#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051888.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_7051888
loop_
_publ_author_name
'Burchell, Tara J.'
'Enright, Gary D.'
'Ripmeester, John A.'
_publ_section_title
;
 Guest capture, storage and removal in the TATM host framework: a
 single-crystal study
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              864
_journal_paper_doi               10.1039/b718592h
_journal_volume                  32
_journal_year                    2008
_chemical_formula_moiety         '2(C19H16O3S3) 0.60(C3H6O1)'
_chemical_formula_sum            'C39.8 H35.6 O6.6 S6'
_chemical_formula_weight         811.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.345(6)
_cell_angle_beta                 107.251(6)
_cell_angle_gamma                95.810(6)
_cell_formula_units_Z            1
_cell_length_a                   8.032(4)
_cell_length_b                   10.645(5)
_cell_length_c                   12.144(6)
_cell_measurement_reflns_used    4120
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.68
_cell_volume                     978.2(8)
_computing_cell_refinement       'SAINT (Bruker 2001)'
_computing_data_collection       SMART
_computing_data_reduction        'SAINT (Bruker 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '/w 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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10967
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.9539
_exptl_absorpt_correction_T_min  0.9107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             423
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0594
_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)+(0.0212P)²+2.2897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                3134
_reflns_number_total             3978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718592h.txt
_cod_data_source_block           1c
_cod_original_formula_sum        'C39.80 H35.60 O6.60 S6'
_cod_database_code               7051888
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.25448(11) 0.54137(8) 0.49040(8) 0.0214(2) Uani 1 1 d . . .
S2 S 0.91472(11) 0.82807(8) 0.34117(8) 0.0235(2) Uani 1 1 d . . .
S3 S 0.07835(13) 0.80599(9) 0.00349(9) 0.0352(3) Uani 1 1 d . . .
O1 O 0.4412(3) 0.5363(2) 0.7413(2) 0.0309(6) Uani 1 1 d . . .
O2 O 1.1417(3) 1.0667(2) 0.3544(2) 0.0295(6) Uani 1 1 d . . .
O3 O 0.0241(4) 0.5776(3) -0.1668(2) 0.0474(8) Uani 1 1 d . . .
C1 C 0.4072(4) 0.8276(3) 0.3292(3) 0.0187(7) Uani 1 1 d . . .
H1A H 0.3719 0.9084 0.3586 0.022 Uiso 1 1 calc R . .
C2 C 0.3778(4) 0.7291(3) 0.4067(3) 0.0180(7) Uani 1 1 d . . .
C3 C 0.4792(4) 0.7402(3) 0.5249(3) 0.0181(7) Uani 1 1 d . . .
H3A H 0.5735 0.8065 0.5612 0.022 Uiso 1 1 calc R . .
C4 C 0.4281(4) 0.6462(3) 0.5820(3) 0.0191(7) Uani 1 1 d . . .
C5 C 0.2518(4) 0.6254(3) 0.3769(3) 0.0215(7) Uani 1 1 d . . .
C6 C 0.4990(4) 0.6269(3) 0.7036(3) 0.0249(8) Uani 1 1 d . . .
C7 C 0.6487(6) 0.7211(4) 0.7800(4) 0.0504(13) Uani 1 1 d . . .
H7A H 0.6399 0.7314 0.8590 0.076 Uiso 1 1 calc R . .
H7B H 0.6444 0.8032 0.7497 0.076 Uiso 1 1 calc R . .
H7C H 0.7602 0.6902 0.7815 0.076 Uiso 1 1 calc R . .
C8 C 0.6004(4) 0.8557(3) 0.3377(3) 0.0181(7) Uani 1 1 d . . .
C9 C 0.6881(4) 0.9787(3) 0.3449(3) 0.0195(7) Uani 1 1 d . . .
C10 C 0.8603(4) 0.9798(3) 0.3472(3) 0.0186(7) Uani 1 1 d . . .
C11 C 0.7081(4) 0.7653(3) 0.3355(3) 0.0209(7) Uani 1 1 d . . .
C12 C 0.9942(4) 1.0865(3) 0.3532(3) 0.0222(7) Uani 1 1 d . . .
C13 C 0.9436(5) 1.2173(3) 0.3547(4) 0.0345(9) Uani 1 1 d . . .
H13A H 1.0491 1.2798 0.3718 0.052 Uiso 1 1 calc R . .
H13B H 0.8862 1.2320 0.4147 0.052 Uiso 1 1 calc R . .
H13C H 0.8621 1.2260 0.2786 0.052 Uiso 1 1 calc R . .
C14 C 0.2955(4) 0.7924(3) 0.2030(3) 0.0203(7) Uani 1 1 d . . .
C15 C 0.2968(4) 0.6798(3) 0.1307(3) 0.0220(7) Uani 1 1 d . . .
H15A H 0.3681 0.6158 0.1565 0.026 Uiso 1 1 calc R . .
C16 C 0.1847(4) 0.6732(3) 0.0199(3) 0.0246(8) Uani 1 1 d . . .
C17 C 0.1838(4) 0.8690(4) 0.1450(3) 0.0262(8) Uani 1 1 d . . .
C18 C 0.1399(5) 0.5706(4) -0.0776(3) 0.0295(9) Uani 1 1 d . . .
C19 C 0.2386(5) 0.4593(4) -0.0646(3) 0.0363(9) Uani 1 1 d . . .
H19A H 0.1599 0.3823 -0.1071 0.054 Uiso 1 1 calc R . .
H19B H 0.2838 0.4492 0.0179 0.054 Uiso 1 1 calc R . .
H19C H 0.3371 0.4730 -0.0962 0.054 Uiso 1 1 calc R . .
H5 H 0.172(5) 0.599(4) 0.309(3) 0.026(10) Uiso 1 1 d . . .
H9 H 0.635(4) 1.048(3) 0.347(3) 0.013(8) Uiso 1 1 d . . .
H11 H 0.683(5) 0.678(4) 0.337(3) 0.023(9) Uiso 1 1 d . . .
H17 H 0.162(5) 0.946(4) 0.171(3) 0.029(11) Uiso 1 1 d . . .
C51 C 0.420(2) 1.0571(18) 0.9656(18) 0.042(4) Uani 0.30 1 d P A -1
H51A H 0.3294 1.0687 0.8942 0.064 Uiso 0.30 1 calc PR A -1
H51B H 0.5212 1.1231 0.9809 0.064 Uiso 0.30 1 calc PR A -1
H51C H 0.3718 1.0635 1.0310 0.064 Uiso 0.30 1 calc PR A -1
C50 C 0.478(2) 0.9267(15) 0.9514(13) 0.041(3) Uani 0.30 1 d P A -1
O50 O 0.4016(16) 0.8498(12) 0.8683(10) 0.061(3) Uani 0.30 1 d P A -1
C52 C 0.637(3) 0.893(2) 1.0460(17) 0.051(5) Uani 0.30 1 d P A -1
H52A H 0.6066 0.8855 1.1177 0.077 Uiso 0.30 1 calc PR A -1
H52B H 0.7375 0.9593 1.0610 0.077 Uiso 0.30 1 calc PR A -1
H52C H 0.6685 0.8111 1.0192 0.077 Uiso 0.30 1 calc PR A -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'
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
_geom_angle_publ_flag
C5 S1 C4 91.19(17) . . ?
C11 S2 C10 91.49(17) . . ?
C17 S3 C16 91.77(18) . . ?
C14 C1 C2 113.4(3) . . ?
C14 C1 C8 110.2(3) . . ?
C2 C1 C8 111.7(3) . . ?
C14 C1 H1A 107.1 . . ?
C2 C1 H1A 107.1 . . ?
C8 C1 H1A 107.1 . . ?
C5 C2 C3 111.3(3) . . ?
C5 C2 C1 126.9(3) . . ?
C3 C2 C1 121.7(3) . . ?
C4 C3 C2 113.3(3) . . ?
C4 C3 H3A 123.3 . . ?
C2 C3 H3A 123.3 . . ?
C3 C4 C6 129.1(3) . . ?
C3 C4 S1 111.2(2) . . ?
C6 C4 S1 119.7(2) . . ?
C2 C5 S1 112.9(3) . . ?
C2 C5 H5 129(2) . . ?
S1 C5 H5 119(2) . . ?
O1 C6 C4 121.4(3) . . ?
O1 C6 C7 120.8(3) . . ?
C4 C6 C7 117.7(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C11 C8 C9 111.7(3) . . ?
C11 C8 C1 124.5(3) . . ?
C9 C8 C1 123.8(3) . . ?
C10 C9 C8 113.2(3) . . ?
C10 C9 H9 124(2) . . ?
C8 C9 H9 122(2) . . ?
C9 C10 C12 130.3(3) . . ?
C9 C10 S2 110.9(2) . . ?
C12 C10 S2 118.9(3) . . ?
C8 C11 S2 112.7(3) . . ?
C8 C11 H11 127(2) . . ?
S2 C11 H11 120(2) . . ?
O2 C12 C10 120.0(3) . . ?
O2 C12 C13 121.8(3) . . ?
C10 C12 C13 118.3(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C17 C14 C15 111.9(3) . . ?
C17 C14 C1 122.8(3) . . ?
C15 C14 C1 125.3(3) . . ?
C16 C15 C14 113.1(3) . . ?
C16 C15 H15A 123.5 . . ?
C14 C15 H15A 123.5 . . ?
C15 C16 C18 129.9(3) . . ?
C15 C16 S3 110.9(3) . . ?
C18 C16 S3 119.1(3) . . ?
C14 C17 S3 112.4(3) . . ?
C14 C17 H17 129(3) . . ?
S3 C17 H17 119(2) . . ?
O3 C18 C16 120.1(4) . . ?
O3 C18 C19 121.2(4) . . ?
C16 C18 C19 118.7(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O50 C50 C51 121.1(16) . . ?
O50 C50 C52 119.6(16) . . ?
C51 C50 C52 119.3(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C5 1.707(4) . ?
S1 C4 1.721(3) . ?
S2 C11 1.705(3) . ?
S2 C10 1.716(3) . ?
S3 C17 1.711(4) . ?
S3 C16 1.722(4) . ?
O1 C6 1.214(4) . ?
O2 C12 1.220(4) . ?
O3 C18 1.214(4) . ?
C1 C14 1.518(4) . ?
C1 C2 1.518(5) . ?
C1 C8 1.521(5) . ?
C1 H1A 1.0000 . ?
C2 C5 1.363(5) . ?
C2 C3 1.412(4) . ?
C3 C4 1.366(5) . ?
C3 H3A 0.9500 . ?
C4 C6 1.458(5) . ?
C5 H5 0.88(4) . ?
C6 C7 1.495(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C11 1.361(5) . ?
C8 C9 1.405(5) . ?
C9 C10 1.374(5) . ?
C9 H9 0.90(3) . ?
C10 C12 1.464(5) . ?
C11 H11 0.93(4) . ?
C12 C13 1.489(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C17 1.359(5) . ?
C14 C15 1.421(5) . ?
C15 C16 1.370(5) . ?
C15 H15A 0.9500 . ?
C16 C18 1.466(5) . ?
C17 H17 0.90(4) . ?
C18 C19 1.486(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C51 C50 1.52(2) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C50 O50 1.201(18) . ?
C50 C52 1.55(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C5 -8.0(5) . . . . ?
C8 C1 C2 C5 -133.2(3) . . . . ?
C14 C1 C2 C3 175.1(3) . . . . ?
C8 C1 C2 C3 49.9(4) . . . . ?
C5 C2 C3 C4 -0.3(4) . . . . ?
C1 C2 C3 C4 177.0(3) . . . . ?
C2 C3 C4 C6 -179.2(3) . . . . ?
C2 C3 C4 S1 0.4(4) . . . . ?
C5 S1 C4 C3 -0.3(3) . . . . ?
C5 S1 C4 C6 179.3(3) . . . . ?
C3 C2 C5 S1 0.1(4) . . . . ?
C1 C2 C5 S1 -177.0(3) . . . . ?
C4 S1 C5 C2 0.1(3) . . . . ?
C3 C4 C6 O1 -178.5(3) . . . . ?
S1 C4 C6 O1 2.0(5) . . . . ?
C3 C4 C6 C7 0.0(6) . . . . ?
S1 C4 C6 C7 -179.5(3) . . . . ?
C14 C1 C8 C11 -82.0(4) . . . . ?
C2 C1 C8 C11 45.0(4) . . . . ?
C14 C1 C8 C9 95.8(4) . . . . ?
C2 C1 C8 C9 -137.2(3) . . . . ?
C11 C8 C9 C10 0.5(4) . . . . ?
C1 C8 C9 C10 -177.6(3) . . . . ?
C8 C9 C10 C12 179.4(3) . . . . ?
C8 C9 C10 S2 -0.3(4) . . . . ?
C11 S2 C10 C9 0.1(3) . . . . ?
C11 S2 C10 C12 -179.7(3) . . . . ?
C9 C8 C11 S2 -0.4(4) . . . . ?
C1 C8 C11 S2 177.6(3) . . . . ?
C10 S2 C11 C8 0.2(3) . . . . ?
C9 C10 C12 O2 180.0(3) . . . . ?
S2 C10 C12 O2 -0.4(4) . . . . ?
C9 C10 C12 C13 -1.5(5) . . . . ?
S2 C10 C12 C13 178.2(3) . . . . ?
C2 C1 C14 C17 123.4(4) . . . . ?
C8 C1 C14 C17 -110.5(4) . . . . ?
C2 C1 C14 C15 -58.3(4) . . . . ?
C8 C1 C14 C15 67.7(4) . . . . ?
C17 C14 C15 C16 -0.7(4) . . . . ?
C1 C14 C15 C16 -179.1(3) . . . . ?
C14 C15 C16 C18 -175.7(3) . . . . ?
C14 C15 C16 S3 0.6(4) . . . . ?
C17 S3 C16 C15 -0.3(3) . . . . ?
C17 S3 C16 C18 176.5(3) . . . . ?
C15 C14 C17 S3 0.4(4) . . . . ?
C1 C14 C17 S3 178.9(3) . . . . ?
C16 S3 C17 C14 -0.1(3) . . . . ?
C15 C16 C18 O3 173.0(4) . . . . ?
S3 C16 C18 O3 -3.0(5) . . . . ?
C15 C16 C18 C19 -6.9(6) . . . . ?
S3 C16 C18 C19 177.1(3) . . . . ?
H1A C1 C2 C5 109.9 . . . . ?
H1A C1 C8 C11 161.9 . . . . ?
H1A C1 C14 C17 5.6 . . . . ?
