Synthesis and Structure of Analogues for the Ni-Fe Site in Hydrogenase Enzymes
Jianfeng Jiang; Myriam Maruani; Jonathan Solaimanzadeh; Wenfeng Lo; Stephen A. Koch; Michelle Millar; Inorganic Chemistry 48 (2009) 6359–6361; doi:10.1021/ic900929u

data_4302785
_publ_section_title
;
Synthesis and Structure of Analogues for the Ni-Fe Site in Hydrogenase
Enzymes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6359
_journal_page_last               6361
_journal_paper_doi               10.1021/ic900929u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C36.42 H34 Fe N2 Ni O2 P2 S2'
_chemical_formula_weight         772.28
_chemical_name_common            '[(dppe)Ni(u-SEt)2Fe(CN)2(CO)2]6'
_chemical_name_systematic
'diphos nickel bis ethanethiolate iron dicyanide dicarbonyl'
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      173
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   25.793(5)
_cell_length_b                   25.793(5)
_cell_length_c                   22.672(9)
_cell_measurement_reflns_used    5053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.86
_cell_measurement_theta_min      2.39
_cell_volume                     13062(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11344
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             4782
_exptl_crystal_recrystallization_method 'CH2Cl2 ether'
_exptl_crystal_size_max          .12
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         5848
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.618
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1747
_reflns_number_gt                2985
_reflns_number_total             5848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900929u_si_002_2.cif
_cod_data_source_block           '[(dppe)Ni(u-SEt)2Fe(CN)2(CO)2]'
_cod_original_cell_volume        13063(6)
_cod_database_code               4302785