#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/60/7116074.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_7116074
loop_
_publ_author_name
'Simon A. Herbert'
'Agnieszka Janiak'
'Praveen K. Thallapally'
'Jerry L. Atwood'
'Leonard J. Barbour'
_publ_section_title
;
 Diffusion of vaporous guests into a seemingly non-porous organic crystal
;
_journal_name_full               Chem.Commun.
_journal_page_first              15509
_journal_paper_doi               10.1039/C4cc07366E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C88 H113 I0.8 O9 S8'
_chemical_formula_weight         1672.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           113
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.523(2)
_cell_length_b                   19.523(2)
_cell_length_c                   11.9511(12)
_cell_measurement_reflns_used    7175
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      1.48
_cell_volume                     4555.1(8)
_computing_cell_refinement       'APEX2 v2012.10-0 (Bruker AXS, 2005-2012)'
_computing_data_collection       'APEX2 v2012.10-0 (Bruker AXS, 2005-2012)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28814
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         1.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1767
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.674
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0611
_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)+(0.1130P)²+5.0112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1841
_reflns_number_gt                4767
_reflns_number_total             5509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07366e3.cif
_cod_data_source_block           TBC_wet_I2
_cod_original_cell_volume        4555.1(10)
_cod_original_formula_sum        'C88 H113 I0.80 O9 S8'
_cod_database_code               7116074
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.45630(4) 0.69550(4) 0.48960(8) 0.0192(2) Uani 1 1 d . . .
C1 C 0.38600(16) 0.57314(16) 0.5106(3) 0.0186(7) Uani 1 1 d . . .
C2 C 0.41205(17) 0.63071(17) 0.5639(3) 0.0182(7) Uani 1 1 d . . .
C3 C 0.39857(18) 0.64240(17) 0.6773(3) 0.0204(7) Uani 1 1 d . . .
H3 H 0.4159 0.6826 0.7120 0.024 Uiso 1 1 calc R . .
C4 C 0.36001(18) 0.59601(18) 0.7406(3) 0.0207(7) Uani 1 1 d . . .
C5 C 0.33577(17) 0.53772(18) 0.6869(3) 0.0195(7) Uani 1 1 d . . .
H5 H 0.3104 0.5049 0.7286 0.023 Uiso 1 1 calc R . .
C6 C 0.34778(18) 0.52623(17) 0.5733(3) 0.0183(7) Uani 1 1 d . . .
C7 C 0.3486(2) 0.6101(2) 0.8651(3) 0.0309(9) Uani 1 1 d . . .
C8 C 0.3137(4) 0.6808(3) 0.8783(5) 0.0650(19) Uani 1 1 d . . .
H8A H 0.3431 0.7163 0.8459 0.097 Uiso 1 1 calc R . .
H8B H 0.3064 0.6904 0.9579 0.097 Uiso 1 1 calc R . .
H8C H 0.2695 0.6805 0.8394 0.097 Uiso 1 1 calc R . .
C9 C 0.3016(2) 0.5565(2) 0.9172(3) 0.0309(9) Uani 1 1 d . . .
H9A H 0.2953 0.5667 0.9968 0.046 Uiso 1 1 calc R . .
H9B H 0.3223 0.5110 0.9090 0.046 Uiso 1 1 calc R . .
H9C H 0.2571 0.5574 0.8793 0.046 Uiso 1 1 calc R . .
C10 C 0.4167(3) 0.6090(4) 0.9258(4) 0.0640(19) Uani 1 1 d . . .
H10A H 0.4377 0.5637 0.9179 0.096 Uiso 1 1 calc R . .
H10B H 0.4094 0.6189 1.0053 0.096 Uiso 1 1 calc R . .
H10C H 0.4471 0.6437 0.8936 0.096 Uiso 1 1 calc R . .
O1 O 0.39947(14) 0.56078(14) 0.4001(2) 0.0257(6) Uani 1 1 d . . .
C11 C 0.3523(2) 0.5912(2) 0.3236(4) 0.0377(10) Uani 1 1 d . . .
H11A H 0.3534 0.6411 0.3321 0.057 Uiso 1 1 calc R . .
H11B H 0.3059 0.5745 0.3394 0.057 Uiso 1 1 calc R . .
H11C H 0.3650 0.5790 0.2469 0.057 Uiso 1 1 calc R . .
S2 S 0.50001(4) 0.79912(4) 0.80952(7) 0.0191(2) Uani 1 1 d . . .
C12 C 0.40205(16) 0.90205(16) 0.8198(4) 0.0173(9) Uani 1 2 d SD B .
C13 C 0.43954(17) 0.85231(17) 0.8784(3) 0.0183(7) Uani 1 1 d . . .
C14 C 0.42494(18) 0.83829(17) 0.9884(3) 0.0216(7) Uani 1 1 d . . .
H14 H 0.4510 0.8044 1.0265 0.026 Uiso 1 1 calc R . .
C15 C 0.37263(19) 0.87263(19) 1.0460(4) 0.0213(10) Uani 1 2 d S A .
C16 C 0.3557(3) 0.8557(3) 1.1684(5) 0.0338(14) Uani 1 2 d S . .
C17 C 0.2983(5) 0.8949(5) 1.2160(7) 0.037(2) Uani 0.50 1 d P A -1
H17A H 0.2552 0.8790 1.1830 0.056 Uiso 0.50 1 calc PR A -1
H17B H 0.3045 0.9437 1.1994 0.056 Uiso 0.50 1 calc PR A -1
H17C H 0.2970 0.8882 1.2972 0.056 Uiso 0.50 1 calc PR A -1
C18 C 0.3351(7) 0.7749(5) 1.1735(8) 0.056(3) Uani 0.50 1 d P A -1
H18A H 0.3759 0.7469 1.1593 0.085 Uiso 0.50 1 calc PR A -1
H18B H 0.3004 0.7651 1.1166 0.085 Uiso 0.50 1 calc PR A -1
H18C H 0.3168 0.7641 1.2478 0.085 Uiso 0.50 1 calc PR A -1
C19 C 0.4221(5) 0.8667(7) 1.2379(7) 0.057(3) Uani 0.50 1 d P A -1
H19A H 0.4125 0.8577 1.3171 0.085 Uiso 0.50 1 calc PR A -1
H19B H 0.4379 0.9140 1.2289 0.085 Uiso 0.50 1 calc PR A -1
H19C H 0.4577 0.8352 1.2116 0.085 Uiso 0.50 1 calc PR A -1
O2 O 0.41535(14) 0.91535(14) 0.7091(3) 0.0244(8) Uani 1 2 d SD . .
C20 C 0.3761(3) 0.8761(3) 0.6338(5) 0.0340(17) Uani 0.80 2 d SPD B 1
H20A H 0.3882 0.8882 0.5568 0.051 Uiso 0.80 2 d SPR B 1
H20B H 0.3274 0.8852 0.6463 0.051 Uiso 0.80 1 d PR B 1
C30 C 0.4646(13) 0.9646(13) 0.681(5) 0.14(3) Uiso 0.20 2 d SPD . .
H30A H 0.4812 0.9797 0.7512 0.213 Uiso 0.20 2 d SPR . .
H30B H 0.5019 0.9477 0.6390 0.213 Uiso 0.20 1 d PR . .
C21 C 0.59608(17) 0.90392(17) 0.7989(4) 0.0189(10) Uani 1 2 d SD . .
C22 C 0.55772(17) 0.85546(18) 0.7402(3) 0.0198(7) Uani 1 1 d . C .
C23 C 0.5710(3) 0.8430(4) 0.6309(5) 0.0261(13) Uani 0.80 1 d PD C 1
H23 H 0.5448 0.8093 0.5928 0.031 Uiso 0.80 1 calc PR C 1
C24 C 0.6220(5) 0.8780(5) 0.5723(7) 0.038(2) Uani 0.80 2 d SPDU C 1
C25 C 0.6357(5) 0.8643(5) 0.4469(7) 0.065(3) Uani 0.80 2 d SPDU C 1
C26 C 0.5632(9) 0.8600(10) 0.3875(14) 0.064(4) Uani 0.40 1 d PDU C 1
H26A H 0.5410 0.9039 0.3892 0.096 Uiso 0.40 1 d PR C 1
H26B H 0.5703 0.8464 0.3112 0.096 Uiso 0.40 1 d PR C 1
H26C H 0.5349 0.8268 0.4245 0.096 Uiso 0.40 1 d PR C 1
C27 C 0.6671(7) 0.7914(7) 0.4400(10) 0.070(4) Uani 0.40 1 d PDU C 1
H27A H 0.7109 0.7891 0.4764 0.104 Uiso 0.40 2 d SPR C 1
H27B H 0.6372 0.7595 0.4767 0.104 Uiso 0.40 1 d PR C 1
H27C H 0.6726 0.7783 0.3631 0.104 Uiso 0.40 1 d PR C 1
C37 C 0.6540(13) 0.9337(15) 0.371(3) 0.029(7) Uiso 0.20 1 d PD C 2
H37A H 0.6435 0.9383 0.2916 0.043 Uiso 0.20 1 calc PR C 2
H37B H 0.6927 0.9023 0.3811 0.043 Uiso 0.20 1 calc PR C 2
H37C H 0.6659 0.9787 0.4022 0.043 Uiso 0.20 1 calc PR C 2
O3 O 0.5824(3) 0.9176(3) 0.9107(6) 0.0251(15) Uani 0.80 2 d SPD D 1
C29 C 0.6225(4) 0.8775(4) 0.9859(7) 0.045(2) Uani 0.80 2 d SPD D 1
H29A H 0.6110 0.8891 1.0616 0.067 Uiso 0.80 2 d SPR D 1
H29B H 0.6134 0.8293 0.9732 0.067 Uiso 0.80 1 d PR D 1
O30 O 0.5964(9) 0.9036(9) 0.911(3) 0.018(8) Uiso 0.20 2 d SPD D 2
C39 C 0.6441(14) 0.8559(14) 0.961(3) 0.066(17) Uiso 0.20 2 d SPD D 2
H39A H 0.6427 0.8574 1.0412 0.099 Uiso 0.20 2 d SPR D 2
H39B H 0.6326 0.8086 0.9357 0.099 Uiso 0.20 1 d PR D 2
I1 I 0.32526(13) 0.82526(13) 0.5838(3) 0.0669(8) Uani 0.20 2 d SP . .
I2 I 0.23709(15) 0.73709(15) 0.4884(4) 0.0874(10) Uani 0.20 2 d SP . .
O1W O 0.5000 1.0000 1.0617(16) 0.074(5) Uani 0.50 4 d SP . .
O2W O 0.5000 0.5000 0.7579(14) 0.034(3) Uani 0.25 2 d SP . .
C34 C 0.6044(9) 0.8956(9) 0.558(2) 0.009(6) Uiso 0.20 2 d SPD C 2
C33 C 0.5550(10) 0.8573(10) 0.6189(16) 0.001(4) Uiso 0.20 1 d PD C 2
H33 H 0.5201 0.8330 0.5803 0.002 Uiso 0.20 1 calc PR C 2
C35 C 0.5936(10) 0.9064(10) 0.431(2) 0.037(7) Uiso 0.20 2 d SPD C 2
C36 C 0.5375(10) 0.9625(10) 0.420(4) 0.098(18) Uiso 0.20 2 d SPD C 2
H36A H 0.5297 0.9703 0.3419 0.147 Uiso 0.40 2 d SPR C 2
H36B H 0.4957 0.9470 0.4547 0.147 Uiso 0.10 1 d PR C 2
C28 C 0.6795(10) 0.9116(10) 0.3904(12) 0.078(5) Uani 0.40 1 d PDU C 1
H28A H 0.7216 0.9128 0.4318 0.117 Uiso 0.40 1 d PR C 1
H28B H 0.6882 0.8948 0.3162 0.117 Uiso 0.40 1 d PR C 1
H28C H 0.6607 0.9570 0.3860 0.117 Uiso 0.40 1 d PR C 1
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'
O O 0.0106 0.0060 '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 S1 C6 104.35(16) . 2_566
O1 C1 C2 121.0(3) . .
O1 C1 C6 120.2(3) . .
C2 C1 C6 118.7(3) . .
C1 C2 C3 120.5(3) . .
C1 C2 S1 121.8(3) . .
C3 C2 S1 117.5(3) . .
C2 C3 C4 121.3(3) . .
C5 C4 C3 117.6(3) . .
C5 C4 C7 123.2(3) . .
C3 C4 C7 119.2(3) . .
C4 C5 C6 121.6(3) . .
C5 C6 C1 120.3(3) . .
C5 C6 S1 117.1(3) . 4_656
C1 C6 S1 122.1(3) . 4_656
C10 C7 C9 108.8(4) . .
C10 C7 C4 109.7(4) . .
C9 C7 C4 111.2(3) . .
C10 C7 C8 110.5(5) . .
C9 C7 C8 107.8(4) . .
C4 C7 C8 108.9(4) . .
C1 O1 C11 114.9(3) . .
C13 S2 C22 105.99(17) . .
O2 C12 C13 120.9(2) . 8_455
O2 C12 C13 120.9(2) . .
C13 C12 C13 118.1(4) 8_455 .
C14 C13 C12 120.5(3) . .
C14 C13 S2 117.8(3) . .
C12 C13 S2 121.3(3) . .
C13 C14 C15 121.8(3) . .
C14 C15 C14 117.1(5) . 8_455
C14 C15 C16 121.4(2) . .
C14 C15 C16 121.4(2) 8_455 .
C17 C16 C15 114.8(4) . .
C17 C16 C15 114.8(4) 8_455 .
C17 C16 C19 110.9(7) . .
C15 C16 C19 107.5(6) . .
C17 C16 C19 110.9(7) 8_455 8_455
C15 C16 C19 107.5(6) . 8_455
C17 C16 C18 107.5(7) 8_455 8_455
C15 C16 C18 107.3(5) . 8_455
C19 C16 C18 145.2(7) . 8_455
C19 C16 C18 108.6(7) 8_455 8_455
C17 C16 C18 107.5(7) . .
C15 C16 C18 107.3(5) . .
C19 C16 C18 108.6(7) . .
C30 O2 C12 120(2) . .
C30 O2 C20 126(2) . .
C12 O2 C20 114.2(5) . .
O30 C21 C22 120.1(3) . 7_665
O3 C21 C22 120.7(2) . 7_665
O30 C21 C22 120.1(3) . .
O3 C21 C22 120.7(2) . .
C22 C21 C22 118.4(5) 7_665 .
C23 C22 C21 120.3(4) . .
C21 C22 C33 120.3(9) . .
C23 C22 S2 117.3(3) . .
C21 C22 S2 121.7(3) . .
C33 C22 S2 117.2(9) . .
C22 C23 C24 122.2(5) . .
C23 C24 C23 116.5(8) 7_665 .
C23 C24 C25 121.7(4) 7_665 .
C23 C24 C25 121.7(4) . .
C28 C25 C24 116.7(7) 7_665 .
C28 C25 C24 116.7(7) . .
C28 C25 C27 109.3(11) . .
C24 C25 C27 106.2(9) . .
C28 C25 C27 109.3(11) 7_665 7_665
C24 C25 C27 106.2(9) . 7_665
C28 C25 C26 111.0(12) . .
C24 C25 C26 106.8(9) . .
C27 C25 C26 106.3(8) . .
C28 C25 C26 111.0(12) 7_665 7_665
C24 C25 C26 106.8(9) . 7_665
C27 C25 C26 140.7(10) . 7_665
C27 C25 C26 106.3(8) 7_665 7_665
C21 O3 C29 113.3(8) . .
C21 O30 C39 115(3) . .
C33 C34 C33 117(3) . 7_665
C33 C34 C35 118.9(12) . .
C33 C34 C35 118.9(12) 7_665 .
C34 C33 C22 120.1(17) . .
C37 C35 C37 110(3) 7_665 .
C37 C35 C34 114.3(17) 7_665 .
C37 C35 C34 114.3(18) . .
C37 C35 C36 105.6(17) 7_665 .
C37 C35 C36 105.6(17) . .
C34 C35 C36 106(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C2 1.771(3) .
S1 C6 1.772(3) 2_566
C1 O1 1.368(4) .
C1 C2 1.388(5) .
C1 C6 1.398(5) .
C2 C3 1.399(5) .
C3 C4 1.400(5) .
C4 C5 1.389(5) .
C4 C7 1.529(5) .
C5 C6 1.397(5) .
C6 S1 1.773(3) 4_656
C7 C10 1.515(7) .
C7 C9 1.524(5) .
C7 C8 1.548(7) .
O1 C11 1.428(5) .
S2 C13 1.775(4) .
S2 C22 1.779(4) .
C12 O2 1.372(6) .
C12 C13 1.404(4) 8_455
C12 C13 1.404(4) .
C13 C14 1.372(5) .
C14 C15 1.402(4) .
C15 C14 1.402(4) 8_455
C15 C16 1.535(7) .
C16 C17 1.472(8) .
C16 C17 1.472(8) 8_455
C16 C19 1.554(12) .
C16 C19 1.554(12) 8_455
C16 C18 1.629(12) 8_455
C16 C18 1.629(12) .
O2 C30 1.40(3) .
O2 C20 1.408(8) .
C20 I1 1.527(8) .
C21 O30 1.34(4) .
C21 O3 1.388(9) .
C21 C22 1.396(4) 7_665
C21 C22 1.396(4) .
C22 C23 1.354(7) .
C22 C33 1.45(2) .
C23 C24 1.396(7) .
C24 C23 1.396(7) 7_665
C24 C25 1.546(11) .
C25 C28 1.429(12) 7_665
C25 C28 1.429(12) .
C25 C27 1.552(16) .
C25 C27 1.552(17) 7_665
C25 C26 1.586(16) .
C25 C26 1.586(16) 7_665
C37 C35 1.47(2) .
O3 C29 1.425(11) .
O30 C39 1.44(3) .
I1 I2 2.688(5) .
C34 C33 1.42(2) .
C34 C33 1.42(2) 7_665
C34 C35 1.55(4) .
C35 C37 1.47(2) 7_665
C35 C36 1.56(3) .
