#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:02:21 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179649 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/02/4510289.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_4510289
loop_
_publ_author_name
'Wöhlert, Susanne'
'Runčevski, Tomče'
'Dinnebier, Robert E.'
'Ebbinghaus, Stefan G.'
'Näther, Christian'
_publ_section_title
;
 Synthesis, Structures, Polymorphism, and Magnetic Properties of
 Transition Metal Thiocyanato Coordination Compounds
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1902
_journal_paper_doi               10.1021/cg500037d
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C16 H18 N4 Ni S2'
_chemical_formula_weight         389.17
_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                67.460(5)
_cell_angle_beta                 67.360(5)
_cell_angle_gamma                83.940(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9684(6)
_cell_length_b                   10.6770(7)
_cell_length_c                   10.9560(7)
_cell_measurement_temperature    200(2)
_cell_volume                     893.21(11)
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_collection       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  IPDS-2
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9813
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  0.8285
_exptl_absorpt_correction_T_min  0.5959
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE)'
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0516
_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)+(0.0688P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                2603
_reflns_number_total             4281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Compound_3-Ni_I_RM254.CIF
_cod_data_source_block           Compound_3-Ni/I_(RM254)
_cod_original_cell_volume        893.21(10)
_cod_database_code               4510289
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
Ni1 Ni 1.0000 0.5000 0.5000 0.02843(17) Uani 1 2 d S
Ni2 Ni 0.5000 0.5000 1.0000 0.02896(17) Uani 1 2 d S
N1 N 0.9007(3) 0.6080(3) 0.6274(3) 0.0329(7) Uani 1 1 d .
C1 C 0.8360(4) 0.6324(4) 0.7287(4) 0.0307(8) Uani 1 1 d .
S1 S 0.74439(11) 0.66634(11) 0.87362(10) 0.0375(2) Uani 1 1 d .
N2 N 0.5859(3) 0.4035(3) 0.8601(3) 0.0325(7) Uani 1 1 d .
C2 C 0.6592(4) 0.3709(4) 0.7655(4) 0.0310(7) Uani 1 1 d .
S2 S 0.76738(11) 0.32447(10) 0.63129(10) 0.0354(2) Uani 1 1 d .
N10 N 0.8834(3) 0.6182(3) 0.3604(3) 0.0330(7) Uani 1 1 d .
C10 C 0.9578(4) 0.6594(4) 0.2182(4) 0.0355(8) Uani 1 1 d .
H10 H 1.0628 0.6290 0.1801 0.043 Uiso 1 1 calc R
C11 C 0.8891(4) 0.7435(4) 0.1251(4) 0.0376(8) Uani 1 1 d .
H11 H 0.9461 0.7684 0.0254 0.045 Uiso 1 1 calc R
C12 C 0.7369(4) 0.7926(4) 0.1756(4) 0.0347(8) Uani 1 1 d .
C13 C 0.6595(4) 0.7482(4) 0.3237(4) 0.0387(8) Uani 1 1 d .
H13 H 0.5544 0.7771 0.3645 0.046 Uiso 1 1 calc R
C14 C 0.7353(4) 0.6624(4) 0.4114(4) 0.0375(8) Uani 1 1 d .
H14 H 0.6800 0.6336 0.5117 0.045 Uiso 1 1 calc R
C15 C 0.6582(5) 0.8884(4) 0.0788(5) 0.0407(9) Uani 1 1 d .
H15A H 0.5777 0.9388 0.1316 0.049 Uiso 1 1 calc R
H15B H 0.5991 0.8344 0.0542 0.049 Uiso 1 1 calc R
C16 C 0.7743(6) 0.9900(5) -0.0582(5) 0.0551(12) Uani 1 1 d .
H16A H 0.7137 1.0480 -0.1150 0.083 Uiso 1 1 calc R
H16B H 0.8532 0.9414 -0.1126 0.083 Uiso 1 1 calc R
H16C H 0.8311 1.0463 -0.0354 0.083 Uiso 1 1 calc R
N20 N 0.3818(4) 0.6356(3) 0.8707(3) 0.0335(7) Uani 1 1 d .
C20 C 0.3206(5) 0.5947(4) 0.7965(4) 0.0406(9) Uani 1 1 d .
H20 H 0.3303 0.5027 0.8045 0.049 Uiso 1 1 calc R
C21 C 0.2444(5) 0.6803(4) 0.7093(5) 0.0440(9) Uani 1 1 d .
H21 H 0.2029 0.6467 0.6593 0.053 Uiso 1 1 calc R
C22 C 0.2289(5) 0.8151(5) 0.6952(4) 0.0420(9) Uani 1 1 d .
C23 C 0.2908(5) 0.8560(4) 0.7721(5) 0.0457(9) Uani 1 1 d .
H23 H 0.2821 0.9473 0.7666 0.055 Uiso 1 1 calc R
C24 C 0.3655(5) 0.7645(4) 0.8573(4) 0.0416(9) Uani 1 1 d .
H24 H 0.4073 0.7958 0.9087 0.050 Uiso 1 1 calc R
C25 C 0.1529(5) 0.9146(5) 0.5963(5) 0.0521(11) Uani 1 1 d .
H25A H 0.0871 0.8634 0.5745 0.063 Uiso 1 1 calc R
H25B H 0.0796 0.9712 0.6454 0.063 Uiso 1 1 calc R
C26 C 0.2772(7) 1.0055(6) 0.4590(6) 0.0696(15) Uani 1 1 d .
H26A H 0.2226 1.0680 0.3990 0.104 Uiso 1 1 calc R
H26B H 0.3484 0.9500 0.4088 0.104 Uiso 1 1 calc R
H26C H 0.3414 1.0575 0.4799 0.104 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 Ni1 N1 180.000(1) . 2_766
N1 Ni1 N10 89.57(12) . 2_766
N1 Ni1 N10 90.43(12) 2_766 2_766
N1 Ni1 N10 90.43(12) . .
N1 Ni1 N10 89.57(12) 2_766 .
N10 Ni1 N10 180.0 2_766 .
N1 Ni1 S2 93.95(9) . .
N1 Ni1 S2 86.05(9) 2_766 .
N10 Ni1 S2 89.89(9) 2_766 .
N10 Ni1 S2 90.11(9) . .
N1 Ni1 S2 86.05(9) . 2_766
N1 Ni1 S2 93.95(9) 2_766 2_766
N10 Ni1 S2 90.11(9) 2_766 2_766
N10 Ni1 S2 89.89(9) . 2_766
S2 Ni1 S2 180.00(5) . 2_766
N2 Ni2 N2 180.000(1) . 2_667
N2 Ni2 N20 90.12(12) . 2_667
N2 Ni2 N20 89.88(12) 2_667 2_667
N2 Ni2 N20 89.88(12) . .
N2 Ni2 N20 90.12(12) 2_667 .
N20 Ni2 N20 180.000(1) 2_667 .
N2 Ni2 S1 86.53(9) . 2_667
N2 Ni2 S1 93.47(9) 2_667 2_667
N20 Ni2 S1 90.18(9) 2_667 2_667
N20 Ni2 S1 89.82(9) . 2_667
N2 Ni2 S1 93.47(9) . .
N2 Ni2 S1 86.53(9) 2_667 .
N20 Ni2 S1 89.82(9) 2_667 .
N20 Ni2 S1 90.18(9) . .
S1 Ni2 S1 180.0 2_667 .
C1 N1 Ni1 160.4(3) . .
N1 C1 S1 179.6(4) . .
C1 S1 Ni2 100.46(13) . .
C2 N2 Ni2 165.5(3) . .
N2 C2 S2 178.7(3) . .
C2 S2 Ni1 100.97(13) . .
C14 N10 C10 117.3(3) . .
C14 N10 Ni1 120.7(2) . .
C10 N10 Ni1 121.9(2) . .
N10 C10 C11 123.0(3) . .
C10 C11 C12 120.6(4) . .
C11 C12 C13 116.0(3) . .
C11 C12 C15 122.9(4) . .
C13 C12 C15 121.0(3) . .
C14 C13 C12 120.3(3) . .
N10 C14 C13 122.7(4) . .
C12 C15 C16 114.6(3) . .
C24 N20 C20 116.6(3) . .
C24 N20 Ni2 122.1(2) . .
C20 N20 Ni2 121.3(3) . .
N20 C20 C21 123.2(4) . .
C20 C21 C22 119.7(4) . .
C23 C22 C21 116.7(4) . .
C23 C22 C25 121.4(4) . .
C21 C22 C25 121.9(4) . .
C22 C23 C24 120.3(4) . .
N20 C24 C23 123.4(4) . .
C26 C25 C22 112.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.033(3) .
Ni1 N1 2.033(3) 2_766
Ni1 N10 2.121(3) 2_766
Ni1 N10 2.121(3) .
Ni1 S2 2.5263(10) .
Ni1 S2 2.5263(10) 2_766
Ni2 N2 2.034(3) .
Ni2 N2 2.034(3) 2_667
Ni2 N20 2.118(3) 2_667
Ni2 N20 2.118(3) .
Ni2 S1 2.5447(10) 2_667
Ni2 S1 2.5447(10) .
N1 C1 1.153(5) .
C1 S1 1.644(4) .
N2 C2 1.154(5) .
C2 S2 1.646(4) .
N10 C14 1.341(4) .
N10 C10 1.342(5) .
C10 C11 1.376(5) .
C11 C12 1.390(5) .
C12 C13 1.397(6) .
C12 C15 1.504(5) .
C13 C14 1.386(5) .
C15 C16 1.517(6) .
N20 C24 1.325(5) .
N20 C20 1.349(5) .
C20 C21 1.384(5) .
C21 C22 1.386(6) .
C22 C23 1.379(6) .
C22 C25 1.517(6) .
C23 C24 1.385(5) .
C25 C26 1.505(7) .
