All-iron hydrogenase: synthesis, structure and properties of {2Fe3S}-assemblies related to the di-iron sub-site of the H-clusterElectronic supplementary information (ESI) available: crystal and structure refinement data for complexes 4a, 4b and 5a. See http://www.rsc.org/suppdata/dt/b2/b209690k/
Razavet, Mathieu; Davies, Sian C.; Hughes, David L.; Barclay, J. Elaine; Evans, David J.; Fairhurst, Shirley A.; Liu, Xiaoming; Pickett, Christopher J.; Dalton Transactions  (2003) 586–; doi:10.1039/b209690k

data_7012293
_publ_section_title
;
 All-iron hydrogenase: synthesis, structure and properties of
 {2Fe3S}-assemblies related to the di-iron sub-site of the
 H-clusterElectronic supplementary information (ESI) available: crystal
 and structure refinement data for complexes 4a, 4b and 5a. See
 http://www.rsc.org/suppdata/dt/b2/b209690k/
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              586
_journal_paper_doi               10.1039/b209690k
_journal_year                    2003
_chemical_formula_moiety         'C8 H20 N, C11 H12 Fe2 N O4 S3'
_chemical_formula_structural     (NEt4)[Fe2(CO)4(CN){MeCH2C(Me)(CH2S)2}]
_chemical_formula_sum            'C19 H32 Fe2 N2 O4 S3'
_chemical_formula_weight         560.35
_chemical_name_common            'Compound 5a'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                85.87(2)
_cell_angle_beta                 78.327(13)
_cell_angle_gamma                77.90(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2990(14)
_cell_length_b                   9.357(4)
_cell_length_c                   16.534(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    140(1)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1228.9(6)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; \w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7586
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        4.4
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_absorpt_process_details   'EMPABS, Sheldrick et al, 1977)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             584
_exptl_crystal_size_max          'ca 0.5'
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         7138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.6394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                5512
_reflns_number_total             7138
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b209690k.txt
_cod_data_source_block           math7
_cod_original_cell_volume        1228.8(6)
_cod_database_code               7012293