Three-component access to 2-pyrrolin-5-ones and their use in target-oriented and diversity-oriented synthesis
Cores, Ángel; Estévez, Verónica; Villacampa, Mercedes; Menéndez, J. Carlos; RSC Advances 6 (2016) 39433–; doi:10.1039/C6RA06317A

data_7236210
_publ_section_title
;
 Three-component access to 2-pyrrolin-5-ones and their use in
 target-oriented and diversity-oriented synthesis
;
_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              39433
_journal_paper_doi               10.1039/C6RA06317A
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C31 H35 N3 O4'
_chemical_formula_sum            'C31 H35 N3 O4'
_chemical_formula_weight         513.62
_chemical_melting_point          429.0(10)
_chemical_name_systematic
'Ethyl (1'S,2'S,3R)-1''-butyl-5''-methyl-2,2''-dioxo-1'-phenyl-1'',2'',5',6',7',7a'-hexahydro-1'H-dispiro[indoline-3,3'-pyrrolizine-2',3''-pyrrole]-4''-carboxylate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_update_record
;
2016-03-01 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                69.094(3)
_cell_angle_beta                 76.462(3)
_cell_angle_gamma                77.265(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9204(4)
_cell_length_b                   11.2869(4)
_cell_length_c                   13.6057(6)
_cell_measurement_temperature    298(2)
_cell_volume                     1367.79(10)
_computing_cell_refinement       'SAINT (Bruker 2006)'
_computing_data_collection       'APEX 2 (Bruker 2006)'
_computing_data_reduction        'SAINT (Bruker 2006)'
_computing_molecular_graphics    'Mercury 2.3 (Macrae et al, 2008)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6679
_diffrn_reflns_theta_full        66.73
_diffrn_reflns_theta_max         66.73
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.996
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.1261
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3169
_refine_ls_wR_factor_ref         0.3544
_reflns_number_gt                2594
_reflns_number_total             3953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra06317a2.cif
_cod_data_source_block           2fin
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '428-430' was changed to
'429.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7236210