Influence of a Pendant Amine in the Second Coordination Sphere on Proton Transfer at a Dissymmetrically Disubstituted Diiron System Related to the [2Fe]H Subsite of [FeFe]H2ase
Salah Ezzaher; Jean-François Capon; Frédéric Gloaguen; François Y. Pétillon; Philippe Schollhammer; Jean Talarmin; Nelly Kervarec; Inorganic Chemistry 48 (2009) 2–4; doi:10.1021/ic801369u

data_4301091
_publ_contact_author_address
;Laboratoire de chimie,
electrochimie moleculaire et chimie analytique (UMR 6521)
Universite de Bretagne occidentale
6, avenue Victor Le Gorgeu
CS 93837
F-29238 BREST cedex 3
FRANCE 
;
_publ_contact_author_email       philippe.schollhammer@univ-brest.fr
_publ_contact_author_name        'Schollhammer, Philippe'
_publ_section_title
;
Influence of a Pendant Amine in the Second Coordination Sphere on Proton
Transfer at a Dissymmetrically Disubstituted Diiron System Related to the
[2Fe]H Subsite of [FeFe]H2ase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2
_journal_page_last               4
_journal_paper_doi               10.1021/ic801369u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
;
        C34 H34 Fe2 N O4 P2 S2 1+, B F4 1-, 2(C3 H6 O)
;
_chemical_formula_sum            'C40 H46 B F4 Fe2 N O6 P2 S2'
_chemical_formula_weight         961.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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             2008-04-22T12:31:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.255(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.0169(15)
_cell_length_b                   11.4623(4)
_cell_length_c                   20.7172(10)
_cell_measurement_reflns_used    6284
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      2.1
_cell_volume                     8699.2(6)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_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 0.88
_diffrn_measured_fraction_theta_max 0.88
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR2'
_diffrn_measurement_method
;
        1 stepped phi-scan over 360 deg with detector angle 30 deg.
1 stepped omega-scans over 106 deg. with kappa -79 deg. (chi -58.3 deg.)
        and detector angle 0
        step 1 deg., exposure time 240 s
        detector distance 50 mm
;
_diffrn_orient_matrix_UB_11      -0.0095545481
_diffrn_orient_matrix_UB_12      -0.0525503924
_diffrn_orient_matrix_UB_13      -0.008825649
_diffrn_orient_matrix_UB_21      0.0162148284
_diffrn_orient_matrix_UB_22      -0.0323172342
_diffrn_orient_matrix_UB_23      0.0096868112
_diffrn_orient_matrix_UB_31      -0.0045437303
_diffrn_orient_matrix_UB_32      -0.0047390625
_diffrn_orient_matrix_UB_33      0.0320065511
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25334
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
truncated lozenge, main faces {1 0 0}, diagonals [0 1 0] and [0 0 1]
;
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         5501
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.06
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                3931
_reflns_number_total             5501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801369u_si_002_2.cif
_cod_data_source_block           sez18-a-compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4301091