#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:09:52 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179914 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/09/7020988.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_7020988
loop_
_publ_author_name
'Yu, Shan-Shan'
'Duan, Hai-Bao'
'Chen, Xuan-Rong'
'Tian, Zheng-Fang'
'Ren, Xiao-Ming'
_publ_section_title
;
 Observation of intramolecular vibrations cooperating with the magnetic
 phase transition in a nickel-bis-dithiolene compound.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3827
_journal_page_last               3834
_journal_paper_doi               10.1039/c2dt31519j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C15 H26 N4, C16 N8 Ni2 S8'
_chemical_formula_sum            'C31 H26 N12 Ni2 S8'
_chemical_formula_weight         940.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.318(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.080(3)
_cell_length_b                   7.1663(10)
_cell_length_c                   31.103(4)
_cell_measurement_reflns_used    4756
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.530
_cell_measurement_theta_min      1.350
_cell_volume                     4120.7(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and 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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            17371
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920.0
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00132(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0523P)²+1.4715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                2732
_reflns_number_total             4719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31519j.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7020988
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'
'-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
Ni1 Ni 0.290456(18) 0.40567(5) 0.274329(12) 0.06065(16) Uani 1 1 d .
S1 S 0.22984(4) 0.40885(10) 0.32407(3) 0.0677(2) Uani 1 1 d .
S2 S 0.39242(4) 0.40034(12) 0.32320(3) 0.0738(2) Uani 1 1 d .
S3 S 0.18886(4) 0.40564(11) 0.22551(3) 0.0674(2) Uani 1 1 d .
S4 S 0.35118(4) 0.40848(11) 0.22474(3) 0.0723(2) Uani 1 1 d .
N1 N 0.2544(2) 0.4173(6) 0.44550(13) 0.1254(13) Uani 1 1 d .
N2 N 0.4695(2) 0.3928(5) 0.44382(11) 0.1125(12) Uani 1 1 d .
N3 N 0.1146(2) 0.4112(4) 0.10342(11) 0.1028(10) Uani 1 1 d .
N4 N 0.3264(2) 0.4221(5) 0.10339(12) 0.1188(13) Uani 1 1 d .
N5 N 0.43242(15) 0.9021(4) 0.08187(9) 0.0770(7) Uani 1 1 d .
N6 N 0.39263(16) 1.0888(4) 0.02695(9) 0.0835(8) Uani 1 1 d .
C1 C 0.2733(2) 0.4119(5) 0.41341(14) 0.0875(10) Uani 1 1 d .
C2 C 0.29604(19) 0.4056(4) 0.37302(11) 0.0707(8) Uani 1 1 d .
C3 C 0.36699(18) 0.4020(4) 0.37249(11) 0.0706(8) Uani 1 1 d .
C4 C 0.42378(19) 0.3968(5) 0.41238(13) 0.0839(10) Uani 1 1 d .
C5 C 0.1584(2) 0.4103(4) 0.13570(12) 0.0767(9) Uani 1 1 d .
C6 C 0.21391(18) 0.4096(3) 0.17630(10) 0.0646(8) Uani 1 1 d .
C7 C 0.28500(18) 0.4112(4) 0.17609(11) 0.0686(8) Uani 1 1 d .
C8 C 0.3077(2) 0.4170(4) 0.13552(13) 0.0841(10) Uani 1 1 d .
C9 C 0.5000 0.9655(6) 0.2500 0.0719(11) Uani 1 2 d S
H9A H 0.4588 1.0451 0.2499 0.086 Uiso 0.50 1 calc PR
H9B H 0.5412 1.0451 0.2501 0.086 Uiso 0.50 1 calc PR
C10 C 0.48359(16) 0.8470(5) 0.20853(10) 0.0731(8) Uani 1 1 d .
H10A H 0.4429 0.7667 0.2092 0.088 Uiso 1 1 calc R
H10B H 0.5249 0.7670 0.2094 0.088 Uiso 1 1 calc R
C11 C 0.46606(17) 0.9524(4) 0.16455(10) 0.0733(9) Uani 1 1 d .
H11A H 0.4243 1.0320 0.1628 0.088 Uiso 1 1 calc R
H11B H 0.5067 1.0310 0.1628 0.088 Uiso 1 1 calc R
C12 C 0.45046(19) 0.8167(5) 0.12628(11) 0.0852(10) Uani 1 1 d .
H12A H 0.4925 0.7373 0.1288 0.102 Uiso 1 1 calc R
H12B H 0.4105 0.7375 0.1289 0.102 Uiso 1 1 calc R
C13 C 0.40656(19) 1.0685(5) 0.07057(12) 0.0823(10) Uani 1 1 d .
H13 H 0.3990 1.1595 0.0903 0.099 Uiso 1 1 calc R
C14 C 0.3619(2) 1.2553(6) 0.00179(12) 0.1100(13) Uani 1 1 d .
H14A H 0.3487 1.3443 0.0215 0.165 Uiso 1 1 calc R
H14B H 0.3197 1.2208 -0.0208 0.165 Uiso 1 1 calc R
H14C H 0.3971 1.3096 -0.0118 0.165 Uiso 1 1 calc R
C15 C 0.4110(2) 0.9291(6) 0.00988(13) 0.1081(14) Uani 1 1 d .
H15 H 0.4072 0.9052 -0.0200 0.130 Uiso 1 1 calc R
C16 C 0.4356(2) 0.8107(6) 0.04348(14) 0.1115(14) Uani 1 1 d .
H16 H 0.4518 0.6894 0.0413 0.134 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
S4 Ni1 S3 92.59(4) . .
S4 Ni1 S1 178.85(3) . .
S3 Ni1 S1 87.52(3) . .
S4 Ni1 S2 87.33(4) . .
S3 Ni1 S2 178.97(3) . .
S1 Ni1 S2 92.59(4) . .
C2 S1 Ni1 103.23(12) . .
C3 S2 Ni1 102.97(12) . .
C6 S3 Ni1 103.26(11) . .
C7 S4 Ni1 102.93(12) . .
C13 N5 C16 107.2(3) . .
C13 N5 C12 128.1(3) . .
C16 N5 C12 124.5(3) . .
C13 N6 C15 107.8(3) . .
C13 N6 C14 126.0(3) . .
C15 N6 C14 126.2(3) . .
N1 C1 C2 179.4(4) . .
C3 C2 C1 122.2(3) . .
C3 C2 S1 120.3(3) . .
C1 C2 S1 117.5(3) . .
C2 C3 C4 122.2(3) . .
C2 C3 S2 120.9(3) . .
C4 C3 S2 116.9(3) . .
N2 C4 C3 179.2(4) . .
N3 C5 C6 179.7(4) . .
C7 C6 C5 121.2(3) . .
C7 C6 S3 120.3(3) . .
C5 C6 S3 118.6(3) . .
C6 C7 C8 121.6(3) . .
C6 C7 S4 120.9(3) . .
C8 C7 S4 117.4(3) . .
N4 C8 C7 179.3(5) . .
C10 C9 C10 111.6(4) . 2_655
C10 C9 H9A 109.3 . .
C10 C9 H9A 109.3 2_655 .
C10 C9 H9B 109.3 . .
C10 C9 H9B 109.3 2_655 .
H9A C9 H9B 108.0 . .
C9 C10 C11 116.1(3) . .
C9 C10 H10A 108.3 . .
C11 C10 H10A 108.3 . .
C9 C10 H10B 108.3 . .
C11 C10 H10B 108.3 . .
H10A C10 H10B 107.4 . .
C12 C11 C10 110.2(3) . .
C12 C11 H11A 109.6 . .
C10 C11 H11A 109.6 . .
C12 C11 H11B 109.6 . .
C10 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
N5 C12 C11 115.3(3) . .
N5 C12 H12A 108.4 . .
C11 C12 H12A 108.4 . .
N5 C12 H12B 108.4 . .
C11 C12 H12B 108.4 . .
H12A C12 H12B 107.5 . .
N5 C13 N6 110.1(3) . .
N5 C13 H13 125.0 . .
N6 C13 H13 125.0 . .
N6 C14 H14A 109.5 . .
N6 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N6 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16 C15 N6 107.9(4) . .
C16 C15 H15 126.1 . .
N6 C15 H15 126.1 . .
C15 C16 N5 107.1(4) . .
C15 C16 H16 126.5 . .
N5 C16 H16 126.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S4 2.1461(9) .
Ni1 S3 2.1466(8) .
Ni1 S1 2.1487(9) .
Ni1 S2 2.1527(9) .
S1 C2 1.721(3) .
S2 C3 1.719(4) .
S3 C6 1.713(3) .
S4 C7 1.714(3) .
N1 C1 1.142(5) .
N2 C4 1.138(4) .
N3 C5 1.136(4) .
N4 C8 1.142(5) .
N5 C13 1.305(4) .
N5 C16 1.376(4) .
N5 C12 1.472(4) .
N6 C13 1.324(4) .
N6 C15 1.344(4) .
N6 C14 1.467(4) .
C1 C2 1.428(5) .
C2 C3 1.358(5) .
C3 C4 1.432(5) .
C5 C6 1.434(5) .
C6 C7 1.358(4) .
C7 C8 1.432(5) .
C9 C10 1.511(4) .
C9 C10 1.511(4) 2_655
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.526(4) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.509(4) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 H13 0.9300 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C16 1.338(5) .
C15 H15 0.9300 .
C16 H16 0.9300 .
