A Giese reaction for electron-rich alkenes.
Huang, Qi; Suravarapu, Sankar Rao; Renaud, Philippe; Chemical science 12 (2020) 2225–2230; doi:10.1039/d0sc06341j

data_1559814
_publ_section_title
;
 A Giese reaction for electron-rich alkenes.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2225
_journal_page_last               2230
_journal_paper_doi               10.1039/d0sc06341j
_journal_volume                  12
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H29 N O4'
_chemical_formula_weight         444.02
_chemical_name_systematic
'Benzyl 3-(((4S,5R)-2-oxo-4,5-diphenyloxazolidin-3-yl)methyl)pentanoate'
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-18T17:30:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-09-10 deposited with the CCDC.	2020-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.472(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.1281(2)
_cell_length_b                   27.1638(5)
_cell_length_c                   28.2117(7)
_cell_measurement_reflns_used    8869
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      76.47
_cell_measurement_theta_min      2.263
_cell_volume                     4694.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0835476
_diffrn_orient_matrix_UB_12      -0.0043885
_diffrn_orient_matrix_UB_13      -0.0508699
_diffrn_orient_matrix_UB_21      -0.2343967
_diffrn_orient_matrix_UB_22      0.0071384
_diffrn_orient_matrix_UB_23      -0.0198504
_diffrn_orient_matrix_UB_31      0.0362942
_diffrn_orient_matrix_UB_32      0.0560916
_diffrn_orient_matrix_UB_33      -0.0014555
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            36979
_diffrn_reflns_point_group_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.694
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.191
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.32761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2607 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.31(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1193
_refine_ls_number_reflns         13824
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+0.3714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.137
_reflns_Friedel_coverage         0.401
_reflns_Friedel_fraction_full    0.45
_reflns_Friedel_fraction_max     0.406
_reflns_number_gt                11416
_reflns_number_total             13824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06341j2.cif
_cod_data_source_block           19pr010_qh124p1
_cod_depositor_comments
;
 Adding full bibliography for 1559814--1559816.cif.

2022-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C112 H116 N4 O16'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1774.08
_cod_database_code               1559814
_shelx_res_checksum              36217