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_4107692
_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
; 
2(C57 H48 Fe2 O3 P4 S2), 9(C H2 Cl2), 2(B F4) 
;
_chemical_formula_sum            'C123 H114 B2 Cl18 F8 Fe4 O6 P8 S4'
_chemical_formula_weight         3099.26
_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
; 
2006-10-06  text and data added, akj 
;
_cell_angle_alpha                97.618(9)
_cell_angle_beta                 94.054(9)
_cell_angle_gamma                100.371(9)
_cell_formula_units_Z            1
_cell_length_a                   10.614(6)
_cell_length_b                   15.276(9)
_cell_length_c                   22.765(13)
_cell_measurement_reflns_used    942
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      2.43
_cell_volume                     3582(4)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  g99mas
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36978
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time  306
_diffrn_standards_number         145
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.8401
_exptl_absorpt_correction_T_min  0.5361
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1576
_exptl_crystal_id                g99mas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 -1 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         13040
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1191P)^2^+4.2884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1936
_reflns_number_gt                9577
_reflns_number_total             13040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7113008-file001_1.cif
_cod_data_source_block           g99mas
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4107692