Magnesium-Promoted Additions of Difluoroenolates to Unactivated Imines.
Nguyen, Alex L.; Khatri, Hari R.; Woods, James R.; Baldwin, Cassidy S.; Fronczek, Frank R.; Colby, David A.; The Journal of organic chemistry 83 (2018) 3109–3118; doi:10.1021/acs.joc.7b03014

data_4033523
_publ_section_title
;
 Magnesium-Promoted Additions of Difluoroenolates to Unactivated Imines.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3109
_journal_page_last               3118
_journal_paper_doi               10.1021/acs.joc.7b03014
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C25 H19 F2 N O'
_chemical_formula_sum            'C25 H19 F2 N O'
_chemical_formula_weight         387.41
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.410(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7571(4)
_cell_length_b                   18.4857(13)
_cell_length_c                   17.5890(13)
_cell_measurement_reflns_used    2911
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.49
_cell_volume                     1866.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23437
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.579
_diffrn_reflns_theta_min         2.203
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0564P)^2^+0.6188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3673
_reflns_number_total             5689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b03014_si_002.cif
_cod_data_source_block           Colby2
_cod_depositor_comments
'Adding full bibliography for 4033523--4033524.cif.'
_cod_original_cell_volume        1866.3(2)
_cod_database_code               4033523
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              23673
_shelx_hkl_checksum              69414