#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:57:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178926 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/55/4115520.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_4115520
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            'C15 H32 N6 O8 S2'
_chemical_formula_weight         488.59
_chemical_name_common
'bis(guanidinium) mesitylenedisulfonate, aceteone and methanol clathrate  '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   7.5013(10)
_cell_length_b                   20.576(3)
_cell_length_c                   15.796(2)
_cell_measurement_reflns_used    3941
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.1
_cell_measurement_theta_min      4.7
_cell_volume                     2438.1(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6325
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.8450
_exptl_absorpt_correction_type   'simulated psi-scans '
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       needle
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1799
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          1.209
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0530P)²+0.2326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                1696
_reflns_number_total             1799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0030257_22.cif
_cod_data_source_block           g:\travis\00074\00074
_cod_database_code               4115520
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -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 1.0000 0.96835(4) 0.32364(6) 0.0252(2) Uani 1 2 d S
O1 O 1.0000 1.27082(11) 0.16810(17) 0.0295(6) Uani 1 2 d S
C1 C 1.0000 1.15893(18) 0.2504(2) 0.0257(8) Uani 1 2 d S
S2 S 1.0000 1.20076(4) 0.15074(5) 0.0234(2) Uani 1 2 d S
O2 O 1.1616(2) 1.18112(8) 0.10737(11) 0.0301(4) Uani 1 1 d .
C2 C 1.0000 1.08961(16) 0.2493(2) 0.0227(7) Uani 1 2 d S
O3 O 1.1616(2) 0.94906(8) 0.27856(12) 0.0294(4) Uani 1 1 d .
C3 C 1.0000 1.05575(16) 0.3268(3) 0.0266(7) Uani 1 2 d S
O4 O 1.0000 0.94413(13) 0.41003(18) 0.0340(6) Uani 1 2 d S
C4 C 1.0000 1.0883(2) 0.4041(3) 0.0397(10) Uani 1 2 d S
C5 C 1.0000 1.1557(2) 0.4011(3) 0.0404(10) Uani 1 2 d S
H5 H 1.0000 1.1783 0.4536 0.049 Uiso 1 2 calc SR
C6 C 1.0000 1.19248(16) 0.3284(3) 0.0317(8) Uani 1 2 d S
C7 C 1.0000 1.05338(17) 0.1656(2) 0.0276(8) Uani 1 2 d S
H7A H 1.0617 1.0117 0.1725 0.041 Uiso 0.50 1 calc PR
H7B H 1.0615 1.0795 0.1227 0.041 Uiso 0.50 1 calc PR
H7C H 0.8768 1.0455 0.1476 0.041 Uiso 0.50 1 calc PR
C8 C 1.0000 1.0576(2) 0.4925(3) 0.0693(18) Uani 1 2 d S
H8A H 0.9178 1.0206 0.4934 0.104 Uiso 0.50 1 calc PR
H8B H 0.9617 1.0899 0.5342 0.104 Uiso 0.50 1 calc PR
H8C H 1.1205 1.0426 0.5064 0.104 Uiso 0.50 1 calc PR
N9 N 1.3475(3) 1.33344(10) 0.17103(15) 0.0318(5) Uani 1 1 d .
H9A H 1.3473 1.3718 0.1958 0.038 Uiso 1 1 calc R
H9B H 1.2460 1.3142 0.1586 0.038 Uiso 1 1 calc R
C9 C 1.0000 1.26585(18) 0.3392(3) 0.0541(14) Uani 1 2 d S
H9C H 0.8837 1.2833 0.3225 0.081 Uiso 0.50 1 calc PR
H9D H 1.0932 1.2849 0.3035 0.081 Uiso 0.50 1 calc PR
H9E H 1.0231 1.2767 0.3986 0.081 Uiso 0.50 1 calc PR
N10 N 1.5000 1.24871(15) 0.1112(2) 0.0317(8) Uani 1 2 d S
H10A H 1.6015 1.2307 0.0961 0.038 Uiso 0.50 1 calc PR
H10B H 1.3985 1.2295 0.0988 0.038 Uiso 0.50 1 calc PR
C10 C 1.5000 0.91708(17) 0.4484(2) 0.0280(8) Uani 1 2 d S
N11 N 1.3469(3) 0.90731(11) 0.48768(15) 0.0359(6) Uani 1 1 d .
H11A H 1.3460 0.8941 0.5407 0.043 Uiso 1 1 calc R
H11B H 1.2457 0.9140 0.4609 0.043 Uiso 1 1 calc R
C11 C 1.5000 1.30480(15) 0.1525(3) 0.0265(7) Uani 1 2 d S
N14 N 1.5000 0.93680(16) 0.3682(2) 0.0314(8) Uani 1 2 d S
H14A H 1.6016 0.9433 0.3416 0.038 Uiso 0.50 1 calc PR
H14B H 1.3984 0.9434 0.3417 0.038 Uiso 0.50 1 calc PR
O1S O 0.5000 1.10057(14) 0.1578(2) 0.0461(7) Uani 1 2 d S
H1S H 0.4547 1.1270 0.1922 0.055 Uiso 0.50 1 calc PR
C1S C 0.5000 1.0393(3) 0.1928(5) 0.087(2) Uani 1 2 d S
H1S1 H 0.3992 1.0351 0.2319 0.130 Uiso 0.50 1 calc PR
H1S2 H 0.6117 1.0324 0.2237 0.130 Uiso 0.50 1 calc PR
H1S3 H 0.4892 1.0068 0.1478 0.130 Uiso 0.50 1 calc PR
O2S O 0.5000 1.1890(3) 0.2952(3) 0.1150(19) Uani 1 2 d S
C2S C 0.5000 1.2599(4) 0.4110(5) 0.116(3) Uani 1 2 d S
H2S1 H 0.4791 1.2932 0.3678 0.175 Uiso 0.50 1 calc PR
H2S2 H 0.6156 1.2676 0.4382 0.175 Uiso 0.50 1 calc PR
H2S3 H 0.4053 1.2620 0.4537 0.175 Uiso 0.50 1 calc PR
C3S C 0.5000 1.1943(4) 0.3706(4) 0.0784(19) Uani 1 2 d S
C4S C 0.5000 1.1369(5) 0.4274(7) 0.125(3) Uani 1 2 d S
H4S1 H 0.3773 1.1219 0.4357 0.187 Uiso 0.50 1 calc PR
H4S2 H 0.5517 1.1490 0.4821 0.187 Uiso 0.50 1 calc PR
H4S3 H 0.5710 1.1021 0.4018 0.187 Uiso 0.50 1 calc PR
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
O4 S1 O3 111.38(10) . .
O4 S1 O3 111.38(10) . 3_755
O3 S1 O3 112.16(15) . 3_755
O4 S1 C3 108.46(18) . .
O3 S1 C3 106.57(10) . .
O3 S1 C3 106.57(10) 3_755 .
C6 C1 C2 120.0(3) . .
C6 C1 S2 122.1(3) . .
C2 C1 S2 117.9(3) . .
O2 S2 O2 113.47(15) 3_755 .
O2 S2 O1 111.23(9) 3_755 .
O2 S2 O1 111.23(9) . .
O2 S2 C1 106.31(10) 3_755 .
O2 S2 C1 106.31(10) . .
O1 S2 C1 107.89(17) . .
C3 C2 C1 118.9(3) . .
C3 C2 C7 120.9(3) . .
C1 C2 C7 120.2(3) . .
C4 C3 C2 121.6(3) . .
C4 C3 S1 120.4(3) . .
C2 C3 S1 118.0(3) . .
C5 C4 C3 116.8(4) . .
C5 C4 C8 116.3(4) . .
C3 C4 C8 126.9(4) . .
C6 C5 C4 125.3(4) . .
C5 C6 C1 117.4(3) . .
C5 C6 C9 116.9(4) . .
C1 C6 C9 125.7(4) . .
N11 C10 N11 120.8(3) 3_855 .
N11 C10 N14 119.60(17) 3_855 .
N11 C10 N14 119.60(17) . .
N9 C11 N9 120.2(3) 3_855 .
N9 C11 N10 119.84(17) 3_855 .
N9 C11 N10 119.84(17) . .
O2S C3S C4S 122.1(8) . .
O2S C3S C2S 120.5(8) . .
C4S C3S C2S 117.4(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O4 1.453(3) .
S1 O3 1.4610(17) .
S1 O3 1.4610(17) 3_755
S1 C3 1.799(3) .
O1 S2 1.468(2) .
C1 C6 1.413(5) .
C1 C2 1.427(5) .
C1 S2 1.794(4) .
S2 O2 1.4501(18) 3_755
S2 O2 1.4501(18) .
C2 C3 1.409(5) .
C2 C7 1.517(5) .
C3 C4 1.393(6) .
C4 C5 1.388(6) .
C4 C8 1.533(6) .
C5 C6 1.375(6) .
C6 C9 1.519(5) .
N9 C11 1.320(3) .
N10 C11 1.326(5) .
C10 N11 1.321(3) 3_855
C10 N11 1.321(3) .
C10 N14 1.330(5) .
C11 N9 1.320(3) 3_855
O1S C1S 1.376(6) .
O2S C3S 1.196(7) .
C2S C3S 1.494(10) .
C3S C4S 1.482(11) .
