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#$Date: 2016-03-23 00:23:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179108 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307031.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_4307031
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_sum            'C22 H12 N6 Ni S4'
_chemical_formula_weight         547.33
_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-97
_cell_angle_alpha                70.565(6)
_cell_angle_beta                 80.957(6)
_cell_angle_gamma                69.641(6)
_cell_formula_units_Z            1
_cell_length_a                   7.3730(6)
_cell_length_b                   8.4850(10)
_cell_length_c                   9.8660(11)
_cell_measurement_temperature    293(2)
_cell_volume                     545.09(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.867
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.55920
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2906
_diffrn_reflns_theta_full        23.58
_diffrn_reflns_theta_max         23.58
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.677
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             278
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0495
_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)+(0.0481P)²+0.6273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                2487
_reflns_number_total             2906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0615269si20060812_022136_3.cif
_cod_data_source_block           '[Ni(Hpydt)2]TCNQ'
_cod_database_code               4307031
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 0.5000 0.0000 0.0000 0.03391(16) Uani 1 2 d S . .
S2 S 0.56076(11) -0.14166(12) -0.15665(9) 0.0444(2) Uani 1 1 d . . .
S1 S 0.20076(12) 0.09819(12) -0.05469(9) 0.0447(2) Uani 1 1 d . . .
C3 C 0.9068(5) -0.3425(4) -0.2429(4) 0.0439(7) Uani 1 1 d . . .
H1 H 0.8396 -0.3596 -0.3063 0.053 Uiso 1 1 calc R . .
N2 N 0.3087(6) -0.3561(5) 0.2023(4) 0.0607(8) Uani 1 1 d . . .
N3 N 0.3367(6) 0.3138(5) -0.4808(4) 0.0679(9) Uani 1 1 d . . .
C1 C 0.8078(4) -0.2405(4) -0.1564(3) 0.0366(6) Uani 1 1 d . . .
C2 C 0.0867(4) 0.2172(4) 0.0610(3) 0.0357(5) Uani 1 1 d . . .
N1 N -0.1071(4) 0.2939(4) 0.0616(3) 0.0486(7) Uani 1 1 d . . .
H3 H -0.1717 0.2777 0.0048 0.058 Uiso 1 1 calc R . .
C4 C 0.2047(5) -0.3950(5) -0.1471(4) 0.0549(9) Uani 1 1 d . . .
H4 H 0.3384 -0.4462 -0.1437 0.066 Uiso 1 1 calc R . .
C5 C 0.1054(6) 0.5792(5) -0.2376(4) 0.0540(9) Uani 1 1 d . . .
H5 H 0.1707 0.5089 -0.2963 0.065 Uiso 1 1 calc R . .
C6 C 0.0228(5) 0.0658(5) -0.3937(3) 0.0431(7) Uani 1 1 d . . .
H6 H 0.0359 0.1099 -0.3225 0.052 Uiso 1 1 calc R . .
C7 C 0.1804(5) -0.0373(4) -0.4474(3) 0.0424(6) Uani 1 1 d . . .
H7 H 0.3015 -0.0627 -0.4139 0.051 Uiso 1 1 calc R . .
C8 C 0.8366(4) 0.1084(4) -0.4441(3) 0.0380(6) Uani 1 1 d . . .
C9 C 0.6749(5) 0.2154(4) -0.3900(3) 0.0411(6) Uani 1 1 d . . .
C10 C 0.3134(5) -0.2919(5) 0.2850(4) 0.0448(7) Uani 1 1 d . . .
C11 C 0.4874(5) 0.2660(5) -0.4410(4) 0.0471(7) Uani 1 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 0.0003 0.0009 '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 0.2610 0.7247 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0010 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0688 0.0765 '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
S1 Ni1 S1 180.0 2_655 . ?
S1 Ni1 S2 92.24(3) 2_655 . ?
S1 Ni1 S2 87.76(3) . . ?
S1 Ni1 S2 87.76(3) 2_655 2_655 ?
S1 Ni1 S2 92.24(3) . 2_655 ?
S2 Ni1 S2 180.0 . 2_655 ?
C1 S2 Ni1 104.23(11) . . ?
C2 S1 Ni1 103.75(11) . . ?
C1 C3 C5 121.0(3) . 1_645 ?
C3 C1 C2 118.3(3) . 2_655 ?
C3 C1 S2 123.1(3) . . ?
C2 C1 S2 118.6(2) 2_655 . ?
N1 C2 C1 118.5(3) . 2_655 ?
N1 C2 S1 120.5(2) . . ?
C1 C2 S1 121.0(2) 2_655 . ?
C2 N1 C4 123.1(3) . 2 ?
C5 C4 N1 119.2(3) 1_545 2 ?
C4 C5 C3 119.9(3) 1_565 1_465 ?
C7 C6 C8 120.9(3) . 1_455 ?
C6 C7 C8 120.5(3) . 2_654 ?
C9 C8 C6 121.0(3) . 1_655 ?
C9 C8 C7 120.5(3) . 2_654 ?
C6 C8 C7 118.6(3) 1_655 2_654 ?
C8 C9 C11 122.7(3) . . ?
C8 C9 C10 122.1(3) . 2_655 ?
C11 C9 C10 115.1(3) . 2_655 ?
N2 C10 C9 178.2(4) . 2_655 ?
N3 C11 C9 176.7(4) . . ?
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 S1 2.1562(8) 2_655 ?
Ni1 S1 2.1562(8) . ?
Ni1 S2 2.1629(8) . ?
Ni1 S2 2.1629(8) 2_655 ?
S2 C1 1.720(3) . ?
S1 C2 1.704(3) . ?
C3 C1 1.367(4) . ?
C3 C5 1.383(5) 1_645 ?
N2 C10 1.133(5) . ?
N3 C11 1.127(5) . ?
C1 C2 1.411(4) 2_655 ?
C2 N1 1.348(4) . ?
C2 C1 1.411(4) 2_655 ?
N1 C4 1.352(5) 2 ?
C4 C5 1.352(6) 1_545 ?
C4 N1 1.352(5) 2 ?
C5 C4 1.352(6) 1_565 ?
C5 C3 1.383(5) 1_465 ?
C6 C7 1.343(5) . ?
C6 C8 1.419(5) 1_455 ?
C7 C8 1.431(4) 2_654 ?
C8 C9 1.379(4) . ?
C8 C6 1.419(5) 1_655 ?
C8 C7 1.431(4) 2_654 ?
C9 C11 1.418(5) . ?
C9 C10 1.419(4) 2_655 ?
C10 C9 1.420(4) 2_655 ?
