Isolation of a Mixed Valence Diiron Hydride: Evidence for a Spectator Hydride in Hydrogen Evolution Catalysis
Wenguang Wang; Mark J. Nilges; Thomas B. Rauchfuss; Matthias Stein; Journal of the American Chemical Society 135 (2013) 3633–3639; doi:10.1021/ja312458f

data_4119418
_publ_section_title
;
 Isolation of a Mixed Valence Diiron Hydride: Evidence for a Spectator
 Hydride in Hydrogen Evolution Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3633
_journal_page_last               3639
_journal_paper_doi               10.1021/ja312458f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C57 H51 Fe2 O2 P4 S2'
_chemical_formula_sum            'C57 H51 Fe2 O2 P4 S2'
_chemical_formula_weight         1067.68
_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
; 
? 
;
_cell_angle_alpha                77.7120(10)
_cell_angle_beta                 74.3210(10)
_cell_angle_gamma                67.3880(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7211(13)
_cell_length_b                   11.9110(13)
_cell_length_c                   20.406(2)
_cell_measurement_reflns_used    6926
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.25
_cell_volume                     2512.9(5)
_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      178(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  bm39uas
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30168
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.9446
_exptl_absorpt_correction_T_min  0.9063
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             1106
_exptl_crystal_id                bm39uas
_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 2 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         10339
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0314P)^2^+1.0399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                8026
_reflns_number_total             10339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja312458f_si_002.cif
_cod_data_source_block           bm39uas
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4119418