#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/14/4001432.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_4001432
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                 99.276(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.211(3)
_cell_length_b                   7.7363(7)
_cell_length_c                   12.7856(18)
_cell_measurement_reflns_used    7272
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      1.8
_cell_volume                     2265.9(5)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0715
_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            10847
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.9271
_exptl_absorpt_correction_T_min  0.7253
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x 12 x  8 =   768 sampling points was used
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0423
_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)+(0.0579P)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         0.1197
_reflns_number_gt                1063
_reflns_number_total             2339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071652q-file001.cif
_cod_data_source_block           CoRTback
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constr.' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4001432
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.8766
#END Tags that were not found in dictionaries
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 0.30140(4) 0.5000 0.01404(7) 0.0792(3) Uani 1 2 d S
Co Co 0.43472(4) 0.0000 0.74362(8) 0.0877(4) Uani 1 2 d S
S1 S 0.27981(12) 0.5000 0.17043(18) 0.1087(8) Uani 1 2 d S
S2 S 0.39360(9) 0.5000 0.07040(16) 0.0970(7) Uani 1 2 d S
S3 S 0.32214(7) 0.5000 -0.14277(14) 0.0883(6) Uani 1 2 d S
S4 S 0.20954(9) 0.5000 -0.04589(18) 0.0951(7) Uani 1 2 d S
C1 C 0.3430(5) 0.5000 0.2470(6) 0.108(3) Uani 1 2 d S
C2 C 0.3950(5) 0.5000 0.2068(7) 0.099(3) Uani 1 2 d S
C3 C 0.4538(7) 0.5000 0.2621(8) 0.126(4) Uani 1 2 d S
C4 C 0.3521(9) 0.5000 0.3689(9) 0.155(5) Uani 1 2 d S
C5 C 0.2056(3) 0.5000 -0.1809(6) 0.079(2) Uani 1 2 d S
C6 C 0.2557(3) 0.5000 -0.2237(5) 0.077(2) Uani 1 2 d S
C7 C 0.1482(4) 0.5000 -0.2422(8) 0.111(3) Uani 1 2 d S
C8 C 0.2566(5) 0.5000 -0.3409(8) 0.104(3) Uani 1 2 d S
C1A C 0.4583(3) -0.0880(8) 0.6083(4) 0.113(2) Uani 1 1 d .
H1A H 0.4901 -0.1581 0.6020 0.136 Uiso 1 1 calc R
C2A C 0.4034(4) -0.1450(12) 0.6193(5) 0.135(3) Uani 1 1 d .
H2A H 0.3923 -0.2600 0.6228 0.162 Uiso 1 1 calc R
C3A C 0.3665(5) 0.0000 0.6242(9) 0.166(6) Uani 1 2 d S
H3A H 0.3270 0.0000 0.6294 0.199 Uiso 1 2 calc SR
C4A C 0.5005(10) 0.100(4) 0.8629(18) 0.080(6) Uani 0.50 1 d P
H4A H 0.5315 0.1742 0.8589 0.095 Uiso 0.50 1 calc PR
C5A C 0.4390(9) -0.143(5) 0.871(3) 0.117(15) Uani 0.50 1 d P
H5A H 0.4237 -0.2542 0.8728 0.140 Uiso 0.50 1 calc PR
C6A C 0.4106(16) 0.0000 0.875(4) 0.18(4) Uani 0.50 2 d SP
H6A H 0.3711 0.0000 0.8805 0.218 Uiso 0.50 2 calc SPR
C5B C 0.4651(8) 0.140(4) 0.8710(17) 0.13(2) Uani 0.50 1 d P
H5B H 0.4781 0.2540 0.8694 0.152 Uiso 0.50 1 calc PR
C4B C 0.4056(15) -0.086(4) 0.885(2) 0.112(10) Uani 0.50 1 d P
H4B H 0.3744 -0.1573 0.8923 0.134 Uiso 0.50 1 calc PR
C6B C 0.4969(19) 0.0000 0.861(3) 0.16(4) Uani 0.50 2 d SP
H6B H 0.5353 0.0000 0.8493 0.194 Uiso 0.50 2 calc SPR
N1 N 0.5020(5) 0.5000 0.3066(8) 0.159(4) Uani 1 2 d S
N2 N 0.1015(3) 0.5000 -0.2861(7) 0.159(4) Uani 1 2 d S
F1 F 0.3076(9) 0.5000 -0.3653(13) 0.150(10) Uani 0.50 2 d SP
F2 F 0.2847(6) 0.642(2) -0.3676(9) 0.159(8) Uani 0.50 1 d P
F'1 F 0.2068(6) 0.5000 -0.3998(15) 0.127(10) Uani 0.50 2 d SP
F4 F 0.2981(5) 0.5000 0.3943(6) 0.271(6) Uani 1 2 d S
F5 F 0.3741(4) 0.6282(9) 0.4140(4) 0.275(4) Uani 1 1 d .
F3 F 0.2329(10) 0.627(3) -0.3874(12) 0.271(15) 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'
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 179.48(10) . .
S3 Ni S2 87.23(8) . .
S1 Ni S2 93.29(10) . .
S3 Ni S4 91.50(8) . .
S1 Ni S4 87.98(10) . .
S2 Ni S4 178.73(8) . .
C6A Co C6B 65.6(13) . .
C6A Co C5A 39.6(12) . 6
C6B Co C5A 54.2(9) . 6
C6A Co C5A 39.6(12) . .
C6B Co C5A 54.2(9) . .
C5A Co C5A 69(2) 6 .
C6A Co C2A 126.9(9) . 6
C6B Co C2A 139.8(5) . 6
C5A Co C2A 108.0(12) 6 6
C5A Co C2A 161.5(6) . 6
C6A Co C2A 126.9(9) . .
C6B Co C2A 139.8(5) . .
C5A Co C2A 161.5(6) 6 .
C5A Co C2A 108.0(12) . .
C2A Co C2A 68.8(5) 6 .
C6A Co C5B 51.5(7) . .
C6B Co C5B 39.8(10) . .
C5A Co C5B 17.6(7) 6 .
C5A Co C5B 70.4(9) . .
C2A Co C5B 112.5(9) 6 .
C2A Co C5B 178.3(8) . .
C6A Co C5B 51.5(7) . 6
C6B Co C5B 39.8(10) . 6
C5A Co C5B 70.4(9) 6 6
C5A Co C5B 17.6(7) . 6
C2A Co C5B 178.3(8) 6 6
C2A Co C5B 112.5(9) . 6
C5B Co C5B 66.2(18) . 6
C6A Co C1A 160.24(18) . 6
C6B Co C1A 113.6(9) . 6
C5A Co C1A 122.5(10) 6 6
C5A Co C1A 157.0(7) . 6
C2A Co C1A 40.2(2) 6 6
C2A Co C1A 67.6(3) . 6
C5B Co C1A 114.1(8) . 6
C5B Co C1A 141.0(6) 6 6
C6A Co C1A 160.24(18) . .
C6B Co C1A 113.6(9) . .
C5A Co C1A 157.0(7) 6 .
C5A Co C1A 122.5(10) . .
C2A Co C1A 67.6(3) 6 .
C2A Co C1A 40.2(2) . .
C5B Co C1A 141.0(6) . .
C5B Co C1A 114.1(7) 6 .
C1A Co C1A 39.5(3) 6 .
C6A Co C3A 111.8(12) . .
C6B Co C3A 177.4(10) . .
C5A Co C3A 123.9(9) 6 .
C5A Co C3A 123.9(9) . .
C2A Co C3A 41.5(3) 6 .
C2A Co C3A 41.5(3) . .
C5B Co C3A 138.7(8) . .
C5B Co C3A 138.7(8) 6 .
C1A Co C3A 68.8(4) 6 .
C1A Co C3A 68.8(4) . .
C6A Co C4A 68.7(13) . .
C6B Co C4A 21.3(9) . .
C5A Co C4A 42.5(11) 6 .
C5A Co C4A 71.0(12) . .
C2A Co C4A 119.9(9) 6 .
C2A Co C4A 155.4(9) . .
C5B Co C4A 25.1(9) . .
C5B Co C4A 59.4(12) 6 .
C1A Co C4A 103.4(6) 6 .
C1A Co C4A 118.4(7) . .
C3A Co C4A 158.7(9) . .
C1 S1 Ni 103.8(3) . .
C2 S2 Ni 101.1(4) . .
C6 S3 Ni 104.5(2) . .
C5 S4 Ni 104.3(2) . .
C2 C1 C4 113.0(11) . .
C2 C1 S1 122.1(6) . .
C4 C1 S1 125.0(10) . .
C1 C2 C3 129.4(9) . .
C1 C2 S2 119.7(7) . .
C3 C2 S2 110.9(8) . .
N1 C3 C2 179.6(12) . .
F5 C4 F5 109.1(17) . 6_565
F5 C4 F4 102.9(9) . .
F5 C4 F4 102.9(9) 6_565 .
F5 C4 C1 117.3(7) . .
F5 C4 C1 117.3(7) 6_565 .
F4 C4 C1 105.3(14) . .
C6 C5 C7 123.9(7) . .
C6 C5 S4 119.7(6) . .
C7 C5 S4 116.4(5) . .
C5 C6 C8 123.5(7) . .
C5 C6 S3 120.0(6) . .
C8 C6 S3 116.5(5) . .
N2 C7 C5 176.5(10) . .
F3 C8 F3 106(3) 6_565 .
F3 C8 F1 104.0(13) 6_565 .
F3 C8 F1 104.0(13) . .
F3 C8 F'1 54.8(14) 6_565 .
F3 C8 F'1 54.8(14) . .
F1 C8 F'1 130.3(13) . .
F3 C8 F2 136.4(12) 6_565 .
F3 C8 F2 54.9(10) . .
F1 C8 F2 55.2(9) . .
F'1 C8 F2 106.3(9) . .
F3 C8 F2 54.9(10) 6_565 6_565
F3 C8 F2 136.4(12) . 6_565
F1 C8 F2 55.2(9) . 6_565
F'1 C8 F2 106.3(9) . 6_565
F2 C8 F2 108.9(17) . 6_565
F3 C8 C6 113.8(10) 6_565 .
F3 C8 C6 113.8(10) . .
F1 C8 C6 114.1(12) . .
F'1 C8 C6 115.6(11) . .
F2 C8 C6 109.8(8) . .
F2 C8 C6 109.8(8) 6_565 .
C1A C1A C2A 108.7(5) 6 .
C1A C1A Co 70.25(17) 6 .
C2A C1A Co 68.7(4) . .
C1A C2A C3A 109.1(9) . .
C1A C2A Co 71.0(4) . .
C3A C2A Co 70.4(6) . .
C2A C3A C2A 104.4(11) 6 .
C2A C3A Co 68.1(5) 6 .
C2A C3A Co 68.1(5) . .
C5A C4A C4A 103(2) 6 6
C5A C4A Co 62.9(14) 6 .
C4A C4A Co 68.7(9) 6 .
C6A C5A C4A 108(2) . 6
C6A C5A Co 66(2) . .
C4A C5A Co 74.6(17) 6 .
C5A C6A C5A 118(2) 6 .
C5A C6A Co 75(2) 6 .
C5A C6A Co 75(2) . .
C6B C5B C4B 109(3) . 6
C6B C5B Co 67(2) . .
C4B C5B Co 74.2(16) 6 .
C4B C4B C5B 106.6(17) 6 6
C4B C4B Co 71.9(9) 6 .
C5B C4B Co 63.8(14) 6 .
C5B C6B C5B 110(3) 6 .
C5B C6B Co 73(2) 6 .
C5B C6B Co 73(2) . .
F2 F1 F2 129(3) 6_565 .
F2 F1 C8 65.5(12) 6_565 .
F2 F1 C8 65.5(12) . .
F3 F2 F1 110(3) . .
F3 F2 C8 57.7(11) . .
F1 F2 C8 59.2(14) . .
F3 F'1 F3 117(3) . 6_565
F3 F'1 C8 60.8(13) . .
F3 F'1 C8 60.8(13) 6_565 .
F'1 F3 F2 127(3) . .
F'1 F3 C8 64.4(17) . .
F2 F3 C8 67.4(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni S3 2.1361(19) .
Ni S1 2.138(2) .
Ni S2 2.145(2) .
Ni S4 2.146(2) .
Co C6A 1.85(5) .
Co C6B 1.91(5) .
Co C5A 1.96(3) 6
Co C5A 1.96(3) .
Co C2A 1.986(7) 6
Co C2A 1.986(7) .
Co C5B 1.99(3) .
Co C5B 1.99(3) 6
Co C1A 2.015(5) 6
Co C1A 2.015(5) .
Co C3A 2.016(10) .
Co C4A 2.12(2) .
S1 C1 1.626(12) .
S2 C2 1.739(9) .
S3 C6 1.714(7) .
S4 C5 1.714(7) .
C1 C2 1.386(12) .
C1 C4 1.539(14) .
C2 C3 1.433(14) .
C3 N1 1.170(14) .
C4 F5 1.218(10) .
C4 F5 1.218(10) 6_565
C4 F4 1.344(17) .
C5 C6 1.362(8) .
C5 C7 1.434(11) .
C6 C8 1.501(11) .
C7 N2 1.136(10) .
C8 F3 1.233(17) 6_565
C8 F3 1.233(17) .
C8 F1 1.273(19) .
C8 F'1 1.274(19) .
C8 F2 1.348(15) .
C8 F2 1.348(15) 6_565
C1A C1A 1.361(12) 6
C1A C2A 1.376(8) .
C2A C3A 1.419(9) .
C3A C2A 1.419(9) 6
C4A C5A 1.49(4) 6
C4A C4A 1.54(7) 6
C5A C6A 1.30(4) .
C5A C4A 1.49(4) 6
C6A C5A 1.30(4) 6
C5B C6B 1.33(4) .
C5B C4B 1.48(5) 6
C4B C4B 1.32(7) 6
C4B C5B 1.48(5) 6
C6B C5B 1.33(4) 6
F1 F2 1.217(18) 6_565
F1 F2 1.217(18) .
F2 F3 1.19(2) .
F'1 F3 1.15(3) .
F'1 F3 1.15(3) 6_565
