Ethyl 2,5-di-<i>tert</i>-butyl-5-ethoxy-4-oxo-4,5-dihydro-1<i>H</i>-pyrrole-3-carboxylate
Rosen, Gerald M.; Muralidharan, Sukumaran; Zavalij, Peter Y.; Fletcher, Steven; Kao, Joseph P. Y.; Acta Crystallographica Section E 69 (2013) o878–; doi:10.1107/S1600536813012282

data_2237930
_publ_section_title
;
 Ethyl
 2,5-di-<i>tert</i>-butyl-5-ethoxy-4-oxo-4,5-dihydro-1<i>H</i>-pyrrole-3-carboxylate
;
_journal_coeditor_code           LD2098
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o878
_journal_paper_doi               10.1107/S1600536813012282
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C17 H29 N O4'
_chemical_formula_moiety         'C17 H29 N O4'
_chemical_formula_sum            'C17 H29 N O4'
_chemical_formula_weight         311.41
_chemical_name_systematic
'Ethyl 2,5-di-<i>tert</i>-butyl-5-ethoxy-4-oxo-4,5-dihydro-1<i>H</i>-pyrrole-3-carboxylate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_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-2012 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 92.5822(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9187(7)
_cell_length_b                   16.3916(11)
_cell_length_c                   22.2115(15)
_cell_measurement_reflns_used    26267
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.2
_cell_volume                     3607.6(4)
_computing_cell_refinement       '<i>APEX2</i> and <i>SAINT</i> (Bruker, 2010)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2010)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2010)'
_computing_molecular_graphics
;
<i>XSHELL</i> (Bruker, 2010)
and <i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL2012</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40948
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.213
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.325
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+2.6980P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                5812
_reflns_number_total             6356
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ld2098.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2237930
_cod_database_fobs_code          2237930