Four Kinds of 21 Helical Assemblies with the Molecular Tilt as Well as Three-directional and Facial Chirality
Watabe, Tsuyoshi; Hisaki, Ichiro; Tohnai, Norimitsu; Miyata, Mikiji; Chemistry Letters 36 (2007) 234–; doi:10.1246/cl.2007.234

data_8000157
_publ_section_title
;
 Four Kinds of 21 Helical Assemblies with the Molecular Tilt as Well as
 Three-directional and Facial Chirality
;
_journal_issue                   2
_journal_name_full               'Chemistry Letters'
_journal_page_first              234
_journal_paper_doi               10.1246/cl.2007.234
_journal_volume                  36
_journal_year                    2007
_chemical_formula_moiety         '2(C23 H27 N2 O4), 2(C15 H21 O3), C3 H6 O'
_chemical_formula_sum            'C79 H102 N4 O15'
_chemical_formula_weight         1347.69
_chemical_name_common
'brucinium 3,5-di-tert-butyl-4-hydroxybenzoate acetone solvate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.496(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   14.8933(6)
_cell_length_b                   12.9949(5)
_cell_length_c                   18.6164(8)
_cell_measurement_reflns_used    12468
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      3.0
_cell_volume                     3542.7(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  SHELXL
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.155
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24773
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448.00
_exptl_crystal_recrystallization_method 'recrystallization from acetone'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.51
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  4899 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.0(7)
_refine_ls_extinction_coef       0.0100(6)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     886
_refine_ls_number_reflns         11406
_refine_ls_R_factor_gt           0.1653
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3851
_reflns_number_gt                3183
_reflns_number_total             11406
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            36-234sup1.cif
_cod_data_source_block           1_2_acetone
_cod_original_cell_volume        3542.7(2)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               8000157