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_4328378
_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         'C57 H54 Fe Ni O2 P4 S2, 2(B F4), 4(CH2Cl2)'
_chemical_formula_sum            'C61 H62 B2 Cl8 F8 Fe Ni O2 P4 S2'
_chemical_formula_weight         1586.89
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                78.9850(10)
_cell_angle_beta                 75.0720(10)
_cell_angle_gamma                64.2600(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4045(3)
_cell_length_b                   14.1949(4)
_cell_length_c                   21.2882(5)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.29
_cell_volume                     3510.93(15)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \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  bm63nasq
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52991
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.9247
_exptl_absorpt_correction_T_min  0.8252
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_id                bm63nasq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 0 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.108
_platon_squeeze_details
; 
The electron count from the "squeeze" model converged in good agreement 
with the four methylene chloride solvent molecules predicted by the complete 
refinement. 
;
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         12834
_refine_ls_number_restraints     548
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0558P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1126
_reflns_number_gt                8867
_reflns_number_total             12834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202329y_si_002_2.cif
_cod_data_source_block           bm63nasq
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4328378