Four <i>N</i>^7^-alkoxybenzyl-substituted 4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-diones: hydrogen-bonded supramolecular structures in zero, one, two or three dimensions
Trilleras, Jorge; Quiroga, Jairo; Cobo, Justo; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 64 (2008) o665–o670; doi:10.1107/S0108270108038778

data_2016883
_publ_section_title
;Four <i>N</i>^7^-alkoxybenzyl-substituted
 4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-diones:
 hydrogen-bonded supramolecular structures in zero, one, two or three
 dimensions
;
_journal_coeditor_code           SK3276
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o665
_journal_page_last               o670
_journal_paper_doi               10.1107/S0108270108038778
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C33 H41 N3 O5, 0.67C2 H6 O'
_chemical_formula_moiety         'C33 H41 N3 O5, 0.67(C2 H6 O)'
_chemical_formula_sum            'C34.34 H45.02 N3 O5.67'
_chemical_formula_weight         590.55
_chemical_name_systematic
;
3-<i>tert</i>-butyl-4',4'-dimethyl-1-phenyl-7-(3,4,5-trimethoxybenzyl)-
4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-
cyclohexane-2',6'-dione ethanol 0.67-solvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5770(17)
_cell_length_b                   17.476(3)
_cell_length_c                   26.670(3)
_cell_measurement_reflns_used    7255
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.88
_cell_volume                     6328.0(15)
_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 (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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            53340
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2539.4
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0866
_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^)+(0.0324P)^2^+20.6148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2056
_reflns_number_gt                4959
_reflns_number_total             7255
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3276.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2016883
_cod_database_fobs_code          2016883