#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/13/4001338.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_4001338
loop_
_publ_author_name
'Ota, Akira'
'Ouahab, Lahcène'
'Golhen, Stéphane'
'Yoshida, Yukihiro'
'Maesato, Mitsuhiko'
'Saito, Gunzi'
'Świetlik, Roman'
_publ_section_title
;
 Phase Transition from Mott Insulating Phase into the Charge Ordering
 Phase with Molecular Deformation in Charge-Transfer Salts
 κ-(ET)4[M(CN)6][N(C2H5)4]·2H2O (M = CoIIIand FeIII)
;
_journal_issue                   10
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2455
_journal_paper_doi               10.1021/cm063036k
_journal_volume                  19
_journal_year                    2007
_chemical_formula_sum            'C54 H56 Co N7 O2 S32'
_chemical_formula_weight         1919.19
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 91.960(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2760(2)
_cell_length_b                   8.917(1)
_cell_length_c                   38.176(6)
_cell_measurement_temperature    295
_cell_volume                     3836.3(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect  (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            39401
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.141
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1968
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1088P)²+3.4394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1780
_reflns_number_gt                6382
_reflns_number_total             9158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm063036ksi20070302_073935.cif
_cod_data_source_block           1-295K
_cod_original_cell_volume        3836(3)
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               4001338
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
C1 C 0.5650(7) 0.4584(7) 1.14420(14) 0.096(2) Uani 1 1 d .
H1A H 0.5740 0.5579 1.1542 0.115 Uiso 1 1 calc R
H1B H 0.5083 0.4059 1.1583 0.115 Uiso 1 1 calc R
C2 C 0.6699(7) 0.3885(10) 1.14963(17) 0.131(4) Uani 1 1 d .
H2A H 0.6762 0.3679 1.1746 0.158 Uiso 1 1 calc R
H2B H 0.7302 0.4628 1.1450 0.158 Uiso 1 1 calc R
C3 C 0.5631(3) 0.3454(4) 1.07754(9) 0.0390(8) Uani 1 1 d .
C4 C 0.6470(3) 0.2455(5) 1.08736(10) 0.0425(8) Uani 1 1 d .
C5 C 0.6034(3) 0.1918(4) 1.02223(9) 0.0409(8) Uani 1 1 d .
C6 C 0.6018(4) 0.1349(4) 0.98887(10) 0.0432(8) Uani 1 1 d .
C7 C 0.5632(4) 0.0930(4) 0.92286(9) 0.0423(8) Uani 1 1 d .
C8 C 0.6481(4) -0.0066(5) 0.93245(10) 0.0461(9) Uani 1 1 d .
C9 C 0.6002(9) 0.0244(8) 0.85463(15) 0.128(3) Uani 1 1 d .
H9A H 0.5537 -0.0145 0.8348 0.153 Uiso 1 1 calc R
H9B H 0.6520 0.1005 0.8453 0.153 Uiso 1 1 calc R
C10 C 0.6705(8) -0.0869(13) 0.86547(15) 0.151(4) Uani 1 1 d .
H10A H 0.7420 -0.0745 0.8524 0.181 Uiso 1 1 calc R
H10B H 0.6325 -0.1768 0.8562 0.181 Uiso 1 1 calc R
C11 C 0.8901(7) 0.7967(8) 1.11535(14) 0.103(2) Uani 1 1 d .
H11A H 0.8461 0.8338 1.1350 0.124 Uiso 1 1 calc R
H11B H 0.9399 0.7157 1.1243 0.124 Uiso 1 1 calc R
C12 C 0.9652(6) 0.9107(12) 1.10563(14) 0.126(3) Uani 1 1 d .
H12A H 1.0242 0.9205 1.1246 0.151 Uiso 1 1 calc R
H12B H 0.9184 1.0019 1.1057 0.151 Uiso 1 1 calc R
C13 C 0.8625(4) 0.7144(5) 1.04681(10) 0.0453(9) Uani 1 1 d .
C14 C 0.9618(4) 0.7935(5) 1.04038(10) 0.0513(10) Uani 1 1 d .
C15 C 0.9149(4) 0.6453(4) 0.98364(9) 0.0424(8) Uani 1 1 d .
C16 C 0.9114(3) 0.5971(4) 0.94949(9) 0.0394(8) Uani 1 1 d .
C17 C 0.8425(3) 0.5036(4) 0.88846(9) 0.0405(8) Uani 1 1 d .
C18 C 0.9413(4) 0.5847(4) 0.88319(9) 0.0408(8) Uani 1 1 d .
C19 C 0.8381(5) 0.4340(7) 0.81888(13) 0.0776(17) Uani 1 1 d .
H19A H 0.9005 0.3592 0.8202 0.093 Uiso 1 1 calc R
H19B H 0.7875 0.4101 0.7986 0.093 Uiso 1 1 calc R
C20 C 0.8926(5) 0.5778(7) 0.81273(12) 0.0765(16) Uani 1 1 d .
H20A H 0.8314 0.6542 0.8125 0.092 Uiso 1 1 calc R
H20B H 0.9262 0.5765 0.7897 0.092 Uiso 1 1 calc R
C21 C 0.1501(6) -0.1317(8) 0.78335(17) 0.096(2) Uani 1 1 d .
H21A H 0.0772 -0.1870 0.7842 0.144 Uiso 1 1 calc R
H21B H 0.1645 -0.0810 0.8053 0.144 Uiso 1 1 calc R
H21C H 0.2143 -0.1995 0.7792 0.144 Uiso 1 1 calc R
C22 C 0.1412(4) -0.0188(6) 0.75432(14) 0.0652(13) Uani 1 1 d .
H22A H 0.1240 -0.0714 0.7325 0.078 Uiso 1 1 calc R
H22B H 0.0746 0.0470 0.7585 0.078 Uiso 1 1 calc R
C23 C 0.2263(5) 0.1735(6) 0.71836(12) 0.0639(12) Uani 1 1 d .
H23A H 0.1534 0.2285 0.7217 0.077 Uiso 1 1 calc R
H23B H 0.2131 0.1089 0.6982 0.077 Uiso 1 1 calc R
C24 C 0.3221(6) 0.2843(7) 0.71003(16) 0.0937(19) Uani 1 1 d .
H24A H 0.2982 0.3410 0.6896 0.141 Uiso 1 1 calc R
H24B H 0.3943 0.2315 0.7057 0.141 Uiso 1 1 calc R
H24C H 0.3349 0.3512 0.7295 0.141 Uiso 1 1 calc R
C25 C 0.6529(4) -0.1191(4) 0.76968(10) 0.0418(8) Uani 1 1 d .
C26 C 0.8482(4) 0.0362(4) 0.79168(10) 0.0451(9) Uani 1 1 d .
C27 C 0.8513(3) 0.1817(4) 0.73116(11) 0.0447(9) Uani 1 1 d .
N1 N 0.2500 0.0760(5) 0.7500 0.0423(10) Uani 1 2 d S
N2 N 0.5956(4) -0.2079(4) 0.78209(10) 0.0612(10) Uani 1 1 d .
N3 N 0.9081(4) 0.0414(5) 0.81616(10) 0.0713(12) Uani 1 1 d .
N4 N 0.9132(3) 0.2685(5) 0.71991(12) 0.0645(11) Uani 1 1 d .
O1 O 0.0522(3) 0.5370(4) 0.72874(11) 0.0771(10) Uani 1 1 d .
S1 S 0.49626(11) 0.48254(13) 1.10237(3) 0.0556(3) Uani 1 1 d .
S2 S 0.71544(12) 0.22263(15) 1.12867(3) 0.0653(3) Uani 1 1 d .
S3 S 0.51168(10) 0.33869(12) 1.03413(2) 0.0479(3) Uani 1 1 d .
S4 S 0.69681(10) 0.12283(13) 1.05535(3) 0.0505(3) Uani 1 1 d .
S5 S 0.50867(11) 0.20629(12) 0.95608(2) 0.0508(3) Uani 1 1 d .
S6 S 0.69583(10) -0.00837(13) 0.97640(3) 0.0520(3) Uani 1 1 d .
S7 S 0.49805(12) 0.12152(14) 0.88149(3) 0.0579(3) Uani 1 1 d .
S8 S 0.71966(13) -0.13539(15) 0.90624(3) 0.0706(4) Uani 1 1 d .
S9 S 0.78348(12) 0.71439(16) 1.08490(3) 0.0648(3) Uani 1 1 d .
S10 S 1.04117(17) 0.91429(19) 1.06792(4) 0.0905(5) Uani 1 1 d .
S11 S 0.81030(9) 0.59241(14) 1.01389(3) 0.0513(3) Uani 1 1 d .
S12 S 1.02570(10) 0.76449(13) 0.99990(3) 0.0525(3) Uani 1 1 d .
S13 S 0.80239(9) 0.47916(13) 0.93208(3) 0.0493(3) Uani 1 1 d .
S14 S 1.01728(9) 0.65419(12) 0.92033(2) 0.0453(2) Uani 1 1 d .
S15 S 0.75182(11) 0.41490(17) 0.85697(3) 0.0657(4) Uani 1 1 d .
S16 S 1.00530(13) 0.6289(2) 0.84384(3) 0.0797(5) Uani 1 1 d .
Co1 Co 0.7500 0.03245(7) 0.7500 0.03516(17) Uani 1 2 d S
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'
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'
Co Co 0.3494 0.9721 '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
C2 C1 S1 123.5(5) . .
C1 C2 S2 125.8(5) . .
C4 C3 S1 129.0(3) . .
C4 C3 S3 116.9(3) . .
S1 C3 S3 114.1(2) . .
C3 C4 S2 128.0(3) . .
C3 C4 S4 117.4(3) . .
S2 C4 S4 114.6(2) . .
C6 C5 S4 122.4(3) . .
C6 C5 S3 122.2(3) . .
S4 C5 S3 115.4(2) . .
C5 C6 S5 121.7(3) . .
C5 C6 S6 122.6(3) . .
S5 C6 S6 115.7(2) . .
C8 C7 S7 128.1(3) . .
C8 C7 S5 116.6(3) . .
S7 C7 S5 115.3(2) . .
C7 C8 S6 117.4(3) . .
C7 C8 S8 128.2(3) . .
S6 C8 S8 114.4(2) . .
C10 C9 S7 124.9(5) . .
C9 C10 S8 130.7(5) . .
C12 C11 S9 121.9(4) . .
C11 C12 S10 124.9(6) . .
C14 C13 S9 127.2(3) . .
C14 C13 S11 117.0(3) . .
S9 C13 S11 115.7(2) . .
C13 C14 S10 128.9(3) . .
C13 C14 S12 116.9(3) . .
S10 C14 S12 114.1(2) . .
C16 C15 S12 121.9(3) . .
C16 C15 S11 123.1(3) . .
S12 C15 S11 115.0(2) . .
C15 C16 S14 121.3(3) . .
C15 C16 S13 123.5(3) . .
S14 C16 S13 115.2(2) . .
C18 C17 S15 127.5(3) . .
C18 C17 S13 116.7(3) . .
S15 C17 S13 115.8(2) . .
C17 C18 S14 117.0(3) . .
C17 C18 S16 128.4(3) . .
S14 C18 S16 114.5(2) . .
C20 C19 S15 117.6(4) . .
C19 C20 S16 114.8(4) . .
N1 C22 C21 115.1(4) . .
N1 C23 C24 116.1(4) . .
N2 C25 Co1 178.5(4) . .
N3 C26 Co1 178.3(4) . .
N4 C27 Co1 178.7(4) . .
C23 N1 C23 109.4(5) 2_556 .
C23 N1 C22 111.1(3) 2_556 .
C23 N1 C22 106.8(3) . .
C23 N1 C22 106.8(3) 2_556 2_556
C23 N1 C22 111.1(3) . 2_556
C22 N1 C22 111.6(5) . 2_556
C3 S1 C1 102.9(2) . .
C4 S2 C2 100.7(2) . .
C5 S3 C3 95.33(18) . .
C5 S4 C4 94.97(18) . .
C6 S5 C7 95.31(18) . .
C6 S6 C8 94.93(19) . .
C7 S7 C9 100.9(3) . .
C10 S8 C8 102.5(3) . .
C13 S9 C11 101.0(3) . .
C12 S10 C14 103.7(3) . .
C15 S11 C13 95.10(19) . .
C15 S12 C14 95.36(19) . .
C16 S13 C17 94.95(18) . .
C16 S14 C18 95.01(18) . .
C17 S15 C19 101.3(2) . .
C18 S16 C20 102.2(2) . .
C25 Co1 C25 89.9(2) . 2_656
C25 Co1 C27 178.22(16) . .
C25 Co1 C27 89.22(17) 2_656 .
C25 Co1 C27 89.22(17) . 2_656
C25 Co1 C27 178.22(16) 2_656 2_656
C27 Co1 C27 91.7(2) . 2_656
C25 Co1 C26 90.92(16) . 2_656
C25 Co1 C26 90.50(17) 2_656 2_656
C27 Co1 C26 90.65(17) . 2_656
C27 Co1 C26 87.95(17) 2_656 2_656
C25 Co1 C26 90.50(17) . .
C25 Co1 C26 90.92(16) 2_656 .
C27 Co1 C26 87.95(17) . .
C27 Co1 C26 90.65(17) 2_656 .
C26 Co1 C26 178.0(2) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.347(8) .
C1 S1 1.764(5) .
C2 S2 1.766(7) .
C3 C4 1.343(5) .
C3 S1 1.735(4) .
C3 S3 1.738(4) .
C4 S2 1.744(4) .
C4 S4 1.747(4) .
C5 C6 1.370(5) .
C5 S4 1.731(4) .
C5 S3 1.739(4) .
C6 S5 1.728(4) .
C6 S6 1.737(4) .
C7 C8 1.348(6) .
C7 S7 1.737(4) .
C7 S5 1.749(4) .
C8 S6 1.745(4) .
C8 S8 1.739(4) .
C9 C10 1.327(10) .
C9 S7 1.792(6) .
C10 S8 1.690(7) .
C11 C12 1.382(10) .
C11 S9 1.800(7) .
C12 S10 1.701(6) .
C13 C14 1.353(6) .
C13 S9 1.732(4) .
C13 S11 1.749(4) .
C14 S10 1.732(4) .
C14 S12 1.747(4) .
C15 C16 1.372(5) .
C15 S12 1.739(4) .
C15 S11 1.744(4) .
C16 S14 1.736(4) .
C16 S13 1.733(4) .
C17 C18 1.349(5) .
C17 S15 1.741(4) .
C17 S13 1.754(4) .
C18 S14 1.745(4) .
C18 S16 1.734(4) .
C19 C20 1.444(8) .
C19 S15 1.786(5) .
C20 S16 1.769(5) .
C21 C22 1.498(7) .
C22 N1 1.504(5) .
C23 N1 1.505(5) .
C23 C24 1.506(8) .
C25 N2 1.136(5) .
C25 Co1 1.909(4) .
C26 N3 1.135(5) .
C26 Co1 1.908(4) .
C27 N4 1.136(5) .
C27 Co1 1.910(4) .
N1 C23 1.505(5) 2_556
N1 C22 1.504(5) 2_556
Co1 C25 1.909(4) 2_656
Co1 C27 1.910(4) 2_656
Co1 C26 1.908(4) 2_656
