#------------------------------------------------------------------------------
#$Date: 2017-02-04 04:15:47 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191350 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/49/4344975.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_4344975
loop_
_publ_author_name
'Evans, Hayden A.'
'Labram, John G.'
'Smock, Sara R.'
'Wu, Guang'
'Chabinyc, Michael L.'
'Seshadri, Ram'
'Wudl, Fred'
_publ_section_title
;
 Mono- and Mixed-Valence Tetrathiafulvalene Semiconductors (TTF)BiI4 and
 (TTF)4BiI6 with 1D and 0D Bismuth-Iodide Networks.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              395
_journal_page_last               401
_journal_paper_doi               10.1021/acs.inorgchem.6b02287
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C24 H16 Bi I6 S16'
_chemical_formula_weight         1787.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                84.283(15)
_cell_angle_beta                 80.45(2)
_cell_angle_gamma                85.85(3)
_cell_formula_units_Z            1
_cell_length_a                   10.237(8)
_cell_length_b                   10.460(5)
_cell_length_c                   11.166(8)
_cell_measurement_reflns_used    695
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.35
_cell_volume                     1171.3(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10557
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.644
_diffrn_reflns_theta_min         1.857
_exptl_absorpt_coefficient_mu    8.449
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             817
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.396
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0728P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3121
_reflns_number_total             4839
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02287_si_003.cif
_cod_data_source_block           hae_135_0m
_cod_depositor_comments          'Adding full bibliography for 4344975.cif.'
_cod_original_cell_volume        1171.4(14)
_cod_database_code               4344975
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Bi01 Bi 0.0000 0.5000 1.0000 0.0319(2) Uani 1 2 d S . P
I002 I 0.02862(9) 0.49708(8) 0.71686(8) 0.0430(3) Uani 1 1 d . . .
I003 I 0.21742(9) 0.27187(9) 0.99841(9) 0.0487(3) Uani 1 1 d . . .
I004 I 0.20541(10) 0.70942(10) 0.96746(9) 0.0529(3) Uani 1 1 d . . .
S005 S 0.5733(4) 0.6703(4) 0.2987(3) 0.0477(9) Uani 1 1 d . . .
S006 S 0.9784(4) 0.8363(3) 0.3983(4) 0.0460(9) Uani 1 1 d . . .
S007 S 0.6885(4) 0.6500(4) 0.5555(4) 0.0485(9) Uani 1 1 d . . .
S008 S 0.4128(4) 0.6536(3) 0.6875(3) 0.0455(9) Uani 1 1 d . . .
S009 S 0.2988(4) 0.6688(4) 0.4330(4) 0.0471(9) Uani 1 1 d . . .
S00A S 1.0102(4) 1.1087(4) 0.3209(4) 0.0586(11) Uani 1 1 d . . .
S00B S 0.6521(5) -0.0008(4) 0.3352(5) 0.0780(15) Uani 1 1 d . . .
S00C S 0.3563(5) 0.0125(4) 0.3704(6) 0.0798(15) Uani 1 1 d . . .
C00D C 0.9862(14) 0.8838(14) 0.2472(14) 0.053(4) Uani 1 1 d . . .
H00D H 0.9812 0.8242 0.1918 0.063 Uiso 1 1 calc R U .
C00E C 0.6655(15) 0.6485(13) 0.7101(14) 0.052(4) Uani 1 1 d . . .
H00E H 0.7381 0.6476 0.7505 0.062 Uiso 1 1 calc R U .
C5 C 0.3172(15) 0.6845(14) 0.2766(14) 0.053(4) Uani 1 1 d . . .
H5 H 0.2441 0.6950 0.2362 0.063 Uiso 1 1 calc R U .
C4 C 0.4429(13) 0.6810(14) 0.2146(13) 0.052(4) Uani 1 1 d . . .
H4 H 0.4592 0.6842 0.1299 0.062 Uiso 1 1 calc R U .
C3 C 0.4667(13) 0.6638(12) 0.4393(13) 0.042(3) Uani 1 1 d . . .
C2 C 0.5185(12) 0.6556(11) 0.5480(12) 0.036(3) Uani 1 1 d . . .
C1 C 0.5411(15) 0.6486(13) 0.7738(14) 0.051(4) Uani 1 1 d . . .
H1 H 0.5247 0.6461 0.8584 0.061 Uiso 1 1 calc R U .
C7 C 0.443(2) 0.0201(16) 0.2174(18) 0.073(5) Uani 1 1 d . . .
H7 H 0.3993 0.0280 0.1503 0.088 Uiso 1 1 calc R U .
C6 C 0.578(2) 0.0134(17) 0.205(2) 0.090(6) Uani 1 1 d . . .
H6 H 0.6293 0.0164 0.1286 0.108 Uiso 1 1 calc R U .
C8 C 0.9960(13) 0.9888(12) 0.4401(12) 0.042(3) Uani 1 1 d . . .
C9 C 0.9996(15) 1.0066(16) 0.2098(16) 0.061(4) Uani 1 1 d . . .
H9 H 1.0032 1.0369 0.1282 0.073 Uiso 1 1 calc R U .
C10 C 0.5011(16) 0.0042(15) 0.4399(16) 0.068(6) 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'
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'
Bi Bi -4.1077 10.2566 '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
I004 Bi01 I004 180.0 2_567 .
I004 Bi01 I002 90.41(3) 2_567 2_567
I004 Bi01 I002 89.59(3) . 2_567
I004 Bi01 I002 89.59(3) 2_567 .
I004 Bi01 I002 90.41(3) . .
I002 Bi01 I002 180.0 2_567 .
I004 Bi01 I003 93.58(6) 2_567 2_567
I004 Bi01 I003 86.42(6) . 2_567
I002 Bi01 I003 88.20(3) 2_567 2_567
I002 Bi01 I003 91.80(3) . 2_567
I004 Bi01 I003 86.42(6) 2_567 .
I004 Bi01 I003 93.58(6) . .
I002 Bi01 I003 91.80(3) 2_567 .
I002 Bi01 I003 88.20(3) . .
I003 Bi01 I003 180.0 2_567 .
C4 S005 C3 93.4(7) . .
C00D S006 C8 94.9(7) . .
C00E S007 C2 94.2(7) . .
C2 S008 C1 94.5(7) . .
C5 S009 C3 95.3(7) . .
C8 S00A C9 94.9(7) . .
C6 S00B C10 95.5(10) . .
C10 S00C C7 95.3(9) . .
C9 C00D S006 118.9(13) . .
C9 C00D H00D 120.5 . .
S006 C00D H00D 120.5 . .
C1 C00E S007 119.6(12) . .
C1 C00E H00E 120.2 . .
S007 C00E H00E 120.2 . .
C4 C5 S009 117.0(12) . .
C4 C5 H5 121.5 . .
S009 C5 H5 121.5 . .
C5 C4 S005 117.9(12) . .
C5 C4 H4 121.0 . .
S005 C4 H4 121.0 . .
C2 C3 S009 123.6(10) . .
C2 C3 S005 120.2(10) . .
S009 C3 S005 116.2(8) . .
C3 C2 S008 120.3(10) . .
C3 C2 S007 123.9(10) . .
S008 C2 S007 115.7(8) . .
C00E C1 S008 116.0(12) . .
C00E C1 H1 122.0 . .
S008 C1 H1 122.0 . .
C6 C7 S00C 115.6(16) . .
C6 C7 H7 122.2 . .
S00C C7 H7 122.2 . .
C7 C6 S00B 119.4(17) . .
C7 C6 H6 120.3 . .
S00B C6 H6 120.3 . .
C8 C8 S00A 122.9(12) 2_776 .
C8 C8 S006 122.3(12) 2_776 .
S00A C8 S006 114.7(8) . .
C00D C9 S00A 116.5(13) . .
C00D C9 H9 121.7 . .
S00A C9 H9 121.7 . .
C10 C10 S00B 122.1(18) 2_656 .
C10 C10 S00C 123.8(17) 2_656 .
S00B C10 S00C 114.1(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi01 I004 3.0995(18) 2_567
Bi01 I004 3.0995(18) .
Bi01 I002 3.129(3) 2_567
Bi01 I002 3.129(3) .
Bi01 I003 3.1426(19) 2_567
Bi01 I003 3.1427(18) .
S005 C4 1.746(15) .
S005 C3 1.755(14) .
S006 C00D 1.701(16) .
S006 C8 1.735(13) .
S007 C00E 1.702(16) .
S007 C2 1.753(13) .
S008 C2 1.743(13) .
S008 C1 1.748(15) .
S009 C5 1.718(16) .
S009 C3 1.729(14) .
S00A C8 1.731(12) .
S00A C9 1.736(17) .
S00B C6 1.73(2) .
S00B C10 1.778(17) .
S00C C10 1.777(18) .
S00C C7 1.79(2) .
C00D C9 1.32(2) .
C00D H00D 0.9300 .
C00E C1 1.35(2) .
C00E H00E 0.9300 .
C5 C4 1.357(19) .
C5 H5 0.9300 .
C4 H4 0.9300 .
C3 C2 1.396(19) .
C1 H1 0.9300 .
C7 C6 1.36(3) .
C7 H7 0.9300 .
C6 H6 0.9300 .
C8 C8 1.40(3) 2_776
C9 H9 0.9300 .
C10 C10 1.33(4) 2_656
