#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:19:54 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180178 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/74/7107476.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_7107476
loop_
_publ_author_name
'Pin-Shen Huang'
'Chih-Hong Kuo'
'Chang-Chih Hsieh'
'Yih-Chern Horng'
_publ_section_title
;
 Selective capture of volatile iodine using amorphous molecular organic
 solids
;
_journal_name_full               Chem.Commun.
_journal_page_first              3227
_journal_paper_doi               10.1039/c2cc17716a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C66 H72 N6 S6, I2'
_chemical_formula_sum            'C66 H72 I2 N6 S6'
_chemical_formula_weight         1395.46
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.583(3)
_cell_length_b                   17.583(3)
_cell_length_c                   48.345(10)
_cell_measurement_reflns_used    2293
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.26
_cell_measurement_theta_min      3.92
_cell_volume                     12944(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1459
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2548
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.8323
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.631
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0924
_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)+(0.1990P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2989
_refine_ls_wR_factor_ref         0.3261
_reflns_number_gt                1182
_reflns_number_total             2548
_reflns_threshold_expression     I>2σ
_cod_data_source_file            c2cc17716a.txt
_cod_data_source_block           1-I2
_cod_original_cell_volume        12943(4)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7107476
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
C1 C 0.6758(5) 0.9299(6) 0.2157(2) 0.102(3) Uani 1 1 d . . .
C2 C 0.5999(11) 0.9287(17) 0.2212(5) 0.125(8) Uani 0.60 1 d PD A 1
H2 H 0.5822 0.9255 0.2399 0.150 Uiso 0.60 1 calc PR A 1
C3 C 0.5424(11) 0.9322(9) 0.1989(5) 0.099(3) Uani 0.60 1 d PD A 1
H3 H 0.4936 0.9400 0.2025 0.119 Uiso 0.60 1 calc PR A 1
C2' C 0.5740(19) 0.885(3) 0.2240(7) 0.125(8) Uani 0.40 1 d PD A 2
H2' H 0.5499 0.8629 0.2418 0.150 Uiso 0.40 1 calc PR A 2
C3' C 0.5237(19) 0.8838(15) 0.1989(7) 0.099(3) Uani 0.40 1 d PD A 2
H3' H 0.4615 0.8563 0.1998 0.119 Uiso 0.40 1 calc PR A 2
C4 C 0.5670(7) 0.9231(7) 0.1736(2) 0.106(3) Uani 1 1 d . . .
H4 H 0.5265 0.9082 0.1588 0.127 Uiso 1 1 calc R A 1
C5 C 0.6464(5) 0.9342(5) 0.16844(18) 0.087(2) Uani 1 1 d . A .
H5 H 0.6644 0.9388 0.1497 0.104 Uiso 1 1 calc R . .
C6 C 0.7050(5) 0.9394(5) 0.18917(18) 0.079(2) Uani 1 1 d . A .
C7 C 0.8186(5) 0.9610(5) 0.15680(16) 0.084(2) Uani 1 1 d . A .
H7A H 0.8137 1.0077 0.1469 0.101 Uiso 1 1 calc R . .
H7B H 0.7827 0.9052 0.1467 0.101 Uiso 1 1 calc R . .
C8 C 0.9131(5) 0.9830(5) 0.15680(14) 0.0730(19) Uani 1 1 d . . .
C9 C 0.9328(5) 0.9112(5) 0.15583(16) 0.080(2) Uani 1 1 d . . .
C10 C 0.8577(5) 0.8193(5) 0.15820(18) 0.091(2) Uani 1 1 d . . .
H10A H 0.8762 0.7845 0.1695 0.110 Uiso 1 1 calc R . .
H10B H 0.8087 0.8202 0.1680 0.110 Uiso 1 1 calc R . .
C11 C 0.8270(8) 0.7772(9) 0.1322(3) 0.164(5) Uani 1 1 d . . .
H11A H 0.7760 0.7186 0.1350 0.246 Uiso 1 1 calc R . .
H11B H 0.8738 0.7717 0.1230 0.246 Uiso 1 1 calc R . .
H11C H 0.8102 0.8121 0.1206 0.246 Uiso 1 1 calc R . .
N1 N 0.7852(4) 0.9526(4) 0.18383(13) 0.0835(18) Uani 1 1 d . . .
H1 H 0.8188 0.9562 0.1978 0.100 Uiso 1 1 calc R A .
S2 S 0.74430(18) 0.9360(2) 0.24422(5) 0.1215(10) Uani 1 1 d . . .
I1 I 0.0000 0.0000 0.22287(2) 0.1141(7) Uani 1 3 d S . .
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'
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'
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
C2 C1 C6 119.7(11) . .
C6 C1 C2' 123.8(14) . .
C2 C1 S2 118.5(12) . .
C6 C1 S2 121.0(6) . .
C2' C1 S2 112.7(12) . .
C1 C2 C3 122.7(18) . .
C1 C2 H2 118.6 . .
C3 C2 H2 118.6 . .
C4 C3 C2 112.8(17) . .
C4 C3 H3 123.6 . .
C2 C3 H3 123.6 . .
C3' C2' C1 108(2) . .
C3' C2' H2' 126.0 . .
C1 C2' H2' 126.0 . .
C4 C3' C2' 121(2) . .
C4 C3' H3' 119.3 . .
C2' C3' H3' 119.3 . .
C3 C4 C5 122.2(11) . .
C5 C4 C3' 119.9(13) . .
C3 C4 H4 118.9 . .
C5 C4 H4 118.9 . .
C3' C4 H4 111.7 . .
C4 C5 C6 123.7(8) . .
C4 C5 H5 118.1 . .
C6 C5 H5 118.1 . .
N1 C6 C1 120.3(8) . .
N1 C6 C5 123.3(8) . .
C1 C6 C5 116.4(7) . .
N1 C7 C8 112.0(6) . .
N1 C7 H7A 109.2 . .
C8 C7 H7A 109.2 . .
N1 C7 H7B 109.2 . .
C8 C7 H7B 109.2 . .
H7A C7 H7B 107.9 . .
C9 C8 C9 120.4(8) 3_675 .
C9 C8 C7 120.5(7) 3_675 .
C9 C8 C7 118.9(7) . .
C8 C9 C8 119.3(8) 2_765 .
C8 C9 C10 122.2(7) 2_765 .
C8 C9 C10 117.8(7) . .
C11 C10 C9 113.3(8) . .
C11 C10 H10A 108.9 . .
C9 C10 H10A 108.9 . .
C11 C10 H10B 108.9 . .
C9 C10 H10B 108.9 . .
H10A C10 H10B 107.7 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C6 N1 C7 123.1(6) . .
C6 N1 H1 118.5 . .
C7 N1 H1 118.5 . .
C1 S2 S2 105.2(3) . 5_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.35(2) .
C1 C6 1.360(12) .
C1 C2' 1.60(3) .
C1 S2 1.798(8) .
C2 C3 1.498(16) .
C2 H2 0.9500 .
C3 C4 1.33(2) .
C3 H3 0.9500 .
C2' C3' 1.499(16) .
C2' H2' 0.9500 .
C3' C4 1.42(3) .
C3' H3' 0.9500 .
C4 C5 1.334(11) .
C4 H4 0.9500 .
C5 C6 1.407(11) .
C5 H5 0.9500 .
C6 N1 1.334(9) .
C7 N1 1.410(10) .
C7 C8 1.507(10) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.345(10) 3_675
C8 C9 1.467(10) .
C9 C8 1.346(10) 2_765
C9 C10 1.495(10) .
C10 C11 1.421(14) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
N1 H1 0.8800 .
S2 S2 2.027(7) 5_675
I1 I1 2.623(2) 4
