8,8′-Dialkyl-1,1′-biisoquinolines: preparation, absolute configuration and unexpected racemization behaviour †
Tsue, Hirohito; Fujinami, Hideyuki; Itakura, Takeshi; Tsuchiya, Ryuta; Kobayashi, Kimiko; Takahashi, Hiroki; Hirao, Ken-ichi; Journal of the Chemical Society, Perkin Transactions 1  (1999) 3677–; doi:10.1039/a905161i

data_7213139
_publ_section_title
;
 8,8&#x2032;-Dialkyl-1,1&#x2032;-biisoquinolines: preparation, absolute
 configuration and unexpected racemization behaviour&#x200A;&#x2020;
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3677
_journal_paper_doi               10.1039/a905161i
_journal_year                    1999
_chemical_formula_moiety         'C22 H20 N2 '
_chemical_formula_sum            'C22 H20 N2'
_chemical_formula_weight         312.41
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             'Thu May 27 16:22:10 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.343(3)
_cell_length_b                   20.316(2)
_cell_length_c                   7.5398(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.7
_cell_measurement_theta_max      23.4
_cell_measurement_theta_min      18.8
_cell_volume                     3269.3(6)
_computing_cell_refinement       'CAD4 express'
_computing_data_collection       'CAD4 express'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      296.7
_diffrn_measurement_device_type  'Enraf nonius CAD4'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.03089
_diffrn_orient_matrix_UB_12      0.03692
_diffrn_orient_matrix_UB_13      -0.00216
_diffrn_orient_matrix_UB_21      0.03488
_diffrn_orient_matrix_UB_22      0.03209
_diffrn_orient_matrix_UB_23      -0.01841
_diffrn_orient_matrix_UB_31      -0.00436
_diffrn_orient_matrix_UB_32      -0.00508
_diffrn_orient_matrix_UB_33      -0.13134
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'CAD4 sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.101
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7392
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        -0.09
_diffrn_standards_interval_count 120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa_analytical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328.00
_exptl_crystal_size_max          0.790
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.14
_refine_diff_density_min         -0.16
_refine_ls_extinction_coef       0.003(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_all   1.165
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00078|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0596
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0466
_reflns_number_gt                2200
_reflns_number_total             3748
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            905161isup1.cif
_cod_data_source_block           2
_cod_original_cell_volume        3269.3(5)
_cod_original_sg_symbol_H-M      'P b c a      '
_cod_original_formula_sum        'C22 H20 N2 '
_cod_database_code               7213139