Hydride-Containing Models for the Active Site of the Nickel-Iron Hydrogenases
Bryan E. Barton; Thomas B. Rauchfuss; Journal of the American Chemical Society 132 (2010) 14877–14885; doi:10.1021/ja105312p

data_4103346
_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
;
 Hydride-Containing Models for the Active Site of the Nickel-Iron
 Hydrogenases
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14877
_journal_page_last               14885
_journal_paper_doi               10.1021/ja105312p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C49 H46 Fe Ni O2 P3 S2, C H2 Cl2, B F4'
_chemical_formula_sum            'C50 H48 B Cl2 F4 Fe Ni O2 P3 S2'
_chemical_formula_weight         1110.18
_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                109.5356(18)
_cell_angle_beta                 100.808(2)
_cell_angle_gamma                91.254(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4707(4)
_cell_length_b                   12.6792(4)
_cell_length_c                   16.9635(5)
_cell_measurement_reflns_used    4066
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.35
_cell_volume                     2472.61(14)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, 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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ba06fas
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30274
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.8366
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_id                ba06fas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research)with the (-2 -2 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         9027
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0340P)^2^+0.8592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                6031
_reflns_number_total             9027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105312p_si_002.cif
_cod_data_source_block           ba06fas
_cod_original_cell_volume        2472.60(13)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4103346