#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307033.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_4307033
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            'C26 H48 N4 Ni O2 S4'
_chemical_formula_weight         635.63
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_date             'Mon Oct 28 17:04:57 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                89
_cell_angle_beta                 89
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.74(1)
_cell_length_b                   14.53(1)
_cell_length_c                   14.246(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     6361(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS86
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10130
_diffrn_reflns_theta_max         30.01
_diffrn_standards_decay_%        2.48
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.48
_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   1.012
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4154
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.0733P)²+0.1239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                4154
_reflns_number_total             9270
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic0615269si20060812_022136_5.cif
_cod_data_source_block           '[Ni(pydt)2]2(Et4N)2H2O'
_cod_original_cell_volume        6362(6)
_cod_original_formula_sum        'C26 H48 N4 O2 Ni S4 '
_cod_database_code               4307033
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,1/2+z
1/2+x,1/2-y,-z
-x,y,1/2-z
-x,-y,-z
1/2+x,1/2+y,1/2-z
1/2-x,1/2+y,z
x,-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 0.37529(1) 0.24962(3) 0.15761(3) 0.0501(1) Uani 1.00 d . . .
S(1) S 0.39385(3) 0.18837(6) 0.02321(7) 0.0584(2) Uani 1.00 d . . .
S(2) S 0.36053(3) 0.38124(6) 0.08987(7) 0.0606(2) Uani 1.00 d . . .
S(3) S 0.36471(3) 0.31376(6) 0.29430(7) 0.0604(2) Uani 1.00 d . . .
S(4) S 0.38140(4) 0.11457(7) 0.22258(7) 0.0657(3) Uani 1.00 d . . .
O(1) O 0.0907(1) 0.0966(2) 0.0658(3) 0.110(1) Uani 1.00 d . . .
O(2) O 0.3436(2) 0.1072(3) 0.7567(3) 0.147(2) Uani 1.00 d . . .
N(1) N 0.3877(1) 0.2539(2) -0.1517(2) 0.0695(8) Uani 1.00 d . . .
N(2) N 0.3697(1) 0.2448(2) 0.4679(3) 0.0675(8) Uani 1.00 d . . .
N(3) N 0.25026(9) 0.1335(2) 0.0266(2) 0.0548(7) Uani 1.00 d . . .
N(4) N 0.5000 0.0827(3) 0.7500 0.0517(9) Uani 1.00 d S . .
N(5) N 0.0000 0.0750(3) 0.7500 0.058(1) Uani 1.00 d S . .
C(1) C 0.3832(1) 0.2743(2) -0.0599(3) 0.0534(8) Uani 1.00 d . . .
C(2) C 0.3695(1) 0.3617(3) -0.0307(3) 0.0539(8) Uani 1.00 d . . .
C(3) C 0.3630(1) 0.4278(3) -0.0979(4) 0.064(1) Uani 1.00 d . . .
C(4) C 0.3683(1) 0.4076(3) -0.1923(4) 0.073(1) Uani 1.00 d . . .
C(5) C 0.3801(1) 0.3203(3) -0.2145(3) 0.072(1) Uani 1.00 d . . .
C(6) C 0.3710(1) 0.2247(3) 0.3751(3) 0.0544(8) Uani 1.00 d . . .
C(7) C 0.3769(1) 0.1339(3) 0.3433(3) 0.0532(8) Uani 1.00 d . . .
C(8) C 0.3790(1) 0.0646(3) 0.4102(3) 0.066(1) Uani 1.00 d . . .
C(9) C 0.3765(1) 0.0862(3) 0.5039(3) 0.068(1) Uani 1.00 d . . .
C(10) C 0.3723(1) 0.1754(3) 0.5296(3) 0.074(1) Uani 1.00 d . . .
C(11) C 0.2205(1) 0.1691(3) 0.1030(3) 0.071(1) Uani 1.00 d . . .
C(12) C 0.2751(1) 0.2110(3) -0.0201(3) 0.069(1) Uani 1.00 d . . .
C(13) C 0.2207(1) 0.0852(3) -0.0419(3) 0.068(1) Uani 1.00 d . . .
C(14) C 0.2837(1) 0.0679(3) 0.0670(3) 0.074(1) Uani 1.00 d . . .
C(15) C 0.2436(2) 0.2206(4) 0.1812(3) 0.103(2) Uani 1.00 d . . .
C(16) C 0.2474(2) 0.2838(4) -0.0644(3) 0.088(1) Uani 1.00 d . . .
C(17) C 0.2429(2) 0.0478(4) -0.1287(3) 0.094(1) Uani 1.00 d . . .
C(18) C 0.2661(2) -0.0112(4) 0.1195(4) 0.101(2) Uani 1.00 d . . .
C(19) C 0.4667(1) 0.1417(3) 0.6995(3) 0.070(1) Uani 1.00 d . . .
C(20) C 0.4749(1) 0.0242(3) 0.8186(3) 0.0668(10) Uani 1.00 d . . .
C(21) C 0.4849(2) 0.2061(4) 0.6264(4) 0.106(2) Uani 1.00 d . . .
C(22) C 0.5027(2) -0.0421(4) 0.8751(4) 0.106(2) Uani 1.00 d . . .
C(23) C 0.0214(1) 0.1335(3) 0.6758(3) 0.078(1) Uani 1.00 d . . .
C(24) C 0.0356(1) 0.0163(3) 0.7927(3) 0.070(1) Uani 1.00 d . . .
C(25) C -0.0087(2) 0.1961(4) 0.6227(4) 0.113(2) Uani 1.00 d . . .
C(26) C 0.0210(2) -0.0433(4) 0.8738(4) 0.114(2) Uani 1.00 d . . .
H(1) H 0.355(1) 0.476(3) -0.083(3) 0.0738(2) Uiso 1.00 calc . . .
H(2) H 0.359(1) 0.456(3) -0.233(3) 0.0908(2) Uiso 1.00 calc . . .
H(3) H 0.3785 0.3057 -0.2865 0.0913 Uiso 1.00 calc . . .
H(4) H 0.383(1) 0.009(3) 0.388(3) 0.0643(1) Uiso 1.00 calc . . .
H(5) H 0.381(1) 0.043(3) 0.538(3) 0.0684(2) Uiso 1.00 calc . . .
H(6) H 0.367(1) 0.195(3) 0.601(3) 0.0801(2) Uiso 1.00 calc . . .
H(7) H 0.1068 0.1414 0.0202 0.0913 Uiso 1.00 calc . . .
H(8) H 0.0941 0.0275 0.0503 0.0913 Uiso 1.00 calc . . .
H(9) H 0.1994 0.2090 0.0763 0.0890 Uiso 1.00 calc . . .
H(10) H 0.2053 0.1173 0.1306 0.0890 Uiso 1.00 calc . . .
H(11) H 0.2943 0.2385 0.0248 0.0840 Uiso 1.00 calc . . .
H(12) H 0.2933 0.1848 -0.0693 0.0840 Uiso 1.00 calc . . .
H(13) H 0.1992 0.1297 -0.0629 0.0843 Uiso 1.00 calc . . .
H(14) H 0.2061 0.0369 -0.0112 0.0843 Uiso 1.00 calc . . .
H(15) H 0.3004 0.0431 0.0143 0.0917 Uiso 1.00 calc . . .
H(16) H 0.3036 0.1027 0.1044 0.0917 Uiso 1.00 calc . . .
H(17) H 0.2653 0.1803 0.2115 0.1278 Uiso 1.00 calc . . .
H(18) H 0.2249 0.2420 0.2285 0.1278 Uiso 1.00 calc . . .
H(19) H 0.2600 0.2717 0.1565 0.1278 Uiso 1.00 calc . . .
H(20) H 0.2281 0.2583 -0.1094 0.1063 Uiso 1.00 calc . . .
H(21) H 0.2293 0.3122 -0.0155 0.1063 Uiso 1.00 calc . . .
H(22) H 0.2640 0.3313 -0.0921 0.1063 Uiso 1.00 calc . . .
H(23) H 0.2570 0.0961 -0.1623 0.1151 Uiso 1.00 calc . . .
H(24) H 0.2222 0.0190 -0.1690 0.1151 Uiso 1.00 calc . . .
H(25) H 0.2641 0.0035 -0.1105 0.1151 Uiso 1.00 calc . . .
H(26) H 0.2466 -0.0465 0.0855 0.1207 Uiso 1.00 calc . . .
H(27) H 0.2890 -0.0496 0.1445 0.1207 Uiso 1.00 calc . . .
H(28) H 0.2506 0.0124 0.1759 0.1207 Uiso 1.00 calc . . .
H(29) H 0.4457 0.1008 0.6712 0.0854 Uiso 1.00 calc . . .
H(30) H 0.4517 0.1778 0.7454 0.0854 Uiso 1.00 calc . . .
H(31) H 0.4605 0.0660 0.8621 0.0801 Uiso 1.00 calc . . .
H(32) H 0.4527 -0.0076 0.7850 0.0801 Uiso 1.00 calc . . .
H(33) H 0.4990 0.1683 0.5777 0.1335 Uiso 1.00 calc . . .
H(34) H 0.4621 0.2388 0.5964 0.1335 Uiso 1.00 calc . . .
H(35) H 0.5054 0.2452 0.6521 0.1335 Uiso 1.00 calc . . .
H(36) H 0.5249 -0.0126 0.9105 0.1311 Uiso 1.00 calc . . .
H(37) H 0.5176 -0.0858 0.8328 0.1311 Uiso 1.00 calc . . .
H(38) H 0.4857 -0.0798 0.9171 0.1311 Uiso 1.00 calc . . .
H(39) H 0.0358 0.0912 0.6324 0.0945 Uiso 1.00 calc . . .
H(40) H 0.0437 0.1693 0.7046 0.0945 Uiso 1.00 calc . . .
H(41) H 0.0586 0.0577 0.8138 0.0890 Uiso 1.00 calc . . .
H(42) H 0.0478 -0.0211 0.7442 0.0890 Uiso 1.00 calc . . .
H(43) H -0.0308 0.1576 0.5915 0.1322 Uiso 1.00 calc . . .
H(44) H -0.0229 0.2358 0.6636 0.1322 Uiso 1.00 calc . . .
H(45) H 0.0063 0.2280 0.5752 0.1322 Uiso 1.00 calc . . .
H(46) H 0.0102 -0.0067 0.9239 0.1344 Uiso 1.00 calc . . .
H(47) H 0.0461 -0.0774 0.8987 0.1344 Uiso 1.00 calc . . .
H(48) H 0.0002 -0.0862 0.8544 0.1344 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)
;
Ni Ni 0.339 1.112
;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)
;
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
? ? ? ? ? ? ? ?
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
? ? ? ? ? ?
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
? ? ? ? ? ?
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
? ? ? ? ? ? ? ? ? ?
