Phosphine Addition to Pyruvoyl Ligands of Iron Complexes: Formation of Zwitterionic Metallalactones
Salaün, J. Y.; Rumin, R.; Setifi, F.; Triki, S.; Jaffrès, P. A.; Organometallics 28 (2009) 216–224; doi:10.1021/om800804b

data_4068394
_publ_section_title
;
 Phosphine Addition to Pyruvoyl Ligands of Iron Complexes: Formation of
 Zwitterionic Metallalactones
;
_journal_coden_ASTM              ORGND7
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              216
_journal_page_last               224
_journal_paper_doi               10.1021/om800804b
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C15 H21 Fe O8 P'
_chemical_formula_weight         416.14
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.409(2)
_cell_length_b                   10.736(2)
_cell_length_c                   17.932(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1811.4(6)
_computing_cell_refinement       'CRYSALIS-RED 170 (Oxford-Diffraction, 2002)'
_computing_data_collection       'CRYSALIS-CCD 170 (Oxford-Diffraction,2002)'
_computing_data_reduction        'CRYSALIS-RED 170 (Oxford-Diffraction, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'Xcalibur 2 CCD Oxford Diffraction'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_sigmaI/netI    0.1300
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6751
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                1886
_reflns_number_total             2550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800804b_si_001.cif
_cod_data_source_block           2b(1)
_cod_original_cell_volume        1811.5(6)
_cod_database_code               4068394