Synthesis, crystal structure, and characterization of charge-transfer salt: (BEDT-TTF)5[Fe(C2O4)3]·(H2O)2·CH2Cl2 (BEDT-TTF = bis(ethylenedithio)tetrathiafulvalene)
Zhang, Bin; Zhang, Yan; Liu, Fen; Guo, Yanjun; CrystEngComm 11 (2009) 2523–; doi:10.1039/b910483f

data_7201408
_publ_section_title
;
 Synthesis, crystal structure, and characterization of charge-transfer
 salt: (BEDT-TTF)5[Fe(C2O4)3]&#x00B7;(H2O)2&#x00B7;CH2Cl2 (BEDT-TTF =
 bis(ethylenedithio)tetrathiafulvalene)
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2523
_journal_paper_doi               10.1039/b910483f
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C57 H46 Cl2 Fe O14 S40'
_chemical_formula_weight         2364.09
_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                89.3682(4)
_cell_angle_beta                 85.1561(5)
_cell_angle_gamma                70.3330(7)
_cell_formula_units_Z            2
_cell_length_a                   11.14800(10)
_cell_length_b                   11.55000(10)
_cell_length_c                   35.3120(6)
_cell_measurement_reflns_used    36311
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.395
_cell_volume                     4265.49(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.1132
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            50118
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00011(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         14778
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                7375
_reflns_number_total             14778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910483f.txt
_cod_data_source_block           CCDC727213-290K
_cod_database_code               7201408