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_4325975
_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         'C24 H21 Cr1 Fe2 O8 P1'
_chemical_formula_sum            'C24 H21 Cr Fe2 O8 P'
_chemical_formula_weight         632.08
_chemical_name_systematic
;
 ?
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.0240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7622(2)
_cell_length_b                   18.5003(3)
_cell_length_c                   13.3338(2)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.275
_cell_measurement_theta_min      2.2
_cell_measurement_wavelength     0.71073
_cell_volume                     2398.88(7)
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_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      100.0(1)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega/phi 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  0.037
_diffrn_reflns_av_unetI/netI     0.018
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            78988
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  0.6667
_exptl_absorpt_correction_T_min  0.5814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.75
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.31
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.027
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0242P)^2^+1.3570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.053
_reflns_number_gt                5050
_reflns_number_total             5730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012342_si_002_6.cif
_cod_data_source_block           compound5a
_cod_original_formula_sum        'C24 H21 Cr1 Fe2 O8 P1'
_cod_database_code               4325975