A Functional [NiFe]-Hydrogenase Model Compound That Undergoes Biologically Relevant Reversible Thiolate Protonation
Katharina Weber; Tobias Krämer; Hannah S. Shafaat; Thomas Weyhermüller; Eckhard Bill; Maurice van Gastel; Frank Neese; Wolfgang Lubitz; Journal of the American Chemical Society 134 (2012) 20745–20755; doi:10.1021/ja309563p

data_4119045
_publ_section_title
;
 A Functional [NiFe]-Hydrogenase Model Compound That Undergoes
 Biologically Relevant Reversible Thiolate Protonation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20745
_journal_page_last               20755
_journal_paper_doi               10.1021/ja309563p
_journal_volume                  134
_journal_year                    2012
_chemical_compound_source        'dichloromethane, diethylether'
_chemical_formula_moiety         'C17 H19 Fe Ni O3 S4, 0.5(C4 H10 O)'
_chemical_formula_sum            'C21 H29 Fe Ni O3.5 S4'
_chemical_formula_weight         580.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                LBZ-WK-210-01
_audit_creation_date             2012-03-27
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.484(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3219(11)
_cell_length_b                   17.114(2)
_cell_length_c                   13.8157(14)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.1273
_cell_measurement_theta_min      2.3802
_cell_volume                     2436.0(5)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            84677
_diffrn_reflns_theta_full        34.19
_diffrn_reflns_theta_max         34.19
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.92490
_exptl_absorpt_correction_T_min  0.71745
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       prism
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         10058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0264P)^2^+0.8655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                8688
_reflns_number_total             10058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309563p_si_003.cif
_cod_data_source_block           7754
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C21 H29 Fe Ni O3.50 S4'
_cod_database_code               4119045