Folded conformations due to arene interactions in dissymmetric and symmetric butylidene-linker models based on pyrazolo[3,4-<i>d</i>]pyrimidine, purine and 7-deazapurine
Avasthi, Kamlakar; Shukla, Lakshmi; Kant, Ruchir; Ravikumar, Krishnan; Acta Crystallographica Section C 70 (2014) 555–561; doi:10.1107/S2053229614009449

data_2019548
_publ_section_title
;
 Folded conformations due to arene interactions in dissymmetric and
 symmetric butylidene-linker models based on
 pyrazolo[3,4-<i>d</i>]pyrimidine, purine and 7-deazapurine
;
_journal_coeditor_code           EG3154
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              555
_journal_page_last               561
_journal_paper_doi               10.1107/S2053229614009449
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C19 H21 N7 O S3'
_chemical_formula_moiety         'C19 H21 N7 O S3'
_chemical_formula_sum            'C19 H21 N7 O S3'
_chemical_formula_weight         459.61
_chemical_name_systematic
;
7-[2-(4,6-Dimethylsulfanyl-1<i>H</i>-pyrazolo[3,4-<i>d</i>]pyrimidin-1-yl)-2-\
methylidenepropyl]-3-methyl-2-methylsulfanyl-3<i>H</i>-pyrrolo[2,3-<i>d</i>]\
pyrimidin-4(7<i>H</i>)-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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.943(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5436(7)
_cell_length_b                   11.5329(8)
_cell_length_c                   21.0042(13)
_cell_measurement_reflns_used    5170
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.1
_cell_volume                     2199.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'CCD area-detector'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25081
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.9375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.3873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                4550
_reflns_number_total             5277
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3154sup1.cif
_cod_data_source_block           XV
_cod_depositor_comments
'Adding full bibliography for 2019546--2019548.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019548
_cod_database_fobs_code          2019548