3-D Coordination Polymers Based on the Tetrathiafulvalenetetracarboxylate (TTF-TC) Derivative: Synthesis, Characterization, and Oxidation Issues
Thi Le Anh Nguyen; Rezan Demir-Cakan; Thomas Devic; Mathieu Morcrette; Tim Ahnfeldt; Pascale Auban-Senzier; Norbert Stock; Anne-Marie Goncalves; Yaroslav Filinchuk; Jean-Marie Tarascon; Gérard Férey; Inorganic Chemistry 49 (2010) 7135–7143; doi:10.1021/ic100950n

data_4316167
_publ_section_title
;
 3-D Coordination Polymers Based on the Tetrathiafulvalenetetracarboxylate
 (TTF-TC) Derivative: Synthesis, Characterization, and Oxidation Issues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7135
_journal_page_last               7143
_journal_paper_doi               10.1021/ic100950n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         C10H2S4O8K2
_chemical_formula_sum            'C10 H2 K2 O8 S4'
_chemical_formula_weight         456.56
_chemical_name_common            K2(TTF-TC)H2
_chemical_name_systematic
;
dipotassium(tetrathiafulvalenedicarboxylic)dicarboxylate
monoclinic polymorph
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.595(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8268(6)
_cell_length_b                   3.9607(3)
_cell_length_c                   22.6386(10)
_cell_measurement_reflns_used    3037
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      3.6
_cell_volume                     790.64(9)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_collection       'MAR345 control software (MAR, 2002)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(1)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'MAR345 Image plate'
_diffrn_measurement_method       \f-scan
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_source         'Beamline BM1A, SNBL, ESRF, Grenoble, France'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.699765
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7876
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         3.60
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9126
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK (Oxford Diffraction, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.9494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                1467
_reflns_number_total             1647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100950n_si_001_1.cif
_cod_data_source_block           MIL132K
_cod_database_code               4316167