#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:02:21 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179649 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/02/4510290.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_4510290
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           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.200(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.1707(8)
_cell_length_b                   39.5124(19)
_cell_length_c                   9.1330(7)
_cell_measurement_temperature    200(2)
_cell_volume                     3647.5(5)
_computing_cell_refinement       'STOE IPDS-1 program package'
_computing_data_collection       'STOE IPDS-1 program package'
_computing_data_reduction        'STOE IPDS-1 program package'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi 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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20354
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  0.8779
_exptl_absorpt_correction_T_min  0.7714
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8521
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0553P)²+4.7701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                7390
_reflns_number_total             8521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Compound_3-Ni_II_RM209A.CIF
_cod_data_source_block           Compound_3-Ni/II_(RM209A)
_cod_original_cell_volume        3647.5(4)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4510290
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
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 0.55761(5) 0.627945(15) 0.81070(6) 0.01829(12) Uani 1 1 d . . .
Ni2 Ni 1.06570(6) 0.623125(16) 0.82975(7) 0.01955(12) Uani 1 1 d . . .
N1 N 0.7294(4) 0.65452(10) 0.8771(5) 0.0230(8) Uani 1 1 d . . .
C1 C 0.8434(4) 0.65875(11) 0.9255(5) 0.0185(8) Uani 1 1 d . . .
S1 S 1.00234(10) 0.66461(3) 0.99704(14) 0.0260(2) Uani 1 1 d . . .
N2 N 0.8861(4) 0.59988(11) 0.7435(5) 0.0246(8) Uani 1 1 d . . .
C2 C 0.7788(5) 0.59296(12) 0.7087(5) 0.0221(9) Uani 1 1 d . . .
S2 S 0.62197(10) 0.58302(3) 0.66240(13) 0.0254(2) Uani 1 1 d . . .
N3 N 0.2424(4) 0.64772(10) 0.9150(5) 0.0257(8) Uani 1 1 d . . .
C3 C 0.3465(4) 0.65845(11) 0.9340(5) 0.0185(8) Uani 1 1 d . . .
S3 S 0.48974(10) 0.67309(3) 0.95891(13) 0.0245(2) Uani 1 1 d . . .
N4 N 0.3868(4) 0.60119(10) 0.7440(5) 0.0217(7) Uani 1 1 d . . .
C4 C 0.2823(5) 0.59223(12) 0.7121(5) 0.0207(9) Uani 1 1 d . . .
S4 S 0.12725(11) 0.58000(3) 0.66509(15) 0.0313(3) Uani 1 1 d . . .
N10 N 0.6459(3) 0.59907(9) 1.0280(4) 0.0195(7) Uani 1 1 d . . .
C10 C 0.7698(4) 0.58878(10) 1.0879(5) 0.0265(8) Uani 1 1 d . . .
H10 H 0.8235 0.5958 1.0362 0.032 Uiso 1 1 calc R . .
C11 C 0.8255(4) 0.56805(11) 1.2236(5) 0.0302(8) Uani 1 1 d . . .
H11 H 0.9155 0.5614 1.2630 0.036 Uiso 1 1 calc R . .
C12 C 0.7492(5) 0.55711(12) 1.3016(5) 0.0307(10) Uani 1 1 d . . .
C13 C 0.6202(4) 0.56933(11) 1.2414(5) 0.0317(8) Uani 1 1 d . . .
H13 H 0.5655 0.5637 1.2939 0.038 Uiso 1 1 calc R . .
C14 C 0.5715(4) 0.58977(10) 1.1046(5) 0.0285(8) Uani 1 1 d . . .
H14 H 0.4826 0.5975 1.0638 0.034 Uiso 1 1 calc R . .
C15 C 0.8011(5) 0.53221(12) 1.4393(5) 0.0329(10) Uani 1 1 d . . .
H15A H 0.8960 0.5368 1.5069 0.040 Uiso 1 1 calc R . .
H15B H 0.7530 0.5352 1.5078 0.040 Uiso 1 1 calc R . .
C16 C 0.7852(8) 0.49674(14) 1.3799(8) 0.0689(18) Uani 1 1 d . . .
H16A H 0.8211 0.4812 1.4723 0.103 Uiso 1 1 calc R . .
H16B H 0.8330 0.4937 1.3123 0.103 Uiso 1 1 calc R . .
H16C H 0.6911 0.4919 1.3158 0.103 Uiso 1 1 calc R . .
N20 N 0.4691(4) 0.65627(10) 0.5925(5) 0.0281(8) Uani 1 1 d . . .
C20 C 0.3398(4) 0.66567(10) 0.5316(5) 0.0260(8) Uani 1 1 d . . .
H20 H 0.2873 0.6579 0.5836 0.031 Uiso 1 1 calc R . .
C21 C 0.2820(4) 0.68614(11) 0.3969(5) 0.0286(8) Uani 1 1 d . . .
H21 H 0.1913 0.6921 0.3575 0.034 Uiso 1 1 calc R . .
C22 C 0.3571(5) 0.69789(11) 0.3194(5) 0.0263(9) Uani 1 1 d . . .
C23 C 0.4872(4) 0.68772(11) 0.3807(5) 0.0320(9) Uani 1 1 d . . .
H23 H 0.5413 0.6950 0.3298 0.038 Uiso 1 1 calc R . .
C24 C 0.5400(4) 0.66705(11) 0.5159(5) 0.0297(8) Uani 1 1 d . . .
H24 H 0.6300 0.6603 0.5552 0.036 Uiso 1 1 calc R . .
C25 C 0.2977(5) 0.72222(12) 0.1777(6) 0.0347(10) Uani 1 1 d . . .
H25A H 0.3549 0.7229 0.1196 0.042 Uiso 1 1 calc R . .
H25B H 0.2098 0.7137 0.1014 0.042 Uiso 1 1 calc R . .
C26 C 0.2825(8) 0.75771(15) 0.2297(8) 0.0624(17) Uani 1 1 d . . .
H26A H 0.2448 0.7724 0.1343 0.094 Uiso 1 1 calc R . .
H26B H 0.3694 0.7664 0.3042 0.094 Uiso 1 1 calc R . .
H26C H 0.2236 0.7573 0.2842 0.094 Uiso 1 1 calc R . .
N30 N 1.1424(3) 0.59008(9) 1.0296(5) 0.0219(7) Uani 1 1 d . . .
C30 C 1.2310(4) 0.60006(11) 1.1762(5) 0.0315(9) Uani 1 1 d . . .
H30 H 1.2592 0.6230 1.1892 0.038 Uiso 1 1 calc R . .
C31 C 1.2836(5) 0.57903(13) 1.3093(5) 0.0408(11) Uani 1 1 d . . .
H31 H 1.3490 0.5873 1.4089 0.049 Uiso 1 1 calc R . .
C32 C 1.2408(6) 0.54575(14) 1.2976(6) 0.0401(12) Uani 1 1 d . . .
C33 C 1.1453(5) 0.53532(12) 1.1468(6) 0.0424(11) Uani 1 1 d . . .
H33 H 1.1120 0.5128 1.1326 0.051 Uiso 1 1 calc R . .
C34 C 1.0991(4) 0.55781(11) 1.0177(5) 0.0346(9) Uani 1 1 d . . .
H34 H 1.0341 0.5502 0.9164 0.042 Uiso 1 1 calc R . .
C35 C 1.2973(8) 0.52195(19) 1.4397(8) 0.0628(18) Uani 1 1 d . . .
H35A H 1.3370 0.5353 1.5407 0.075 Uiso 1 1 calc R . .
H35B H 1.2247 0.5082 1.4440 0.075 Uiso 1 1 calc R . .
C36 C 1.3993(9) 0.49898(19) 1.4310(9) 0.086(3) Uani 1 1 d . . .
H36A H 1.4327 0.4841 1.5257 0.129 Uiso 1 1 calc R . .
H36B H 1.4724 0.5124 1.4293 0.129 Uiso 1 1 calc R . .
H36C H 1.3600 0.4853 1.3322 0.129 Uiso 1 1 calc R . .
N40 N 0.9936(5) 0.65640(11) 0.6302(5) 0.0340(10) Uani 1 1 d . A .
C40 C 0.9054(5) 0.64704(13) 0.4828(5) 0.0408(11) Uani 1 1 d . . .
H40 H 0.8768 0.6241 0.4677 0.049 Uiso 1 1 calc R . .
C41 C 0.8535(7) 0.66844(17) 0.3518(6) 0.0649(17) Uani 1 1 d . A .
H41 H 0.7922 0.6600 0.2499 0.078 Uiso 1 1 calc R . .
C42 C 0.8892(9) 0.7011(2) 0.3673(8) 0.069(2) Uani 1 1 d D . .
C43 C 0.9824(7) 0.71189(14) 0.5208(7) 0.0590(16) Uani 1 1 d . A .
H43 H 1.0122 0.7347 0.5371 0.071 Uiso 1 1 calc R . .
C44 C 1.0300(5) 0.68912(12) 0.6472(6) 0.0397(10) Uani 1 1 d . . .
H44 H 1.0911 0.6969 0.7506 0.048 Uiso 1 1 calc R A .
C45 C 0.8098(12) 0.7253(3) 0.2244(14) 0.052(3) Uiso 0.50 1 d PD A 1
H45A H 0.7509 0.7124 0.1274 0.062 Uiso 0.50 1 calc PR A 1
H45B H 0.7559 0.7413 0.2542 0.062 Uiso 0.50 1 calc PR A 1
C46 C 0.9186(12) 0.7439(4) 0.1943(16) 0.067(3) Uiso 0.50 1 d PD A 1
H46A H 0.8777 0.7602 0.1060 0.101 Uiso 0.50 1 calc PR A 1
H46B H 0.9704 0.7275 0.1649 0.101 Uiso 0.50 1 calc PR A 1
H46C H 0.9769 0.7559 0.2929 0.101 Uiso 0.50 1 calc PR A 1
C45' C 0.8749(16) 0.7281(4) 0.2309(18) 0.073(4) Uiso 0.50 1 d PD A 2
H45C H 0.9545 0.7426 0.2651 0.087 Uiso 0.50 1 calc PR A 2
H45D H 0.8595 0.7169 0.1275 0.087 Uiso 0.50 1 calc PR A 2
C46' C 0.7591(15) 0.7476(4) 0.217(2) 0.078(4) Uiso 0.50 1 d PD A 2
H46D H 0.7408 0.7653 0.1348 0.118 Uiso 0.50 1 calc PR A 2
H46E H 0.7765 0.7580 0.3212 0.118 Uiso 0.50 1 calc PR A 2
H46F H 0.6824 0.7325 0.1844 0.118 Uiso 0.50 1 calc PR A 2
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'
S S 0.1246 0.1234 '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'
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
N4 Ni1 N1 179.6(2) . .
N4 Ni1 N20 89.46(17) . .
N1 Ni1 N20 90.62(16) . .
N4 Ni1 N10 90.20(15) . .
N1 Ni1 N10 89.72(15) . .
N20 Ni1 N10 179.40(19) . .
N4 Ni1 S2 85.33(12) . .
N1 Ni1 S2 94.30(12) . .
N20 Ni1 S2 89.56(12) . .
N10 Ni1 S2 89.92(11) . .
N4 Ni1 S3 94.00(12) . .
N1 Ni1 S3 86.36(12) . .
N20 Ni1 S3 90.27(12) . .
N10 Ni1 S3 90.25(11) . .
S2 Ni1 S3 179.31(6) . .
N3 Ni2 N2 178.3(2) 1_655 .
N3 Ni2 N30 89.66(16) 1_655 .
N2 Ni2 N30 91.49(16) . .
N3 Ni2 N40 89.10(17) 1_655 .
N2 Ni2 N40 89.77(18) . .
N30 Ni2 N40 178.6(2) . .
N3 Ni2 S1 86.26(12) 1_655 .
N2 Ni2 S1 92.46(12) . .
N30 Ni2 S1 89.64(11) . .
N40 Ni2 S1 90.91(13) . .
N3 Ni2 S4 94.80(12) 1_655 1_655
N2 Ni2 S4 86.51(12) . 1_655
N30 Ni2 S4 89.10(11) . 1_655
N40 Ni2 S4 90.38(13) . 1_655
S1 Ni2 S4 178.35(6) . 1_655
C1 N1 Ni1 157.2(4) . .
N1 C1 S1 178.7(4) . .
C1 S1 Ni2 101.69(16) . .
C2 N2 Ni2 165.1(4) . .
N2 C2 S2 178.5(5) . .
C2 S2 Ni1 102.00(17) . .
C3 N3 Ni2 164.5(4) . 1_455
N3 C3 S3 179.5(5) . .
C3 S3 Ni1 100.09(16) . .
C4 N4 Ni1 166.3(4) . .
N4 C4 S4 178.6(5) . .
C4 S4 Ni2 99.54(16) . 1_455
C10 N10 C14 118.2(4) . .
C10 N10 Ni1 122.6(3) . .
C14 N10 Ni1 119.2(3) . .
N10 C10 C11 122.9(4) . .
C12 C11 C10 120.0(4) . .
C11 C12 C13 116.5(4) . .
C11 C12 C15 121.9(5) . .
C13 C12 C15 121.5(5) . .
C14 C13 C12 120.0(4) . .
N10 C14 C13 122.3(4) . .
C16 C15 C12 111.6(4) . .
C24 N20 C20 117.7(4) . .
C24 N20 Ni1 121.2(3) . .
C20 N20 Ni1 121.1(3) . .
N20 C20 C21 122.4(4) . .
C20 C21 C22 119.7(4) . .
C23 C22 C21 117.2(4) . .
C23 C22 C25 122.3(4) . .
C21 C22 C25 120.4(4) . .
C22 C23 C24 120.7(4) . .
N20 C24 C23 122.3(4) . .
C26 C25 C22 112.7(4) . .
C30 N30 C34 116.4(4) . .
C30 N30 Ni2 122.5(3) . .
C34 N30 Ni2 121.0(3) . .
N30 C30 C31 124.0(4) . .
C30 C31 C32 119.9(5) . .
C31 C32 C33 116.7(4) . .
C31 C32 C35 121.4(6) . .
C33 C32 C35 121.9(5) . .
C34 C33 C32 120.0(5) . .
N30 C34 C33 123.0(4) . .
C36 C35 C32 112.7(6) . .
C40 N40 C44 116.0(4) . .
C40 N40 Ni2 122.9(4) . .
C44 N40 Ni2 120.9(3) . .
N40 C40 C41 124.2(5) . .
C42 C41 C40 120.2(6) . .
C41 C42 C43 117.2(5) . .
C41 C42 C45 117.7(8) . .
C43 C42 C45 124.4(8) . .
C41 C42 C45' 129.4(8) . .
C43 C42 C45' 111.1(9) . .
C45 C42 C45' 26.1(6) . .
C44 C43 C42 119.6(6) . .
N40 C44 C43 122.7(5) . .
C46 C45 C42 103.4(10) . .
C46' C45' C42 102.3(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N4 2.034(4) .
Ni1 N1 2.040(4) .
Ni1 N20 2.127(4) .
Ni1 N10 2.132(4) .
Ni1 S2 2.5163(13) .
Ni1 S3 2.5422(13) .
Ni2 N3 2.034(4) 1_655
Ni2 N2 2.035(4) .
Ni2 N30 2.107(4) .
Ni2 N40 2.109(4) .
Ni2 S1 2.5383(13) .
Ni2 S4 2.5531(15) 1_655
N1 C1 1.169(6) .
C1 S1 1.626(5) .
N2 C2 1.134(6) .
C2 S2 1.665(5) .
N3 C3 1.179(6) .
N3 Ni2 2.034(4) 1_455
C3 S3 1.624(5) .
N4 C4 1.133(6) .
C4 S4 1.669(5) .
S4 Ni2 2.5531(15) 1_455
N10 C10 1.317(5) .
N10 C14 1.345(5) .
C10 C11 1.392(5) .
C11 C12 1.391(7) .
C12 C13 1.392(7) .
C12 C15 1.504(6) .
C13 C14 1.389(5) .
C15 C16 1.486(8) .
N20 C24 1.331(6) .
N20 C20 1.360(6) .
C20 C21 1.381(5) .
C21 C22 1.387(6) .
C22 C23 1.377(6) .
C22 C25 1.519(6) .
C23 C24 1.385(5) .
C25 C26 1.513(8) .
N30 C30 1.341(6) .
N30 C34 1.352(6) .
C30 C31 1.381(6) .
C31 C32 1.388(7) .
C32 C33 1.397(8) .
C32 C35 1.506(7) .
C33 C34 1.389(6) .
C35 C36 1.485(10) .
N40 C40 1.338(6) .
N40 C44 1.344(7) .
C40 C41 1.376(7) .
C41 C42 1.340(10) .
C42 C43 1.410(10) .
C42 C45 1.554(12) .
C42 C45' 1.596(14) .
C43 C44 1.379(7) .
C45 C46 1.543(15) .
C45' C46' 1.464(16) .
