Four <i>N</i>^7^-benzyl-substituted 4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-diones as ethanol hemisolvates: similar molecular constitutions but different crystal structures
Cruz, Silvia; Trilleras, Jorge; Cobo, Justo; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 64 (2008) o637–o642; doi:10.1107/S0108270108036937

data_2016860
_publ_section_title
;Four <i>N</i>^7^-benzyl-substituted
 4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[3,4-<i>b</i>]pyridine-5-spiro-1'-cyclohexane-2',6'-diones
 as ethanol hemisolvates: similar molecular constitutions but different
 crystal structures
;
_journal_coeditor_code           GA3109
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o637
_journal_page_last               o642
_journal_paper_doi               10.1107/S0108270108036937
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C30 H34 Cl N3 O2 , 0.5C2 H6 O'
_chemical_formula_moiety         'C30 H34 Cl N3 O2 , 0.5C2 H6 O'
_chemical_formula_sum            'C31 H37 Cl N3 O2.5'
_chemical_formula_weight         527.09
_chemical_name_systematic
;
3-<i>tert</i>-Butyl-7-(4-chlorobenzyl)-4',4'-dimethyl-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 ethanol hemisolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 122.625(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.419(4)
_cell_length_b                   10.5860(13)
_cell_length_c                   21.580(3)
_cell_measurement_reflns_used    6021
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.96
_cell_volume                     5275.4(14)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36250
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.522
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6021
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0455P)^2^+11.7674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                4812
_reflns_number_total             6021
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3109.cif
_cod_data_source_block           I
_cod_original_cell_volume        5275.5(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C31 H37 Cl1 N3 O2.5'
_cod_database_code               2016860
_cod_database_fobs_code          2016860