Conformational and Optical Characteristics of Unidirectionally Twisted Binaphthyl-Bipyridyl Cyclic Dyads.
Takaishi, Kazuto; Suzuki, Jun; Yabe, Tatsuya; Asano, Hikaru; Nishikawa, Michihiro; Hashizume, Daisuke; Muranaka, Atsuya; Uchiyama, Masanobu; Yokoyama, Akihiro; Organic letters 17 (2015) 4098–4101; doi:10.1021/acs.orglett.5b02041

data_1555218
_publ_section_title
;
 Conformational and Optical Characteristics of Unidirectionally Twisted
 Binaphthyl-Bipyridyl Cyclic Dyads.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4098
_journal_page_last               4101
_journal_paper_doi               10.1021/acs.orglett.5b02041
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C32 H22 N2 O2, C H Cl3'
_chemical_formula_sum            'C33 H23 Cl3 N2 O2'
_chemical_formula_weight         585.88
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 106.9450(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.07268(16)
_cell_length_b                   11.9732(2)
_cell_length_c                   13.4535(3)
_cell_measurement_reflns_used    24340
_cell_measurement_temperature    165
_cell_measurement_theta_max      68.275
_cell_measurement_theta_min      3.435
_cell_volume                     1397.99(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      165
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku Raxis-Rapid'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24557
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.241
_exptl_absorpt_correction_T_max  0.6651
_exptl_absorpt_correction_T_min  0.3248
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numabs
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4935
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0337P)^2^+0.1484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                4686
_reflns_number_total             4935
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol5b02041_si_002.cif
_cod_data_source_block           R11-chloroform
_cod_original_cell_volume        1397.98(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1555218