#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:19:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180072 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051876.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_7051876
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) 1.0(C2H4Cl2)'
_chemical_formula_sum            'C40 H36 Cl2 O6 S6'
_chemical_formula_weight         875.95
_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                97.623(5)
_cell_angle_beta                 105.816(4)
_cell_angle_gamma                96.665(4)
_cell_formula_units_Z            1
_cell_length_a                   7.9495(7)
_cell_length_b                   10.9743(10)
_cell_length_c                   12.1800(12)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      38.99
_cell_measurement_theta_min      2.70
_cell_volume                     1000.33(16)
_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      100(1)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35685
_diffrn_reflns_theta_full        38.99
_diffrn_reflns_theta_max         38.89
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.9027
_exptl_absorpt_correction_T_min  0.8383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         11389
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0335
_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)+(0.0479P)²+0.1954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                9237
_reflns_number_total             11389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718592h.txt
_cod_data_source_block           dce-ace-100-0
_cod_database_code               7051876
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 0.05597(10) 0.07197(7) -0.17124(6) 0.02711(15) Uani 1 1 d . . .
O2 O 0.43764(9) 0.02765(6) 0.73186(6) 0.02195(12) Uani 1 1 d . . .
O3 O 1.14177(8) 0.56825(6) 0.35473(6) 0.02043(12) Uani 1 1 d . . .
S1 S 0.08977(3) 0.29014(2) 0.005273(18) 0.01797(4) Uani 1 1 d . . .
S2 S 0.24044(2) 0.040025(18) 0.487921(18) 0.01469(4) Uani 1 1 d . . .
S3 S 0.91777(2) 0.333229(18) 0.348945(18) 0.01465(4) Uani 1 1 d . . .
C1 C 0.40104(9) 0.32015(7) 0.33434(6) 0.01304(11) Uani 1 1 d . . .
H1 H 0.3629 0.3963 0.3641 0.016 Uiso 1 1 calc R . .
C2 C 0.29462(9) 0.28168(7) 0.20779(7) 0.01364(12) Uani 1 1 d . . .
C3 C 0.30099(10) 0.17056(7) 0.13442(7) 0.01458(12) Uani 1 1 d . . .
C4 C 0.19574(10) 0.16185(8) 0.02214(7) 0.01522(12) Uani 1 1 d . . .
C5 C 0.18477(10) 0.35416(8) 0.14810(7) 0.01633(13) Uani 1 1 d . . .
C6 C 0.15877(11) 0.06179(8) -0.07844(7) 0.01741(13) Uani 1 1 d . . .
C7 C 0.24759(13) -0.05118(9) -0.06581(8) 0.02167(15) Uani 1 1 d . . .
H7A H 0.1644 -0.1243 -0.1068 0.033 Uiso 1 1 calc R . .
H7B H 0.2892 -0.0573 0.0147 0.033 Uiso 1 1 calc R . .
H7C H 0.3460 -0.0441 -0.0972 0.033 Uiso 1 1 calc R . .
C8 C 0.37053(9) 0.22416(7) 0.40908(6) 0.01258(11) Uani 1 1 d . . .
C9 C 0.47957(9) 0.23188(7) 0.52459(6) 0.01267(11) Uani 1 1 d . . .
C10 C 0.42540(9) 0.13837(7) 0.57851(7) 0.01312(11) Uani 1 1 d . . .
C11 C 0.23590(10) 0.12409(7) 0.37840(7) 0.01493(12) Uani 1 1 d . . .
C12 C 0.50397(10) 0.11521(7) 0.69620(7) 0.01542(12) Uani 1 1 d . . .
C13 C 0.66842(13) 0.20016(9) 0.77187(8) 0.02377(17) Uani 1 1 d . . .
H13A H 0.6611 0.2164 0.8497 0.036 Uiso 1 1 calc R . .
H13B H 0.6790 0.2772 0.7431 0.036 Uiso 1 1 calc R . .
H13C H 0.7702 0.1612 0.7711 0.036 Uiso 1 1 calc R . .
C14 C 0.59674(9) 0.35267(7) 0.34448(6) 0.01245(11) Uani 1 1 d . . .
C15 C 0.68346(10) 0.47538(7) 0.35100(7) 0.01360(12) Uani 1 1 d . . .
C16 C 0.85897(10) 0.47965(7) 0.35353(7) 0.01357(12) Uani 1 1 d . . .
C17 C 0.70992(10) 0.26698(7) 0.34325(7) 0.01448(12) Uani 1 1 d . . .
C18 C 0.99150(10) 0.58497(7) 0.35493(7) 0.01584(13) Uani 1 1 d . . .
C19 C 0.93747(13) 0.71168(8) 0.35274(9) 0.02276(16) Uani 1 1 d . . .
H19A H 1.0403 0.7745 0.3856 0.034 Uiso 1 1 calc R . .
H19B H 0.8553 0.7212 0.3970 0.034 Uiso 1 1 calc R . .
H19C H 0.8824 0.7202 0.2742 0.034 Uiso 1 1 calc R . .
H3 H 0.3653(19) 0.1108(13) 0.1582(12) 0.025(3) Uiso 1 1 d . . .
H5 H 0.1619(18) 0.4320(13) 0.1780(12) 0.021(3) Uiso 1 1 d . . .
H9 H 0.5772(17) 0.2941(12) 0.5581(11) 0.017(3) Uiso 1 1 d . . .
H11 H 0.1455(17) 0.0980(12) 0.3078(12) 0.021(3) Uiso 1 1 d . . .
H15 H 0.6321(16) 0.5425(12) 0.3542(11) 0.016(3) Uiso 1 1 d . . .
H17 H 0.6880(17) 0.1803(12) 0.3418(11) 0.019(3) Uiso 1 1 d . . .
Cl1 Cl 0.71616(18) 0.39961(16) 0.05465(18) 0.03091(16) Uani 0.776(3) 1 d PDU A
1
C21 C 0.55804(16) 0.50149(13) 0.06057(10) 0.0230(3) Uani 0.776(3) 1 d PDU . 1
H21A H 0.4864 0.4749 0.1086 0.028 Uiso 0.776(3) 1 calc PR A 1
H21B H 0.6185 0.5856 0.0942 0.028 Uiso 0.776(3) 1 calc PR A 1
Cl2 Cl 0.6869(8) 0.3783(7) 0.0552(7) 0.0448(12) Uani 0.224(3) 1 d PDU A 2
C22 C 0.5195(6) 0.4442(4) -0.0342(4) 0.0241(9) Uani 0.224(3) 1 d PDU . 2
H22A H 0.5578 0.4687 -0.0983 0.029 Uiso 0.224(3) 1 calc PR A 2
H22B H 0.4128 0.3829 -0.0657 0.029 Uiso 0.224(3) 1 calc PR A 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 91.49(4) . . ?
C11 S2 C10 91.57(4) . . ?
C17 S3 C16 91.84(4) . . ?
C2 C1 C8 113.62(6) . . ?
C2 C1 C14 109.83(6) . . ?
C8 C1 C14 111.39(6) . . ?
C2 C1 H1 107.2 . . ?
C8 C1 H1 107.2 . . ?
C14 C1 H1 107.2 . . ?
C5 C2 C3 111.47(7) . . ?
C5 C2 C1 123.30(7) . . ?
C3 C2 C1 125.17(7) . . ?
C4 C3 C2 112.74(7) . . ?
C4 C3 H3 122.8(9) . . ?
C2 C3 H3 124.4(9) . . ?
C3 C4 C6 130.30(8) . . ?
C3 C4 S1 111.40(6) . . ?
C6 C4 S1 118.26(6) . . ?
C2 C5 S1 112.91(6) . . ?
C2 C5 H5 126.6(8) . . ?
S1 C5 H5 120.5(8) . . ?
O1 C6 C4 119.57(8) . . ?
O1 C6 C7 121.09(8) . . ?
C4 C6 C7 119.34(7) . . ?
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 111.51(7) . . ?
C11 C8 C1 126.22(7) . . ?
C9 C8 C1 122.23(6) . . ?
C10 C9 C8 112.97(7) . . ?
C10 C9 H9 125.0(8) . . ?
C8 C9 H9 122.0(8) . . ?
C9 C10 C12 128.83(7) . . ?
C9 C10 S2 111.32(6) . . ?
C12 C10 S2 119.85(6) . . ?
C8 C11 S2 112.63(6) . . ?
C8 C11 H11 129.0(8) . . ?
S2 C11 H11 118.4(8) . . ?
O2 C12 C10 120.73(7) . . ?
O2 C12 C13 120.63(8) . . ?
C10 C12 C13 118.64(7) . . ?
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 111.49(7) . . ?
C17 C14 C1 124.51(7) . . ?
C15 C14 C1 123.94(7) . . ?
C16 C15 C14 112.86(7) . . ?
C16 C15 H15 123.0(8) . . ?
C14 C15 H15 124.1(8) . . ?
C15 C16 C18 130.34(7) . . ?
C15 C16 S3 111.09(6) . . ?
C18 C16 S3 118.52(6) . . ?
C14 C17 S3 112.71(6) . . ?
C14 C17 H17 129.0(8) . . ?
S3 C17 H17 118.2(8) . . ?
O3 C18 C16 120.12(8) . . ?
O3 C18 C19 121.33(7) . . ?
C16 C18 C19 118.52(7) . . ?
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 . . ?
C21 C21 Cl1 108.73(13) 2_665 . ?
C21 C21 H21A 109.9 2_665 . ?
Cl1 C21 H21A 109.9 . . ?
C21 C21 H21B 109.9 2_665 . ?
Cl1 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
C22 C22 Cl2 110.2(5) 2_665 . ?
C22 C22 H22A 109.6 2_665 . ?
Cl2 C22 H22A 109.6 . . ?
C22 C22 H22B 109.6 2_665 . ?
Cl2 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
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 1.2285(10) . ?
O2 C12 1.2280(10) . ?
O3 C18 1.2301(10) . ?
S1 C5 1.7108(9) . ?
S1 C4 1.7296(8) . ?
S2 C11 1.7146(8) . ?
S2 C10 1.7250(8) . ?
S3 C17 1.7055(8) . ?
S3 C16 1.7229(8) . ?
C1 C2 1.5178(11) . ?
C1 C8 1.5207(11) . ?
C1 C14 1.5224(10) . ?
C1 H1 0.9800 . ?
C2 C5 1.3756(11) . ?
C2 C3 1.4276(11) . ?
C3 C4 1.3793(11) . ?
C3 H3 0.907(14) . ?
C4 C6 1.4713(12) . ?
C5 H5 0.941(14) . ?
C6 C7 1.5013(13) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C11 1.3753(11) . ?
C8 C9 1.4229(10) . ?
C9 C10 1.3785(11) . ?
C9 H9 0.931(13) . ?
C10 C12 1.4679(11) . ?
C11 H11 0.942(13) . ?
C12 C13 1.5034(12) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C17 1.3762(11) . ?
C14 C15 1.4217(11) . ?
C15 C16 1.3823(11) . ?
C15 H15 0.884(13) . ?
C16 C18 1.4658(11) . ?
C17 H17 0.943(13) . ?
C18 C19 1.5037(12) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
Cl1 C21 1.786(2) . ?
C21 C21 1.506(2) 2_665 ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
Cl2 C22 1.767(6) . ?
C22 C22 1.498(8) 2_665 ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
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
C8 C1 C2 C5 125.98(8) . . . . ?
C14 C1 C2 C5 -108.51(8) . . . . ?
C8 C1 C2 C3 -57.12(10) . . . . ?
C14 C1 C2 C3 68.39(9) . . . . ?
C5 C2 C3 C4 -0.31(10) . . . . ?
C1 C2 C3 C4 -177.53(7) . . . . ?
C2 C3 C4 C6 -177.19(8) . . . . ?
C2 C3 C4 S1 0.51(9) . . . . ?
C5 S1 C4 C3 -0.45(6) . . . . ?
C5 S1 C4 C6 177.56(7) . . . . ?
C3 C2 C5 S1 -0.04(9) . . . . ?
C1 C2 C5 S1 177.24(6) . . . . ?
C4 S1 C5 C2 0.28(7) . . . . ?
C3 C4 C6 O1 178.20(9) . . . . ?
S1 C4 C6 O1 0.63(11) . . . . ?
C3 C4 C6 C7 -1.82(13) . . . . ?
S1 C4 C6 C7 -179.39(6) . . . . ?
C2 C1 C8 C11 -13.89(11) . . . . ?
C14 C1 C8 C11 -138.57(8) . . . . ?
C2 C1 C8 C9 168.61(7) . . . . ?
C14 C1 C8 C9 43.93(10) . . . . ?
C11 C8 C9 C10 -0.11(10) . . . . ?
C1 C8 C9 C10 177.73(7) . . . . ?
C8 C9 C10 C12 179.67(7) . . . . ?
C8 C9 C10 S2 0.09(9) . . . . ?
C11 S2 C10 C9 -0.04(6) . . . . ?
C11 S2 C10 C12 -179.66(7) . . . . ?
C9 C8 C11 S2 0.07(9) . . . . ?
C1 C8 C11 S2 -177.65(6) . . . . ?
C10 S2 C11 C8 -0.02(6) . . . . ?
C9 C10 C12 O2 179.15(8) . . . . ?
S2 C10 C12 O2 -1.30(11) . . . . ?
C9 C10 C12 C13 -1.43(13) . . . . ?
S2 C10 C12 C13 178.12(7) . . . . ?
C2 C1 C14 C17 -83.13(9) . . . . ?
C8 C1 C14 C17 43.65(10) . . . . ?
C2 C1 C14 C15 93.80(9) . . . . ?
C8 C1 C14 C15 -139.42(7) . . . . ?
C17 C14 C15 C16 0.52(10) . . . . ?
C1 C14 C15 C16 -176.76(7) . . . . ?
C14 C15 C16 C18 177.02(8) . . . . ?
C14 C15 C16 S3 -0.43(9) . . . . ?
C17 S3 C16 C15 0.17(6) . . . . ?
C17 S3 C16 C18 -177.61(7) . . . . ?
C15 C14 C17 S3 -0.39(9) . . . . ?
C1 C14 C17 S3 176.88(6) . . . . ?
C16 S3 C17 C14 0.13(6) . . . . ?
C15 C16 C18 O3 -178.45(8) . . . . ?
S3 C16 C18 O3 -1.17(11) . . . . ?
C15 C16 C18 C19 -0.39(13) . . . . ?
S3 C16 C18 C19 176.90(6) . . . . ?
H1 C1 C14 C17 160.7 . . . . ?
H1 C1 C8 C11 104.4 . . . . ?
H1 C1 C2 C5 7.7 . . . . ?
