Diversity oriented syntheses of fused pyrimidines designed as potential antifolates
Gibson, Colin L.; Huggan, Judith K.; Kennedy, Alan; Kiefer, Lionel; Lee, Jeong Hwan; Suckling, Colin J.; Clements, Carol; Harvey, Alan L.; Hunter, William N.; Tulloch, Lindsay B.; Organic & Biomolecular Chemistry 7 (2009) 1829–1842; doi:10.1039/b818339b

data_7150571
_publ_section_title
;
 Diversity oriented syntheses of fused pyrimidines designed as
 potential antifolates
;
_journal_issue                   9
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              1829
_journal_page_last               1842
_journal_paper_doi               10.1039/b818339b
_journal_volume                  7
_journal_year                    2009
_chemical_formula_sum            'C16.8 H19.2 N4 O4.8'
_chemical_formula_weight         353.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                81.282(3)
_cell_angle_beta                 77.534(2)
_cell_angle_gamma                81.436(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1471(3)
_cell_length_b                   10.1809(4)
_cell_length_c                   12.3149(5)
_cell_measurement_reflns_used    3734
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     858.56(6)
_computing_data_collection       'Denzo & Collect'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.040
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15464
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut needle'
_exptl_crystal_F_000             373
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.031(7)
_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   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3900
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0659P)^2^+0.3762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                2695
_reflns_number_total             3900
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b818339b.txt
_cod_data_source_block           suc205
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C16.80 H19.20 N4 O4.80'
_cod_database_code               7150571