Structural Models of the Bimetallic Subunit at the A-Cluster of Acetyl Coenzyme A Synthase/CO Dehydrogenase: Binuclear Sulfur-Bridged Ni-Cu and Ni-Ni Complexes and Their Reactions with CO
Todd C. Harrop; Marilyn M. Olmstead; Pradip K. Mascharak; Journal of the American Chemical Society 126 (2004) 14714–14715; doi:10.1021/ja045284s

data_4113159
_publ_section_title
;
 Structural Models of the Bimetallic Subunit at the A-Cluster of Acetyl
 Coenzyme A Synthase/CO Dehydrogenase: Binuclear Sulfur-Bridged Ni-Cu and
 Ni-Ni Complexes and Their Reactions with CO
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14714
_journal_page_last               14715
_journal_paper_doi               10.1021/ja045284s
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C48 H49.5 Cu N5 Ni O3 S2'
_chemical_formula_weight         930.80
_chemical_name_common            (Et4N)[Ni(NpPepS)Cu(neo)].0.5Et2O.0.5H2O
_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                108.535(4)
_cell_angle_beta                 93.198(6)
_cell_angle_gamma                110.092(6)
_cell_formula_units_Z            4
_cell_length_a                   12.4276(18)
_cell_length_b                   17.482(2)
_cell_length_c                   22.792(3)
_cell_measurement_reflns_used    922
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.5
_cell_volume                     4332.8(10)
_computing_cell_refinement       'SMART 5.054'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_av_sigmaI/netI    0.097
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41039
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       plate
_exptl_crystal_F_000             1942
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.046
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         16443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+16.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1705
_reflns_number_gt                9918
_reflns_number_total             16443
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja045284ssi20040804_032642_1.cif
_cod_data_source_block           mn1514
_cod_original_cell_volume        4332.9(10)
_cod_original_formula_sum        'C48 H49.50 Cu N5 Ni O3 S2'
_cod_database_code               4113159