#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051873.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_7051873
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) 0.40(C2H4Cl2) 0.60(C3H6O1)'
_chemical_formula_sum            'C40.6 H37.2 Cl0.8 O6.6 S6'
_chemical_formula_weight         851.42
_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                97.149(4)
_cell_angle_beta                 106.072(4)
_cell_angle_gamma                96.567(4)
_cell_formula_units_Z            1
_cell_length_a                   7.9717(6)
_cell_length_b                   10.8775(7)
_cell_length_c                   12.1307(9)
_cell_measurement_reflns_used    5564
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.50
_cell_measurement_theta_min      2.75
_cell_volume                     990.62(13)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       ' φ & ω 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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13226
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.9157
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             443
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5736
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0638P)²+0.7403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                4448
_reflns_number_total             5736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718592h.txt
_cod_data_source_block           dce-ace-40-60
_cod_original_cell_volume        990.62(12)
_cod_original_formula_sum        'C40.60 H37.20 Cl0.80 O6.60 S6'
_cod_database_code               7051873
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
O1 O 0.36029(19) -0.06885(14) 0.14556(14) 0.0218(3) Uani 1 1 d . . .
O2 O 1.0596(2) 0.47111(15) -0.23517(15) 0.0238(3) Uani 1 1 d . . .
O3 O 1.4517(2) 0.42538(17) 0.67002(15) 0.0324(4) Uani 1 1 d . . .
S1 S 0.58591(6) 0.16765(5) 0.15485(5) 0.01662(12) Uani 1 1 d . . .
S2 S 1.25582(6) 0.45961(4) 0.01046(4) 0.01617(12) Uani 1 1 d . . .
S3 S 1.41296(7) 0.20458(5) 0.49401(5) 0.02138(13) Uani 1 1 d . . .
C1 C 1.0980(2) 0.17730(18) 0.16586(17) 0.0140(4) Uani 1 1 d . . .
H1 H 1.1356 0.0987 0.1352 0.017 Uiso 1 1 calc R . .
C2 C 0.9033(2) 0.14584(18) 0.15672(16) 0.0131(3) Uani 1 1 d . . .
C3 C 0.8155(3) 0.02288(19) 0.14888(17) 0.0148(4) Uani 1 1 d . . .
C4 C 0.6423(3) 0.01980(18) 0.14768(17) 0.0146(4) Uani 1 1 d . . .
C5 C 0.7934(3) 0.23293(19) 0.15979(18) 0.0157(4) Uani 1 1 d . . .
C6 C 0.5092(3) -0.08645(19) 0.14442(18) 0.0172(4) Uani 1 1 d . . .
C7 C 0.5612(3) -0.2144(2) 0.1436(2) 0.0243(5) Uani 1 1 d . . .
H7A H 0.6245 -0.2240 0.2230 0.036 Uiso 1 1 calc R . .
H7B H 0.6383 -0.2248 0.0937 0.036 Uiso 1 1 calc R . .
H7C H 0.4551 -0.2780 0.1136 0.036 Uiso 1 1 calc R . .
C8 C 1.1278(2) 0.27407(18) 0.09042(17) 0.0136(4) Uani 1 1 d . . .
C9 C 1.0203(2) 0.26612(18) -0.02540(17) 0.0136(4) Uani 1 1 d . . .
C10 C 1.0725(2) 0.36044(18) -0.08025(17) 0.0137(4) Uani 1 1 d . . .
C11 C 1.2607(3) 0.37528(19) 0.12078(18) 0.0163(4) Uani 1 1 d . . .
C12 C 0.9943(3) 0.38341(19) -0.19800(18) 0.0172(4) Uani 1 1 d . . .
C13 C 0.8312(3) 0.2978(2) -0.2732(2) 0.0291(5) Uani 1 1 d . . .
H13A H 0.7264 0.3337 -0.2665 0.044 Uiso 1 1 calc R . .
H13B H 0.8278 0.2156 -0.2479 0.044 Uiso 1 1 calc R . .
H13C H 0.8326 0.2881 -0.3543 0.044 Uiso 1 1 calc R . .
C14 C 1.2056(2) 0.21458(19) 0.29230(17) 0.0154(4) Uani 1 1 d . . .
C15 C 1.2010(3) 0.3260(2) 0.36565(18) 0.0165(4) Uani 1 1 d . . .
C16 C 1.3071(3) 0.3340(2) 0.47761(18) 0.0179(4) Uani 1 1 d . . .
C17 C 1.3150(3) 0.1412(2) 0.35120(18) 0.0184(4) Uani 1 1 d . . .
C18 C 1.3464(3) 0.4348(2) 0.57776(19) 0.0215(4) Uani 1 1 d . . .
C19 C 1.2541(3) 0.5468(2) 0.5654(2) 0.0255(5) Uani 1 1 d . . .
H19A H 1.1545 0.5374 0.5978 0.038 Uiso 1 1 calc R . .
H19B H 1.2103 0.5537 0.4829 0.038 Uiso 1 1 calc R . .
H19C H 1.3370 0.6226 0.6073 0.038 Uiso 1 1 calc R . .
H3 H 0.866(3) -0.047(2) 0.144(2) 0.017(6) Uiso 1 1 d . . .
H5 H 0.822(3) 0.322(2) 0.163(2) 0.019(6) Uiso 1 1 d . . .
H9 H 0.923(3) 0.201(2) -0.060(2) 0.021(6) Uiso 1 1 d . . .
H11 H 1.352(3) 0.398(2) 0.193(2) 0.016(6) Uiso 1 1 d . . .
H15 H 1.140(3) 0.389(2) 0.340(2) 0.017(6) Uiso 1 1 d . . .
H17 H 1.330(4) 0.061(3) 0.324(3) 0.030(7) Uiso 1 1 d . . .
O4 O 0.9248(10) 0.8611(7) 0.3606(7) 0.0479(18) Uani 0.30 1 d PU A -1
C20 C 0.9963(9) 0.9362(7) 0.4546(7) 0.0190(13) Uani 0.30 1 d PDU A -1
C21 C 0.9211(15) 1.0602(9) 0.4710(11) 0.039(2) Uani 0.30 1 d PDU A -1
H21A H 0.8347 1.0683 0.3981 0.059 Uiso 0.30 1 calc PR A -1
H21B H 1.0176 1.1313 0.4927 0.059 Uiso 0.30 1 calc PR A -1
H21C H 0.8633 1.0593 0.5325 0.059 Uiso 0.30 1 calc PR A -1
C22 C 1.1407(14) 0.8943(13) 0.5481(10) 0.037(3) Uani 0.30 1 d PDU A -1
H22A H 1.1668 0.8134 0.5173 0.056 Uiso 0.30 1 calc PR A -1
H22B H 1.0998 0.8857 0.6162 0.056 Uiso 0.30 1 calc PR A -1
H22C H 1.2478 0.9570 0.5705 0.056 Uiso 0.30 1 calc PR A -1
C31 C 0.9423(8) 0.9981(7) 0.4402(5) 0.0351(15) Uani 0.40 1 d PDU . 2
H31A H 0.8768 0.9123 0.4082 0.042 Uiso 0.40 1 calc PR . 2
H31B H 1.0147 1.0214 0.3893 0.042 Uiso 0.40 1 calc PR . 2
Cl1 Cl 0.7903(3) 1.1064(2) 0.44482(17) 0.0335(4) Uani 0.40 1 d PD B 2
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'
Cl Cl 0.1484 0.1585 '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 91.64(10) . . ?
C11 S2 C10 91.58(10) . . ?
C17 S3 C16 91.35(10) . . ?
C14 C1 C8 113.77(15) . . ?
C14 C1 C2 109.75(15) . . ?
C8 C1 C2 111.37(16) . . ?
C14 C1 H1 107.2 . . ?
C8 C1 H1 107.2 . . ?
C2 C1 H1 107.2 . . ?
C5 C2 C3 111.65(17) . . ?
C5 C2 C1 124.27(17) . . ?
C3 C2 C1 124.03(17) . . ?
C4 C3 C2 112.90(18) . . ?
C4 C3 H3 122.7(16) . . ?
C2 C3 H3 124.4(16) . . ?
C3 C4 C6 130.10(19) . . ?
C3 C4 S1 111.20(14) . . ?
C6 C4 S1 118.68(15) . . ?
C2 C5 S1 112.61(15) . . ?
C2 C5 H5 127.1(15) . . ?
S1 C5 H5 120.3(15) . . ?
O1 C6 C4 119.96(19) . . ?
O1 C6 C7 121.50(18) . . ?
C4 C6 C7 118.52(18) . . ?
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 111.31(18) . . ?
C11 C8 C1 126.39(18) . . ?
C9 C8 C1 122.26(16) . . ?
C10 C9 C8 113.31(17) . . ?
C10 C9 H9 124.9(16) . . ?
C8 C9 H9 121.7(16) . . ?
C9 C10 C12 128.99(18) . . ?
C9 C10 S2 111.05(15) . . ?
C12 C10 S2 119.96(15) . . ?
C8 C11 S2 112.75(16) . . ?
C8 C11 H11 126.3(15) . . ?
S2 C11 H11 120.9(15) . . ?
O2 C12 C10 121.07(19) . . ?
O2 C12 C13 120.4(2) . . ?
C10 C12 C13 118.52(18) . . ?
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 111.60(18) . . ?
C17 C14 C1 123.28(18) . . ?
C15 C14 C1 125.07(18) . . ?
C16 C15 C14 112.8(2) . . ?
C16 C15 H15 123.2(16) . . ?
C14 C15 H15 123.8(16) . . ?
C15 C16 C18 130.2(2) . . ?
C15 C16 S3 111.29(16) . . ?
C18 C16 S3 118.46(16) . . ?
C14 C17 S3 112.93(16) . . ?
C14 C17 H17 126.9(19) . . ?
S3 C17 H17 119.9(19) . . ?
O3 C18 C16 119.8(2) . . ?
O3 C18 C19 121.1(2) . . ?
C16 C18 C19 119.10(19) . . ?
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 . . ?
O4 C20 C22 118.0(8) . . ?
O4 C20 C21 117.4(8) . . ?
C22 C20 C21 124.4(10) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C31 C31 Cl1 108.5(7) 2_776 . ?
C31 C31 H31A 110.0 2_776 . ?
Cl1 C31 H31A 110.0 . . ?
C31 C31 H31B 110.0 2_776 . ?
Cl1 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
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
O1 C6 1.227(2) . ?
O2 C12 1.228(2) . ?
O3 C18 1.223(3) . ?
S1 C5 1.706(2) . ?
S1 C4 1.717(2) . ?
S2 C11 1.708(2) . ?
S2 C10 1.7217(19) . ?
S3 C17 1.708(2) . ?
S3 C16 1.727(2) . ?
C1 C14 1.513(3) . ?
C1 C8 1.518(3) . ?
C1 C2 1.520(3) . ?
C1 H1 1.0000 . ?
C2 C5 1.366(3) . ?
C2 C3 1.416(3) . ?
C3 C4 1.373(3) . ?
C3 H3 0.90(3) . ?
C4 C6 1.466(3) . ?
C5 H5 0.97(3) . ?
C6 C7 1.496(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C11 1.374(3) . ?
C8 C9 1.415(3) . ?
C9 C10 1.376(3) . ?
C9 H9 0.95(3) . ?
C10 C12 1.457(3) . ?
C11 H11 0.96(3) . ?
C12 C13 1.498(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C17 1.366(3) . ?
C14 C15 1.421(3) . ?
C15 C16 1.373(3) . ?
C15 H15 0.93(3) . ?
C16 C18 1.468(3) . ?
C17 H17 0.93(3) . ?
C18 C19 1.496(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O4 C20 1.262(10) . ?
C20 C22 1.531(9) . ?
C20 C21 1.550(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C31 C31 1.481(12) 2_776 ?
C31 Cl1 1.791(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
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 82.4(2) . . . . ?
C8 C1 C2 C5 -44.5(3) . . . . ?
C14 C1 C2 C3 -94.8(2) . . . . ?
C8 C1 C2 C3 138.31(19) . . . . ?
C5 C2 C3 C4 -0.8(2) . . . . ?
C1 C2 C3 C4 176.76(17) . . . . ?
C2 C3 C4 C6 -177.7(2) . . . . ?
C2 C3 C4 S1 0.5(2) . . . . ?
C5 S1 C4 C3 -0.14(16) . . . . ?
C5 S1 C4 C6 178.33(17) . . . . ?
C3 C2 C5 S1 0.7(2) . . . . ?
C1 C2 C5 S1 -176.87(15) . . . . ?
C4 S1 C5 C2 -0.30(17) . . . . ?
C3 C4 C6 O1 178.9(2) . . . . ?
S1 C4 C6 O1 0.8(3) . . . . ?
C3 C4 C6 C7 0.9(3) . . . . ?
S1 C4 C6 C7 -177.27(16) . . . . ?
C14 C1 C8 C11 12.7(3) . . . . ?
C2 C1 C8 C11 137.38(19) . . . . ?
C14 C1 C8 C9 -169.87(17) . . . . ?
C2 C1 C8 C9 -45.2(2) . . . . ?
C11 C8 C9 C10 -0.2(2) . . . . ?
C1 C8 C9 C10 -177.93(17) . . . . ?
C8 C9 C10 C12 -179.52(19) . . . . ?
C8 C9 C10 S2 0.3(2) . . . . ?
C11 S2 C10 C9 -0.32(15) . . . . ?
C11 S2 C10 C12 179.54(16) . . . . ?
C9 C8 C11 S2 -0.1(2) . . . . ?
C1 C8 C11 S2 177.57(15) . . . . ?
C10 S2 C11 C8 0.24(16) . . . . ?
C9 C10 C12 O2 -178.4(2) . . . . ?
S2 C10 C12 O2 1.8(3) . . . . ?
C9 C10 C12 C13 1.9(3) . . . . ?
S2 C10 C12 C13 -177.93(17) . . . . ?
C8 C1 C14 C17 -125.6(2) . . . . ?
C2 C1 C14 C17 108.9(2) . . . . ?
C8 C1 C14 C15 57.1(2) . . . . ?
C2 C1 C14 C15 -68.4(2) . . . . ?
C17 C14 C15 C16 0.2(2) . . . . ?
C1 C14 C15 C16 177.76(17) . . . . ?
C14 C15 C16 C18 176.74(19) . . . . ?
C14 C15 C16 S3 -0.2(2) . . . . ?
C17 S3 C16 C15 0.14(16) . . . . ?
C17 S3 C16 C18 -177.21(16) . . . . ?
C15 C14 C17 S3 -0.1(2) . . . . ?
C1 C14 C17 S3 -177.70(14) . . . . ?
C16 S3 C17 C14 -0.03(16) . . . . ?
C15 C16 C18 O3 -177.0(2) . . . . ?
S3 C16 C18 O3 -0.2(3) . . . . ?
C15 C16 C18 C19 4.0(3) . . . . ?
S3 C16 C18 C19 -179.23(15) . . . . ?
H1 C1 C14 C17 -7.2 . . . . ?
H1 C1 C8 C11 -105.6 . . . . ?
H1 C1 C2 C5 -161.4 . . . . ?
