Direct conjugate alkylation of α,β-unsaturated carbonyls by Ti(III)-catalysed reductive umpolung of simple activated alkenes.
Bichovski, Plamen; Haas, Thomas M.; Keller, Manfred; Streuff, Jan; Organic & biomolecular chemistry 14 (2016) 5673–5682; doi:10.1039/c5ob02631h

data_7154938
_publ_section_title
;
 Direct conjugate alkylation of \a,\b-unsaturated carbonyls by
 Ti(III)-catalysed reductive umpolung of simple activated alkenes.
;
_journal_issue                   24
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5673
_journal_page_last               5682
_journal_paper_doi               10.1039/c5ob02631h
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         'C13 H13 N O2'
_chemical_formula_sum            'C13 H13 N O2'
_chemical_formula_weight         215.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-03 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;
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_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
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_computing_structure_solution    'SIR-97 (Giacovazzo, 1997)'
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_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'long-fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.415
_diffrn_reflns_theta_min         2.071
_exptl_absorpt_coefficient_mu    0.088
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_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0572
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_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^)+(0.0402P)^2^+0.2285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2026
_reflns_number_total             2522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob02631h2.cif
_cod_data_source_block           mk568al
_cod_depositor_comments
'Adding full bibliography for 7154938--7154939.cif.'
_cod_original_cell_volume        1105.86(12)
_cod_database_code               7154938
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              91935