#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:50:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180358 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/27/7202745.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_7202745
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_moiety         'C8 H20 N, C8 F6 N2 Ni S4'
_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           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.384(3)
_cell_length_b                   7.7447(15)
_cell_length_c                   19.192(4)
_cell_measurement_reflns_used    3225
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      1.60
_cell_volume                     2435.3(8)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1050
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18225
_diffrn_reflns_theta_full        22.37
_diffrn_reflns_theta_max         22.37
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.515
_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         0.361
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.793
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1696
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1758P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2721
_reflns_number_gt                559
_reflns_number_total             1696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701480e.txt
_cod_data_source_block           tma_pnma
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7202745
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.52530(15) 0.2500 0.54768(10) 0.1407(11) Uani 1 2 d S . .
S1 S 0.4576(3) 0.2500 0.4537(2) 0.1574(19) Uani 1 2 d S . .
S2 S 0.4167(4) 0.2500 0.6078(2) 0.182(2) Uani 1 2 d S . .
S3 S 0.6348(3) 0.2500 0.4883(2) 0.166(2) Uani 1 2 d S . .
S4 S 0.5918(4) 0.2500 0.6428(2) 0.185(2) Uani 1 2 d S . .
C1 C 0.3590(10) 0.2500 0.4804(10) 0.131(5) Uani 1 2 d SD . .
C2 C 0.2987(16) 0.2500 0.4264(12) 0.188(9) Uani 1 2 d SD . .
C3 C 0.3399(11) 0.2500 0.5507(11) 0.165(7) Uani 1 2 d SD . .
C4 C 0.2526(12) 0.2500 0.5760(12) 0.230(11) Uiso 1 2 d SD . .
F1 F 0.2426(10) 0.113(2) 0.6174(8) 0.224(10) Uiso 0.59(3) 1 d PD . .
F2 F 0.2112(13) 0.117(3) 0.5475(12) 0.221(14) Uiso 0.41(3) 1 d PD . .
F3 F 0.1937(17) 0.2500 0.5279(14) 0.284(14) Uiso 0.59(3) 2 d SPD . .
F3' F 0.236(3) 0.2500 0.6435(13) 0.28(2) Uiso 0.41(3) 2 d SPD . .
C5 C 0.7132(14) 0.2500 0.5518(11) 0.169(7) Uani 1 2 d SD . .
C6 C 0.7955(17) 0.2500 0.5256(14) 0.246(13) Uani 1 2 d SD . .
N2 N 0.8544(15) 0.2500 0.5031(17) 0.340(18) Uani 1 2 d SD . .
C7 C 0.6927(13) 0.2500 0.6180(11) 0.165(7) Uani 1 2 d SD . .
C8 C 0.7516(15) 0.2500 0.6788(13) 0.273(14) Uiso 1 2 d SD . .
F4 F 0.7491(11) 0.113(2) 0.7212(9) 0.245(11) Uiso 0.58(3) 1 d PD . .
F5 F 0.8050(17) 0.122(4) 0.6703(18) 0.285(18) Uiso 0.42(3) 1 d PD . .
F6 F 0.8308(17) 0.2500 0.6620(19) 0.303(18) Uiso 0.58(3) 2 d SPD . .
F6' F 0.711(3) 0.2500 0.740(2) 0.36(3) Uiso 0.42(3) 2 d SPD . .
N1 N 0.2568(16) 0.2500 0.3841(14) 0.288(14) Uani 1 2 d SD . .
N3 N 0.4956(10) 0.2500 0.1937(8) 0.191(7) Uani 1 2 d SD . .
C10 C 0.450(3) 0.138(10) 0.247(3) 0.88(16) Uani 0.50 1 d PD . .
C11 C 0.379(4) 0.2500 0.220(4) 0.42(3) Uiso 1 2 d SD . .
C12 C 0.544(3) 0.130(4) 0.242(2) 0.34(3) Uiso 0.50 1 d PD . .
C13 C 0.602(2) 0.2500 0.2808(17) 0.274(13) Uiso 1 2 d SD . .
C14 C 0.518(2) 0.137(5) 0.1296(15) 0.49(3) Uiso 1 1 d D . .
C15 C 0.483(3) -0.033(7) 0.158(2) 0.55(3) Uiso 1 1 d 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'
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
S1 Ni1 S2 91.4(2) . . ?
S1 Ni1 S4 179.3(2) . . ?
S2 Ni1 S4 87.9(2) . . ?
S1 Ni1 S3 89.2(2) . . ?
S2 Ni1 S3 179.4(2) . . ?
S4 Ni1 S3 91.6(2) . . ?
C1 S1 Ni1 104.0(7) . . ?
C3 S2 Ni1 106.0(7) . . ?
C5 S3 Ni1 104.1(8) . . ?
C7 S4 Ni1 104.8(7) . . ?
C3 C1 C2 123.3(17) . . ?
C3 C1 S1 120.7(14) . . ?
C2 C1 S1 116.1(15) . . ?
N1 C2 C1 177(3) . . ?
C1 C3 C4 121.8(18) . . ?
C1 C3 S2 118.0(14) . . ?
C4 C3 S2 120.2(17) . . ?
F3' C4 F1 52.5(12) . 7_565 ?
F3' C4 F1 52.5(12) . . ?
F1 C4 F1 105(2) 7_565 . ?
F3' C4 F3 122(3) . . ?
F1 C4 F3 108.9(16) 7_565 . ?
F1 C4 F3 108.9(16) . . ?
F3' C4 F2 107(2) . . ?
F1 C4 F2 142(2) 7_565 . ?
F1 C4 F2 64.9(11) . . ?
F3 C4 F2 49.9(14) . . ?
F3' C4 F2 107(2) . 7_565 ?
F1 C4 F2 64.9(11) 7_565 7_565 ?
F1 C4 F2 142(2) . 7_565 ?
F3 C4 F2 49.9(14) . 7_565 ?
F2 C4 F2 99(3) . 7_565 ?
F3' C4 C3 121(3) . . ?
F1 C4 C3 107.9(14) 7_565 . ?
F1 C4 C3 107.9(14) . . ?
F3 C4 C3 118(2) . . ?
F2 C4 C3 110.3(15) . . ?
F2 C4 C3 110.3(15) 7_565 . ?
F3' F1 C4 63.4(8) . . ?
F3' F1 F2 110(2) . . ?
C4 F1 F2 58.0(7) . . ?
F3 F2 C4 64.6(10) . . ?
F3 F2 F1 115.0(17) . . ?
C4 F2 F1 57.2(7) . . ?
F2 F3 F2 131(2) 7_565 . ?
F2 F3 C4 65.6(10) 7_565 . ?
F2 F3 C4 65.6(10) . . ?
F1 F3' F1 128.2(18) 7_565 . ?
F1 F3' C4 64.1(9) 7_565 . ?
F1 F3' C4 64.1(9) . . ?
C7 C5 C6 125(2) . . ?
C7 C5 S3 118.7(17) . . ?
C6 C5 S3 116.1(16) . . ?
N2 C6 C5 176(4) . . ?
C5 C7 C8 126(2) . . ?
C5 C7 S4 120.8(16) . . ?
C8 C7 S4 113.6(17) . . ?
F5 C8 F5 96(4) 7_565 . ?
F5 C8 F6 48.3(19) 7_565 . ?
F5 C8 F6 48(2) . . ?
F5 C8 F4 60.2(14) 7_565 7_565 ?
F5 C8 F4 133(2) . 7_565 ?
F6 C8 F4 100.2(18) . 7_565 ?
F5 C8 F4 133(2) 7_565 . ?
F5 C8 F4 60.2(14) . . ?
F6 C8 F4 100.2(18) . . ?
F4 C8 F4 105(3) 7_565 . ?
F5 C8 F6' 115(2) 7_565 . ?
F5 C8 F6' 115(2) . . ?
F6 C8 F6' 134(3) . . ?
F4 C8 F6' 57.1(15) 7_565 . ?
F4 C8 F6' 57.1(15) . . ?
F5 C8 C7 109(2) 7_565 . ?
F5 C8 C7 109(2) . . ?
F6 C8 C7 116(3) . . ?
F4 C8 C7 116.6(14) 7_565 . ?
F4 C8 C7 116.6(14) . . ?
F6' C8 C7 111(3) . . ?
F6' F4 F5 119.5(15) . . ?
F6' F4 C8 61.7(9) . . ?
F5 F4 C8 59.8(9) . . ?
F6 F5 C8 65.9(12) . . ?
F6 F5 F4 115(3) . . ?
C8 F5 F4 60.1(9) . . ?
F5 F6 F5 131(2) 7_565 . ?
F5 F6 C8 65.8(12) 7_565 . ?
F5 F6 C8 65.8(12) . . ?
F4 F6' F4 112(3) 7_565 . ?
F4 F6' C8 61.2(10) 7_565 . ?
F4 F6' C8 61.2(10) . . ?
C10 N3 C10 69(7) 7_565 . ?
C10 N3 C12 61(3) 7_565 7_565 ?
C10 N3 C12 102(4) . 7_565 ?
C10 N3 C12 102(4) 7_565 . ?
C10 N3 C12 61(3) . . ?
C12 N3 C12 75(3) 7_565 . ?
C10 N3 C14 164(3) 7_565 . ?
C10 N3 C14 109(4) . . ?
C12 N3 C14 134(3) 7_565 . ?
C12 N3 C14 91(2) . . ?
C10 N3 C14 109(4) 7_565 7_565 ?
C10 N3 C14 164(3) . 7_565 ?
C12 N3 C14 91(2) 7_565 7_565 ?
C12 N3 C14 134(3) . 7_565 ?
C14 N3 C14 68(3) . 7_565 ?
C11 C10 N3 80(3) . . ?
C13 C12 N3 104(2) . . ?
C15 C14 N3 96(3) . . ?
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 2.118(5) . ?
Ni1 S2 2.120(6) . ?
Ni1 S4 2.125(5) . ?
Ni1 S3 2.125(5) . ?
S1 C1 1.695(16) . ?
S2 C3 1.669(19) . ?
S3 C5 1.77(2) . ?
S4 C7 1.72(2) . ?
C1 C3 1.38(2) . ?
C1 C2 1.43(2) . ?
C2 N1 1.06(2) . ?
C3 C4 1.511(10) . ?
C4 F3' 1.326(10) . ?
C4 F1 1.335(9) 7_565 ?
C4 F1 1.335(9) . ?
C4 F3 1.335(10) . ?
C4 F2 1.347(10) . ?
C4 F2 1.347(10) 7_565 ?
F1 F3' 1.18(2) . ?
F1 F2 1.44(2) . ?
F2 F3 1.13(3) . ?
F3 F2 1.13(3) 7_565 ?
F3' F1 1.18(2) 7_565 ?
C5 C7 1.31(2) . ?
C5 C6 1.44(2) . ?
C6 N2 1.06(2) . ?
C7 C8 1.514(10) . ?
C8 F5 1.335(10) 7_565 ?
C8 F5 1.335(10) . ?
C8 F6 1.336(10) . ?
C8 F4 1.340(10) 7_565 ?
C8 F4 1.340(10) . ?
C8 F6' 1.346(10) . ?
F4 F6' 1.28(3) . ?
F4 F5 1.34(3) . ?
F5 F6 1.09(4) . ?
F6 F5 1.09(4) 7_565 ?
F6' F4 1.28(3) 7_565 ?
N3 C10 1.531(10) 7_565 ?
N3 C10 1.531(10) . ?
N3 C12 1.535(10) 7_565 ?
N3 C12 1.535(10) . ?
N3 C14 1.552(10) . ?
N3 C14 1.552(10) 7_565 ?
C10 C11 1.529(10) . ?
C12 C13 1.521(10) . ?
C14 C15 1.535(10) . ?
