Protonation Studies of the New Iron Carbonyl Cyanidetrans-[Fe(CO)3(CN)2]2-: Implications with Respect to Hydrogenases
Ajay Kayal; Thomas B. Rauchfuss; Inorganic Chemistry 42 (2003) 5046–5048; doi:10.1021/ic034455b

data_4314109
_publ_contact_author_address
;
Department of Chemistry
University of Illinois at Urbana-Champaign
600 South Matthews Avenue
Urbana
IL 61801
USA
;
_publ_contact_author_email       rauchfuz@uiuc.edu
_publ_contact_author_fax         '1 217 333 2685'
_publ_contact_author_name        'Prof. Thomas B. Rauchfuss'
_publ_contact_author_phone       '1 217 333 7355'
_publ_section_title
;
 Protonation Studies of the New Iron Carbonyl
 Cyanidetrans-[Fe(CO)3(CN)2]2-: Implications with Respect to Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5046
_journal_page_last               5048
_journal_paper_doi               10.1021/ic034455b
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '2 (C8 H20 N), C5 Fe N2 O3'
_chemical_formula_sum            'C21 H40 Fe N4 O3'
_chemical_formula_weight         452.42
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.429(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.775(4)
_cell_length_b                   15.764(7)
_cell_length_c                   16.184(7)
_cell_measurement_reflns_used    958
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.87
_cell_volume                     2493.8(19)
_computing_cell_refinement       'SAINT V6 (BRUKER, 2001)'
_computing_data_collection       'SMART V5 (BRUKER, 1998)'
_computing_data_reduction        'SAINT V6 (BRUKER, 2001)'
_computing_molecular_graphics    'SHELXTL v6 (Bruker, 2000)'
_computing_publication_material  'SHELXTL v6 (Bruker, 2000)'
_computing_structure_refinement  'SHELXTL v6 (Bruker, 2000)'
_computing_structure_solution    'SHELXTL v6 (Bruker, 2000)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32623
_diffrn_reflns_theta_full        28.76
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.8432
_exptl_absorpt_correction_T_min  0.8001
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0535P)^2^+0.5041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                5162
_reflns_number_total             6425
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic034455bsi20030430_021454.cif
_cod_data_source_block           global
_cod_original_cell_volume        2493.7(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4314109