#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/13/4001343.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_4001343
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 Fe N7 O2 S32'
_chemical_formula_weight         1916.83
_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                 90.1420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0498(6)
_cell_length_b                   8.8371(6)
_cell_length_c                   38.573(3)
_cell_measurement_temperature    106
_cell_volume                     3766.6(4)
_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      106
_diffrn_measured_fraction_theta_full 0.644
_diffrn_measured_fraction_theta_max 0.644
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            4950
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.135
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1966
_refine_diff_density_max         2.473
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.382
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.382
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.002
_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          0.2076
_refine_ls_wR_factor_ref         0.2281
_reflns_number_gt                3291
_reflns_number_total             4441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm063036ksi20070302_073935.cif
_cod_data_source_block           2-106K
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               4001343
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 0.5692(11) 0.4489(12) 1.1421(3) 0.049(3) Uani 1 1 d .
H1A H 0.5719 0.5484 1.1527 0.058 Uiso 1 1 calc R
H1B H 0.5226 0.3841 1.1574 0.058 Uiso 1 1 calc R
C2 C 0.6879(11) 0.3925(15) 1.1409(4) 0.064(4) Uani 1 1 d .
H2A H 0.7209 0.3975 1.1642 0.077 Uiso 1 1 calc R
H2B H 0.7350 0.4612 1.1267 0.077 Uiso 1 1 calc R
C3 C 0.5568(8) 0.3266(9) 1.0765(3) 0.025(2) Uani 1 1 d .
C4 C 0.6450(8) 0.2251(10) 1.0854(3) 0.031(3) Uani 1 1 d .
C5 C 0.6000(7) 0.1796(10) 1.0207(3) 0.027(2) Uani 1 1 d .
C6 C 0.6033(7) 0.1264(9) 0.9865(3) 0.023(2) Uani 1 1 d .
C7 C 0.5731(7) 0.0962(9) 0.9220(3) 0.022(2) Uani 1 1 d .
C8 C 0.6628(7) -0.0018(10) 0.9306(3) 0.025(2) Uani 1 1 d .
C9 C 0.6351(10) 0.0494(11) 0.8552(3) 0.042(3) Uani 1 1 d .
H9A H 0.6125 0.0522 0.8309 0.051 Uiso 1 1 calc R
H9B H 0.7050 0.1146 0.8582 0.051 Uiso 1 1 calc R
C10 C 0.6703(9) -0.1089(10) 0.8645(3) 0.033(3) Uani 1 1 d .
H10A H 0.7228 -0.1481 0.8465 0.040 Uiso 1 1 calc R
H10B H 0.5979 -0.1710 0.8648 0.040 Uiso 1 1 calc R
C11 C 0.8749(14) 0.7661(16) 1.1140(4) 0.088(6) Uani 1 1 d .
H11A H 0.8364 0.8238 1.1324 0.106 Uiso 1 1 calc R
H11B H 0.8996 0.6707 1.1243 0.106 Uiso 1 1 calc R
C12 C 0.9793(11) 0.8420(17) 1.1057(3) 0.069(4) Uani 1 1 d .
H12A H 1.0449 0.7693 1.1071 0.083 Uiso 1 1 calc R
H12B H 0.9934 0.9157 1.1239 0.083 Uiso 1 1 calc R
C13 C 0.8391(8) 0.7166(10) 1.0443(3) 0.023(2) Uani 1 1 d .
C14 C 0.9366(8) 0.8042(10) 1.0374(3) 0.025(2) Uani 1 1 d .
C15 C 0.9061(7) 0.6381(9) 0.9836(3) 0.021(2) Uani 1 1 d .
C16 C 0.9096(7) 0.5911(9) 0.9503(3) 0.022(2) Uani 1 1 d .
C17 C 0.8375(8) 0.5218(9) 0.8884(3) 0.021(2) Uani 1 1 d .
C18 C 0.9370(8) 0.6039(9) 0.8836(3) 0.022(2) Uani 1 1 d .
C19 C 0.8563(8) 0.4430(10) 0.8207(3) 0.033(3) Uani 1 1 d .
H19A H 0.9236 0.3783 0.8271 0.039 Uiso 1 1 calc R
H19B H 0.8188 0.4000 0.8001 0.039 Uiso 1 1 calc R
C20 C 0.9050(8) 0.6006(10) 0.8118(3) 0.029(2) Uani 1 1 d .
H20A H 0.8372 0.6674 0.8072 0.035 Uiso 1 1 calc R
H20B H 0.9529 0.5941 0.7909 0.035 Uiso 1 1 calc R
C21 C 0.1651(19) -0.130(2) 0.7831(6) 0.148(8) Uiso 1 1 d .
H21A H 0.0940 -0.1920 0.7854 0.222 Uiso 1 1 calc R
H21B H 0.1776 -0.0739 0.8041 0.222 Uiso 1 1 calc R
H21C H 0.2340 -0.1941 0.7789 0.222 Uiso 1 1 calc R
C22 C 0.143(3) 0.015(3) 0.7427(9) 0.221(13) Uiso 1 1 d .
H22A H 0.1441 -0.0351 0.7203 0.266 Uiso 1 1 calc R
H22B H 0.0722 0.0785 0.7449 0.266 Uiso 1 1 calc R
C23 C 0.225(3) 0.193(3) 0.7092(8) 0.236(14) Uiso 1 1 d .
H23A H 0.2350 0.1292 0.6890 0.283 Uiso 1 1 calc R
H23B H 0.1471 0.2435 0.7084 0.283 Uiso 1 1 calc R
C24 C 0.3260(16) 0.298(2) 0.7144(5) 0.118(6) Uiso 1 1 d .
H24A H 0.3261 0.3716 0.6961 0.176 Uiso 1 1 calc R
H24B H 0.4008 0.2428 0.7141 0.176 Uiso 1 1 calc R
H24C H 0.3172 0.3482 0.7363 0.176 Uiso 1 1 calc R
C25 C 0.6493(8) -0.0995(11) 0.7714(3) 0.027(2) Uani 1 1 d .
C26 C 0.8523(8) 0.0564(10) 0.7911(3) 0.025(2) Uani 1 1 d .
C27 C 0.8515(7) 0.2109(10) 0.7291(3) 0.028(3) Uani 1 1 d .
N1 N 0.2500 0.0905(13) 0.7500 0.036(3) Uani 1 2 d S
N2 N 0.5884(7) -0.1888(9) 0.7836(2) 0.035(2) Uani 1 1 d .
N3 N 0.9131(7) 0.0613(9) 0.8151(3) 0.034(2) Uani 1 1 d .
N4 N 0.9126(6) 0.2985(9) 0.7174(3) 0.036(2) Uani 1 1 d .
O1 O 0.0609(6) 0.5595(7) 0.7259(2) 0.042(2) Uani 1 1 d .
S1 S 0.4896(2) 0.4647(3) 1.10204(8) 0.0332(7) Uani 1 1 d .
S2 S 0.7142(3) 0.2030(3) 1.12480(9) 0.0478(9) Uani 1 1 d .
S3 S 0.5050(2) 0.3235(3) 1.03400(7) 0.0252(6) Uani 1 1 d .
S4 S 0.6962(2) 0.1079(3) 1.05200(8) 0.0303(7) Uani 1 1 d .
S5 S 0.5111(2) 0.2011(3) 0.95522(7) 0.0264(6) Uani 1 1 d .
S6 S 0.7052(2) -0.0085(3) 0.97366(8) 0.0310(7) Uani 1 1 d .
S7 S 0.5115(2) 0.1244(3) 0.88054(7) 0.0289(6) Uani 1 1 d .
S8 S 0.7447(2) -0.1276(3) 0.90462(8) 0.0400(8) Uani 1 1 d .
S9 S 0.7594(2) 0.7226(3) 1.08324(7) 0.0340(7) Uani 1 1 d .
S10 S 0.9950(2) 0.9399(3) 1.06524(8) 0.0341(7) Uani 1 1 d .
S11 S 0.80330(19) 0.5739(2) 1.01449(7) 0.0240(6) Uani 1 1 d .
S12 S 1.0174(2) 0.7626(3) 0.99948(7) 0.0257(6) Uani 1 1 d .
S13 S 0.8047(2) 0.4639(3) 0.93115(7) 0.0276(6) Uani 1 1 d .
S14 S 1.02301(19) 0.6473(3) 0.92106(7) 0.0249(6) Uani 1 1 d .
S15 S 0.7479(2) 0.4439(3) 0.85524(7) 0.0292(6) Uani 1 1 d .
S16 S 0.9965(2) 0.6822(3) 0.84583(8) 0.0425(8) Uani 1 1 d .
Fe1 Fe 0.7500 0.0548(2) 0.7500 0.0213(5) 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'
Fe Fe 0.3463 0.8444 '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 117.2(10) . .
C1 C2 S2 119.5(9) . .
C4 C3 S1 128.5(8) . .
C4 C3 S3 117.4(8) . .
S1 C3 S3 114.0(5) . .
C3 C4 S4 115.8(8) . .
C3 C4 S2 127.9(9) . .
S4 C4 S2 116.2(5) . .
C6 C5 S3 122.9(7) . .
C6 C5 S4 121.2(7) . .
S3 C5 S4 115.9(6) . .
C5 C6 S6 121.5(7) . .
C5 C6 S5 121.2(7) . .
S6 C6 S5 117.2(6) . .
C8 C7 S5 116.8(8) . .
C8 C7 S7 126.6(8) . .
S5 C7 S7 116.5(5) . .
C7 C8 S8 130.0(9) . .
C7 C8 S6 117.1(8) . .
S8 C8 S6 113.0(5) . .
C10 C9 S7 114.2(8) . .
C9 C10 S8 114.8(7) . .
C12 C11 S9 123.4(11) . .
C11 C12 S10 121.5(10) . .
C14 C13 S9 123.8(8) . .
C14 C13 S11 117.5(7) . .
S9 C13 S11 118.3(5) . .
C13 C14 S12 116.8(7) . .
C13 C14 S10 124.8(8) . .
S12 C14 S10 118.1(5) . .
C16 C15 S11 124.8(7) . .
C16 C15 S12 120.1(7) . .
S11 C15 S12 114.9(6) . .
C15 C16 S14 123.0(7) . .
C15 C16 S13 124.8(7) . .
S14 C16 S13 112.2(6) . .
C18 C17 S13 117.4(7) . .
C18 C17 S15 125.2(8) . .
S13 C17 S15 116.8(5) . .
C17 C18 S16 130.3(8) . .
C17 C18 S14 116.5(8) . .
S16 C18 S14 113.2(5) . .
C20 C19 S15 113.3(7) . .
C19 C20 S16 113.5(7) . .
N1 C22 C21 92.8(17) . .
C24 C23 N1 94.8(19) . .
N2 C25 Fe1 178.7(9) . .
N3 C26 Fe1 178.2(9) . .
N4 C27 Fe1 178.1(9) . .
C22 N1 C22 122(3) . 2_556
C22 N1 C23 86.3(14) . .
C22 N1 C23 122.7(16) 2_556 .
C22 N1 C23 122.7(16) . 2_556
C22 N1 C23 86.3(14) 2_556 2_556
C23 N1 C23 121(2) . 2_556
C3 S1 C1 103.1(5) . .
C2 S2 C4 97.3(5) . .
C5 S3 C3 95.3(5) . .
C4 S4 C5 95.6(5) . .
C7 S5 C6 94.5(5) . .
C6 S6 C8 94.4(5) . .
C9 S7 C7 98.5(5) . .
C8 S8 C10 101.8(5) . .
C13 S9 C11 102.6(6) . .
C12 S10 C14 99.7(6) . .
C15 S11 C13 93.9(4) . .
C15 S12 C14 93.7(4) . .
C16 S13 C17 94.0(4) . .
C16 S14 C18 94.6(4) . .
C17 S15 C19 99.6(5) . .
C18 S16 C20 103.7(5) . .
C27 Fe1 C27 90.1(5) 2_656 .
C27 Fe1 C25 89.5(4) 2_656 .
C27 Fe1 C25 179.2(4) . .
C27 Fe1 C25 179.2(4) 2_656 2_656
C27 Fe1 C25 89.5(4) . 2_656
C25 Fe1 C25 91.0(6) . 2_656
C27 Fe1 C26 89.5(4) 2_656 .
C27 Fe1 C26 89.9(4) . .
C25 Fe1 C26 89.5(4) . .
C25 Fe1 C26 91.1(4) 2_656 .
C27 Fe1 C26 89.9(4) 2_656 2_656
C27 Fe1 C26 89.5(4) . 2_656
C25 Fe1 C26 91.1(4) . 2_656
C25 Fe1 C26 89.5(4) 2_656 2_656
C26 Fe1 C26 179.2(5) . 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 1.404(15) .
C1 S1 1.783(11) .
C2 S2 1.809(13) .
C3 C4 1.368(12) .
C3 S1 1.737(10) .
C3 S3 1.734(10) .
C4 S4 1.747(11) .
C4 S2 1.712(11) .
C5 C6 1.403(14) .
C5 S3 1.727(9) .
C5 S4 1.727(10) .
C6 S6 1.714(9) .
C6 S5 1.708(10) .
C7 C8 1.357(12) .
C7 S5 1.726(9) .
C7 S7 1.754(11) .
C8 S8 1.751(9) .
C8 S6 1.724(11) .
C9 C10 1.495(13) .
C9 S7 1.807(10) .
C10 S8 1.759(10) .
C11 C12 1.374(16) .
C11 S9 1.784(12) .
C12 S10 1.794(14) .
C13 C14 1.353(12) .
C13 S9 1.743(10) .
C13 S11 1.752(10) .
C14 S12 1.756(10) .
C14 S10 1.733(9) .
C15 C16 1.350(13) .
C15 S11 1.743(10) .
C15 S12 1.759(9) .
C16 S14 1.760(9) .
C16 S13 1.774(9) .
C17 C18 1.331(11) .
C17 S13 1.765(10) .
C17 S15 1.756(10) .
C18 S16 1.743(10) .
C18 S14 1.769(10) .
C19 C20 1.532(13) .
C19 S15 1.795(10) .
C20 S16 1.804(10) .
C21 C22 2.03(3) .
C22 N1 1.38(3) .
C23 C24 1.47(3) .
C23 N1 1.83(3) .
C25 N2 1.140(11) .
C25 Fe1 1.945(10) .
C26 N3 1.145(12) .
C26 Fe1 1.944(11) .
C27 N4 1.123(11) .
C27 Fe1 1.953(10) .
N1 C22 1.38(3) 2_556
N1 C23 1.83(3) 2_556
Fe1 C27 1.953(10) 2_656
Fe1 C25 1.945(10) 2_656
Fe1 C26 1.944(11) 2_656
