#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/82/7108229.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_7108229
loop_
_publ_author_name
'Yih-Chern Horng'
'Pin-Shen Huang'
'Chang-Chih Hsieh'
'Chih-Hong Kuo'
'Ting-Shen Kuo'
_publ_section_title
;
 Selective encapsulation of volatile and reactive methyl iodide
;
_journal_name_full               Chem.Commun.
_journal_page_first              8844
_journal_paper_doi               10.1039/c2cc34346k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C67 H75 I1 N6 S6'
_chemical_formula_sum            'C67 H75 I N6 S6'
_chemical_formula_weight         1283.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_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                   17.8042(2)
_cell_length_b                   17.8042(2)
_cell_length_c                   47.6257(12)
_cell_measurement_reflns_used    4626
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.508
_cell_measurement_theta_min      2.623
_cell_volume                     13074.3(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX2'
_diffrn_measurement_method       'phi and omega 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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            26581
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.8938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2003 '
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4476
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_platon_squeeze_details
; 
?
;
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0744
_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)+(0.1618P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2291
_refine_ls_wR_factor_ref         0.2543
_reflns_number_gt                1320
_reflns_number_total             2580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34346k.txt
_cod_data_source_block           Compd1-MeI
_cod_original_cell_volume        13074.2(4)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C67 H75 I1 N6 S6'
_cod_database_code               7108229
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
C1 C 0.3437(3) 0.0779(3) 0.04889(11) 0.0749(14) Uani 1 1 d .
C2 C 0.2645(4) 0.0101(5) 0.05406(15) 0.120(2) Uani 1 1 d .
H2 H 0.2430 -0.0020 0.0727 0.144 Uiso 1 1 calc R
C3 C 0.2133(4) -0.0428(4) 0.03188(16) 0.131(3) Uani 1 1 d .
H3 H 0.1598 -0.0939 0.0358 0.157 Uiso 1 1 calc R
C4 C 0.2396(3) -0.0212(3) 0.00512(13) 0.0917(16) Uani 1 1 d .
H4 H 0.2031 -0.0544 -0.0100 0.110 Uiso 1 1 calc R
C5 C 0.3194(3) 0.0488(3) -0.00006(11) 0.0802(14) Uani 1 1 d .
H5 H 0.3383 0.0631 -0.0190 0.096 Uiso 1 1 calc R
C6 C 0.3737(3) 0.0998(3) 0.02139(11) 0.0671(12) Uani 1 1 d .
C7 C 0.4871(3) 0.1915(3) -0.01140(9) 0.0687(13) Uani 1 1 d .
H7A H 0.4502 0.2100 -0.0214 0.082 Uiso 1 1 calc R
H7B H 0.4837 0.1416 -0.0217 0.082 Uiso 1 1 calc R
C8 C 0.5802(3) 0.2655(3) -0.01118(9) 0.0618(11) Uani 1 1 d .
C9 C 0.5981(3) 0.3513(3) -0.01080(9) 0.0627(12) Uani 1 1 d .
C10 C 0.5249(3) 0.3710(3) -0.00886(11) 0.0810(15) Uani 1 1 d .
H10A H 0.4764 0.3238 0.0017 0.097 Uiso 1 1 calc R
H10B H 0.5453 0.4253 0.0019 0.097 Uiso 1 1 calc R
C11 C 0.4935(4) 0.3801(5) -0.03509(16) 0.133(2) Uani 1 1 d .
H11A H 0.4475 0.3943 -0.0322 0.199 Uiso 1 1 calc R
H11B H 0.4702 0.3256 -0.0456 0.199 Uiso 1 1 calc R
H11C H 0.5410 0.4268 -0.0458 0.199 Uiso 1 1 calc R
I1 I 0.6667 0.3333 0.0617 0.0854(5) Uani 0.50 3 d SP
C12 C 0.6667 0.3333 0.1058 0.0854(5) Uani 0.50 3 d SP
H12' H 0.6410 0.2780 0.1140 0.102 Uiso 1 1 d R
N1 N 0.4555(2) 0.1657(2) 0.01632(8) 0.0799(12) Uani 1 1 d .
H1 H 0.4898 0.1931 0.0306 0.096 Uiso 1 1 calc R
S1 S 0.41206(10) 0.14211(9) 0.07746(3) 0.0939(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'
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'
O O 0.0106 0.0060 '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 120.4(5) . .
C2 C1 S1 120.3(5) . .
C6 C1 S1 119.3(3) . .
C1 C2 C3 120.2(6) . .
C1 C2 H2 119.9 . .
C3 C2 H2 119.9 . .
C4 C3 C2 120.2(6) . .
C4 C3 H3 119.9 . .
C2 C3 H3 119.9 . .
C3 C4 C5 119.1(5) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C4 C5 C6 122.1(5) . .
C4 C5 H5 119.0 . .
C6 C5 H5 119.0 . .
N1 C6 C5 122.0(5) . .
N1 C6 C1 120.2(4) . .
C5 C6 C1 117.7(4) . .
N1 C7 C8 111.0(4) . .
N1 C7 H7A 109.4 . .
C8 C7 H7A 109.4 . .
N1 C7 H7B 109.4 . .
C8 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
C9 C8 C9 120.4(4) . 2_655
C9 C8 C7 120.1(4) . .
C9 C8 C7 119.4(4) 2_655 .
C8 C9 C8 119.6(4) . 3_665
C8 C9 C10 120.2(4) . .
C8 C9 C10 120.2(4) 3_665 .
C11 C10 C9 114.1(5) . .
C11 C10 H10A 108.7 . .
C9 C10 H10A 108.7 . .
C11 C10 H10B 108.7 . .
C9 C10 H10B 108.7 . .
H10A C10 H10B 107.6 . .
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 . .
I1 I1 C12 0.0 16_544 .
I1 C12 I1 0.1 16_544 .
I1 C12 H12' 114.5 16_544 .
I1 C12 H12' 114.6 . .
C6 N1 C7 121.6(4) . .
C6 N1 H1 119.2 . .
C7 N1 H1 119.2 . .
C1 S1 S1 103.98(17) . 16_544
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.344(7) .
C1 C6 1.394(6) .
C1 S1 1.802(5) .
C2 C3 1.406(8) .
C2 H2 0.9500 .
C3 C4 1.346(8) .
C3 H3 0.9500 .
C4 C5 1.364(6) .
C4 H4 0.9500 .
C5 C6 1.388(6) .
C5 H5 0.9500 .
C6 N1 1.360(5) .
C7 N1 1.418(5) .
C7 C8 1.517(5) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.397(6) .
C8 C9 1.416(6) 2_655
C9 C8 1.416(6) 3_665
C9 C10 1.512(6) .
C10 C11 1.411(7) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
I1 I1 2.0637 16_544
I1 C12 2.1015 .
C12 I1 0.0378 16_544
C12 H12' 0.9391 .
N1 H1 0.8800 .
S1 S1 2.033(3) 16_544
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.145 -0.141 -0.001 4525.1 836.3
