#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001433.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_4001433
loop_
_publ_author_name
'Jeannin, Olivier'
'Clérac, Rodolphe'
'Fourmigué, Marc'
_publ_section_title
;
 Phase Competition and Weak Hydrogen Bonding in the Giant Hysteresis of an
 S = 1/2 Nickel Dithiolene Complex: Combined Structural and Magnetic
 Studies
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5946
_journal_paper_doi               10.1021/cm071652q
_journal_volume                  19
_journal_year                    2007
_chemical_formula_moiety         'C8 F6 N2 Ni S4, C10 H10 Co'
_chemical_formula_sum            'C18 H10 Co F6 N2 Ni S4'
_chemical_formula_weight         614.16
_chemical_name_common            'Cp2Co, 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                 99.309(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.180(3)
_cell_length_b                   7.7477(5)
_cell_length_c                   12.7587(11)
_cell_measurement_reflns_used    5904
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.25
_cell_volume                     2261.2(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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0431
_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       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8785
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  0.7998
_exptl_absorpt_correction_T_min  0.4633
_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    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    Constr.
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0618P)²+2.6675P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                1511
_reflns_number_total             2344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071652q-file002.cif
_cod_data_source_block           CoRTinit
_cod_original_cell_volume        2261.2(3)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4001433
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 0.30136(4) 0.5000 0.01389(6) 0.0814(3) Uani 1 2 d S
Co Co 0.43463(4) 1.0000 0.74362(7) 0.0893(4) Uani 1 2 d S
S1 S 0.27999(12) 0.5000 0.17053(16) 0.1113(7) Uani 1 2 d S
S2 S 0.39354(10) 0.5000 0.07031(15) 0.1004(6) Uani 1 2 d S
S3 S 0.32221(7) 0.5000 -0.14271(13) 0.0904(6) Uani 1 2 d S
S4 S 0.20939(9) 0.5000 -0.04623(16) 0.0978(6) Uani 1 2 d S
C1 C 0.3447(5) 0.5000 0.2479(6) 0.110(3) Uani 1 2 d S
C2 C 0.3961(5) 0.5000 0.2073(6) 0.102(2) Uani 1 2 d S
C3 C 0.4539(6) 0.5000 0.2635(7) 0.125(3) Uani 1 2 d S
C4 C 0.3503(8) 0.5000 0.3684(9) 0.154(5) Uani 1 2 d S
C5 C 0.2056(3) 0.5000 -0.1819(6) 0.0838(18) Uani 1 2 d S
C6 C 0.2559(3) 0.5000 -0.2241(5) 0.0800(17) Uani 1 2 d S
C7 C 0.1486(3) 0.5000 -0.2424(7) 0.109(3) Uani 1 2 d S
C8 C 0.2572(4) 0.5000 -0.3412(7) 0.112(3) Uani 1 2 d S
N1 N 0.5023(5) 0.5000 0.3047(8) 0.158(4) Uani 1 2 d S
N2 N 0.1020(3) 0.5000 -0.2861(8) 0.165(4) Uani 1 2 d S
F1 F 0.3085(8) 0.5000 -0.3633(12) 0.150(7) Uani 0.50 2 d SP
F2 F 0.2844(6) 0.641(2) -0.3671(8) 0.167(7) Uani 0.50 1 d P
F'1 F 0.2084(5) 0.5000 -0.4011(12) 0.122(6) Uani 0.50 2 d SP
F4 F 0.2978(5) 0.5000 0.3949(6) 0.275(7) Uani 1 2 d S
F5 F 0.3748(4) 0.6278(9) 0.4136(4) 0.278(4) Uani 1 1 d .
F3 F 0.2314(11) 0.628(3) -0.3894(11) 0.286(14) Uani 0.50 1 d P
C1A C 0.4583(3) 0.9124(8) 0.6082(3) 0.1147(19) Uani 1 1 d .
H1A H 0.4904 0.8430 0.6021 0.138 Uiso 1 1 calc R
C2A C 0.4035(4) 0.8532(12) 0.6187(5) 0.138(3) Uani 1 1 d .
H2A H 0.3922 0.7382 0.6216 0.166 Uiso 1 1 calc R
C3A C 0.3670(5) 1.0000 0.6243(9) 0.167(6) Uani 1 2 d S
H3A H 0.3276 1.0000 0.6304 0.200 Uiso 1 2 calc SR
C4A C 0.5012(10) 1.093(2) 0.8630(15) 0.078(4) Uani 0.50 1 d P
H4A H 0.5331 1.1645 0.8588 0.093 Uiso 0.50 1 calc PR
C5A C 0.4641(11) 1.136(4) 0.8725(15) 0.147(17) Uani 0.50 1 d P
H5A H 0.4778 1.2491 0.8745 0.177 Uiso 0.50 1 calc PR
C6A C 0.409(2) 1.0000 0.880(5) 0.19(5) Uani 0.50 2 d SP
H6A H 0.3701 1.0000 0.8911 0.232 Uiso 0.50 2 calc SPR
C7A C 0.4400(10) 0.849(4) 0.871(2) 0.128(14) Uani 0.50 1 d P
H7A H 0.4260 0.7363 0.8699 0.154 Uiso 0.50 1 calc PR
C8A C 0.4077(16) 0.916(5) 0.884(2) 0.115(9) Uani 0.50 1 d P
H8A H 0.3762 0.8444 0.8897 0.138 Uiso 0.50 1 calc PR
C9A C 0.493(2) 1.0000 0.859(3) 0.23(4) Uani 0.50 2 d SP
H9A H 0.5310 1.0000 0.8422 0.281 Uiso 0.50 2 calc SPR
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'
Co Co 0.3494 0.9721 '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 179.71(10) . .
S3 Ni S2 87.13(7) . .
S1 Ni S2 93.16(10) . .
S3 Ni S4 91.59(8) . .
S1 Ni S4 88.12(9) . .
S2 Ni S4 178.72(8) . .
C9A Co C6A 64.9(19) . .
C9A Co C5A 39.0(11) . .
C6A Co C5A 50.7(13) . .
C9A Co C5A 39.0(11) . 6_575
C6A Co C5A 50.7(13) . 6_575
C5A Co C5A 64.4(17) . 6_575
C9A Co C7A 53.5(10) . 6_575
C6A Co C7A 41.5(12) . 6_575
C5A Co C7A 16.4(11) . 6_575
C5A Co C7A 70.6(8) 6_575 6_575
C9A Co C7A 53.5(10) . .
C6A Co C7A 41.5(12) . .
C5A Co C7A 70.6(8) . .
C5A Co C7A 16.4(11) 6_575 .
C7A Co C7A 72(2) 6_575 .
C9A Co C2A 140.0(6) . .
C6A Co C2A 126.5(12) . .
C5A Co C2A 176.9(8) . .
C5A Co C2A 113.0(9) 6_575 .
C7A Co C2A 162.5(7) 6_575 .
C7A Co C2A 106.4(10) . .
C9A Co C2A 140.0(6) . 6_575
C6A Co C2A 126.5(12) . 6_575
C5A Co C2A 113.0(9) . 6_575
C5A Co C2A 176.9(8) 6_575 6_575
C7A Co C2A 106.4(10) 6_575 6_575
C7A Co C2A 162.5(7) . 6_575
C2A Co C2A 69.5(5) . 6_575
C9A Co C3A 176.4(13) . .
C6A Co C3A 111.5(17) . .
C5A Co C3A 139.0(9) . .
C5A Co C3A 139.0(9) 6_575 .
C7A Co C3A 124.0(7) 6_575 .
C7A Co C3A 124.0(7) . .
C2A Co C3A 41.8(3) . .
C2A Co C3A 41.8(3) 6_575 .
C9A Co C1A 114.7(12) . .
C6A Co C1A 160.3(2) . .
C5A Co C1A 141.9(7) . .
C5A Co C1A 115.3(7) 6_575 .
C7A Co C1A 155.4(9) 6_575 .
C7A Co C1A 120.8(10) . .
C2A Co C1A 40.2(3) . .
C2A Co C1A 67.7(3) 6_575 .
C3A Co C1A 68.6(4) . .
C9A Co C1A 114.7(12) . 6_575
C6A Co C1A 160.3(2) . 6_575
C5A Co C1A 115.3(7) . 6_575
C5A Co C1A 141.9(7) 6_575 6_575
C7A Co C1A 120.8(10) 6_575 6_575
C7A Co C1A 155.4(9) . 6_575
C2A Co C1A 67.7(3) . 6_575
C2A Co C1A 40.2(3) 6_575 6_575
C3A Co C1A 68.6(4) . 6_575
C1A Co C1A 39.4(4) . 6_575
C9A Co C8A 66.5(16) . 6_575
C6A Co C8A 18.2(10) . 6_575
C5A Co C8A 40.0(14) . 6_575
C5A Co C8A 64.3(13) 6_575 6_575
C7A Co C8A 26.7(10) 6_575 6_575
C7A Co C8A 58.2(15) . 6_575
C2A Co C8A 137.8(10) . 6_575
C2A Co C8A 112.7(11) 6_575 6_575
C3A Co C8A 110.2(11) . 6_575
C1A Co C8A 177.9(10) . 6_575
C1A Co C8A 142.1(11) 6_575 6_575
C1 S1 Ni 103.5(3) . .
C2 S2 Ni 102.0(4) . .
C6 S3 Ni 104.5(2) . .
C5 S4 Ni 104.2(2) . .
C2 C1 C4 116.3(11) . .
C2 C1 S1 122.1(6) . .
C4 C1 S1 121.6(9) . .
C1 C2 C3 128.1(8) . .
C1 C2 S2 119.2(7) . .
C3 C2 S2 112.6(8) . .
N1 C3 C2 176.6(12) . .
F5 C4 F5 106.4(15) . 6_565
F5 C4 F4 104.7(9) . .
F5 C4 F4 104.7(9) 6_565 .
F5 C4 C1 115.4(7) . .
F5 C4 C1 115.4(7) 6_565 .
F4 C4 C1 109.1(13) . .
C6 C5 C7 124.6(7) . .
C6 C5 S4 119.3(6) . .
C7 C5 S4 116.1(5) . .
C5 C6 C8 123.4(7) . .
C5 C6 S3 120.3(5) . .
C8 C6 S3 116.3(5) . .
N2 C7 C5 176.6(10) . .
F'1 C8 F1 130.6(12) . .
F'1 C8 F3 53.0(13) . 6_565
F1 C8 F3 106.3(13) . 6_565
F'1 C8 F3 53.0(13) . .
F1 C8 F3 106.3(12) . .
F3 C8 F3 103(2) 6_565 .
F'1 C8 F2 105.4(8) . .
F1 C8 F2 56.2(8) . .
F3 C8 F2 136.9(11) 6_565 .
F3 C8 F2 56.1(11) . .
F'1 C8 F2 105.4(8) . 6_565
F1 C8 F2 56.2(8) . 6_565
F3 C8 F2 56.1(11) 6_565 6_565
F3 C8 F2 136.9(11) . 6_565
F2 C8 F2 110.4(16) . 6_565
F'1 C8 C6 116.2(10) . .
F1 C8 C6 113.2(10) . .
F3 C8 C6 113.5(9) 6_565 .
F3 C8 C6 113.5(9) . .
F2 C8 C6 109.6(7) . .
F2 C8 C6 109.6(7) 6_565 .
F2 F1 F2 126(2) 6_565 .
F2 F1 C8 64.5(10) 6_565 .
F2 F1 C8 64.5(10) . .
F3 F2 F1 112(2) . .
F3 F2 C8 59.5(11) . .
F1 F2 C8 59.3(12) . .
F3 F'1 F3 124(3) . 6_565
F3 F'1 C8 63.9(12) . .
F3 F'1 C8 63.9(12) 6_565 .
F'1 F3 F2 122(2) . .
F'1 F3 C8 63.2(14) . .
F2 F3 C8 64.4(10) . .
C1A C1A C2A 109.4(5) 6_575 .
C1A C1A Co 70.30(18) 6_575 .
C2A C1A Co 69.2(4) . .
C1A C2A C3A 107.6(8) . .
C1A C2A Co 70.6(3) . .
C3A C2A Co 69.3(5) . .
C2A C3A C2A 105.9(10) . 6_575
C2A C3A Co 69.0(4) . .
C2A C3A Co 69.0(4) 6_575 .
C4A C4A C7A 107.2(15) 6_575 6_575
C4A C4A Co 70.0(6) 6_575 .
C7A C4A Co 64.1(13) 6_575 .
C9A C5A C8A 108(3) . 6_575
C9A C5A Co 65(2) . .
C8A C5A Co 74.2(17) 6_575 .
C7A C6A C7A 115(3) 6_575 .
C7A C6A Co 72(2) 6_575 .
C7A C6A Co 72(2) . .
C7A C6A C9A 57.3(15) 6_575 .
C7A C6A C9A 57.3(15) . .
Co C6A C9A 55.4(18) . .
C6A C7A C4A 105(2) . 6_575
C6A C7A Co 67(2) . .
C4A C7A Co 72.9(12) 6_575 .
C8A C8A C5A 107(2) 6_575 6_575
C8A C8A Co 71.8(10) 6_575 .
C5A C8A Co 65.8(14) 6_575 .
C5A C9A C5A 111(4) 6_575 .
C5A C9A Co 76(3) 6_575 .
C5A C9A Co 76(3) . .
C5A C9A C6A 56(2) 6_575 .
C5A C9A C6A 56(2) . .
Co C9A C6A 60(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni S3 2.1303(17) .
Ni S1 2.1354(19) .
Ni S2 2.142(2) .
Ni S4 2.146(2) .
Co C9A 1.84(5) .
Co C6A 1.93(5) .
Co C5A 1.98(2) .
Co C5A 1.98(2) 6_575
Co C7A 1.99(3) 6_575
Co C7A 1.99(3) .
Co C2A 1.996(7) .
Co C2A 1.996(6) 6_575
Co C3A 2.000(9) .
Co C1A 2.014(5) .
Co C1A 2.014(5) 6_575
Co C8A 2.09(3) 6_575
S1 C1 1.656(11) .
S2 C2 1.739(8) .
S3 C6 1.710(7) .
S4 C5 1.720(7) .
C1 C2 1.375(12) .
C1 C4 1.522(12) .
C2 C3 1.414(14) .
C3 N1 1.160(13) .
C4 F5 1.236(10) .
C4 F5 1.236(10) 6_565
C4 F4 1.316(18) .
C5 C6 1.360(8) .
C5 C7 1.418(11) .
C6 C8 1.501(10) .
C7 N2 1.132(10) .
C8 F'1 1.260(17) .
C8 F1 1.264(18) .
C8 F3 1.268(15) 6_565
C8 F3 1.268(15) .
C8 F2 1.327(12) .
C8 F2 1.327(12) 6_565
F1 F2 1.222(17) 6_565
F1 F2 1.222(17) .
F2 F3 1.22(2) .
F'1 F3 1.13(3) .
F'1 F3 1.13(3) 6_565
C1A C1A 1.358(12) 6_575
C1A C2A 1.379(9) .
C2A C3A 1.425(10) .
C3A C2A 1.425(10) 6_575
C4A C4A 1.45(4) 6_575
C4A C7A 1.51(4) 6_575
C5A C9A 1.28(4) .
C5A C8A 1.40(5) 6_575
C6A C7A 1.39(4) 6_575
C6A C7A 1.39(4) .
C6A C9A 2.02(6) .
C7A C4A 1.51(4) 6_575
C8A C8A 1.30(8) 6_575
C8A C5A 1.40(5) 6_575
C9A C5A 1.28(4) 6_575
