SF5-Enolates in Ti(IV)-Mediated Aldol Reactions.
Ponomarenko, Maksym V.; Grabowsky, Simon; Pal, Rumpa; Röschenthaler, Gerd-Volker; Fokin, Andrey A.; The Journal of organic chemistry 81 (2016) 6783–6791; doi:10.1021/acs.joc.6b00946

data_4032034
_publ_section_title
;
 SF5-Enolates in Ti(IV)-Mediated Aldol Reactions.
;
_journal_issue                   15
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6783
_journal_page_last               6791
_journal_paper_doi               10.1021/acs.joc.6b00946
_journal_volume                  81
_journal_year                    2016
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C9 H5 F5 O2 S'
_chemical_formula_sum            'C9 H5 F5 O2 S'
_chemical_formula_weight         272.19
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.891(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9912(6)
_cell_length_b                   9.2127(3)
_cell_length_c                   12.1513(3)
_cell_measurement_reflns_used    29993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.3
_cell_volume                     1943.83(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'micro focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29993
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.572
_diffrn_reflns_theta_min         2.346
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.96535
_exptl_absorpt_correction_T_min  0.94242
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Busing, W.R. et al.,1957)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0488P)^2^+1.3956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                2588
_reflns_number_total             2972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00946_si_003.cif
_cod_data_source_block           global
_cod_depositor_comments
'Adding full bibliography for 4032034--4032036.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4032034