#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322370.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_4322370
loop_
_publ_author_name
'Dieter Sellmann'
'Jürgen Utz'
'Frank W. Heinemann'
_publ_contact_author
;
        Prof. Dr. D. Sellmann
        Institut für Anorganische Chemie II
        Universität Erlangen-Nürnberg
        Egerlandstr. 1
        D-91058 Erlangen
        Bundesrepublik Deutschland
;
_publ_contact_author_email       SELLMANN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 852-7367'
_publ_contact_author_phone       '049 9131 852-7360'
_publ_section_title
;
 Transition Metal Complexes with Sulfur Ligands. 136.1 Enforced Trans
 Coordination of Thiolate Donors in Electron Rich Iron, Ruthenium, and
 Nickel [M(L)(pyN₂H₂S₂)] and [M(L)(pyS₄)] Complexes (L = CO,
 PPh₃, DMSO) (pyN2H2S22-=
 2,6-Bis(2-mercaptophenylamino)dimethylpyridine(2-); pyS4²⁻ =
 2,6-Bis(2-mercaptophenylthio)dimethylpyridine(2-))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5314
_journal_page_last               5322
_journal_paper_doi               10.1021/ic990169h
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C38 H30 N2 Ni2 S8'
_chemical_formula_weight         888.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                77.560(10)
_cell_angle_beta                 79.19(2)
_cell_angle_gamma                81.24(2)
_cell_formula_units_Z            1
_cell_length_a                   8.376(2)
_cell_length_b                   10.649(2)
_cell_length_c                   10.942(2)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.2
_cell_measurement_theta_min      2.5
_cell_volume                     929.8(3)
_computing_cell_refinement
'XSCAnS 2.10b (Siemens An. X-Ray Instr., 1994)'
_computing_data_collection
'XSCAnS 2.10b (Siemens An. X-Ray Instr. 1994)'
_computing_data_reduction
'XSCAnS 2.10b (Siemens An. X-Ray Instr., 1994)'
_computing_molecular_graphics
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_publication_material
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_refinement
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_solution
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'profile data from ω-scans'
_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  0.1064
_diffrn_reflns_av_sigmaI/netI    0.3164
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4422
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        5.99
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.494
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.685
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.685
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.1750
_refine_ls_R_factor_obs          0.0586
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0457P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1486
_refine_ls_wR_factor_obs         0.1260
_reflns_number_observed          1162
_reflns_number_total             3641
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990169h_2.cif
_cod_data_source_block           ju9704
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0457P)^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^)+(0.0457P)^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               4322370
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_group
Ni1 Ni 0.0899(2) 0.83592(11) 0.53618(12) 0.0356(4) Uani 1 d . .
S1 S 0.1765(3) 1.0378(2) 0.4182(2) 0.0367(6) Uani 1 d . .
S2 S -0.0054(3) 0.6388(2) 0.6543(2) 0.0490(7) Uani 1 d . .
S3 S 0.0451(3) 0.7938(2) 0.3395(2) 0.0461(7) Uani 1 d . .
S4 S 0.2041(3) 0.8491(2) 0.7153(2) 0.0456(7) Uani 1 d . .
N1 N 0.3210(10) 0.7475(7) 0.4815(7) 0.050(2) Uani 1 d . .
C10 C 0.1985(12) 1.0199(8) 0.2603(8) 0.045(3) Uani 1 d . .
C11 C 0.2745(12) 1.1103(9) 0.1606(8) 0.056(3) Uani 1 d . .
H11 H 0.3122(12) 1.1802(9) 0.1803(8) 0.084 Uiso 1 calc R .
C12 C 0.2949(14) 1.0989(9) 0.0356(9) 0.071(4) Uani 1 d . .
H12 H 0.3470(14) 1.1597(9) -0.0274(9) 0.107 Uiso 1 calc R .
C13 C 0.2375(15) 0.9962(11) 0.0035(9) 0.079(4) Uani 1 d . .
H13 H 0.2506(15) 0.9885(11) -0.0810(9) 0.119 Uiso 1 calc R .
C14 C 0.1612(14) 0.9060(10) 0.0972(9) 0.070(3) Uani 1 d . .
H14 H 0.1209(14) 0.8388(10) 0.0749(9) 0.105 Uiso 1 calc R .
C15 C 0.1434(11) 0.9134(8) 0.2239(8) 0.043(2) Uani 1 d . .
C16 C 0.2041(11) 0.6597(8) 0.3374(8) 0.047(3) Uani 1 d . .
H16A H 0.1589(11) 0.5821(8) 0.3863(8) 0.070 Uiso 1 calc R .
H16B H 0.2377(11) 0.6472(8) 0.2506(8) 0.070 Uiso 1 calc R .
C20 C 0.1099(12) 0.6004(9) 0.7722(9) 0.050(3) Uani 1 d . .
C21 C 0.1166(13) 0.4775(10) 0.8525(10) 0.061(3) Uani 1 d . .
H21 H 0.0608(13) 0.4156(10) 0.8358(10) 0.092 Uiso 1 calc R .
C22 C 0.1994(16) 0.4433(12) 0.9528(11) 0.084(4) Uani 1 d . .
H22 H 0.1953(16) 0.3614(12) 1.0036(11) 0.127 Uiso 1 calc R .
C23 C 0.2906(15) 0.5306(13) 0.9800(10) 0.080(4) Uani 1 d . .
H23 H 0.3502(15) 0.5066(13) 1.0467(10) 0.120 Uiso 1 calc R .
C24 C 0.2901(12) 0.6544(11) 0.9049(9) 0.063(3) Uani 1 d . .
H24 H 0.3472(12) 0.7148(11) 0.9229(9) 0.094 Uiso 1 calc R .
C25 C 0.2058(12) 0.6871(9) 0.8049(8) 0.048(3) Uani 1 d . .
C26 C 0.4132(11) 0.8451(8) 0.6349(8) 0.048(3) Uani 1 d . .
H26A H 0.4348(11) 0.9324(8) 0.5938(8) 0.072 Uiso 1 calc R .
H26B H 0.4860(11) 0.8138(8) 0.6970(8) 0.072 Uiso 1 calc R .
C31 C 0.3519(12) 0.6741(8) 0.3883(8) 0.038(2) Uani 1 d . .
C32 C 0.5055(12) 0.6221(8) 0.3484(10) 0.054(3) Uani 1 d . .
H32 H 0.5239(12) 0.5764(8) 0.2826(10) 0.080 Uiso 1 calc R .
C33 C 0.6346(13) 0.6357(10) 0.4035(11) 0.068(3) Uani 1 d . .
H33 H 0.7398(13) 0.5985(10) 0.3769(11) 0.102 Uiso 1 calc R .
C34 C 0.6047(12) 0.7065(9) 0.5004(9) 0.052(3) Uani 1 d . .
H34 H 0.6891(12) 0.7177(9) 0.5401(9) 0.078 Uiso 1 calc R .
C35 C 0.4512(11) 0.7580(8) 0.5347(8) 0.038(2) Uani 1 d . .
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'
Ni Ni 0.3393 1.1124 '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
_geom_angle_publ_flag
N1 Ni1 S4 82.5(2) . . ?
N1 Ni1 S2 93.3(2) . . ?
S4 Ni1 S2 87.53(10) . . ?
N1 Ni1 S1 88.7(2) . . ?
S4 Ni1 S1 93.05(9) . . ?
S2 Ni1 S1 178.05(12) . . ?
N1 Ni1 S3 82.3(2) . . ?
S4 Ni1 S3 164.81(10) . . ?
S2 Ni1 S3 92.86(10) . . ?
S1 Ni1 S3 87.07(9) . . ?
N1 Ni1 S1 173.4(2) . 2_576 ?
S4 Ni1 S1 99.58(9) . 2_576 ?
S2 Ni1 S1 93.08(9) . 2_576 ?
S1 Ni1 S1 84.99(9) . 2_576 ?
S3 Ni1 S1 95.56(9) . 2_576 ?
C10 S1 Ni1 103.3(3) . . ?
C10 S1 Ni1 106.4(3) . 2_576 ?
Ni1 S1 Ni1 95.01(9) . 2_576 ?
C20 S2 Ni1 102.0(3) . . ?
C15 S3 C16 99.9(4) . . ?
C15 S3 Ni1 103.6(3) . . ?
C16 S3 Ni1 94.1(3) . . ?
C25 S4 C26 100.5(4) . . ?
C25 S4 Ni1 102.5(3) . . ?
C26 S4 Ni1 95.6(3) . . ?
C35 N1 C31 116.2(8) . . ?
C35 N1 Ni1 122.2(6) . . ?
C31 N1 Ni1 121.6(7) . . ?
C11 C10 C15 116.2(8) . . ?
C11 C10 S1 120.9(7) . . ?
C15 C10 S1 123.0(7) . . ?
C12 C11 C10 122.5(9) . . ?
C11 C12 C13 119.9(9) . . ?
C14 C13 C12 119.9(9) . . ?
C13 C14 C15 121.3(9) . . ?
C14 C15 C10 120.3(9) . . ?
C14 C15 S3 119.0(7) . . ?
C10 C15 S3 120.7(7) . . ?
C31 C16 S3 115.2(6) . . ?
C21 C20 C25 112.8(10) . . ?
C21 C20 S2 121.6(8) . . ?
C25 C20 S2 125.5(7) . . ?
C22 C21 C20 124.4(11) . . ?
C21 C22 C23 120.5(12) . . ?
C24 C23 C22 118.5(12) . . ?
C25 C24 C23 120.1(11) . . ?
C24 C25 C20 123.6(9) . . ?
C24 C25 S4 118.0(8) . . ?
C20 C25 S4 118.3(7) . . ?
C35 C26 S4 112.9(6) . . ?
C32 C31 N1 121.2(9) . . ?
C32 C31 C16 124.5(8) . . ?
N1 C31 C16 114.3(8) . . ?
C31 C32 C33 120.9(9) . . ?
C32 C33 C34 118.5(10) . . ?
C35 C34 C33 118.1(10) . . ?
C34 C35 N1 124.9(9) . . ?
C34 C35 C26 120.2(8) . . ?
N1 C35 C26 114.7(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.060(8) . ?
Ni1 S4 2.375(3) . ?
Ni1 S2 2.381(3) . ?
Ni1 S1 2.396(3) . ?
Ni1 S3 2.397(3) . ?
Ni1 S1 2.448(3) 2_576 ?
S1 C10 1.752(8) . ?
S1 Ni1 2.448(3) 2_576 ?
S2 C20 1.698(11) . ?
S3 C15 1.770(9) . ?
S3 C16 1.799(9) . ?
S4 C25 1.790(9) . ?
S4 C26 1.805(8) . ?
N1 C35 1.357(11) . ?
N1 C31 1.379(9) . ?
C10 C11 1.412(11) . ?
C10 C15 1.443(11) . ?
C11 C12 1.377(11) . ?
C12 C13 1.392(13) . ?
C13 C14 1.379(12) . ?
C14 C15 1.384(11) . ?
C16 C31 1.490(12) . ?
C20 C21 1.410(12) . ?
C20 C25 1.449(12) . ?
C21 C22 1.363(15) . ?
C22 C23 1.40(2) . ?
C23 C24 1.395(14) . ?
C24 C25 1.367(12) . ?
C26 C35 1.543(11) . ?
C31 C32 1.353(11) . ?
C32 C33 1.373(13) . ?
C33 C34 1.394(12) . ?
C34 C35 1.337(11) . ?
