#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/63/4306365.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_4306365
loop_
_publ_author_name
'Marc Fourmigué'
'Pascale Auban-Senzier'
_publ_section_title
;
Anionic Layered Networks Reconstructed from [Cd(SCN)3]∞-Chains in
Pseudo One-Dimensional Conducting Salts of Halogenated Tetrathiafulvalenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9979
_journal_page_last               9986
_journal_paper_doi               10.1021/ic801207v
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '(C8 H4 I4 S6)2, Cd1.5(NCS)4, C2 H3 N, H2 O'
_chemical_formula_sum            'C22 H12 Cd1.5 I4 N5 O S16'
_chemical_formula_weight         1551.53
_chemical_name_common            '(EDT-TTF-I2)2 Cd1.5(NCS)4, CH3CN, H2O'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2007-07-17T11:08:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.318(8)
_cell_angle_beta                 95.7570(10)
_cell_angle_gamma                95.48590(10)
_cell_formula_units_Z            2
_cell_length_a                   8.79570(10)
_cell_length_b                   12.9571(2)
_cell_length_c                   19.6473(4)
_cell_measurement_reflns_used    25956
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     2141.74(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.566573E-1
_diffrn_orient_matrix_UB_12      0.121088E-1
_diffrn_orient_matrix_UB_13      -0.435233E-1
_diffrn_orient_matrix_UB_21      -0.982686E-1
_diffrn_orient_matrix_UB_22      -0.26427E-2
_diffrn_orient_matrix_UB_23      0.214292E-1
_diffrn_orient_matrix_UB_31      0.199343E-1
_diffrn_orient_matrix_UB_32      0.793181E-1
_diffrn_orient_matrix_UB_33      0.212644E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37828
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.444
_exptl_absorpt_correction_T_max  0.285
_exptl_absorpt_correction_T_min  0.1913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1454
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.302
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         9766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.051
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0518P)²+2.0422P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                8004
_reflns_number_total             9766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801207v_si_001_2.cif
_cod_data_source_block           EDTI2Cd
_cod_original_cell_volume        2141.74(6)
_cod_original_formula_sum        'C22 H12 Cd1.50 I4 N5 O S16'
_cod_database_code               4306365
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
Cd1 Cd 0 0 0 0.04022(12) Uani 1 2 d S . .
Cd2 Cd 0.54877(4) 0.27452(2) -0.007953(17) 0.03972(10) Uani 1 1 d . . .
S1 S 0.14569(17) 0.13892(12) 0.12413(7) 0.0566(3) Uani 1 1 d . . .
S2 S 0.37196(16) 0.32765(10) -0.11449(7) 0.0513(3) Uani 1 1 d . . .
S3 S 0.78197(16) 0.29305(11) -0.08523(7) 0.0512(3) Uani 1 1 d . . .
S4 S 0.50408(15) 0.06914(10) -0.09047(8) 0.0528(3) Uani 1 1 d . . .
C1 C 0.2763(5) 0.1924(4) 0.0845(2) 0.0437(10) Uani 1 1 d . . .
C2 C 0.3925(5) 0.4576(4) -0.0818(2) 0.0387(9) Uani 1 1 d . . .
C3 C 0.8810(5) 0.2061(4) -0.0578(2) 0.0396(10) Uani 1 1 d . . .
C4 C 0.3372(5) 0.0253(3) -0.0698(2) 0.0376(9) Uani 1 1 d . . .
N1 N 0.3664(5) 0.2319(3) 0.0574(2) 0.0531(10) Uani 1 1 d . . .
N2 N 0.4074(5) 0.5505(3) -0.0596(2) 0.0483(9) Uani 1 1 d . . .
N3 N 0.9495(5) 0.1446(3) -0.0406(2) 0.0519(10) Uani 1 1 d . . .
N4 N 0.2202(4) -0.0070(3) -0.0567(2) 0.0482(9) Uani 1 1 d . . .
O1 O 0.7184(4) 0.2417(3) 0.08486(19) 0.0513(8) Uani 1 1 d . . .
I1A I -1.07971(3) 0.39601(2) 0.745880(16) 0.04320(10) Uani 1 1 d . . .
I2A I -1.45563(4) 0.21015(3) 0.706734(17) 0.04695(10) Uani 1 1 d . . .
S1A S -1.03028(14) 0.25758(10) 0.58945(6) 0.0437(3) Uani 1 1 d . . .
S2A S -1.32095(13) 0.11269(10) 0.55934(6) 0.0443(3) Uani 1 1 d . . .
S3A S -0.93050(14) 0.13452(10) 0.44003(6) 0.0450(3) Uani 1 1 d . . .
S4A S -1.21953(13) -0.01160(10) 0.40985(6) 0.0447(3) Uani 1 1 d . . .
S5A S -0.81038(15) 0.03908(11) 0.30848(7) 0.0510(3) Uani 1 1 d . . .
S6A S -1.15338(14) -0.13648(10) 0.27012(7) 0.0471(3) Uani 1 1 d . . .
C1A C -1.1532(5) 0.2743(4) 0.6545(2) 0.0369(9) Uani 1 1 d . . .
C2A C -1.2852(5) 0.2080(4) 0.6409(2) 0.0374(9) Uani 1 1 d . . .
C3A C -1.1455(5) 0.1481(4) 0.5317(2) 0.0403(10) Uani 1 1 d . . .
C4A C -1.1035(5) 0.0957(4) 0.4684(2) 0.0392(10) Uani 1 1 d . . .
C5A C -0.9603(5) 0.0353(4) 0.3594(2) 0.0400(10) Uani 1 1 d . . .
C6A C -1.0938(5) -0.0319(4) 0.3458(2) 0.0386(9) Uani 1 1 d . . .
C7A C -0.8789(6) -0.0633(5) 0.2280(3) 0.0545(13) Uani 1 1 d . . .
H7A1 H -0.8325 -0.044 0.1894 0.065 Uiso 1 1 calc R . .
H7A2 H -0.8439 -0.1303 0.2327 0.065 Uiso 1 1 calc R . .
C8A C -1.0504(6) -0.0815(5) 0.2088(3) 0.0582(14) Uani 1 1 d . . .
H8A1 H -1.0751 -0.1302 0.1619 0.07 Uiso 1 1 calc R . .
H8A2 H -1.0865 -0.0137 0.2067 0.07 Uiso 1 1 calc R . .
I1B I -0.41669(3) 0.10239(2) 0.244320(16) 0.04277(10) Uani 1 1 d . . .
I2B I -0.03632(4) 0.28575(3) 0.289485(18) 0.04837(10) Uani 1 1 d . . .
S1B S -0.46393(14) 0.23287(10) 0.40389(6) 0.0462(3) Uani 1 1 d . . .
S2B S -0.17172(14) 0.37591(10) 0.43771(6) 0.0454(3) Uani 1 1 d . . .
S3B S -0.57147(14) 0.35344(11) 0.55084(6) 0.0483(3) Uani 1 1 d . . .
S4B S -0.28312(14) 0.50007(10) 0.58658(6) 0.0454(3) Uani 1 1 d . . .
S5B S -0.70539(15) 0.44908(12) 0.67812(7) 0.0551(3) Uani 1 1 d . . .
S6B S -0.36252(15) 0.62305(11) 0.72476(7) 0.0505(3) Uani 1 1 d . . .
C1B C -0.3406(5) 0.2186(4) 0.3392(2) 0.0375(9) Uani 1 1 d . . .
C2B C -0.2076(5) 0.2834(4) 0.3545(2) 0.0382(9) Uani 1 1 d . . .
C3B C -0.3498(5) 0.3411(4) 0.4631(2) 0.0419(10) Uani 1 1 d . . .
C4B C -0.3959(5) 0.3931(4) 0.5256(2) 0.0420(10) Uani 1 1 d . . .
C5B C -0.5508(5) 0.4529(4) 0.6304(3) 0.0423(10) Uani 1 1 d . . .
C6B C -0.4154(5) 0.5202(4) 0.6477(2) 0.0412(10) Uani 1 1 d . . .
C7B C -0.6367(7) 0.5425(6) 0.7620(3) 0.0668(16) Uani 1 1 d . . .
H7B1 H -0.6756 0.61 0.7618 0.08 Uiso 1 1 calc R . .
H7B2 H -0.6818 0.5158 0.7984 0.08 Uiso 1 1 calc R . .
C8B C -0.4679(7) 0.5650(6) 0.7830(3) 0.0692(16) Uani 1 1 d . . .
H8B1 H -0.4287 0.4984 0.7855 0.083 Uiso 1 1 calc R . .
H8B2 H -0.4479 0.6134 0.8301 0.083 Uiso 1 1 calc R . .
C5 C 0.0555(7) 0.4197(4) 0.0844(3) 0.0572(13) Uani 1 1 d . . .
N5 N -0.0245(7) 0.4186(5) 0.1251(3) 0.0822(17) Uani 1 1 d . . .
C6 C 0.1579(7) 0.4201(5) 0.0312(4) 0.0712(17) Uani 1 1 d . . .
H6A H 0.1366 0.3534 -0.0048 0.107 Uiso 1 1 calc R . .
H6B H 0.2627 0.4286 0.0528 0.107 Uiso 1 1 calc R . .
H6C H 0.1424 0.4784 0.0103 0.107 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 0 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
1 -1 9 0.101
-1 1 -11 0.151
-16 1 -8 0.253
-1 -1 8 0.157
14 -1 8 0.145
10 1 -8 0.191
3 1 -8 0.196
3 -3 1 0.097
-8 -7 -2 0.225
-3 7 -1 0.138
0 0 1 0.092
-1 0 -16 0.14
-7 2 -3 0.229
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
N3 Cd1 N3 180.00(19) 2_655 1_455 ?
N3 Cd1 N4 91.24(15) 2_655 . ?
N3 Cd1 N4 88.76(15) 1_455 . ?
N3 Cd1 N4 88.76(15) 2_655 2 ?
N3 Cd1 N4 91.24(15) 1_455 2 ?
N4 Cd1 N4 180.00(19) . 2 ?
N3 Cd1 S1 91.28(12) 2_655 . ?
N3 Cd1 S1 88.72(12) 1_455 . ?
N4 Cd1 S1 94.48(11) . . ?
N4 Cd1 S1 85.52(11) 2 . ?
N3 Cd1 S1 88.72(12) 2_655 2 ?
N3 Cd1 S1 91.28(12) 1_455 2 ?
N4 Cd1 S1 85.52(11) . 2 ?
N4 Cd1 S1 94.48(11) 2 2 ?
S1 Cd1 S1 180.00(10) . 2 ?
N1 Cd2 N2 91.91(15) . 2_665 ?
N1 Cd2 O1 82.76(15) . . ?
N2 Cd2 O1 84.03(14) 2_665 . ?
N1 Cd2 S3 170.30(12) . . ?
N2 Cd2 S3 95.32(11) 2_665 . ?
O1 Cd2 S3 91.57(9) . . ?
N1 Cd2 S4 89.96(11) . . ?
N2 Cd2 S4 178.13(11) 2_665 . ?
O1 Cd2 S4 96.22(9) . . ?
S3 Cd2 S4 82.82(4) . . ?
N1 Cd2 S2 101.04(12) . . ?
N2 Cd2 S2 92.44(10) 2_665 . ?
O1 Cd2 S2 174.93(9) . . ?
S3 Cd2 S2 85.12(4) . . ?
S4 Cd2 S2 87.19(4) . . ?
C1 S1 Cd1 93.63(16) . . ?
C2 S2 Cd2 98.66(16) . . ?
C3 S3 Cd2 96.00(15) . . ?
C4 S4 Cd2 100.94(15) . . ?
N1 C1 S1 178.5(5) . . ?
N2 C2 S2 178.9(4) . . ?
N3 C3 S3 178.2(4) . . ?
N4 C4 S4 178.5(4) . . ?
C1 N1 Cd2 168.2(4) . . ?
C2 N2 Cd2 167.3(4) . 2_665 ?
C3 N3 Cd1 159.3(4) . 1_655 ?
C4 N4 Cd1 156.0(4) . . ?
C3A S1A C1A 95.2(2) . . ?
C2A S2A C3A 94.9(2) . . ?
C4A S3A C5A 95.3(2) . . ?
C4A S4A C6A 95.7(2) . . ?
C5A S5A C7A 103.5(2) . . ?
C6A S6A C8A 97.9(2) . . ?
C2A C1A S1A 117.3(3) . . ?
C2A C1A I1A 126.4(3) . . ?
S1A C1A I1A 116.4(2) . . ?
C1A C2A S2A 117.4(3) . . ?
C1A C2A I2A 126.1(3) . . ?
S2A C2A I2A 116.4(2) . . ?
C4A C3A S1A 122.4(4) . . ?
C4A C3A S2A 122.5(4) . . ?
S1A C3A S2A 115.1(3) . . ?
C3A C4A S4A 122.7(4) . . ?
C3A C4A S3A 122.1(4) . . ?
S4A C4A S3A 115.2(3) . . ?
C6A C5A S5A 129.7(4) . . ?
C6A C5A S3A 116.7(3) . . ?
S5A C5A S3A 113.7(3) . . ?
C5A C6A S6A 126.4(4) . . ?
C5A C6A S4A 117.1(3) . . ?
S6A C6A S4A 116.6(3) . . ?
C8A C7A S5A 114.9(4) . . ?
C7A C8A S6A 114.0(4) . . ?
C1B S1B C3B 95.3(2) . . ?
C3B S2B C2B 94.7(2) . . ?
C4B S3B C5B 95.7(2) . . ?
C4B S4B C6B 95.8(2) . . ?
C5B S5B C7B 103.7(3) . . ?
C6B S6B C8B 98.1(3) . . ?
C2B C1B S1B 117.2(3) . . ?
C2B C1B I1B 126.2(3) . . ?
S1B C1B I1B 116.6(2) . . ?
C1B C2B S2B 117.4(3) . . ?
C1B C2B I2B 126.6(3) . . ?
S2B C2B I2B 116.0(2) . . ?
C4B C3B S1B 122.1(4) . . ?
C4B C3B S2B 122.9(4) . . ?
S1B C3B S2B 115.0(3) . . ?
C3B C4B S4B 123.1(4) . . ?
C3B C4B S3B 121.8(4) . . ?
S4B C4B S3B 115.1(3) . . ?
C6B C5B S5B 128.9(4) . . ?
C6B C5B S3B 116.8(4) . . ?
S5B C5B S3B 114.3(3) . . ?
C5B C6B S6B 126.2(4) . . ?
C5B C6B S4B 116.6(4) . . ?
S6B C6B S4B 117.2(3) . . ?
C8B C7B S5B 117.5(4) . . ?
C7B C8B S6B 115.1(5) . . ?
N5 C5 C6 179.3(7) . . ?
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
Cd1 N3 2.275(4) 2_655 ?
Cd1 N3 2.275(4) 1_455 ?
Cd1 N4 2.328(4) . ?
Cd1 N4 2.328(4) 2 ?
Cd1 S1 2.7551(14) . ?
Cd1 S1 2.7551(14) 2 ?
Cd2 N1 2.262(4) . ?
Cd2 N2 2.301(4) 2_665 ?
Cd2 O1 2.386(3) . ?
Cd2 S3 2.6983(13) . ?
Cd2 S4 2.7209(12) . ?
Cd2 S2 2.7455(14) . ?
S1 C1 1.643(5) . ?
S2 C2 1.632(5) . ?
S3 C3 1.647(5) . ?
S4 C4 1.648(5) . ?
C1 N1 1.148(6) . ?
C2 N2 1.163(6) . ?
C3 N3 1.139(6) . ?
C4 N4 1.150(6) . ?
N2 Cd2 2.301(4) 2_665 ?
N3 Cd1 2.275(4) 1_655 ?
I1A C1A 2.074(4) . ?
I2A C2A 2.074(4) . ?
S1A C3A 1.739(4) . ?
S1A C1A 1.742(4) . ?
S2A C2A 1.742(4) . ?
S2A C3A 1.745(5) . ?
S3A C4A 1.745(4) . ?
S3A C5A 1.754(5) . ?
S4A C4A 1.732(4) . ?
S4A C6A 1.745(5) . ?
S5A C5A 1.738(5) . ?
S5A C7A 1.800(6) . ?
S6A C6A 1.741(5) . ?
S6A C8A 1.817(6) . ?
C1A C2A 1.338(6) . ?
C3A C4A 1.365(6) . ?
C5A C6A 1.355(6) . ?
C7A C8A 1.499(8) . ?
I1B C1B 2.088(4) . ?
I2B C2B 2.073(4) . ?
S1B C1B 1.739(4) . ?
S1B C3B 1.737(5) . ?
S2B C3B 1.744(5) . ?
S2B C2B 1.750(5) . ?
S3B C4B 1.738(5) . ?
S3B C5B 1.742(5) . ?
S4B C4B 1.737(5) . ?
S4B C6B 1.745(5) . ?
S5B C5B 1.732(5) . ?
S5B C7B 1.795(6) . ?
S6B C6B 1.740(5) . ?
S6B C8B 1.800(7) . ?
C1B C2B 1.334(6) . ?
C3B C4B 1.367(6) . ?
C5B C6B 1.367(6) . ?
C7B C8B 1.481(8) . ?
C5 N5 1.118(8) . ?
C5 C6 1.447(8) . ?
