#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307029.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_4307029
loop_
_publ_author_name
'Sota Shibahara'
'Hiroshi Kitagawa'
'Yoshiki Ozawa'
'Koshiro Toriumi'
'Takashi Kubo'
'Kazuhiro Nakasuji'
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science, Kyushu University 
Higasi-ku, Hakozaki 6-10-1, Fukuoka, Fukuoka, 812-8581, Japan
;
_publ_contact_author_email       ' sota-s.scc@mbox.nc.kyushu-u.ac.jp '
_publ_contact_author_fax         ' +81 92 642 2319 '
_publ_contact_author_name        ' Sota Shibahara'
_publ_contact_author_phone       ' +81 92 642 2319 '
_publ_section_title
;
Syntheses and Unusual Segregated-Alternated Hybrid Stacking Structure of
Hydrogen-Bonded Charge-Transfer Complexes Composed of
Bis[2,3-pyridinedithiolate]metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1162
_journal_page_last               1170
_journal_paper_doi               10.1021/ic0615269
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C16 H22 N4 O2 Ni S4 '
_chemical_formula_sum            'C16 H22 N4 Ni O2 S4'
_chemical_formula_weight         489.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Fri Jun 21 11:01:08 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 100.477(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6204(4)
_cell_length_b                   14.3138(5)
_cell_length_c                   9.7129(4)
_cell_measurement_reflns_used    7991
_cell_measurement_temperature    200.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     1041.79(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9885
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.25
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2115
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.0358P)²+0.2935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                2115
_reflns_number_total             2385
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic0615269si20060812_022136_1.cif
_cod_data_source_block           '[Ni(Hpydt)2]2DMF'
_cod_original_cell_volume        1041.80(7)
_cod_original_formula_sum        'C16 H22 N4 O2 Ni S4 '
_cod_database_code               4307029
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni(1) Ni 0.5000 0.0000 1.0000 0.02747(9) Uani 1.00 d S . .
S(1) S 0.64190(6) -0.06954(3) 1.18588(4) 0.0339(1) Uani 1.00 d . . .
S(2) S 0.47131(6) 0.12752(3) 1.11609(4) 0.0369(1) Uani 1.00 d . . .
O(1) O 1.1053(2) 0.16932(9) 1.4770(1) 0.0493(3) Uani 1.00 d . . .
N(1) N 0.7245(2) -0.00766(9) 1.4482(2) 0.0360(3) Uani 1.00 d . . .
N(2) N 0.9980(2) 0.3099(1) 1.5296(2) 0.0358(3) Uani 1.00 d . . .
C(1) C 0.6462(2) 0.0127(1) 1.3160(2) 0.0302(3) Uani 1.00 d . . .
C(2) C 0.5659(2) 0.1010(1) 1.2878(2) 0.0302(3) Uani 1.00 d . . .
C(3) C 0.5655(2) 0.1621(1) 1.3985(2) 0.0364(4) Uani 1.00 d . . .
C(4) C 0.6457(3) 0.1373(1) 1.5334(2) 0.0413(4) Uani 1.00 d . . .
C(5) C 0.7260(3) 0.0520(1) 1.5560(2) 0.0414(4) Uani 1.00 d . . .
C(6) C 0.9040(3) 0.3275(1) 1.3880(2) 0.0437(4) Uani 1.00 d . . .
C(7) C 1.0030(3) 0.3854(2) 1.6300(2) 0.0496(5) Uani 1.00 d . . .
C(8) C 1.0932(2) 0.2331(1) 1.5599(2) 0.0378(4) Uani 1.00 d . . .
H(1) H 0.771(3) -0.064(2) 1.465(2) 0.05134(8) Uiso 1.00 calc . . .
H(2) H 0.505(3) 0.219(2) 1.382(2) 0.0552 Uiso 1.00 calc . . .
H(3) H 0.643(3) 0.176(2) 1.604(2) 0.0552 Uiso 1.00 calc . . .
H(4) H 0.784(3) 0.032(2) 1.642(2) 0.0552 Uiso 1.00 calc . . .
H(5) H 0.977(3) 0.373(2) 1.341(2) 0.0552 Uiso 1.00 calc . . .
H(6) H 0.800(3) 0.356(2) 1.397(2) 0.0552 Uiso 1.00 calc . . .
H(7) H 0.888(3) 0.271(2) 1.340(2) 0.0552 Uiso 1.00 calc . . .
H(8) H 0.887(3) 0.401(2) 1.634(2) 0.0552 Uiso 1.00 calc . . .
H(9) H 1.079(3) 0.437(2) 1.597(2) 0.0552 Uiso 1.00 calc . . .
H(10) H 1.067(3) 0.364(2) 1.721(2) 0.0552 Uiso 1.00 calc . . .
H(11) H 1.153(3) 0.231(2) 1.657(2) 0.0552 Uiso 1.00 calc . . .
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)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 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)
;
O O 0.011 0.006
;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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S(1) Ni(1) S(1) 180.0 . . 3_657 yes
S(1) Ni(1) S(2) 92.03(2) . . . yes
S(1) Ni(1) S(2) 87.97(2) . . 3_657 yes
S(1) Ni(1) S(2) 87.97(2) 3_657 . . yes
S(1) Ni(1) S(2) 92.03(2) 3_657 . 3_657 yes
S(2) Ni(1) S(2) 180.0 . . 3_657 yes
Ni(1) S(1) C(1) 103.69(5) . . . yes
Ni(1) S(2) C(2) 104.56(5) . . . yes
C(1) N(1) C(5) 122.9(1) . . . yes
C(6) N(2) C(7) 117.1(1) . . . yes
C(6) N(2) C(8) 120.8(2) . . . yes
C(7) N(2) C(8) 121.5(1) . . . yes
S(1) C(1) N(1) 119.8(1) . . . yes
S(1) C(1) C(2) 121.4(1) . . . yes
N(1) C(1) C(2) 118.8(1) . . . yes
S(2) C(2) C(1) 118.2(1) . . . yes
S(2) C(2) C(3) 123.3(1) . . . yes
C(1) C(2) C(3) 118.5(1) . . . yes
C(2) C(3) C(4) 120.5(2) . . . yes
C(3) C(4) C(5) 119.3(2) . . . yes
N(1) C(5) C(4) 120.0(2) . . . yes
O(1) C(8) N(2) 125.1(2) . . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni(1) S(1) 2.1702(4) . . yes
Ni(1) S(1) 2.1702(4) . 3_657 yes
Ni(1) S(2) 2.1773(4) . . yes
Ni(1) S(2) 2.1773(4) . 3_657 yes
S(1) C(1) 1.723(2) . . yes
S(2) C(2) 1.734(2) . . yes
O(1) C(8) 1.232(2) . . yes
N(1) C(1) 1.346(2) . . yes
N(1) C(5) 1.349(2) . . yes
N(2) C(6) 1.453(2) . . yes
N(2) C(7) 1.452(3) . . yes
N(2) C(8) 1.320(2) . . yes
C(1) C(2) 1.409(2) . . yes
C(2) C(3) 1.387(2) . . yes
C(3) C(4) 1.388(2) . . yes
C(4) C(5) 1.365(3) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
S(2) C(8) 3.465(2) . 4_454 ?
O(1) N(1) 2.687(2) . 3_758 ?
O(1) C(7) 3.409(3) . 4_554 ?
O(1) C(5) 3.455(2) . 3_758 ?
N(1) C(4) 3.408(3) . 3_658 ?
N(1) C(5) 3.484(3) . 3_658 ?
N(1) C(8) 3.520(2) . 3_758 ?
C(1) C(5) 3.425(3) . 3_658 ?
C(1) C(4) 3.589(3) . 3_658 ?
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
Ni(1) S(1) C(1) N(1) 179.5(1) . . . . yes
Ni(1) S(1) C(1) C(2) 0.8(1) . . . . yes
Ni(1) S(2) C(2) C(1) 3.7(1) . . . . yes
Ni(1) S(2) C(2) C(3) -175.9(1) . . . . yes
Ni(1) S(2) C(2) C(1) -3.7(1) . 3_657 3_657 3_657 yes
Ni(1) S(2) C(2) C(3) 175.9(1) . 3_657 3_657 3_657 yes
S(1) Ni(1) S(2) C(2) -2.53(6) . . . . yes
S(1) Ni(1) S(2) C(2) -177.47(6) . . 3_657 3_657 yes
S(1) C(1) N(1) C(5) -177.1(1) . . . . yes
S(1) C(1) C(2) S(2) -3.2(2) . . . . yes
S(1) C(1) C(2) C(3) 176.5(1) . . . . yes
S(2) Ni(1) S(1) C(1) 1.22(6) . . . . yes
S(2) Ni(1) S(1) C(1) 178.78(6) . . 3_657 3_657 yes
S(2) C(2) C(1) N(1) 178.2(1) . . . . yes
S(2) C(2) C(3) C(4) -179.1(1) . . . . yes
O(1) C(8) N(2) C(6) -3.4(3) . . . . yes
O(1) C(8) N(2) C(7) -174.6(2) . . . . yes
N(1) C(1) C(2) C(3) -2.2(2) . . . . yes
N(1) C(5) C(4) C(3) -1.0(3) . . . . yes
C(1) N(1) C(5) C(4) 0.0(3) . . . . yes
C(1) C(2) C(3) C(4) 1.3(3) . . . . yes
C(2) C(1) N(1) C(5) 1.6(3) . . . . yes
C(2) C(3) C(4) C(5) 0.3(3) . . . . yes
C(2) C(3) C(4) C(5) 0.3(3) . . . . yes
