#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:49:53 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179817 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/13/7011314.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_7011314
loop_
_publ_author_name
'Johanna A. W. Verhagen'
'Dianne D. Ellis'
'Martin Lutz'
'Anthony L. Spek'
'Elisabeth Bouwman'
_publ_section_title
;
 Synthesis, characterisation and crystal structures of new nickel
 complexes in S4 coordination spheres; an unprecedented rearrangement
 during ligand synthesis
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1275
_journal_page_last               1280
_journal_paper_doi               10.1039/b110332f
_journal_year                    2002
_chemical_formula_moiety         'C22 H30 Ni S4'
_chemical_formula_sum            'C22 H30 Ni S4'
_chemical_formula_weight         481.41
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.6417(16)
_cell_angle_beta                 105.6636(17)
_cell_angle_gamma                89.9694(19)
_cell_formula_units_Z            1
_cell_length_a                   7.1006(2)
_cell_length_b                   8.3936(2)
_cell_length_c                   10.4298(4)
_cell_measurement_temperature    150(2)
_cell_volume                     564.61(3)
_computing_cell_refinement       'DENZO 1.11'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'DENZO 1.11'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'PLATON (Spek, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, et al. 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6230
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.8084
_exptl_absorpt_correction_T_min  0.7560
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagons
_exptl_crystal_F_000             254
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0186P)²+0.1845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                2283
_reflns_number_total             2670
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b110332f.txt
_cod_data_source_block           s2323a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7011314
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.5000 0.5000 0.01367(10) Uani 1 2 d S . .
S6 S -0.12639(7) 0.26301(5) 0.50178(5) 0.01826(12) Uani 1 1 d . . .
S9 S 0.08945(6) 0.35403(5) 0.31656(4) 0.01565(11) Uani 1 1 d . . .
C4 C 0.3075(3) 0.1650(2) 0.4732(2) 0.0264(4) Uani 1 1 d . . .
H4A H 0.2865 0.2530 0.5549 0.040 Uiso 1 1 calc R . .
H4B H 0.4300 0.1960 0.4569 0.040 Uiso 1 1 calc R . .
H4C H 0.3163 0.0573 0.4914 0.040 Uiso 1 1 calc R . .
C5 C 0.1710(3) 0.0219(2) 0.2114(2) 0.0304(5) Uani 1 1 d . . .
H5A H 0.1840 -0.0893 0.2230 0.046 Uiso 1 1 calc R . .
H5B H 0.2915 0.0601 0.1969 0.046 Uiso 1 1 calc R . .
H5C H 0.0594 0.0142 0.1295 0.046 Uiso 1 1 calc R . .
C7 C -0.0597(3) 0.1008(2) 0.36080(18) 0.0186(4) Uani 1 1 d . . .
H7A H -0.0535 -0.0066 0.3815 0.022 Uiso 1 1 calc R . .
H7B H -0.1634 0.0822 0.2708 0.022 Uiso 1 1 calc R . .
C8 C 0.1366(3) 0.1476(2) 0.34338(18) 0.0186(4) Uani 1 1 d . . .
C10 C 0.3217(3) 0.4352(2) 0.30735(18) 0.0194(4) Uani 1 1 d . . .
H10A H 0.3268 0.5599 0.3359 0.023 Uiso 1 1 calc R . .
H10B H 0.4307 0.4063 0.3759 0.023 Uiso 1 1 calc R . .
C11 C 0.3532(3) 0.3677(2) 0.16346(18) 0.0168(4) Uani 1 1 d . . .
C12 C 0.5325(3) 0.3105(2) 0.15109(19) 0.0246(4) Uani 1 1 d . . .
H12 H 0.6309 0.3082 0.2327 0.029 Uiso 1 1 calc R . .
C13 C 0.5699(3) 0.2564(3) 0.0212(2) 0.0336(5) Uani 1 1 d . . .
H13 H 0.6939 0.2181 0.0143 0.040 Uiso 1 1 calc R . .
C14 C 0.4282(3) 0.2581(3) -0.0983(2) 0.0320(5) Uani 1 1 d . . .
H14 H 0.4539 0.2205 -0.1875 0.038 Uiso 1 1 calc R . .
C15 C 0.2489(3) 0.3146(3) -0.0876(2) 0.0305(5) Uani 1 1 d . . .
H15 H 0.1511 0.3167 -0.1696 0.037 Uiso 1 1 calc R . .
C16 C 0.2109(3) 0.3683(2) 0.0425(2) 0.0249(4) Uani 1 1 d . . .
H16 H 0.0864 0.4059 0.0490 0.030 Uiso 1 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'
Ni Ni 0.3393 1.1124 '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'
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
S9 Ni1 S9 180.0 2_566 . ?
S9 Ni1 S6 91.874(16) 2_566 . ?
S9 Ni1 S6 88.127(16) . . ?
S9 Ni1 S6 88.127(16) 2_566 2_566 ?
S9 Ni1 S6 91.873(16) . 2_566 ?
S6 Ni1 S6 180.0 . 2_566 ?
C7 S6 Ni1 104.05(6) . . ?
C10 S9 C8 105.17(9) . . ?
C10 S9 Ni1 114.51(6) . . ?
C8 S9 Ni1 103.97(6) . . ?
C8 C4 H4A 109.5 . . ?
C8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C8 C5 H5A 109.5 . . ?
C8 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C8 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C8 C7 S6 112.74(12) . . ?
C8 C7 H7A 109.0 . . ?
S6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
S6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C4 C8 C7 112.69(15) . . ?
C4 C8 C5 111.27(16) . . ?
C7 C8 C5 110.64(15) . . ?
C4 C8 S9 111.88(12) . . ?
C7 C8 S9 99.98(11) . . ?
C5 C8 S9 109.87(13) . . ?
C11 C10 S9 113.90(12) . . ?
C11 C10 H10A 108.8 . . ?
S9 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
S9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C12 C11 C16 118.65(17) . . ?
C12 C11 C10 119.34(16) . . ?
C16 C11 C10 121.94(16) . . ?
C13 C12 C11 120.75(18) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 120.27(19) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 119.64(18) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C14 C15 C16 120.17(18) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 120.53(18) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
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 S9 2.1730(4) 2_566 ?
Ni1 S9 2.1730(4) . y
Ni1 S6 2.1903(4) . y
Ni1 S6 2.1903(4) 2_566 ?
S6 C7 1.8264(17) . y
S9 C10 1.8226(18) . y
S9 C8 1.8581(18) . y
C4 C8 1.521(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C8 1.523(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 C8 1.521(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C10 C11 1.504(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.384(3) . ?
C11 C16 1.389(2) . ?
C12 C13 1.384(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S9 Ni1 S6 C7 -175.92(6) 2_566 . . . ?
S9 Ni1 S6 C7 4.08(6) . . . . ?
S6 Ni1 S9 C10 -145.45(7) . . . . ?
S6 Ni1 S9 C10 34.55(7) 2_566 . . . ?
S6 Ni1 S9 C8 -31.25(6) . . . . ?
S6 Ni1 S9 C8 148.75(6) 2_566 . . . ?
Ni1 S6 C7 C8 32.33(13) . . . . ?
S6 C7 C8 C4 63.26(17) . . . . ?
S6 C7 C8 C5 -171.46(12) . . . . ?
S6 C7 C8 S9 -55.67(13) . . . . ?
C10 S9 C8 C4 56.22(15) . . . . ?
Ni1 S9 C8 C4 -64.47(13) . . . . ?
C10 S9 C8 C7 175.74(11) . . . . ?
Ni1 S9 C8 C7 55.04(11) . . . . ?
C10 S9 C8 C5 -67.89(14) . . . . ?
Ni1 S9 C8 C5 171.42(12) . . . . ?
C8 S9 C10 C11 83.69(14) . . . . ?
Ni1 S9 C10 C11 -162.82(11) . . . . ?
S9 C10 C11 C12 -133.63(16) . . . . ?
S9 C10 C11 C16 49.5(2) . . . . ?
C16 C11 C12 C13 0.6(3) . . . . ?
C10 C11 C12 C13 -176.36(18) . . . . ?
C11 C12 C13 C14 -0.4(3) . . . . ?
C12 C13 C14 C15 0.3(3) . . . . ?
C13 C14 C15 C16 -0.5(3) . . . . ?
C14 C15 C16 C11 0.7(3) . . . . ?
C12 C11 C16 C15 -0.8(3) . . . . ?
C10 C11 C16 C15 176.09(18) . . . . ?
