Quinolinone and pyridopyrimidinone inhibitors of DNA-dependent protein kinase
Barbeau, Olivier R.; Cano-Soumillac, Celine; Griffin, Roger J.; Hardcastle, Ian R.; Smith, Graeme C. M.; Richardson, Caroline; Clegg, William; Harrington, Ross W.; Golding, Bernard T.; Organic & Biomolecular Chemistry 5 (2007) 2670–; doi:10.1039/b705095j

data_7151131
_publ_section_title
;
 Quinolinone and pyridopyrimidinone inhibitors of DNA-dependent protein
 kinase
;
_journal_issue                   16
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              2670
_journal_paper_doi               10.1039/b705095j
_journal_volume                  5
_journal_year                    2007
_chemical_formula_moiety         'C13 H12 F3 N3 O5 S'
_chemical_formula_sum            'C13 H12 F3 N3 O5 S'
_chemical_formula_weight         379.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 110.821(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            20
_cell_length_a                   20.220(9)
_cell_length_b                   16.889(7)
_cell_length_c                   23.103(10)
_cell_measurement_reflns_used    11035
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      2.24
_cell_volume                     7374(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6898
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60275
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00018(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         15066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+3.2967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                10025
_reflns_number_total             15066
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b705095j.txt
_cod_data_source_block           ssc0450_compound_16
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7151131