Synthesis, Structural Characterization, and Electrochemical Properties of Dinuclear Ni/Mn Model Complexes for the Active Site of [NiFe]-Hydrogenases
Li-Cheng Song; Jia-Peng Li; Zhao-Jun Xie; Hai-Bin Song; Inorganic Chemistry 52 (2013) 11618–11626; doi:10.1021/ic401978h

data_4336372
_publ_section_title
;
 Synthesis, Structural Characterization, and Electrochemical Properties of
 Dinuclear Ni/Mn Model Complexes for the Active Site of
 [NiFe]-Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11618
_journal_page_last               11626
_journal_paper_doi               10.1021/ic401978h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C38.3 H44.6 Br Cl0.6 Mn N Ni O5 P2 S2'
_chemical_formula_weight         939.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                69.068(14)
_cell_angle_beta                 78.86(2)
_cell_angle_gamma                84.86(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5722(17)
_cell_length_b                   13.933(2)
_cell_length_c                   17.134(2)
_cell_measurement_reflns_used    7226
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.6
_cell_volume                     2093.6(6)
_computing_cell_refinement       Crystalclear
_computing_data_collection       Crystalclear
_computing_data_reduction        Crystalclear
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn 724 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1051
_diffrn_reflns_av_sigmaI/netI    0.1007
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18631
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.961
_exptl_absorpt_correction_T_max  0.7987
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Crystalclear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       Prism
_exptl_crystal_F_000             963
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7368
_refine_ls_number_restraints     926
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0473P)^2^+2.4966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                6261
_reflns_number_total             7368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401978h_si_003_6.cif
_cod_data_source_block           10
_cod_original_formula_sum        'C38.30 H44.60 Br Cl0.60 Mn N Ni O5 P2 S2'
_cod_database_code               4336372