Quaternary β<sup>2,2</sup>-amino acid derivatives by asymmetric addition of isoxazolidin-5-ones to para-quinone methides.
Eitzinger, Andreas; Winter, Michael; Schörgenhumer, Johannes; Waser, Mario; Chemical communications (Cambridge, England) 56 (2020) 579–582; doi:10.1039/c9cc09239k

data_7125904
_publ_section_title
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 Quaternary \b<sup>2,2</sup>-amino acid derivatives by asymmetric addition
 of isoxazolidin-5-ones to para-quinone methides.
;
_journal_issue                   4
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              579
_journal_page_last               582
_journal_paper_doi               10.1039/c9cc09239k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_iupac          C42H49NO5
_chemical_formula_moiety         C42H49NO5
_chemical_formula_sum            'C42 H49 N O5'
_chemical_formula_weight         647.82
_chemical_name_common            EIT758
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2019-07-29 deposited with the CCDC.	2019-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                66.7160(10)
_cell_angle_beta                 71.4260(10)
_cell_angle_gamma                78.9980(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1974(3)
_cell_length_b                   10.5189(3)
_cell_length_c                   11.2152(4)
_cell_measurement_reflns_used    201
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      16.3495
_cell_measurement_theta_min      0.5040
_cell_volume                     942.12(5)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  'publCIF, Diamond 3.2k'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest Eco'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25464
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.34
_diffrn_source                   Mo
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.426
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.174
_refine_ls_abs_structure_details
;

Flack x determined using 1561 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(7)
_refine_ls_extinction_coef       0.040(7)
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         5411
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0689P)^2^+0.1068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                4003
_reflns_number_total             5411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09239k2.cif
_cod_data_source_block           FAK_EIT758_191218
_cod_database_code               7125904
_shelx_res_checksum              83015
_publcif_funding_html
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