Traceless Solid-Phase Synthesis of N1,N7-Disubstituted Purines
Fu, Han; Lam, Yulin; Journal of Combinatorial Chemistry 7 (2005) 734–; doi:10.1021/cc050058f

data_1506341
_publ_section_title
;
 Traceless Solid-Phase Synthesis of N1,N7-Disubstituted Purines
;
_journal_issue                   5
_journal_name_full               'Journal of Combinatorial Chemistry'
_journal_page_first              734
_journal_paper_doi               10.1021/cc050058f
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C17 H27 Br N4 O3'
_chemical_formula_weight         415.34
_chemical_name_systematic
; 
 3-(1,7-dibutyl-6-oxo-1,6-dihydro-purin-9-yl)-propionic acid methyl ester salt 
;
_space_group_IT_number           2
_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                74.71(2)
_cell_angle_beta                 78.79(2)
_cell_angle_gamma                86.66(2)
_cell_formula_units_Z            4
_cell_length_a                   11.841(12)
_cell_length_b                   13.069(13)
_cell_length_c                   13.905(14)
_cell_measurement_reflns_used    5840
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.13
_cell_measurement_theta_min      2.32
_cell_volume                     2036(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22142
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7165
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.151
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2523
_refine_ls_wR_factor_ref         0.2737
_reflns_number_gt                5296
_reflns_number_total             7165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cc050058fsi20050505_124306.cif
_cod_data_source_block
3-(1,7-dibutyl-6-oxo-1,6-dihydro-purin-9-yl)-propionic_acid_methyl_ester_salt
_cod_database_code               1506341