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_4305627
_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         'C25 H48 Fe3 O4 P2 S6'
_chemical_formula_sum            'C25 H48 Fe3 O4 P2 S6'
_chemical_formula_weight         834.48
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2008-08-27   text and data added, srw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.939(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.243(3)
_cell_length_b                   11.4089(18)
_cell_length_c                   18.414(3)
_cell_measurement_reflns_used    2534
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      21.62
_cell_measurement_theta_min      2.96
_cell_volume                     3617.7(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  ga33gas
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0893
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31532
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.651
_exptl_absorpt_correction_T_max  0.94207
_exptl_absorpt_correction_T_min  0.87607
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_id                ga33gas
_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          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6883
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+3.1736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                4345
_reflns_number_total             6883
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4305626
_cod_data_source_file            ic800601k-file003_1.cif
_cod_data_source_block           ga33gas
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        3617.8(10)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4305627