#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:57:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178926 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/55/4115516.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_4115516
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            'C16 H42 N6 O6 S2'
_chemical_formula_weight         478.68
_chemical_name_common
'bis(guanidinium) 1,8-octanedisulfonate, hexane clathrate '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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                   14.4260(11)
_cell_length_b                   7.4303(6)
_cell_length_c                   22.4383(17)
_cell_measurement_reflns_used    2216
_cell_measurement_temperature    173(2)
_cell_volume                     2405.2(3)
_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  0.1093
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17601
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.9895
_exptl_absorpt_correction_T_min  0.8663
_exptl_absorpt_correction_type   'simulated psi-scans '
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.106
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1601P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2372
_reflns_number_gt                1544
_reflns_number_total             2296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0030257_18.cif
_cod_data_source_block           d:\steve\00284\pnma284
_cod_database_code               4115516
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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_group
S1 S 0.32265(10) 0.2500 0.20807(6) 0.0597(5) Uani 1 2 d S .
O1 O 0.2730(2) 0.0895(3) 0.22585(11) 0.0672(8) Uani 1 1 d . .
S2 S 0.87045(9) 0.2500 0.54458(5) 0.0497(4) Uani 1 2 d S .
O2 O 0.3444(4) 0.2500 0.14445(19) 0.0925(16) Uani 1 2 d S .
O3 O 0.8466(3) 0.2500 0.60793(14) 0.0623(10) Uani 1 2 d S .
O4 O 0.91994(19) 0.4110(3) 0.52735(10) 0.0614(7) Uani 1 1 d . .
N4 N 1.1853(3) 0.2500 0.66594(17) 0.0572(12) Uani 1 2 d S .
H4A H 1.2047 0.1475 0.6811 0.069 Uiso 0.50 1 calc PR .
H4B H 1.2028 0.3525 0.6820 0.069 Uiso 0.50 1 calc PR .
N6 N 1.1037(2) 0.4038(4) 0.59536(12) 0.0584(9) Uani 1 1 d . .
H6A H 1.0686 0.4047 0.5633 0.070 Uiso 1 1 calc R .
H6B H 1.1215 0.5060 0.6116 0.070 Uiso 1 1 calc R .
N8 N 0.0963(3) 0.2500 0.41083(18) 0.0590(11) Uani 1 2 d S .
H8A H 0.0807 0.1475 0.4277 0.071 Uiso 0.50 1 calc PR .
H8B H 0.0831 0.3525 0.4285 0.071 Uiso 0.50 1 calc PR .
N9 N 0.1592(2) 0.0973(4) 0.33268(12) 0.0603(9) Uani 1 1 d . .
H9A H 0.1857 0.0975 0.2973 0.072 Uiso 1 1 calc R .
H9B H 0.1460 -0.0054 0.3503 0.072 Uiso 1 1 calc R .
C9 C 0.1395(3) 0.2500 0.3591(2) 0.0480(11) Uani 1 2 d S .
C10 C 1.1296(3) 0.2500 0.61904(19) 0.0463(11) Uani 1 2 d S .
C1A C 0.4352(9) 0.192(2) 0.2385(8) 0.085(5) Uani 0.38 1 d P 1
C2A C 0.4249(10) 0.175(3) 0.3029(6) 0.113(8) Uani 0.38 1 d P 1
C3A C 0.5301(13) 0.106(4) 0.3249(10) 0.140(8) Uani 0.38 1 d P 1
C4A C 0.5283(9) 0.056(3) 0.3857(7) 0.125(7) Uani 0.38 1 d P 1
C5A C 0.6278(8) 0.049(3) 0.4136(5) 0.103(5) Uani 0.38 1 d P 1
C6A C 0.6178(8) 0.040(2) 0.4821(6) 0.092(4) Uani 0.38 1 d P 1
C7A C 0.7133(8) 0.043(2) 0.5133(5) 0.070(3) Uani 0.38 1 d P 1
C8A C 0.7669(4) 0.2500 0.5035(3) 0.0825(19) Uani 1 2 d S .
C1B C 0.410(3) 0.2500 0.229(2) 0.088(15) Uiso 0.25 2 d SP 2
C2B C 0.414(2) 0.2500 0.2790(18) 0.067(8) Uiso 0.25 2 d SP 2
C4B C 0.514(3) 0.2500 0.3988(17) 0.120(11) Uiso 0.25 2 d SP 2
C5B C 0.619(3) 0.2500 0.423(2) 0.158(17) Uiso 0.25 2 d SP 2
C6B C 0.601(3) 0.165(5) 0.494(2) 0.089(13) Uiso 0.13 1 d P 2
C7B C 0.723(4) 0.140(7) 0.516(2) 0.085(15) Uiso 0.13 1 d P 2
C1S C 0.666(2) -0.2500 0.5092(14) 0.198(11) Uiso 0.50 2 d SP 3
C2S C 0.574(2) -0.2500 0.3907(15) 0.191(10) Uiso 0.50 2 d SP 3
C3S C 0.478(4) -0.2500 0.304(2) 0.139(14) Uiso 0.25 2 d SP 3
C4S C 0.514(3) -0.2500 0.2611(18) 0.112(10) Uiso 0.25 2 d SP 3
C5S C 0.623(2) -0.160(5) 0.4559(15) 0.167(13) Uiso 0.25 1 d P 3
C6S C 0.465(3) 0.016(5) 0.2651(14) 0.159(11) Uiso 0.25 1 d P 3
C7S C 0.558(3) -0.002(6) 0.3057(16) 0.156(13) Uiso 0.25 1 d P 3
C9S C 0.549(5) -0.184(9) 0.310(3) 0.14(2) Uiso 0.13 1 d P 3
C10S C 0.538(5) -0.133(11) 0.353(4) 0.15(2) Uiso 0.13 1 d P 3
C12S C 0.405(6) -0.2500 0.323(4) 0.24(3) Uiso 0.25 2 d SP 3
C3B C 0.527(3) 0.2500 0.328(2) 0.114(13) Uiso 0.25 2 d SP 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'
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
C1B S1 O1 111.6(10) . .
C1B S1 O1 111.6(10) . 8_565
O1 S1 O1 111.0(2) . 8_565
C1B S1 O2 98(2) . .
O1 S1 O2 112.05(15) . .
O1 S1 O2 112.05(15) 8_565 .
C1B S1 C1A 14.0(6) . 8_565
O1 S1 C1A 122.3(6) . 8_565
O1 S1 C1A 98.3(5) 8_565 8_565
O2 S1 C1A 100.1(7) . 8_565
C1B S1 C1A 14.0(6) . .
O1 S1 C1A 98.3(5) . .
O1 S1 C1A 122.3(6) 8_565 .
O2 S1 C1A 100.1(7) . .
C1A S1 C1A 27.4(10) 8_565 .
C1B S1 C2B 30(2) . .
O1 S1 C2B 96.0(6) . .
O1 S1 C2B 96.0(6) 8_565 .
O2 S1 C2B 127.8(10) . .
C1A S1 C2B 30.4(9) 8_565 .
C1A S1 C2B 30.4(9) . .
O4 S2 O4 111.7(2) . 8_565
O4 S2 O3 112.09(13) . .
O4 S2 O3 112.09(13) 8_565 .
O4 S2 C8A 106.23(17) . .
O4 S2 C8A 106.23(17) 8_565 .
O3 S2 C8A 108.1(3) . .
N9 C9 N9 119.8(4) . 8_565
N9 C9 N8 120.1(2) . .
N9 C9 N8 120.1(2) 8_565 .
N6 C10 N6 120.8(4) 8_565 .
N6 C10 N4 119.6(2) 8_565 .
N6 C10 N4 119.6(2) . .
C2A C1A C2A 39.3(17) . 8_565
C2A C1A S1 107.7(12) . .
C2A C1A S1 95.8(9) 8_565 .
C1A C2A C3A 103.1(14) . .
C4A C3A C2A 110.4(16) . .
C4A C3A C3A 105.3(13) . 8_565
C2A C3A C3A 72.3(11) . 8_565
C3A C4A C5A 112.2(14) . .
C6A C5A C4A 108.3(11) . .
C7A C6A C5A 111.5(10) . .
C6A C7A C8A 110.7(10) . .
C7B C8A C7B 99(5) . 8_565
C7B C8A C7A 13(3) . .
C7B C8A C7A 112(3) 8_565 .
C7B C8A C7A 112(3) . 8_565
C7B C8A C7A 13(3) 8_565 8_565
C7A C8A C7A 124.7(10) . 8_565
C7B C8A S2 112(3) . .
C7B C8A S2 112(3) 8_565 .
C7A C8A S2 108.2(4) . .
C7A C8A S2 108.2(4) 8_565 .
C2B C1B S1 113(4) . .
C1B C2B C3B 127(4) . .
C1B C2B S1 37(3) . .
C3B C2B S1 164(3) . .
C3B C4B C5B 103(3) . .
C4B C5B C6B 100(3) . 8_565
C4B C5B C6B 100(3) . .
C6B C5B C6B 43(3) 8_565 .
C5B C6B C7B 98(3) . .
C8A C7B C6B 115(4) . .
C5S C1S C5S 53(3) 8 .
C10S C2S C10S 83(7) 8 .
C10S C2S C5S 160(4) 8 .
C10S C2S C5S 116(4) . .
C10S C2S C5S 116(4) 8 8
C10S C2S C5S 160(4) . 8
C5S C2S C5S 45(3) . 8
C10S C2S C9S 59(5) 8 .
C10S C2S C9S 32(4) . .
C5S C2S C9S 140(3) . .
C5S C2S C9S 164(3) 8 .
C10S C2S C9S 32(4) 8 8
C10S C2S C9S 59(5) . 8
C5S C2S C9S 164(3) . 8
C5S C2S C9S 140(3) 8 8
C9S C2S C9S 30(4) . 8
C4S C3S C9S 71(5) . 8
C4S C3S C9S 71(5) . .
C9S C3S C9S 51(7) 8 .
C4S C3S C12S 140(7) . .
C9S C3S C12S 142(7) 8 .
C9S C3S C12S 142(7) . .
C4S C3S C10S 110(5) . .
C9S C3S C10S 72(5) 8 .
C9S C3S C10S 40(4) . .
C12S C3S C10S 104(6) . .
C4S C3S C10S 110(5) . 8
C9S C3S C10S 40(4) 8 8
C9S C3S C10S 72(5) . 8
C12S C3S C10S 104(6) . 8
C10S C3S C10S 64(6) . 8
C3S C4S C9S 56(3) . .
C3S C4S C9S 56(3) . 8
C9S C4S C9S 45(6) . 8
C5S C5S C1S 63.7(15) 8 .
C5S C5S C2S 67.7(13) 8 .
C1S C5S C2S 131(3) . .
C9S C7S C10S 43(4) . .
C9S C7S C6S 92(4) . .
C10S C7S C6S 107(4) . .
C10S C9S C9S 111(6) . 8
C10S C9S C3S 97(8) . .
C9S C9S C3S 64(3) 8 .
C10S C9S C4S 149(8) . .
C9S C9S C4S 68(3) 8 .
C3S C9S C4S 53(4) . .
C10S C9S C7S 74(6) . .
C9S C9S C7S 173(4) 8 .
C3S C9S C7S 121(5) . .
C4S C9S C7S 111(5) . .
C10S C9S C10S 75(8) . 8
C9S C9S C10S 36(3) 8 8
C3S C9S C10S 68(5) . 8
C4S C9S C10S 98(5) . 8
C7S C9S C10S 149(6) . 8
C10S C9S C2S 41(5) . .
C9S C9S C2S 75(2) 8 .
C3S C9S C2S 99(6) . .
C4S C9S C2S 141(5) . .
C7S C9S C2S 108(5) . .
C10S C9S C2S 42(3) 8 .
C9S C10S C2S 107(8) . .
C9S C10S C7S 63(6) . .
C2S C10S C7S 145(6) . .
C9S C10S C3S 43(5) . .
C2S C10S C3S 106(6) . .
C7S C10S C3S 88(5) . .
C9S C10S C9S 33(5) . 8
C2S C10S C9S 78(6) . 8
C7S C10S C9S 96(5) . 8
C3S C10S C9S 40(3) . 8
C9S C10S C10S 69(6) . 8
C2S C10S C10S 49(4) . 8
C7S C10S C10S 131(4) . 8
C3S C10S C10S 58(3) . 8
C9S C10S C10S 36(3) 8 8
C4B C3B C2B 117(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C1B 1.35(5) .
S1 O1 1.447(3) .
S1 O1 1.447(3) 8_565
S1 O2 1.461(4) .
S1 C1A 1.813(13) 8_565
S1 C1A 1.813(13) .
S1 C2B 2.07(4) .
S2 O4 1.446(2) .
S2 O4 1.446(2) 8_565
S2 O3 1.462(3) .
S2 C8A 1.756(6) .
N4 C10 1.324(6) .
N6 C10 1.315(3) .
N8 C9 1.318(6) .
N9 C9 1.311(4) .
C9 N9 1.311(4) 8_565
C10 N6 1.315(3) 8_565
C1A C2A 1.46(2) .
C1A C2A 1.76(2) 8_565
C2A C3A 1.67(2) .
C3A C4A 1.41(3) .
C3A C3A 2.14(5) 8_565
C4A C5A 1.568(16) .
C5A C6A 1.545(17) .
C6A C7A 1.546(15) .
C7A C8A 1.733(14) .
C8A C7B 1.07(5) .
C8A C7B 1.07(5) 8_565
C8A C7A 1.733(14) 8_565
C1B C2B 1.13(6) .
C2B C3B 1.96(6) .
C4B C3B 1.60(5) .
C4B C5B 1.61(6) .
C5B C6B 1.73(6) 8_565
C5B C6B 1.73(6) .
C6B C7B 1.83(7) .
C1S C5S 1.50(3) 8
C1S C5S 1.50(3) .
C2S C10S 1.32(7) 8
C2S C10S 1.32(7) .
C2S C5S 1.76(4) .
C2S C5S 1.76(4) 8
C2S C9S 1.91(8) .
C2S C9S 1.91(8) 8
C3S C4S 1.10(5) .
C3S C9S 1.14(6) 8
C3S C9S 1.14(6) .
C3S C12S 1.14(8) .
C3S C10S 1.64(8) .
C3S C10S 1.64(8) 8
C4S C9S 1.30(7) .
C4S C9S 1.30(7) 8
C5S C5S 1.33(7) 8
C6S C7S 1.63(5) .
C7S C9S 1.36(7) .
C7S C10S 1.47(8) .
C9S C10S 1.06(8) .
C9S C9S 0.99(14) 8
C9S C10S 1.68(10) 8
C10S C9S 1.68(10) 8
C10S C10S 1.74(17) 8
