A Cyclochiral Conformational Motif Constructed Using a Robust Hydrogen-Bonding Network
Kenji Mishiro; Takumi Furuta; Takahiro Sasamori; Kazuhiro Hayashi; Norihiro Tokitoh; Shiroh Futaki; Takeo Kawabata; Journal of the American Chemical Society 135 (2013) 13644–13647; doi:10.1021/ja407051k

data_4120807
_publ_section_title
;
 A Cyclochiral Conformational Motif Constructed Using a Robust
 Hydrogen-Bonding Network
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13644
_journal_page_last               13647
_journal_paper_doi               10.1021/ja407051k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C37 H32 N6 O4'
_chemical_formula_sum            'C37 H32 N6 O4'
_chemical_formula_weight         624.69
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 98.213(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.959(7)
_cell_length_b                   13.032(5)
_cell_length_c                   15.286(6)
_cell_measurement_reflns_used    3467
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.28
_cell_measurement_theta_min      2.03
_cell_volume                     3147(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        Yadokari2008
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10902
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_correction_T_min  0.9741
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0680P)^2^+0.9001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                2085
_reflns_number_total             2932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407051k_si_001.cif
_cod_data_source_block           km-4
_cod_database_code               4120807