#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:19:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179241 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/61/4316171.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4316171
loop_
_publ_author_name
'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'
_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         C10H2KO8S4
_chemical_formula_sum            'C10 H2 K O8 S4'
_chemical_formula_weight         417.46
_chemical_name_common            K(TTF-TC+)H2
_chemical_name_systematic
;
potassium(tetrathiafulvalenedicarboxylic)dicarboxylate
;
_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   fourier
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.659(3)
_cell_angle_beta                 86.035(3)
_cell_angle_gamma                86.061(3)
_cell_formula_units_Z            1
_cell_length_a                   5.1094(7)
_cell_length_b                   6.0771(9)
_cell_length_c                   11.0989(17)
_cell_measurement_reflns_used    1063
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.84
_cell_volume                     342.99(9)
_computing_cell_refinement       SAINT
_computing_data_collection       SAINT
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2593
_diffrn_reflns_theta_full        29.56
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.7463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             209
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0422
_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/[σ²(Fo²)+(0.0609P)²+0.1068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                1426
_reflns_number_total             1862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100950n_si_001_5.cif
_cod_data_source_block           MIL135K
_cod_database_code               4316171
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.5000 0.0000 0.5000 0.0407(3) Uani 1 2 d S . .
S1 S -0.35056(13) 0.31282(11) 0.84041(6) 0.02947(19) Uani 1 1 d . . .
S2 S -0.20654(13) 0.72840(10) 0.94122(6) 0.02708(18) Uani 1 1 d . . .
C1 C -0.0976(5) 0.4417(4) 0.7636(2) 0.0267(5) Uani 1 1 d . . .
C2 C -0.0284(5) 0.6333(4) 0.8111(2) 0.0252(5) Uani 1 1 d . . .
C3 C -0.4039(5) 0.5085(4) 0.9524(2) 0.0246(5) Uani 1 1 d . . .
C4 C 0.0086(6) 0.3188(5) 0.6502(3) 0.0353(6) Uani 1 1 d . . .
O1 O 0.2158(5) 0.3836(4) 0.5933(2) 0.0467(6) Uani 1 1 d . . .
O2 O -0.1105(5) 0.1618(4) 0.6210(2) 0.0514(6) Uani 1 1 d . . .
C5 C 0.1862(5) 0.7838(5) 0.7714(3) 0.0320(6) Uani 1 1 d . . .
O3 O 0.3391(4) 0.7250(4) 0.6787(2) 0.0437(5) Uani 1 1 d . . .
H3 H 0.299(8) 0.559(8) 0.640(4) 0.066 Uiso 1 1 d . . .
O4 O 0.2031(5) 0.9471(4) 0.8326(2) 0.0464(6) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 K1 O3 180.0 2_666 1_545 ?
O3 K1 O2 84.51(8) 2_666 1_655 ?
O3 K1 O2 95.49(8) 1_545 1_655 ?
O3 K1 O2 95.49(8) 2_666 2_556 ?
O3 K1 O2 84.51(8) 1_545 2_556 ?
O2 K1 O2 180.0 1_655 2_556 ?
O3 K1 O1 96.41(7) 2_666 2_656 ?
O3 K1 O1 83.59(7) 1_545 2_656 ?
O2 K1 O1 97.84(7) 1_655 2_656 ?
O2 K1 O1 82.16(7) 2_556 2_656 ?
O3 K1 O1 83.59(7) 2_666 . ?
O3 K1 O1 96.41(7) 1_545 . ?
O2 K1 O1 82.16(7) 1_655 . ?
O2 K1 O1 97.84(7) 2_556 . ?
O1 K1 O1 180.0 2_656 . ?
O3 K1 O2 68.40(7) 2_666 2_656 ?
O3 K1 O2 111.60(7) 1_545 2_656 ?
O2 K1 O2 67.01(7) 1_655 2_656 ?
O2 K1 O2 112.99(7) 2_556 2_656 ?
O1 K1 O2 40.53(7) 2_656 2_656 ?
O1 K1 O2 139.47(7) . 2_656 ?
O3 K1 O2 111.60(7) 2_666 . ?
O3 K1 O2 68.40(7) 1_545 . ?
O2 K1 O2 112.99(7) 1_655 . ?
O2 K1 O2 67.01(7) 2_556 . ?
O1 K1 O2 139.47(7) 2_656 . ?
O1 K1 O2 40.53(7) . . ?
O2 K1 O2 180.0 2_656 . ?
O3 K1 C4 78.25(7) 2_666 2_656 ?
O3 K1 C4 101.75(7) 1_545 2_656 ?
O2 K1 C4 85.45(7) 1_655 2_656 ?
O2 K1 C4 94.55(7) 2_556 2_656 ?
O1 K1 C4 21.11(7) 2_656 2_656 ?
O1 K1 C4 158.89(7) . 2_656 ?
O2 K1 C4 20.71(6) 2_656 2_656 ?
O2 K1 C4 159.29(6) . 2_656 ?
O3 K1 C4 101.75(7) 2_666 . ?
O3 K1 C4 78.25(7) 1_545 . ?
O2 K1 C4 94.55(7) 1_655 . ?
O2 K1 C4 85.45(7) 2_556 . ?
O1 K1 C4 158.89(7) 2_656 . ?
O1 K1 C4 21.11(7) . . ?
O2 K1 C4 159.29(6) 2_656 . ?
O2 K1 C4 20.71(6) . . ?
C4 K1 C4 180.0 2_656 . ?
C3 S1 C1 95.06(12) . . ?
C3 S2 C2 94.76(12) . . ?
C2 C1 C4 130.5(3) . . ?
C2 C1 S1 117.0(2) . . ?
C4 C1 S1 112.6(2) . . ?
C1 C2 C5 131.3(2) . . ?
C1 C2 S2 116.9(2) . . ?
C5 C2 S2 111.80(19) . . ?
C3 C3 S1 122.2(3) 2_467 . ?
C3 C3 S2 121.5(3) 2_467 . ?
S1 C3 S2 116.29(15) . . ?
O2 C4 O1 124.9(3) . . ?
O2 C4 C1 116.8(3) . . ?
O1 C4 C1 118.3(3) . . ?
O2 C4 K1 78.89(18) . . ?
O1 C4 K1 52.66(15) . . ?
C1 C4 K1 149.36(18) . . ?
C4 O1 K1 106.23(19) . . ?
C4 O1 H3 113.0(19) . . ?
K1 O1 H3 130.0(19) . . ?
C4 O2 K1 149.6(2) . 1_455 ?
C4 O2 K1 80.40(19) . . ?
K1 O2 K1 112.99(7) 1_455 . ?
O4 C5 O3 125.6(3) . . ?
O4 C5 C2 116.8(3) . . ?
O3 C5 C2 117.5(3) . . ?
C5 O3 K1 124.77(19) . 1_565 ?
C5 O3 H3 114(2) . . ?
K1 O3 H3 110(2) 1_565 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O3 2.707(2) 2_666 ?
K1 O3 2.707(2) 1_545 ?
K1 O2 2.717(2) 1_655 ?
K1 O2 2.717(2) 2_556 ?
K1 O1 2.823(2) 2_656 ?
K1 O1 2.823(2) . ?
K1 O2 3.394(3) 2_656 ?
K1 O2 3.394(3) . ?
K1 C4 3.410(3) 2_656 ?
K1 C4 3.410(3) . ?
S1 C3 1.720(3) . ?
S1 C1 1.729(3) . ?
S2 C3 1.728(3) . ?
S2 C2 1.734(3) . ?
C1 C2 1.360(4) . ?
C1 C4 1.516(4) . ?
C2 C5 1.516(4) . ?
C3 C3 1.401(5) 2_467 ?
C4 O2 1.223(4) . ?
C4 O1 1.279(4) . ?
O1 H3 1.30(5) . ?
O2 K1 2.717(2) 1_455 ?
C5 O4 1.217(4) . ?
C5 O3 1.285(4) . ?
O3 K1 2.707(2) 1_565 ?
O3 H3 1.14(5) . ?
