Nickel-Iron Dithiolato Hydrides Relevant to the [NiFe]-Hydrogenase Active Site
Bryan E. Barton; C. Matthew Whaley; Thomas B. Rauchfuss; Danielle L. Gray; Journal of the American Chemical Society 131 (2009) 6942–6943; doi:10.1021/ja902570u

data_4104421
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Nickel-Iron Dithiolato Hydrides Relevant to the [NiFe]-Hydrogenase Active
 Site
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6942
_journal_page_last               6943
_journal_paper_doi               10.1021/ja902570u
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C56 H54 Cl Fe Ni O P4 S2, C H2 Cl2, B F4'
_chemical_formula_sum            'C57 H56 B Cl3 F4 Fe Ni O P4 S2'
_chemical_formula_weight         1252.74
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2008-01-29   text and data added, cmw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.473(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9468(10)
_cell_length_b                   10.5250(8)
_cell_length_c                   20.5386(18)
_cell_measurement_reflns_used    3967
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.15
_cell_measurement_theta_min      2.50
_cell_volume                     2793.6(4)
_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, TWINABS V2007/5 (Bruker, 2005 & 2007) 
;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  ga56x1as5
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13581
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.9232
_exptl_absorpt_correction_T_min  0.8672
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1288
_exptl_crystal_id                ga56x1as5
_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 -2 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack (1983),  8007 Friedels'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         13580
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+1.2820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                10755
_reflns_number_total             13580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902570u_si_002_1.cif
_cod_data_source_block           ga56x1as5
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               4104421