First Determination of the Absolute Configuration of an Atropisomeric Flavin Derivative
Yasushi Kawai; Jun Kunitomo; Atsuyoshi Ohno; Acta Crystallographica Section C 54 (1998) 77–79; doi:10.1107/S0108270197013838

data_2006949
_publ_section_title
;
 First Determination of the Absolute Configuration of an Atropisomeric
 Flavin Derivative
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              77
_journal_page_last               79
_journal_paper_doi               10.1107/S0108270197013838
_journal_volume                  54
_journal_year                    1998
_chemical_formula_analytical     'C55.52 H4.30 N6.65'
_chemical_formula_moiety         'C28 H23 Br2 N3 O2, C H4 O'
_chemical_formula_sum            'C29 H27 Br2 N3 O3'
_chemical_formula_weight         625.36
_chemical_name_systematic
;
3-(4,6-dibromo-o-tolyl)-10-(4-tert-butylphenyl)pyrimido[4,5-b]quinoline-
2,4(3H,10H)-dione
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 100.45(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.913(7)
_cell_length_b                   10.868(8)
_cell_length_c                   12.030(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    173.2
_cell_measurement_theta_max      15.1
_cell_measurement_theta_min      14.9
_cell_volume                     2689(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1992)
;
_computing_data_reduction
'TEXSAN PROCESS (Molecular Structure Corporation, 1995)'
_computing_publication_material  'TEXSAN FINISH'
_computing_structure_refinement  'TEXSAN LS'
_computing_structure_solution    'direct methods SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      173.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9752
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0.17
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.061
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      1.51
_exptl_crystal_density_method
;
flotation in C~6~H~14~/CCl~4~
;
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.70
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.0210(10)
_refine_ls_extinction_coef       0.0002(5)
_refine_ls_extinction_method
;
Zachariasen (1967) type 2 Gaussian isotropic
;
_refine_ls_goodness_of_fit_all   0.828
_refine_ls_goodness_of_fit_obs   0.862
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     667
_refine_ls_number_reflns         8524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.052
_refine_ls_R_factor_obs          .034
_refine_ls_shift/esd_max         0.0204
_refine_ls_shift/esd_mean        0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F~o~) + 0.0025|F~o~|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.066
_refine_ls_wR_factor_obs         .052
_reflns_number_observed          8524
_reflns_number_total             9469
_reflns_observed_criterion       >1.5sigma(I)
_cod_data_source_file            oa1036.cif
_cod_data_source_block           Br2dFl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F~o~) +
0.0025|F~o~|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(F~o~) + 0.0025|F~o~|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2687(2)
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2006949