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_4327388
_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 H22 Fe2 N O7 P2, B F4'
_chemical_formula_sum            'C23 H22 B F4 Fe2 N O7 P2'
_chemical_formula_weight         684.87
_chemical_name_common            km2403
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-08-17T12:14:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.1670
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9407(3)
_cell_length_b                   30.1453(10)
_cell_length_c                   11.2557(3)
_cell_measurement_reflns_used    160435
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.19
_cell_volume                     2809.42(15)
_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 19'
_computing_molecular_graphics    'WINGX (Farrugia (1997)'
_computing_publication_material  'WINGX (Farrugia (1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method
'CCD rotation images, thick slice \f & \w scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.66452E-2
_diffrn_orient_matrix_UB_12      0.61969E-2
_diffrn_orient_matrix_UB_13      0.851513E-1
_diffrn_orient_matrix_UB_21      0.720631E-1
_diffrn_orient_matrix_UB_22      0.263325E-1
_diffrn_orient_matrix_UB_23      0.111392E-1
_diffrn_orient_matrix_UB_31      -0.966913E-1
_diffrn_orient_matrix_UB_32      0.191995E-1
_diffrn_orient_matrix_UB_33      -0.427617E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.044
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            36940
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
 Final data set contains 5548 Friedel pairs
;
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  0.8881
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SORTAV option in WINGX (Farrugia, 1997)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         12131
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0272P)^2^+1.5644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                10704
_reflns_number_total             12131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0487722Bsi20040902_034532_1.cif
_cod_data_source_block           4
_cod_original_cell_volume        2809.41(15)
_cod_database_code               4327388