#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:57:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178926 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/55/4115509.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_4115509
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            'C54 H44 N6 O6 S2'
_chemical_formula_weight         937.07
_chemical_name_common
'bis(guanidinium)-4,4'-biphenyldisulfonate, 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            4
_cell_length_a                   13.6864(7)
_cell_length_b                   12.4544(7)
_cell_length_c                   26.4727(14)
_cell_measurement_reflns_used    5160
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      47.1
_cell_measurement_theta_min      4.7
_cell_volume                     4512.4(4)
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0390
_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       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22842
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_type   'simulated psi-scans '
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0422
_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)+(0.0649P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                2676
_reflns_number_total             3975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0030257_11.cif
_cod_data_source_block           g:\travis\00164\00164
_cod_database_code               4115509
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 0.08331(4) 0.43971(4) 0.19362(2) 0.03545(18) Uani 1 1 d .
O1 O 0.17888(11) 0.48834(11) 0.20204(5) 0.0393(4) Uani 1 1 d .
N1 N 0.22711(15) 0.71032(14) 0.21637(7) 0.0438(5) Uani 1 1 d .
H1A H 0.2211 0.6415 0.2094 0.053 Uiso 1 1 calc R
H1B H 0.2822 0.7439 0.2097 0.053 Uiso 1 1 calc R
C1 C 0.05509(16) 0.46066(16) 0.12949(8) 0.0341(5) Uani 1 1 d .
O2 O 0.00618(12) 0.49115(11) 0.22282(5) 0.0417(4) Uani 1 1 d .
N2 N 0.07021(14) 0.71388(14) 0.24716(7) 0.0435(5) Uani 1 1 d .
H2A H 0.0213 0.7497 0.2606 0.052 Uiso 1 1 calc R
H2B H 0.0639 0.6450 0.2405 0.052 Uiso 1 1 calc R
C2 C -0.0362(2) 0.4379(3) 0.11124(10) 0.0731(9) Uani 1 1 d .
H2 H -0.0851 0.4115 0.1335 0.088 Uiso 1 1 calc R
O3 O 0.08562(11) 0.32410(11) 0.20169(5) 0.0375(4) Uani 1 1 d .
N3 N 0.16209(14) 0.86715(14) 0.24711(6) 0.0417(5) Uani 1 1 d .
H3A H 0.1130 0.9026 0.2606 0.050 Uiso 1 1 calc R
H3B H 0.2172 0.9006 0.2404 0.050 Uiso 1 1 calc R
C3 C -0.0575(2) 0.4529(3) 0.06101(10) 0.0759(10) Uani 1 1 d .
H3 H -0.1212 0.4362 0.0491 0.091 Uiso 1 1 calc R
C4 C 0.01139(16) 0.49169(16) 0.02723(8) 0.0354(5) Uani 1 1 d .
C5 C 0.10120(18) 0.5162(2) 0.04671(9) 0.0558(7) Uani 1 1 d .
H5 H 0.1500 0.5442 0.0249 0.067 Uiso 1 1 calc R
C6 C 0.12334(19) 0.5014(2) 0.09738(9) 0.0548(7) Uani 1 1 d .
H6 H 0.1864 0.5198 0.1097 0.066 Uiso 1 1 calc R
C7 C 0.15305(17) 0.76344(17) 0.23698(8) 0.0364(5) Uani 1 1 d .
C8 C 0.20243(19) -0.1847(2) 0.01869(9) 0.0519(7) Uani 1 1 d .
H8 H 0.2287 -0.2366 -0.0038 0.062 Uiso 1 1 calc R
C9 C 0.1984(2) -0.2081(2) 0.07028(10) 0.0605(8) Uani 1 1 d .
H9 H 0.2225 -0.2747 0.0825 0.073 Uiso 1 1 calc R
C10 C 0.1598(2) -0.1350(2) 0.10307(10) 0.0578(7) Uani 1 1 d .
H10 H 0.1557 -0.1523 0.1380 0.069 Uiso 1 1 calc R
C11 C 0.12621(17) -0.0350(2) 0.08621(9) 0.0454(6) Uani 1 1 d .
C12 C 0.09015(18) 0.0430(2) 0.12014(9) 0.0526(7) Uani 1 1 d .
H12 H 0.0862 0.0270 0.1552 0.063 Uiso 1 1 calc R
C13 C 0.06123(19) 0.1404(2) 0.10312(10) 0.0556(7) Uani 1 1 d .
H13 H 0.0379 0.1925 0.1264 0.067 Uiso 1 1 calc R
C14 C 0.06523(18) 0.1650(2) 0.05198(9) 0.0516(7) Uani 1 1 d .
H14 H 0.0443 0.2340 0.0410 0.062 Uiso 1 1 calc R
C15 C 0.09874(16) 0.09236(19) 0.01657(9) 0.0401(6) Uani 1 1 d .
C16 C 0.10246(17) 0.11698(19) -0.03799(9) 0.0422(6) Uani 1 1 d .
C17 C 0.06929(19) 0.2139(2) -0.05703(10) 0.0554(7) Uani 1 1 d .
H17 H 0.0451 0.2670 -0.0345 0.067 Uiso 1 1 calc R
C18 C 0.0710(2) 0.2349(2) -0.10932(12) 0.0658(8) Uani 1 1 d .
H18 H 0.0468 0.3015 -0.1217 0.079 Uiso 1 1 calc R
C19 C 0.1065(2) 0.1614(2) -0.14218(11) 0.0613(8) Uani 1 1 d .
H19 H 0.1079 0.1773 -0.1773 0.074 Uiso 1 1 calc R
C20 C 0.14134(18) 0.0619(2) -0.12488(9) 0.0506(7) Uani 1 1 d .
C21 C 0.1768(2) -0.0172(3) -0.15890(9) 0.0614(8) Uani 1 1 d .
H21 H 0.1789 -0.0022 -0.1941 0.074 Uiso 1 1 calc R
C22 C 0.2078(2) -0.1138(3) -0.14181(10) 0.0657(8) Uani 1 1 d .
H22 H 0.2310 -0.1661 -0.1650 0.079 Uiso 1 1 calc R
C23 C 0.20566(19) -0.1369(2) -0.09020(9) 0.0543(7) Uani 1 1 d .
H23 H 0.2277 -0.2052 -0.0789 0.065 Uiso 1 1 calc R
C24 C 0.17234(16) -0.06306(19) -0.05511(9) 0.0424(6) Uani 1 1 d .
C25 C 0.16915(17) -0.08791(19) -0.00053(8) 0.0416(6) Uani 1 1 d .
C26 C 0.13108(16) -0.00993(19) 0.03362(8) 0.0389(6) Uani 1 1 d .
C27 C 0.13911(17) 0.03819(19) -0.07237(8) 0.0422(6) Uani 1 1 d .
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_3
O2 S1 O3 111.89(9) .
O2 S1 O1 112.71(9) .
O3 S1 O1 111.64(9) .
O2 S1 C1 106.71(10) .
O3 S1 C1 107.02(9) .
O1 S1 C1 106.42(10) .
C6 C1 C2 118.9(2) .
C6 C1 S1 120.46(18) .
C2 C1 S1 120.65(18) .
C1 C2 C3 120.5(2) .
C2 C3 C4 121.8(2) .
C5 C4 C3 116.5(2) .
C5 C4 C4 121.5(3) 5_565
C3 C4 C4 122.0(3) 5_565
C4 C5 C6 122.1(2) .
C1 C6 C5 120.2(2) .
N2 C7 N3 119.7(2) .
N2 C7 N1 120.5(2) .
N3 C7 N1 119.8(2) .
C25 C8 C9 121.8(2) .
C10 C9 C8 119.9(2) .
C9 C10 C11 121.2(2) .
C10 C11 C12 121.6(2) .
C10 C11 C26 119.3(2) .
C12 C11 C26 119.1(2) .
C13 C12 C11 120.5(2) .
C12 C13 C14 120.8(2) .
C15 C14 C13 122.0(3) .
C14 C15 C26 118.3(2) .
C14 C15 C16 122.6(2) .
C26 C15 C16 119.0(2) .
C17 C16 C27 118.8(2) .
C17 C16 C15 121.7(2) .
C27 C16 C15 119.5(2) .
C16 C17 C18 120.9(3) .
C19 C18 C17 120.8(3) .
C18 C19 C20 120.6(3) .
C19 C20 C27 119.7(3) .
C19 C20 C21 121.4(2) .
C27 C20 C21 118.9(2) .
C22 C21 C20 120.8(2) .
C21 C22 C23 120.3(3) .
C24 C23 C22 121.7(3) .
C23 C24 C27 118.7(2) .
C23 C24 C25 121.8(2) .
C27 C24 C25 119.5(2) .
C8 C25 C26 118.7(2) .
C8 C25 C24 122.1(2) .
C26 C25 C24 119.2(2) .
C15 C26 C25 121.5(2) .
C15 C26 C11 119.4(2) .
C25 C26 C11 119.1(2) .
C24 C27 C20 119.6(2) .
C24 C27 C16 121.2(2) .
C20 C27 C16 119.2(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O2 1.4568(16) .
S1 O3 1.4559(15) .
S1 O1 1.4585(16) .
S1 C1 1.761(2) .
N1 C7 1.328(3) .
C1 C6 1.361(3) .
C1 C2 1.369(3) .
N2 C7 1.319(3) .
C2 C3 1.374(3) .
N3 C7 1.325(3) .
C3 C4 1.387(3) .
C4 C5 1.368(3) .
C4 C4 1.489(4) 5_565
C5 C6 1.387(3) .
C8 C25 1.385(3) .
C8 C9 1.397(3) .
C9 C10 1.364(4) .
C10 C11 1.401(4) .
C11 C12 1.412(3) .
C11 C26 1.429(3) .
C12 C13 1.353(4) .
C13 C14 1.389(3) .
C14 C15 1.382(3) .
C15 C26 1.422(3) .
C15 C16 1.477(3) .
C16 C17 1.385(3) .
C16 C27 1.429(3) .
C17 C18 1.409(4) .
C18 C19 1.353(4) .
C19 C20 1.405(4) .
C20 C27 1.421(3) .
C20 C21 1.421(4) .
C21 C22 1.353(4) .
C22 C23 1.396(3) .
C23 C24 1.385(3) .
C24 C27 1.416(3) .
C24 C25 1.478(3) .
C25 C26 1.425(3) .
