A new and efficient approach to the synthesis of 6-amidino-2-oxopurines
Booth, Brian L.; Cabral, Isabel M.; Dias, Alice M.; Freitas, A. Paula; Matos Beja, Ana M.; Proença, M. Fernanda; Silva, Manuela Ramos; Journal of the Chemical Society, Perkin Transactions 1  (2001) 1241–; doi:10.1039/b010224p

data_7204065
_publ_contact_author
;
Dr M Fernanda J R P Procenca
Centro de Quimica-IBQF
Universidade do Minho
Campus de Gualtar
Braga
4710
PORTUGAL
;
_publ_section_title
;
 A new and efficient approach to the synthesis of
 6-amidino-2-oxopurines
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1241
_journal_paper_doi               10.1039/b010224p
_journal_year                    2001
_chemical_formula_moiety         'C20H18N6O4S, C2H4O2, H2O'
_chemical_formula_sum            'C22 H24 N6 O7 S'
_chemical_formula_weight         516.53
_chemical_name_systematic
; 
4-(p-anisidino)-8-tosylimino pyrimido[5,4-d]pyrimidina-2-one 
;
_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                 95.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.063(4)
_cell_length_b                   29.246(6)
_cell_length_c                   16.325(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.82
_cell_measurement_theta_min      5.71
_cell_volume                     2404(2)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.569
_diffrn_measured_fraction_theta_max 0.569
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       '\w-2\q 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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            1863
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        2.8
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.8652
_exptl_absorpt_correction_T_min  0.7953
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         1790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                996
_reflns_number_total             1790
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b010224p.txt
_cod_data_source_block           uminho
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7204065