Hydrogen-bonded chains of rings in 3-<i>tert</i>-butyl-1-phenyl-7-(4-trifluoromethylbenzyl)-4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-dione and 3-<i>tert</i>-butyl-7-(4-methoxybenzyl)-1-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-dione
Trilleras, Jorge; Cruz, Silvia; Cobo, Justo; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 64 (2008) o671–o674; doi:10.1107/S0108270108038808

data_2016885
_publ_section_title
;Hydrogen-bonded chains of rings in
 3-<i>tert</i>-butyl-1-phenyl-7-(4-trifluoromethylbenzyl)-4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-dione
 and
 3-<i>tert</i>-butyl-7-(4-methoxybenzyl)-1-phenyl-4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-dione
;
_journal_coeditor_code           SK3277
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o671
_journal_page_last               o674
_journal_paper_doi               10.1107/S0108270108038808
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C29 H33 N3 O3'
_chemical_formula_moiety         'C29 H33 N3 O3'
_chemical_formula_sum            'C29 H33 N3 O3'
_chemical_formula_weight         471.58
_chemical_name_systematic
;
3-<i>tert</i>-butyl-7-(4-methoxybenzyl)-1-phenyl-4,5,6,7-tetrahydro-
1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-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                 97.287(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1904(10)
_cell_length_b                   11.9402(14)
_cell_length_c                   22.2888(16)
_cell_measurement_reflns_used    5566
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.87
_cell_volume                     2426.1(4)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg <i>et al.</i>,  2000)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>,  2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement
'OSCAIL (McArdle, 2003) and 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'
_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  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37788
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.315
_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     320
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0550P)^2^+1.2855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                3161
_reflns_number_total             5566
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3277.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016885
_cod_database_fobs_code          2016885