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_4113161
_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_moiety         'C20 H12 N2 Ni O2 S2, 2(C8 H20 N)'
_chemical_formula_sum            'C36 H52 N4 Ni O2 S2'
_chemical_formula_weight         695.65
_chemical_name_common            (Et4N)2[Ni(PhPepS)]
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 109.900(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6126(9)
_cell_length_b                   19.7239(14)
_cell_length_c                   14.6251(10)
_cell_measurement_reflns_used    2430
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      19.98
_cell_measurement_theta_min      2.54
_cell_volume                     3421.0(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'Apex 2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       \w
_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  0.0883
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30467
_diffrn_reflns_theta_full        24.61
_diffrn_reflns_theta_max         24.61
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5764
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0580P)^2^+0.9699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                4017
_reflns_number_total             5764
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja045284ssi20040804_032642_3.cif
_cod_data_source_block           mn1686
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4113161