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_7216961
_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 H43 N O2 S2 '
_chemical_formula_moiety         'C33 H43 N O2 S2 '
_chemical_formula_sum            'C33 H43 N O2 S2'
_chemical_formula_weight         549.83
_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             'Tue Apr 27 12:34:30 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 95.63(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.415(2)
_cell_length_b                   14.115(4)
_cell_length_c                   16.489(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      28.3
_cell_volume                     3107.2(15)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR88
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.05550
_diffrn_orient_matrix_UB_12      -0.04744
_diffrn_orient_matrix_UB_13      0.00755
_diffrn_orient_matrix_UB_21      0.04848
_diffrn_orient_matrix_UB_22      0.05189
_diffrn_orient_matrix_UB_23      0.01671
_diffrn_orient_matrix_UB_31      -0.01344
_diffrn_orient_matrix_UB_32      -0.00876
_diffrn_orient_matrix_UB_33      0.05812
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5029
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.09
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        -2.40
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1184.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.39
_refine_ls_extinction_coef       0.0165(8)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   3.644
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     344
_refine_ls_number_reflns         3433
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.2400
_refine_ls_shift/su_mean         0.0080
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                3433
_reflns_number_total             4845
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            b106154m.txt
_cod_data_source_block           Amino[1.3.3]MCP
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3107(1)
_cod_original_sg_symbol_H-M      'P 21/n  '
_cod_original_formula_sum        'C33 H43 N O2 S2 '
_cod_database_code               7216961