5-<i>tert</i>-Butyl 3-ethyl 1-isopropyl-4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[4,3-<i>c</i>]pyridine-3,5-dicarboxylate
Guo, Huan-Mei; Acta Crystallographica Section E 67 (2011) o3239–; doi:10.1107/S1600536811046332

data_2232703
_publ_section_title
;
 5-<i>tert</i>-Butyl 3-ethyl
 1-isopropyl-4,5,6,7-tetrahydro-1<i>H</i>-pyrazolo[4,3-<i>c</i>]pyridine-3,5-dicarboxylate
;
_journal_coeditor_code           HB6476
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3239
_journal_paper_doi               10.1107/S1600536811046332
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C17 H27 N3 O4'
_chemical_formula_moiety         'C17 H27 N3 O4'
_chemical_formula_sum            'C17 H27 N3 O4'
_chemical_formula_weight         337.42
_chemical_name_systematic
;
5-<i>tert</i>-Butyl 3-ethyl 1-isopropyl-4,5,6,7-tetrahydro-1<i>H</i>-
pyrazolo[4,3-<i>c</i>]pyridine-3,5-dicarboxylate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.760(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.017(3)
_cell_length_b                   12.771(3)
_cell_length_c                   11.952(3)
_cell_measurement_reflns_used    5928
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      1.59
_cell_volume                     1789.4(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku MM007-HF CCD (Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7844
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9946
_exptl_absorpt_correction_T_min  0.9814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+1.0152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                3330
_reflns_number_total             4013
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6476.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2232703
_cod_database_fobs_code          2232703