#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:19:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180072 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051878.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_7051878
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) 0.26(C2H4Cl2)'
_chemical_formula_sum            'C38.52 H33.03 Cl0.52 O6 S6'
_chemical_formula_weight         802.71
_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                96.507(6)
_cell_angle_beta                 105.889(6)
_cell_angle_gamma                96.037(6)
_cell_formula_units_Z            1
_cell_length_a                   7.925(3)
_cell_length_b                   10.805(5)
_cell_length_c                   11.946(5)
_cell_measurement_reflns_used    3225
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      2.70
_cell_volume                     967.5(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8231
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9661
_exptl_absorpt_correction_T_min  0.8735
_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             417
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0872
_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)+(0.1001P)²+5.0402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2038
_refine_ls_wR_factor_ref         0.2183
_reflns_number_gt                1966
_reflns_number_total             2769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718592h.txt
_cod_data_source_block           2a
_cod_original_cell_volume        967.6(7)
_cod_database_code               7051878
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 0.2512(2) 0.04136(17) 0.49101(17) 0.0182(5) Uani 1 1 d U . .
S2 S 0.9213(2) 0.33012(17) 0.34436(17) 0.0200(5) Uani 1 1 d U . .
S3 S 0.0902(3) 0.3011(2) -0.00007(18) 0.0283(6) Uani 1 1 d U . .
C9 C 0.6881(9) 0.4760(7) 0.3437(6) 0.0153(16) Uani 1 1 d U . .
H9 H 0.6313 0.5491 0.3447 0.018 Uiso 1 1 calc R . .
O1 O 0.4399(7) 0.0345(5) 0.7417(5) 0.0282(13) Uani 1 1 d U . .
O2 O 1.1447(6) 0.5671(5) 0.3520(4) 0.0231(12) Uani 1 1 d U . .
O3 O 0.0326(8) 0.0729(5) -0.1706(5) 0.0408(16) Uani 1 1 d U . .
C1 C 0.4072(9) 0.3242(7) 0.3305(6) 0.0149(16) Uani 1 1 d U . .
H1 H 0.3693 0.4035 0.3609 0.018 Uiso 1 1 calc R . .
C2 C 0.3771(9) 0.2263(6) 0.4091(6) 0.0150(16) Uani 1 1 d U . .
C3 C 0.4775(9) 0.2377(7) 0.5267(6) 0.0157(16) Uani 1 1 d U . .
H3 H 0.5728 0.3035 0.5633 0.019 Uiso 1 1 calc R . .
C4 C 0.4258(9) 0.1456(6) 0.5835(6) 0.0159(16) Uani 1 1 d U . .
C5 C 0.2493(10) 0.1242(7) 0.3788(6) 0.0175(17) Uani 1 1 d U . .
H5 H 0.1674 0.1017 0.3026 0.021 Uiso 1 1 calc R . .
C6 C 0.4982(10) 0.1251(7) 0.7050(7) 0.0212(18) Uani 1 1 d U . .
C7 C 0.6451(13) 0.2178(9) 0.7835(8) 0.047(3) Uani 1 1 d U . .
H7A H 0.6228 0.2373 0.8599 0.071 Uiso 1 1 calc R . .
H7B H 0.6533 0.2949 0.7482 0.071 Uiso 1 1 calc R . .
H7C H 0.7566 0.1827 0.7946 0.071 Uiso 1 1 calc R . .
C8 C 0.6013(9) 0.3535(6) 0.3394(6) 0.0146(16) Uani 1 1 d U . .
C10 C 0.8625(9) 0.4786(7) 0.3462(6) 0.0165(16) Uani 1 1 d U . .
C11 C 0.7131(9) 0.2669(7) 0.3394(6) 0.0179(17) Uani 1 1 d U . .
H11 H 0.6787 0.1794 0.3369 0.021 Uiso 1 1 calc R . .
C12 C 0.9937(10) 0.5838(7) 0.3510(6) 0.0185(17) Uani 1 1 d U . .
C13 C 0.9404(11) 0.7123(7) 0.3496(7) 0.030(2) Uani 1 1 d U . .
H13A H 1.0465 0.7753 0.3691 0.045 Uiso 1 1 calc R . .
H13B H 0.8754 0.7277 0.4076 0.045 Uiso 1 1 calc R . .
H13C H 0.8642 0.7183 0.2711 0.045 Uiso 1 1 calc R . .
C14 C 0.2980(9) 0.2869(6) 0.2019(6) 0.0157(16) Uani 1 1 d U . .
C15 C 0.2980(9) 0.1758(7) 0.1296(6) 0.0160(16) Uani 1 1 d U . .
H15 H 0.3652 0.1116 0.1564 0.019 Uiso 1 1 calc R . .
C16 C 0.1935(10) 0.1682(7) 0.0181(6) 0.0206(18) Uani 1 1 d U . .
C17 C 0.1906(10) 0.3638(7) 0.1422(7) 0.0252(19) Uani 1 1 d U . .
H17 H 0.1741 0.4435 0.1769 0.030 Uiso 1 1 calc R . .
C18 C 0.1474(10) 0.0637(7) -0.0794(7) 0.0224(18) Uani 1 1 d U . .
C19 C 0.2342(11) -0.0488(7) -0.0659(7) 0.029(2) Uani 1 1 d U . .
H19A H 0.1556 -0.1215 -0.1175 0.043 Uiso 1 1 calc R . .
H19B H 0.2600 -0.0638 0.0161 0.043 Uiso 1 1 calc R . .
H19C H 0.3450 -0.0367 -0.0873 0.043 Uiso 1 1 calc R . .
Cl1 Cl 0.2936(12) 0.6096(8) 0.9445(8) 0.040(4) Uani 0.258(9) 1 d PDU A 1
C32 C 0.441(5) 0.498(4) 0.9383(10) 0.076(14) Uiso 0.258(9) 1 d PD . 1
H32A H 0.3731 0.4124 0.9084 0.091 Uiso 0.258(9) 1 calc PR A 1
H32B H 0.5121 0.5185 0.8850 0.091 Uiso 0.258(9) 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'
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 91.0(4) . . ?
C11 S2 C10 91.4(4) . . ?
C17 S3 C16 91.1(4) . . ?
C10 C9 C8 113.2(6) . . ?
C8 C1 C14 110.2(6) . . ?
C8 C1 C2 111.1(6) . . ?
C14 C1 C2 113.6(6) . . ?
C5 C2 C3 111.5(6) . . ?
C5 C2 C1 126.4(6) . . ?
C3 C2 C1 122.0(6) . . ?
C4 C3 C2 113.4(6) . . ?
C3 C4 C6 129.4(7) . . ?
C3 C4 S1 111.1(5) . . ?
C6 C4 S1 119.4(5) . . ?
C2 C5 S1 112.9(6) . . ?
O1 C6 C4 121.3(7) . . ?
O1 C6 C7 120.3(7) . . ?
C4 C6 C7 118.4(7) . . ?
C11 C8 C9 111.1(6) . . ?
C11 C8 C1 125.1(6) . . ?
C9 C8 C1 123.8(6) . . ?
C9 C10 C12 129.8(7) . . ?
C9 C10 S2 110.9(5) . . ?
C12 C10 S2 119.2(5) . . ?
C8 C11 S2 113.3(5) . . ?
O2 C12 C10 120.3(7) . . ?
O2 C12 C13 120.7(7) . . ?
C10 C12 C13 118.9(7) . . ?
C17 C14 C15 111.7(7) . . ?
C17 C14 C1 122.5(7) . . ?
C15 C14 C1 125.8(6) . . ?
C16 C15 C14 113.7(7) . . ?
C15 C16 C18 129.8(7) . . ?
C15 C16 S3 110.9(5) . . ?
C18 C16 S3 119.1(6) . . ?
C14 C17 S3 112.6(6) . . ?
O3 C18 C19 121.8(7) . . ?
O3 C18 C16 118.4(7) . . ?
C19 C18 C16 119.8(7) . . ?
C32 C32 Cl1 107.2(13) 2_667 . ?
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 1.692(7) . ?
S1 C4 1.719(7) . ?
S2 C11 1.701(7) . ?
S2 C10 1.716(7) . ?
S3 C17 1.693(8) . ?
S3 C16 1.732(8) . ?
C9 C10 1.372(10) . ?
C9 C8 1.415(10) . ?
O1 C6 1.216(9) . ?
O2 C12 1.227(9) . ?
O3 C18 1.235(9) . ?
C1 C8 1.509(10) . ?
C1 C14 1.527(10) . ?
C1 C2 1.533(10) . ?
C2 C5 1.360(10) . ?
C2 C3 1.396(10) . ?
C3 C4 1.356(10) . ?
C4 C6 1.459(10) . ?
C6 C7 1.477(12) . ?
C8 C11 1.355(10) . ?
C10 C12 1.443(10) . ?
C12 C13 1.494(11) . ?
C14 C17 1.368(10) . ?
C14 C15 1.397(10) . ?
C15 C16 1.351(10) . ?
C16 C18 1.466(11) . ?
C18 C19 1.462(11) . ?
Cl1 C32 1.775(11) . ?
C32 C32 1.509(11) 2_667 ?
