Catalytic asymmetric defluorinative allylation of silyl enol ethers.
Duran, Jordi; Mateos, Javier; Moyano, Albert; Companyó, Xavier; Chemical science 14 (2023) 7147–7153; doi:10.1039/d3sc01498c

data_1569200
_publ_section_title
;
 Catalytic asymmetric defluorinative allylation of silyl enol ethers.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7147
_journal_page_last               7153
_journal_paper_doi               10.1039/d3sc01498c
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C17 H19 Br O3'
_chemical_formula_sum            'C17 H19 Br O3'
_chemical_formula_weight         351.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3235(17)
_cell_length_b                   9.838(2)
_cell_length_c                   17.181(4)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.24
_cell_measurement_theta_min      2.39
_cell_volume                     1575.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38606
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         2.371
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    2.616
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.118
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_refine_diff_density_min         -0.473
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_refine_ls_abs_structure_details
;
 Flack x determined using 1687 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+0.3265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                4258
_reflns_number_total             4799
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           mo_O42AAB104_0m
_cod_depositor_comments          'Adding full bibliography for 1569200.cif.'
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_shelx_hkl_checksum              77018