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_4112570
_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[Fe3NiS4(LS3)(dmpe)].2.5MeCN
_chemical_formula_sum            'C156 H217 Fe6 N9 Ni2 P4 S26'
_chemical_formula_weight         3628.22
_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                78.940(4)
_cell_angle_beta                 89.892(3)
_cell_angle_gamma                82.579(3)
_cell_formula_units_Z            2
_cell_length_a                   18.295(2)
_cell_length_b                   18.925(2)
_cell_length_c                   27.004(4)
_cell_measurement_temperature    193(2)
_cell_volume                     9096.6(19)
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.1552
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41360
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       plate
_exptl_crystal_F_000             1915
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.796
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1858
_refine_ls_number_reflns         23693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.796
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                12305
_reflns_number_total             23693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030627s_1.cif
_cod_data_source_block           (Et4N)2[3a].2.5MeCN
_cod_original_cell_volume        9097(2)
_cod_database_code               4112570