Basicities and Nucleophilicities of Pyrrolidines and Imidazolidinones Used as Organocatalysts.
An, Feng; Maji, Biplab; Min, Elizabeth; Ofial, Armin R.; Mayr, Herbert; Journal of the American Chemical Society 142 (2020) 1526–1547; doi:10.1021/jacs.9b11877

data_4134103
_publ_section_title
;
 Basicities and Nucleophilicities of Pyrrolidines and Imidazolidinones
 Used as Organocatalysts.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1526
_journal_page_last               1547
_journal_paper_doi               10.1021/jacs.9b11877
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C40 H43 N3'
_chemical_formula_sum            'C40 H43 N3'
_chemical_formula_weight         565.790
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                C40H43N3_rq001_mayr
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             03-Jan-13
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.6748(7)
_cell_length_b                   15.0381(10)
_cell_length_c                   36.178(2)
_cell_measurement_reflns_used    619
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.6068
_cell_measurement_theta_min      2.8067
_cell_volume                     6351.7(7)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'mix of phi and omega scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            101984
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         23.01
_diffrn_reflns_theta_min         2.25
_diffrn_source_current           1
_diffrn_source_power             50
_diffrn_source_type              'Bruker I\mS'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9419
_exptl_absorpt_correction_T_min  0.9142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.18334(13)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0339P)^2^+3.3938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                3255
_reflns_number_total             4403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b11877_si_002.cif
_cod_data_source_block           rq001
_cod_database_code               4134103
_shelx_res_checksum              72902
_shelx_hkl_checksum              9652