#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:03:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179275 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/95/4319574.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_4319574
loop_
_publ_author_name
'Olivier J. Dautel'
'Marc Fourmigué'
_publ_section_title
;
 Stabilization of Isolated Mixed-Valence Trimers in a Novel Nickel
 Dithiolene Complex with CF2 Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2083
_journal_page_last               2087
_journal_paper_doi               10.1021/ic0013835
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         3(C10H8F8NiS8),3(C6H4S4),CH2Cl2
_chemical_formula_sum            'C49 H36 Cl2 F12 Ni3 S36'
_chemical_formula_weight         2253.97
_chemical_name_common            '[(F4Ni)3 (TTF)3,CH2Cl2]'
_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                91.10(3)
_cell_angle_beta                 110.78(3)
_cell_angle_gamma                116.01(3)
_cell_formula_units_Z            1
_cell_length_a                   12.330(3)
_cell_length_b                   12.726(3)
_cell_length_c                   15.706(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      1.85
_cell_volume                     2025.5(12)
_computing_cell_refinement       'Select, cell (STOE-IPDS)'
_computing_data_collection       'Expose (STOE-IPDS)'
_computing_data_reduction        'integrate (STOE-IPDS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, phi inc.=1.6'
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.1714
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19853
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.749
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_correction_T_min  0.7826
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Faceit, STOE-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0450
_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 
 [0.00000+1.00000exp(3.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+3.0000*P+(0.0264P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                3076
_reflns_number_total             7360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0013835_2.cif
_cod_data_source_block           doe36bmer
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2025.3(7)
_cod_database_code               4319574
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 0.5000 0.5000 0.5000 0.0333(3) Uani 1 2 d S . .
S1 S 0.35738(18) 0.5253(2) 0.39101(13) 0.0416(5) Uani 1 1 d . . .
S2 S 0.61180(18) 0.5218(2) 0.41904(14) 0.0423(5) Uani 1 1 d . . .
S4 S 0.3257(2) 0.5888(2) 0.20699(15) 0.0483(5) Uani 1 1 d . . .
S3 S 0.6040(2) 0.5882(2) 0.23955(15) 0.0478(5) Uani 1 1 d . . .
C1 C 0.4131(7) 0.5524(7) 0.3056(5) 0.0375(18) Uani 1 1 d . . .
C2 C 0.5306(6) 0.5518(7) 0.3184(5) 0.0355(18) Uani 1 1 d . . .
C3 C 0.4888(8) 0.4659(7) 0.1406(5) 0.046(2) Uani 1 1 d . . .
H3A H 0.5354 0.4586 0.1044 0.055 Uiso 1 1 calc R . .
H3B H 0.4566 0.3926 0.1630 0.055 Uiso 1 1 calc R . .
C4 C 0.3718(8) 0.4783(7) 0.0773(5) 0.0437(19) Uani 1 1 d . . .
C5 C 0.2730(8) 0.4692(8) 0.1147(6) 0.050(2) Uani 1 1 d . . .
H5A H 0.2449 0.3951 0.1369 0.060 Uiso 1 1 calc R . .
H5B H 0.1964 0.4634 0.0636 0.060 Uiso 1 1 calc R . .
F1 F 0.4127(5) 0.5800(4) 0.0448(3) 0.0587(13) Uani 1 1 d . . .
F2 F 0.3081(5) 0.3889(5) -0.0004(3) 0.0666(14) Uani 1 1 d . . .
Ni2 Ni 0.67972(9) 0.85661(9) 0.45947(7) 0.0366(2) Uani 1 1 d . . .
S5 S 0.55729(18) 0.83406(19) 0.53380(14) 0.0437(5) Uani 1 1 d . . .
S6 S 0.54640(19) 0.8912(2) 0.34763(14) 0.0435(5) Uani 1 1 d . . .
S7 S 0.5430(2) 0.9734(2) 0.17300(15) 0.0476(5) Uani 1 1 d . . .
S8 S 0.82016(19) 0.96014(19) 0.21572(14) 0.0456(5) Uani 1 1 d . . .
S9 S 0.80455(19) 0.88104(19) 0.38749(14) 0.0426(5) Uani 1 1 d . . .
S10 S 0.81757(19) 0.82784(19) 0.57172(14) 0.0423(5) Uani 1 1 d . . .
S11 S 0.8403(2) 0.7728(2) 0.75698(14) 0.0461(5) Uani 1 1 d . . .
S12 S 0.56602(19) 0.7825(2) 0.71859(15) 0.0489(5) Uani 1 1 d . . .
C6 C 0.6180(7) 0.9257(7) 0.2694(5) 0.0376(18) Uani 1 1 d . . .
C7 C 0.4945(8) 0.8612(8) 0.0769(5) 0.047(2) Uani 1 1 d . . .
H7A H 0.4592 0.7839 0.0936 0.056 Uiso 1 1 calc R . .
H7B H 0.4234 0.8619 0.0246 0.056 Uiso 1 1 calc R . .
C8 C 0.5978(8) 0.8718(8) 0.0459(5) 0.047(2) Uani 1 1 d . . .
C9 C 0.7068(8) 0.8503(8) 0.1091(5) 0.045(2) Uani 1 1 d . . .
H9A H 0.7569 0.8458 0.0747 0.054 Uiso 1 1 calc R . .
H9B H 0.6674 0.7730 0.1249 0.054 Uiso 1 1 calc R . .
C10 C 0.7329(7) 0.9215(7) 0.2874(5) 0.0376(17) Uani 1 1 d . . .
C11 C 0.7526(7) 0.8011(7) 0.6541(5) 0.0390(18) Uani 1 1 d . . .
C12 C 0.9024(7) 0.9076(8) 0.8367(5) 0.046(2) Uani 1 1 d . . .
H12A H 0.9804 0.9183 0.8892 0.055 Uiso 1 1 calc R . .
H12B H 0.9293 0.9742 0.8061 0.055 Uiso 1 1 calc R . .
C13 C 0.8067(8) 0.9117(8) 0.8727(6) 0.049(2) Uani 1 1 d . . .
C14 C 0.6849(8) 0.9150(8) 0.8079(6) 0.050(2) Uani 1 1 d . . .
H14A H 0.7118 0.9825 0.7781 0.060 Uiso 1 1 calc R . .
H14B H 0.6420 0.9291 0.8446 0.060 Uiso 1 1 calc R . .
C15 C 0.6367(7) 0.8024(7) 0.6373(5) 0.0418(19) Uani 1 1 d . . .
F3 F 0.7698(5) 0.8205(5) 0.9176(3) 0.0646(14) Uani 1 1 d . . .
F4 F 0.8745(5) 1.0139(5) 0.9408(4) 0.0769(17) Uani 1 1 d . . .
F5 F 0.5372(5) 0.7905(5) -0.0368(3) 0.0631(14) Uani 1 1 d . . .
F6 F 0.6514(5) 0.9795(5) 0.0226(3) 0.0632(14) Uani 1 1 d . . .
S13 S 0.9631(2) 0.6487(2) 0.51895(18) 0.0600(6) Uani 1 1 d . . .
S14 S 1.20446(19) 0.6377(2) 0.55312(19) 0.0627(7) Uani 1 1 d . . .
C16 C 1.0356(7) 0.5619(7) 0.5152(6) 0.048(2) Uani 1 1 d . . .
C17 C 1.2162(9) 0.7742(8) 0.5775(7) 0.068(3) Uani 1 1 d . . .
H17 H 1.2978 0.8428 0.6013 0.081 Uiso 1 1 calc R . .
C18 C 1.1070(9) 0.7809(8) 0.5620(7) 0.069(3) Uani 1 1 d . . .
H18 H 1.1084 0.8535 0.5738 0.083 Uiso 1 1 calc R . .
S15 S 0.9809(2) 1.5829(2) 0.73496(19) 0.0619(7) Uani 1 1 d . . .
S16 S 0.8075(2) 1.2950(2) 0.65850(19) 0.0645(7) Uani 1 1 d . . .
S17 S 1.0496(2) 1.2813(2) 0.6954(2) 0.0678(7) Uani 1 1 d . . .
S18 S 1.2207(2) 1.5653(2) 0.7723(2) 0.0731(8) Uani 1 1 d . . .
C19 C 1.0502(7) 1.4904(8) 0.7322(6) 0.056(2) Uani 1 1 d . . .
C20 C 0.9785(8) 1.3713(7) 0.6994(7) 0.055(2) Uani 1 1 d . . .
C21 C 0.7959(9) 1.1579(8) 0.6345(7) 0.066(3) Uani 1 1 d . . .
H21 H 0.7140 1.0896 0.6098 0.079 Uiso 1 1 calc R . .
C22 C 0.9030(9) 1.1505(8) 0.6513(7) 0.064(3) Uani 1 1 d . . .
H22 H 0.9004 1.0772 0.6398 0.077 Uiso 1 1 calc R . .
C23 C 1.2373(9) 1.7032(8) 0.7992(7) 0.067(3) Uani 1 1 d . . .
H23 H 1.3199 1.7704 0.8270 0.081 Uiso 1 1 calc R . .
C24 C 1.1249(5) 1.7107(5) 0.7784(3) 0.064(3) Uani 1 1 d . . .
H24 H 1.1273 1.7842 0.7877 0.077 Uiso 1 1 calc R . .
Cl1 Cl 0.0064(5) 0.7385(5) 0.1014(3) 0.127(3) Uani 0.50 1 d PR . .
Cl2 Cl 0.1255(5) 0.6627(5) -0.0029(3) 0.172(5) Uani 0.50 1 d PR . .
C25 C 0.1333(5) 0.7415(5) 0.0963(3) 0.083(6) Uiso 0.50 1 d PR . .
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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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
S1 Ni1 S1 179.999(1) . 2_666 ?
S1 Ni1 S2 89.02(8) . 2_666 ?
S1 Ni1 S2 90.98(8) 2_666 2_666 ?
S1 Ni1 S2 90.98(8) . . ?
S1 Ni1 S2 89.02(8) 2_666 . ?
S2 Ni1 S2 180.00(13) 2_666 . ?
C1 S1 Ni1 105.6(3) . . ?
C2 S2 Ni1 105.5(2) . . ?
C1 S4 C5 103.1(4) . . ?
C2 S3 C3 102.5(4) . . ?
C2 C1 S1 119.1(6) . . ?
C2 C1 S4 122.3(6) . . ?
S1 C1 S4 118.5(4) . . ?
C1 C2 S2 118.6(6) . . ?
C1 C2 S3 123.5(6) . . ?
S2 C2 S3 117.7(4) . . ?
C4 C3 S3 114.8(5) . . ?
F1 C4 F2 104.2(6) . . ?
F1 C4 C5 110.0(7) . . ?
F2 C4 C5 107.9(7) . . ?
F1 C4 C3 110.3(7) . . ?
F2 C4 C3 106.3(6) . . ?
C5 C4 C3 117.3(7) . . ?
C4 C5 S4 116.8(6) . . ?
S9 Ni2 S10 87.18(8) . . ?
S9 Ni2 S6 92.01(9) . . ?
S10 Ni2 S6 178.16(10) . . ?
S9 Ni2 S5 179.03(10) . . ?
S10 Ni2 S5 92.16(9) . . ?
S6 Ni2 S5 88.64(9) . . ?
C15 S5 Ni2 103.6(3) . . ?
C6 S6 Ni2 104.3(3) . . ?
C6 S7 C7 103.1(4) . . ?
C10 S8 C9 103.2(4) . . ?
C10 S9 Ni2 103.8(3) . . ?
C11 S10 Ni2 104.4(3) . . ?
C11 S11 C12 100.7(4) . . ?
C15 S12 C14 101.5(4) . . ?
C10 C6 S6 119.4(6) . . ?
C10 C6 S7 123.6(6) . . ?
S6 C6 S7 116.9(4) . . ?
C8 C7 S7 116.7(6) . . ?
F6 C8 F5 104.0(6) . . ?
F6 C8 C7 110.3(7) . . ?
F5 C8 C7 107.7(7) . . ?
F6 C8 C9 109.0(7) . . ?
F5 C8 C9 106.7(6) . . ?
C7 C8 C9 118.2(7) . . ?
C8 C9 S8 116.2(5) . . ?
C6 C10 S9 120.4(6) . . ?
C6 C10 S8 124.3(6) . . ?
S9 C10 S8 115.3(4) . . ?
C15 C11 S10 119.9(6) . . ?
C15 C11 S11 122.9(6) . . ?
S10 C11 S11 117.2(4) . . ?
C13 C12 S11 114.7(6) . . ?
F3 C13 F4 104.9(7) . . ?
F3 C13 C12 109.6(7) . . ?
F4 C13 C12 107.1(7) . . ?
F3 C13 C14 108.5(7) . . ?
F4 C13 C14 105.5(6) . . ?
C12 C13 C14 120.1(7) . . ?
C13 C14 S12 115.5(6) . . ?
C11 C15 S5 119.9(6) . . ?
C11 C15 S12 123.4(6) . . ?
S5 C15 S12 116.6(4) . . ?
C18 S13 C16 95.3(4) . . ?
C17 S14 C16 94.3(4) . . ?
C16 C16 S13 122.9(7) 2_766 . ?
C16 C16 S14 121.7(7) 2_766 . ?
S13 C16 S14 115.4(4) . . ?
C18 C17 S14 118.8(7) . . ?
C17 C18 S13 116.3(7) . . ?
C24 S15 C19 95.5(3) . . ?
C21 S16 C20 94.3(4) . . ?
C22 S17 C20 94.9(4) . . ?
C23 S18 C19 95.4(4) . . ?
C20 C19 S18 122.4(6) . . ?
C20 C19 S15 123.4(6) . . ?
S18 C19 S15 114.1(5) . . ?
C19 C20 S17 122.6(6) . . ?
C19 C20 S16 123.0(6) . . ?
S17 C20 S16 114.4(5) . . ?
C22 C21 S16 119.1(7) . . ?
C21 C22 S17 117.3(7) . . ?
C24 C23 S18 117.0(6) . . ?
C23 C24 S15 117.8(5) . . ?
Cl1 C25 Cl2 121.8 . . ?
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 S1 2.123(2) . ?
Ni1 S1 2.123(2) 2_666 ?
Ni1 S2 2.125(2) 2_666 ?
Ni1 S2 2.125(2) . ?
S1 C1 1.690(8) . ?
S2 C2 1.697(8) . ?
S4 C1 1.748(8) . ?
S4 C5 1.794(8) . ?
S3 C2 1.737(8) . ?
S3 C3 1.804(8) . ?
C1 C2 1.393(9) . ?
C3 C4 1.510(10) . ?
C4 F1 1.350(9) . ?
C4 F2 1.373(9) . ?
C4 C5 1.492(11) . ?
Ni2 S9 2.138(2) . ?
Ni2 S10 2.139(2) . ?
Ni2 S6 2.144(2) . ?
Ni2 S5 2.147(2) . ?
S5 C15 1.733(8) . ?
S6 C6 1.713(8) . ?
S7 C6 1.746(8) . ?
S7 C7 1.789(8) . ?
S8 C10 1.756(8) . ?
S8 C9 1.802(8) . ?
S9 C10 1.721(8) . ?
S10 C11 1.716(8) . ?
S11 C11 1.741(8) . ?
S11 C12 1.783(8) . ?
S12 C15 1.750(8) . ?
S12 C14 1.800(9) . ?
C6 C10 1.368(9) . ?
C7 C8 1.473(11) . ?
C8 F6 1.358(9) . ?
C8 F5 1.377(9) . ?
C8 C9 1.501(11) . ?
C11 C15 1.366(10) . ?
C12 C13 1.497(10) . ?
C13 F3 1.359(10) . ?
C13 F4 1.375(9) . ?
C13 C14 1.505(11) . ?
S13 C18 1.710(10) . ?
S13 C16 1.711(7) . ?
S14 C17 1.703(9) . ?
S14 C16 1.719(8) . ?
C16 C16 1.393(15) 2_766 ?
C17 C18 1.321(12) . ?
S15 C24 1.682(6) . ?
S15 C19 1.739(8) . ?
S16 C21 1.709(9) . ?
S16 C20 1.738(8) . ?
S17 C22 1.717(9) . ?
S17 C20 1.733(8) . ?
S18 C23 1.702(9) . ?
S18 C19 1.733(8) . ?
C19 C20 1.348(11) . ?
C21 C22 1.299(12) . ?
C23 C24 1.354(10) . ?
Cl1 C25 1.5782 . ?
Cl2 C25 1.7875 . ?
