Unidentate and Bidentate Binding of Nickel(II) Complexes to an Fe4S4 Cluster via Bridging Thiolates: Synthesis, Crystal Structures, and Electrochemical Properties of Model Compounds for the Active Sites of Nickel Containing CO Dehydrogenase/Acetyl-CoA Synthase
Frank Osterloh; Wolfgang Saak; Siegfried Pohl; Journal of the American Chemical Society 119 (1997) 5648–5656; doi:10.1021/ja970194r

data_4116984
_publ_contact_author
;
   W.Saak
   Universitaet Oldenburg
   FB 9 Anorganische Chemie
   Carl-von-Ossietzkystr. 9-11
   Postfach 2503
   D-26111 Oldenburg
   Germany
;
_publ_contact_author_fax         '+49 441 7983329'
_publ_contact_author_phone       '+49 441 7983658 / 7983741'
_publ_section_title
;
 Unidentate and Bidentate Binding of Nickel(II) Complexes to an Fe4S4
 Cluster via Bridging Thiolates: Synthesis, Crystal Structures, and
 Electrochemical Properties of Model Compounds for the Active Sites of
 Nickel Containing CO Dehydrogenase/Acetyl-CoA Synthase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5648
_journal_page_last               5656
_journal_paper_doi               10.1021/ja970194r
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C56 H102 Fe4 N4 Ni2 O S10'
_chemical_formula_weight         1508.84
_chemical_name_systematic
; 
C11H24N2S2=N,N-diethyl-3,7-diazanonane-1,9-dithiolat
C15H23S=2,4,6-trisiopropylbenzenethiolat
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9750(10)
_cell_length_b                   19.4730(10)
_cell_length_c                   28.242(2)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.0
_cell_measurement_theta_min      12.4
_cell_volume                     8235.6(9)
_computing_cell_refinement       'STADI4 (STOE, 1995)'
_computing_data_collection       'STADI4 (STOE, 1995)'
_computing_data_reduction        'X-RED  (STOE, 1995)'
_computing_molecular_graphics    'SHELXTL-PC (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-PC (Siemens, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens StOE AED2 4-circle-diffractometer'
_diffrn_measurement_method       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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6289
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        11.2
_diffrn_standards_interval_time  45
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       prism
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.262
_refine_ls_goodness_of_fit_obs   1.255
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         6275
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.483
_refine_ls_restrained_S_obs      1.254
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_obs          0.0761
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+14.9712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2485
_refine_ls_wR_factor_obs         0.1921
_reflns_number_observed          5223
_reflns_number_total             6289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja970194r_3.cif
_cod_data_source_block           compound"5"
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+14.9712P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+14.9712P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116984