#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001487.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_4001487
loop_
_publ_author_name
'Hervé, Katel'
'Cador, Olivier'
'Golhen, Stéphane'
'Costuas, Karine'
'Halet, Jean-François'
'Shirahata, Takashi'
'Muto, Tsuyoshi'
'Imakubo, Tatsuro'
'Miyazaki, Akira'
'Ouahab, Lahcène'
_publ_section_title
;
 Iodine Substituted Tetrathiafulvalene Radical Cation Salts with
 [M(isoq)2(NCS)4]-Anions where M = CrIII, GaIII:  Role of
 I···S and S···S Contacts on
 Structural and Magnetic Properties
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              790
_journal_paper_doi               10.1021/cm052199q
_journal_volume                  18
_journal_year                    2006
_chemical_formula_sum            'C38 H22 Cr I4 N6 S16'
_chemical_formula_weight         1635.18
_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                101.256(2)
_cell_angle_beta                 96.755(2)
_cell_angle_gamma                97.342(5)
_cell_formula_units_Z            1
_cell_length_a                   10.6760(5)
_cell_length_b                   11.3000(6)
_cell_length_c                   11.3930(9)
_cell_measurement_reflns_used    3923
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.998
_cell_volume                     1322.51(14)
_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    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.1097
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7547
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    3.220
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0489
_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)+(0.0622P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                2458
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm052199qsi20051128_120741.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4001487
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
Cr Cr 0.0000 0.0000 0.0000 0.0421(6) Uani 1 2 d S
C1 C -0.0830(9) 0.0216(9) 0.2422(10) 0.045(3) Uani 1 1 d .
H1 H 0.0014 0.0590 0.2661 0.054 Uiso 1 1 calc R
C2 C -0.1640(9) 0.0141(9) 0.3333(10) 0.044(3) Uani 1 1 d .
C3 C -0.1201(11) 0.0641(10) 0.4550(10) 0.054(3) Uani 1 1 d .
H3 H -0.0362 0.1029 0.4792 0.064 Uiso 1 1 calc R
C4 C -0.2011(12) 0.0561(11) 0.5393(11) 0.066(4) Uani 1 1 d .
H4 H -0.1734 0.0912 0.6206 0.079 Uiso 1 1 calc R
C5 C -0.3283(11) -0.0068(11) 0.5004(12) 0.064(4) Uani 1 1 d .
H5 H -0.3823 -0.0156 0.5576 0.077 Uiso 1 1 calc R
C6 C -0.3726(10) -0.0549(11) 0.3797(10) 0.057(3) Uani 1 1 d .
H6 H -0.4565 -0.0937 0.3557 0.068 Uiso 1 1 calc R
C7 C -0.2914(9) -0.0452(10) 0.2938(11) 0.049(3) Uani 1 1 d .
C8 C -0.3303(10) -0.0894(10) 0.1677(11) 0.052(3) Uani 1 1 d .
H8 H -0.4139 -0.1271 0.1390 0.062 Uiso 1 1 calc R
C9 C -0.2478(9) -0.0773(9) 0.0899(11) 0.049(3) Uani 1 1 d .
H9 H -0.2758 -0.1073 0.0078 0.059 Uiso 1 1 calc R
C10 C -0.2038(9) 0.1326(10) -0.1183(9) 0.042(3) Uani 1 1 d .
C11 C -0.1057(9) -0.2602(11) -0.1543(10) 0.044(3) Uani 1 1 d .
C12 C -0.6967(10) -0.3257(10) 0.6099(9) 0.047(3) Uani 1 1 d .
C13 C -0.5972(10) -0.2838(9) 0.6949(9) 0.045(3) Uani 1 1 d .
C14 C -0.5018(9) -0.3400(11) 0.4957(10) 0.050(3) Uani 1 1 d .
C15 C -0.4240(9) -0.3595(9) 0.4085(10) 0.046(3) Uani 1 1 d .
C16 C -0.3285(10) -0.3894(10) 0.2096(10) 0.049(3) Uani 1 1 d .
C17 C -0.2285(10) -0.3465(9) 0.2979(10) 0.048(3) Uani 1 1 d .
C18 C -0.1683(11) -0.4722(12) 0.0647(11) 0.066(4) Uani 1 1 d .
H18A H -0.1684 -0.5368 0.1097 0.079 Uiso 1 1 calc R
H18B H -0.1516 -0.5050 -0.0162 0.079 Uiso 1 1 calc R
C19 C -0.0620(11) -0.3661(13) 0.1270(11) 0.072(4) Uani 1 1 d .
H19A H -0.0656 -0.3006 0.0835 0.086 Uiso 1 1 calc R
H19B H 0.0198 -0.3937 0.1208 0.086 Uiso 1 1 calc R
I1 I -0.88726(6) -0.36041(7) 0.63927(7) 0.0514(3) Uani 1 1 d .
I2 I -0.60301(7) -0.23580(8) 0.87787(7) 0.0586(3) Uani 1 1 d .
S1 S -0.3070(3) 0.2143(3) -0.1637(3) 0.0698(10) Uani 1 1 d .
S2 S -0.1540(3) -0.3979(3) -0.2386(3) 0.0627(9) Uani 1 1 d .
S3 S -0.6693(3) -0.3718(3) 0.4605(3) 0.0553(8) Uani 1 1 d .
S4 S -0.4472(3) -0.2831(3) 0.6481(3) 0.0572(8) Uani 1 1 d .
S5 S -0.4792(3) -0.4191(3) 0.2571(3) 0.0530(8) Uani 1 1 d .
S6 S -0.2585(3) -0.3308(3) 0.4473(3) 0.0532(8) Uani 1 1 d .
S7 S -0.3224(3) -0.4234(3) 0.0556(3) 0.0608(8) Uani 1 1 d .
S8 S -0.0697(3) -0.3058(3) 0.2838(3) 0.0661(9) Uani 1 1 d .
N1 N -0.1230(8) -0.0221(8) 0.1265(8) 0.044(2) Uani 1 1 d .
N2 N -0.1309(8) 0.0732(9) -0.0873(8) 0.055(3) Uani 1 1 d .
N3 N -0.0735(8) -0.1642(9) -0.0967(9) 0.055(3) Uani 1 1 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'
Cr Cr 0.3209 0.6236 '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'
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'
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
N3 Cr N3 180.0(7) 2 .
N3 Cr N2 89.3(4) 2 .
N3 Cr N2 90.7(4) . .
N3 Cr N2 90.7(4) 2 2
N3 Cr N2 89.3(4) . 2
N2 Cr N2 180.0(7) . 2
N3 Cr N1 90.0(3) 2 .
N3 Cr N1 90.0(3) . .
N2 Cr N1 88.7(3) . .
N2 Cr N1 91.3(3) 2 .
N3 Cr N1 90.0(3) 2 2
N3 Cr N1 90.0(3) . 2
N2 Cr N1 91.3(3) . 2
N2 Cr N1 88.7(3) 2 2
N1 Cr N1 180.0(6) . 2
N1 C1 C2 122.8(10) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C3 C2 C7 121.3(10) . .
C3 C2 C1 121.6(10) . .
C7 C2 C1 117.1(10) . .
C4 C3 C2 119.8(11) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C5 119.1(12) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C6 C5 C4 121.2(10) . .
C6 C5 H5 119.4 . .
C4 C5 H5 119.4 . .
C5 C6 C7 119.8(11) . .
C5 C6 H6 120.1 . .
C7 C6 H6 120.1 . .
C6 C7 C2 118.7(11) . .
C6 C7 C8 123.4(10) . .
C2 C7 C8 117.9(10) . .
C9 C8 C7 120.5(10) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 N1 122.6(11) . .
C8 C9 H9 118.7 . .
N1 C9 H9 118.7 . .
N2 C10 S1 179.1(11) . .
N3 C11 S2 179.1(11) . .
C13 C12 S3 118.4(8) . .
C13 C12 I1 125.6(8) . .
S3 C12 I1 115.7(6) . .
C12 C13 S4 116.3(8) . .
C12 C13 I2 125.9(8) . .
S4 C13 I2 117.5(6) . .
C15 C14 S4 124.3(8) . .
C15 C14 S3 121.9(9) . .
S4 C14 S3 113.8(6) . .
C14 C15 S5 123.9(8) . .
C14 C15 S6 120.6(8) . .
S5 C15 S6 115.4(5) . .
C17 C16 S7 126.2(8) . .
C17 C16 S5 116.2(9) . .
S7 C16 S5 117.5(7) . .
C16 C17 S8 128.4(9) . .
C16 C17 S6 117.3(8) . .
S8 C17 S6 114.3(6) . .
C19 C18 S7 111.4(8) . .
C19 C18 H18A 109.4 . .
S7 C18 H18A 109.4 . .
C19 C18 H18B 109.4 . .
S7 C18 H18B 109.4 . .
H18A C18 H18B 108.0 . .
C18 C19 S8 114.8(8) . .
C18 C19 H19A 108.6 . .
S8 C19 H19A 108.6 . .
C18 C19 H19B 108.6 . .
S8 C19 H19B 108.6 . .
H19A C19 H19B 107.5 . .
C12 S3 C14 94.9(5) . .
C14 S4 C13 96.6(5) . .
C15 S5 C16 94.8(5) . .
C15 S6 C17 94.5(5) . .
C16 S7 C18 97.0(5) . .
C17 S8 C19 104.0(6) . .
C1 N1 C9 119.2(9) . .
C1 N1 Cr 119.9(7) . .
C9 N1 Cr 120.9(7) . .
C10 N2 Cr 167.0(9) . .
C11 N3 Cr 174.2(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr N3 1.975(10) 2
Cr N3 1.975(10) .
Cr N2 1.979(9) .
Cr N2 1.979(9) 2
Cr N1 2.090(8) .
Cr N1 2.090(8) 2
C1 N1 1.313(13) .
C1 C2 1.435(14) .
C1 H1 0.9300 .
C2 C3 1.391(14) .
C2 C7 1.416(14) .
C3 C4 1.374(14) .
C3 H3 0.9300 .
C4 C5 1.426(16) .
C4 H4 0.9300 .
C5 C6 1.379(15) .
C5 H5 0.9300 .
C6 C7 1.393(14) .
C6 H6 0.9300 .
C7 C8 1.418(15) .
C8 C9 1.334(14) .
C8 H8 0.9300 .
C9 N1 1.376(12) .
C9 H9 0.9300 .
C10 N2 1.158(12) .
C10 S1 1.628(11) .
C11 N3 1.140(13) .
C11 S2 1.645(12) .
C12 C13 1.320(14) .
C12 S3 1.750(10) .
C12 I1 2.100(10) .
C13 S4 1.746(10) .
C13 I2 2.059(10) .
C14 C15 1.371(13) .
C14 S4 1.732(11) .
C14 S3 1.761(10) .
C15 S5 1.727(11) .
C15 S6 1.742(10) .
C16 C17 1.346(14) .
C16 S7 1.732(12) .
C16 S5 1.769(10) .
C17 S8 1.734(10) .
C17 S6 1.749(11) .
C18 C19 1.536(16) .
C18 S7 1.799(11) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 S8 1.799(13) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
