#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:50:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180358 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/27/7202744.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_7202744
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            'C16 H20 F6 N3 Ni S4'
_chemical_formula_weight         555.30
_chemical_name_common            'Et4N+, [Ni(tfadt)2]-'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6741(6)
_cell_length_b                   18.8293(19)
_cell_length_c                   16.2154(19)
_cell_measurement_reflns_used    5972
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.25
_cell_volume                     2321.1(4)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 1.2 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  0.1074
_diffrn_reflns_av_sigmaI/netI    0.1079
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22061
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.8704
_exptl_absorpt_correction_T_min  0.7377
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of 8 x 8 x 8 = 512 sampling points was used
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0472
_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)+(0.0529P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                1794
_reflns_number_total             4478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701480e.txt
_cod_data_source_block           oj2b60
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7202744
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.8538
#END Tags that were not found in dictionaries
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
Ni Ni 0.27229(10) 0.54613(4) 0.97536(4) 0.0701(2) Uani 1 1 d . . .
S1 S 0.3222(3) 0.64302(8) 0.91303(10) 0.0876(5) Uani 1 1 d . . .
S2 S 0.2439(2) 0.48762(8) 0.86104(9) 0.0788(4) Uani 1 1 d . . .
S3 S 0.2257(2) 0.45001(8) 1.03978(9) 0.0777(4) Uani 1 1 d . . .
S4 S 0.2931(3) 0.60678(8) 1.08802(10) 0.0913(5) Uani 1 1 d . . .
C1 C 0.3053(8) 0.6188(3) 0.8104(3) 0.0738(16) Uani 1 1 d . . .
C2 C 0.2690(8) 0.5518(3) 0.7872(3) 0.0743(15) Uani 1 1 d . . .
C3 C 0.3272(13) 0.6772(4) 0.7503(5) 0.101(2) Uani 1 1 d . . .
C4 C 0.2429(11) 0.5290(4) 0.7024(4) 0.099(2) Uani 1 1 d . . .
C5 C 0.2294(8) 0.4768(3) 1.1415(3) 0.0712(15) Uani 1 1 d . . .
C6 C 0.2583(8) 0.5453(3) 1.1620(3) 0.0755(15) Uani 1 1 d . . .
C7 C 0.1967(10) 0.4222(4) 1.1986(4) 0.0875(19) Uani 1 1 d . . .
C8 C 0.2691(15) 0.5722(5) 1.2498(5) 0.100(2) Uani 1 1 d . . .
C1A C 0.175(4) 0.1233(12) 0.9549(11) 0.116(11) Uani 0.30 1 d P . .
H1A1 H 0.0920 0.0875 0.9678 0.139 Uiso 0.30 1 calc PR . .
H1A2 H 0.1366 0.1391 0.8984 0.139 Uiso 0.30 1 calc PR . .
C'1A C 0.3292(12) 0.1450(5) 1.0221(5) 0.089(3) Uani 0.70 1 d P . .
H'1A H 0.4264 0.1779 1.0220 0.106 Uiso 0.70 1 calc PR . .
H'1B H 0.3438 0.1216 1.0759 0.106 Uiso 0.70 1 calc PR . .
C2A C 0.3431(12) 0.0891(4) 0.9556(4) 0.116(3) Uani 1 1 d . . .
C3A C 0.292(3) 0.2529(16) 0.979(3) 0.168(19) Uani 0.30 1 d P . .
H3A1 H 0.2838 0.2934 1.0150 0.202 Uiso 0.30 1 calc PR . .
H3A2 H 0.4116 0.2353 0.9916 0.202 Uiso 0.30 1 calc PR . .
C'3A C 0.1357(15) 0.2295(5) 0.9342(5) 0.096(3) Uani 0.70 1 d P . .
H'3A H 0.1074 0.1961 0.8889 0.115 Uiso 0.70 1 calc PR . .
H'3B H 0.0333 0.2596 0.9349 0.115 Uiso 0.70 1 calc PR . .
C4A C 0.2821(17) 0.2758(5) 0.9126(5) 0.146(5) Uani 1 1 d . . .
C5A C 0.203(4) 0.1650(19) 1.1056(16) 0.139(11) Uani 0.30 1 d P . .
H5A1 H 0.1392 0.1211 1.1108 0.167 Uiso 0.30 1 calc PR . .
H5A2 H 0.3269 0.1525 1.1135 0.167 Uiso 0.30 1 calc PR . .
C'5A C 0.1657(14) 0.2391(5) 1.0878(5) 0.088(3) Uani 0.70 1 d P . .
H'5A H 0.2663 0.2702 1.0872 0.106 Uiso 0.70 1 calc PR . .
H'5B H 0.0611 0.2686 1.0792 0.106 Uiso 0.70 1 calc PR . .
C6A C 0.1773(13) 0.2059(5) 1.1737(4) 0.131(3) Uani 1 1 d . . .
C7A C -0.032(4) 0.2178(16) 1.0008(16) 0.125(10) Uani 0.30 1 d P . .
H7A1 H -0.0335 0.2604 1.0343 0.150 Uiso 0.30 1 calc PR . .
H7A2 H -0.0601 0.2318 0.9430 0.150 Uiso 0.30 1 calc PR . .
C'7A C 0.0066(13) 0.1357(5) 1.0161(6) 0.095(3) Uani 0.70 1 d P . .
H'7A H 0.0355 0.1045 1.0636 0.114 Uiso 0.70 1 calc PR . .
H'7B H -0.0034 0.1064 0.9665 0.114 Uiso 0.70 1 calc PR . .
C8A C -0.1740(10) 0.1695(5) 1.0217(5) 0.125(3) Uani 1 1 d . . .
N1 N 0.2119(12) 0.5128(4) 0.6380(4) 0.154(3) Uani 1 1 d . . .
N2 N 0.1684(10) 0.3781(4) 1.2427(4) 0.123(2) Uani 1 1 d . . .
N1A N 0.1593(6) 0.1877(2) 1.0137(2) 0.0648(12) Uani 1 1 d . . .
F1 F 0.4307(9) 0.7293(3) 0.7801(4) 0.190(3) Uani 1 1 d . . .
F2 F 0.1824(9) 0.7108(4) 0.7237(4) 0.209(3) Uani 1 1 d . . .
F3 F 0.3885(11) 0.6607(3) 0.6844(4) 0.214(3) Uani 1 1 d . . .
F4 F 0.151(3) 0.5396(12) 1.2904(9) 0.133(6) Uani 0.50 1 d P . .
F5 F 0.420(3) 0.571(4) 1.288(2) 0.30(2) Uani 0.50 1 d P . .
F6 F 0.207(7) 0.6355(9) 1.2554(11) 0.193(16) Uani 0.50 1 d P . .
F'4 F 0.379(3) 0.6194(11) 1.2711(9) 0.123(5) Uani 0.50 1 d P . .
F'5 F 0.126(3) 0.609(3) 1.255(3) 0.28(3) Uani 0.50 1 d P . .
F'6 F 0.316(8) 0.5249(9) 1.3055(10) 0.25(2) Uani 0.50 1 d P . .
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'
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
_geom_angle_publ_flag
S2 Ni S4 178.05(8) . . ?
S2 Ni S3 89.05(6) . . ?
S4 Ni S3 91.86(7) . . ?
S2 Ni S1 91.90(7) . . ?
S4 Ni S1 87.20(7) . . ?
S3 Ni S1 178.88(8) . . ?
C1 S1 Ni 103.7(2) . . ?
C2 S2 Ni 103.4(2) . . ?
C5 S3 Ni 103.7(2) . . ?
C6 S4 Ni 103.7(2) . . ?
C2 C1 C3 123.3(6) . . ?
C2 C1 S1 120.7(5) . . ?
C3 C1 S1 116.0(5) . . ?
C1 C2 C4 123.5(6) . . ?
C1 C2 S2 120.2(4) . . ?
C4 C2 S2 116.3(5) . . ?
F3 C3 F2 103.8(8) . . ?
F3 C3 F1 102.6(8) . . ?
F2 C3 F1 101.8(7) . . ?
F3 C3 C1 117.3(7) . . ?
F2 C3 C1 114.0(7) . . ?
F1 C3 C1 115.3(7) . . ?
N1 C4 C2 175.3(9) . . ?
C6 C5 C7 124.6(5) . . ?
C6 C5 S3 120.0(5) . . ?
C7 C5 S3 115.4(4) . . ?
C5 C6 C8 123.0(6) . . ?
C5 C6 S4 120.7(4) . . ?
C8 C6 S4 116.2(5) . . ?
N2 C7 C5 178.5(8) . . ?
F5 C8 F'4 47(2) . . ?
F5 C8 F'6 59(2) . . ?
F'4 C8 F'6 100.7(19) . . ?
F5 C8 F6 108(2) . . ?
F'4 C8 F6 63.8(17) . . ?
F'6 C8 F6 131.4(17) . . ?
F5 C8 F'5 135.9(17) . . ?
F'4 C8 F'5 98.5(18) . . ?
F'6 C8 F'5 119(2) . . ?
F6 C8 F'5 36(2) . . ?
F5 C8 F4 114(3) . . ?
F'4 C8 F4 132.0(11) . . ?
F'6 C8 F4 59(2) . . ?
F6 C8 F4 96.2(19) . . ?
F'5 C8 F4 65(2) . . ?
F5 C8 C6 113.0(11) . . ?
F'4 C8 C6 117.0(10) . . ?
F'6 C8 C6 113.9(13) . . ?
F6 C8 C6 113.9(11) . . ?
F'5 C8 C6 107.2(17) . . ?
F4 C8 C6 111.0(10) . . ?
C2A C1A N1A 119.2(17) . . ?
C2A C'1A N1A 116.4(7) . . ?
C1A C2A C'1A 63.0(8) . . ?
C4A C3A N1A 127(2) . . ?
C4A C'3A N1A 120.0(9) . . ?
C3A C4A C'3A 61.4(14) . . ?
C6A C5A N1A 126(2) . . ?
C6A C5A C'7A 123(2) . . ?
N1A C5A C'7A 48.7(8) . . ?
C6A C'5A N1A 116.7(7) . . ?
C6A C'5A C7A 121.1(11) . . ?
N1A C'5A C7A 51.1(7) . . ?
C5A C6A C'5A 59.6(13) . . ?
C8A C7A N1A 116.8(19) . . ?
C8A C7A C'5A 118.5(16) . . ?
N1A C7A C'5A 50.2(9) . . ?
N1A C'7A C8A 115.8(7) . . ?
N1A C'7A C5A 49.1(9) . . ?
C8A C'7A C5A 115.7(11) . . ?
C7A C8A C'7A 63.1(10) . . ?
C'3A N1A C'1A 110.8(6) . . ?
C'3A N1A C'7A 110.8(7) . . ?
C'1A N1A C'7A 108.0(6) . . ?
C'3A N1A C'5A 109.1(6) . . ?
C'1A N1A C'5A 109.1(6) . . ?
C'7A N1A C'5A 109.0(6) . . ?
C'3A N1A C5A 163.8(15) . . ?
C'1A N1A C5A 72.3(12) . . ?
C'7A N1A C5A 82.2(13) . . ?
C'5A N1A C5A 56.0(12) . . ?
C'3A N1A C1A 83.9(9) . . ?
C'1A N1A C1A 60.4(12) . . ?
C'7A N1A C1A 69.0(10) . . ?
C'5A N1A C1A 166.2(11) . . ?
C5A N1A C1A 110.5(15) . . ?
C'3A N1A C7A 72.2(11) . . ?
C'1A N1A C7A 169.3(13) . . ?
C'7A N1A C7A 61.8(12) . . ?
C'5A N1A C7A 78.7(11) . . ?
C5A N1A C7A 107.9(15) . . ?
C1A N1A C7A 110.6(16) . . ?
C'3A N1A C3A 50.0(13) . . ?
C'1A N1A C3A 82.4(11) . . ?
C'7A N1A C3A 160.8(14) . . ?
C'5A N1A C3A 81.5(11) . . ?
C5A N1A C3A 116.7(19) . . ?
C1A N1A C3A 104.6(12) . . ?
C7A N1A C3A 106.4(15) . . ?
F'6 F4 C8 58.5(12) . . ?
F'6 F4 F'5 110(2) . . ?
C8 F4 F'5 56.2(12) . . ?
F'4 F5 C8 66.6(16) . . ?
F'4 F5 F'6 121(3) . . ?
C8 F5 F'6 62.5(18) . . ?
F'5 F6 C8 73(3) . . ?
F'5 F6 F'4 127(5) . . ?
C8 F6 F'4 56.2(15) . . ?
F5 F'4 C8 66(2) . . ?
F5 F'4 F6 122(3) . . ?
C8 F'4 F6 59.9(11) . . ?
F6 F'5 C8 71(3) . . ?
F6 F'5 F4 121(6) . . ?
C8 F'5 F4 59(2) . . ?
F5 F'6 C8 58.7(16) . . ?
F5 F'6 F4 117(4) . . ?
C8 F'6 F4 63(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
Ni S2 2.1417(16) . ?
Ni S4 2.1418(17) . ?
Ni S3 2.1441(17) . ?
Ni S1 2.1452(18) . ?
S1 C1 1.713(6) . ?
S2 C2 1.730(6) . ?
S3 C5 1.721(6) . ?
S4 C6 1.714(6) . ?
C1 C2 1.336(8) . ?
C1 C3 1.494(9) . ?
C2 C4 1.429(8) . ?
C3 F3 1.264(8) . ?
C3 F2 1.300(9) . ?
C3 F1 1.312(8) . ?
C4 N1 1.082(7) . ?
C5 C6 1.342(7) . ?
C5 C7 1.429(9) . ?
C6 C8 1.502(9) . ?
C7 N2 1.137(8) . ?
C8 F5 1.238(19) . ?
C8 F'4 1.240(15) . ?
C8 F'6 1.29(3) . ?
C8 F6 1.29(2) . ?
C8 F'5 1.31(3) . ?
C8 F4 1.340(18) . ?
C1A C2A 1.44(3) . ?
C1A N1A 1.56(2) . ?
C'1A C2A 1.522(11) . ?
C'1A N1A 1.522(10) . ?
C3A C4A 1.15(5) . ?
C3A N1A 1.74(4) . ?
C'3A C4A 1.501(15) . ?
C'3A N1A 1.501(9) . ?
C5A C6A 1.38(3) . ?
C5A N1A 1.54(3) . ?
C5A C'7A 2.02(3) . ?
C'5A C6A 1.519(11) . ?
C'5A N1A 1.539(8) . ?
C'5A C7A 1.96(3) . ?
C7A C8A 1.49(3) . ?
C7A N1A 1.56(3) . ?
C'7A N1A 1.532(10) . ?
C'7A C8A 1.539(12) . ?
F4 F'6 1.29(5) . ?
F4 F'5 1.43(6) . ?
F5 F'4 0.99(5) . ?
F5 F'6 1.24(5) . ?
F6 F'5 0.80(4) . ?
F6 F'4 1.34(3) . ?
