#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:05:59 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179775 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/71/7007163.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_7007163
loop_
_publ_author_name
'Deplano, Paola'
'Faulmann, Christophe'
'Mercuri, Maria Laura'
'Pilia, Luca'
'Salidu, Marco'
'Serpe, Angela'
_publ_section_title
;
 Synthesis, crystal structure and properties of the semiconducting
 salts (TTF)2[Ni(dtcr)2] and (ET)2[Ni(dtcr)2] based on [Ni(dtcr)2]
 dianions (dtcr = dithiocroconate).
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2456
_journal_page_last               2462
_journal_paper_doi               10.1039/b600820h
_journal_year                    2006
_chemical_formula_moiety         '2(C10 H8 S8), C10 Ni O6 S4'
_chemical_formula_sum            'C30 H16 Ni O6 S20'
_chemical_formula_weight         1172.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.039(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3700(7)
_cell_length_b                   7.4410(6)
_cell_length_c                   28.278(2)
_cell_measurement_reflns_used    1268
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.7
_cell_measurement_theta_min      3.5
_cell_volume                     1947.1(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
;
_computing_molecular_graphics
'Cameron (Watkin et al., 1996); Ortep3 (Farrugia, 1997); Mercury (CCDC, 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir97 (Altomare, 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'XCalibur Oxford Diffraction'
_diffrn_measurement_method       'φ scan '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            20052
_diffrn_reflns_theta_full        32.14
_diffrn_reflns_theta_max         32.14
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  0.8302
_exptl_absorpt_correction_T_min  0.6053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.625
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0340
_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)+(0.0233P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                4443
_reflns_number_total             6442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b600820h.txt
_cod_data_source_block           (ET)2[Ni(dtcroc)2]
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7007163
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.5000 0.5000 0.5000 0.01381(8) Uani 1 2 d S . .
S1 S 0.30646(5) 0.63564(7) 0.463924(17) 0.01758(11) Uani 1 1 d . . .
S2 S 0.58404(5) 0.44917(7) 0.433776(17) 0.01654(11) Uani 1 1 d . . .
C1 C 0.3313(2) 0.6231(3) 0.40621(6) 0.0138(4) Uani 1 1 d . . .
C2 C 0.4537(2) 0.5415(3) 0.39255(6) 0.0136(4) Uani 1 1 d . . .
C3 C 0.2360(2) 0.6939(3) 0.36437(7) 0.0157(4) Uani 1 1 d . . .
C5 C 0.3128(2) 0.6543(3) 0.32239(7) 0.0166(4) Uani 1 1 d . . .
C4 C 0.4481(2) 0.5506(3) 0.34100(7) 0.0152(4) Uani 1 1 d . . .
O1 O 0.11942(15) 0.7676(2) 0.36240(5) 0.0248(3) Uani 1 1 d . . .
O2 O 0.27117(16) 0.6981(2) 0.28083(5) 0.0277(4) Uani 1 1 d . . .
O3 O 0.53388(14) 0.49195(19) 0.31609(5) 0.0199(3) Uani 1 1 d . . .
S11 S 0.18729(5) 0.13993(7) 0.673312(17) 0.01841(11) Uani 1 1 d . . .
S12 S 0.50338(5) -0.03139(7) 0.638144(18) 0.01942(12) Uani 1 1 d . . .
S13 S 0.09723(5) 0.20112(7) 0.568995(17) 0.01625(11) Uani 1 1 d . . .
S14 S 0.35689(5) 0.04407(7) 0.541266(17) 0.01800(11) Uani 1 1 d . . .
S15 S -0.01925(5) 0.29431(7) 0.456793(17) 0.01681(11) Uani 1 1 d . . .
S16 S 0.24384(5) 0.14012(7) 0.431449(17) 0.01815(11) Uani 1 1 d . . .
S17 S -0.14977(5) 0.39219(7) 0.359430(18) 0.01835(11) Uani 1 1 d . . .
S18 S 0.17537(5) 0.22366(7) 0.328031(18) 0.01934(12) Uani 1 1 d . . .
C11 C 0.3621(2) 0.1043(3) 0.70930(7) 0.0181(4) Uani 1 1 d . . .
C12 C 0.4420(2) -0.0592(3) 0.69499(7) 0.0190(4) Uani 1 1 d . . .
C13 C 0.2269(2) 0.1209(3) 0.61538(6) 0.0141(4) Uani 1 1 d . . .
C14 C 0.3494(2) 0.0505(3) 0.60213(7) 0.0149(4) Uani 1 1 d . . .
C15 C 0.1937(2) 0.1487(3) 0.52371(7) 0.0145(4) Uani 1 1 d . . .
C16 C 0.1438(2) 0.1889(3) 0.47572(7) 0.0144(4) Uani 1 1 d . . .
C17 C -0.0021(2) 0.2992(3) 0.39623(6) 0.0147(4) Uani 1 1 d . . .
C18 C 0.1228(2) 0.2306(3) 0.38455(6) 0.0146(4) Uani 1 1 d . . .
C19 C -0.0775(2) 0.4216(3) 0.30420(7) 0.0169(4) Uani 1 1 d . . .
C20 C 0.0038(2) 0.2599(3) 0.28987(7) 0.0182(4) Uani 1 1 d . . .
H122 H 0.384(2) -0.168(3) 0.6930(7) 0.024(6) Uiso 1 1 d . . .
H112 H 0.420(2) 0.211(3) 0.7098(7) 0.017(5) Uiso 1 1 d . . .
H111 H 0.341(2) 0.084(2) 0.7406(7) 0.015(5) Uiso 1 1 d . . .
H192 H -0.021(2) 0.528(3) 0.3069(7) 0.022(6) Uiso 1 1 d . . .
H201 H -0.047(2) 0.155(3) 0.2898(7) 0.023(6) Uiso 1 1 d . . .
H202 H 0.033(2) 0.273(3) 0.2607(8) 0.021(6) Uiso 1 1 d . . .
H191 H -0.168(2) 0.449(3) 0.2812(8) 0.034(7) Uiso 1 1 d . . .
H121 H 0.534(2) -0.075(3) 0.7161(8) 0.030(6) Uiso 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'
O O 0.0106 0.0060 '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 S2 180.0 . 3_666 ?
S2 Ni1 S1 86.299(19) . 3_666 ?
S2 Ni1 S1 93.701(18) 3_666 3_666 ?
S2 Ni1 S1 93.701(18) . . ?
S2 Ni1 S1 86.299(18) 3_666 . ?
S1 Ni1 S1 180.00(2) 3_666 . ?
C1 S1 Ni1 101.28(7) . . ?
C2 S2 Ni1 101.69(6) . . ?
C2 C1 C3 110.74(16) . . ?
C2 C1 S1 122.21(15) . . ?
C3 C1 S1 127.04(14) . . ?
C1 C2 C4 110.69(16) . . ?
C1 C2 S2 121.12(14) . . ?
C4 C2 S2 128.19(14) . . ?
O1 C3 C1 128.99(18) . . ?
O1 C3 C5 125.96(18) . . ?
C1 C3 C5 105.04(16) . . ?
O2 C5 C4 126.57(18) . . ?
O2 C5 C3 125.74(18) . . ?
C4 C5 C3 107.68(16) . . ?
O3 C4 C2 129.39(18) . . ?
O3 C4 C5 124.88(18) . . ?
C2 C4 C5 105.71(16) . . ?
C13 S11 C11 102.09(9) . . ?
C14 S12 C12 102.19(10) . . ?
C15 S13 C13 95.52(9) . . ?
C15 S14 C14 95.84(9) . . ?
C16 S15 C17 95.77(9) . . ?
C16 S16 C18 96.24(9) . . ?
C17 S17 C19 101.20(9) . . ?
C18 S18 C20 100.91(9) . . ?
C12 C11 S11 114.15(15) . . ?
C12 C11 H112 111.7(12) . . ?
S11 C11 H112 110.2(12) . . ?
C12 C11 H111 107.7(11) . . ?
S11 C11 H111 104.1(12) . . ?
H112 C11 H111 108.6(16) . . ?
C11 C12 S12 112.69(14) . . ?
C11 C12 H122 112.9(12) . . ?
S12 C12 H122 107.4(13) . . ?
C11 C12 H121 110.8(13) . . ?
S12 C12 H121 100.8(13) . . ?
H122 C12 H121 111.7(17) . . ?
C14 C13 S11 126.98(15) . . ?
C14 C13 S13 116.11(14) . . ?
S11 C13 S13 116.91(11) . . ?
C13 C14 S14 116.70(14) . . ?
C13 C14 S12 128.93(15) . . ?
S14 C14 S12 114.36(11) . . ?
C16 C15 S14 121.69(14) . . ?
C16 C15 S13 122.55(15) . . ?
S14 C15 S13 115.76(11) . . ?
C15 C16 S16 121.67(15) . . ?
C15 C16 S15 122.96(14) . . ?
S16 C16 S15 115.35(11) . . ?
C18 C17 S17 129.51(15) . . ?
C18 C17 S15 116.38(15) . . ?
S17 C17 S15 114.12(11) . . ?
C17 C18 S16 116.21(14) . . ?
C17 C18 S18 127.51(15) . . ?
S16 C18 S18 116.27(10) . . ?
C20 C19 S17 114.02(15) . . ?
C20 C19 H192 112.8(12) . . ?
S17 C19 H192 108.1(12) . . ?
C20 C19 H191 113.5(13) . . ?
S17 C19 H191 100.9(13) . . ?
H192 C19 H191 106.6(17) . . ?
C19 C20 S18 113.35(15) . . ?
C19 C20 H201 113.3(13) . . ?
S18 C20 H201 106.8(13) . . ?
C19 C20 H202 112.9(13) . . ?
S18 C20 H202 100.8(13) . . ?
H201 C20 H202 108.8(18) . . ?
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 2.1756(5) . ?
Ni1 S2 2.1756(5) 3_666 ?
Ni1 S1 2.1833(5) 3_666 ?
Ni1 S1 2.1833(5) . ?
S1 C1 1.6869(19) . ?
S2 C2 1.6954(19) . ?
C1 C2 1.405(3) . ?
C1 C3 1.464(3) . ?
C2 C4 1.452(3) . ?
C3 O1 1.216(2) . ?
C3 C5 1.511(3) . ?
C5 O2 1.223(2) . ?
C5 C4 1.507(3) . ?
C4 O3 1.229(2) . ?
S11 C13 1.7413(19) . ?
S11 C11 1.807(2) . ?
S12 C14 1.740(2) . ?
S12 C12 1.802(2) . ?
S13 C15 1.7246(19) . ?
S13 C13 1.7472(19) . ?
S14 C15 1.7178(19) . ?
S14 C14 1.7340(19) . ?
S15 C16 1.7257(19) . ?
S15 C17 1.7452(19) . ?
S16 C16 1.7167(19) . ?
S16 C18 1.7394(19) . ?
S17 C17 1.7387(19) . ?
S17 C19 1.810(2) . ?
S18 C18 1.7457(19) . ?
S18 C20 1.810(2) . ?
C11 C12 1.517(3) . ?
C11 H112 0.96(2) . ?
C11 H111 0.951(19) . ?
C12 H122 0.97(2) . ?
C12 H121 0.97(2) . ?
C13 C14 1.367(3) . ?
C15 C16 1.397(3) . ?
C17 C18 1.365(3) . ?
C19 C20 1.513(3) . ?
C19 H192 0.94(2) . ?
C19 H191 1.00(2) . ?
C20 H201 0.92(2) . ?
C20 H202 0.92(2) . ?
