Synthesis and Reactivity of η4-Diene-Fe(CO)3Complexes fromexo-2-Oxazolidinone Dienes. A Facile Generation of Stable Conjugated Enol-Enamido Species
Ortega-Jiménez, Fernando; Benavides, Adriana; Delgado, Francisco; Jiménez-Vázquez, Hugo A.; Tamariz, Joaquín; Organometallics 29 (2010) 149–; doi:10.1021/om900772z

data_4067288
_publ_section_title
;
 Synthesis and Reactivity of \h4-Diene-Fe(CO)3Complexes
 fromexo-2-Oxazolidinone Dienes. A Facile Generation of Stable Conjugated
 Enol-Enamido Species
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              149
_journal_paper_doi               10.1021/om900772z
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C19 H21 Fe1 N1 O5'
_chemical_formula_sum            'C19 H21 Fe N O5'
_chemical_formula_weight         399.22
_chemical_name_systematic
;
 Tricarbonyl-?4-[(Z)-3-hydroxy-2-(N-phenypivalamido)hexa-1,3-diene]iron(0)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-03-10T21:03:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.760(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.77120(10)
_cell_length_b                   26.8224(7)
_cell_length_c                   10.7305(2)
_cell_measurement_reflns_used    7505
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      32.4494
_cell_measurement_theta_min      2.434
_cell_measurement_wavelength     0.71073
_cell_volume                     1939.03(7)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'PLATON (Spek, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.2257
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.03892692
_diffrn_orient_matrix_UB_12      0.0231618416
_diffrn_orient_matrix_UB_13      0.0232818675
_diffrn_orient_matrix_UB_21      0.0886076965
_diffrn_orient_matrix_UB_22      -0.0121345089
_diffrn_orient_matrix_UB_23      0.0244687884
_diffrn_orient_matrix_UB_31      0.041498154
_diffrn_orient_matrix_UB_32      0.0042184958
_diffrn_orient_matrix_UB_33      -0.0572272866
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16071
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         32.53
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.688
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         6282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0924
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0066P)^2^+6.0388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                4697
_reflns_number_total             6282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900772z_si_001.cif
_cod_data_source_block           cmplx-10b
_cod_database_code               4067288