Role of the Azadithiolate Cofactor in Models for [FeFe]-Hydrogenase: Novel Structures and Catalytic Implications
Matthew T. Olsen; Thomas B. Rauchfuss; Scott R. Wilson; Journal of the American Chemical Society 132 (2010) 17733–17740; doi:10.1021/ja103998v

data_4103694
_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
;
 Role of the Azadithiolate Cofactor in Models for [FeFe]-Hydrogenase:
 Novel Structures and Catalytic Implications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17733
_journal_page_last               17740
_journal_paper_doi               10.1021/ja103998v
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'C43 H45 Fe2 N2 O3 P3 S2, 2(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C45 H49 B2 Cl4 F8 Fe2 N2 O3 P3 S2'
_chemical_formula_weight         1250.01
_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
; 
2008-09-19   text and data added, mto 
;
_cell_angle_alpha                77.934(7)
_cell_angle_beta                 72.938(7)
_cell_angle_gamma                69.865(7)
_cell_formula_units_Z            2
_cell_length_a                   11.9738(13)
_cell_length_b                   13.2467(15)
_cell_length_c                   19.321(2)
_cell_measurement_reflns_used    1117
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      16.94
_cell_measurement_theta_min      2.22
_cell_volume                     2730.6(5)
_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 (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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  ba79cas
_diffrn_reflns_av_R_equivalents  0.2437
_diffrn_reflns_av_sigmaI/netI    0.3853
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30921
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.8015
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1272
_exptl_crystal_id                ba79cas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-3 0 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9961
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.2969
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.2443
_reflns_number_gt                3056
_reflns_number_total             9961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103998v_si_002.cif
_cod_data_source_block           ba79cas
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4103694