Disappearance of intramolecular stacking due to one-atom movement or increment of a `propylene linker' in pyrazolo[3,4-<i>d</i>]pyrimidine-based flexible models
Maulik, Prakas R.; Avasthi, Kamlakar; Sarkhel, Sanjay; Chandra, Tilak; Rawat, Diwan S.; Logsdon, Brad; Jacobson, Robert A.; Acta Crystallographica Section C 56 (2000) 1361–1363; doi:10.1107/S0108270100010775

data_2011585
_publ_section_title
;
 Disappearance of intramolecular stacking due to one-atom movement or
 increment of a `propylene linker' in
 pyrazolo[3,4-<i>d</i>]pyrimidine-based flexible models
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1361
_journal_page_last               1363
_journal_paper_doi               10.1107/S0108270100010775
_journal_volume                  56
_journal_year                    2000
_chemical_formula_sum            'C18 H22 N8 O2 S2'
_chemical_formula_weight         446.56
_chemical_melting_point          150
_chemical_name_common            Pyrazolo[3,4-d]pyrimidine
_chemical_name_systematic
;
 1-[4-(4-methoxy-6-methylthio-1H-pyrazolo[3,4-d]pyrimidin-1-yl)butyl]-
 5-methyl-6-methylthio-4,5-dihydro-1H-pyrazolo[3,4-d]pyrimidin-4-one
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 115.12(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.736(7)
_cell_length_b                   8.308(2)
_cell_length_c                   17.467(4)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.8
_cell_measurement_theta_min      4.9
_cell_volume                     4169.8(18)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1992)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'NRCVAX (Gabe et al., 1989)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Siemens P4 diffractometer'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .0324
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3616
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .289
_exptl_absorpt_correction_T_max  .835
_exptl_absorpt_correction_T_min  .772
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(local program; Karcher, 1981)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Trapezoidal
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          .8
_exptl_crystal_size_mid          .6
_exptl_crystal_size_min          .5
_refine_diff_density_max         .282
_refine_diff_density_min         -.221
_refine_ls_extinction_coef       .0068(5)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          .0460
_refine_ls_R_factor_gt           .0410
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0685P)^2^+1.3387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1210
_reflns_number_gt                3189
_reflns_number_total             3616
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            vj1110.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4169.8(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2011585
_cod_database_fobs_code          2011585