#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/35/4343514.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_4343514
loop_
_publ_author_name
'Oliveira, Sandrina'
'Ministro, José'
'Santos, Isabel C.'
'Belo, Dulce'
'Lopes, Elsa B.'
'Rabaça, Sandra'
'Canadell, Enric'
'Almeida, Manuel'
_publ_section_title
;
 Bilayer Molecular Metals Based on Dissymmetrical Electron Donors.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6677
_journal_page_last               6679
_journal_paper_doi               10.1021/acs.inorgchem.5b01240
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C26 H14 I1.5 N2 S12'
_chemical_formula_weight         929.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.908(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.981(3)
_cell_length_b                   8.1197(8)
_cell_length_c                   13.6070(15)
_cell_measurement_reflns_used    5661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      2.93
_cell_volume                     3069.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17245
_diffrn_reflns_theta_full        23.71
_diffrn_reflns_theta_max         23.71
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    2.388
_exptl_absorpt_correction_T_max  0.9538
_exptl_absorpt_correction_T_min  0.7158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1822
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.565
_refine_diff_density_min         -2.085
_refine_diff_density_rms         0.368
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1493
_refine_ls_R_factor_gt           0.1329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1143P)²+2.3426P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3190
_refine_ls_wR_factor_ref         0.3285
_reflns_number_gt                3596
_reflns_number_total             4395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01240_si_004.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4343514--4343516.cif.'
_cod_original_cell_volume        3069.1(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C26 H14 I1.50 N2 S12'
_cod_database_code               4343514
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_group
I3 I 0.0000 0.5000 0.5000 0.012(9) Uiso 0.065(7) 2 d SP 1
I1 I 0.0000 0.0000 0.5000 0.0215(7) Uani 0.935(7) 2 d SP 2
I2 I -0.00142(6) 0.2675(2) 0.64388(13) 0.0359(6) Uani 1 1 d . .
S1 S 0.29567(19) 0.7751(7) 0.3288(4) 0.0185(12) Uani 1 1 d . .
S2 S 0.34554(19) 0.5314(7) 0.4683(4) 0.0197(12) Uani 1 1 d . .
S3 S 0.20600(18) 0.7777(7) 0.4553(4) 0.0191(12) Uani 1 1 d . .
S4 S 0.25329(19) 0.5272(6) 0.5906(4) 0.0187(12) Uani 1 1 d . .
S5 S 0.1199(2) 0.8138(8) 0.5596(5) 0.0303(15) Uani 1 1 d . .
S6 S 0.1751(2) 0.5039(8) 0.7165(4) 0.0269(14) Uani 1 1 d . .
S7 S 0.29354(19) 0.4577(7) 0.1179(4) 0.0197(12) Uani 1 1 d . .
S8 S 0.34277(19) 0.2164(7) 0.2587(4) 0.0200(12) Uani 1 1 d . .
S9 S 0.20377(19) 0.4663(7) 0.2435(4) 0.0205(12) Uani 1 1 d . .
S10 S 0.25231(18) 0.2336(6) 0.3865(4) 0.0170(12) Uani 1 1 d . .
S11 S 0.1096(2) 0.4436(9) 0.3126(6) 0.047(2) Uani 1 1 d . .
S12 S 0.1673(2) 0.1693(8) 0.4895(5) 0.0312(15) Uani 1 1 d . .
N1 N 0.4665(8) 0.837(2) 0.0782(14) 0.028(5) Uani 1 1 d . .
N2 N 0.4611(7) 0.497(3) -0.1420(13) 0.029(5) Uani 1 1 d . .
C1 C 0.4449(8) 0.779(3) 0.1351(17) 0.025(5) Uiso 1 1 d . .
C2 C 0.4227(8) 0.715(3) 0.2167(16) 0.020(5) Uiso 1 1 d . .
C3 C 0.4441(7) 0.596(3) 0.2798(14) 0.015(4) Uiso 1 1 d . .
H3 H 0.4744 0.5524 0.2679 0.018 Uiso 1 1 calc R .
C4 C 0.3757(7) 0.773(2) 0.2278(15) 0.015(4) Uiso 1 1 d . .
H4 H 0.3600 0.8494 0.1819 0.018 Uiso 1 1 calc R .
C5 C 0.4230(8) 0.538(3) 0.3594(16) 0.020(5) Uiso 1 1 d . .
H5 H 0.4386 0.4584 0.4037 0.024 Uiso 1 1 calc R .
C6 C 0.3530(7) 0.716(3) 0.3072(15) 0.015(4) Uiso 1 1 d . .
C7 C 0.3770(7) 0.601(3) 0.3719(15) 0.018(5) Uiso 1 1 d . .
C8 C 0.2936(7) 0.652(3) 0.4357(15) 0.017(5) Uiso 1 1 d . .
C9 C 0.2572(7) 0.657(2) 0.4873(15) 0.015(4) Uiso 1 1 d . .
C10 C 0.1759(9) 0.714(3) 0.5538(18) 0.029(6) Uiso 1 1 d . .
C11 C 0.1960(7) 0.600(2) 0.6151(14) 0.014(4) Uiso 1 1 d . .
C12 C 0.0907(8) 0.677(3) 0.6376(15) 0.020(5) Uiso 1 1 d . .
H12B H 0.0608 0.7299 0.6544 0.024 Uiso 1 1 calc R .
H12A H 0.0813 0.5750 0.6002 0.024 Uiso 1 1 calc R .
C13 C 0.1227(9) 0.630(3) 0.7354(19) 0.034(6) Uiso 1 1 d . .
H13B H 0.1028 0.5691 0.7786 0.041 Uiso 1 1 calc R .
H13A H 0.1340 0.7323 0.7703 0.041 Uiso 1 1 calc R .
C14 C 0.4421(7) 0.444(3) -0.0771(16) 0.019(5) Uiso 1 1 d . .
C15 C 0.4194(7) 0.389(3) 0.0049(15) 0.017(4) Uiso 1 1 d . .
C16 C 0.4409(7) 0.270(2) 0.0718(13) 0.007(4) Uiso 1 1 d . .
H16 H 0.4713 0.2261 0.0616 0.008 Uiso 1 1 calc R .
C17 C 0.3734(8) 0.450(3) 0.0147(16) 0.021(5) Uiso 1 1 d . .
H17 H 0.3581 0.5282 -0.0306 0.025 Uiso 1 1 calc R .
C18 C 0.4199(8) 0.218(3) 0.1492(16) 0.020(5) Uiso 1 1 d . .
H18 H 0.4356 0.1431 0.1961 0.024 Uiso 1 1 calc R .
C19 C 0.3507(7) 0.390(2) 0.0945(13) 0.009(4) Uiso 1 1 d . .
C20 C 0.3745(7) 0.277(2) 0.1583(14) 0.012(4) Uiso 1 1 d . .
C21 C 0.2932(7) 0.341(2) 0.2252(14) 0.014(4) Uiso 1 1 d . .
C22 C 0.2551(7) 0.345(3) 0.2766(15) 0.019(5) Uiso 1 1 d . .
C23 C 0.1690(7) 0.371(3) 0.3261(16) 0.019(5) Uiso 1 1 d . .
C24 C 0.1906(8) 0.274(3) 0.3912(16) 0.021(5) Uiso 1 1 d . .
C25 C 0.0838(9) 0.311(3) 0.3966(17) 0.028(5) Uiso 1 1 d . .
H25A H 0.0515 0.3533 0.4067 0.033 Uiso 1 1 calc R .
H25B H 0.0797 0.2000 0.3671 0.033 Uiso 1 1 calc R .
C26 C 0.1144(9) 0.299(3) 0.4958(18) 0.032(6) Uiso 1 1 d . .
H26A H 0.0948 0.2523 0.5450 0.039 Uiso 1 1 calc R .
H26B H 0.1249 0.4104 0.5183 0.039 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_1
_geom_angle_site_symmetry_3
I2 I3 I2 180.0 . 3_566
I2 I1 I2 180.0 3_556 .
I3 I2 I1 91.78(5) . .
C6 S1 C8 96.1(10) . .
C7 S2 C8 96.0(10) . .
C10 S3 C9 95.6(11) . .
C9 S4 C11 95.4(9) . .
C10 S5 C12 102.1(11) . .
C11 S6 C13 102.2(11) . .
C21 S7 C19 94.5(9) . .
C21 S8 C20 95.3(9) . .
C23 S9 C22 95.1(10) . .
C22 S10 C24 94.6(10) . .
C23 S11 C25 100.6(11) . .
C24 S12 C26 97.6(11) . .
N1 C1 C2 172(3) . .
C3 C2 C4 120.3(19) . .
C3 C2 C1 123(2) . .
C4 C2 C1 117.0(19) . .
C5 C3 C2 122.3(19) . .
C6 C4 C2 119.0(19) . .
C3 C5 C7 117(2) . .
C4 C6 C7 118.7(18) . .
C4 C6 S1 123.8(16) . .
C7 C6 S1 117.5(15) . .
C6 C7 C5 122.8(19) . .
C6 C7 S2 116.0(15) . .
C5 C7 S2 121.1(16) . .
C9 C8 S2 123.5(17) . .
C9 C8 S1 122.1(17) . .
S2 C8 S1 114.3(11) . .
C8 C9 S3 123.4(16) . .
C8 C9 S4 122.5(16) . .
S3 C9 S4 113.9(11) . .
C11 C10 S3 119.0(18) . .
C11 C10 S5 127.0(19) . .
S3 C10 S5 114.1(14) . .
C10 C11 S6 130.8(17) . .
C10 C11 S4 115.9(16) . .
S6 C11 S4 113.3(11) . .
C13 C12 S5 113.5(16) . .
C12 C13 S6 113.9(17) . .
N2 C14 C15 177(2) . .
C17 C15 C16 120.3(18) . .
C17 C15 C14 117.7(19) . .
C16 C15 C14 121.9(18) . .
C18 C16 C15 122.3(18) . .
C15 C17 C19 117.1(19) . .
C16 C18 C20 117(2) . .
C20 C19 C17 119.2(18) . .
C20 C19 S7 118.4(14) . .
C17 C19 S7 122.4(15) . .
C18 C20 C19 123.8(18) . .
C18 C20 S8 121.4(16) . .
C19 C20 S8 114.8(14) . .
C22 C21 S8 122.3(16) . .
C22 C21 S7 120.7(16) . .
S8 C21 S7 117.0(11) . .
C21 C22 S9 123.7(16) . .
C21 C22 S10 123.5(17) . .
S9 C22 S10 112.9(11) . .
C24 C23 S9 117.6(17) . .
C24 C23 S11 129.8(18) . .
S9 C23 S11 112.3(12) . .
C23 C24 S10 118.0(17) . .
C23 C24 S12 129.2(18) . .
S10 C24 S12 112.8(12) . .
C26 C25 S11 112.5(17) . .
C25 C26 S12 111.9(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I3 I2 2.7236(18) .
I3 I2 2.7236(18) 3_566
I1 I2 2.9274(18) 3_556
I1 I2 2.9274(18) .
S1 C6 1.73(2) .
S1 C8 1.77(2) .
S2 C7 1.76(2) .
S2 C8 1.77(2) .
S3 C10 1.74(2) .
S3 C9 1.75(2) .
S4 C9 1.77(2) .
S4 C11 1.78(2) .
S5 C10 1.78(2) .
S5 C12 1.80(2) .
S6 C11 1.75(2) .
S6 C13 1.83(3) .
S7 C21 1.74(2) .
S7 C19 1.757(19) .
S8 C21 1.73(2) .
S8 C20 1.79(2) .
S9 C23 1.75(2) .
S9 C22 1.76(2) .
S10 C22 1.76(2) .
S10 C24 1.77(2) .
S11 C23 1.75(2) .
S11 C25 1.78(2) .
S12 C24 1.77(2) .
S12 C26 1.83(3) .
N1 C1 1.14(3) .
N2 C14 1.17(3) .
C1 C2 1.43(3) .
C2 C3 1.38(3) .
C2 C4 1.42(3) .
C3 C5 1.38(3) .
C4 C6 1.40(3) .
C5 C7 1.42(3) .
C6 C7 1.40(3) .
C8 C9 1.31(3) .
C10 C11 1.32(3) .
C12 C13 1.56(3) .
C14 C15 1.42(3) .
C15 C17 1.40(3) .
C15 C16 1.41(3) .
C16 C18 1.34(3) .
C17 C19 1.41(3) .
C18 C20 1.38(3) .
C19 C20 1.38(3) .
C21 C22 1.34(3) .
C23 C24 1.28(3) .
C25 C26 1.51(3) .
