Synthesis and Decarbonylation Reactions of the Triiron Phosphinidene Complex [Fe3Cp3(μ-H)(μ3-PPh)(CO)4]: Easy Cleavage and Formation of P-H and Fe-Fe Bonds
Celedonio M. Alvarez; M. Angeles Alvarez; M. Esther García; Rocío González; Alberto Ramos; Miguel A. Ruiz; Inorganic Chemistry 50 (2011) 10937–10948; doi:10.1021/ic201491v

data_4326681
_publ_section_title
;
 Synthesis and Decarbonylation Reactions of the Triiron Phosphinidene
 Complex [Fe3Cp3(\m-H)(\m3-PPh)(CO)4]: Easy Cleavage and Formation of P-H
 and Fe-Fe Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10937
_journal_page_last               10948
_journal_paper_doi               10.1021/ic201491v
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H20 Fe3 O2 P'
_chemical_formula_sum            'C23 H20 Fe3 O2 P'
_chemical_formula_weight         526.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.1320(8)
_cell_length_b                   9.3911(2)
_cell_length_c                   14.1378(4)
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     4000.61(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997) 
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '90 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27007
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    2.244
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.75
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.655
_refine_diff_density_min         -2.061
_refine_diff_density_rms         0.531
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.58(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1692P)^2^+11.2139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2122
_refine_ls_wR_factor_ref         0.2237
_reflns_number_gt                6695
_reflns_number_total             7244
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201491v_si_001_3.cif
_cod_data_source_block           compound6
_cod_database_code               4326681