Memory of Chirality Concept in Asymmetric Intermolecular Michael Addition of α-Amino Ester Enolates to Enones and Nitroalkenes.
Veeraswamy, Vadlamuri; Goswami, Gaurav; Mukherjee, Satobhisha; Ghosh, Koena; Saha, Manik Lal; Sengupta, Arunava; Ghorai, Manas K.; The Journal of organic chemistry 83 (2018) 1106–1115; doi:10.1021/acs.joc.7b02315

data_4033417
_publ_section_title
;
 Memory of Chirality Concept in Asymmetric Intermolecular Michael Addition
 of \a-Amino Ester Enolates to Enones and Nitroalkenes.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1106
_journal_page_last               1115
_journal_paper_doi               10.1021/acs.joc.7b02315
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C22 H27 F N2 O4'
_chemical_formula_sum            'C22 H27 F N2 O4'
_chemical_formula_weight         402.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                104.581(5)
_cell_angle_beta                 101.069(5)
_cell_angle_gamma                97.470(5)
_cell_formula_units_Z            4
_cell_length_a                   11.123(5)
_cell_length_b                   11.216(5)
_cell_length_c                   18.015(5)
_cell_measurement_reflns_used    10458
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.4
_cell_volume                     2096.7(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'Bruker SAINT PLUS'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR97(Altomare et al. 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1186
_diffrn_reflns_av_unetI/netI     0.1839
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32044
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.384
_diffrn_reflns_theta_min         2.428
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1953
_refine_ls_R_factor_gt           0.0748
_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^)+(0.0510P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4838
_reflns_number_total             10458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02315_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
Adding full bibliography for 4033416--4033417.cif.

2020-08-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C44 H54 F2 N4 O8'
_cod_original_formula_sum        'C44 H54 F2 N4 O8'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     804.91
_cod_database_code               4033417
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              3828
_shelx_hkl_checksum              93863