Initial Structure Modification of Tetrahedral to Planar Nickel(II) in a Nickel-Iron-Sulfur Cluster Related to the C-Cluster of Carbon Monoxide Dehydrogenase
Rashmishree Panda; Yugen Zhang; Craig C. McLauchlan; P. Venkateswara Rao; F. A. Tiago de Oliveira; E. Münck; R. H. Holm; Journal of the American Chemical Society 126 (2004) 6448–6459; doi:10.1021/ja030627s

data_4112571
_publ_section_title
;
 Initial Structure Modification of Tetrahedral to Planar Nickel(II) in a
 Nickel-Iron-Sulfur Cluster Related to the C-Cluster of Carbon Monoxide
 Dehydrogenase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6448
_journal_page_last               6459
_journal_paper_doi               10.1021/ja030627s
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         (et4n)2[(LS3)NiFe3S4(dmpe)].0.25MeCN
_chemical_formula_sum            'C147 H203.5 Fe6 N4.5 Ni2 P4 S26'
_chemical_formula_weight         3443.94
_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                70.974(4)
_cell_angle_beta                 83.543(5)
_cell_angle_gamma                79.737(5)
_cell_formula_units_Z            2
_cell_length_a                   18.219(4)
_cell_length_b                   18.485(4)
_cell_length_c                   27.031(5)
_cell_measurement_temperature    193(2)
_cell_volume                     8454(3)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(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 scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.1533
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39798
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       plate
_exptl_crystal_F_000             3591
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1754
_refine_ls_number_reflns         23408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                11763
_reflns_number_total             23408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030627s_2.cif
_cod_data_source_block           (et4n)2[3b].0.25MeCN
_cod_database_code               4112571