Asymmetric transformation (deracemisation) of an atropisomeric bisheterocyclic amine†
Coogan, Michael P.; Smart, Emma; Hibbs, David E.; Chemical Communications  (1999) 1991–; doi:10.1039/a905018c

data_7110632
_publ_section_title
;
 Asymmetric transformation (deracemisation) of an atropisomeric
 bisheterocyclic amine&#x2020;
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1991
_journal_paper_doi               10.1039/a905018c
_journal_year                    1999
_chemical_formula_sum            'C18 H15 N5 O3'
_chemical_formula_weight         349.35
_space_group_IT_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                73.144(10)
_cell_angle_beta                 78.90(2)
_cell_angle_gamma                88.302(10)
_cell_formula_units_Z            2
_cell_length_a                   4.684(4)
_cell_length_b                   13.470(5)
_cell_length_c                   13.786(6)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_volume                     816.5(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       'bisect mode'
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.3223
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2307
_diffrn_reflns_theta_full        22.76
_diffrn_reflns_theta_max         22.76
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         2201
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.2872
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                714
_reflns_number_total             2201
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            905018csup1.cif
_cod_data_source_block           99dai007
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        816.6(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110632