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_2019546
_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          'C18 H20 N8 S4'
_chemical_formula_moiety         'C18 H20 N8 S4'
_chemical_formula_sum            'C18 H20 N8 S4'
_chemical_formula_weight         476.66
_chemical_name_systematic
1-[2-(2,6-Dimethylsulfanyl-9<i>H</i>-purin-9-yl)-2-methylidenepropyl]-4,6-bis(methylsulfanyl)-1<i>H</i>-pyrazolo[3,4-<i>d</i>]pyrimidine
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                98.707(7)
_cell_angle_beta                 103.080(3)
_cell_angle_gamma                109.593(4)
_cell_formula_units_Z            2
_cell_length_a                   9.285(4)
_cell_length_b                   9.818(4)
_cell_length_c                   13.400(6)
_cell_measurement_reflns_used    1622
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.1
_cell_volume                     1086.0(8)
_computing_cell_refinement       '<i>CrystalClear-SM Expert</i> (Rigaku, 2012)'
_computing_data_collection       '<i>CrystalClear-SM Expert</i> (Rigaku, 2012)'
_computing_data_reduction        '<i>CrystalClear-SM Expert</i> (Rigaku, 2012)'
_computing_molecular_graphics    'SHELXTL (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_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'AFC12 (Right) Kappa three-circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8577
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.9510
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                2711
_reflns_number_total             3891
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3154sup1.cif
_cod_data_source_block           XI
_cod_depositor_comments
'Adding full bibliography for 2019546--2019548.cif.'
_cod_database_code               2019546
_cod_database_fobs_code          2019546