Chelate Control of Diiron(I) Dithiolates Relevant to the [Fe-Fe]- Hydrogenase Active Site
Aaron K. Justice; Giuseppe Zampella; Luca De Gioia; Thomas B. Rauchfuss; Jarl Ivar van der Vlugt; Scott R. Wilson; Inorganic Chemistry 46 (2007) 1655–1664; doi:10.1021/ic0618706

data_4307331
_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
;
Chelate Control of Diiron(I) Dithiolates Relevant to the [Fe-Fe]-
Hydrogenase Active Site
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1655
_journal_page_last               1664
_journal_paper_doi               10.1021/ic0618706
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
; 
C32 H26 Fe2 N O3 P2 S2, C8 H20 N, C H2 Cl2 
;
_chemical_formula_sum            'C41 H48 Cl2 Fe2 N2 O3 P2 S2'
_chemical_formula_weight         925.47
_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
; 
2006-08-31   text and data added, akj 
;
_cell_angle_alpha                88.297(10)
_cell_angle_beta                 74.230(10)
_cell_angle_gamma                66.601(9)
_cell_formula_units_Z            2
_cell_length_a                   11.219(7)
_cell_length_b                   11.505(7)
_cell_length_c                   18.994(12)
_cell_measurement_reflns_used    968
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.3
_cell_volume                     2157(2)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  g12ias
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18473
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  313
_diffrn_standards_number         313
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.8773
_exptl_absorpt_correction_T_min  0.5901
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             960
_exptl_crystal_id                g12ias
_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 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7884
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                5846
_reflns_number_total             7884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0618706si20060928_102657.cif
_cod_data_source_block           g12ias
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4307331