
# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Chris Pigge'
_publ_contact_author_email       CHRIS-PIGGE@UIOWA.EDU

_publ_section_title              
;
A 1D crystalline organic polyrotaxane formed via hydrogen
bond-mediated self-assembly of a conformationally flexible
tri-carboxylic acid
;
loop_
_publ_author_name
'Chris Pigge'
'Mayuri K. Dighe'
'Dale C. Swenson'

# Attachment '6-DMF.cif'

data_fcp83z
_database_code_depnum_ccdc_archive 'CCDC 715817'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C30 H17 O9)-1, (C2 H8 N1)+1, 0.5(C3 H7 N1 O1), 0.595(H2 O1)'
_chemical_formula_sum            'C33.50 H29.69 N1.50 O10.10'
_chemical_formula_weight         614.80

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   ' C 2/c '
_symmetry_space_group_name_Hall  ' -C 2yc '

loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.7490(19)
_cell_length_b                   13.8366(15)
_cell_length_c                   25.634(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.396(5)
_cell_angle_gamma                90.00
_cell_volume                     6039.3(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    5337
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      25.0

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2576
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9831
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18610
_diffrn_reflns_av_R_equivalents  0.1191
_diffrn_reflns_av_sigmaI/netI    0.1278
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.3
_diffrn_reflns_theta_max         23.0
_reflns_number_total             4135
_reflns_number_gt                2071
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXTL v6.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL v6.1 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL v6.1 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.1 (Sheldrick, 2008)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Several low angle reflections were omitted from refinement due to beam
stop shadowing effects.

Few data above two-theta=46 were above background, thus were omitted from
the final cycles of refinement.

The dimethyl ammonium cation was disordered over three sites. The cation
was modelled as rigid groups (tetrahedral angles, C-N=1.50A, N-H=1.0A
methyl C-H=0.98A) with partial occupancy (restrained to sum to one).
A single overall isotropic displacement parameter (Uiso) was
used for the partial C and N atoms with the ammonium H atoms 1.2 times
and the methyl H atoms 1.5 times the Uiso.

A solvent molecule of DMF is situated near a two-fold axis and is
necessarily disordered. Bond distances were restrained to be
chemically reasonable (C-O=1.25A, C-N=1.35A, C-N=1.5A), an individual
isotropic displacement parameters were used and H atoms were added using
shelxl default values.

Water molecules were also present at two sites with partial occupancy.
The occupancy was refined for each site with an isotropic displacement
parameter for each. H atoms were not located or included.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0913P)²+2.5327P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4135
_refine_ls_number_parameters     404
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.2067
_refine_ls_wR_factor_gt          0.1652
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C1 C 0.5040(2) 0.1745(3) 0.4619(2) 0.0419(13) Uani 1 1 d . . .
C2 C 0.4606(2) 0.1598(3) 0.4081(2) 0.0450(13) Uani 1 1 d . . .
H2 H 0.4773 0.1889 0.3796 0.054 Uiso 1 1 calc R . .
C3 C 0.3939(2) 0.1037(3) 0.39551(19) 0.0411(12) Uani 1 1 d . . .
C4 C 0.3672(2) 0.0644(3) 0.43708(19) 0.0408(12) Uani 1 1 d . . .
H4 H 0.3214 0.0252 0.4285 0.049 Uiso 1 1 calc R . .
C5 C 0.4078(2) 0.0826(3) 0.49122(19) 0.0374(12) Uani 1 1 d . . .
C6 C 0.4778(2) 0.1353(3) 0.5029(2) 0.0435(13) Uani 1 1 d . . .
H6 H 0.5077 0.1442 0.5397 0.052 Uiso 1 1 calc R . .
C7 C 0.5828(3) 0.2236(4) 0.4761(2) 0.0568(15) Uani 1 1 d . . .
O7 O 0.63360(19) 0.1981(3) 0.51703(16) 0.0784(12) Uani 1 1 d . . .
C8 C 0.3508(3) 0.0890(4) 0.3370(2) 0.0496(14) Uani 1 1 d . . .
O8 O 0.3437(2) 0.1568(3) 0.30549(16) 0.0773(13) Uani 1 1 d . . .
C9 C 0.3801(3) 0.0452(3) 0.5371(2) 0.0467(13) Uani 1 1 d . . .
O9 O 0.42774(18) 0.0251(3) 0.58077(15) 0.0616(10) Uani 1 1 d . . .
C11 C 0.5978(3) 0.2982(4) 0.4388(2) 0.0512(14) Uani 1 1 d . . .
C12 C 0.5401(3) 0.3623(4) 0.4108(2) 0.0533(14) Uani 1 1 d . . .
H12 H 0.4885 0.3574 0.4146 0.064 Uiso 1 1 calc R . .
C13 C 0.5569(3) 0.4330(4) 0.3778(2) 0.0616(15) Uani 1 1 d . . .
C14 C 0.6321(4) 0.4375(5) 0.3715(3) 0.0774(18) Uani 1 1 d . . .
H14 H 0.6441 0.4847 0.3481 0.093 Uiso 1 1 calc R . .
C15 C 0.6893(4) 0.3739(5) 0.3989(3) 0.0764(19) Uani 1 1 d . . .
H15 H 0.7405 0.3777 0.3944 0.092 Uiso 1 1 calc R . .
C16 C 0.6730(3) 0.3053(4) 0.4328(2) 0.0674(17) Uani 1 1 d . . .
H16 H 0.7132 0.2627 0.4522 0.081 Uiso 1 1 calc R . .
C17 C 0.4969(4) 0.5048(5) 0.3492(3) 0.0742(18) Uani 1 1 d . . .
O17 O 0.5128(3) 0.5682(4) 0.3206(2) 0.1161(18) Uani 1 1 d . . .
O18 O 0.4287(2) 0.4973(2) 0.35829(15) 0.0697(11) Uani 1 1 d . . .
H18 H 0.4022 0.5474 0.3472 0.105 Uiso 1 1 calc R . .
C21 C 0.3192(3) -0.0077(4) 0.31744(19) 0.0456(13) Uani 1 1 d . . .
C22 C 0.3595(3) -0.0897(4) 0.34088(19) 0.0459(13) Uani 1 1 d . . .
H22 H 0.4061 -0.0838 0.3702 0.055 Uiso 1 1 calc R . .
C23 C 0.3319(3) -0.1805(4) 0.32151(19) 0.0452(13) Uani 1 1 d . . .
C24 C 0.2631(3) -0.1888(4) 0.2795(2) 0.0580(15) Uani 1 1 d . . .
H24 H 0.2430 -0.2509 0.2671 0.070 Uiso 1 1 calc R . .
C25 C 0.2238(3) -0.1068(4) 0.2557(2) 0.0620(16) Uani 1 1 d . . .
H25 H 0.1772 -0.1128 0.2265 0.074 Uiso 1 1 calc R . .
C26 C 0.2518(3) -0.0163(4) 0.2740(2) 0.0586(15) Uani 1 1 d . . .
H26 H 0.2252 0.0399 0.2570 0.070 Uiso 1 1 calc R . .
C27 C 0.3772(3) -0.2695(4) 0.3457(2) 0.0535(14) Uani 1 1 d . . .
O27 O 0.3483(2) -0.3509(3) 0.32809(15) 0.0712(12) Uani 1 1 d . . .
O28 O 0.4405(2) -0.2574(2) 0.38212(15) 0.0692(11) Uani 1 1 d . . .
C31 C 0.2937(2) 0.0334(4) 0.53043(19) 0.0452(13) Uani 1 1 d . . .
C32 C 0.2391(3) 0.0952(4) 0.4983(2) 0.0465(13) Uani 1 1 d . . .
H32 H 0.2557 0.1446 0.4783 0.056 Uiso 1 1 calc R . .
C33 C 0.1594(3) 0.0857(4) 0.4949(2) 0.0463(13) Uani 1 1 d . . .
C34 C 0.1357(3) 0.0134(4) 0.5237(2) 0.0570(15) Uani 1 1 d . . .
H34 H 0.0817 0.0064 0.5214 0.068 Uiso 1 1 calc R . .
C35 C 0.1907(3) -0.0495(4) 0.5562(2) 0.0618(15) Uani 1 1 d . . .
H35 H 0.1740 -0.0996 0.5757 0.074 Uiso 1 1 calc R . .
C36 C 0.2695(3) -0.0387(4) 0.5598(2) 0.0595(15) Uani 1 1 d . . .
H36 H 0.3072 -0.0807 0.5825 0.071 Uiso 1 1 calc R . .
C37 C 0.1026(3) 0.1527(4) 0.4581(2) 0.0511(14) Uani 1 1 d . . .
O37 O 0.12447(18) 0.2206(3) 0.43628(15) 0.0679(11) Uani 1 1 d . . .
O38 O 0.02869(18) 0.1304(2) 0.45228(14) 0.0622(10) Uani 1 1 d . . .
H38 H -0.0004 0.1676 0.4294 0.093 Uiso 1 1 calc R . .
O41 O -0.0150(7) 0.4995(10) 0.2210(4) 0.170(5) Uiso 0.50 1 d PD A -1
C42 C -0.0430(9) 0.5830(10) 0.2122(6) 0.133(6) Uiso 0.50 1 d PD A -1
H42 H -0.0893 0.5969 0.1839 0.159 Uiso 0.50 1 calc PR A -1
N43 N -0.0027(10) 0.6515(7) 0.2458(8) 0.123(3) Uiso 0.50 1 d PD A -1
C44 C 0.0719(8) 0.6452(14) 0.2911(7) 0.139(6) Uiso 0.50 1 d PD A -1
H44A H 0.0856 0.7094 0.3071 0.208 Uiso 0.50 1 calc PR A -1
H44B H 0.1141 0.6214 0.2768 0.208 Uiso 0.50 1 calc PR A -1
H44C H 0.0646 0.6007 0.3190 0.208 Uiso 0.50 1 calc PR A -1
C45 C -0.0284(8) 0.7543(8) 0.2352(7) 0.128(6) Uiso 0.50 1 d PD A -1
H45A H 0.0061 0.7960 0.2627 0.193 Uiso 0.50 1 calc PR A -1
H45B H -0.0826 0.7609 0.2369 0.193 Uiso 0.50 1 calc PR A -1
H45C H -0.0254 0.7732 0.1990 0.193 Uiso 0.50 1 calc PR A -1
N51 N 0.1622(8) 0.3002(13) 0.3466(11) 0.133(9) Uiso 0.347(7) 1 d PG B 2
C52 C 0.2497(8) 0.3023(15) 0.3702(9) 0.133 Uiso 0.347(7) 1 d PG B 2
H52A H 0.2676 0.2406 0.3882 0.199 Uiso 0.347(7) 1 calc PR B 2
H52B H 0.2642 0.3550 0.3967 0.199 Uiso 0.347(7) 1 calc PR B 2
H52C H 0.2746 0.3128 0.3410 0.199 Uiso 0.347(7) 1 calc PR B 2
C53 C 0.1348(12) 0.3946(15) 0.3190(9) 0.133 Uiso 0.347(7) 1 d PG B 2
H53A H 0.0776 0.3931 0.3036 0.199 Uiso 0.347(7) 1 calc PR B 2
H53B H 0.1596 0.4051 0.2898 0.199 Uiso 0.347(7) 1 calc PR B 2
H53C H 0.1492 0.4472 0.3455 0.199 Uiso 0.347(7) 1 calc PR B 2
H51 H 0.1369 0.2895 0.3764 0.160 Uiso 0.347(7) 1 d PG B 2
H52 H 0.1475 0.2465 0.3195 0.160 Uiso 0.347(7) 1 d PG B 2
N61 N 0.0846(10) 0.3207(14) 0.3321(8) 0.133 Uiso 0.373(8) 1 d PG C 3
C62 C 0.0524(10) 0.2609(17) 0.2819(8) 0.133 Uiso 0.373(8) 1 d PG C 3
H62A H -0.0048 0.2560 0.2743 0.199 Uiso 0.373(8) 1 calc PR C 3
H62B H 0.0755 0.1961 0.2877 0.199 Uiso 0.373(8) 1 calc PR C 3
H62C H 0.0654 0.2915 0.2511 0.199 Uiso 0.373(8) 1 calc PR C 3
C63 C 0.1722(10) 0.328(2) 0.3439(12) 0.133 Uiso 0.373(8) 1 d PG C 3
H63A H 0.1932 0.3673 0.3767 0.199 Uiso 0.373(8) 1 calc PR C 3
H63B H 0.1852 0.3589 0.3131 0.199 Uiso 0.373(8) 1 calc PR C 3
H63C H 0.1953 0.2635 0.3497 0.199 Uiso 0.373(8) 1 calc PR C 3
H61 H 0.0714 0.2894 0.3636 0.160 Uiso 0.373(8) 1 d PG C 3
H62 H 0.0610 0.3868 0.3262 0.160 Uiso 0.373(8) 1 d PG C 3
N71 N 0.0885(12) 0.2518(16) 0.3333(11) 0.133 Uiso 0.280(8) 1 d PG D 4
C72 C 0.1677(14) 0.222(2) 0.3288(12) 0.133 Uiso 0.280(8) 1 d PG D 4
H72A H 0.1770 0.1538 0.3395 0.199 Uiso 0.280(8) 1 calc PR D 4
H72B H 0.2083 0.2620 0.3528 0.199 Uiso 0.280(8) 1 calc PR D 4
H72C H 0.1693 0.2297 0.2912 0.199 Uiso 0.280(8) 1 calc PR D 4
C73 C 0.0741(17) 0.3558(16) 0.3170(13) 0.133 Uiso 0.280(8) 1 d PG D 4
H73A H 0.0224 0.3753 0.3200 0.199 Uiso 0.280(8) 1 calc PR D 4
H73B H 0.0757 0.3638 0.2793 0.199 Uiso 0.280(8) 1 calc PR D 4
H73C H 0.1147 0.3961 0.3410 0.199 Uiso 0.280(8) 1 calc PR D 4
H71 H 0.0869 0.2437 0.3718 0.199 Uiso 0.280(8) 1 d PG D 4
H72 H 0.0471 0.2107 0.3088 0.199 Uiso 0.280(8) 1 d PG D 4
O81 O 0.1210(9) 0.1543(11) 0.2792(6) 0.143(9) Uiso 0.397(18) 1 d P E 5
O82 O 0.0409(14) 0.184(2) 0.2526(11) 0.121(15) Uiso 0.198(16) 1 d P . 6


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 C6 1.376(6) . ?
C1 C2 1.392(6) . ?
C1 C7 1.504(6) . ?
C2 C3 1.375(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(6) . ?
C3 C8 1.493(6) . ?
C4 C5 1.394(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(6) . ?
C5 C9 1.490(6) . ?
C6 H6 0.9500 . ?
C7 O7 1.226(5) . ?
C7 C11 1.483(7) . ?
C8 O8 1.220(5) . ?
C8 C21 1.482(7) . ?
C9 O9 1.229(5) . ?
C9 C31 1.503(6) . ?
C11 C12 1.390(7) . ?
C11 C16 1.390(7) . ?
C12 C13 1.380(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(7) . ?
C13 C17 1.490(8) . ?
C14 C15 1.377(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 O17 1.227(7) . ?
C17 O18 1.300(7) . ?
O18 H18 0.8400 . ?
C21 C22 1.385(6) . ?
C21 C26 1.389(6) . ?
C22 C23 1.389(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(6) . ?
C23 C27 1.505(7) . ?
C24 C25 1.380(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 O28 1.253(5) . ?
C27 O27 1.268(6) . ?
C31 C32 1.378(6) . ?
C31 C36 1.390(7) . ?
C32 C33 1.398(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(7) . ?
C33 C37 1.493(7) . ?
C34 C35 1.394(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 O37 1.211(6) . ?
C37 O38 1.315(5) . ?
O38 H38 0.8400 . ?
O41 C42 1.252(5) . ?
C42 N43 1.343(5) . ?
C42 H42 0.9500 . ?
N43 C45 1.494(5) . ?
N43 C44 1.495(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
N51 C52 1.5000 . ?
N51 C53 1.5000 . ?
N51 H51 1.0000 . ?
N51 H52 1.0000 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
N61 C62 1.5000 . ?
N61 C63 1.5000 . ?
N61 H61 1.0000 . ?
N61 H62 1.0000 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
N71 C72 1.5000 . ?
N71 C73 1.5000 . ?
N71 H71 1.0000 . ?
N71 H72 1.0000 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?

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
C6 C1 C2 119.2(4) . . ?
C6 C1 C7 118.9(4) . . ?
C2 C1 C7 121.6(5) . . ?
C3 C2 C1 120.9(5) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 C8 118.4(4) . . ?
C4 C3 C8 121.8(4) . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 C9 122.1(4) . . ?
C6 C5 C9 118.9(4) . . ?
C1 C6 C5 120.9(4) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
O7 C7 C11 122.0(4) . . ?
O7 C7 C1 119.1(5) . . ?
C11 C7 C1 118.8(5) . . ?
O8 C8 C21 120.8(5) . . ?
O8 C8 C3 119.2(5) . . ?
C21 C8 C3 120.0(5) . . ?
O9 C9 C5 120.1(4) . . ?
O9 C9 C31 119.8(5) . . ?
C5 C9 C31 120.1(4) . . ?
C12 C11 C16 119.3(5) . . ?
C12 C11 C7 122.5(5) . . ?
C16 C11 C7 118.2(5) . . ?
C13 C12 C11 120.9(5) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 118.9(6) . . ?
C12 C13 C17 121.8(6) . . ?
C14 C13 C17 119.3(6) . . ?
C15 C14 C13 120.3(6) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 120.7(6) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C11 119.9(6) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
O17 C17 O18 123.2(7) . . ?
O17 C17 C13 121.2(7) . . ?
O18 C17 C13 115.5(6) . . ?
C17 O18 H18 109.5 . . ?
C22 C21 C26 120.0(5) . . ?
C22 C21 C8 119.5(4) . . ?
C26 C21 C8 120.4(5) . . ?
C21 C22 C23 119.9(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 119.8(5) . . ?
C24 C23 C27 120.2(5) . . ?
C22 C23 C27 119.9(4) . . ?
C25 C24 C23 119.9(5) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 120.5(5) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.7(5) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
O28 C27 O27 124.9(5) . . ?
O28 C27 C23 117.4(5) . . ?
O27 C27 C23 117.7(4) . . ?
C32 C31 C36 119.8(4) . . ?
C32 C31 C9 121.5(5) . . ?
C36 C31 C9 118.5(4) . . ?
C31 C32 C33 120.4(5) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 119.4(5) . . ?
C34 C33 C37 122.4(5) . . ?
C32 C33 C37 118.1(5) . . ?
C33 C34 C35 120.4(5) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C36 C35 C34 119.8(5) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C31 120.1(5) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
O37 C37 O38 124.7(5) . . ?
O37 C37 C33 121.8(4) . . ?
O38 C37 C33 113.6(5) . . ?
C37 O38 H38 109.5 . . ?
O41 C42 N43 115.1(15) . . ?
O41 C42 H42 122.5 . . ?
N43 C42 H42 122.5 . . ?
C42 N43 C45 118.3(12) . . ?
C42 N43 C44 130.6(15) . . ?
C45 N43 C44 110.8(13) . . ?
N43 C44 H44A 109.5 . . ?
N43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N43 C45 H45A 109.5 . . ?
N43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C52 N51 C53 109.5 . . ?
C52 N51 H51 109.4 . . ?
C53 N51 H51 109.4 . . ?
C52 N51 H52 109.4 . . ?
C53 N51 H52 109.4 . . ?
H51 N51 H52 109.5 . . ?
N51 C52 H52A 109.5 . . ?
N51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N51 C53 H53A 109.5 . . ?
N51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
N51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C62 N61 C63 109.5 . . ?
N61 C62 H62A 109.5 . . ?
N61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
N61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N61 C63 H63A 109.5 . . ?
N61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
N61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C72 N71 C73 109.5 . . ?
H52 N71 H72 109.2 . . ?
N71 C72 H72A 109.5 . . ?
H52 C72 H72A 145.6 . . ?
N71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
N71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N71 C73 H73A 109.5 . . ?
N71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
N71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.6(7) . . . . ?
C7 C1 C2 C3 171.2(4) . . . . ?
C1 C2 C3 C4 2.9(7) . . . . ?
C1 C2 C3 C8 -178.8(4) . . . . ?
C2 C3 C4 C5 0.5(7) . . . . ?
C8 C3 C4 C5 -177.8(4) . . . . ?
C3 C4 C5 C6 -4.0(6) . . . . ?
C3 C4 C5 C9 177.7(4) . . . . ?
C2 C1 C6 C5 -1.1(7) . . . . ?
C7 C1 C6 C5 -175.1(4) . . . . ?
C4 C5 C6 C1 4.4(6) . . . . ?
C9 C5 C6 C1 -177.3(4) . . . . ?
C6 C1 C7 O7 27.7(7) . . . . ?
C2 C1 C7 O7 -146.1(5) . . . . ?
C6 C1 C7 C11 -155.2(5) . . . . ?
C2 C1 C7 C11 31.0(7) . . . . ?
C2 C3 C8 O8 -39.9(6) . . . . ?
C4 C3 C8 O8 138.4(5) . . . . ?
C2 C3 C8 C21 138.4(5) . . . . ?
C4 C3 C8 C21 -43.2(6) . . . . ?
C4 C5 C9 O9 149.0(4) . . . . ?
C6 C5 C9 O9 -29.3(7) . . . . ?
C4 C5 C9 C31 -31.9(7) . . . . ?
C6 C5 C9 C31 149.9(4) . . . . ?
O7 C7 C11 C12 -146.5(5) . . . . ?
C1 C7 C11 C12 36.5(7) . . . . ?
O7 C7 C11 C16 31.9(7) . . . . ?
C1 C7 C11 C16 -145.1(5) . . . . ?
C16 C11 C12 C13 -0.5(7) . . . . ?
C7 C11 C12 C13 177.8(5) . . . . ?
C11 C12 C13 C14 1.9(7) . . . . ?
C11 C12 C13 C17 -177.5(5) . . . . ?
C12 C13 C14 C15 -1.6(8) . . . . ?
C17 C13 C14 C15 177.8(5) . . . . ?
C13 C14 C15 C16 0.0(9) . . . . ?
C14 C15 C16 C11 1.4(9) . . . . ?
C12 C11 C16 C15 -1.1(8) . . . . ?
C7 C11 C16 C15 -179.5(5) . . . . ?
C12 C13 C17 O17 178.9(6) . . . . ?
C14 C13 C17 O17 -0.5(8) . . . . ?
C12 C13 C17 O18 1.1(8) . . . . ?
C14 C13 C17 O18 -178.3(5) . . . . ?
O8 C8 C21 C22 144.5(5) . . . . ?
C3 C8 C21 C22 -33.9(7) . . . . ?
O8 C8 C21 C26 -32.1(7) . . . . ?
C3 C8 C21 C26 149.6(5) . . . . ?
C26 C21 C22 C23 -1.1(7) . . . . ?
C8 C21 C22 C23 -177.6(4) . . . . ?
C21 C22 C23 C24 -1.3(7) . . . . ?
C21 C22 C23 C27 178.0(4) . . . . ?
C22 C23 C24 C25 2.4(7) . . . . ?
C27 C23 C24 C25 -176.9(5) . . . . ?
C23 C24 C25 C26 -1.1(8) . . . . ?
C24 C25 C26 C21 -1.3(8) . . . . ?
C22 C21 C26 C25 2.4(8) . . . . ?
C8 C21 C26 C25 178.9(5) . . . . ?
C24 C23 C27 O28 177.3(5) . . . . ?
C22 C23 C27 O28 -2.0(7) . . . . ?
C24 C23 C27 O27 -3.2(7) . . . . ?
C22 C23 C27 O27 177.5(5) . . . . ?
O9 C9 C31 C32 145.9(5) . . . . ?
C5 C9 C31 C32 -33.3(7) . . . . ?
O9 C9 C31 C36 -30.7(7) . . . . ?
C5 C9 C31 C36 150.1(5) . . . . ?
C36 C31 C32 C33 -0.2(7) . . . . ?
C9 C31 C32 C33 -176.8(4) . . . . ?
C31 C32 C33 C34 -0.5(7) . . . . ?
C31 C32 C33 C37 -178.2(4) . . . . ?
C32 C33 C34 C35 0.3(7) . . . . ?
C37 C33 C34 C35 177.9(5) . . . . ?
C33 C34 C35 C36 0.6(8) . . . . ?
C34 C35 C36 C31 -1.2(8) . . . . ?
C32 C31 C36 C35 1.0(8) . . . . ?
C9 C31 C36 C35 177.7(5) . . . . ?
C34 C33 C37 O37 174.2(5) . . . . ?
C32 C33 C37 O37 -8.2(7) . . . . ?
C34 C33 C37 O38 -5.8(7) . . . . ?
C32 C33 C37 O38 171.8(4) . . . . ?
O41 C42 N43 C45 174.9(18) . . . . ?
O41 C42 N43 C44 2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        23.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.055

# Attachment '6-polyrotaxane.cif'

data_fcp86
_database_code_depnum_ccdc_archive 'CCDC 715818'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H18 O9'
_chemical_formula_sum            'C30 H18 O9'
_chemical_formula_weight         522.44

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4264(8)
_cell_length_b                   11.3620(12)
_cell_length_c                   15.2805(16)
_cell_angle_alpha                103.301(5)
_cell_angle_beta                 94.507(5)
_cell_angle_gamma                108.265(5)
_cell_volume                     1175.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    5259
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale orange'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.9593
_exptl_absorpt_correction_T_max  0.9772
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28836
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.4
_diffrn_reflns_theta_max         25.0
_reflns_number_total             4135
_reflns_number_gt                3069
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV< 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXTL v6.2 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL v6.2 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL v6.2 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.2 (Sheldrick, 2008)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Data above 25 degrees theta were excluded from the final cycles of
refinement due to the paucity of data above the noise level. Several low
angle reflections were excluded due to beam-stop shadowing effects.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0725P)²+0.2722P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4135
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1331
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C1 C 0.8009(3) -0.05206(18) 0.60156(13) 0.0318(5) Uani 1 1 d . . .
C2 C 0.9789(3) -0.04269(18) 0.64499(13) 0.0324(5) Uani 1 1 d . . .
H2 H 1.0853 0.0345 0.6549 0.039 Uiso 1 1 calc R . .
C3 C 1.0023(3) -0.14506(18) 0.67390(13) 0.0318(5) Uani 1 1 d . . .
C4 C 0.8433(3) -0.25581(18) 0.66109(13) 0.0308(4) Uani 1 1 d . . .
H4 H 0.8589 -0.3272 0.6791 0.037 Uiso 1 1 calc R . .
C5 C 0.6622(3) -0.26445(18) 0.62260(13) 0.0309(4) Uani 1 1 d . . .
C6 C 0.6428(3) -0.16282(18) 0.59063(13) 0.0325(5) Uani 1 1 d . . .
H6 H 0.5212 -0.1692 0.5613 0.039 Uiso 1 1 calc R . .
C7 C 0.7793(3) 0.05176(19) 0.55974(14) 0.0335(5) Uani 1 1 d . . .
O7 O 0.6973(2) 0.02170(14) 0.48110(10) 0.0440(4) Uani 1 1 d . . .
C8 C 1.1905(3) -0.14775(19) 0.71457(14) 0.0353(5) Uani 1 1 d . . .
O8 O 1.2303(2) -0.24495(14) 0.68776(12) 0.0520(4) Uani 1 1 d . . .
C9 C 0.4925(3) -0.38641(19) 0.60645(14) 0.0334(5) Uani 1 1 d . . .
O9 O 0.3607(2) -0.41410(14) 0.54404(10) 0.0436(4) Uani 1 1 d . . .
C11 C 0.8629(3) 0.18926(19) 0.61411(14) 0.0322(5) Uani 1 1 d . . .
C12 C 0.9202(3) 0.22471(18) 0.70799(14) 0.0329(5) Uani 1 1 d . . .
H12 H 0.9045 0.1602 0.7396 0.039 Uiso 1 1 calc R . .
C13 C 1.0000(3) 0.35318(18) 0.75576(14) 0.0334(5) Uani 1 1 d . . .
C14 C 1.0202(3) 0.44801(19) 0.70965(15) 0.0372(5) Uani 1 1 d . . .
H14 H 1.0760 0.5363 0.7421 0.045 Uiso 1 1 calc R . .
C15 C 0.9589(3) 0.4134(2) 0.61672(15) 0.0381(5) Uani 1 1 d . . .
H15 H 0.9700 0.4782 0.5857 0.046 Uiso 1 1 calc R . .
C16 C 0.8816(3) 0.28519(19) 0.56856(14) 0.0359(5) Uani 1 1 d . . .
H16 H 0.8411 0.2621 0.5045 0.043 Uiso 1 1 calc R . .
C17 C 1.0707(3) 0.38873(19) 0.85460(15) 0.0390(5) Uani 1 1 d . . .
O17 O 1.0585(2) 0.30349(14) 0.89549(10) 0.0477(4) Uani 1 1 d . . .
O18 O 1.1460(3) 0.51020(14) 0.89407(11) 0.0571(5) Uani 1 1 d . . .
H18 H 1.1984 0.5212 0.9475 0.086 Uiso 1 1 calc R . .
C21 C 1.3190(3) -0.03958(18) 0.79102(14) 0.0327(5) Uani 1 1 d . . .
C22 C 1.4947(3) -0.04740(19) 0.82365(14) 0.0352(5) Uani 1 1 d . . .
H22 H 1.5345 -0.1151 0.7925 0.042 Uiso 1 1 calc R . .
C23 C 1.6115(3) 0.04258(19) 0.90091(14) 0.0362(5) Uani 1 1 d . . .
C24 C 1.5549(3) 0.1427(2) 0.94600(15) 0.0420(5) Uani 1 1 d . . .
H24 H 1.6352 0.2052 0.9986 0.050 Uiso 1 1 calc R . .
C25 C 1.3807(3) 0.1511(2) 0.91396(15) 0.0423(5) Uani 1 1 d . . .
H25 H 1.3418 0.2195 0.9448 0.051 Uiso 1 1 calc R . .
C26 C 1.2632(3) 0.06049(19) 0.83728(14) 0.0363(5) Uani 1 1 d . . .
H26 H 1.1436 0.0666 0.8161 0.044 Uiso 1 1 calc R . .
C27 C 1.7888(3) 0.0273(2) 0.93943(15) 0.0391(5) Uani 1 1 d . . .
O27 O 1.8330(2) -0.06807(16) 0.89886(11) 0.0529(4) Uani 1 1 d . . .
O28 O 1.8846(2) 0.10852(15) 1.01323(11) 0.0531(4) Uani 1 1 d . . .
H28 H 1.9714 0.0841 1.0332 0.080 Uiso 1 1 calc R . .
C31 C 0.4960(3) -0.47659(18) 0.66359(14) 0.0327(5) Uani 1 1 d . . .
C32 C 0.5811(3) -0.43579(18) 0.75431(13) 0.0326(5) Uani 1 1 d . . .
H32 H 0.6333 -0.3465 0.7845 0.039 Uiso 1 1 calc R . .
C33 C 0.5900(3) -0.52604(19) 0.80106(14) 0.0343(5) Uani 1 1 d . . .
C34 C 0.5139(3) -0.65695(19) 0.75684(14) 0.0394(5) Uani 1 1 d . . .
H34 H 0.5231 -0.7183 0.7884 0.047 Uiso 1 1 calc R . .
C35 C 0.4254(3) -0.69736(19) 0.66723(14) 0.0398(5) Uani 1 1 d . . .
H35 H 0.3724 -0.7867 0.6371 0.048 Uiso 1 1 calc R . .
C36 C 0.4137(3) -0.60830(19) 0.62144(14) 0.0366(5) Uani 1 1 d . . .
H36 H 0.3488 -0.6368 0.5603 0.044 Uiso 1 1 calc R . .
C37 C 0.6892(3) -0.4852(2) 0.89607(15) 0.0405(5) Uani 1 1 d . . .
O37 O 0.6927(3) -0.56644(15) 0.93772(11) 0.0650(5) Uani 1 1 d . . .
O38 O 0.7742(2) -0.36309(13) 0.93168(11) 0.0513(4) Uani 1 1 d . . .
H38 H 0.8343 -0.3504 0.9838 0.077 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 C2 1.393(3) . ?
C1 C6 1.392(3) . ?
C1 C7 1.508(3) . ?
C2 C3 1.389(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(3) . ?
C3 C8 1.497(3) . ?
C4 C5 1.389(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(3) . ?
C5 C9 1.506(3) . ?
C6 H6 0.9500 . ?
C7 O7 1.224(2) . ?
C7 C11 1.493(3) . ?
C8 O8 1.221(2) . ?
C8 C21 1.488(3) . ?
C9 O9 1.220(2) . ?
C9 C31 1.496(3) . ?
C11 C12 1.390(3) . ?
C11 C16 1.400(3) . ?
C12 C13 1.384(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(3) . ?
C13 C17 1.477(3) . ?
C14 C15 1.381(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 O17 1.252(2) . ?
C17 O18 1.289(2) . ?
O18 H18 0.8400 . ?
C21 C26 1.391(3) . ?
C21 C22 1.396(3) . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(3) . ?
C23 C27 1.476(3) . ?
C24 C25 1.386(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 O28 1.270(3) . ?
C27 O27 1.270(3) . ?
O28 H28 0.8400 . ?
C31 C32 1.385(3) . ?
C31 C36 1.396(3) . ?
C32 C33 1.392(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.392(3) . ?
C33 C37 1.474(3) . ?
C34 C35 1.378(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.376(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 O37 1.241(3) . ?
C37 O38 1.292(2) . ?
O38 H38 0.8400 . ?

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
C2 C1 C6 119.73(18) . . ?
C2 C1 C7 121.05(17) . . ?
C6 C1 C7 119.06(18) . . ?
C3 C2 C1 120.67(17) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 118.76(18) . . ?
C2 C3 C8 124.47(17) . . ?
C4 C3 C8 116.70(17) . . ?
C5 C4 C3 121.49(18) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 118.92(17) . . ?
C4 C5 C9 120.94(17) . . ?
C6 C5 C9 119.85(18) . . ?
C1 C6 C5 120.26(18) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
O7 C7 C11 121.30(18) . . ?
O7 C7 C1 119.22(17) . . ?
C11 C7 C1 119.45(17) . . ?
O8 C8 C21 120.42(18) . . ?
O8 C8 C3 118.26(18) . . ?
C21 C8 C3 121.12(17) . . ?
O9 C9 C31 121.00(17) . . ?
O9 C9 C5 120.05(18) . . ?
C31 C9 C5 118.80(17) . . ?
C12 C11 C16 119.24(18) . . ?
C12 C11 C7 122.26(17) . . ?
C16 C11 C7 118.49(18) . . ?
C13 C12 C11 120.54(18) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.79(19) . . ?
C12 C13 C17 119.70(17) . . ?
C14 C13 C17 120.46(18) . . ?
C15 C14 C13 119.92(19) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.46(18) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 120.02(19) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
O17 C17 O18 123.4(2) . . ?
O17 C17 C13 120.50(18) . . ?
O18 C17 C13 116.09(18) . . ?
C17 O18 H18 109.5 . . ?
C26 C21 C22 118.87(19) . . ?
C26 C21 C8 122.94(18) . . ?
C22 C21 C8 117.79(18) . . ?
C23 C22 C21 120.71(19) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 119.83(19) . . ?
C22 C23 C27 120.32(19) . . ?
C24 C23 C27 119.70(19) . . ?
C25 C24 C23 119.8(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C26 C25 C24 120.3(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 120.47(19) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
O28 C27 O27 123.9(2) . . ?
O28 C27 C23 117.6(2) . . ?
O27 C27 C23 118.39(19) . . ?
C27 O28 H28 109.5 . . ?
C32 C31 C36 119.18(18) . . ?
C32 C31 C9 123.33(17) . . ?
C36 C31 C9 117.46(18) . . ?
C31 C32 C33 119.80(18) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 120.19(19) . . ?
C34 C33 C37 118.83(18) . . ?
C32 C33 C37 120.89(17) . . ?
C35 C34 C33 119.90(19) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C36 C35 C34 119.94(19) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 120.90(19) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
O37 C37 O38 122.7(2) . . ?
O37 C37 C33 120.33(18) . . ?
O38 C37 C33 116.92(18) . . ?
C37 O38 H38 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 2.9(3) . . . . ?
C7 C1 C2 C3 -172.44(18) . . . . ?
C1 C2 C3 C4 -1.9(3) . . . . ?
C1 C2 C3 C8 175.11(19) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C8 C3 C4 C5 -179.02(18) . . . . ?
C3 C4 C5 C6 4.4(3) . . . . ?
C3 C4 C5 C9 178.10(19) . . . . ?
C2 C1 C6 C5 -0.3(3) . . . . ?
C7 C1 C6 C5 175.15(18) . . . . ?
C4 C5 C6 C1 -3.3(3) . . . . ?
C9 C5 C6 C1 -177.08(18) . . . . ?
C2 C1 C7 O7 129.5(2) . . . . ?
C6 C1 C7 O7 -45.9(3) . . . . ?
C2 C1 C7 C11 -48.9(3) . . . . ?
C6 C1 C7 C11 135.70(19) . . . . ?
C2 C3 C8 O8 -134.7(2) . . . . ?
C4 C3 C8 O8 42.3(3) . . . . ?
C2 C3 C8 C21 50.3(3) . . . . ?
C4 C3 C8 C21 -132.7(2) . . . . ?
C4 C5 C9 O9 -150.8(2) . . . . ?
C6 C5 C9 O9 22.9(3) . . . . ?
C4 C5 C9 C31 24.7(3) . . . . ?
C6 C5 C9 C31 -161.62(18) . . . . ?
O7 C7 C11 C12 166.2(2) . . . . ?
C1 C7 C11 C12 -15.4(3) . . . . ?
O7 C7 C11 C16 -13.1(3) . . . . ?
C1 C7 C11 C16 165.30(18) . . . . ?
C16 C11 C12 C13 -1.8(3) . . . . ?
C7 C11 C12 C13 178.88(19) . . . . ?
C11 C12 C13 C14 1.1(3) . . . . ?
C11 C12 C13 C17 -176.34(19) . . . . ?
C12 C13 C14 C15 0.6(3) . . . . ?
C17 C13 C14 C15 177.99(19) . . . . ?
C13 C14 C15 C16 -1.5(3) . . . . ?
C14 C15 C16 C11 0.7(3) . . . . ?
C12 C11 C16 C15 0.9(3) . . . . ?
C7 C11 C16 C15 -179.78(19) . . . . ?
C12 C13 C17 O17 -0.2(3) . . . . ?
C14 C13 C17 O17 -177.6(2) . . . . ?
C12 C13 C17 O18 178.9(2) . . . . ?
C14 C13 C17 O18 1.5(3) . . . . ?
O8 C8 C21 C26 -165.8(2) . . . . ?
C3 C8 C21 C26 9.1(3) . . . . ?
O8 C8 C21 C22 6.9(3) . . . . ?
C3 C8 C21 C22 -178.24(18) . . . . ?
C26 C21 C22 C23 0.2(3) . . . . ?
C8 C21 C22 C23 -172.83(19) . . . . ?
C21 C22 C23 C24 -0.8(3) . . . . ?
C21 C22 C23 C27 174.74(18) . . . . ?
C22 C23 C24 C25 0.7(3) . . . . ?
C27 C23 C24 C25 -174.82(19) . . . . ?
C23 C24 C25 C26 -0.1(3) . . . . ?
C24 C25 C26 C21 -0.5(3) . . . . ?
C22 C21 C26 C25 0.5(3) . . . . ?
C8 C21 C26 C25 173.08(19) . . . . ?
C22 C23 C27 O28 -176.01(19) . . . . ?
C24 C23 C27 O28 -0.5(3) . . . . ?
C22 C23 C27 O27 1.6(3) . . . . ?
C24 C23 C27 O27 177.1(2) . . . . ?
O9 C9 C31 C32 -149.9(2) . . . . ?
C5 C9 C31 C32 34.6(3) . . . . ?
O9 C9 C31 C36 32.1(3) . . . . ?
C5 C9 C31 C36 -143.42(19) . . . . ?
C36 C31 C32 C33 2.4(3) . . . . ?
C9 C31 C32 C33 -175.56(19) . . . . ?
C31 C32 C33 C34 0.1(3) . . . . ?
C31 C32 C33 C37 176.58(19) . . . . ?
C32 C33 C34 C35 -1.6(3) . . . . ?
C37 C33 C34 C35 -178.1(2) . . . . ?
C33 C34 C35 C36 0.5(3) . . . . ?
C34 C35 C36 C31 2.1(3) . . . . ?
C32 C31 C36 C35 -3.5(3) . . . . ?
C9 C31 C36 C35 174.54(19) . . . . ?
C34 C33 C37 O37 -5.0(3) . . . . ?
C32 C33 C37 O37 178.5(2) . . . . ?
C34 C33 C37 O38 173.3(2) . . . . ?
C32 C33 C37 O38 -3.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.0
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.048


