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_4032036
_publ_contact_author
;
Dr. Simon Grabowsky
Emmy Noether Research Group Leader
Universit&#x00E4;t Bremen
Fachbereich 2 - Biologie/Chemie
Leobener Str. NW2
28359 Bremen
Germany
E-Mail: simon.grabowsky@uni-bremen.de
;
_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         'C11 H11 F5 O3 S'
_chemical_formula_sum            'C11 H11 F5 O3 S'
_chemical_formula_weight         318.26
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                99.478(1)
_cell_angle_beta                 110.838(1)
_cell_angle_gamma                95.682(1)
_cell_formula_units_Z            2
_cell_length_a                   8.4711(2)
_cell_length_b                   8.8607(2)
_cell_length_c                   8.9602(2)
_cell_measurement_reflns_used    54199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.660
_cell_measurement_theta_min      2.365
_cell_volume                     610.85(2)
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            54199
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.660
_diffrn_reflns_theta_min         2.365
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.97651
_exptl_absorpt_correction_T_min  0.95693
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Busing, W.R. et al.,1957)'
_exptl_crystal_colour            ' colorless'
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       ' block'
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0506P)^2^+0.3172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                3434
_reflns_number_total             3785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00946_si_002.cif
_cod_data_source_block           global
_cod_depositor_comments
'Adding full bibliography for 4032034--4032036.cif.'
_cod_database_code               4032036