Active-Site Models for the Nickel-Iron Hydrogenases: Effects of Ligands on Reactivity and Catalytic Properties
Maria E. Carroll; Bryan E. Barton; Danielle L. Gray; Amanda E. Mack; Thomas B. Rauchfuss; Inorganic Chemistry 50 (2011) 9554–9563; doi:10.1021/ic2012759

data_4326374
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       dgray@illinois.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Active-Site Models for the Nickel-Iron Hydrogenases: Effects of Ligands
 on Reactivity and Catalytic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9554
_journal_page_last               9563
_journal_paper_doi               10.1021/ic2012759
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C31 H34 Fe I2 Ni P2 S2, 0.5(C6 H14)'
_chemical_formula_sum            'C37 H52 Fe I2 Ni P2 S2'
_chemical_formula_weight         991.21
_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                76.220(3)
_cell_angle_beta                 83.195(3)
_cell_angle_gamma                89.252(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7463(4)
_cell_length_b                   13.3510(5)
_cell_length_c                   13.4828(6)
_cell_measurement_reflns_used    5093
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      67.79
_cell_measurement_theta_min      3.40
_cell_volume                     1865.29(13)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  bc79oasq
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11815
_diffrn_reflns_theta_full        68.27
_diffrn_reflns_theta_max         68.27
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    18.788
_exptl_absorpt_correction_T_max  0.3762
_exptl_absorpt_correction_T_min  0.0712
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_id                bc79oasq
_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 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.074
_platon_squeeze_details
; 
The positions for the hexane solvate molecule was poorly determined 
so it was "squeezed" from the structure.  The electron count from the 
"squeeze" model converged in good agreement with 1/2 of a hexane per 
asymetric unit or 1 total hexane per unit cell as predicted by the 
original refinement. 
;
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         6177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                5386
_reflns_number_total             6177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012759_si_002_5.cif
_cod_data_source_block           bc79oasq
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4326374