Redox active iron nitrosyl units in proton reduction electrocatalysis
Hsieh, Chung-Hung; Ding, Shengda; Erdem, Ozlen F.; Crouthers, Danielle J.; Liu, Tianbiao; McCrory, Charles C. L.; Lubitz, Wolfgang; Popescu, Codrina V.; Reibenspies, Joseph H.; Hall, Michael B.; Darenbourg, Marcetta Y.; Nature Communications 5 (2014) 3684–; doi:10.1038/ncomms4684

data_1547478
_publ_section_title
;
 Redox active iron nitrosyl units in proton reduction electrocatalysis
;
_journal_name_full               'Nature Communications'
_journal_page_first              3684
_journal_paper_doi               10.1038/ncomms4684
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C9 H18 Fe2 N5 O3 S2'
_chemical_formula_weight         420.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.240(7)
_cell_length_b                   14.263(7)
_cell_length_c                   14.821(7)
_cell_measurement_reflns_used    7783
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.44
_cell_volume                     3010(3)
_computing_cell_refinement       'APEXII (Bruker, 2012a)'
_computing_data_collection       'APEXII (Bruker, 2012a)'
_computing_data_reduction        'SAINT (Bruker, 2012b)'
_computing_molecular_graphics    'shelXLe (H\"ubschle 2011)'
_computing_publication_material  'Ciftab (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32153
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.444
_exptl_absorpt_coefficient_mu    2.220
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2009) was employed for absorption correction.
wR2(int) was   0.1108 before and   0.0733 after correction.
The ratio of minimum to maximum transmission factors was   0.8082.
Additional spherical absorption correction applied with mu*r =  0.2000.
The \l/2 correction factor of 0.0015 was applied.
;
_exptl_crystal_colour            'dark green '
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       'plate     '
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+3.0424P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2853
_reflns_number_total             3470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms4684-s2.cif
_cod_data_source_block           fefe
_cod_database_code               1547478
_shelx_estimated_absorpt_t_min   0.665
_shelx_estimated_absorpt_t_max   0.808
_shelxl_version_number           2013-2
_shelx_res_checksum              88550
_shelx_hkl_checksum              30215