Precursors to [FeFe]-Hydrogenase Models: Syntheses of Fe2(SR)2(CO)6 from CO-Free Iron Sources
Phillip I. Volkers; Christine A. Boyke; Jinzhu Chen; Thomas B. Rauchfuss; C. Matthew Whaley; Scott R. Wilson; Haijun Yao; Inorganic Chemistry 47 (2008) 7002–7008; doi:10.1021/ic800601k

data_4305628
_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
;
Precursors to [FeFe]-Hydrogenase Models: Syntheses of Fe2(SR)2(CO)6 from
CO-Free Iron Sources
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7002
_journal_page_last               7008
_journal_paper_doi               10.1021/ic800601k
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
; 
2(C16 H24 Fe3 O4 S8), 3(C4 H8 O), 2(C25 H22 P) 
;
_chemical_formula_sum            'C94 H116 Fe6 O11 P2 S16'
_chemical_formula_weight         2331.87
_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
; 
2006-12-19   text and data added, piv 
;
_cell_angle_alpha                72.961(6)
_cell_angle_beta                 80.745(7)
_cell_angle_gamma                65.861(6)
_cell_formula_units_Z            1
_cell_length_a                   12.409(5)
_cell_length_b                   14.658(5)
_cell_length_c                   16.276(6)
_cell_measurement_reflns_used    928
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      19.18
_cell_measurement_theta_min      2.28
_cell_volume                     2580.1(17)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  g59oas
_diffrn_reflns_av_R_equivalents  0.1772
_diffrn_reflns_av_sigmaI/netI    0.2791
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24749
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        25.2
_diffrn_standards_interval_time  305
_diffrn_standards_number         19
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.9647
_exptl_absorpt_correction_T_min  0.6910
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1210
_exptl_crystal_id                g59oas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2 -1 -6) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         9454
_refine_ls_number_restraints     575
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.2241
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                3396
_reflns_number_total             9454
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4305625
_cod_data_source_file            ic800601k-file003_2.cif
_cod_data_source_block           g59oas
_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_cell_volume        2580.2(16)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4305628