#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/78/4337847.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_4337847
loop_
_publ_author_name
'Huang, Yu-De'
'Huo, Peng'
'Shao, Ming-Yan'
'Yin, Jing-Xue'
'Shen, Wei-Chun'
'Zhu, Qin-Yu'
'Dai, Jie'
_publ_section_title
;
 A New Type of Charge-Transfer Salts Based on
 Tetrathiafulvalene-Tetracarboxylate Coordination Polymers and Methyl
 Viologen.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3480
_journal_paper_doi               10.1021/ic402926n
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C10 H4 Mn O10 S4, C12 H14 N2, 2(O)'
_chemical_formula_sum            'C22 H22 Mn N2 O12 S4'
_chemical_formula_weight         689.64
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.034(3)
_cell_length_b                   11.188(3)
_cell_length_c                   25.730(5)
_cell_measurement_reflns_used    3852
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2596.3(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_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  0.1179
_diffrn_reflns_av_sigmaI/netI    0.1602
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11581
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.7147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.0043(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0715
_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)+(0.0010P)²+15.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                1375
_reflns_number_total             2980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402926n_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4337845--4337848.cif.'
_cod_original_sg_symbol_Hall     '-C 2yc   '
_cod_original_sg_symbol_H-M      'C 2/c  '
_cod_database_code               4337847
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Mn1 Mn 0.5000 0.26861(13) 0.2500 0.0304(4) Uani 1 2 d S
S1 S 0.81781(16) 0.18088(17) 0.07746(6) 0.0341(5) Uani 1 1 d .
S2 S 0.54813(17) 0.30711(16) 0.03623(6) 0.0334(5) Uani 1 1 d .
O1 O 0.8303(5) 0.1012(5) 0.17979(17) 0.0519(14) Uani 1 1 d .
O2 O 0.7080(4) 0.2523(4) 0.21461(15) 0.0344(11) Uani 1 1 d .
O3 O 0.4016(4) 0.2760(4) 0.17405(15) 0.0359(12) Uani 1 1 d .
O4 O 0.3207(5) 0.3465(5) 0.09715(17) 0.0478(14) Uani 1 1 d .
O5 O 0.5000 0.4658(6) 0.2500 0.0392(16) Uani 1 2 d SD
O6 O 0.5000 0.0706(7) 0.2500 0.0514(19) Uani 1 2 d SD
O7 O 0.6190(5) -0.1317(4) 0.20385(18) 0.0496(13) Uiso 1 1 d .
N1 N 0.2787(5) 0.0326(5) 0.10631(19) 0.0339(13) Uani 1 1 d .
C1 C 0.6849(6) 0.2218(6) 0.1226(2) 0.0269(14) Uani 1 1 d .
C2 C 0.5604(7) 0.2735(6) 0.1036(2) 0.0316(15) Uani 1 1 d .
C3 C 0.7262(6) 0.2483(6) 0.0236(2) 0.0281(15) Uani 1 1 d .
C4 C 0.7428(7) 0.1871(6) 0.1770(2) 0.0332(15) Uani 1 1 d .
C5 C 0.4166(6) 0.3031(6) 0.1279(2) 0.0286(15) Uani 1 1 d .
C6 C 0.2282(7) 0.0729(6) 0.0589(2) 0.0382(17) Uani 1 1 d .
H6 H 0.1355 0.1090 0.0549 0.046 Uiso 1 1 calc R
C7 C 0.3125(6) 0.0605(6) 0.0176(2) 0.0346(16) Uani 1 1 d .
H7 H 0.2765 0.0882 -0.0148 0.042 Uiso 1 1 calc R
C8 C 0.4518(6) 0.0073(5) 0.0223(2) 0.0278(15) Uani 1 1 d .
C9 C 0.4980(7) -0.0349(6) 0.0725(2) 0.0348(16) Uani 1 1 d .
H9 H 0.5894 -0.0727 0.0776 0.042 Uiso 1 1 calc R
C10 C 0.4119(7) -0.0212(6) 0.1132(3) 0.0402(17) Uani 1 1 d .
H10 H 0.4443 -0.0489 0.1460 0.048 Uiso 1 1 calc R
C11 C 0.1851(7) 0.0470(7) 0.1513(2) 0.0434(18) Uani 1 1 d .
H11A H 0.2018 -0.0189 0.1748 0.065 Uiso 1 1 calc R
H11B H 0.0826 0.0488 0.1393 0.065 Uiso 1 1 calc R
H11C H 0.2103 0.1203 0.1690 0.065 Uiso 1 1 calc R
H6A H 0.561(6) 0.021(5) 0.238(3) 0.05(2) Uiso 1 1 d D
H5A H 0.568(6) 0.506(6) 0.266(3) 0.07(3) Uiso 1 1 d 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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
O3 Mn1 O3 175.5(3) . 2_655
O3 Mn1 O2 86.70(14) . .
O3 Mn1 O2 93.68(14) 2_655 .
O3 Mn1 O2 93.68(14) . 2_655
O3 Mn1 O2 86.70(14) 2_655 2_655
O2 Mn1 O2 170.2(3) . 2_655
O3 Mn1 O5 87.75(13) . .
O3 Mn1 O5 87.75(13) 2_655 .
O2 Mn1 O5 94.89(13) . .
O2 Mn1 O5 94.89(13) 2_655 .
O3 Mn1 O6 92.25(13) . .
O3 Mn1 O6 92.25(13) 2_655 .
O2 Mn1 O6 85.11(13) . .
O2 Mn1 O6 85.11(13) 2_655 .
O5 Mn1 O6 180.000(1) . .
C3 S1 C1 95.8(3) . .
C2 S2 C3 95.4(3) . .
C4 O2 Mn1 129.5(4) . .
C5 O3 Mn1 146.7(4) . .
Mn1 O5 H5A 122(6) . .
Mn1 O6 H6A 130(5) . .
C10 N1 C6 121.3(5) . .
C10 N1 C11 119.4(5) . .
C6 N1 C11 119.3(5) . .
C2 C1 C4 133.6(5) . .
C2 C1 S1 117.3(4) . .
C4 C1 S1 109.1(4) . .
C1 C2 C5 132.1(6) . .
C1 C2 S2 117.1(5) . .
C5 C2 S2 110.6(4) . .
C3 C3 S1 125.6(6) 7_655 .
C3 C3 S2 120.3(6) 7_655 .
S1 C3 S2 113.9(3) . .
O1 C4 O2 125.9(6) . .
O1 C4 C1 115.8(5) . .
O2 C4 C1 118.0(6) . .
O4 C5 O3 126.6(5) . .
O4 C5 C2 114.1(5) . .
O3 C5 C2 119.1(6) . .
C7 C6 N1 119.9(6) . .
C7 C6 H6 120.0 . .
N1 C6 H6 120.0 . .
C6 C7 C8 121.6(6) . .
C6 C7 H7 119.2 . .
C8 C7 H7 119.2 . .
C7 C8 C9 116.0(5) . .
C7 C8 C8 123.2(7) . 5_655
C9 C8 C8 120.8(6) . 5_655
C10 C9 C8 121.2(6) . .
C10 C9 H9 119.4 . .
C8 C9 H9 119.4 . .
C9 C10 N1 120.0(6) . .
C9 C10 H10 120.0 . .
N1 C10 H10 120.0 . .
N1 C11 H11A 109.5 . .
N1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O3 2.101(4) .
Mn1 O3 2.101(4) 2_655
Mn1 O2 2.142(4) .
Mn1 O2 2.142(4) 2_655
Mn1 O5 2.207(7) .
Mn1 O6 2.216(8) .
S1 C3 1.745(6) .
S1 C1 1.778(6) .
S2 C2 1.771(6) .
S2 C3 1.785(5) .
O1 C4 1.243(7) .
O2 C4 1.266(7) .
O3 C5 1.241(6) .
O4 C5 1.238(7) .
O5 H5A 0.85(2) .
O6 H6A 0.85(2) .
N1 C10 1.348(8) .
N1 C6 1.354(7) .
N1 C11 1.482(7) .
C1 C2 1.332(8) .
C1 C4 1.516(8) .
C2 C5 1.510(8) .
C3 C3 1.310(10) 7_655
C6 C7 1.350(8) .
C6 H6 0.9300 .
C7 C8 1.392(7) .
C7 H7 0.9300 .
C8 C9 1.416(8) .
C8 C8 1.488(11) 5_655
C9 C10 1.348(8) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
