Controlled Self-Assembly of Multiple Diastereomeric Macrocyclic Boronic Esters Composed of Two Chiral Units
Suguru Ito; Kosuke Ono; Nobuharu Iwasawa; Journal of the American Chemical Society 134 (2012) 13962–13965; doi:10.1021/ja306249f

data_4118559
_publ_contact_author             'Nobuharu Iwasawa'
_publ_contact_author_email       niwasawa@chem.titech.ac.jp
_publ_section_title
;
 Controlled Self-Assembly of Multiple Diastereomeric Macrocyclic Boronic
 Esters Composed of Two Chiral Units
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13962
_journal_page_last               13965
_journal_paper_doi               10.1021/ja306249f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C76 H68 B4 O12, 4(C H Cl3)'
_chemical_formula_sum            'C40 H36 B2 Cl6 O6'
_chemical_formula_weight         847.01
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.874(4)
_cell_angle_beta                 79.210(4)
_cell_angle_gamma                88.593(5)
_cell_formula_units_Z            2
_cell_length_a                   12.970(4)
_cell_length_b                   13.166(4)
_cell_length_c                   13.637(4)
_cell_measurement_reflns_used    2019
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      3.05
_cell_volume                     2067.1(11)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998) '
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998) '
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID IP area detector system'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20193
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'rotating anode x-ray tube'
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.9135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'absorption was corrected by ABSCOR'
_exptl_crystal_colour            platelet
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       colorless
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9214
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1313P)^2^+0.0285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2584
_reflns_number_gt                4645
_reflns_number_total             9214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja306249f_meso-3e.cif
_cod_data_source_block           meso-3e
_cod_original_cell_volume        2067.1(10)
_cod_database_code               4118559