2,5-Dimethyl-6,7-dihydrobenzo[<i>h</i>]pyrazolo[1,5-<i>a</i>]quinazoline and 2-<i>tert</i>-butyl-5-methyl-6,7-dihydrobenzo[<i>h</i>]pyrazolo[1,5-<i>a</i>]quinazoline
Portilla, Jaime; Quiroga, Jairo; Cobo, Justo; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 63 (2007) o458–o461; doi:10.1107/S0108270107029010

data_2016109
_publ_section_title
;2,5-Dimethyl-6,7-dihydrobenzo[<i>h</i>]pyrazolo[1,5-<i>a</i>]quinazoline and
 2-<i>tert</i>-butyl-5-methyl-6,7-dihydrobenzo[<i>h</i>]pyrazolo[1,5-<i>a</i>]quinazoline
;
_journal_coeditor_code           SK3137
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o458
_journal_page_last               o461
_journal_paper_doi               10.1107/S0108270107029010
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C19 H21 N3'
_chemical_formula_moiety         'C19 H21 N3'
_chemical_formula_sum            'C19 H21 N3'
_chemical_formula_weight         291.39
_chemical_name_systematic
;
2-tert-Butyl-5-methyl-6,7-dihydrobenzo[h]pyrazolo[1,5-a]quinazoline
;
_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                93.449(5)
_cell_angle_beta                 90.313(4)
_cell_angle_gamma                102.791(6)
_cell_formula_units_Z            4
_cell_length_a                   11.2632(5)
_cell_length_b                   11.4574(7)
_cell_length_c                   12.1317(6)
_cell_measurement_reflns_used    6991
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.26
_cell_volume                     1523.66(14)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>,  2000)'
_computing_data_collection       'COLLECT (Hooft, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>,  2003)'
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            37817
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1120P)^2^+0.7885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.2129
_reflns_number_gt                4144
_reflns_number_total             6991
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3137.cif
_cod_data_source_block           II
_cod_database_code               2016109
_cod_database_fobs_code          2016109