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_7107644
_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_absolute_configuration unk
_chemical_formula_moiety         'C33 H36 N6 O6, 2(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C37 H46 N8 O8'
_chemical_formula_weight         730.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.344(15)
_cell_length_b                   15.344(15)
_cell_length_c                   38.99(4)
_cell_measurement_reflns_used    7012
_cell_measurement_temperature    253
_cell_measurement_theta_max      19.15
_cell_measurement_theta_min      2.45
_cell_volume                     9180(16)
_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      253
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            45859
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.31
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.9559
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;
;
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_coef       0.0026(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         9671
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1855P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2408
_refine_ls_wR_factor_ref         0.2729
_reflns_number_gt                5030
_reflns_number_total             9671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc18177k.txt
_cod_data_source_block           a1009061mas_p43
_cod_original_sg_symbol_H-M      'P4(3)2(1)2 '
_cod_database_code               7107644