Hydrogen-bonded bilayers in 7-benzyl-3-<i>tert</i>-butyl-1-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-spiro[pyrazolo[3,4-<i>b</i>]pyridine-5,2'-indan]-1',3'-dione
Quiroga, Jairo; Pantoja, Dayana; Cobo, Justo; Glidewell, Christopher; Acta Crystallographica Section C 69 (2013) 884–887; doi:10.1107/S0108270113017435

data_2019081
_publ_section_title
;
 Hydrogen-bonded bilayers in
 7-benzyl-3-<i>tert</i>-butyl-1-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-spiro[pyrazolo[3,4-<i>b</i>]pyridine-5,2'-indan]-1',3'-dione
;
_journal_coeditor_code           FG3298
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              884
_journal_page_last               887
_journal_paper_doi               10.1107/S0108270113017435
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C31 H29 N3 O2'
_chemical_formula_moiety         'C31 H29 N3 O2'
_chemical_formula_sum            'C31 H29 N3 O2'
_chemical_formula_weight         475.57
_chemical_name_systematic
7-Benzyl-3-<i>tert</i>-butyl-1-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-spiro[pyrazolo[3,4-<i>b</i>]pyridine-5,2'-indan]-1',3'-dione
_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                 91.841(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6917(18)
_cell_length_b                   5.9748(4)
_cell_length_c                   24.840(3)
_cell_measurement_reflns_used    5680
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.98
_cell_volume                     2476.0(4)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>, 2000)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38299
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0452P)^2^+1.1191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3889
_reflns_number_total             5679
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3298.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019081
_cod_database_fobs_code          2019081