Redetermined structure of oxaline: absolute configuration using Cu <i>K</i>α radiation
Qu, Peng; Wu, Zhi-Yong; Zhu, Wei-Ming; Acta Crystallographica Section E 68 (2012) o1626–; doi:10.1107/S1600536812019423

data_2235015
_publ_section_title
;
 Redetermined structure of oxaline: absolute configuration using Cu
 <i>K</i>\a radiation
;
_journal_coeditor_code           HB6738
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1626
_journal_paper_doi               10.1107/S1600536812019423
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C24 H25 N5 O4'
_chemical_formula_moiety         'C24 H25 N5 O4'
_chemical_formula_sum            'C24 H25 N5 O4'
_chemical_formula_weight         447.49
_chemical_name_systematic        oxaline
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7897(2)
_cell_length_b                   13.2457(3)
_cell_length_c                   15.6436(4)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.99
_cell_measurement_theta_min      2.82
_cell_volume                     2235.74(9)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11202
_diffrn_reflns_theta_full        69.44
_diffrn_reflns_theta_max         69.44
_diffrn_reflns_theta_min         4.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.9142
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.263
_refine_ls_abs_structure_details 'Flack (1983), 1403 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.05(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0539P)^2^+0.6080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                3766
_reflns_number_total             3786
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6738.cif
_cod_data_source_block           I
_cod_database_code               2235015
_cod_database_fobs_code          2235015