Activation of H-H and H-O Bonds at Phosphorus with Diiron Complexes Bearing Pyramidal Phosphinidene Ligands
M. Angeles Alvarez; M. Esther García; Daniel García-Vivó; Alberto Ramos; Miguel A. Ruiz; Inorganic Chemistry 51 (2012) 3698–3706; doi:10.1021/ic2026945

data_4328677
_publ_section_title
;
 Activation of H-H and H-O Bonds at Phosphorus with Diiron Complexes
 Bearing Pyramidal Phosphinidene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3698
_journal_page_last               3706
_journal_paper_doi               10.1021/ic2026945
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H27 Fe2 O4 P1'
_chemical_formula_sum            'C21 H27 Fe2 O4 P'
_chemical_formula_weight         486.1
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.293(4)
_cell_length_b                   11.795(3)
_cell_length_c                   23.293(6)
_cell_measurement_reflns_used    923
_cell_measurement_temperature    110.0(1)
_cell_measurement_theta_max      25.9955
_cell_measurement_theta_min      2.7955
_cell_measurement_wavelength     0.71073
_cell_volume                     4201.6(19)
_computing_cell_refinement       'Brucker Smart'
_computing_data_collection       'Brucker Smart'
_computing_data_reduction        'Brucker 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      110(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            35866
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.747940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.44
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.073
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0276P)^2^+10.7231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                3062
_reflns_number_total             4290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2026945_si_002.cif
_cod_data_source_block           compound5
_cod_database_code               4328677