Diiron Dithiolato Carbonyls Related to the HoxCO State of [FeFe]-Hydrogenase
Aaron K. Justice; Mark J. Nilges; Thomas B. Rauchfuss; Scott R. Wilson; Luca De Gioia; Giuseppe Zampella; Journal of the American Chemical Society 130 (2008) 5293–5301; doi:10.1021/ja7113008

data_4107693
_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
;
 Diiron Dithiolato Carbonyls Related to the HoxCO State of
 [FeFe]-Hydrogenase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5293
_journal_page_last               5301
_journal_paper_doi               10.1021/ja7113008
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety
; 
C57 H48 Fe2 O3 P4 S2, F6 P, 3(C H2 Cl2) 
;
_chemical_formula_sum            'C60 H54 Cl6 F6 Fe2 O3 P5 S2'
_chemical_formula_weight         1480.40
_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
; 
2007-08-23   text and data added, akj 
;
_cell_angle_alpha                88.476(6)
_cell_angle_beta                 74.783(5)
_cell_angle_gamma                86.220(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5296(9)
_cell_length_b                   16.4228(14)
_cell_length_c                   19.2603(16)
_cell_measurement_reflns_used    5807
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.30
_cell_volume                     3206.7(5)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2001)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction        'SAINT V7.23A(Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_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  ga74qasi
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38551
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.9271
_exptl_absorpt_correction_T_min  0.8499
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       prism
_exptl_crystal_F_000             1506
_exptl_crystal_id                ga74qasi
_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 5) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         12128
_refine_ls_number_restraints     562
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1249P)^2^+6.6757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2573
_reflns_number_gt                7022
_reflns_number_total             12128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7113008-file001_2.cif
_cod_data_source_block           ga74qasi
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4107693