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_4116982
_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            'C47 H80 Cl6 Fe4 Ni2 S14'
_chemical_formula_weight         1647.47
_chemical_name_systematic
; 
C7H14S4=3,7-dithianonane-1,9-dithiolat
C15H23S=2,4,6-trisiopropylbenzenethiolat
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.21(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.184(2)
_cell_length_b                   13.2340(10)
_cell_length_c                   29.102(4)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      10.9
_cell_volume                     6992.3(13)
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10221
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        17.0
_diffrn_standards_interval_time  45
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  0.9969
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            schwarz
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.854
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.280
_refine_ls_goodness_of_fit_obs   1.315
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         9687
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.291
_refine_ls_restrained_S_obs      1.311
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_obs          0.0971
_refine_ls_shift/esd_max         0.237
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+45.7296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2110
_refine_ls_wR_factor_obs         0.1914
_reflns_number_observed          7797
_reflns_number_total             9709
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja970194r_1.cif
_cod_data_source_block           compound"6"
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+45.7296P] 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^)+(0.0602P)^2^+45.7296P] 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               4116982