#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/24/4502418.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_4502418
loop_
_publ_author_name
'Zhang, Bin'
'Kurmoo, Mohamedally'
'Mori, Takehiko'
'Zhang, Yan'
'Pratt, Francis Laurence'
'Zhu, Daoben'
_publ_section_title
;
 Polymorphism in Hybrid Organic−Inorganic Bilayered Magnetic
 Conductors (BEDT-TTF)3(FeIIICl4)2, BEDT-TTF =
 bis(ethylenedithio)tetrathiafulvalene
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              782
_journal_paper_doi               10.1021/cg9011718
_journal_volume                  10
_journal_year                    2010
_chemical_formula_sum            'C15 H12 Cl4 Fe S12'
_chemical_formula_weight         774.62
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.526(2)
_cell_angle_beta                 81.032(2)
_cell_angle_gamma                81.066(3)
_cell_formula_units_Z            2
_cell_length_a                   6.7396(3)
_cell_length_b                   9.9694(5)
_cell_length_c                   21.1318(12)
_cell_measurement_reflns_used    17138
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      3.43
_cell_volume                     1367.28(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.1523
_diffrn_reflns_av_sigmaI/netI    0.2693
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17138
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.2123
_refine_ls_R_factor_gt           0.0569
_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)+(0.0117P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                1803
_reflns_number_total             4738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9011718_si_001.cif
_cod_data_source_block           CCDC698222
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constr.' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4502418
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
Fe1 Fe 0.72420(14) 0.69636(10) 0.16793(5) 0.0464(3) Uani 1 1 d .
Cl1 Cl 0.6674(3) 0.84660(18) 0.23513(9) 0.0657(6) Uani 1 1 d .
Cl2 Cl 0.8781(3) 0.77835(17) 0.07279(8) 0.0563(5) Uani 1 1 d .
Cl3 Cl 0.9155(3) 0.51726(18) 0.21104(9) 0.0667(6) Uani 1 1 d .
Cl4 Cl 0.4386(3) 0.63378(19) 0.15445(9) 0.0722(6) Uani 1 1 d .
S1 S 0.3522(2) -0.08294(17) 0.42242(9) 0.0486(6) Uani 1 1 d .
S2 S 0.7576(2) 0.00052(17) 0.40751(8) 0.0487(6) Uani 1 1 d .
S3 S 0.4790(2) -0.33424(17) 0.53470(9) 0.0497(6) Uani 1 1 d .
S4 S 0.8803(2) -0.24610(17) 0.52227(8) 0.0451(5) Uani 1 1 d .
S5 S 0.2149(3) 0.11047(19) 0.31180(9) 0.0560(6) Uani 1 1 d .
S6 S 0.7016(3) 0.21371(19) 0.29358(9) 0.0592(6) Uani 1 1 d .
S7 S 0.5581(3) -0.57729(18) 0.63396(9) 0.0585(6) Uani 1 1 d .
S8 S 1.0414(3) -0.4747(2) 0.61685(10) 0.0756(7) Uani 1 1 d .
S9 S 0.2023(2) 1.46758(18) 0.05061(9) 0.0523(6) Uani 1 1 d .
S10 S 0.5590(2) 1.27625(18) 0.01924(9) 0.0527(6) Uani 1 1 d .
S11 S -0.0463(3) 1.25656(19) 0.12165(9) 0.0615(6) Uani 1 1 d .
S12 S 0.3908(3) 1.02720(19) 0.08589(10) 0.0674(7) Uani 1 1 d .
C1 C 0.5912(8) -0.1134(6) 0.4482(3) 0.0389(18) Uani 1 1 d .
C2 C 0.6419(8) -0.2178(6) 0.4954(3) 0.0385(18) Uani 1 1 d .
C3 C 0.4133(9) 0.0465(6) 0.3579(3) 0.0376(18) Uani 1 1 d .
C4 C 0.5964(10) 0.0874(6) 0.3509(3) 0.0384(18) Uani 1 1 d .
C5 C 0.6514(9) -0.4368(6) 0.5832(3) 0.0369(18) Uani 1 1 d .
C6 C 0.8341(9) -0.3952(6) 0.5766(3) 0.0358(18) Uani 1 1 d .
C7 C 0.3260(14) 0.2391(9) 0.2559(4) 0.126(4) Uani 1 1 d .
H7A H 0.2986 0.2254 0.2140 0.151 Uiso 1 1 calc R
H7B H 0.2437 0.3244 0.2644 0.151 Uiso 1 1 calc R
C8 C 0.5028(13) 0.2661(10) 0.2463(5) 0.153(5) Uani 1 1 d .
H8A H 0.4895 0.3658 0.2391 0.184 Uiso 1 1 calc R
H8B H 0.5573 0.2391 0.2045 0.184 Uiso 1 1 calc R
C9 C 0.7713(10) -0.6524(7) 0.6771(4) 0.074(3) Uani 1 1 d .
H9A H 0.7568 -0.6116 0.7162 0.089 Uiso 1 1 calc R
H9B H 0.7610 -0.7496 0.6907 0.089 Uiso 1 1 calc R
C10 C 0.9697(11) -0.6399(7) 0.6443(4) 0.079(3) Uani 1 1 d .
H10A H 0.9871 -0.6866 0.6069 0.095 Uiso 1 1 calc R
H10B H 1.0648 -0.6899 0.6730 0.095 Uiso 1 1 calc R
C11 C 0.4493(9) 1.4459(6) 0.0155(3) 0.0402(19) Uani 1 1 d .
C12 C 0.1865(9) 1.2965(6) 0.0801(3) 0.0416(19) Uani 1 1 d .
C13 C 0.3516(10) 1.2067(7) 0.0655(3) 0.0458(19) Uani 1 1 d .
C14 C -0.0273(10) 1.0793(6) 0.1120(3) 0.064(2) Uani 1 1 d .
H14A H -0.1470 1.0414 0.1354 0.076 Uiso 1 1 calc R
H14B H -0.0236 1.0744 0.0664 0.076 Uiso 1 1 calc R
C15 C 0.1588(9) 0.9932(7) 0.1364(3) 0.064(2) Uani 1 1 d .
H15A H 0.1448 0.8967 0.1396 0.077 Uiso 1 1 calc R
H15B H 0.1661 1.0100 0.1797 0.077 Uiso 1 1 calc R
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.015
0 -1 0 0.025
-4 -1 -2 0.260
4 1 2 0.250
0 0 1 0.015
0 0 -1 0.025
0 1 1 0.010
0 -1 -1 0.020
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
Cl3 Fe1 Cl4 109.12(8) .
Cl3 Fe1 Cl2 108.91(8) .
Cl4 Fe1 Cl2 108.69(8) .
Cl3 Fe1 Cl1 107.64(8) .
Cl4 Fe1 Cl1 110.20(8) .
Cl2 Fe1 Cl1 112.23(8) .
C3 S1 C1 95.1(3) .
C1 S2 C4 95.7(3) .
C2 S3 C5 96.3(3) .
C6 S4 C2 94.9(3) .
C3 S5 C7 100.2(3) .
C4 S6 C8 99.7(4) .
C5 S7 C9 102.0(3) .
C6 S8 C10 100.2(3) .
C11 S9 C12 96.4(3) .
C11 S10 C13 95.5(3) .
C12 S11 C14 100.1(3) .
C13 S12 C15 101.8(3) .
C2 C1 S2 123.1(4) .
C2 C1 S1 122.3(5) .
S2 C1 S1 114.6(3) .
C1 C2 S3 123.3(4) .
C1 C2 S4 122.1(5) .
S3 C2 S4 114.5(3) .
C4 C3 S1 118.2(4) .
C4 C3 S5 128.5(5) .
S1 C3 S5 113.3(4) .
C3 C4 S6 129.6(5) .
C3 C4 S2 116.0(5) .
S6 C4 S2 114.4(4) .
C6 C5 S7 129.4(4) .
C6 C5 S3 115.7(5) .
S7 C5 S3 114.9(4) .
C5 C6 S4 118.5(4) .
C5 C6 S8 127.4(5) .
S4 C6 S8 114.1(4) .
C8 C7 S5 130.0(7) .
C7 C8 S6 130.8(7) .
C10 C9 S7 118.2(5) .
C9 C10 S8 119.0(5) .
C11 C11 S9 122.8(6) 2_685
C11 C11 S10 122.4(6) 2_685
S9 C11 S10 114.7(3) .
C13 C12 S9 116.7(5) .
C13 C12 S11 126.7(5) .
S9 C12 S11 116.4(4) .
C12 C13 S10 116.5(5) .
C12 C13 S12 129.7(5) .
S10 C13 S12 113.8(4) .
C15 C14 S11 112.7(5) .
C14 C15 S12 113.8(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl3 2.1772(17) .
Fe1 Cl4 2.1873(19) .
Fe1 Cl2 2.1914(19) .
Fe1 Cl1 2.198(2) .
S1 C3 1.745(6) .
S1 C1 1.745(6) .
S2 C1 1.740(6) .
S2 C4 1.760(6) .
S3 C2 1.733(6) .
S3 C5 1.751(5) .
S4 C6 1.742(6) .
S4 C2 1.752(6) .
S5 C3 1.749(6) .
S5 C7 1.753(8) .
S6 C4 1.735(6) .
S6 C8 1.754(7) .
S7 C5 1.739(6) .
S7 C9 1.812(6) .
S8 C6 1.757(6) .
S8 C10 1.759(7) .
S9 C11 1.712(6) .
S9 C12 1.720(6) .
S10 C11 1.730(6) .
S10 C13 1.737(6) .
S11 C12 1.740(6) .
S11 C14 1.798(6) .
S12 C13 1.751(6) .
S12 C15 1.793(6) .
C1 C2 1.347(7) .
C3 C4 1.337(7) .
C5 C6 1.339(7) .
C7 C8 1.240(9) .
C9 C10 1.420(8) .
C11 C11 1.376(10) 2_685
C12 C13 1.349(8) .
C14 C15 1.511(7) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C8 H8A Cl4 0.97 2.94 3.817(8) 151.5 .
C7 H7B Cl3 0.97 2.92 3.704(9) 138.6 1_455
C9 H9A Cl4 0.97 2.83 3.646(8) 142.3 2_656
C10 H10B Cl1 0.97 2.93 3.898(7) 176.8 2_756
C14 H14A Cl1 0.97 2.87 3.743(7) 150.5 1_455
C15 H15A Cl2 0.97 2.94 3.615(7) 127.3 1_455
C10 H10A S4 0.97 2.90 3.832(9) 161.0 2_746
C8 H8B S11 0.97 2.97 3.699(10) 133.2 1_645
