#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:56:49 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180364 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/33/7203318.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_7203318
loop_
_publ_author_name
'D. Simão'
'J. A. Ayllón'
'S. Rabaça'
'M. J. Figueira'
'I. C. Santos'
'R. T. Henriques'
'M. Almeida'
_publ_section_title
;
 [Fe(qdt)<small>₂</small>]<small>⁻</small>
 salts; an undimerised Fe<small>III</small> bisdithiolene
 complex stabilised by cation interactions
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              658
_journal_paper_doi               10.1039/b602268e
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C32 H16 Fe2 N8 S8, 2(C24 H20 As)'
_chemical_formula_sum            'C80 H56 As2 Fe2 N8 S8'
_chemical_formula_weight         1647.43
_chemical_name_common            (Ph)4As(Fe(qdt)2)
_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                100.228(9)
_cell_angle_beta                 91.538(8)
_cell_angle_gamma                100.917(8)
_cell_formula_units_Z            1
_cell_length_a                   10.6406(12)
_cell_length_b                   11.3943(10)
_cell_length_c                   15.4041(19)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     1801.1(3)
_computing_cell_refinement       'CAD4 Software (Enraf-Nonius,1994) '
_computing_data_collection       'CAD4 Software (Enraf-Nonius,1994) '
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
'SCHAKAL (Keller, 1989), Ortep3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  cad4
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7330
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_interval_count 500
_diffrn_standards_interval_time  3600
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.598
_exptl_absorpt_correction_T_max  0.8512
_exptl_absorpt_correction_T_min  0.7108
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'psi-scan (North,1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0350P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                4077
_reflns_number_total             7053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602268e.txt
_cod_data_source_block           II
_cod_database_code               7203318
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
Fe Fe 0.64210(6) 0.03987(5) 0.47047(4) 0.03358(17) Uani 1 1 d . . .
S1 S 0.57752(11) -0.04712(9) 0.58513(7) 0.0322(3) Uani 1 1 d . . .
S2 S 0.69417(12) 0.22209(10) 0.56024(8) 0.0424(3) Uani 1 1 d . . .
S3 S 0.66889(12) -0.14517(10) 0.40837(8) 0.0413(3) Uani 1 1 d . . .
S4 S 0.74436(12) 0.11582(10) 0.36243(8) 0.0436(3) Uani 1 1 d . . .
C1 C 0.5994(4) 0.0735(4) 0.6770(3) 0.0320(10) Uani 1 1 d . . .
C2 C 0.6516(4) 0.1951(4) 0.6642(3) 0.0344(11) Uani 1 1 d . . .
N1 N 0.5682(3) 0.0470(3) 0.7530(2) 0.0376(9) Uani 1 1 d . . .
N2 N 0.6676(4) 0.2870(3) 0.7313(2) 0.0399(10) Uani 1 1 d . . .
C3 C 0.5843(4) 0.1414(4) 0.8232(3) 0.0383(11) Uani 1 1 d . . .
C4 C 0.6316(4) 0.2614(4) 0.8120(3) 0.0403(12) Uani 1 1 d . . .
C5 C 0.5489(5) 0.1208(4) 0.9069(3) 0.0547(14) Uani 1 1 d . . .
H5 H 0.5189 0.0416 0.9148 0.066 Uiso 1 1 calc R . .
C6 C 0.6406(5) 0.3571(4) 0.8846(3) 0.0577(15) Uani 1 1 d . . .
H6 H 0.6722 0.4367 0.8781 0.069 Uiso 1 1 calc R . .
C7 C 0.5573(6) 0.2143(5) 0.9769(3) 0.0688(17) Uani 1 1 d . . .
H7 H 0.5330 0.1993 1.0320 0.083 Uiso 1 1 calc R . .
C8 C 0.6031(5) 0.3335(5) 0.9643(4) 0.0664(17) Uani 1 1 d . . .
H8 H 0.6080 0.3978 1.0117 0.080 Uiso 1 1 calc R . .
C9 C 0.7119(4) -0.1308(4) 0.3021(3) 0.0354(11) Uani 1 1 d . . .
C10 C 0.7430(4) -0.0109(4) 0.2799(3) 0.0367(11) Uani 1 1 d . . .
N3 N 0.7147(4) -0.2297(3) 0.2450(3) 0.0454(10) Uani 1 1 d . . .
N4 N 0.7720(4) 0.0043(3) 0.2005(3) 0.0498(11) Uani 1 1 d . . .
C11 C 0.7466(5) -0.2152(4) 0.1617(3) 0.0463(13) Uani 1 1 d . . .
C12 C 0.7740(5) -0.0991(4) 0.1389(3) 0.0532(14) Uani 1 1 d . . .
C13 C 0.7533(6) -0.3171(5) 0.0979(4) 0.0724(18) Uani 1 1 d . . .
H13 H 0.7350 -0.3940 0.1126 0.087 Uiso 1 1 calc R . .
C14 C 0.8074(7) -0.0889(5) 0.0530(4) 0.090(2) Uani 1 1 d . . .
H14 H 0.8261 -0.0128 0.0371 0.109 Uiso 1 1 calc R . .
C15 C 0.7858(7) -0.3061(6) 0.0147(4) 0.095(2) Uani 1 1 d . . .
H15 H 0.7902 -0.3748 -0.0270 0.114 Uiso 1 1 calc R . .
C16 C 0.8126(8) -0.1917(6) -0.0078(4) 0.111(3) Uani 1 1 d . . .
H16 H 0.8345 -0.1844 -0.0650 0.133 Uiso 1 1 calc R . .
As As 0.82216(5) 0.71627(4) 0.68734(3) 0.04107(15) Uani 1 1 d . . .
C20 C 0.9340(4) 0.6614(4) 0.7648(3) 0.0390(11) Uani 1 1 d . . .
C21 C 1.0371(5) 0.7401(4) 0.8104(4) 0.0540(14) Uani 1 1 d . . .
H21 H 1.0583 0.8192 0.8000 0.065 Uiso 1 1 calc R . .
C22 C 1.1098(5) 0.7029(5) 0.8715(4) 0.0657(16) Uani 1 1 d . . .
H22 H 1.1799 0.7568 0.9025 0.079 Uiso 1 1 calc R . .
C23 C 1.0787(5) 0.5860(5) 0.8867(4) 0.0642(16) Uani 1 1 d . . .
H23 H 1.1252 0.5618 0.9300 0.077 Uiso 1 1 calc R . .
C24 C 0.9794(5) 0.5053(5) 0.8382(4) 0.0632(16) Uani 1 1 d . . .
H24 H 0.9610 0.4252 0.8467 0.076 Uiso 1 1 calc R . .
C25 C 0.9064(5) 0.5418(4) 0.7771(3) 0.0505(13) Uani 1 1 d . . .
H25 H 0.8389 0.4866 0.7442 0.061 Uiso 1 1 calc R . .
C30 C 0.6511(5) 0.6742(4) 0.7225(3) 0.0430(12) Uani 1 1 d . . .
C31 C 0.5832(5) 0.7645(4) 0.7490(3) 0.0486(13) Uani 1 1 d . . .
H31 H 0.6200 0.8453 0.7487 0.058 Uiso 1 1 calc R . .
C32 C 0.4606(5) 0.7349(4) 0.7761(3) 0.0494(13) Uani 1 1 d . . .
H32 H 0.4141 0.7955 0.7934 0.059 Uiso 1 1 calc R . .
C33 C 0.4074(5) 0.6158(5) 0.7773(3) 0.0595(15) Uani 1 1 d . . .
H33 H 0.3254 0.5964 0.7967 0.071 Uiso 1 1 calc R . .
C34 C 0.4738(5) 0.5248(5) 0.7503(4) 0.0614(16) Uani 1 1 d . . .
H34 H 0.4364 0.4442 0.7505 0.074 Uiso 1 1 calc R . .
C35 C 0.5963(5) 0.5537(4) 0.7229(4) 0.0554(14) Uani 1 1 d . . .
H35 H 0.6420 0.4927 0.7047 0.067 Uiso 1 1 calc R . .
C40 C 0.8731(4) 0.8896(4) 0.6986(3) 0.0422(12) Uani 1 1 d . . .
C41 C 0.8789(5) 0.9640(4) 0.7797(4) 0.0588(15) Uani 1 1 d . . .
H41 H 0.8567 0.9310 0.8295 0.071 Uiso 1 1 calc R . .
C42 C 0.9181(5) 1.0887(5) 0.7869(4) 0.0687(17) Uani 1 1 d . . .
H42 H 0.9217 1.1394 0.8417 0.082 Uiso 1 1 calc R . .
C43 C 0.9511(5) 1.1369(5) 0.7149(5) 0.0719(19) Uani 1 1 d . . .
H43 H 0.9785 1.2205 0.7204 0.086 Uiso 1 1 calc R . .
C44 C 0.9441(5) 1.0628(5) 0.6334(5) 0.0673(17) Uani 1 1 d . . .
H44 H 0.9664 1.0967 0.5840 0.081 Uiso 1 1 calc R . .
C45 C 0.9044(4) 0.9382(4) 0.6244(4) 0.0510(14) Uani 1 1 d . . .
H45 H 0.8989 0.8880 0.5692 0.061 Uiso 1 1 calc R . .
C50 C 0.8317(5) 0.6399(4) 0.5683(3) 0.0459(13) Uani 1 1 d . . .
C51 C 0.9479(5) 0.6583(4) 0.5286(4) 0.0576(15) Uani 1 1 d . . .
H51 H 1.0204 0.7068 0.5607 0.069 Uiso 1 1 calc R . .
C52 C 0.9562(6) 0.6053(5) 0.4423(4) 0.0663(16) Uani 1 1 d . . .
H52 H 1.0331 0.6201 0.4151 0.080 Uiso 1 1 calc R . .
C53 C 0.8516(7) 0.5313(6) 0.3969(4) 0.088(2) Uani 1 1 d . . .
H53 H 0.8574 0.4959 0.3382 0.106 Uiso 1 1 calc R . .
C54 C 0.7377(7) 0.5077(6) 0.4354(4) 0.101(2) Uani 1 1 d . . .
H54 H 0.6679 0.4537 0.4042 0.121 Uiso 1 1 calc R . .
C55 C 0.7269(6) 0.5648(6) 0.5214(4) 0.0768(19) Uani 1 1 d . . .
H55 H 0.6486 0.5521 0.5472 0.092 Uiso 1 1 calc R . .
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'
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'
As As 0.0499 2.0058 '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
S4 Fe S3 89.65(5) . . ?
S4 Fe S1 168.26(5) . . ?
S3 Fe S1 84.88(4) . . ?
S4 Fe S2 90.40(5) . . ?
S3 Fe S2 155.75(6) . . ?
S1 Fe S2 90.35(5) . . ?
S4 Fe S1 96.25(5) . 2_656 ?
S3 Fe S1 103.75(5) . 2_656 ?
S1 Fe S1 95.14(4) . 2_656 ?
S2 Fe S1 100.35(5) . 2_656 ?
C1 S1 Fe 105.16(14) . . ?
C1 S1 Fe 99.92(14) . 2_656 ?
Fe S1 Fe 84.86(4) . 2_656 ?
C2 S2 Fe 105.03(14) . . ?
C9 S3 Fe 104.43(15) . . ?
C10 S4 Fe 104.26(15) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C1 S1 117.6(3) . . ?
C2 C1 S1 118.9(3) . . ?
N2 C2 C1 120.2(4) . . ?
N2 C2 S2 119.3(3) . . ?
C1 C2 S2 120.5(3) . . ?
C1 N1 C3 116.9(4) . . ?
C2 N2 C4 117.2(4) . . ?
N1 C3 C5 120.4(4) . . ?
N1 C3 C4 120.7(4) . . ?
C5 C3 C4 118.9(4) . . ?
N2 C4 C6 119.3(4) . . ?
N2 C4 C3 121.4(4) . . ?
C6 C4 C3 119.3(4) . . ?
C7 C5 C3 121.5(5) . . ?
C8 C6 C4 120.0(5) . . ?
C5 C7 C8 118.9(5) . . ?
C6 C8 C7 121.4(5) . . ?
N3 C9 C10 122.4(4) . . ?
N3 C9 S3 118.3(3) . . ?
C10 C9 S3 119.3(3) . . ?
N4 C10 C9 121.6(4) . . ?
N4 C10 S4 119.6(3) . . ?
C9 C10 S4 118.8(3) . . ?
C9 N3 C11 116.8(4) . . ?
C10 N4 C12 116.9(4) . . ?
N3 C11 C13 119.6(5) . . ?
N3 C11 C12 121.3(4) . . ?
C13 C11 C12 119.1(5) . . ?
N4 C12 C14 119.8(5) . . ?
N4 C12 C11 121.1(4) . . ?
C14 C12 C11 119.2(5) . . ?
C15 C13 C11 121.3(5) . . ?
C16 C14 C12 119.8(6) . . ?
C13 C15 C16 119.7(6) . . ?
C14 C16 C15 121.0(6) . . ?
C50 As C30 109.6(2) . . ?
C50 As C40 109.8(2) . . ?
C30 As C40 110.47(19) . . ?
C50 As C20 110.5(2) . . ?
C30 As C20 107.82(18) . . ?
C40 As C20 108.73(19) . . ?
C21 C20 C25 119.7(5) . . ?
C21 C20 As 120.7(3) . . ?
C25 C20 As 119.5(4) . . ?
C20 C21 C22 120.3(5) . . ?
C23 C22 C21 119.9(5) . . ?
C24 C23 C22 119.9(5) . . ?
C23 C24 C25 120.4(5) . . ?
C24 C25 C20 119.6(5) . . ?
C31 C30 C35 120.2(5) . . ?
C31 C30 As 119.5(3) . . ?
C35 C30 As 120.3(4) . . ?
C30 C31 C32 119.8(4) . . ?
C33 C32 C31 119.9(5) . . ?
C32 C33 C34 120.8(5) . . ?
C33 C34 C35 119.7(5) . . ?
C34 C35 C30 119.7(5) . . ?
C41 C40 C45 120.5(4) . . ?
C41 C40 As 120.3(4) . . ?
C45 C40 As 119.2(4) . . ?
C40 C41 C42 119.6(5) . . ?
C43 C42 C41 120.4(6) . . ?
C42 C43 C44 120.2(5) . . ?
C43 C44 C45 120.6(5) . . ?
C40 C45 C44 118.8(5) . . ?
C55 C50 C51 119.3(5) . . ?
C55 C50 As 121.2(4) . . ?
C51 C50 As 119.5(4) . . ?
C52 C51 C50 120.3(5) . . ?
C53 C52 C51 119.6(6) . . ?
C52 C53 C54 121.3(6) . . ?
C53 C54 C55 119.6(6) . . ?
C50 C55 C54 119.8(6) . . ?
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
Fe S4 2.2259(13) . ?
Fe S3 2.2289(13) . ?
Fe S1 2.2368(12) . ?
Fe S2 2.2436(13) . ?
Fe S1 2.4884(13) 2_656 ?
S1 C1 1.765(4) . ?
S1 Fe 2.4884(13) 2_656 ?
S2 C2 1.739(4) . ?
S3 C9 1.739(4) . ?
S4 C10 1.744(4) . ?
C1 N1 1.297(5) . ?
C1 C2 1.442(5) . ?
C2 N2 1.317(5) . ?
N1 C3 1.365(5) . ?
N2 C4 1.375(5) . ?
C3 C5 1.399(6) . ?
C3 C4 1.407(6) . ?
C4 C6 1.404(6) . ?
C5 C7 1.362(6) . ?
C6 C8 1.357(7) . ?
C7 C8 1.403(7) . ?
C9 N3 1.306(5) . ?
C9 C10 1.447(5) . ?
C10 N4 1.302(5) . ?
N3 C11 1.365(6) . ?
N4 C12 1.380(6) . ?
C11 C13 1.396(6) . ?
C11 C12 1.408(6) . ?
C12 C14 1.398(7) . ?
C13 C15 1.356(7) . ?
C14 C16 1.375(7) . ?
C15 C16 1.388(8) . ?
As C50 1.899(5) . ?
As C30 1.911(5) . ?
As C40 1.922(4) . ?
As C20 1.924(5) . ?
C20 C21 1.365(6) . ?
C20 C25 1.386(6) . ?
C21 C22 1.375(7) . ?
C22 C23 1.374(7) . ?
C23 C24 1.366(7) . ?
C24 C25 1.372(7) . ?
C30 C31 1.377(6) . ?
C30 C35 1.387(6) . ?
C31 C32 1.379(6) . ?
C32 C33 1.371(6) . ?
C33 C34 1.373(7) . ?
C34 C35 1.379(6) . ?
C40 C41 1.372(6) . ?
C40 C45 1.378(6) . ?
C41 C42 1.387(6) . ?
C42 C43 1.348(8) . ?
C43 C44 1.375(8) . ?
C44 C45 1.383(6) . ?
C50 C55 1.368(7) . ?
C50 C51 1.391(6) . ?
C51 C52 1.372(7) . ?
C52 C53 1.353(7) . ?
C53 C54 1.366(8) . ?
C54 C55 1.386(8) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C25 H25 N2 0.93 2.60 3.430(5) 1_555 148.1 ?
C35 H35 N2 0.93 2.51 3.292(6) 1_555 141.5 ?
C21 H21 N4 0.93 2.44 3.253(6) 2_766 146.6 ?
C31 H31 N1 0.93 2.45 3.243(6) 1_565 142.7 ?
C34 H34 N3 0.93 2.67 3.589(6) 2_656 168.5 ?
