A hydrogen-bonded chain of rings in 7-amino-5-<i>tert</i>-butyl-2-methylpyrazolo[1,5-<i>a</i>]pyrimidine, and a hydrogen-bonded framework structure in 3,7-diamino-2,5-dimethylpyrazolo[1,5-<i>a</i>]pyrimidine monohydrate
Portilla, Jaime; Quiroga, Jairo; Torre, José M. de la; Cobo, Justo; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 62 (2006) o521–o524; doi:10.1107/S0108270106025893

data_2015521
_publ_section_title
;
 A hydrogen-bonded chain of rings in
 7-amino-5-<i>tert</i>-butyl-2-methylpyrazolo[1,5-<i>a</i>]pyrimidine,
 and a hydrogen-bonded framework structure in
 3,7-diamino-2,5-dimethylpyrazolo[1,5-<i>a</i>]pyrimidine monohydrate
;
_journal_coeditor_code           SK3040
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o521
_journal_page_last               o524
_journal_paper_doi               10.1107/S0108270106025893
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C11 H16 N4'
_chemical_formula_moiety         'C11 H16 N4'
_chemical_formula_sum            'C11 H16 N4'
_chemical_formula_weight         204.28
_chemical_name_systematic
;
7-amino-5-tert-butyl-2-methylpyrazolo[1,5-a]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                70.429(3)
_cell_angle_beta                 69.895(4)
_cell_angle_gamma                66.454(4)
_cell_formula_units_Z            4
_cell_length_a                   9.8216(5)
_cell_length_b                   11.3582(7)
_cell_length_c                   12.2783(8)
_cell_measurement_reflns_used    4863
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      1.81
_cell_volume                     1147.66(13)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement
'OSCAIL (McArdle, 2003) and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22882
_diffrn_reflns_theta_full        26.77
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.230
_refine_ls_extinction_coef       0.015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.1822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                2931
_reflns_number_total             4863
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3040.cif
_cod_data_source_block           I
_cod_original_cell_volume        1147.66(12)
_cod_database_code               2015521
_cod_database_fobs_code          2015521