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_4302786
_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_moiety         'C33 H30 Fe N2 Ni1 O2 P2 S2'
_chemical_formula_sum            'C33 H30 Fe N2 Ni O2 P2 S2'
_chemical_formula_weight         727.21
_chemical_name_common            (dppe)Ni(pdt)Fe(CN)2(CO)2]
_chemical_name_systematic
'diphos Nickel 1,3-propanedithiolate Iron dicyanide dicarbonyl'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 113.1660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.8950(12)
_cell_length_b                   20.1718(13)
_cell_length_c                   19.5362(13)
_cell_measurement_temperature    100(2)
_cell_volume                     6483.5(7)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77927
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.31
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_recrystallization_method 'CH2Cl2 ether'
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .15
_refine_diff_density_max         2.155
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         15789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+11.7161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                13453
_reflns_number_total             15789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900929u_si_002_3.cif
_cod_data_source_block           (dppe)Ni(pdt)Fe(CN)2(CO)2]
_cod_original_cell_volume        6483.4(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C33 H30 Fe N2 Ni1 O2 P2 S2'
_cod_database_code               4302786