#------------------------------------------------------------------------------
#$Date: 2024-11-17 23:25:13 +0200 (Sun, 17 Nov 2024) $
#$Revision: 295978 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/69/4116983.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4116983
loop_
_publ_author_name
'Frank Osterloh'
'Wolfgang Saak'
'Siegfried Pohl'
_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            'C26 H54 Fe4 I2 N6 Ni2 S8'
_chemical_formula_weight         1301.86
_chemical_name_systematic
; 
C11H24N2S2=N,N-diethyl-3,7-diazanonane-1,9-dithiolat
;
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_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            8
_cell_length_a                   20.8880(10)
_cell_length_b                   20.8880(10)
_cell_length_c                   20.5320(10)
_cell_measurement_temperature    296(2)
_cell_volume                     8958.3(7)
_computing_cell_refinement       'DIF4 (STOE)'
_computing_data_collection       'DIF4 (STOE)'
_computing_data_reduction        'RD4 (STOE)'
_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-2theta-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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4445
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.95
_diffrn_standards_interval_time  45
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.864
_exptl_absorpt_correction_T_max  0.3742
_exptl_absorpt_correction_T_min  0.2027
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2271
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_obs          0.0353
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0277P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0715
_refine_ls_wR_factor_obs         0.0655
_reflns_number_observed          1870
_reflns_number_total             2273
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ja970194r_2.cif
_cod_data_source_block           compound"3"
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.0000P] 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^)+(0.0277P)^2^+0.0000P] 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               4116983
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.89713(4) 0.35892(3) 0.10532(4) 0.0811(2) Uani 1 d .
Fe1 Fe 0.96431(5) 0.44316(5) 0.16518(5) 0.0447(3) Uani 1 d .
Fe2 Fe 0.93693(5) 0.53971(5) 0.25439(5) 0.0432(3) Uani 1 d .
S1 S 0.95815(10) 0.43032(10) 0.27227(10) 0.0509(5) Uani 1 d .
S2 S 0.92873(9) 0.54522(10) 0.14369(9) 0.0440(4) Uani 1 d .
Ni1 Ni 0.81914(4) 0.60305(4) 0.23331(4) 0.0399(2) Uani 1 d .
S3 S 0.82935(10) 0.52488(10) 0.30127(10) 0.0524(5) Uani 1 d .
S4 S 0.89266(9) 0.64532(10) 0.29501(10) 0.0507(5) Uani 1 d .
N1 N 0.7516(3) 0.5520(3) 0.1878(3) 0.0483(15) Uani 1 d .
N2 N 0.8186(3) 0.6829(3) 0.1812(3) 0.054(2) Uani 1 d .
C1 C 0.7892(4) 0.4610(4) 0.2578(5) 0.067(3) Uani 1 d .
H1A H 0.8166(4) 0.4236(4) 0.2558(5) 0.081 Uiso 1 calc R
H1B H 0.7501(4) 0.4493(4) 0.2803(5) 0.081 Uiso 1 calc R
C2 C 0.7737(4) 0.4840(4) 0.1897(5) 0.063(2) Uani 1 d .
H2A H 0.8116(4) 0.4797(4) 0.1627(5) 0.076 Uiso 1 calc R
H2B H 0.7406(4) 0.4568(4) 0.1714(5) 0.076 Uiso 1 calc R
C3 C 0.7416(4) 0.5682(5) 0.1181(4) 0.062(2) Uani 1 d .
H3A H 0.7775(4) 0.5520(5) 0.0931(4) 0.075 Uiso 1 calc R
H3B H 0.7033(4) 0.5467(5) 0.1028(4) 0.075 Uiso 1 calc R
C4 C 0.7350(5) 0.6373(5) 0.1053(4) 0.076(3) Uani 1 d .
H4A H 0.7037(5) 0.6549(5) 0.1353(4) 0.091 Uiso 1 calc R
H4B H 0.7186(5) 0.6431(5) 0.0615(4) 0.091 Uiso 1 calc R
C5 C 0.7972(5) 0.6750(5) 0.1121(4) 0.068(2) Uani 1 d .
H5A H 0.8306(5) 0.6532(5) 0.0879(4) 0.081 Uiso 1 calc R
H5B H 0.7914(5) 0.7170(5) 0.0929(4) 0.081 Uiso 1 calc R
C6 C 0.8863(4) 0.7072(4) 0.1788(4) 0.060(2) Uani 1 d .
H6A H 0.9118(4) 0.6784(4) 0.1524(4) 0.072 Uiso 1 calc R
H6B H 0.8866(4) 0.7489(4) 0.1578(4) 0.072 Uiso 1 calc R
C7 C 0.9160(4) 0.7130(4) 0.2444(5) 0.067(2) Uani 1 d .
H7A H 0.9023(4) 0.7526(4) 0.2648(5) 0.080 Uiso 1 calc R
H7B H 0.9622(4) 0.7142(4) 0.2402(5) 0.080 Uiso 1 calc R
C8 C 0.6915(3) 0.5606(4) 0.2261(4) 0.047(2) Uani 1 d .
H8A H 0.6797(3) 0.6055(4) 0.2244(4) 0.057 Uiso 1 calc R
H8B H 0.7006(3) 0.5503(4) 0.2712(4) 0.057 Uiso 1 calc R
C9 C 0.6334(4) 0.5210(5) 0.2044(5) 0.075(3) Uani 1 d .
H9A H 0.5977(4) 0.5302(5) 0.2323(5) 0.112 Uiso 1 calc R
H9B H 0.6436(4) 0.4762(5) 0.2072(5) 0.112 Uiso 1 calc R
H9C H 0.6227(4) 0.5316(5) 0.1603(5) 0.112 Uiso 1 calc R
C10 C 0.7757(4) 0.7300(4) 0.2165(4) 0.058(2) Uani 1 d .
H10A H 0.7902(4) 0.7329(4) 0.2613(4) 0.070 Uiso 1 calc R
H10B H 0.7327(4) 0.7124(4) 0.2173(4) 0.070 Uiso 1 calc R
C11 C 0.7717(6) 0.7979(5) 0.1890(6) 0.098(4) Uani 1 d .
H11A H 0.7432(6) 0.8230(5) 0.2154(6) 0.146 Uiso 1 calc R
H11B H 0.7558(6) 0.7963(5) 0.1452(6) 0.146 Uiso 1 calc R
H11C H 0.8135(6) 0.8169(5) 0.1893(6) 0.146 Uiso 1 calc R
N3 N 0.4163(6) 0.3142(6) 0.2118(6) 0.110(4) Uani 1 d .
C12 C 0.4605(7) 0.3454(6) 0.2126(5) 0.082(4) Uani 1 d .
C13 C 0.5156(6) 0.3890(7) 0.2117(6) 0.110(4) Uani 1 d .
H13A H 0.5527(6) 0.3665(7) 0.1963(6) 0.165 Uiso 1 calc R
H13B H 0.5235(6) 0.4047(7) 0.2549(6) 0.165 Uiso 1 calc R
H13C H 0.5067(6) 0.4244(7) 0.1832(6) 0.165 Uiso 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S1 Fe1 S2 105.09(9) . 10_654
S1 Fe1 S2 106.46(9) . .
S2 Fe1 S2 100.37(8) 10_654 .
S1 Fe1 I1 111.11(7) . .
S2 Fe1 I1 120.95(7) 10_654 .
S2 Fe1 I1 111.54(7) . .
S1 Fe1 Fe2 53.56(6) . 10_654
S2 Fe1 Fe2 52.40(6) 10_654 10_654
S2 Fe1 Fe2 104.28(7) . 10_654
I1 Fe1 Fe2 144.06(5) . 10_654
S1 Fe1 Fe2 54.81(6) . .
S2 Fe1 Fe2 104.50(7) 10_654 .
S2 Fe1 Fe2 52.30(6) . .
I1 Fe1 Fe2 134.43(5) . .
Fe2 Fe1 Fe2 68.03(5) 10_654 .
S1 Fe1 Fe1 97.66(6) . 10_654
S2 Fe1 Fe1 52.52(6) 10_654 10_654
S2 Fe1 Fe1 52.19(6) . 10_654
I1 Fe1 Fe1 150.71(3) . 10_654
Fe2 Fe1 Fe1 59.78(4) 10_654 10_654
Fe2 Fe1 Fe1 59.71(4) . 10_654
S2 Fe2 S1 102.47(9) . 10_654
S2 Fe2 S1 102.61(8) . .
S1 Fe2 S1 93.42(9) 10_654 .
S2 Fe2 S3 109.08(9) . .
S1 Fe2 S3 146.89(9) 10_654 .
S1 Fe2 S3 89.36(7) . .
S2 Fe2 S4 104.87(8) . .
S1 Fe2 S4 93.32(7) 10_654 .
S1 Fe2 S4 149.52(8) . .
S3 Fe2 S4 69.39(7) . .
S2 Fe2 Fe1 52.66(6) . 10_654
S1 Fe2 Fe1 50.65(6) 10_654 10_654
S1 Fe2 Fe1 95.04(7) . 10_654
S3 Fe2 Fe1 161.73(7) . 10_654
S4 Fe2 Fe1 112.05(7) . 10_654
S2 Fe2 Fe1 52.89(6) . .
S1 Fe2 Fe1 96.09(7) 10_654 .
S1 Fe2 Fe1 50.31(6) . .
S3 Fe2 Fe1 110.69(7) . .
S4 Fe2 Fe1 157.30(7) . .
Fe1 Fe2 Fe1 60.50(5) 10_654 .
S2 Fe2 Ni1 76.03(6) . .
S1 Fe2 Ni1 136.35(7) 10_654 .
S1 Fe2 Ni1 129.90(7) . .
S3 Fe2 Ni1 47.54(5) . .
S4 Fe2 Ni1 47.55(5) . .
Fe1 Fe2 Ni1 118.97(5) 10_654 .
Fe1 Fe2 Ni1 114.66(5) . .
S2 Fe2 Fe2 95.19(5) . 10_654
S1 Fe2 Fe2 48.79(6) 10_654 10_654
S1 Fe2 Fe2 47.48(6) . 10_654
S3 Fe2 Fe2 134.81(7) . 10_654
S4 Fe2 Fe2 140.61(7) . 10_654
Fe1 Fe2 Fe2 56.01(4) 10_654 10_654
Fe1 Fe2 Fe2 55.95(4) . 10_654
Ni1 Fe2 Fe2 170.37(4) . 10_654
Fe1 S1 Fe2 75.79(7) . 10_654
Fe1 S1 Fe2 74.88(7) . .
Fe2 S1 Fe2 83.73(8) 10_654 .
Fe2 S2 Fe1 74.94(7) . 10_654
Fe2 S2 Fe1 74.81(7) . .
Fe1 S2 Fe1 75.29(7) 10_654 .
N2 Ni1 N1 101.1(3) . .
N2 Ni1 S3 170.5(2) . .
N1 Ni1 S3 88.2(2) . .
N2 Ni1 S4 88.7(2) . .
N1 Ni1 S4 170.1(2) . .
S3 Ni1 S4 82.00(9) . .
N2 Ni1 Fe2 118.8(2) . .
N1 Ni1 Fe2 115.8(2) . .
S3 Ni1 Fe2 57.38(6) . .
S4 Ni1 Fe2 59.13(6) . .
C1 S3 Ni1 101.1(3) . .
C1 S3 Fe2 108.8(3) . .
Ni1 S3 Fe2 75.08(7) . .
C7 S4 Ni1 99.9(3) . .
C7 S4 Fe2 113.0(3) . .
Ni1 S4 Fe2 73.32(7) . .
C3 N1 C8 111.2(6) . .
C3 N1 C2 106.7(7) . .
C8 N1 C2 111.2(6) . .
C3 N1 Ni1 115.3(5) . .
C8 N1 Ni1 106.4(5) . .
C2 N1 Ni1 106.1(5) . .
C5 N2 C6 106.7(6) . .
C5 N2 C10 110.4(6) . .
C6 N2 C10 110.6(6) . .
C5 N2 Ni1 114.9(5) . .
C6 N2 Ni1 107.3(5) . .
C10 N2 Ni1 106.9(4) . .
C2 C1 S3 108.7(6) . .
N1 C2 C1 113.0(7) . .
C4 C3 N1 114.1(7) . .
C3 C4 C5 114.2(8) . .
N2 C5 C4 113.5(7) . .
C7 C6 N2 113.0(6) . .
C6 C7 S4 110.0(6) . .
N1 C8 C9 116.6(7) . .
N2 C10 C11 117.3(7) . .
N3 C12 C13 176.5(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Fe1 2.5644(13) .
Fe1 S1 2.219(2) .
Fe1 S2 2.290(2) 10_654
Fe1 S2 2.300(2) .
Fe1 Fe2 2.7816(15) 10_654
Fe1 Fe2 2.7836(14) .
Fe1 Fe1 2.804(2) 10_654
Fe2 S2 2.282(2) .
Fe2 S1 2.309(2) 10_654
Fe2 S1 2.356(2) .
Fe2 S3 2.464(2) .
Fe2 S4 2.533(2) .
Fe2 Fe1 2.7816(15) 10_654
Fe2 Ni1 2.8271(14) .
Fe2 Fe2 3.113(2) 10_654
S1 Fe2 2.309(2) 10_654
S2 Fe1 2.290(2) 10_654
Ni1 N2 1.982(6) .
Ni1 N1 2.000(7) .
Ni1 S3 2.158(2) .
Ni1 S4 2.178(2) .
S3 C1 1.811(9) .
S4 C7 1.822(9) .
N1 C3 1.486(10) .
N1 C8 1.493(9) .
N1 C2 1.493(10) .
N2 C5 1.495(11) .
N2 C6 1.503(11) .
N2 C10 1.516(10) .
C1 C2 1.513(12) .
C3 C4 1.473(13) .
C4 C5 1.525(13) .
C6 C7 1.489(13) .
C8 C9 1.534(11) .
C10 C11 1.528(12) .
N3 C12 1.13(2) .
C12 C13 1.47(2) .
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2024-11-17T23:38:10+02:00
;
 Replaced the '&G' character sequence with the backslash character ('\')
 in the '_reflns_observed_criterion' data value.
;
