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_7207061
_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
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90.00
_cell_angle_beta                 92.915(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2763(6)
_cell_length_b                   20.0670(10)
_cell_length_c                   35.369(2)
_cell_measurement_radiation      CuK\a
_cell_measurement_reflns_used    8138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9421
_cell_measurement_theta_min      3.7509
_cell_volume                     7284.2(7)
_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
'Ortep-3 for Windows (Farrugia, 1997), 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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            50869
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         31.68
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Scale3AbsPack program of CrysAlisPro software'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4038
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         11242
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+11.7459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                8874
_reflns_number_total             11242
_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-(X)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7207061