#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:00:39 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178881 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/10/4111059.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_4111059
loop_
_publ_author_name
'Olivier Jeannin'
'Rodolphe Clérac'
'Marc Fourmigué'
_publ_contact_author_address
;
Sciences Chimiques de Rennes
UMR 6226 CNRS-Université Rennes1
Campus de Beaulieu Bat 10C
35042 Rennes cedex
France
;
_publ_contact_author_email       marc.fourmigue@univ-rennes1.fr
_publ_contact_author_fax         '33(0)2 23 23 52 43'
_publ_contact_author_name        'FOURMIGUE Marc'
_publ_contact_author_phone       '33(0)2 23 23 67 32'
_publ_section_title
;
 Order-Disorder Transition Coupled with Magnetic Bistability in the
 Ferricinium Salt of a Radical Nickel Dithiolene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14649
_journal_page_last               14656
_journal_paper_doi               10.1021/ja064842v
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C10 H10 Fe, C8 F6 N2 Ni S4'
_chemical_formula_sum            'C18 H10 F6 Fe N2 Ni S4'
_chemical_formula_weight         611.08
_chemical_name_common            Cp2Fe,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                 99.459(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.039(3)
_cell_length_b                   7.7428(7)
_cell_length_c                   12.9602(14)
_cell_measurement_reflns_used    5208
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.15
_cell_volume                     2280.5(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11252
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  0.5772
_exptl_absorpt_correction_T_min  0.5398
_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    1.780
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0647P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                1287
_reflns_number_total             2375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064842vsi20060707_123756.cif
_cod_data_source_block           oj123b
_cod_database_code               4111059
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
Ni Ni 0.80141(4) 0.0000 0.01622(6) 0.0822(3) Uani 1 2 d S
Fe Fe 0.93471(4) 0.5000 0.74140(6) 0.0918(3) Uani 1 2 d S
S1 S 0.77918(10) 0.0000 0.16995(13) 0.1106(6) Uani 1 2 d S
S2 S 0.89392(8) 0.0000 0.07369(13) 0.1024(6) Uani 1 2 d S
S3 S 0.82333(7) 0.0000 -0.13741(12) 0.0922(5) Uani 1 2 d S
S4 S 0.70909(8) 0.0000 -0.04532(14) 0.0965(5) Uani 1 2 d S
C1 C 0.8451(5) 0.0000 0.2479(5) 0.108(2) Uani 1 2 d S
C2 C 0.8963(4) 0.0000 0.2088(5) 0.104(2) Uani 1 2 d S
C4 C 0.9552(5) 0.0000 0.2646(6) 0.130(3) Uani 1 2 d S
C5 C 0.7569(2) 0.0000 -0.2201(4) 0.0812(15) Uani 1 2 d S
C6 C 0.7063(2) 0.0000 -0.1781(5) 0.0807(15) Uani 1 2 d S
C7 C 0.6490(3) 0.0000 -0.2400(6) 0.112(2) Uani 1 2 d S
C8 C 0.7583(4) 0.0000 -0.3348(6) 0.112(3) Uani 1 2 d S
C1A C 1.0020(12) 0.592(3) 0.8659(17) 0.084(5) Uani 0.50 1 d P
H1A H 1.0341 0.6638 0.8631 0.101 Uiso 0.50 1 calc PR
C'1A C 0.996(3) 0.5000 0.862(3) 0.23(5) Uani 0.50 2 d SP
H'1A H 1.0333 0.5000 0.8448 0.278 Uiso 0.50 2 calc SPR
C2A C 0.9403(10) 0.648(4) 0.871(2) 0.125(12) Uani 0.50 1 d P
H2A H 0.9256 0.7600 0.8679 0.150 Uiso 0.50 1 calc PR
C'2A C 0.9660(10) 0.638(4) 0.8757(14) 0.137(15) Uani 0.50 1 d P
H'2A H 0.9805 0.7504 0.8802 0.164 Uiso 0.50 1 calc PR
C'3A C 0.9063(17) 0.587(4) 0.883(3) 0.111(8) Uani 0.50 1 d P
H'3A H 0.8745 0.6589 0.8867 0.133 Uiso 0.50 1 calc PR
C3A C 0.911(2) 0.5000 0.881(4) 0.19(4) Uani 0.50 2 d SP
H3A H 0.8722 0.5000 0.8949 0.226 Uiso 0.50 2 calc SPR
C4A C 0.9598(3) 0.5866(7) 0.6050(3) 0.1166(18) Uani 1 1 d .
H4A H 0.9922 0.6565 0.6012 0.140 Uiso 1 1 calc R
C5A C 0.9038(3) 0.6443(10) 0.6116(4) 0.140(2) Uani 1 1 d .
H5A H 0.8923 0.7592 0.6131 0.168 Uiso 1 1 calc R
C6A C 0.8672(4) 0.5000 0.6157(7) 0.170(5) Uani 1 2 d S
H6A H 0.8273 0.5000 0.6201 0.204 Uiso 1 2 calc SR
N1 N 1.0024(4) 0.0000 0.3066(6) 0.166(3) Uani 1 2 d S
N2 N 0.6021(3) 0.0000 -0.2838(7) 0.163(3) Uani 1 2 d S
C3 C 0.8495(7) 0.0000 0.3668(8) 0.154(4) Uani 1 2 d S
F1 F 0.7973(5) 0.0000 0.3918(5) 0.272(6) Uani 1 2 d S
F2 F 0.8743(4) -0.1284(8) 0.4106(3) 0.278(4) Uani 1 1 d .
F3 F 0.7097(5) 0.0000 -0.3939(11) 0.132(7) Uani 0.50 2 d SP
F4 F 0.7879(6) -0.138(2) -0.3578(8) 0.170(6) Uani 0.50 1 d P
F'3 F 0.8110(9) 0.0000 -0.3567(12) 0.158(7) Uani 0.50 2 d SP
F'4 F 0.7357(9) -0.133(3) -0.3818(9) 0.281(13) 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'
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'
Fe Fe 0.3463 0.8444 '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
S3 Ni S1 179.83(8) . .
S3 Ni S2 87.12(7) . .
S1 Ni S2 93.04(8) . .
S3 Ni S4 91.45(7) . .
S1 Ni S4 88.38(8) . .
S2 Ni S4 178.58(7) . .
C'1A Fe C3A 62(2) . .
C'1A Fe C2A 52.1(11) . .
C3A Fe C2A 39.5(12) . .
C'1A Fe C2A 52.1(11) . 6_565
C3A Fe C2A 39.5(12) . 6_565
C2A Fe C2A 69.1(19) . 6_565
C'1A Fe C5A 141.0(7) . 6_565
C3A Fe C5A 129.8(11) . 6_565
C2A Fe C5A 163.5(7) . 6_565
C2A Fe C5A 109.9(9) 6_565 6_565
C'1A Fe C5A 141.0(7) . .
C3A Fe C5A 129.8(11) . .
C2A Fe C5A 109.9(9) . .
C2A Fe C5A 163.5(7) 6_565 .
C5A Fe C5A 66.1(4) 6_565 .
C'1A Fe C6A 177.9(14) . .
C3A Fe C6A 115.8(16) . .
C2A Fe C6A 126.5(7) . .
C2A Fe C6A 126.5(7) 6_565 .
C5A Fe C6A 40.1(2) 6_565 .
C5A Fe C6A 40.1(2) . .
C'1A Fe C4A 115.3(13) . .
C3A Fe C4A 160.97(17) . .
C2A Fe C4A 122.7(9) . .
C2A Fe C4A 155.5(8) 6_565 .
C5A Fe C4A 65.2(2) 6_565 .
C5A Fe C4A 39.2(2) . .
C6A Fe C4A 66.6(3) . .
C'1A Fe C4A 115.3(13) . 6_565
C3A Fe C4A 160.97(17) . 6_565
C2A Fe C4A 155.5(8) . 6_565
C2A Fe C4A 122.7(9) 6_565 6_565
C5A Fe C4A 39.2(2) 6_565 6_565
C5A Fe C4A 65.2(2) . 6_565
C6A Fe C4A 66.6(3) . 6_565
C4A Fe C4A 38.0(3) . 6_565
C'1A Fe C'2A 37.7(10) . .
C3A Fe C'2A 48.8(12) . .
C2A Fe C'2A 16.6(10) . .
C2A Fe C'2A 68.1(8) 6_565 .
C5A Fe C'2A 178.0(8) 6_565 .
C5A Fe C'2A 115.8(8) . .
C6A Fe C'2A 141.2(8) . .
C4A Fe C'2A 116.5(7) . .
C4A Fe C'2A 141.5(6) 6_565 .
C'1A Fe C'2A 37.7(10) . 6_565
C3A Fe C'2A 48.8(12) . 6_565
C2A Fe C'2A 68.1(8) . 6_565
C2A Fe C'2A 16.6(10) 6_565 6_565
C5A Fe C'2A 115.8(8) 6_565 6_565
C5A Fe C'2A 178.0(8) . 6_565
C6A Fe C'2A 141.2(8) . 6_565
C4A Fe C'2A 141.5(6) . 6_565
C4A Fe C'2A 116.5(7) 6_565 6_565
C'2A Fe C'2A 62.2(15) . 6_565
C'1A Fe C'3A 65.9(17) . .
C3A Fe C'3A 18.3(10) . .
C2A Fe C'3A 26.1(10) . .
C2A Fe C'3A 56.9(12) 6_565 .
C5A Fe C'3A 139.2(10) 6_565 .
C5A Fe C'3A 114.6(10) . .
C6A Fe C'3A 112.2(11) . .
C4A Fe C'3A 142.8(9) . .
C4A Fe C'3A 178.4(10) 6_565 .
C'2A Fe C'3A 40.1(13) . .
C'2A Fe C'3A 63.7(13) 6_565 .
C1 S1 Ni 103.3(3) . .
C2 S2 Ni 102.4(3) . .
C5 S3 Ni 105.0(2) . .
C6 S4 Ni 104.2(2) . .
C2 C1 C3 117.3(9) . .
C2 C1 S1 122.0(5) . .
C3 C1 S1 120.7(9) . .
C1 C2 C4 128.4(7) . .
C1 C2 S2 119.3(6) . .
C4 C2 S2 112.3(7) . .
N1 C4 C2 178.4(11) . .
C6 C5 C8 123.9(6) . .
C6 C5 S3 118.9(5) . .
C8 C5 S3 117.2(5) . .
C5 C6 C7 123.2(6) . .
C5 C6 S4 120.5(5) . .
C7 C6 S4 116.3(5) . .
N2 C7 C6 176.0(8) . .
F3 C8 F'4 56.4(12) . .
F3 C8 F'4 56.4(12) . 6
F'4 C8 F'4 109(2) . 6
F3 C8 F'3 130.2(11) . .
F'4 C8 F'3 102.8(11) . .
F'4 C8 F'3 102.8(11) 6 .
F3 C8 F4 107.7(8) . .
F'4 C8 F4 54.7(10) . .
F'4 C8 F4 137.2(9) 6 .
F'3 C8 F4 54.2(8) . .
F3 C8 F4 107.7(8) . 6
F'4 C8 F4 137.2(9) . 6
F'4 C8 F4 54.7(10) 6 6
F'3 C8 F4 54.2(8) . 6
F4 C8 F4 107.3(16) . 6
F3 C8 C5 116.5(9) . .
F'4 C8 C5 113.9(8) . .
F'4 C8 C5 113.9(7) 6 .
F'3 C8 C5 113.3(11) . .
F4 C8 C5 108.7(6) . .
F4 C8 C5 108.7(6) 6 .
C1A C1A C2A 106.8(15) 6_565 .
C1A C1A Fe 70.8(7) 6_565 .
C2A C1A Fe 63.9(13) . .
C'2A C'1A C'2A 111(5) 6_565 .
C'2A C'1A Fe 77(3) 6_565 .
C'2A C'1A Fe 77(3) . .
C'2A C'1A C3A 56(3) 6_565 .
C'2A C'1A C3A 56(3) . .
Fe C'1A C3A 60(2) . .
C3A C2A C1A 105(2) . .
C3A C2A Fe 68.8(18) . .
C1A C2A Fe 74.3(12) . .
C'1A C'2A C'3A 108(3) . .
C'1A C'2A Fe 65(3) . .
C'3A C'2A Fe 73.1(17) . .
C'3A C'3A C'2A 106.0(17) 6_565 .
C'3A C'3A Fe 71.9(9) 6_565 .
C'2A C'3A Fe 66.8(14) . .
C2A C3A C2A 116(3) . 6_565
C2A C3A Fe 71.7(16) . .
C2A C3A Fe 71.7(16) 6_565 .
C2A C3A C'1A 58.0(15) . .
C2A C3A C'1A 58.0(15) 6_565 .
Fe C3A C'1A 57.4(16) . .
C4A C4A C5A 108.9(4) 6_565 .
C4A C4A Fe 70.99(15) 6_565 .
C5A C4A Fe 69.9(3) . .
C4A C5A C6A 108.5(7) . .
C4A C5A Fe 70.9(3) . .
C6A C5A Fe 70.4(4) . .
C5A C6A C5A 105.2(9) . 6_565
C5A C6A Fe 69.5(4) . .
C5A C6A Fe 69.5(4) 6_565 .
F2 C3 F2 106.9(13) 6 .
F2 C3 F1 105.3(8) 6 .
F2 C3 F1 105.3(8) . .
F2 C3 C1 114.3(7) 6 .
F2 C3 C1 114.3(7) . .
F1 C3 C1 110.0(12) . .
F'4 F3 F'4 120(2) 6 .
F'4 F3 C8 62.4(11) 6 .
F'4 F3 C8 62.4(11) . .
F'4 F4 F'3 113(2) . .
F'4 F4 C8 59.8(10) . .
F'3 F4 C8 61.2(13) . .
F4 F'3 F4 127(3) . 6
F4 F'3 C8 64.6(12) . .
F4 F'3 C8 64.6(12) 6 .
F3 F'4 F4 122(2) . .
F3 F'4 C8 61.2(13) . .
F4 F'4 C8 65.5(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni S3 2.1331(16) .
Ni S1 2.1371(17) .
Ni S2 2.139(2) .
Ni S4 2.145(2) .
Fe C'1A 1.92(6) .
Fe C3A 1.98(4) .
Fe C2A 2.02(2) .
Fe C2A 2.02(2) 6_565
Fe C5A 2.047(5) 6_565
Fe C5A 2.047(5) .
Fe C6A 2.059(8) .
Fe C4A 2.060(4) .
Fe C4A 2.060(4) 6_565
Fe C'2A 2.07(3) .
Fe C'2A 2.07(3) 6_565
Fe C'3A 2.15(3) .
S1 C1 1.680(9) .
S2 C2 1.743(7) .
S3 C5 1.718(6) .
S4 C6 1.711(6) .
C1 C2 1.359(11) .
C1 C3 1.527(11) .
C2 C4 1.429(12) .
C4 N1 1.133(11) .
C5 C6 1.364(8) .
C5 C8 1.493(9) .
C6 C7 1.429(9) .
C7 N2 1.135(8) .
C8 F3 1.249(16) .
C8 F'4 1.264(14) .
C8 F'4 1.264(14) 6
C8 F'3 1.291(19) .
C8 F4 1.331(12) .
C8 F4 1.331(12) 6
C1A C1A 1.43(5) 6_565
C1A C2A 1.50(4) .
C'1A C'2A 1.30(4) 6_565
C'1A C'2A 1.30(4) .
C'1A C3A 2.02(7) .
C2A C3A 1.35(4) .
C'2A C'3A 1.45(5) .
C'3A C'3A 1.34(7) 6_565
C3A C2A 1.35(4) 6_565
C4A C4A 1.342(10) 6_565
C4A C5A 1.379(8) .
C5A C6A 1.406(8) .
C6A C5A 1.406(8) 6_565
C3 F2 1.238(9) 6
C3 F2 1.238(9) .
C3 F1 1.295(15) .
F3 F'4 1.19(2) 6
F3 F'4 1.19(2) .
F4 F'4 1.19(2) .
F4 F'3 1.195(17) .
F'3 F4 1.195(17) 6
