#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:24:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180077 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/23/7052367.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_7052367
loop_
_publ_author_name
'Olivier Jeannin'
'Marc Fourmigué'
_publ_section_title
;
 Perylene salts of unsymmetrical nickel and gold dithiolene complexes
 with 3 ∶ 2 stoichiometry: conformational polymorphism and
 strong antiferromagnetic interactions
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1774
_journal_paper_doi               10.1039/b608420f
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety         '3(C20 H12), 2(C8 F6 N2 Au S4)'
_chemical_formula_sum            'C76 H36 Au2 F12 N4 S8'
_chemical_formula_weight         1883.50
_chemical_name_common            '(Perylene)3, [Au(tfadt)2]2'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.176(13)
_cell_angle_beta                 103.135(14)
_cell_angle_gamma                96.571(15)
_cell_formula_units_Z            1
_cell_length_a                   10.8670(13)
_cell_length_b                   12.7568(16)
_cell_length_c                   13.2210(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.1
_cell_volume                     1624.9(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 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 1.8 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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15849
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    4.853
_exptl_absorpt_correction_T_max  0.8153
_exptl_absorpt_correction_T_min  0.1486
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of 14 x 8 x 8 = 896 sampling points was used
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    Constr.
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0258
_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)+(0.0232P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0499
_reflns_number_gt                4750
_reflns_number_total             5865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608420f.txt
_cod_data_source_block           ojec162
_cod_original_cell_volume        1624.9(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052367
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.6558
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au Au 0.094203(18) -0.038430(17) -0.116927(13) 0.03715(6) Uani 1 1 d . . .
S1 S 0.24502(12) 0.08682(10) 0.04974(8) 0.0520(3) Uani 1 1 d . . .
S2 S 0.05327(12) 0.11291(10) -0.16546(8) 0.0492(3) Uani 1 1 d . . .
S3 S -0.05715(12) -0.16312(10) -0.28366(8) 0.0520(3) Uani 1 1 d . . .
S4 S 0.13813(12) -0.19073(10) -0.07076(9) 0.0493(3) Uani 1 1 d . . .
C1 C 0.2320(4) 0.2192(4) 0.0409(3) 0.0473(11) Uani 1 1 d . . .
C2 C 0.1535(4) 0.2293(4) -0.0476(3) 0.0439(10) Uani 1 1 d . . .
C3 C 0.3141(5) 0.3146(5) 0.1382(4) 0.0647(14) Uani 1 1 d . . .
C4 C 0.1445(5) 0.3442(4) -0.0540(4) 0.0563(12) Uani 1 1 d . . .
C5 C -0.0375(5) -0.2962(4) -0.2794(3) 0.0498(11) Uani 1 1 d . . .
C6 C 0.0441(4) -0.3070(4) -0.1928(3) 0.0482(11) Uani 1 1 d . . .
C7 C -0.1204(6) -0.3923(5) -0.3785(4) 0.0741(16) Uani 1 1 d . . .
C8 C 0.0651(6) -0.4221(4) -0.1969(4) 0.0638(14) Uani 1 1 d . . .
C1A C 0.2263(4) -0.1932(4) -0.3975(3) 0.0522(12) Uani 1 1 d . . .
C2A C 0.1319(5) -0.2466(5) -0.5047(4) 0.0711(16) Uani 1 1 d . . .
H2A H 0.0998 -0.3257 -0.5350 0.085 Uiso 1 1 calc R . .
C3A C 0.0879(5) -0.1852(6) -0.5632(4) 0.0724(17) Uani 1 1 d . . .
H3A H 0.0274 -0.2222 -0.6342 0.087 Uiso 1 1 calc R . .
C4A C 0.1321(4) -0.0671(5) -0.5186(3) 0.0593(14) Uani 1 1 d . . .
H4A H 0.0993 -0.0263 -0.5604 0.071 Uiso 1 1 calc R . .
C5A C 0.2239(4) -0.0068(4) -0.4134(3) 0.0390(10) Uani 1 1 d . . .
C6A C 0.2722(4) 0.1166(4) -0.3656(3) 0.0407(10) Uani 1 1 d . . .
C7A C 0.2301(5) 0.1858(5) -0.4213(4) 0.0588(13) Uani 1 1 d . . .
H7A H 0.1681 0.1515 -0.4917 0.071 Uiso 1 1 calc R . .
C8A C 0.2769(6) 0.3030(6) -0.3760(5) 0.0768(17) Uani 1 1 d . . .
H8A H 0.2453 0.3462 -0.4156 0.092 Uiso 1 1 calc R . .
C9A C 0.3692(6) 0.3567(5) -0.2735(5) 0.0707(15) Uani 1 1 d . . .
H9A H 0.4007 0.4358 -0.2443 0.085 Uiso 1 1 calc R . .
C10A C 0.4164(5) 0.2931(4) -0.2121(4) 0.0537(12) Uani 1 1 d . . .
C11A C 0.5112(5) 0.3452(5) -0.1052(4) 0.0716(15) Uani 1 1 d . . .
H11A H 0.5444 0.4242 -0.0746 0.086 Uiso 1 1 calc R . .
C12A C 0.5549(5) 0.2821(6) -0.0462(4) 0.0723(16) Uani 1 1 d . . .
H12A H 0.6163 0.3185 0.0243 0.087 Uiso 1 1 calc R . .
C13A C 0.5087(4) 0.1646(5) -0.0903(3) 0.0572(13) Uani 1 1 d . . .
H13A H 0.5395 0.1229 -0.0487 0.069 Uiso 1 1 calc R . .
C14A C 0.4161(4) 0.1067(4) -0.1965(3) 0.0423(11) Uani 1 1 d . . .
C15A C 0.3694(4) -0.0168(4) -0.2432(3) 0.0408(10) Uani 1 1 d . . .
C16A C 0.4137(5) -0.0871(5) -0.1891(3) 0.0559(12) Uani 1 1 d . . .
H16A H 0.4762 -0.0533 -0.1189 0.067 Uiso 1 1 calc R . .
C17A C 0.3686(6) -0.2040(5) -0.2355(4) 0.0672(14) Uani 1 1 d . . .
H17A H 0.4012 -0.2475 -0.1968 0.081 Uiso 1 1 calc R . .
C18A C 0.2773(6) -0.2568(5) -0.3370(4) 0.0690(15) Uani 1 1 d . . .
H18A H 0.2478 -0.3363 -0.3672 0.083 Uiso 1 1 calc R . .
C19A C 0.2734(4) -0.0712(4) -0.3512(3) 0.0392(10) Uani 1 1 d . . .
C20A C 0.3682(4) 0.1717(4) -0.2574(3) 0.0397(10) Uani 1 1 d . . .
C1B C 0.5953(5) 0.2428(4) 0.5963(4) 0.0556(12) Uani 1 1 d . . .
C2B C 0.5483(6) 0.3079(5) 0.5368(5) 0.0721(16) Uani 1 1 d . . .
H2B H 0.5782 0.3874 0.5689 0.087 Uiso 1 1 calc R . .
C3B C 0.4596(6) 0.2571(5) 0.4328(5) 0.0753(17) Uani 1 1 d . . .
H3B H 0.4309 0.3016 0.3938 0.090 Uiso 1 1 calc R . .
C4B C 0.4119(5) 0.1393(5) 0.3851(4) 0.0598(14) Uani 1 1 d . . .
H4B H 0.3503 0.1060 0.3144 0.072 Uiso 1 1 calc R . .
C5B C 0.4537(4) 0.0684(4) 0.4401(3) 0.0418(10) Uani 1 1 d . . .
C6B C 0.4057(4) -0.0541(4) 0.3919(3) 0.0424(11) Uani 1 1 d . . .
C7B C 0.3137(4) -0.1132(5) 0.2853(3) 0.0585(13) Uani 1 1 d . . .
H7B H 0.2820 -0.0712 0.2445 0.070 Uiso 1 1 calc R . .
C8B C 0.2685(5) -0.2308(6) 0.2388(4) 0.0742(17) Uani 1 1 d . . .
H8B H 0.2081 -0.2666 0.1676 0.089 Uiso 1 1 calc R . .
C9B C 0.6881(5) 0.2944(5) 0.7035(4) 0.0725(16) Uani 1 1 d . . .
H9B H 0.7203 0.3736 0.7352 0.087 Uiso 1 1 calc R . .
C10B C 0.5477(4) 0.1217(4) 0.5480(3) 0.0416(10) Uani 1 1 d . . .
N1 N 0.3824(6) 0.3871(5) 0.2185(4) 0.1001(18) Uani 1 1 d . . .
N2 N -0.1881(7) -0.4633(4) -0.4579(4) 0.119(2) Uani 1 1 d . . .
F1 F 0.2326(12) 0.4313(8) 0.0146(11) 0.094(4) Uani 0.50 1 d P . .
F2 F 0.1424(11) 0.3373(8) -0.1584(7) 0.075(3) Uani 0.50 1 d P . .
F3 F 0.0356(9) 0.3707(7) -0.0444(12) 0.072(2) Uani 0.50 1 d P . .
F'1 F 0.2543(12) 0.3977(11) -0.0468(15) 0.119(6) Uani 0.50 1 d P . .
F'2 F 0.056(2) 0.3416(9) -0.1358(16) 0.193(9) Uani 0.50 1 d P . .
F'3 F 0.125(2) 0.4166(10) 0.0396(12) 0.134(4) Uani 0.50 1 d P . .
F4 F 0.1279(3) -0.4192(3) -0.0978(3) 0.0959(11) Uani 1 1 d . . .
F5 F -0.0437(4) -0.4991(3) -0.2298(3) 0.1147(14) Uani 1 1 d . . .
F6 F 0.1287(6) -0.4668(4) -0.2662(4) 0.172(2) Uani 1 1 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'
Au Au -2.0133 8.8022 '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'
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 Au S1 90.47(4) . . ?
S2 Au S4 178.77(5) . . ?
S1 Au S4 89.70(4) . . ?
S2 Au S3 89.31(4) . . ?
S1 Au S3 179.75(5) . . ?
S4 Au S3 90.52(4) . . ?
C1 S1 Au 100.78(14) . . ?
C2 S2 Au 101.46(14) . . ?
C5 S3 Au 100.72(15) . . ?
C6 S4 Au 101.12(15) . . ?
C2 C1 C3 123.8(4) . . ?
C2 C1 S1 123.7(3) . . ?
C3 C1 S1 112.6(3) . . ?
C1 C2 C4 122.8(4) . . ?
C1 C2 S2 123.5(4) . . ?
C4 C2 S2 113.6(3) . . ?
N1 C3 C1 176.3(6) . . ?
F'2 C4 F1 125.8(8) . . ?
F'2 C4 F'1 112.4(12) . . ?
F1 C4 F'1 40.1(6) . . ?
F'2 C4 F3 56.8(11) . . ?
F1 C4 F3 106.9(7) . . ?
F'1 C4 F3 135.9(7) . . ?
F'2 C4 F'3 106.3(12) . . ?
F1 C4 F'3 60.0(8) . . ?
F'1 C4 F'3 99.8(9) . . ?
F3 C4 F'3 54.2(7) . . ?
F'2 C4 F2 47.2(12) . . ?
F1 C4 F2 106.1(9) . . ?
F'1 C4 F2 72.6(8) . . ?
F3 C4 F2 102.9(7) . . ?
F'3 C4 F2 138.7(7) . . ?
F'2 C4 C2 115.7(6) . . ?
F1 C4 C2 118.1(5) . . ?
F'1 C4 C2 110.7(7) . . ?
F3 C4 C2 111.9(5) . . ?
F'3 C4 C2 110.8(5) . . ?
F2 C4 C2 109.8(5) . . ?
C6 C5 C7 123.9(4) . . ?
C6 C5 S3 123.6(4) . . ?
C7 C5 S3 112.4(3) . . ?
C5 C6 C8 121.7(4) . . ?
C5 C6 S4 123.6(4) . . ?
C8 C6 S4 114.7(3) . . ?
N2 C7 C5 176.2(6) . . ?
F6 C8 F4 106.8(5) . . ?
F6 C8 F5 105.4(5) . . ?
F4 C8 F5 104.7(4) . . ?
F6 C8 C6 112.6(4) . . ?
F4 C8 C6 113.3(4) . . ?
F5 C8 C6 113.3(5) . . ?
C18A C1A C2A 122.0(5) . . ?
C18A C1A C19A 119.2(4) . . ?
C2A C1A C19A 118.7(5) . . ?
C3A C2A C1A 121.3(5) . . ?
C2A C3A C4A 120.3(5) . . ?
C3A C4A C5A 122.6(5) . . ?
C4A C5A C19A 117.7(4) . . ?
C4A C5A C6A 123.4(4) . . ?
C19A C5A C6A 118.8(3) . . ?
C7A C6A C20A 117.5(4) . . ?
C7A C6A C5A 122.6(4) . . ?
C20A C6A C5A 119.9(4) . . ?
C8A C7A C6A 122.4(5) . . ?
C9A C8A C7A 120.7(5) . . ?
C8A C9A C10A 120.3(5) . . ?
C9A C10A C11A 122.2(5) . . ?
C9A C10A C20A 119.6(4) . . ?
C11A C10A C20A 118.1(5) . . ?
C12A C11A C10A 121.4(5) . . ?
C11A C12A C13A 120.5(5) . . ?
C12A C13A C14A 121.3(5) . . ?
C13A C14A C20A 118.6(4) . . ?
C13A C14A C15A 121.1(4) . . ?
C20A C14A C15A 120.2(4) . . ?
C16A C15A C19A 117.7(4) . . ?
C16A C15A C14A 123.6(4) . . ?
C19A C15A C14A 118.8(4) . . ?
C17A C16A C15A 122.4(4) . . ?
C18A C17A C16A 120.9(5) . . ?
C17A C18A C1A 120.8(5) . . ?
C5A C19A C1A 119.4(4) . . ?
C5A C19A C15A 121.6(4) . . ?
C1A C19A C15A 119.0(4) . . ?
C14A C20A C10A 120.0(4) . . ?
C14A C20A C6A 120.6(4) . . ?
C10A C20A C6A 119.4(4) . . ?
C2B C1B C9B 121.7(5) . . ?
C2B C1B C10B 119.3(5) . . ?
C9B C1B C10B 119.0(5) . . ?
C3B C2B C1B 121.2(5) . . ?
C2B C3B C4B 120.1(5) . . ?
C3B C4B C5B 121.9(5) . . ?
C4B C5B C10B 117.8(4) . . ?
C4B C5B C6B 122.8(4) . . ?
C10B C5B C6B 119.4(4) . . ?
C7B C6B C10B 117.0(4) . 2_656 ?
C7B C6B C5B 122.8(4) . . ?
C10B C6B C5B 120.2(4) 2_656 . ?
C8B C7B C6B 122.8(5) . . ?
C9B C8B C7B 120.1(5) 2_656 . ?
C8B C9B C1B 121.2(5) 2_656 . ?
C1B C10B C5B 119.7(4) . . ?
C1B C10B C6B 119.9(4) . 2_656 ?
C5B C10B C6B 120.4(4) . 2_656 ?
F'1 F1 C4 70.1(11) . . ?
F'1 F1 F'3 131.8(16) . . ?
C4 F1 F'3 62.4(7) . . ?
F'2 F2 C4 62.0(9) . . ?
F'2 F2 F'1 106.5(11) . . ?
C4 F2 F'1 51.5(5) . . ?
F'3 F3 F'2 119.0(11) . . ?
F'3 F3 C4 64.7(6) . . ?
F'2 F3 C4 60.4(8) . . ?
F1 F'1 C4 69.8(11) . . ?
F1 F'1 F2 116.6(15) . . ?
C4 F'1 F2 56.0(7) . . ?
F2 F'2 F3 131.6(12) . . ?
F2 F'2 C4 70.8(10) . . ?
F3 F'2 C4 62.8(8) . . ?
F3 F'3 F1 110.8(9) . . ?
F3 F'3 C4 61.1(7) . . ?
F1 F'3 C4 57.6(5) . . ?
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
Au S2 2.3019(12) . ?
Au S1 2.3044(13) . ?
Au S4 2.3047(12) . ?
Au S3 2.3054(13) . ?
S1 C1 1.753(5) . ?
S2 C2 1.734(4) . ?
S3 C5 1.754(5) . ?
S4 C6 1.738(4) . ?
C1 C2 1.341(6) . ?
C1 C3 1.425(7) . ?
C2 C4 1.511(6) . ?
C3 N1 1.143(6) . ?
C4 F'2 1.258(10) . ?
C4 F1 1.267(10) . ?
C4 F'1 1.270(12) . ?
C4 F3 1.288(8) . ?
C4 F'3 1.330(9) . ?
C4 F2 1.346(8) . ?
C5 C6 1.340(6) . ?
C5 C7 1.443(7) . ?
C6 C8 1.495(6) . ?
C7 N2 1.129(6) . ?
C8 F6 1.282(6) . ?
C8 F4 1.318(5) . ?
C8 F5 1.321(6) . ?
C1A C18A 1.405(7) . ?
C1A C2A 1.417(7) . ?
C1A C19A 1.431(6) . ?
C2A C3A 1.340(8) . ?
C3A C4A 1.383(8) . ?
C4A C5A 1.393(6) . ?
C5A C19A 1.424(6) . ?
C5A C6A 1.447(6) . ?
C6A C7A 1.393(6) . ?
C6A C20A 1.433(5) . ?
C7A C8A 1.376(8) . ?
C8A C9A 1.366(8) . ?
C9A C10A 1.401(7) . ?
C10A C11A 1.416(7) . ?
C10A C20A 1.426(6) . ?
C11A C12A 1.362(8) . ?
C12A C13A 1.379(7) . ?
C13A C14A 1.403(5) . ?
C14A C20A 1.413(6) . ?
C14A C15A 1.447(6) . ?
C15A C16A 1.398(6) . ?
C15A C19A 1.431(5) . ?
C16A C17A 1.369(7) . ?
C17A C18A 1.352(7) . ?
C1B C2B 1.399(7) . ?
C1B C9B 1.408(7) . ?
C1B C10B 1.421(6) . ?
C2B C3B 1.360(8) . ?
C3B C4B 1.384(7) . ?
C4B C5B 1.404(6) . ?
C5B C10B 1.421(6) . ?
C5B C6B 1.437(6) . ?
C6B C7B 1.404(6) . ?
C6B C10B 1.429(6) 2_656 ?
C7B C8B 1.377(8) . ?
C8B C9B 1.354(8) 2_656 ?
C9B C8B 1.354(8) 2_656 ?
C10B C6B 1.429(6) 2_656 ?
F1 F'1 0.870(12) . ?
F1 F'3 1.299(15) . ?
F2 F'2 1.05(3) . ?
F2 F'1 1.549(17) . ?
F3 F'3 1.193(15) . ?
F3 F'2 1.21(2) . ?
