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_8000158
_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         'C23 H27 N2 O4, C7 H5 O2, H2 O'
_chemical_formula_sum            'C30 H34 N2 O7'
_chemical_formula_weight         534.61
_chemical_name_common            'brucinium benzoate hydrate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.7284(2)
_cell_length_b                   13.6981(3)
_cell_length_c                   25.2319(6)
_cell_measurement_reflns_used    7955
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      67.6
_cell_measurement_theta_min      3.2
_cell_volume                     2671.16(11)
_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 0.904
_diffrn_measured_fraction_theta_max 0.904
_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  0.060
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10441
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.571
_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    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1136.00
_exptl_crystal_recrystallization_method 'recrystallization from acetonitrile'
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1582 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.6(6)
_refine_ls_extinction_coef       0.0295(15)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4111
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0651P)^2^+3.4634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2151
_reflns_number_gt                2583
_reflns_number_total             4111
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            36-234sup1.cif
_cod_data_source_block           1_3_water
_cod_database_code               8000158