Mixed-Valence Nickel-Iron Dithiolate Models of the [NiFe]-Hydrogenase Active Site
David Schilter; Mark J. Nilges; Mrinmoy Chakrabarti; Paul A. Lindahl; Thomas B. Rauchfuss; Matthias Stein; Inorganic Chemistry 51 (2012) 2338–2348; doi:10.1021/ic202329y

data_4328377
_publ_section_title
;
 Mixed-Valence Nickel-Iron Dithiolate Models of the [NiFe]-Hydrogenase
 Active Site
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2338
_journal_page_last               2348
_journal_paper_doi               10.1021/ic202329y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C32 H54 Fe Ni O3 P2 S2, 2(C H2 Cl2), B F4 '
_chemical_formula_sum            'C34 H58 B Cl4 F4 Fe Ni O3 P2 S2'
_chemical_formula_weight         984.03
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.840(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.680(2)
_cell_length_b                   15.715(2)
_cell_length_c                   17.193(2)
_cell_measurement_reflns_used    3591
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.01
_cell_measurement_theta_min      2.37
_cell_volume                     4501.2(9)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm53nas
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36785
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.9402
_exptl_absorpt_correction_T_min  0.7292
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             2044
_exptl_crystal_id                bm53nas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 -1 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8246
_refine_ls_number_restraints     476
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0495P)^2^+1.9360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                4865
_reflns_number_total             8246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202329y_si_002_1.cif
_cod_data_source_block           bm53nas
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4328377