#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/22/8102224.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_8102224
loop_
_publ_author_name
'Jacimovic, Zeljko K.'
'Radovic, Ana'
'Leovac, Vukadin M.'
'Tomic, Zoran D.'
'Radosavljevic Evans, Ivana'
_publ_section_title
;
Crystal structure of bis(μ₂-thiocyanato)tetrakis(3,5-dimethyl-
1-(thiocarbamoyl)pyrazole)dinickel(II) dichloride ethanol disolvate, 
[Ni(NCS)₂(C₆H₆N₃S)₄][Cl]₂ · 2C₂H₅OH
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              430
_journal_page_last               432
_journal_volume                  222
_journal_year                    2007
_chemical_formula_moiety         'C26 H36 N14 Ni2 S6, 2(C2 H6 O), 2(Cl)'
_chemical_formula_structural     '[Ni(NCS)2(C6H6N3S)4][Cl]2 &#x00B7; 2C2H5OH'
_chemical_formula_sum            'C30 H48 Cl2 N14 Ni2 O2 S6'
_chemical_formula_weight         1017.5
_chemical_name_systematic
; 
bis(μ₂-thiocyanato)tetrakis(3,5-dimethyl-1-(thiocarbamoyl)pyrazole)-
dinickel(II) dichloride ethanol disolvate 
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 93.9040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0407(7)
_cell_length_b                   11.8861(6)
_cell_length_c                   15.7389(9)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2247.3(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       omega/phi
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27632
_diffrn_reflns_theta_full        28.791
_diffrn_reflns_theta_max         29.991
_diffrn_reflns_theta_min         1.695
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     107
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.008885
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                4062
_reflns_number_total             6381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2162.cff
_cod_data_source_block           cunew_sq
_cod_original_sg_symbol_H-M      P12(1)/c1
_cod_database_code               8102224
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,1/2-z
3 -x,-y,-z
4 x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni Uani 0.83558(3) 0.15012(3) 0.04438(2) 1 4 e 0.0177(1) . .
S2 S Uani 0.74876(5) 0.03482(6) 0.14810(4) 1 4 e 0.0216(2) . .
S3 S Uani 1.01656(5) 0.13779(6) 0.12758(4) 1 4 e 0.0234(2) . .
S5 S Uani 0.79333(6) 0.31496(6) 0.13741(4) 1 4 e 0.0252(2) . .
N8 N Uani 0.58958(16) 0.13817(19) 0.04903(12) 1 4 e 0.0180(5) . .
N9 N Uani 0.83468(19) 0.38299(19) -0.01871(14) 1 4 e 0.0234(6) . .
N10 N Uani 0.67238(17) 0.15817(19) -0.00577(12) 1 4 e 0.0190(6) . .
N11 N Uani 0.87167(17) 0.0255(2) -0.03623(14) 1 4 e 0.0224(6) . .
N12 N Uani 0.88727(18) 0.28191(19) -0.03090(14) 1 4 e 0.0235(6) . .
N13 N Uani 0.54716(18) 0.0962(2) 0.18667(14) 1 4 e 0.0236(6) . .
N14 N Uani 0.6762(2) 0.4548(2) 0.03501(15) 1 4 e 0.0288(7) . .
C1 C Uani 1.0223(3) 0.2089(3) -0.1286(2) 1 4 e 0.0459(11) . .
C7 C Uani 0.8717(2) 0.4652(2) -0.07172(18) 1 4 e 0.0289(8) . .
C15 C Uani 0.9471(2) 0.4136(3) -0.1196(2) 1 4 e 0.0354(9) . .
C16 C Uani 0.6210(2) 0.0923(2) 0.12948(15) 1 4 e 0.0187(6) . .
C17 C Uani 0.5041(2) 0.1791(2) -0.07482(16) 1 4 e 0.0257(7) . .
C18 C Uani 0.7635(2) 0.3903(2) 0.04891(17) 1 4 e 0.0233(7) . .
C19 C Uani 0.9535(2) 0.3001(3) -0.09394(18) 1 4 e 0.0305(8) . .
C20 C Uani 0.4853(2) 0.1500(2) 0.00650(15) 1 4 e 0.0223(7) . .
C21 C Uani 0.3763(2) 0.1303(3) 0.04323(17) 1 4 e 0.0288(8) . .
C22 C Uani 1.08338(19) 0.0425(2) 0.07436(16) 1 4 e 0.0205(7) . .
C23 C Uani 0.6205(2) 0.1832(2) -0.08015(16) 1 4 e 0.0225(7) . .
C25 C Uani 0.6816(3) 0.2091(3) -0.15784(17) 1 4 e 0.0315(9) . .
C27 C Uani 0.8388(3) 0.5859(3) -0.0673(2) 1 4 e 0.0389(10) . .
O6 O Uani 0.39213(17) 0.24654(18) -0.26816(13) 1 4 e 0.0284(6) . .
C24 C Uani 0.2717(3) 0.3805(3) -0.2140(3) 1 4 e 0.0553(13) . .
C26 C Uani 0.2792(2) 0.2670(3) -0.2505(2) 1 4 e 0.0359(10) . .
Cl4 Cl Uani 0.54856(6) -0.03139(6) 0.36392(4) 1 4 e 0.0287(2) . .
H5 H Uiso 0.6610(17) 0.4859(12) -0.0139(12) 1 4 e 0.0403(19) . .
H6 H Uiso 0.6298(15) 0.4634(13) 0.0748(12) 1 4 e 0.0411(19) . .
H7 H Uiso 0.5616(17) 0.0615(12) 0.2339(11) 1 4 e 0.0334(19) . .
H8 H Uiso 0.3180(17) 0.128(3) -0.0011(13) 1 4 e 0.0512(19) . .
H9 H Uiso 0.4516(15) 0.1934(9) -0.1184(11) 1 4 e 0.0365(19) . .
H10 H Uiso 0.7508(18) 0.170(2) -0.1553(16) 1 4 e 0.056(2) . .
H11 H Uiso 0.379(2) 0.0624(19) 0.0753(17) 1 4 e 0.0514(19) . .
H12 H Uiso 0.7692(19) 0.598(2) -0.0988(19) 1 4 e 0.068(2) . .
H14 H Uiso 0.4870(14) 0.1356(11) 0.1798(13) 1 4 e 0.0339(19) . .
H15 H Uiso 0.362(2) 0.1901(19) 0.0809(16) 1 4 e 0.0514(19) . .
H16 H Uiso 0.9855(12) 0.4472(16) -0.1622(9) 1 4 e 0.0509(19) . .
H17 H Uiso 0.895(2) 0.630(2) -0.092(2) 1 4 e 0.068(2) . .
H18 H Uiso 0.638(2) 0.185(2) -0.2070(13) 1 4 e 0.057(2) . .
H22 H Uiso 1.060(3) 0.166(2) -0.0840(14) 1 4 e 0.084(2) . .
H23 H Uiso 0.834(3) 0.610(2) -0.0096(13) 1 4 e 0.069(2) . .
H25 H Uiso 0.976(2) 0.158(2) -0.163(2) 1 4 e 0.084(2) . .
H30 H Uiso 1.076(2) 0.239(2) -0.164(2) 1 4 e 0.084(2) . .
H34 H Uiso 0.695(2) 0.2884(16) -0.1610(16) 1 4 e 0.057(2) . .
H1 H Uiso 0.319(3) 0.384(2) -0.1627(17) 1 4 e 0.099(2) . .
H2 H Uiso 0.1964(18) 0.397(2) -0.200(2) 1 4 e 0.098(2) . .
H3 H Uiso 0.2320(19) 0.261(2) -0.3034(13) 1 4 e 0.0520(19) . .
H4 H Uiso 0.401(3) 0.187(2) -0.295(2) 1 4 e 0.051(2) . .
H13 H Uiso 0.257(2) 0.2098(18) -0.2107(14) 1 4 e 0.0522(19) . .
H241 H Uiso 0.296(3) 0.436(2) -0.2527(17) 1 4 e 0.099(2) . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 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
S2 Ni1 S3 90.85(2) . . . yes
S2 Ni1 S5 86.26(2) . . . yes
S2 Ni1 N10 80.85(6) . . . yes
S2 Ni1 N11 97.46(7) . . . yes
S2 Ni1 N12 165.33(7) . . . yes
S3 Ni1 S5 86.78(2) . . . yes
S3 Ni1 N10 170.37(6) . . . yes
S3 Ni1 N11 94.01(6) . . . yes
S3 Ni1 N12 93.39(6) . . . yes
S5 Ni1 N10 87.80(6) . . . yes
S5 Ni1 N11 176.18(7) . . . yes
S5 Ni1 N12 79.97(6) . . . yes
N10 Ni1 N11 91.93(8) . . . yes
N10 Ni1 N12 93.50(8) . . . yes
N11 Ni1 N12 96.25(9) . . . yes
Ni1 S2 C16 94.81(9) . . . yes
Ni1 S3 C22 102.40(9) . . . yes
Ni1 S5 C18 88.44(9) . . . yes
C26 O6 H4 114(2) . . . no
N10 N8 C20 110.40(18) . . . yes
C16 N8 C20 130.7(2) . . . yes
N10 N8 C16 117.84(19) . . . yes
N12 N9 C18 117.8(2) . . . yes
C7 N9 C18 130.5(2) . . . yes
N12 N9 C7 111.3(2) . . . yes
Ni1 N10 C23 136.63(17) . . . yes
N8 N10 C23 105.88(19) . . . yes
Ni1 N10 N8 117.42(14) . . . yes
Ni1 N11 C22 164.5(2) . . 3_755 yes
Ni1 N12 C19 139.7(2) . . . yes
N9 N12 C19 105.4(2) . . . yes
Ni1 N12 N9 114.73(16) . . . yes
H7 N13 H14 119.2(19) . . . no
C16 N13 H14 122.5(13) . . . no
C16 N13 H7 118.2(13) . . . no
C18 N14 H5 121.3(13) . . . no
H5 N14 H6 118.9(18) . . . no
C18 N14 H6 119.7(12) . . . no
N9 C7 C15 105.7(2) . . . yes
N9 C7 C27 123.8(2) . . . yes
C15 C7 C27 130.3(3) . . . no
C7 C15 C19 107.3(3) . . . no
S2 C16 N8 119.90(17) . . . yes
S2 C16 N13 123.23(19) . . . yes
N8 C16 N13 116.9(2) . . . yes
C20 C17 C23 107.1(2) . . . no
S5 C18 N9 119.12(18) . . . yes
S5 C18 N14 125.3(2) . . . yes
N9 C18 N14 115.6(2) . . . yes
C1 C19 C15 127.8(3) . . . no
N12 C19 C15 110.2(3) . . . yes
N12 C19 C1 122.0(3) . . . yes
N8 C20 C17 106.1(2) . . . yes
N8 C20 C21 126.1(2) . . . yes
C17 C20 C21 127.8(2) . . . no
S3 C22 N11 178.6(2) . . 3_755 yes
N10 C23 C17 110.5(2) . . . yes
N10 C23 C25 122.6(2) . . . yes
C17 C23 C25 126.8(2) . . . no
C19 C1 H25 110.3(15) . . . no
C19 C1 H30 111.0(15) . . . no
H22 C1 H25 108(2) . . . no
H22 C1 H30 109(3) . . . no
H25 C1 H30 107(2) . . . no
C19 C1 H22 111.5(16) . . . no
C7 C15 H16 126.0(12) . . . no
C19 C15 H16 126.7(11) . . . no
C23 C17 H9 125.9(11) . . . no
C20 C17 H9 127.0(11) . . . no
C20 C21 H8 110.1(13) . . . no
C20 C21 H15 109.1(15) . . . no
H8 C21 H11 111(3) . . . no
C20 C21 H11 109.9(15) . . . no
H11 C21 H15 108(2) . . . no
H8 C21 H15 109(2) . . . no
C23 C25 H18 109.1(14) . . . no
C23 C25 H34 109.7(15) . . . no
C23 C25 H10 110.0(15) . . . no
H10 C25 H34 109(2) . . . no
H18 C25 H34 110(2) . . . no
H10 C25 H18 109(2) . . . no
C7 C27 H17 108.1(15) . . . no
C7 C27 H23 111.4(15) . . . no
H12 C27 H17 109(2) . . . no
H12 C27 H23 110(3) . . . no
H17 C27 H23 108(3) . . . no
C7 C27 H12 110.3(15) . . . no
O6 C26 C24 108.5(3) . . . yes
C26 C24 H1 108.7(15) . . . no
C26 C24 H2 111.0(15) . . . no
C26 C24 H241 110.7(16) . . . no
H1 C24 H2 108(3) . . . no
H1 C24 H241 109(3) . . . no
H2 C24 H241 110(3) . . . no
O6 C26 H3 109.1(13) . . . no
O6 C26 H13 108.3(14) . . . no
C24 C26 H3 110.6(14) . . . no
C24 C26 H13 111.2(13) . . . no
H3 C26 H13 109.1(19) . . . no
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
Ni1 S2 2.4224(7) . . yes
Ni1 S3 2.4691(7) . . yes
Ni1 S5 2.5185(8) . . yes
Ni1 N10 2.069(2) . . yes
Ni1 N11 2.017(2) . . yes
Ni1 N12 2.085(2) . . yes
S2 C16 1.691(2) . . yes
S3 C22 1.650(2) . . yes
S5 C18 1.674(3) . . yes
O6 C26 1.427(3) . . yes
O6 H4 0.84(3) . . no
N8 C20 1.389(3) . . yes
N8 N10 1.383(3) . . yes
N8 C16 1.407(3) . . yes
N9 C7 1.379(3) . . yes
N9 N12 1.378(3) . . yes
N9 C18 1.414(3) . . yes
N10 C23 1.323(3) . . yes
N11 C22 1.162(3) . 3_755 yes
N12 C19 1.332(3) . . yes
N13 C16 1.308(3) . . yes
N14 C18 1.307(3) . . yes
N13 H14 0.863(16) . . no
N13 H7 0.858(17) . . no
N14 H5 0.862(18) . . no
N14 H6 0.873(19) . . no
C1 C19 1.490(5) . . no
C7 C15 1.364(4) . . no
C7 C27 1.491(4) . . no
C15 C19 1.409(5) . . no
C17 C20 1.360(3) . . no
C17 C23 1.411(3) . . no
C20 C21 1.488(3) . . no
C23 C25 1.501(4) . . no
C1 H30 0.95(3) . . no
C1 H25 0.96(3) . . no
C1 H22 0.96(3) . . no
C15 H16 0.930(16) . . no
C17 H9 0.917(17) . . no
C21 H8 0.96(2) . . no
C21 H15 0.95(2) . . no
C21 H11 0.95(2) . . no
C25 H34 0.96(2) . . no
C25 H10 0.95(2) . . no
C25 H18 0.95(2) . . no
C27 H17 0.96(3) . . no
C27 H12 0.96(3) . . no
C27 H23 0.96(2) . . no
C24 C26 1.472(5) . . no
C24 H1 0.96(3) . . no
C24 H2 0.97(2) . . no
C24 H241 0.96(3) . . no
C26 H3 0.98(2) . . no
C26 H13 0.97(2) . . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O6 H4 Cl4 0.84(3) 2.25(3) 3.077(2) 172(3) 3_655 yes
N14 H5 Cl4 0.862(18) 2.339(19) 3.143(2) 155.4(18) 4_554 yes
N14 H6 Cl4 0.873(19) 2.414(18) 3.235(3) 156.9(16) 2_655 yes
N13 H7 Cl4 0.858(17) 2.340(17) 3.174(2) 164.5(19) . yes
