5-<i>tert</i>-Butyl 1-ethyl 3-amino-1,4,5,6-tetrahydropyrrolo[3,4-<i>c</i>]pyrazole-1,5-dicarboxylate
Xia, Wen-Bin; Bai, Xiao-Guang; Liu, Hong-Tao; Wang, Ju-Xian; Acta Crystallographica Section E 67 (2011) o1150–; doi:10.1107/S1600536811013444

data_2230134
_publ_section_title
;
 5-<i>tert</i>-Butyl 1-ethyl
 3-amino-1,4,5,6-tetrahydropyrrolo[3,4-<i>c</i>]pyrazole-1,5-dicarboxylate
;
_journal_coeditor_code           RZ2580
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1150
_journal_paper_doi               10.1107/S1600536811013444
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C13 H20 N4 O4'
_chemical_formula_moiety         'C13 H20 N4 O4'
_chemical_formula_sum            'C13 H20 N4 O4'
_chemical_formula_weight         296.33
_chemical_name_systematic
;
5-<i>tert</i>-Butyl 1-ethyl
3-amino-1,4,5,6-tetrahydropyrrolo[3,4-<i>c</i>]pyrazole-1,5-dicarboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.845(5)
_cell_angle_beta                 65.875(4)
_cell_angle_gamma                85.821(5)
_cell_formula_units_Z            4
_cell_length_a                   10.772(3)
_cell_length_b                   12.180(4)
_cell_length_c                   12.986(4)
_cell_measurement_reflns_used    2737
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.63
_cell_volume                     1465.2(8)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7444
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9960
_exptl_absorpt_correction_T_min  0.9940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0632P)^2^+0.4323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                3915
_reflns_number_total             5102
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2580.cif
_cod_data_source_block           I
_cod_original_cell_volume        1465.2(7)
_cod_database_code               2230134
_cod_database_fobs_code          2230134