Synthesis and Characterization of Pentaphosphino Zero-Valent Iron Complexes and Their Corresponding Iron(II)-Chloride and -Hydride Complexes
Kristen A. Thoreson; Angela D. Follett; Kristopher McNeill; Inorganic Chemistry 49 (2010) 3942–3949; doi:10.1021/ic1003325

data_4315350
_publ_section_title
;
 Synthesis and Characterization of Pentaphosphino Zero-Valent Iron
 Complexes and Their Corresponding Iron(II)-Chloride and -Hydride
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3942
_journal_page_last               3949
_journal_paper_doi               10.1021/ic1003325
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C15 H40 Fe P5'
_chemical_formula_sum            'C15 H40 Fe P5'
_chemical_formula_weight         431.17
_chemical_name_common            (dmpe)5Fe2
_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                101.020(2)
_cell_angle_beta                 98.323(2)
_cell_angle_gamma                113.373(2)
_cell_formula_units_Z            2
_cell_length_a                   9.075(1)
_cell_length_b                   9.224(1)
_cell_length_c                   15.328(2)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.50
_cell_volume                     1120.9(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scan per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12929
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.827760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0327P)^2^+0.3290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                4053
_reflns_number_total             4986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1003325_si_002_5.cif
_cod_data_source_block           06056m
_cod_database_code               4315350