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_4328037
_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 F), (H3 O)'
_chemical_formula_sum            'C52 H40 F Fe O13 S32'
_chemical_formula_weight         1973.61
_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                89.149(2)
_cell_angle_beta                 86.762(2)
_cell_angle_gamma                62.578(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2595(3)
_cell_length_b                   11.1403(3)
_cell_length_c                   34.9516(9)
_cell_measurement_reflns_used    21638
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.3847
_cell_measurement_theta_min      2.2340
_cell_volume                     3539.96(19)
_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 0.995
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
  1 omega   51.00   78.20   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613   77.0000   30.0000 34

  2 omega   45.00   97.00   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613   77.0000  150.0000 65

  3 omega   36.00   96.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613  179.0000  150.0000 76

  4 omega   -4.00   88.00   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613 -124.0000  160.0000 115

  5 omega   34.00   90.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613   77.0000  -60.0000 71

  6 omega    8.00   89.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613   77.0000    0.0000 102

  7 omega   14.00   93.20   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613   37.0000  -90.0000 99

  8 omega  -76.00  -21.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.3363  124.0000 -160.0000 68

  9 omega    3.00   41.40   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.3363   77.0000  -90.0000 48

 10 omega   -5.00   20.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613   77.0000  -30.0000 32

 11 omega   34.00  106.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613  179.0000  -60.0000 91

 12 omega   -4.00  100.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4613   37.0000  120.0000 131

 13 omega -113.00  -53.00   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.3363  179.0000 -150.0000 75

 14 omega    1.00   30.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.3363 -130.0000 -136.0000 37

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0109951000
_diffrn_orient_matrix_UB_12      0.0123477000
_diffrn_orient_matrix_UB_13      0.0190106000
_diffrn_orient_matrix_UB_21      0.0530592000
_diffrn_orient_matrix_UB_22      0.0204741000
_diffrn_orient_matrix_UB_23      -0.0069824000
_diffrn_orient_matrix_UB_31      -0.0560537000
_diffrn_orient_matrix_UB_32      0.0676353000
_diffrn_orient_matrix_UB_33      -0.0016280000
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            68228
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.46
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.688
_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    1.852
_exptl_crystal_description       prism
_exptl_crystal_F_000             2006
_exptl_crystal_size_max          0.5003
_exptl_crystal_size_mid          0.2036
_exptl_crystal_size_min          0.0758
_refine_diff_density_max         5.652
_refine_diff_density_min         -4.207
_refine_diff_density_rms         0.363
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         23574
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1955
_refine_ls_R_factor_gt           0.1815
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+256.6391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3770
_refine_ls_wR_factor_ref         0.3823
_reflns_number_gt                19487
_reflns_number_total             23574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202269x_si_002_5.cif
_cod_data_source_block           Compound_1_120K
_cod_database_code               4328037