#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:50:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180358 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/27/7202743.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_7202743
loop_
_publ_author_name
'Olivier Jeannin'
'Rodolphe Clérac'
'Marc Fourmigué'
_publ_section_title
;
 Trifluoromethyl order?disorder transition in nickel dithiolene uniform
 spin chains
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              488
_journal_paper_doi               10.1039/b701480e
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C12 H12 F6 N3 Ni S4'
_chemical_formula_weight         499.20
_chemical_name_common            'Me4N+, [Ni(tfadt)2]-'
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 97.587(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.016(3)
_cell_length_b                   7.4363(6)
_cell_length_c                   11.1585(10)
_cell_measurement_reflns_used    4539
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.4
_cell_volume                     1975.4(3)
_computing_cell_refinement       '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, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 1 deg'
_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  0.1049
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7693
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.5896
_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    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0648
_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)+(0.1173P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                1109
_reflns_number_total             1940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701480e.txt
_cod_data_source_block           oj133
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7202743
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Ni01 Ni 0.70063(4) 0.0000 0.47476(10) 0.0643(4) Uani 1 2 d S . .
S1 S 0.61032(11) 0.0000 0.4656(3) 0.0940(8) Uani 1 2 d S . .
S2 S 0.69631(12) 0.0000 0.2828(2) 0.0835(7) Uani 1 2 d S . .
S3 S 0.79012(9) 0.0000 0.4872(2) 0.0708(6) Uani 1 2 d S . .
S4 S 0.70450(10) 0.0000 0.6666(2) 0.0795(7) Uani 1 2 d S . .
C1 C 0.5867(5) 0.0000 0.3183(12) 0.093(3) Uani 1 2 d S . .
C2 C 0.6247(4) 0.0000 0.2346(9) 0.082(3) Uani 1 2 d S . .
C3 C 0.5274(7) 0.0000 0.2807(17) 0.140(6) Uani 1 2 d S . .
C4 C 0.6034(7) 0.0000 0.1020(11) 0.113(4) Uani 1 2 d S . .
C5 C 0.8130(3) 0.0000 0.6408(8) 0.064(2) Uani 1 2 d S . .
C6 C 0.7742(4) 0.0000 0.7215(8) 0.070(2) Uani 1 2 d S . .
C7 C 0.8737(5) 0.0000 0.6715(10) 0.085(3) Uani 1 2 d S . .
C8 C 0.7889(6) 0.0000 0.8488(12) 0.104(3) Uani 1 2 d S . .
C1B C 0.5602(7) 0.5000 0.6478(14) 0.150(7) Uani 0.86 2 d SP . .
H1B1 H 0.5522 0.6216 0.6223 0.224 Uiso 0.43 1 calc PR . .
H1B2 H 0.5257 0.4353 0.6482 0.224 Uiso 0.43 1 calc PR . .
H1B3 H 0.5824 0.4430 0.5930 0.224 Uiso 0.43 1 calc PR . .
C'1B C 0.656(2) 0.5000 0.808(5) 0.060(13) Uani 0.14 2 d SP . .
H'1A H 0.6636 0.5000 0.8942 0.090 Uiso 0.14 2 calc SPR . .
H'1B H 0.6718 0.6054 0.7762 0.090 Uiso 0.07 1 calc PR . .
H'1C H 0.6718 0.3946 0.7762 0.090 Uiso 0.07 1 calc PR . .
C2B C 0.5507(5) 0.5000 0.8608(12) 0.125(4) Uani 1 2 d S . .
H2B1 H 0.5711 0.5000 0.9408 0.187 Uiso 1 2 calc SR . .
H2B2 H 0.5275 0.3946 0.8501 0.187 Uiso 0.50 1 calc PR . .
H2B3 H 0.5275 0.6054 0.8501 0.187 Uiso 0.50 1 calc PR . .
C3B C 0.6267(5) 0.3389(13) 0.7909(12) 0.133(4) Uani 0.86 1 d P . .
H3B1 H 0.6464 0.3426 0.8715 0.199 Uiso 0.86 1 calc PR . .
H3B2 H 0.6533 0.3353 0.7338 0.199 Uiso 0.86 1 calc PR . .
H3B3 H 0.6035 0.2334 0.7816 0.199 Uiso 0.86 1 calc PR . .
C'3B C 0.573(2) 0.331(5) 0.702(6) 0.10(2) Uani 0.14 1 d P . .
H'3A H 0.5864 0.2288 0.7501 0.155 Uiso 0.14 1 calc PR . .
H'3B H 0.5880 0.3287 0.6269 0.155 Uiso 0.14 1 calc PR . .
H'3C H 0.5327 0.3278 0.6873 0.155 Uiso 0.14 1 calc PR . .
F1 F 0.6450(4) 0.0000 0.0354(8) 0.152(3) Uani 1 2 d S . .
F2 F 0.5715(4) -0.1418(9) 0.0694(6) 0.193(3) Uani 1 1 d . . .
F3 F 0.7700(4) 0.1357(8) 0.9041(5) 0.179(3) Uani 1 1 d . . .
F4 F 0.8411(4) 0.0000 0.8887(8) 0.252(8) Uani 1 2 d S . .
N1 N 0.4835(6) 0.0000 0.2641(16) 0.176(6) Uani 1 2 d S . .
N2 N 0.9199(4) 0.0000 0.6920(12) 0.132(4) Uani 1 2 d S . .
N1B N 0.5914(3) 0.5000 0.7693(7) 0.0722(18) Uani 1 2 d S . .
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'
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'
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
S4 Ni01 S2 179.72(11) . . ?
S4 Ni01 S3 91.41(10) . . ?
S2 Ni01 S3 88.87(10) . . ?
S4 Ni01 S1 87.58(11) . . ?
S2 Ni01 S1 92.14(12) . . ?
S3 Ni01 S1 178.99(12) . . ?
C1 S1 Ni01 104.8(4) . . ?
C2 S2 Ni01 103.1(4) . . ?
C5 S3 Ni01 104.4(3) . . ?
C6 S4 Ni01 105.8(3) . . ?
C2 C1 C3 121.3(12) . . ?
C2 C1 S1 119.7(9) . . ?
C3 C1 S1 119.1(11) . . ?
C1 C2 C4 119.7(11) . . ?
C1 C2 S2 120.3(8) . . ?
C4 C2 S2 120.0(10) . . ?
N1 C3 C1 173(2) . . ?
F1 C4 F2 107.4(9) . . ?
F1 C4 F2 107.4(9) . 6 ?
F2 C4 F2 105.3(12) . 6 ?
F1 C4 C2 111.8(12) . . ?
F2 C4 C2 112.3(8) . . ?
F2 C4 C2 112.3(8) 6 . ?
C6 C5 C7 126.1(8) . . ?
C6 C5 S3 119.7(7) . . ?
C7 C5 S3 114.2(6) . . ?
C5 C6 C8 123.7(10) . . ?
C5 C6 S4 118.7(7) . . ?
C8 C6 S4 117.6(8) . . ?
N2 C7 C5 178.4(12) . . ?
F4 C8 F3 103.0(9) . . ?
F4 C8 F3 103.0(9) . 6 ?
F3 C8 F3 102.3(12) . 6 ?
F4 C8 C6 117.0(12) . . ?
F3 C8 C6 114.9(8) . . ?
F3 C8 C6 114.9(8) 6 . ?
C1B N1B C3B 111.5(7) . 6_565 ?
C1B N1B C3B 111.5(7) . . ?
C3B N1B C3B 109.2(11) 6_565 . ?
C1B N1B C'3B 57(2) . . ?
C3B N1B C'3B 153(3) 6_565 . ?
C3B N1B C'3B 61.6(18) . . ?
C1B N1B C'3B 57(2) . 6_565 ?
C3B N1B C'3B 61.6(18) 6_565 6_565 ?
C3B N1B C'3B 153(3) . 6_565 ?
C'3B N1B C'3B 114(4) . 6_565 ?
C1B N1B C2B 109.4(10) . . ?
C3B N1B C2B 107.5(6) 6_565 . ?
C3B N1B C2B 107.5(6) . . ?
C'3B N1B C2B 99(3) . . ?
C'3B N1B C2B 99(3) 6_565 . ?
C1B N1B C'1B 129(2) . . ?
C3B N1B C'1B 54.6(5) 6_565 . ?
C3B N1B C'1B 54.6(5) . . ?
C'3B N1B C'1B 111(2) . . ?
C'3B N1B C'1B 111(2) 6_565 . ?
C2B N1B C'1B 122(2) . . ?
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
Ni01 S4 2.130(3) . ?
Ni01 S2 2.131(3) . ?
Ni01 S3 2.136(2) . ?
Ni01 S1 2.158(3) . ?
S1 C1 1.666(13) . ?
S2 C2 1.733(10) . ?
S3 C5 1.730(9) . ?
S4 C6 1.706(9) . ?
C1 C2 1.389(16) . ?
C1 C3 1.429(17) . ?
C2 C4 1.500(15) . ?
C3 N1 1.047(17) . ?
C4 F1 1.321(17) . ?
C4 F2 1.326(10) . ?
C4 F2 1.326(10) 6 ?
C5 C6 1.377(12) . ?
C5 C7 1.454(13) . ?
C6 C8 1.418(15) . ?
C7 N2 1.102(13) . ?
C8 F4 1.272(15) . ?
C8 F3 1.296(10) . ?
C8 F3 1.296(10) 6 ?
C1B N1B 1.459(16) . ?
C'1B N1B 1.55(6) . ?
C2B N1B 1.504(12) . ?
C3B N1B 1.470(10) . ?
C'3B N1B 1.50(4) . ?
N1B C3B 1.470(10) 6_565 ?
N1B C'3B 1.50(4) 6_565 ?
