#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/16/4331681.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4331681
loop_
_publ_author_name
'Kobayashi, Atsushi'
'Kojima, Takahiko'
'Ikeda, Ryuichi'
'Kitagawa, Hiroshi'
_publ_section_title
;
 Synthesis of a One-Dimensional Metal-Dimer Assembled System with
 Interdimer Interaction, M2(dtp)4(M = Ni, Pd; dtp = Dithiopropionato)
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              322
_journal_page_last               327
_journal_paper_doi               10.1021/ic051387f
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C6 H10 Ni S4 '
_chemical_formula_sum            'C6 H10 Ni S4'
_chemical_formula_weight         269.09
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.9440(13)
_cell_length_b                   12.9440(13)
_cell_length_c                   6.1728(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.4
_cell_volume                     1034.2(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1332
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        -0.20
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.620
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             552.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.44
_refine_ls_extinction_coef       0.003(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1191
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                971
_reflns_number_total             1293
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic051387fsup1.cif
_cod_data_source_block           '_3ni2dtp4.xtl_____________'
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C6 H10 Ni S4 '
_cod_database_code               4331681
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-Y,+X,+Z
3 1/2-X,1/2-Y,+Z
4 +Y,1/2-X,+Z
5 -X,-Y,-Z
6 1/2+Y,-X,-Z
7 1/2+X,1/2+Y,-Z
8 -Y,1/2+X,-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
Ni(1) Ni 0.2500 0.2500 0.53845(10) 0.0412(2) Uani 1.00 4 d S
Ni(2) Ni 0.2500 0.2500 0.12912(12) 0.0564(3) Uani 1.00 4 d S
S(1) S 0.41559(6) 0.29010(6) 0.55796(12) 0.0530(3) Uani 1.00 1 d .
S(2) S 0.37427(9) 0.36706(8) 0.11058(17) 0.0699(3) Uani 1.00 1 d .
C(1) C 0.4475(2) 0.3547(2) 0.3321(5) 0.0571(8) Uani 1.00 1 d .
C(2) C 0.5535(3) 0.4048(3) 0.3277(7) 0.0773(12) Uani 1.00 1 d .
C(3) C 0.6317(4) 0.3426(6) 0.2101(16) 0.149(3) Uani 1.00 1 d .
H(1) H 0.5480 0.4721 0.2594 0.093 Uiso 1.00 1 c R
H(2) H 0.5768 0.4154 0.4754 0.093 Uiso 1.00 1 c R
H(3) H 0.6647 0.2959 0.3092 0.178 Uiso 1.00 1 c R
H(4) H 0.6825 0.3877 0.1477 0.178 Uiso 1.00 1 c R
H(5) H 0.5985 0.3039 0.0973 0.178 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
S S 0.125 0.123
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.339 1.112
;
International Tables for Crystallography
(1992, 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
Ni(2) Ni(1) S(1) 93.13(2) . .
Ni(2) Ni(1) S(1) 93.13(2) . 55502
Ni(2) Ni(1) S(1) 93.13(2) . 55503
Ni(2) Ni(1) S(1) 93.13(2) . 55504
S(1) Ni(1) S(1) 89.83(2) . 55502
S(1) Ni(1) S(1) 173.75(4) . 55503
S(1) Ni(1) S(1) 89.83(2) . 55504
S(1) Ni(1) S(1) 89.83(2) 55502 55503
S(1) Ni(1) S(1) 173.75(4) 55502 55504
S(1) Ni(1) S(1) 89.83(2) 55503 55504
Ni(1) Ni(2) S(2) 92.96(3) . .
Ni(1) Ni(2) S(2) 92.96(3) . 55502
Ni(1) Ni(2) S(2) 92.96(3) . 55503
Ni(1) Ni(2) S(2) 92.96(3) . 55504
S(2) Ni(2) S(2) 89.85(4) . 55502
S(2) Ni(2) S(2) 174.07(5) . 55503
S(2) Ni(2) S(2) 89.85(4) . 55504
S(2) Ni(2) S(2) 89.85(4) 55502 55503
S(2) Ni(2) S(2) 174.07(5) 55502 55504
S(2) Ni(2) S(2) 89.85(4) 55503 55504
Ni(1) S(1) C(1) 108.11(12) . .
Ni(2) S(2) C(1) 107.72(12) . .
S(1) C(1) S(2) 126.0(2) . .
S(1) C(1) C(2) 116.8(2) . .
S(2) C(1) C(2) 117.2(2) . .
C(1) C(2) C(3) 113.1(4) . .
C(1) C(2) H(1) 109.0(3) . .
C(1) C(2) H(2) 109.0(3) . .
C(3) C(2) H(1) 109.0(5) . .
C(3) C(2) H(2) 108.9(4) . .
H(1) C(2) H(2) 107.8(4) . .
C(2) C(3) H(3) 109.5 . .
C(2) C(3) H(4) 109.5 . .
C(2) C(3) H(5) 109.5 . .
H(3) C(3) H(4) 109.5 . .
H(3) C(3) H(5) 109.5 . .
H(4) C(3) H(5) 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni(1) Ni(2) 2.5267(10) .
Ni(1) S(1) 2.2086(7) .
Ni(1) S(1) 2.2086(7) 55502
Ni(1) S(1) 2.2086(7) 55503
Ni(1) S(1) 2.2086(7) 55504
Ni(2) S(2) 2.2128(11) .
Ni(2) S(2) 2.2128(10) 55502
Ni(2) S(2) 2.2128(11) 55503
Ni(2) S(2) 2.2128(10) 55504
S(1) C(1) 1.677(3) .
S(2) C(1) 1.672(3) .
C(1) C(2) 1.519(5) .
C(2) C(3) 1.484(8) .
C(2) H(1) 0.970(4) .
C(2) H(2) 0.970(4) .
C(3) H(3) 0.960 .
C(3) H(4) 0.960 .
C(3) H(5) 0.960 .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
S(1) S(2) 3.5937(13) 55601
S(2) S(1) 3.5937(13) 55401
C(2) C(2) 3.537(6) 66605
S(1) H(1) 3.3119(7) 66605
S(1) H(2) 3.5280(7) 64608
S(1) H(4) 3.424 64608
S(2) H(1) 3.2499(10) 66505
C(1) H(1) 3.375(3) 66605
C(1) H(2) 3.219(3) 66605
C(2) H(1) 3.280(4) 66605
C(2) H(2) 3.120(4) 66605
C(3) H(3) 3.245 65503
C(3) H(4) 3.039 64508
C(3) H(5) 3.024 56506
H(1) S(1) 3.3119(7) 66605
H(1) S(2) 3.2499(10) 66505
H(1) C(1) 3.375(3) 66605
H(1) C(2) 3.280(4) 66605
H(1) H(1) 3.510 66505
H(1) H(1) 3.300 66605
H(1) H(2) 2.722 66605
H(2) S(1) 3.5280(7) 56606
H(2) C(1) 3.219(3) 66605
H(2) C(2) 3.120(4) 66605
H(2) H(1) 2.722 66605
H(2) H(2) 2.974 66605
H(2) H(3) 3.299 56606
H(3) C(3) 3.245 65503
H(3) H(2) 3.299 64608
H(3) H(3) 2.508 65503
H(3) H(3) 2.948 56606
H(3) H(3) 2.948 64608
H(3) H(4) 3.249 65503
H(3) H(4) 3.251 64508
H(3) H(5) 3.574 65503
H(3) H(5) 3.378 56506
H(4) S(1) 3.424 56606
H(4) C(3) 3.039 56506
H(4) H(3) 3.249 65503
H(4) H(3) 3.251 56506
H(4) H(4) 3.347 56506
H(4) H(4) 3.347 64508
H(4) H(5) 2.187 56506
H(5) C(3) 3.024 64508
H(5) H(3) 3.574 65503
H(5) H(3) 3.378 64508
H(5) H(4) 2.187 64508
H(5) H(5) 3.179 56506
H(5) H(5) 3.179 64508
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_3
_geom_torsion_site_symmetry_4
Ni(2) Ni(1) S(1) C(1) 26.66(12) . . .
S(1) Ni(1) Ni(2) S(2) -29.68(3) . . .
S(1) Ni(1) Ni(2) S(2) -119.68(3) . . 55502
S(1) Ni(1) Ni(2) S(2) 150.32(3) . . 55503
S(1) Ni(1) Ni(2) S(2) 60.32(3) . . 55504
Ni(2) Ni(1) S(1) C(1) 26.66(12) . 55502 55502
S(1) Ni(1) Ni(2) S(2) 60.32(3) 55502 . .
S(1) Ni(1) Ni(2) S(2) -29.68(3) 55502 . 55502
S(1) Ni(1) Ni(2) S(2) -119.68(3) 55502 . 55503
S(1) Ni(1) Ni(2) S(2) 150.32(3) 55502 . 55504
Ni(2) Ni(1) S(1) C(1) 26.66(12) . 55503 55503
S(1) Ni(1) Ni(2) S(2) 150.32(3) 55503 . .
S(1) Ni(1) Ni(2) S(2) 60.32(3) 55503 . 55502
S(1) Ni(1) Ni(2) S(2) -29.68(3) 55503 . 55503
S(1) Ni(1) Ni(2) S(2) -119.68(3) 55503 . 55504
Ni(2) Ni(1) S(1) C(1) 26.66(12) . 55504 55504
S(1) Ni(1) Ni(2) S(2) -119.68(3) 55504 . .
S(1) Ni(1) Ni(2) S(2) 150.32(3) 55504 . 55502
S(1) Ni(1) Ni(2) S(2) 60.32(3) 55504 . 55503
S(1) Ni(1) Ni(2) S(2) -29.68(3) 55504 . 55504
S(1) Ni(1) S(1) C(1) 119.78(12) . 55502 55502
S(1) Ni(1) S(1) C(1) -66.46(13) 55502 . .
S(1) Ni(1) S(1) C(1) -153.3(2) . 55503 55503
S(1) Ni(1) S(1) C(1) -153.3(2) 55503 . .
S(1) Ni(1) S(1) C(1) -66.46(12) . 55504 55504
S(1) Ni(1) S(1) C(1) 119.78(13) 55504 . .
S(1) Ni(1) S(1) C(1) 119.78(13) 55502 55503 55503
S(1) Ni(1) S(1) C(1) -66.46(12) 55503 55502 55502
S(1) Ni(1) S(1) C(1) -153.3(2) 55502 55504 55504
S(1) Ni(1) S(1) C(1) -153.3(2) 55504 55502 55502
S(1) Ni(1) S(1) C(1) 119.78(12) 55503 55504 55504
S(1) Ni(1) S(1) C(1) -66.46(13) 55504 55503 55503
Ni(1) Ni(2) S(2) C(1) 28.78(13) . . .
Ni(1) Ni(2) S(2) C(1) 28.78(13) . 55502 55502
Ni(1) Ni(2) S(2) C(1) 28.78(13) . 55503 55503
Ni(1) Ni(2) S(2) C(1) 28.78(13) . 55504 55504
S(2) Ni(2) S(2) C(1) -64.18(13) . 55502 55502
S(2) Ni(2) S(2) C(1) 121.74(13) 55502 . .
S(2) Ni(2) S(2) C(1) -151.2(3) . 55503 55503
S(2) Ni(2) S(2) C(1) -151.2(3) 55503 . .
S(2) Ni(2) S(2) C(1) 121.74(13) . 55504 55504
S(2) Ni(2) S(2) C(1) -64.18(13) 55504 . .
S(2) Ni(2) S(2) C(1) -64.18(13) 55502 55503 55503
S(2) Ni(2) S(2) C(1) 121.74(13) 55503 55502 55502
S(2) Ni(2) S(2) C(1) -151.2(3) 55502 55504 55504
S(2) Ni(2) S(2) C(1) -151.2(3) 55504 55502 55502
S(2) Ni(2) S(2) C(1) -64.18(13) 55503 55504 55504
S(2) Ni(2) S(2) C(1) 121.74(13) 55504 55503 55503
Ni(1) S(1) C(1) S(2) -10.8(2) . . .
Ni(1) S(1) C(1) C(2) 170.4(2) . . .
Ni(2) S(2) C(1) S(1) -15.5(2) . . .
Ni(2) S(2) C(1) C(2) 163.3(2) . . .
S(1) C(1) C(2) C(3) 98.9(5) . . .
S(2) C(1) C(2) C(3) -80.1(5) . . .
S(1) C(1) C(2) H(1) -139.8(3) . . .
S(1) C(1) C(2) H(2) -22.4(4) . . .
S(2) C(1) C(2) H(1) 41.3(4) . . .
S(2) C(1) C(2) H(2) 158.6(2) . . .
C(1) C(2) C(3) H(3) -89.4 . . .
C(1) C(2) C(3) H(4) 150.6 . . .
C(1) C(2) C(3) H(5) 30.6 . . .
H(1) C(2) C(3) H(3) 149.3 . . .
H(1) C(2) C(3) H(4) 29.3 . . .
H(1) C(2) C(3) H(5) -90.7 . . .
H(2) C(2) C(3) H(3) 32.0 . . .
H(2) C(2) C(3) H(4) -88.0 . . .
H(2) C(2) C(3) H(5) 152.0 . . .
