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_4328039
_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 Br), (H3 O)'
_chemical_formula_sum            'C52 H40 Br Fe O13 S32'
_chemical_formula_weight         2034.52
_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                89.1001(12)
_cell_angle_beta                 86.3083(12)
_cell_angle_gamma                62.7251(16)
_cell_formula_units_Z            2
_cell_length_a                   10.25554(17)
_cell_length_b                   11.16966(18)
_cell_length_c                   35.1997(5)
_cell_measurement_reflns_used    75259
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.4838
_cell_measurement_theta_min      2.2343
_cell_volume                     3575.98(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
  1 omega  -45.00   87.30   0.7000    1.7000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250   77.0000 -120.0000 189

  2 omega  -89.00   44.00   0.7000    1.7000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250  -77.0000 -180.0000 190

  3 omega   61.00  117.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   37.0000   30.0000 80

  4 omega   -6.00  124.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   77.0000 -120.0000 186

  5 omega   -8.00  101.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   77.0000   60.0000 156

  6 omega   80.00  111.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  125.0000  -30.0000 45

  7 omega   -8.00  118.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   77.0000  -30.0000 180

  8 omega  -15.00   17.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   37.0000   30.0000 46

  9 omega   -8.00   85.10   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   77.0000  150.0000 133

 10 omega  -41.00   81.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  -77.0000  -90.0000 175

 11 omega  -40.00   69.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  -37.0000  -30.0000 156

 12 omega  -43.00   81.60   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  -77.0000  150.0000 178

 13 omega  -28.00   -0.70   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   37.0000 -150.0000 39

 14 omega   61.00  119.10   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   37.0000 -150.0000 83

 15 omega  -23.00    4.30   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124  -77.0000  150.0000 39

 16 omega -122.00  -70.90   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124  -77.0000  150.0000 73

 17 omega  -98.50  -18.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124  125.0000   60.0000 115

 18 omega    8.00   33.90   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124 -128.0000  139.0000 37

 19 omega   34.00   95.60   0.7000    1.7000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250  179.0000  -60.0000 88

 20 omega   34.00   95.60   0.7000    1.7000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250  179.0000  150.0000 88

 21 omega   -9.00  124.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   77.0000  -30.0000 190

 22 omega   -9.00  124.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   77.0000 -180.0000 190

 23 omega   -9.00  124.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624   77.0000  120.0000 190

 24 omega   73.00  118.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  125.0000   30.0000 65

 25 omega   73.00  118.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  125.0000  -90.0000 65

 26 omega   73.00  118.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  125.0000  150.0000 65

 27 omega   73.00  118.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  125.0000   90.0000 65

 28 omega -109.00  -18.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124  125.0000   30.0000 130

 29 omega  -83.00   50.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124   77.0000 -120.0000 190

 30 omega   -1.00   34.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124 -128.0000  139.0000 50

 31 omega  -46.00   87.00   0.7000    1.7000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250   77.0000  120.0000 190

 32 omega   34.00   95.60   0.7000    1.7000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250  179.0000   60.0000 88

 33 omega  -52.00   81.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  -77.0000   30.0000 190

 34 omega  -52.00   81.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  -77.0000  -60.0000 190

 35 omega   73.00  118.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6624  125.0000 -150.0000 65

 36 omega -126.00    7.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124  -77.0000  -90.0000 190

 37 omega -126.00    7.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124  -77.0000   60.0000 190

 38 omega -126.00    7.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9124  -77.0000  -30.0000 190

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0483121000
_diffrn_orient_matrix_UB_12      -0.0276291000
_diffrn_orient_matrix_UB_13      -0.0033195000
_diffrn_orient_matrix_UB_21      0.0580558000
_diffrn_orient_matrix_UB_22      -0.0547070000
_diffrn_orient_matrix_UB_23      -0.0102171000
_diffrn_orient_matrix_UB_31      0.0193826000
_diffrn_orient_matrix_UB_32      -0.0367359000
_diffrn_orient_matrix_UB_33      0.0171007000
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            142750
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.527
_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    1.889
_exptl_crystal_description       prism
_exptl_crystal_F_000             2058
_exptl_crystal_size_max          0.4582
_exptl_crystal_size_mid          0.3472
_exptl_crystal_size_min          0.1738
_refine_diff_density_max         5.172
_refine_diff_density_min         -3.008
_refine_diff_density_rms         0.467
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         19405
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1915
_refine_ls_R_factor_gt           0.1884
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+365.8219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4307
_refine_ls_wR_factor_ref         0.4318
_reflns_number_gt                18328
_reflns_number_total             19405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202269x_si_002_7.cif
_cod_data_source_block           Compound_3_120K
_cod_original_cell_volume        3575.99(10)
_cod_database_code               4328039