Synthetic Analogues of the Active Site of the A-Cluster of Acetyl Coenzyme A Synthase/CO Dehydrogenase: Syntheses, Structures, and Reactions with CO
Harrop, Todd C.; Olmstead, Marilyn M.; Mascharak, Pradip K.; Inorganic Chemistry 45 (2006) 3424–3436; doi:10.1021/ic0520465

data_4332030
_publ_section_title
;
 Synthetic Analogues of the Active Site of the A-Cluster of Acetyl
 Coenzyme A Synthase/CO Dehydrogenase:&#x00A0; Syntheses, Structures, and
 Reactions with CO
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3424
_journal_page_last               3436
_journal_paper_doi               10.1021/ic0520465
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
'C54 H42 N6 Ni3 O6 S4, 2(C8 H20 N), 3(C3 H7 N O)'
_chemical_formula_sum            'C79 H103 N11 Ni3 O9 S4'
_chemical_formula_weight         1655.09
_chemical_name_common            (Et4N)2[Ni(DMF)2{Ni(NpPepS)}2].3DMF
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.902(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.009(3)
_cell_length_b                   13.0882(16)
_cell_length_c                   37.076(4)
_cell_measurement_reflns_used    45
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.2
_cell_volume                     8076(2)
_computing_cell_refinement       'Siemens P3/PC'
_computing_data_collection       'Siemens P3/PC'
_computing_data_reduction        'Siemens XDISK'
_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      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            16932
_diffrn_reflns_theta_full        55.99
_diffrn_reflns_theta_max         55.99
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.277
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2, Parkin, S., Moezzi, B. and Hope, H. J. Appl. Crystallogr. 28 (1995)
53-56.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         10484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+11.1419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                7809
_reflns_number_total             10484
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0520465sup5.cif
_cod_data_source_block           mn1545
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4332030