#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:57:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178926 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/55/4115514.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_4115514
loop_
_publ_author_name
'K. Travis Holman'
'Stephen M. Martin'
'Daniel P. Parker'
'Michael D. Ward'
_publ_section_title
;
 The Generality of Architectural Isomerism in Designer Inclusion
 Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4421
_journal_page_last               4431
_journal_paper_doi               10.1021/ja0030257
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C28 H22 N3 O3 S'
_chemical_formula_weight         480.55
_chemical_name_common
'bis(guanidinium) 2,6-anthracenedisulfonate, perylene clathrate  '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   13.7891(12)
_cell_length_b                   12.3034(10)
_cell_length_c                   26.784(2)
_cell_measurement_reflns_used    3136
_cell_measurement_temperature    173(2)
_cell_volume                     4544.0(6)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker (or Siemens)'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics
'XSEED, L. Barbour (1999); http://www.lbarbour.com/xseed'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART platform CCD, Bruker (or Siemens)'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22713
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.9946
_exptl_absorpt_correction_T_min  0.9683
_exptl_absorpt_correction_type   'simulated psi-scans '
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0439
_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)+(0.0516P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                2403
_reflns_number_total             4005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0030257_16.cif
_cod_data_source_block           g:\users\travis\n99098
_cod_original_cell_volume        4544.0(7)
_cod_database_code               4115514
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
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
S1 S 0.08604(5) 0.41948(5) 0.30637(2) 0.02667(17) Uani 1 1 d .
O1 O 0.18129(12) 0.47074(13) 0.30703(6) 0.0291(4) Uani 1 1 d .
O2 O 0.09254(12) 0.30272(12) 0.29641(6) 0.0307(4) Uani 1 1 d .
O3 O 0.01883(13) 0.47288(13) 0.27219(6) 0.0310(4) Uani 1 1 d .
C17 C 0.17189(18) 0.5843(2) 0.00559(9) 0.0281(6) Uani 1 1 d .
C6 C 0.08736(19) 0.47614(18) 0.40490(9) 0.0258(6) Uani 1 1 d .
H6 H 0.1528 0.4975 0.3997 0.031 Uiso 1 1 calc R
C1 C 0.03550(18) 0.43422(18) 0.36628(9) 0.0245(6) Uani 1 1 d .
N1 N -0.15507(16) 0.35782(16) 0.23960(7) 0.0352(6) Uani 1 1 d .
H1A H -0.2096 0.3913 0.2322 0.042 Uiso 1 1 calc R
H1B H -0.1064 0.3945 0.2526 0.042 Uiso 1 1 calc R
C3 C -0.10553(18) 0.4130(2) 0.41816(9) 0.0295(6) Uani 1 1 d .
H3 H -0.1711 0.3911 0.4223 0.035 Uiso 1 1 calc R
C4 C -0.05372(18) 0.45694(18) 0.45982(9) 0.0253(6) Uani 1 1 d .
C5 C 0.04511(18) 0.48848(18) 0.45297(9) 0.0238(6) Uani 1 1 d .
C26 C 0.09530(19) 0.3771(2) 0.03833(10) 0.0304(6) Uani 1 1 d .
C7 C -0.09630(18) 0.46901(18) 0.50663(9) 0.0273(6) Uani 1 1 d .
H7 H -0.1619 0.4477 0.5111 0.033 Uiso 1 1 calc R
C18 C 0.2082(2) 0.6823(2) -0.01163(10) 0.0341(7) Uani 1 1 d .
H18 H 0.2340 0.7327 0.0117 0.041 Uiso 1 1 calc R
C16 C 0.17193(18) 0.5556(2) 0.05881(9) 0.0296(6) Uani 1 1 d .
C21 C 0.13493(19) 0.5367(2) -0.08142(10) 0.0309(6) Uani 1 1 d .
C8 C -0.1462(2) 0.2515(2) 0.23113(9) 0.0298(6) Uani 1 1 d .
C25 C 0.09513(18) 0.4062(2) -0.01477(9) 0.0292(6) Uani 1 1 d .
C11 C 0.0946(2) 0.3234(2) 0.14079(11) 0.0441(8) Uani 1 1 d .
H11 H 0.0933 0.3048 0.1752 0.053 Uiso 1 1 calc R
N3 N -0.06437(16) 0.20218(16) 0.24269(8) 0.0369(6) Uani 1 1 d .
H3A H -0.0580 0.1319 0.2375 0.044 Uiso 1 1 calc R
H3B H -0.0161 0.2395 0.2556 0.044 Uiso 1 1 calc R
N2 N -0.21926(16) 0.19733(16) 0.21174(8) 0.0385(6) Uani 1 1 d .
H2A H -0.2140 0.1270 0.2063 0.046 Uiso 1 1 calc R
H2B H -0.2735 0.2314 0.2042 0.046 Uiso 1 1 calc R
C28 C 0.13394(18) 0.50903(19) -0.03000(9) 0.0270(6) Uani 1 1 d .
C2 C -0.06290(19) 0.40222(19) 0.37316(9) 0.0297(6) Uani 1 1 d .
H2 H -0.0986 0.3732 0.3459 0.036 Uiso 1 1 calc R
C27 C 0.13340(19) 0.4525(2) 0.07412(10) 0.0309(6) Uani 1 1 d .
C10 C 0.0593(2) 0.2527(2) 0.10610(12) 0.0474(8) Uani 1 1 d .
H10 H 0.0342 0.1844 0.1165 0.057 Uiso 1 1 calc R
C15 C 0.2096(2) 0.6239(2) 0.09502(10) 0.0382(7) Uani 1 1 d .
H15 H 0.2362 0.6919 0.0852 0.046 Uiso 1 1 calc R
C12 C 0.1333(2) 0.4249(2) 0.12547(10) 0.0372(7) Uani 1 1 d .
C13 C 0.1717(2) 0.4990(3) 0.16087(11) 0.0469(8) Uani 1 1 d .
H13 H 0.1711 0.4813 0.1954 0.056 Uiso 1 1 calc R
C20 C 0.1722(2) 0.6387(2) -0.09667(10) 0.0366(7) Uani 1 1 d .
H20 H 0.1721 0.6579 -0.1310 0.044 Uiso 1 1 calc R
C9 C 0.0595(2) 0.2791(2) 0.05567(11) 0.0401(7) Uani 1 1 d .
H9 H 0.0342 0.2283 0.0324 0.048 Uiso 1 1 calc R
C22 C 0.0972(2) 0.4624(2) -0.11700(11) 0.0377(7) Uani 1 1 d .
H22 H 0.0978 0.4806 -0.1515 0.045 Uiso 1 1 calc R
C24 C 0.0595(2) 0.3376(2) -0.05150(10) 0.0367(7) Uani 1 1 d .
H24 H 0.0336 0.2692 -0.0419 0.044 Uiso 1 1 calc R
C19 C 0.2080(2) 0.7093(2) -0.06223(10) 0.0375(7) Uani 1 1 d .
H19 H 0.2331 0.7776 -0.0727 0.045 Uiso 1 1 calc R
C23 C 0.0601(2) 0.3652(2) -0.10195(11) 0.0405(7) Uani 1 1 d .
H23 H 0.0346 0.3161 -0.1259 0.049 Uiso 1 1 calc R
C14 C 0.2095(2) 0.5958(3) 0.14538(11) 0.0468(8) Uani 1 1 d .
H14 H 0.2360 0.6446 0.1692 0.056 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 '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
O1 S1 O3 112.66(10) . .
O1 S1 O2 111.83(10) . .
O3 S1 O2 111.49(10) . .
O1 S1 C1 107.55(11) . .
O3 S1 C1 105.92(11) . .
O2 S1 C1 106.96(10) . .
C18 C17 C28 118.3(2) . .
C18 C17 C16 122.2(2) . .
C28 C17 C16 119.5(2) . .
C1 C6 C5 121.0(2) . .
C6 C1 C2 120.5(2) . .
C6 C1 S1 121.7(2) . .
C2 C1 S1 117.83(19) . .
C2 C3 C4 121.1(2) . .
C7 C4 C5 119.3(2) . .
C7 C4 C3 122.1(2) . .
C5 C4 C3 118.6(2) . .
C7 C5 C6 122.4(2) 5_566 .
C7 C5 C4 119.0(2) 5_566 .
C6 C5 C4 118.6(2) . .
C9 C26 C27 118.0(2) . .
C9 C26 C25 122.5(2) . .
C27 C26 C25 119.5(2) . .
C4 C7 C5 121.7(2) . 5_566
C17 C18 C19 122.0(2) . .
C15 C16 C27 118.4(2) . .
C15 C16 C17 122.2(2) . .
C27 C16 C17 119.3(2) . .
C20 C21 C22 120.7(3) . .
C20 C21 C28 119.7(2) . .
C22 C21 C28 119.6(2) . .
N2 C8 N3 121.0(2) . .
N2 C8 N1 119.6(2) . .
N3 C8 N1 119.4(2) . .
C24 C25 C28 117.9(2) . .
C24 C25 C26 122.7(2) . .
C28 C25 C26 119.4(2) . .
C10 C11 C12 119.9(3) . .
C21 C28 C17 119.3(2) . .
C21 C28 C25 119.4(2) . .
C17 C28 C25 121.3(2) . .
C3 C2 C1 120.3(2) . .
C12 C27 C26 119.6(2) . .
C12 C27 C16 119.3(2) . .
C26 C27 C16 121.1(2) . .
C11 C10 C9 120.8(3) . .
C16 C15 C14 121.8(3) . .
C27 C12 C11 119.5(3) . .
C27 C12 C13 119.7(3) . .
C11 C12 C13 120.9(3) . .
C14 C13 C12 120.0(3) . .
C19 C20 C21 120.2(3) . .
C26 C9 C10 122.1(3) . .
C23 C22 C21 120.3(3) . .
C25 C24 C23 122.5(3) . .
C20 C19 C18 120.5(3) . .
C22 C23 C24 120.3(3) . .
C13 C14 C15 120.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O1 1.4570(17) .
S1 O3 1.4591(16) .
S1 O2 1.4638(16) .
S1 C1 1.759(2) .
C17 C18 1.385(3) .
C17 C28 1.428(3) .
C17 C16 1.469(3) .
C6 C1 1.359(3) .
C6 C5 1.421(3) .
C1 C2 1.425(3) .
N1 C8 1.333(3) .
C3 C2 1.348(3) .
C3 C4 1.431(3) .
C4 C7 1.392(3) .
C4 C5 1.429(3) .
C5 C7 1.394(3) 5_566
C26 C9 1.383(3) .
C26 C27 1.433(3) .
C26 C25 1.466(3) .
C7 C5 1.394(3) 5_566
C18 C19 1.396(4) .
C16 C15 1.385(3) .
C16 C27 1.435(3) .
C21 C20 1.417(3) .
C21 C22 1.419(4) .
C21 C28 1.419(3) .
C8 N2 1.315(3) .
C8 N3 1.318(3) .
C25 C24 1.386(3) .
C25 C28 1.433(3) .
C11 C10 1.363(4) .
C11 C12 1.418(4) .
C27 C12 1.417(4) .
C10 C9 1.389(4) .
C15 C14 1.393(4) .
C12 C13 1.418(4) .
C13 C14 1.365(4) .
C20 C19 1.360(4) .
C22 C23 1.361(4) .
C24 C23 1.393(4) .
