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_4083479
_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            'C14 H18 B F4 Fe O7 P'
_chemical_formula_weight         471.91
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.194(10)
_cell_angle_beta                 94.811(10)
_cell_angle_gamma                99.008(10)
_cell_formula_units_Z            4
_cell_length_a                   11.3650(10)
_cell_length_b                   13.0800(10)
_cell_length_c                   14.277(2)
_cell_measurement_temperature    170(2)
_cell_volume                     1931.5(4)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.614
_diffrn_measured_fraction_theta_max 0.614
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15304
_diffrn_reflns_theta_full        26.86
_diffrn_reflns_theta_max         26.86
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                3738
_reflns_number_total             5107
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4068395
_cod_data_source_file            om800804b_si_002.cif
_cod_data_source_block           5b
_cod_database_code               4083479