Molecular chirality and chiral capsule-type dimer formation of cyclic triamides via hydrogen-bonding interactions
Noriko Fujimoto; Mio Matsumura; Isao Azumaya; Shizuka Nishiyama; Hyuma Masu; Hiroyuki Kagechika; Aya Tanatani; Chem.Commun. 48 (2012) 4809–; doi:10.1039/c2cc18177k

data_7107642
_publ_section_title
;
 Molecular chirality and chiral capsule-type dimer formation of cyclic
 triamides via hydrogen-bonding interactions
;
_journal_name_full               Chem.Commun.
_journal_page_first              4809
_journal_paper_doi               10.1039/c2cc18177k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C39 H45 N3 O9, 1.5(C2N)'
_chemical_formula_sum            'C42 H45 N4.5 O9'
_chemical_formula_weight         756.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   16.5789(8)
_cell_length_b                   16.5789(8)
_cell_length_c                   19.1248(9)
_cell_measurement_reflns_used    6239
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.56
_cell_volume                     4552.4(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22648
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.9693
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;
;
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1822P)^2^+1.9114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2654
_refine_ls_wR_factor_ref         0.2769
_reflns_number_gt                2574
_reflns_number_total             3351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc18177k.txt
_cod_data_source_block           2d(a0808281mas)
_cod_original_sg_symbol_H-M      'P6(3)/m '
_cod_original_formula_sum        'C42 H45 N4.50 O9'
_cod_database_code               7107642