 N O4 S2 '
_cod_database_code               7216957