#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:38:36 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233311 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/87/4348751.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_4348751
loop_
_publ_author_name
'Rabaça, Sandra'
'Oliveira, Sandrina'
'Santos, Isabel C.'
'Gama, Vasco'
'Belo, Dulce'
'Lopes, Elsa B.'
'Canadell, Enric'
'Almeida, Manuel'
_publ_section_title
;
 Polymorphism and Superconductivity in Bilayer Molecular Metals
 (CNB-EDT-TTF)₄I₃.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10343
_journal_page_last               10350
_journal_paper_doi               10.1021/acs.inorgchem.6b01555
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C26 H14 I1.5 N2 S12'
_chemical_formula_weight         929.46
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                86.793(2)
_cell_angle_beta                 89.0790(10)
_cell_angle_gamma                84.558(2)
_cell_formula_units_Z            2
_cell_length_a                   5.7669(2)
_cell_length_b                   9.7113(3)
_cell_length_c                   27.7724(7)
_cell_measurement_reflns_used    5491
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.94
_cell_volume                     1545.84(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20199
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_correction_T_min  0.3304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             911
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         6.292
_refine_diff_density_min         -2.887
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1075P)²+2.7046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2457
_reflns_number_gt                3600
_reflns_number_total             5546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01555_si_002.cif
_cod_data_source_block           I3S5
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26 H14 I1.50 N2 S12'
_cod_database_code               4348751
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
I1 I 0.5000 1.0000 0.5000 0.1416(13) Uani 1 2 d S
I2 I 0.49302(16) 0.7011(2) 0.49473(3) 0.1308(9) Uani 1 1 d .
S1 S 0.0503(3) 0.2461(3) 0.15054(8) 0.0193(6) Uani 1 1 d .
S3 S -0.0719(4) 0.0417(3) 0.24239(7) 0.0185(6) Uani 1 1 d .
S7 S 0.0506(4) 0.7419(3) 0.15246(8) 0.0181(5) Uani 1 1 d .
S2 S 0.4619(4) 0.3207(3) 0.20296(8) 0.0186(6) Uani 1 1 d .
S10 S 0.3354(4) 0.6205(3) 0.29530(8) 0.0190(6) Uani 1 1 d .
S4 S 0.3330(4) 0.1234(3) 0.29345(8) 0.0205(6) Uani 1 1 d .
S8 S 0.4617(4) 0.8173(3) 0.20470(8) 0.0187(6) Uani 1 1 d .
S9 S -0.0693(4) 0.5368(3) 0.24451(8) 0.0191(6) Uani 1 1 d .
S5 S -0.2195(4) -0.1482(3) 0.32030(8) 0.0236(6) Uani 1 1 d .
S6 S 0.2671(4) -0.0540(3) 0.38104(8) 0.0263(7) Uani 1 1 d .
S11 S -0.2181(4) 0.3492(3) 0.32315(9) 0.0249(6) Uani 1 1 d .
S12 S 0.2670(4) 0.4455(3) 0.38385(8) 0.0240(6) Uani 1 1 d .
N2 N 0.7471(14) 1.2362(11) 0.0416(3) 0.032(2) Uani 1 1 d .
N1 N 0.7478(14) 0.7415(9) 0.0400(3) 0.026(2) Uani 1 1 d .
C4 C 0.5493(14) 0.4994(10) 0.1258(3) 0.017(2) Uani 1 1 d .
H4 H 0.6787 0.5256 0.1427 0.021 Uiso 1 1 calc R
C18 C 0.1631(15) 0.9226(12) 0.0774(3) 0.025(2) Uani 1 1 d .
H18 H 0.0332 0.8964 0.0607 0.029 Uiso 1 1 calc R
C5 C 0.1624(14) 0.4269(10) 0.0757(3) 0.018(2) Uani 1 1 d .
H5 H 0.0312 0.4024 0.0590 0.022 Uiso 1 1 calc R
C11 C -0.0136(14) -0.0399(11) 0.2999(3) 0.018(2) Uani 1 1 d .
C17 C 0.5491(15) 0.9964(10) 0.1275(3) 0.019(2) Uani 1 1 d .
H17 H 0.6789 1.0226 0.1443 0.023 Uiso 1 1 calc R
C19 C 0.4109(14) 0.8990(11) 0.1479(3) 0.018(2) Uani 1 1 d .
C8 C 0.2173(14) 0.2271(10) 0.2029(3) 0.018(2) Uani 1 1 d .
C10 C 0.1737(14) -0.0007(10) 0.3231(3) 0.0149(19) Uani 1 1 d .
C24 C -0.0119(14) 0.4577(10) 0.3025(3) 0.015(2) Uani 1 1 d .
C7 C 0.2151(14) 0.3667(10) 0.1209(3) 0.015(2) Uani 1 1 d .
C23 C 0.1750(14) 0.4960(11) 0.3253(3) 0.020(2) Uani 1 1 d .
C21 C 0.2187(14) 0.7209(10) 0.2050(3) 0.0151(19) Uani 1 1 d .
C1 C 0.6346(15) 0.6600(11) 0.0576(3) 0.024(2) Uani 1 1 d .
C22 C 0.1673(14) 0.6371(11) 0.2431(3) 0.020(2) Uani 1 1 d .
C20 C 0.2150(14) 0.8650(11) 0.1228(3) 0.018(2) Uani 1 1 d .
C13 C -0.1157(16) -0.2046(12) 0.3802(3) 0.027(3) Uani 1 1 d .
H13A H -0.2482 -0.2363 0.3996 0.032 Uiso 1 1 calc R
H13B H 0.0011 -0.2854 0.3774 0.032 Uiso 1 1 calc R
C14 C 0.6323(15) 1.1563(11) 0.0592(3) 0.021(2) Uani 1 1 d .
C9 C 0.1653(14) 0.1393(10) 0.2411(3) 0.017(2) Uani 1 1 d .
C6 C 0.4101(13) 0.4019(10) 0.1461(3) 0.0136(19) Uani 1 1 d .
C2 C 0.4935(14) 0.5581(10) 0.0797(3) 0.015(2) Uani 1 1 d .
C26 C -0.1130(16) 0.2914(11) 0.3829(3) 0.024(2) Uani 1 1 d .
H26A H -0.2437 0.2572 0.4022 0.029 Uiso 1 1 calc R
H26B H 0.0076 0.2126 0.3798 0.029 Uiso 1 1 calc R
C15 C 0.4922(15) 1.0552(11) 0.0814(3) 0.021(2) Uani 1 1 d .
C3 C 0.3003(15) 0.5225(11) 0.0549(3) 0.021(2) Uani 1 1 d .
H3 H 0.2645 0.5643 0.0239 0.026 Uiso 1 1 calc R
C16 C 0.3003(14) 1.0186(10) 0.0564(3) 0.018(2) Uani 1 1 d .
H16 H 0.2650 1.0595 0.0251 0.021 Uiso 1 1 calc R
C12 C -0.0082(16) -0.0974(11) 0.4073(3) 0.024(2) Uani 1 1 d .
H12A H 0.0170 -0.1326 0.4412 0.029 Uiso 1 1 calc R
H12B H -0.1176 -0.0125 0.4076 0.029 Uiso 1 1 calc R
C25 C -0.0105(15) 0.4031(11) 0.4100(3) 0.024(2) Uani 1 1 d .
H25A H 0.0121 0.3706 0.4441 0.029 Uiso 1 1 calc R
H25B H -0.1213 0.4876 0.4091 0.029 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'
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'
I I -0.4742 1.8119 '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'
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_3
I2 I1 I2 180.000(4) 2_676
C7 S1 C8 95.5(4) .
C9 S3 C11 95.6(4) .
C21 S7 C20 95.9(4) .
C6 S2 C8 94.9(4) .
C22 S10 C23 95.6(4) .
C10 S4 C9 95.3(4) .
C19 S8 C21 95.7(4) .
C22 S9 C24 95.6(4) .
C11 S5 C13 102.3(4) .
C10 S6 C12 99.2(4) .
C24 S11 C26 102.6(4) .
C23 S12 C25 98.9(4) .
C6 C4 C2 118.1(8) .
C20 C18 C16 119.7(9) .
C3 C5 C7 119.8(8) .
C10 C11 S5 129.4(7) .
C10 C11 S3 116.1(7) .
S5 C11 S3 114.2(5) .
C19 C17 C15 118.1(9) .
C17 C19 C20 119.8(8) .
C17 C19 S8 123.0(7) .
C20 C19 S8 117.1(7) .
C9 C8 S2 121.7(7) .
C9 C8 S1 121.9(7) .
S2 C8 S1 116.3(5) .
C11 C10 S6 127.3(7) .
C11 C10 S4 117.5(7) .
S6 C10 S4 115.1(5) .
C23 C24 S11 129.4(7) .
C23 C24 S9 116.5(7) .
S11 C24 S9 114.0(5) .
C5 C7 C6 120.6(8) .
C5 C7 S1 123.4(7) .
C6 C7 S1 116.0(6) .
C24 C23 S12 127.6(7) .
C24 C23 S10 117.4(7) .
S12 C23 S10 114.8(5) .
C22 C21 S7 122.9(7) .
C22 C21 S8 121.7(7) .
S7 C21 S8 115.4(5) .
N1 C1 C2 179.8(11) .
C21 C22 S10 121.9(7) .
C21 C22 S9 123.2(7) .
S10 C22 S9 114.9(5) .
C18 C20 C19 121.3(9) .
C18 C20 S7 122.9(7) .
C19 C20 S7 115.8(7) .
C12 C13 S5 115.6(7) .
N2 C14 C15 179.1(10) .
C8 C9 S3 123.5(7) .
C8 C9 S4 121.1(7) .
S3 C9 S4 115.3(5) .
C4 C6 C7 120.2(8) .
C4 C6 S2 122.6(7) .
C7 C6 S2 117.2(6) .
C3 C2 C4 121.4(8) .
C3 C2 C1 119.0(8) .
C4 C2 C1 119.6(8) .
C25 C26 S11 114.1(7) .
C16 C15 C17 121.7(9) .
C16 C15 C14 118.7(8) .
C17 C15 C14 119.6(9) .
C5 C3 C2 119.8(8) .
C18 C16 C15 119.4(8) .
C13 C12 S6 112.5(6) .
C26 C25 S12 111.6(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 I2 2.918(2) .
I1 I2 2.918(2) 2_676
S1 C7 1.740(9) .
S1 C8 1.750(9) .
S3 C9 1.735(9) .
S3 C11 1.764(9) .
S7 C21 1.756(9) .
S7 C20 1.756(9) .
S2 C6 1.743(8) .
S2 C8 1.749(9) .
S10 C22 1.749(9) .
S10 C23 1.757(9) .
S4 C10 1.746(9) .
S4 C9 1.751(9) .
S8 C19 1.743(8) .
S8 C21 1.757(9) .
S9 C22 1.749(9) .
S9 C24 1.766(8) .
S5 C11 1.728(9) .
S5 C13 1.816(9) .
S6 C10 1.741(8) .
S6 C12 1.813(9) .
S11 C24 1.733(9) .
S11 C26 1.816(9) .
S12 C23 1.747(9) .
S12 C25 1.819(9) .
N2 C14 1.151(13) .
N1 C1 1.156(13) .
C4 C6 1.389(12) .
C4 C2 1.401(12) .
C18 C20 1.375(13) .
C18 C16 1.379(13) .
C5 C3 1.375(13) .
C5 C7 1.382(12) .
C11 C10 1.362(12) .
C17 C19 1.385(13) .
C17 C15 1.403(12) .
C19 C20 1.411(12) .
C8 C9 1.370(12) .
C24 C23 1.352(13) .
C7 C6 1.412(12) .
C21 C22 1.345(12) .
C1 C2 1.444(13) .
C13 C12 1.503(15) .
C14 C15 1.437(13) .
C2 C3 1.400(13) .
C26 C25 1.523(15) .
C15 C16 1.401(13) .
