Eight 7-benzyl-3-<i>tert</i>-butyl-1-phenylpyrazolo[3,4-<i>d</i>]oxazines, encompassing structures containing no intermolecular hydrogen bonds, and hydrogen-bonded structures in one, two or three dimensions
Castillo, Juan C.; Abonía, Rodrigo; Cobo, Justo; Glidewell, Christopher; Acta Crystallographica Section C 65 (2009) o423–o430; doi:10.1107/S0108270109028017

data_2017224
_publ_section_title
;
 Eight
 7-benzyl-3-<i>tert</i>-butyl-1-phenylpyrazolo[3,4-<i>d</i>]oxazines,
 encompassing structures containing no intermolecular hydrogen bonds,
 and hydrogen-bonded structures in one, two or three dimensions
;
_journal_coeditor_code           FA3197
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o423
_journal_page_last               o430
_journal_paper_doi               10.1107/S0108270109028017
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C24 H29 N3 O3'
_chemical_formula_moiety         'C24 H29 N3 O3'
_chemical_formula_sum            'C24 H29 N3 O3'
_chemical_formula_weight         407.50
_chemical_name_systematic
;
3-<i>tert</i>-butyl-7-(2,3-dimethoxybenzyl)-1-phenyl-6,7-dihydro-
1<i>H</i>,4<i>H</i>-pyrazolo[3,4-<i>d</i>][1,3]oxazine
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.747(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8268(10)
_cell_length_b                   11.6521(10)
_cell_length_c                   10.3831(7)
_cell_measurement_reflns_used    2560
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.94
_cell_volume                     1065.63(17)
_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, 2009)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       '\f & \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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17934
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2560
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.2363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                2132
_reflns_number_total             2560
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3197.cif
_cod_data_source_block           VI
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2017224
_cod_database_fobs_code          2017224