Unusual molecular conformation in dissymmetric propylene-linker compounds containing pyrazolo[3,4-<i>d</i>]pyrimidine and phthalimide moieties
Avasthi, Kamlakar; Bhagat, Deepa; Bal, Chandralata; Sharon, Ashoke; Yadav, Umesh; Maulik, Prakas R.; Acta Crystallographica Section C 59 (2003) o409–o412; doi:10.1107/S0108270103011442

data_2013409
_publ_section_title
;
 Unusual molecular conformation in dissymmetric propylene-linker
 compounds containing pyrazolo[3,4-<i>d</i>]pyrimidine and phthalimide
 moieties
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o409
_journal_page_last               o412
_journal_paper_doi               10.1107/S0108270103011442
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C18 H17 N5 O2 S2'
_chemical_formula_moiety         'C18 H17 N5 O2 S2'
_chemical_formula_sum            'C18 H17 N5 O2 S2'
_chemical_formula_weight         399.49
_chemical_melting_point          393
_chemical_name_common            pyrazolo[3,4-d]pyrimidine
_chemical_name_systematic
;
4,6-Bis(methylsulfanyl)-1-phthalimidopropyl-1H-pyrazolo[3,4-d]pyrimidine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4710(10)
_cell_length_b                   13.1323(11)
_cell_length_c                   14.0516(12)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.82
_cell_measurement_theta_min      4.79
_cell_volume                     1888.6(3)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4 diffractometer'
_diffrn_measurement_method       \q-2\q
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4279
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.255
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.178
_refine_ls_extinction_coef       0.0189(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0372
_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^)+(0.027P)^2^+0.7345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                2566
_reflns_number_total             3327
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            de1208.cif
_cod_data_source_block           VI
_cod_original_cell_volume        1888.7(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013409