Di-Iron Aza Diphosphido Complexes: Mimics for the Active Site of Fe-Only Hydrogenase, and Effects of Changing the Coordinating Atoms of the Bridging Ligand in [Fe2{μ-(ECH2)2NR}(CO)6]
Pankaj Das; Jean-François Capon; Frédéric Gloaguen; François Y. Pétillon; Philippe Schollhammer; Jean Talarmin; Kenneth W. Muir; Inorganic Chemistry 43 (2004) 8203–8205; doi:10.1021/ic048772+

data_4327389
_publ_contact_author             'Muir, Kenneth W.'
_publ_contact_author_email       ken@chem.gla.ac.uk
_publ_section_title
;
 Di-Iron Aza Diphosphido Complexes: Mimics for the Active Site of Fe-Only
 Hydrogenase, and Effects of Changing the Coordinating Atoms of the
 Bridging Ligand in [Fe2{\m-(ECH2)2NR}(CO)6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8203
_journal_page_last               8205
_journal_paper_doi               10.1021/ic048772+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C23 H21 Fe2 N1 O7 P2'
_chemical_formula_sum            'C23 H21 Fe2 N O7 P2'
_chemical_formula_weight         597.05
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2b'
_symmetry_space_group_name_H-M   'P b n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-08-17T12:09:08-00:00
_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                   7.96470(10)
_cell_length_b                   20.44020
_cell_length_c                   31.0173(3)
_cell_measurement_reflns_used    6519
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0
_cell_volume                     5049.62(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38080
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
        empirical multi-scan correction gave
        a very slightly poorer result
        R1 0.435 Rw 0.0729 Max peak & hole 0.55 & -0.30 eA**3
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       needle
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.27
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0379P)^2^+2.8721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.072
_reflns_number_gt                5021
_reflns_number_total             6077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0487722Bsi20040902_034532_2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_Hall     '-P 2n 2ab'
_cod_database_code               4327389