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_4104422
_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
;
 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_formula_moiety
'2(C32 H31 Fe Ni O3 P2 S2), 5(C4 H8 O), 2(B F4) '
_chemical_formula_sum            'C84 H102 B2 F8 Fe2 Ni2 O11 P4 S4'
_chemical_formula_weight         1942.52
_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                74.482(5)
_cell_angle_beta                 84.864(4)
_cell_angle_gamma                77.498(4)
_cell_formula_units_Z            1
_cell_length_a                   9.8894(7)
_cell_length_b                   11.6430(8)
_cell_length_c                   20.6688(15)
_cell_measurement_reflns_used    1985
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.53
_cell_measurement_theta_min      2.31
_cell_volume                     2237.5(3)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  ba67eas
_diffrn_reflns_av_R_equivalents  0.1563
_diffrn_reflns_av_sigmaI/netI    0.2224
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35151
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1008
_exptl_crystal_id                ba67eas
_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 1 -4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         8363
_refine_ls_number_restraints     532
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.2166
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0701P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1780
_reflns_number_gt                3378
_reflns_number_total             8363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902570u_si_002_2.cif
_cod_data_source_block           ba67eas
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4104422