Terminal vs Bridging Hydrides of Diiron Dithiolates: Protonation of Fe2(dithiolate)(CO)2(PMe3)4
Riccardo Zaffaroni; Thomas B. Rauchfuss; Danielle L. Gray; Luca De Gioia; Giuseppe Zampella; Journal of the American Chemical Society 134 (2012) 19260–19269; doi:10.1021/ja3094394

data_4118920
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       dgray@illinois.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Terminal vs Bridging Hydrides of Diiron Dithiolates: Protonation of
 Fe2(dithiolate)(CO)2(PMe3)4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19260
_journal_page_last               19269
_journal_paper_doi               10.1021/ja3094394
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C17 H42 Fe2 O2 P4 S2, 1.5(C5 H12)'
_chemical_formula_sum            'C24.5 H60 Fe2 O2 P4 S2'
_chemical_formula_weight         686.43
_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
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.131(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.4446(16)
_cell_length_b                   32.134(4)
_cell_length_c                   16.0011(19)
_cell_measurement_reflns_used    9668
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.91
_cell_measurement_theta_min      2.29
_cell_volume                     6911.6(14)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \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  bm54tasq
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            74431
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  0.9608
_exptl_absorpt_correction_T_min  0.7822
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             2936
_exptl_crystal_id                bm54tasq
_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 0 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.034
_platon_squeeze_details
; 
The squeezed electron count is consistant with 11.5 pentane molecules 
in the unit cell.  This is half of a molecule less than that predicted 
by the disordered model. 
;
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         12625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                9098
_reflns_number_total             12625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3094394_si_002_2.cif
_cod_data_source_block           bm54tasq
_cod_original_cell_volume        6911.7(14)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C24.50 H60 Fe2 O2 P4 S2'
_cod_database_code               4118920