#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:54:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179268 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318857.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_4318857
loop_
_publ_author_name
'Xiaoming Ren'
'Qingjin Meng'
'You Song'
'Chuanjiang Hu'
'Changsheng Lu'
'Xiaoyuan Chen'
'Ziling Xue'
_publ_section_title
;
 Unusual Magnetic Property Associated with Dimerization within a Nickel
 Tetramer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5931
_journal_page_last               5933
_journal_paper_doi               10.1021/ic0255860
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C20 H13 N6 Ni S4'
_chemical_formula_weight         524.31
_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                74.00(3)
_cell_angle_beta                 77.30(3)
_cell_angle_gamma                68.04(3)
_cell_formula_units_Z            4
_cell_length_a                   11.220(2)
_cell_length_b                   14.295(3)
_cell_length_c                   15.609(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.4
_cell_measurement_theta_min      11.1
_cell_volume                     2212.7(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'FR590 CAD4'
_diffrn_measurement_method       '2θ/ω 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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8207
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0321
_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)+(0.0550P)²+1.4218P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                5239
_reflns_number_total             7766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255860_s3_1.cif
_cod_data_source_block           Complex1_293K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2212.7(8)
_cod_database_code               4318857
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 0.81213(4) 0.55603(3) 0.49249(3) 0.03994(13) Uani 1 1 d . . .
Ni2 Ni 0.49514(4) 0.36313(3) 0.32837(3) 0.04576(13) Uani 1 1 d . . .
S1 S 0.80562(9) 0.40465(7) 0.56021(6) 0.0476(2) Uani 1 1 d . . .
S2 S 0.86938(9) 0.57698(7) 0.60611(6) 0.0488(2) Uani 1 1 d . . .
S3 S 0.76144(10) 0.53486(7) 0.37576(6) 0.0515(2) Uani 1 1 d . . .
S4 S 0.81320(9) 0.70923(7) 0.42853(6) 0.0504(2) Uani 1 1 d . . .
S5 S 0.48389(11) 0.21235(7) 0.39028(7) 0.0614(3) Uani 1 1 d . . .
S6 S 0.55132(10) 0.37703(7) 0.44619(6) 0.0530(2) Uani 1 1 d . . .
S7 S 0.42810(10) 0.35149(7) 0.21453(7) 0.0546(2) Uani 1 1 d . . .
S8 S 0.50342(10) 0.51490(7) 0.26540(7) 0.0554(2) Uani 1 1 d . . .
C1 C 0.8570(4) 0.2929(3) 0.7269(2) 0.0519(9) Uani 1 1 d . . .
C2 C 0.8496(3) 0.3888(2) 0.6631(2) 0.0414(7) Uani 1 1 d . . .
C3 C 0.8775(3) 0.4642(2) 0.6833(2) 0.0403(7) Uani 1 1 d . . .
C4 C 0.9171(3) 0.4510(3) 0.7688(2) 0.0465(8) Uani 1 1 d . . .
C5 C 0.7264(4) 0.6611(3) 0.2111(3) 0.0589(10) Uani 1 1 d . . .
C6 C 0.7537(3) 0.6496(3) 0.3001(2) 0.0477(8) Uani 1 1 d . . .
C7 C 0.7757(3) 0.7258(3) 0.3235(2) 0.0471(8) Uani 1 1 d . . .
C8 C 0.7652(4) 0.8229(3) 0.2611(3) 0.0585(10) Uani 1 1 d . . .
C9 C 0.5165(5) 0.0988(3) 0.5594(3) 0.0788(13) Uani 1 1 d . . .
C10 C 0.5194(4) 0.1926(3) 0.4965(3) 0.0564(9) Uani 1 1 d . . .
C11 C 0.5481(3) 0.2646(3) 0.5210(2) 0.0493(8) Uani 1 1 d . . .
C12 C 0.5755(4) 0.2486(3) 0.6107(3) 0.0551(9) Uani 1 1 d . . .
C13 C 0.3557(4) 0.4904(3) 0.0624(3) 0.0549(9) Uani 1 1 d . . .
C14 C 0.4095(3) 0.4707(3) 0.1436(2) 0.0478(8) Uani 1 1 d . . .
C15 C 0.4438(3) 0.5423(3) 0.1657(2) 0.0490(8) Uani 1 1 d . . .
C16 C 0.4328(4) 0.6403(3) 0.1061(3) 0.0576(10) Uani 1 1 d . . .
C17 C -0.3261(4) 1.0331(3) 0.8592(2) 0.0547(9) Uani 1 1 d . . .
H17A H -0.3010 1.0874 0.8218 0.066 Uiso 1 1 calc R . .
C18 C -0.4163(4) 1.0059(3) 0.8359(3) 0.0617(10) Uani 1 1 d . . .
H18A H -0.4523 1.0414 0.7829 0.074 Uiso 1 1 calc R . .
C19 C -0.4553(4) 0.9242(3) 0.8915(3) 0.0589(10) Uani 1 1 d . . .
C20 C -0.3994(3) 0.8750(3) 0.9705(3) 0.0549(9) Uani 1 1 d . . .
H20A H -0.4240 0.8214 1.0100 0.066 Uiso 1 1 calc R . .
C21 C -0.3101(3) 0.9051(3) 0.9896(2) 0.0522(9) Uani 1 1 d . . .
H21A H -0.2729 0.8709 1.0422 0.063 Uiso 1 1 calc R . .
C22 C -0.1691(4) 1.0093(3) 0.9582(3) 0.0565(10) Uani 1 1 d . . .
H22A H -0.1875 1.0138 1.0209 0.068 Uiso 1 1 calc R . .
H22B H -0.1682 1.0762 0.9220 0.068 Uiso 1 1 calc R . .
C23 C -0.0380(3) 0.9294(3) 0.9421(2) 0.0476(8) Uani 1 1 d . . .
C24 C 0.0091(4) 0.8446(3) 1.0086(2) 0.0523(9) Uani 1 1 d . . .
H24A H -0.0404 0.8368 1.0646 0.063 Uiso 1 1 calc R . .
C25 C 0.1283(4) 0.7711(3) 0.9937(3) 0.0600(10) Uani 1 1 d . . .
H25A H 0.1584 0.7144 1.0395 0.072 Uiso 1 1 calc R . .
C26 C 0.2034(4) 0.7810(3) 0.9114(3) 0.0614(10) Uani 1 1 d . . .
H26A H 0.2837 0.7311 0.9012 0.074 Uiso 1 1 calc R . .
C27 C 0.1583(4) 0.8652(4) 0.8446(3) 0.0674(11) Uani 1 1 d . . .
H27A H 0.2089 0.8727 0.7890 0.081 Uiso 1 1 calc R . .
C28 C 0.0391(4) 0.9387(3) 0.8590(2) 0.0592(10) Uani 1 1 d . . .
H28A H 0.0097 0.9953 0.8129 0.071 Uiso 1 1 calc R . .
C29 C -0.1328(4) 0.7369(3) 0.7572(3) 0.0588(10) Uani 1 1 d . . .
H29A H -0.2023 0.7712 0.7243 0.071 Uiso 1 1 calc R . .
C30 C -0.1568(4) 0.7011(3) 0.8472(3) 0.0604(10) Uani 1 1 d . . .
H30A H -0.2415 0.7097 0.8747 0.072 Uiso 1 1 calc R . .
C31 C -0.0538(5) 0.6512(3) 0.8980(3) 0.0628(11) Uani 1 1 d . . .
C32 C 0.0712(5) 0.6333(3) 0.8511(3) 0.0699(12) Uani 1 1 d . . .
H32A H 0.1428 0.5954 0.8815 0.084 Uiso 1 1 calc R . .
C33 C 0.0882(4) 0.6710(3) 0.7618(3) 0.0687(11) Uani 1 1 d . . .
H33A H 0.1721 0.6595 0.7319 0.082 Uiso 1 1 calc R . .
C34 C 0.0074(5) 0.7796(4) 0.6197(3) 0.0790(13) Uani 1 1 d . . .
H34A H -0.0664 0.7921 0.5903 0.095 Uiso 1 1 calc R . .
H34B H 0.0841 0.7371 0.5880 0.095 Uiso 1 1 calc R . .
C35 C 0.0233(4) 0.8814(3) 0.6155(2) 0.0584(10) Uani 1 1 d . . .
C36 C 0.1436(4) 0.8900(3) 0.6051(3) 0.0670(11) Uani 1 1 d . . .
H36A H 0.2173 0.8327 0.5988 0.080 Uiso 1 1 calc R . .
C37 C 0.1565(5) 0.9830(4) 0.6040(3) 0.0729(12) Uani 1 1 d . . .
H37A H 0.2385 0.9880 0.5972 0.087 Uiso 1 1 calc R . .
C38 C 0.0498(5) 1.0667(4) 0.6127(3) 0.0735(12) Uani 1 1 d . . .
H38A H 0.0588 1.1291 0.6116 0.088 Uiso 1 1 calc R . .
C39 C -0.0713(5) 1.0603(3) 0.6231(3) 0.0747(12) Uani 1 1 d . . .
H39A H -0.1444 1.1179 0.6295 0.090 Uiso 1 1 calc R . .
C40 C -0.0847(4) 0.9677(4) 0.6243(3) 0.0693(11) Uani 1 1 d . . .
H40A H -0.1670 0.9633 0.6310 0.083 Uiso 1 1 calc R . .
N1 N 0.8636(4) 0.2177(3) 0.7778(2) 0.0788(11) Uani 1 1 d . . .
N2 N 0.9488(3) 0.4411(3) 0.8363(2) 0.0634(9) Uani 1 1 d . . .
N3 N 0.7082(4) 0.6712(3) 0.1399(2) 0.0813(11) Uani 1 1 d . . .
N4 N 0.7563(4) 0.8995(3) 0.2114(3) 0.0876(12) Uani 1 1 d . . .
N5 N 0.5167(6) 0.0263(4) 0.6133(3) 0.128(2) Uani 1 1 d . . .
N6 N 0.5967(4) 0.2326(3) 0.6828(3) 0.0741(10) Uani 1 1 d . . .
N7 N 0.3109(4) 0.5044(3) -0.0003(2) 0.0742(10) Uani 1 1 d . . .
N8 N 0.4235(4) 0.7180(3) 0.0567(3) 0.0799(11) Uani 1 1 d . . .
N9 N -0.5444(4) 0.8954(3) 0.8718(3) 0.0896(13) Uani 1 1 d . . .
H9A H -0.5679 0.8461 0.9081 0.108 Uiso 1 1 calc R . .
H9B H -0.5784 0.9262 0.8229 0.108 Uiso 1 1 calc R . .
N10 N -0.2724(3) 0.9831(2) 0.93523(19) 0.0487(7) Uani 1 1 d . . .
N11 N -0.0735(5) 0.6207(3) 0.9872(2) 0.0906(13) Uani 1 1 d . . .
H11A H -0.1512 0.6316 1.0147 0.109 Uiso 1 1 calc R . .
H11B H -0.0086 0.5901 1.0171 0.109 Uiso 1 1 calc R . .
N12 N -0.0122(3) 0.7245(2) 0.7144(2) 0.0568(8) 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 0.0033 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
_geom_angle_publ_flag
S2 Ni1 S4 86.60(5) . . ?
S2 Ni1 S3 177.92(4) . . ?
S4 Ni1 S3 92.66(5) . . ?
S2 Ni1 S1 92.47(4) . . ?
S4 Ni1 S1 177.95(4) . . ?
S3 Ni1 S1 88.33(4) . . ?
S7 Ni2 S5 86.86(5) . . ?
S7 Ni2 S8 92.38(5) . . ?
S5 Ni2 S8 179.03(4) . . ?
S7 Ni2 S6 176.78(4) . . ?
S5 Ni2 S6 92.55(5) . . ?
S8 Ni2 S6 88.17(5) . . ?
C2 S1 Ni1 102.93(12) . . ?
C3 S2 Ni1 103.47(12) . . ?
C6 S3 Ni1 102.85(13) . . ?
C7 S4 Ni1 103.23(13) . . ?
C10 S5 Ni2 103.08(13) . . ?
C11 S6 Ni2 102.85(13) . . ?
C14 S7 Ni2 103.39(13) . . ?
C15 S8 Ni2 103.53(13) . . ?
N1 C1 C2 179.1(4) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 S1 120.8(2) . . ?
C1 C2 S1 118.0(3) . . ?
C2 C3 C4 121.3(3) . . ?
C2 C3 S2 120.4(2) . . ?
C4 C3 S2 118.3(3) . . ?
N2 C4 C3 179.4(4) . . ?
N3 C5 C6 177.9(4) . . ?
C7 C6 C5 121.2(3) . . ?
C7 C6 S3 120.7(3) . . ?
C5 C6 S3 118.1(3) . . ?
C6 C7 C8 120.6(3) . . ?
C6 C7 S4 120.6(3) . . ?
C8 C7 S4 118.7(3) . . ?
N4 C8 C7 179.3(5) . . ?
N5 C9 C10 175.5(5) . . ?
C11 C10 C9 120.6(4) . . ?
C11 C10 S5 120.7(3) . . ?
C9 C10 S5 118.8(3) . . ?
C10 C11 C12 120.5(3) . . ?
C10 C11 S6 120.8(3) . . ?
C12 C11 S6 118.7(3) . . ?
N6 C12 C11 177.7(4) . . ?
N7 C13 C14 178.0(4) . . ?
C15 C14 C13 122.6(3) . . ?
C15 C14 S7 120.3(3) . . ?
C13 C14 S7 117.1(3) . . ?
C14 C15 C16 120.8(3) . . ?
C14 C15 S8 120.2(3) . . ?
C16 C15 S8 119.0(3) . . ?
N8 C16 C15 178.4(4) . . ?
N10 C17 C18 121.4(3) . . ?
C17 C18 C19 120.0(4) . . ?
N9 C19 C20 120.5(4) . . ?
N9 C19 C18 122.1(4) . . ?
C20 C19 C18 117.3(3) . . ?
C21 C20 C19 119.8(3) . . ?
C20 C21 N10 122.4(3) . . ?
N10 C22 C23 111.3(3) . . ?
C24 C23 C28 117.8(4) . . ?
C24 C23 C22 121.1(3) . . ?
C28 C23 C22 121.0(3) . . ?
C25 C24 C23 121.1(4) . . ?
C26 C25 C24 120.5(4) . . ?
C27 C26 C25 119.1(4) . . ?
C26 C27 C28 120.7(4) . . ?
C27 C28 C23 120.7(4) . . ?
N12 C29 C30 122.2(4) . . ?
C29 C30 C31 119.7(4) . . ?
N11 C31 C30 121.6(5) . . ?
N11 C31 C32 121.4(4) . . ?
C30 C31 C32 117.0(4) . . ?
C33 C32 C31 120.1(4) . . ?
N12 C33 C32 122.2(4) . . ?
N12 C34 C35 110.5(3) . . ?
C36 C35 C40 118.6(4) . . ?
C36 C35 C34 121.3(4) . . ?
C40 C35 C34 120.0(4) . . ?
C35 C36 C37 120.6(4) . . ?
C38 C37 C36 120.0(4) . . ?
C37 C38 C39 120.5(4) . . ?
C38 C39 C40 119.7(4) . . ?
C35 C40 C39 120.5(4) . . ?
C17 N10 C21 119.1(3) . . ?
C17 N10 C22 121.3(3) . . ?
C21 N10 C22 119.6(3) . . ?
C29 N12 C33 118.5(4) . . ?
C29 N12 C34 119.8(4) . . ?
C33 N12 C34 121.3(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 S2 2.1414(10) . ?
Ni1 S4 2.1452(11) . ?
Ni1 S3 2.1500(11) . ?
Ni1 S1 2.1514(11) . ?
Ni2 S7 2.1436(11) . ?
Ni2 S5 2.1441(12) . ?
Ni2 S8 2.1487(12) . ?
Ni2 S6 2.1503(11) . ?
S1 C2 1.714(3) . ?
S2 C3 1.711(3) . ?
S3 C6 1.721(3) . ?
S4 C7 1.714(4) . ?
S5 C10 1.713(4) . ?
S6 C11 1.714(3) . ?
S7 C14 1.723(4) . ?
S8 C15 1.717(4) . ?
C1 N1 1.134(5) . ?
C1 C2 1.440(5) . ?
C2 C3 1.358(5) . ?
C3 C4 1.439(5) . ?
C4 N2 1.141(4) . ?
C5 N3 1.134(5) . ?
C5 C6 1.441(5) . ?
C6 C7 1.357(5) . ?
C7 C8 1.439(5) . ?
C8 N4 1.138(5) . ?
C9 N5 1.139(5) . ?
C9 C10 1.434(6) . ?
C10 C11 1.352(5) . ?
C11 C12 1.438(5) . ?
C12 N6 1.145(5) . ?
C13 N7 1.133(5) . ?
C13 C14 1.436(5) . ?
C14 C15 1.365(5) . ?
C15 C16 1.431(5) . ?
C16 N8 1.146(5) . ?
C17 N10 1.344(4) . ?
C17 C18 1.358(5) . ?
C18 C19 1.402(5) . ?
C19 N9 1.332(5) . ?
C19 C20 1.393(5) . ?
C20 C21 1.343(5) . ?
C21 N10 1.347(4) . ?
C22 N10 1.480(4) . ?
C22 C23 1.507(5) . ?
C23 C24 1.377(5) . ?
C23 C28 1.395(5) . ?
C24 C25 1.376(5) . ?
C25 C26 1.375(6) . ?
C26 C27 1.370(6) . ?
C27 C28 1.375(6) . ?
C29 N12 1.341(5) . ?
C29 C30 1.359(5) . ?
C30 C31 1.397(6) . ?
C31 N11 1.334(5) . ?
C31 C32 1.397(6) . ?
C32 C33 1.347(6) . ?
C33 N12 1.347(5) . ?
C34 N12 1.482(5) . ?
C34 C35 1.513(6) . ?
C35 C36 1.371(6) . ?
C35 C40 1.382(6) . ?
C36 C37 1.386(6) . ?
C37 C38 1.353(6) . ?
C38 C39 1.367(6) . ?
C39 C40 1.382(6) . ?
