Dimethyl 3-(<i>tert</i>-butylamino)-5-oxo-7-phenyl-1<i>H</i>,5<i>H</i>-pyrazolo[1,2-<i>a</i>]pyrazole-1,2-dicarboxylate
Abbasi, Alireza; Adib, Mehdi; Eriksson, Lars; Acta Crystallographica Section E 63 (2007) o2115–o2116; doi:10.1107/S1600536807013773

data_2213287
_publ_section_title
;Dimethyl
 3-(<i>tert</i>-butylamino)-5-oxo-7-phenyl-1<i>H</i>,5<i>H</i>-pyrazolo[1,2-<i>a</i>]pyrazole-1,2-dicarboxylate
;
_journal_coeditor_code           EZ2068
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2115
_journal_page_last               o2116
_journal_paper_doi               10.1107/S1600536807013773
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H23 N3 O5'
_chemical_formula_moiety         'C20 H23 N3 O5'
_chemical_formula_sum            'C20 H23 N3 O5'
_chemical_formula_weight         385.41
_chemical_name_systematic
;
Dimethyl
3-(<i>tert</i>-butylamino)-7-phenyl-5-oxo-1<i>H</i>,5<i>H</i>-pyrazolo[1,2-\
<i>a</i>]pyrazole-1,2-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.059(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1826(8)
_cell_length_b                   9.4017(6)
_cell_length_c                   17.1789(12)
_cell_measurement_reflns_used    13972
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      32.1
_cell_measurement_theta_min      3.9
_cell_volume                     1967.3(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'Diamond (Brandenburg, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 12
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford X-calibur 3 CCD'
_diffrn_measurement_method       '\w-scans at different \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.033
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13972
_diffrn_reflns_theta_full        27.0
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         4.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.20
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.057
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.101
_refine_ls_wR_factor_ref         0.105
_reflns_number_gt                2751
_reflns_number_total             4282
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ez2068.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2213287
_cod_database_fobs_code          2213287