Diiron species containing a cyclic PPh2NPh2 diphosphine related to the [FeFe]H2ases active site
Sondes Lounissi; Jean-Francois Capon; Frederic Gloaguen; Fatma Matoussi; Francois Petillon; Philippe Schollhammer; Jean Talarmin; Chem.Commun. 47 (2011) 878–; doi:10.1039/c0cc03295f

data_7105845
_publ_section_title
;
 Diiron species containing a cyclic PPh2NPh2 diphosphine related to the
 [FeFe]H2ases active site
;
_journal_name_full               Chem.Commun.
_journal_page_first              878
_journal_paper_doi               10.1039/c0cc03295f
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C36 H34 Fe2 N2 O5 P2 S3, C H2 Cl2'
_chemical_formula_sum            'C37 H36 Cl2 Fe2 N2 O5 P2 S3'
_chemical_formula_weight         929.4
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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_date             2010-08-05T17:14:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.263(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7119(8)
_cell_length_b                   12.2358(5)
_cell_length_c                   19.4661(10)
_cell_measurement_reflns_used    5372
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      22.8
_cell_measurement_theta_min      2.88
_cell_volume                     3969.5(3)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1980-2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method
;
4 stepped omega-scans over 115 deg. with kappa -79 deg. (chi -58.3 deg.),
phi 0, 90, 180, 270 deg.
step 1 deg., exposure time 60 s
detector distance 50 mm
detector angle 30 deg.
;
_diffrn_orient_matrix_UB_11      0.0424386577
_diffrn_orient_matrix_UB_12      0.0023602207
_diffrn_orient_matrix_UB_13      0.0051478118
_diffrn_orient_matrix_UB_21      -0.0028658433
_diffrn_orient_matrix_UB_22      0.0003490606
_diffrn_orient_matrix_UB_23      0.0361704545
_diffrn_orient_matrix_UB_31      0.001679204
_diffrn_orient_matrix_UB_32      -0.0579113045
_diffrn_orient_matrix_UB_33      0.0004220773
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29973
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
        fragment of planar crystal, main faces {1 0 0}
;
_exptl_crystal_F_000             1904
_exptl_crystal_recrystallization_method
'Slow evaporation of dichloromethane solution'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8080
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.051
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                4527
_reflns_number_total             8080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03295F.TXT
_cod_data_source_block           sl95-a0
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7105845