Structural phase transition in the β′′-(BEDT-TTF)4H3O[Fe(C2O4)3]·G crystals (where G is a guest solvent molecule)
Zorina, Leokadiya V.; Khasanov, Salavat S.; Simonov, Sergey V.; Shibaeva, Rimma P.; Bulanchuk, Pavlo O.; Zverev, Vladimir N.; Canadell, Enric; Prokhorova, Tatiana G.; Yagubskii, Eduard B.; CrystEngComm 14 (2012) 460–; doi:10.1039/c1ce05878a

data_7207062
_publ_section_title
;
 Structural phase transition in the
 \b&#x2032;&#x2032;-(BEDT-TTF)4H3O[Fe(C2O4)3]&#x00B7;G crystals (where G
 is a guest solvent molecule)
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              460
_journal_paper_doi               10.1039/c1ce05878a
_journal_volume                  14
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'4(C10 H8 S8), C6 Fe O12, 0.35(C7 H5 N), 0.65(C6 H5 Cl), H3 O'
_chemical_formula_sum            'C52.35 H40 Cl0.65 Fe N0.35 O13 S32'
_chemical_formula_weight         1986.76
_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
;
CrysAlis RED (Oxford Diffraction Ltd.),
SHELXL-97 and WinGX routine-INITIALISE
;
_cell_angle_alpha                88.619(2)
_cell_angle_beta                 86.651(2)
_cell_angle_gamma                62.748(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2649(3)
_cell_length_b                   11.1956(3)
_cell_length_c                   35.1514(10)
_cell_measurement_reflns_used    22669
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      33.1050
_cell_measurement_theta_min      2.5499
_cell_volume                     3585.1(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 10.4752
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0428
_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       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            45485
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         32.99
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2019
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.201
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         23141
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+4.7785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                19179
_reflns_number_total             23141
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1ce05878a.txt
_cod_data_source_block
beta''-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.35(CB)0.65-150K
_cod_database_code               7207062