General and stereoselective aminoxylation of biradical titanium(iv) enolates with TEMPO: a detailed study on the effect of the chiral auxiliary.
Kennington, Stuart C. D.; Gómez-Palomino, Alejandro; Salomó, Ernest; Romea, Pedro; Urpí, Fèlix; Font-Bardia, Mercè; Organic & biomolecular chemistry 16 (2018) 4807–4815; doi:10.1039/c8ob01074a

data_7156284
_publ_section_title
;
 General and stereoselective aminoxylation of biradical titanium(iv)
 enolates with TEMPO: a detailed study on the effect of the chiral
 auxiliary.
;
_journal_issue                   26
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4807
_journal_page_last               4815
_journal_paper_doi               10.1039/c8ob01074a
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C25 H38 N2 O3 S'
_chemical_formula_sum            'C25 H38 N2 O3 S'
_chemical_formula_weight         446.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2018-04-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.58(2)
_cell_length_b                   7.180(5)
_cell_length_c                   16.940(15)
_cell_measurement_reflns_used    9419
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.69
_cell_measurement_theta_min      3.05
_cell_volume                     2540(4)
_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    'XT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.976
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29378
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.787
_diffrn_reflns_theta_min         2.946
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
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_exptl_crystal_size_mid          0.457
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2771 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7660
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0820P)^2^+2.3941P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                6709
_reflns_number_total             7660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob01074a2.cif
_cod_data_source_block           mo_O31VB194_0m_a
_cod_depositor_comments          'Adding full bibliography for 7156284.cif.'
_cod_original_cell_volume        2541(4)
_cod_database_code               7156284
_shelxl_version_number           2012-9
_shelx_res_checksum              75083