The Series of Molecular Conductors and Superconductors ET4[AFe(C2O4)3].PhX (ET = bis(ethylenedithio)tetrathiafulvalene; (C2O4)2-= oxalate; A+= H3O+, K+; X = F, Cl, Br, and I): Influence of the Halobenzene Guest Molecules on the Crystal Structure and Superconducting Properties
Eugenio Coronado; Simona Curreli; Carlos Giménez-Saiz; Carlos J. Gómez-García; Inorganic Chemistry 51 (2012) 1111–1126; doi:10.1021/ic202269x

data_4328038
_publ_section_title
;
 The Series of Molecular Conductors and Superconductors
 ET4[AFe(C2O4)3].PhX (ET = bis(ethylenedithio)tetrathiafulvalene;
 (C2O4)2-= oxalate; A+= H3O+, K+; X = F, Cl, Br, and I): Influence of the
 Halobenzene Guest Molecules on the Crystal Structure and Superconducting
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1111
_journal_page_last               1126
_journal_paper_doi               10.1021/ic202269x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'4(C10 H8 S8), (C6 Fe O12), (C6 H5 Cl), (H3 O)'
_chemical_formula_sum            'C52 H40 Cl Fe O13 S32'
_chemical_formula_weight         1990.06
_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                89.0829(10)
_cell_angle_beta                 86.5203(11)
_cell_angle_gamma                62.6678(13)
_cell_formula_units_Z            2
_cell_length_a                   10.25276(14)
_cell_length_b                   11.15081(13)
_cell_length_c                   35.1363(5)
_cell_measurement_reflns_used    44293
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.5006
_cell_measurement_theta_min      2.2356
_cell_volume                     3561.65(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega  -50.00  -23.00   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469  112.0000   -8.0000 45

  2 omega   26.00   68.00   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469 -112.0000 -171.0000 70

  3 omega  -69.00  -39.60   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469  112.0000  101.0000 49

  4 omega    8.00   34.40   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469 -112.0000   78.0000 44

  5 omega   -5.00   21.40   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469 -112.0000 -171.0000 44

  6 omega   80.00  128.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250  112.0000  -78.0000 80

  7 omega  -14.00   44.20   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250 -112.0000 -101.0000 97

  8 omega   26.00   54.80   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250 -112.0000    8.0000 48

  9 omega   92.00  131.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250  112.0000  171.0000 65

 10 omega  -72.00  -45.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5187  112.0000  -78.0000 45

 11 omega  -51.00  -21.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5187  112.0000  101.0000 50

 12 omega -110.00  -26.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5187  112.0000  171.0000 139

 13 omega  -42.00   99.00   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469   77.0000  -60.0000 235

 14 omega  -87.00   55.20   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469  -37.0000  -60.0000 237

 15 omega  -38.00  -11.00   0.6000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469  112.0000  101.0000 45

 16 omega  -42.00  -12.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   37.0000   90.0000 49

 17 omega  -18.00   53.40   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   37.0000  -90.0000 119

 18 omega   65.00  107.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   37.0000  -90.0000 71

 19 omega   57.00  124.20   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   37.0000   90.0000 112

 20 omega   -4.00   37.40   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000  -30.0000 69

 21 omega   53.00  128.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000  -30.0000 125

 22 omega   -9.00  138.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000  120.0000 245

 23 omega   -2.00  121.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000  -90.0000 205

 24 omega   -7.00   45.20   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000   30.0000 87

 25 omega   59.00   89.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000   30.0000 51

 26 omega   94.00  139.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000   30.0000 75

 27 omega  -49.00    5.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250  -37.0000    0.0000 90

 28 omega   73.00  125.80   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250  125.0000   60.0000 88

 29 omega   23.00   69.80   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250  -37.0000    0.0000 78

 30 omega   10.00   46.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   37.0000   90.0000 60

 31 omega   65.00  104.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000 -150.0000 66

 32 omega  -11.00   31.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4250   77.0000 -150.0000 70

 33 omega    7.00   37.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5187 -127.0000 -169.0000 50

 34 omega -109.00  -22.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5187  112.0000   -8.0000 144

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0616464000
_diffrn_orient_matrix_UB_12      0.0245306000
_diffrn_orient_matrix_UB_13      -0.0113966000
_diffrn_orient_matrix_UB_21      0.0457026000
_diffrn_orient_matrix_UB_22      -0.0023537000
_diffrn_orient_matrix_UB_23      -0.0162537000
_diffrn_orient_matrix_UB_31      0.0140546000
_diffrn_orient_matrix_UB_32      -0.0672361000
_diffrn_orient_matrix_UB_33      -0.0038772000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            82681
_diffrn_reflns_theta_full        30.75
_diffrn_reflns_theta_max         31.57
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       prism
_exptl_crystal_F_000             2022
_exptl_crystal_size_max          0.4065
_exptl_crystal_size_mid          0.2743
_exptl_crystal_size_min          0.1774
_refine_diff_density_max         3.600
_refine_diff_density_min         -2.552
_refine_diff_density_rms         0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         22856
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.1369
_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/[\s^2^(Fo^2^)+(0.0359P)^2^+134.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3116
_refine_ls_wR_factor_ref         0.3130
_reflns_number_gt                21205
_reflns_number_total             22856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202269x_si_002_6.cif
_cod_data_source_block           Compound_2_120K
_cod_original_cell_volume        3561.65(8)
_cod_database_code               4328038