Heterometallic Derivatives of [Fe2Cp2(μ-PCy)(μ-CO)(CO)2]: Rational Synthesis of Polynuclear Complexes from Neutral Precursors Having Pyramidal-Phosphinidene Bridges
M. Angeles Alvarez; M. Esther García; Rocío González; Alberto Ramos; Miguel A. Ruiz; Inorganic Chemistry 50 (2011) 7894–7906; doi:10.1021/ic2012342

data_4325971
_publ_section_title
;
 Heterometallic Derivatives of [Fe2Cp2(\m-PCy)(\m-CO)(CO)2]: Rational
 Synthesis of Polynuclear Complexes from Neutral Precursors Having
 Pyramidal-Phosphinidene Bridges
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7894
_journal_page_last               7906
_journal_paper_doi               10.1021/ic2012342
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H21 Fe3 O7 P1'
_chemical_formula_sum            'C23 H21 Fe3 O7 P'
_chemical_formula_weight         607.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                109.399(8)
_cell_angle_beta                 109.268(7)
_cell_angle_gamma                90.931(9)
_cell_formula_units_Z            4
_cell_length_a                   11.0549(10)
_cell_length_b                   14.8440(12)
_cell_length_c                   16.0361(18)
_cell_measurement_reflns_used    1478
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.88
_cell_measurement_wavelength     0.71073
_cell_volume                     2319.6(4)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Smart'
_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    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27935
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.571749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0281P)^2^+0.5678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                8569
_reflns_number_total             9792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012342_si_002_2.cif
_cod_data_source_block           compound2e
_cod_database_code               4325971