# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2007

data_global
_journal_name_full               'New J.Chem.'

#====================================================================
_journal_coden_Cambridge         0440
# 1. SUBMISSION DETAILS
_publ_contact_author_name        'Scott Dalgarno'
_publ_contact_author_address     
;
Department of Chemistry
University of Missouri-Columbia
601 S. College Ave
Columbia
MO 65211
USA
;

_publ_contact_author_email       DALGARNOS@MISSOURI.EDU
_publ_contact_letter             
;
The following 2 sets of data are supplementary data for the the crystal
structures included in the paper, details of which are given below
;

#=======================================================================

# 2. TITLE AND AUTHOR LIST
_publ_section_title              
;
Large diameter non-covalent nanotubes based on the self-asembly of p-
carboxylatocalix4arene
;
loop_
_publ_author_name
_publ_author_address
'Scott J. Dalgarno'
;
Department of Chemistry
University of Missouri-Columbia
601 S. College Ave
Columbia
MO 65211
USA
;
'J. E. Warren'
;
Station 9.8
STFC Daresbury Laboratory
Daresbury
Warrington
WA44AD
;
'Jochen Antesberger'
;
Department of Chemistry
University of Missouri-Columbia
601 S. College Ave
Columbia
MO 65211
USA
;
'Timothy E. Glass'
;
Department of Chemistry
University of Missouri-Columbia
601 S. College Ave
Columbia
MO 65211
USA
;
'Jerry L. Atwood'
;
Department of Chemistry
University of Missouri-Columbia
601 S. College Ave
Columbia
MO 65211
USA
;

#=================================================================

data_CO2Ord
_database_code_depnum_ccdc_archive 'CCDC 660905'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18.50 H14.50 N0.50 O12'
_chemical_formula_weight         435.81

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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6/mcc

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

_cell_length_a                   28.9049(14)
_cell_length_b                   28.9049(14)
_cell_length_c                   21.444(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     15516.3(19)
_cell_formula_units_Z            24
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5400
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker-Nonius, 2004)'

_exptl_special_details           
;
Beam decay, scaling and absorption correction undertaken
using SADABS-2004/1 (Bruker-Nonius, 2004)
;

_diffrn_source_type              'Station 9.8, SRS, Daresbury'
_diffrn_source                   synchrotron
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.67100
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       'APEXII CCD camera on D8 diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            82857
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         17.76
_reflns_number_total             2123
_reflns_number_gt                1968
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_cell_refinement       'APEXII (Bruker, 2004)'
_computing_data_reduction        'SAINT v7.34a (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'Ortep-3 for Windows (Farrugia, 1997), XSeed (Barbour, 2001)'
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. Due to severe disorder, the
calculated formula is based on one half calixarene and half of a pyridine
molecule. Many more solvent molecules should occupy the channels in the
structure, but it was not possible to identify these due to very weak
diffraction even with a synchrotron source. Severe disorder in the calix-
arene was modelled as well as possible, with carbon atoms at partial
occupancies.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2123
_refine_ls_number_parameters     113
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.3731
_refine_ls_R_factor_gt           0.3692
_refine_ls_wR_factor_ref         0.7561
_refine_ls_wR_factor_gt          0.7500
_refine_ls_goodness_of_fit_ref   8.178
_refine_ls_restrained_S_all      8.168
_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
O1 O 0.7570(7) 0.0159(7) 0.0000 0.112(6) Uiso 0.50 2 d SP . 1
H1 H 0.7652 0.0136 0.0360 0.135 Uiso 0.25 1 calc PR . 1
C1 C 0.7129(9) 0.0209(9) 0.0000 0.084(6) Uiso 0.50 2 d SPD . 1
O2 O 0.5615(6) 0.0526(6) 0.0528(6) 0.127(5) Uiso 0.50 1 d P . 1
C2 C 0.6925(6) 0.0265(7) -0.0553(6) 0.091(5) Uiso 0.50 1 d PD . 1
O3 O 0.7334(5) -0.0636(5) -0.0781(5) 0.210(5) Uiso 1 1 d . . .
H3 H 0.7444 -0.0328 -0.0663 0.252 Uiso 1 1 calc R A 1
C3 C 0.6489(6) 0.0347(6) -0.0526(6) 0.086(5) Uiso 0.50 1 d PD . 1
H3A H 0.6361 0.0390 -0.0907 0.104 Uiso 0.50 1 calc PR . 1
O4 O 0.5601(12) -0.1486(14) -0.2904(13) 0.237(10) Uiso 0.50 1 d P . .
C4 C 0.6222(10) 0.0373(11) 0.0000 0.109(8) Uiso 0.50 2 d SPD . 1
O5 O 0.5684(10) -0.0745(11) -0.2699(10) 0.193(8) Uiso 0.50 1 d P . .
C5 C 0.5771(11) 0.0498(11) 0.0000 0.104(8) Uiso 0.50 2 d SP . 1
O6 O 0.7263(8) -0.1272(9) 0.0000 0.137(7) Uiso 0.50 2 d SP . 1
H6 H 0.7358 -0.1177 -0.0360 0.165 Uiso 0.25 1 calc PR . 1
C6 C 0.7157(10) 0.0194(10) -0.1137(9) 0.138(8) Uiso 0.50 1 d P . 1
H6A H 0.7522 0.0282 -0.1055 0.165 Uiso 0.50 1 calc PR . 1
H6B H 0.7168 0.0445 -0.1444 0.165 Uiso 0.50 1 calc PR . 1
O7 O 0.4981(11) -0.3203(12) -0.0398(12) 0.216(10) Uiso 0.50 1 d P . .
C7 C 0.6858(8) -0.0363(8) -0.1413(8) 0.119(6) Uiso 0.50 1 d PD . 1
C8 C 0.6480(7) -0.0477(8) -0.1866(7) 0.109(6) Uiso 0.50 1 d PD . 1
H8 H 0.6428 -0.0201 -0.2005 0.130 Uiso 0.50 1 calc PR . 1
C9 C 0.6170(10) -0.0980(8) -0.2127(11) 0.148(8) Uiso 0.50 1 d PD . 1
C10 C 0.6278(11) -0.1362(11) -0.1874(11) 0.162(9) Uiso 0.50 1 d PD . 1
H10 H 0.6080 -0.1705 -0.2035 0.195 Uiso 0.50 1 calc PR . 1
C11 C 0.6649(12) -0.1292(10) -0.1405(13) 0.193(12) Uiso 0.50 1 d PD . 1
C12 C 0.6985(8) -0.0750(7) -0.1227(8) 0.111(6) Uiso 0.50 1 d PD . 1
C13 C 0.5807(11) -0.1010(13) -0.2643(11) 0.145(8) Uiso 0.50 1 d P . .
C14 C 0.6756(12) -0.1699(12) -0.1247(11) 0.166(9) Uiso 0.50 1 d P . 1
H14A H 0.7139 -0.1556 -0.1229 0.199 Uiso 0.50 1 calc PR . 1
H14B H 0.6609 -0.1976 -0.1563 0.199 Uiso 0.50 1 calc PR . 1
C15 C 0.6485(12) -0.1955(12) -0.0560(12) 0.190(12) Uiso 0.50 1 d PD . 1
C16 C 0.5984(13) -0.2408(14) -0.0404(17) 0.229(15) Uiso 0.50 1 d PD . 1
C17 C 0.5580(14) -0.275(2) 0.0000 0.24(2) Uiso 0.50 2 d SPD . 1
C18 C 0.6756(16) -0.1738(17) 0.0000 0.167(13) Uiso 0.50 2 d SPD . 1
C19 C 0.5003(11) -0.3211(11) 0.0000 0.107(9) Uiso 0.50 2 d SPD . .
C200 C 0.5773(8) -0.1156(7) -0.0181(9) 0.116(8) Uiso 0.50 1 d P . .
H200 H 0.6050 -0.1208 -0.0316 0.140 Uiso 0.50 1 calc PR . .
C202 C 0.5587(9) -0.1122(9) 0.0560(11) 0.121(7) Uiso 0.50 1 d P . .
H202 H 0.5634 -0.1250 0.0938 0.145 Uiso 0.50 1 calc PR . .
C204 C 0.5090(6) -0.0856(6) -0.0185(6) 0.086(6) Uiso 0.50 1 d P . .
H204 H 0.4827 -0.0788 -0.0329 0.104 Uiso 0.50 1 calc PR . .
C205 C 0.5280(9) -0.0905(9) -0.0551(11) 0.123(7) Uiso 0.50 1 d P . .
H205 H 0.5232 -0.0781 -0.0932 0.147 Uiso 0.50 1 calc PR . .

_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
O1 C1 1.36(3) . ?
C1 C2 1.369(14) . ?
C1 C2 1.369(14) 16 ?
O2 C5 1.238(16) . ?
C2 C3 1.395(15) . ?
C2 C6 1.48(2) . ?
O3 C12 1.306(19) . ?
C3 C4 1.390(15) . ?
O4 C13 1.32(4) . ?
C4 C3 1.390(15) 16 ?
C4 C5 1.52(4) . ?
O5 C13 1.00(3) . ?
C5 O2 1.238(16) 16 ?
O6 C18 1.41(4) . ?
C6 C7 1.51(3) . ?
O7 C19 0.86(2) . ?
O7 O7 1.71(5) 16 ?
O7 C17 1.78(4) . ?
C7 C8 1.375(16) . ?
C7 C12 1.399(16) . ?
C8 C9 1.390(17) . ?
C9 C10 1.398(17) . ?
C9 C13 1.50(3) . ?
C10 C11 1.408(18) . ?
C11 C14 1.40(4) . ?
C11 C12 1.422(18) . ?
C14 C15 1.66(4) . ?
C15 C18 1.399(18) . ?
C15 C16 1.423(19) . ?
C16 C17 1.394(18) . ?
C16 C16 1.73(7) 16 ?
C17 C16 1.394(18) 16 ?
C17 C19 1.527(14) . ?
C17 O7 1.78(4) 16 ?
C18 C15 1.399(18) 16 ?
C19 O7 0.86(2) 16 ?
C200 C200 0.78(4) 16 ?
C200 C202 1.01(2) 16 ?
C200 C202 1.70(3) . ?
C202 C200 1.01(2) 16 ?
C202 C205 1.32(3) 16 ?
C204 C204 0.79(3) 16 ?
C204 C205 1.01(2) . ?
C204 C205 1.70(3) 16 ?
C205 C202 1.32(3) 16 ?
C205 C204 1.70(3) 16 ?

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
O1 C1 C2 119.8(10) . . ?
O1 C1 C2 119.8(10) . 16 ?
C2 C1 C2 120.0(19) . 16 ?
C1 C2 C3 117.6(15) . . ?
C1 C2 C6 117.6(15) . . ?
C3 C2 C6 124.6(14) . . ?
C4 C3 C2 127.9(16) . . ?
C3 C4 C3 109(2) . 16 ?
C3 C4 C5 125.3(11) . . ?
C3 C4 C5 125.3(11) 16 . ?
O2 C5 O2 133(3) 16 . ?
O2 C5 C4 113.7(14) 16 . ?
O2 C5 C4 113.7(14) . . ?
C2 C6 C7 114.9(18) . . ?
C19 O7 O7 5(3) . 16 ?
C19 O7 C17 59(2) . . ?
O7 O7 C17 61.4(10) 16 . ?
C8 C7 C12 120.4(18) . . ?
C8 C7 C6 119.5(17) . . ?
C12 C7 C6 120.0(17) . . ?
C7 C8 C9 123.6(19) . . ?
C8 C9 C10 113(2) . . ?
C8 C9 C13 115(2) . . ?
C10 C9 C13 132(2) . . ?
C9 C10 C11 128(3) . . ?
C14 C11 C10 122(2) . . ?
C14 C11 C12 123(2) . . ?
C10 C11 C12 114(3) . . ?
O3 C12 C7 118.9(16) . . ?
O3 C12 C11 119.5(18) . . ?
C7 C12 C11 120(2) . . ?
O5 C13 O4 127(3) . . ?
O5 C13 C9 124(3) . . ?
O4 C13 C9 108(3) . . ?
C11 C14 C15 110(3) . . ?
C18 C15 C16 107(3) . . ?
C18 C15 C14 122(2) . . ?
C16 C15 C14 131(2) . . ?
C17 C16 C15 155(4) . . ?
C17 C16 C16 51.6(18) . 16 ?
C15 C16 C16 103.6(19) . 16 ?
C16 C17 C16 77(4) 16 . ?
C16 C17 C19 141.4(19) 16 . ?
C16 C17 C19 141.5(19) . . ?
C16 C17 O7 112.7(18) 16 16 ?
C16 C17 O7 169(3) . 16 ?
C19 C17 O7 28.8(10) . 16 ?
C16 C17 O7 169(3) 16 . ?
C16 C17 O7 112.7(18) . . ?
C19 C17 O7 28.8(10) . . ?
O7 C17 O7 57(2) 16 . ?
C15 C18 C15 118(4) 16 . ?
C15 C18 O6 121(2) 16 . ?
C15 C18 O6 121(2) . . ?
O7 C19 O7 169(6) 16 . ?
O7 C19 C17 92(3) 16 . ?
O7 C19 C17 92(3) . . ?
C200 C200 C202 143.8(17) 16 16 ?
C200 C200 C202 20.5(10) 16 . ?
C202 C200 C202 123(3) 16 . ?
C200 C202 C205 124(3) 16 16 ?
C200 C202 C200 15.7(10) 16 . ?
C205 C202 C200 109(2) 16 . ?
C204 C204 C205 141.2(16) 16 . ?
C204 C204 C205 21.8(10) 16 16 ?
C205 C204 C205 119(3) . 16 ?
C204 C205 C202 128(3) . 16 ?
C204 C205 C204 17.0(8) . 16 ?
C202 C205 C204 112(2) 16 16 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        17.76
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.109

#==END

data_CO2Dis
_database_code_depnum_ccdc_archive 'CCDC 660906'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18.50 H14.50 N0.50 O12'
_chemical_formula_weight         435.81

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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6/mcc

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

_cell_length_a                   28.9049(14)
_cell_length_b                   28.9049(14)
_cell_length_c                   21.444(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     15516.3(19)
_cell_formula_units_Z            24
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5400
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker-Nonius, 2004)'

_exptl_special_details           
;
Beam decay, scaling and absorption correction undertaken
using SADABS-2004/1 (Bruker-Nonius, 2004)
;

_diffrn_source_type              'Station 9.8, SRS, Daresbury'
_diffrn_source                   synchrotron
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.67100
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       'APEXII CCD camera on D8 diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            82857
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         17.76
_reflns_number_total             2123
_reflns_number_gt                1968
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_cell_refinement       'APEXII (Bruker, 2004)'
_computing_data_reduction        'SAINT v7.34a (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'Ortep-3 for Windows (Farrugia, 1997), XSeed (Barbour, 2001)'
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. Due to severe disorder, the
calculated formula is based on one half calixarene and half of a pyridine
molecule. Many more solvent molecules should occupy the channels in the
structure, but it was not possible to identify these due to very weak
diffraction even with a synchrotron source. Severe disorder in the calix-
arene was modelled as well as possible, with carbon atoms at partial
occupancies.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2123
_refine_ls_number_parameters     200
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2663
_refine_ls_R_factor_gt           0.2609
_refine_ls_wR_factor_ref         0.6184
_refine_ls_wR_factor_gt          0.6108
_refine_ls_goodness_of_fit_ref   5.895
_refine_ls_restrained_S_all      5.893
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.016

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
O1 O 0.2384(11) 0.2570(10) 0.0000 0.107(9) Uiso 0.50 2 d SP . 1
C2 C 0.2840(9) 0.3042(11) 0.0000 0.043(5) Uiso 0.50 2 d SP . 1
C3 C 0.3089(6) 0.3349(7) 0.0648(10) 0.052(4) Uiso 0.50 1 d P . .
O4 O 0.4380(4) 0.4910(4) 0.0508(4) 0.173(4) Uiso 1 1 d . . .
C5 C 0.3753(12) 0.4128(12) 0.0000 0.077(8) Uiso 0.50 2 d SP . 1
O6 O 0.2648(4) 0.2038(4) 0.0797(4) 0.170(4) Uiso 1 1 d . . .
O7 O 0.2735(6) 0.1425(7) 0.0000 0.194(5) Uiso 1 2 d S . .
C8 C 0.3409(16) 0.3749(17) 0.0518(13) 0.113(10) Uiso 0.50 1 d P . 1
C9 C 0.4242(7) 0.4748(7) 0.0000 0.062(5) Uiso 0.50 2 d SP . 1
C10 C 0.2841(10) 0.3040(10) 0.1275(14) 0.118(11) Uiso 0.50 1 d P . 1
C11 C 0.3300(11) 0.1527(9) 0.0000 0.175(7) Uiso 1 2 d S . .
C12 C 0.4231(19) 0.1685(13) 0.0249(15) 0.068(11) Uiso 0.25 1 d P . .
C13 C 0.401(3) 0.1622(18) 0.024(2) 0.12(2) Uiso 0.25 1 d P . .
C15 C 0.3114(14) 0.2775(14) 0.1281(19) 0.147(15) Uiso 0.50 1 d P . .
C18 C 0.3511(12) 0.2978(12) 0.1809(14) 0.111(9) Uiso 0.50 1 d P . .
C19 C 0.3094(10) 0.2257(9) 0.1121(11) 0.110(8) Uiso 0.50 1 d P . .
C20 C 0.3305(11) 0.2118(10) 0.1590(14) 0.135(8) Uiso 0.50 1 d P . .
C22 C 0.3423(9) 0.1543(8) 0.0706(14) 0.191(7) Uiso 1 1 d . . .
C25 C 0.3739(10) 0.2903(9) 0.2141(11) 0.115(7) Uiso 0.50 1 d P . .
O26 O 0.4293(12) 0.3653(14) 0.2745(13) 0.114(11) Uiso 0.25 1 d P . .
C27 C 0.3612(12) 0.2351(13) 0.1988(13) 0.127(7) Uiso 0.50 1 d P . .
O29 O 0.4603(16) 0.2727(13) 0.2595(15) 0.149(11) Uiso 0.25 1 d P . .
C33 C 0.4312(11) 0.3442(18) 0.2738(13) 0.130(10) Uiso 0.50 1 d P . .
C16 C 0.4963(15) 0.4129(16) 0.0000 0.123(10) Uiso 0.50 2 d SP . .
C24 C 0.4398(8) 0.3277(9) -0.0513(13) 0.099(6) Uiso 0.50 1 d P . .
C1 C 0.5036(10) 0.1807(9) 0.0000 0.173(8) Uiso 1 2 d SD . .
O3 O 0.5022(11) 0.1833(11) -0.0431(15) 0.209(8) Uiso 0.50 1 d P . .
O2 O 0.4315(16) 0.2762(16) 0.2715(19) 0.142(12) Uiso 0.25 1 d P . .
C4 C 0.3614(9) 0.3988(10) 0.0316(19) 0.020(6) Uiso 0.25 1 d P . 2
C6 C 0.2996(8) 0.3242(9) 0.0309(16) 0.009(5) Uiso 0.25 1 d P . 2
O10 O 0.2490(15) 0.2610(16) 0.0238(17) 0.125(13) Uiso 0.25 1 d P . 2
C7 C 0.3594(10) 0.3918(10) 0.0707(13) 0.034(7) Uiso 0.25 1 d P . 2
C14 C 0.2852(14) 0.3070(15) 0.101(2) 0.070(12) Uiso 0.25 1 d P . 2
C23 C 0.4108(14) 0.1697(10) 0.064(2) 0.060(8) Uiso 0.25 1 d P . .
C26 C 0.4779(10) 0.3895(11) -0.0331(15) 0.121(7) Uiso 0.50 1 d P . .
C28 C 0.4475(19) 0.165(6) 0.0000 0.38(6) Uiso 0.50 2 d SPD . .
C29 C 0.4691(16) 0.3736(18) -0.070(2) 0.194(14) Uiso 0.50 1 d P . .
C30 C 0.4445(16) 0.3294(18) -0.087(3) 0.112(13) Uiso 0.25 1 d P . .
O8 O 0.4933(16) 0.1709(18) -0.095(2) 0.181(13) Uiso 0.25 1 d P A 1
O9 O 0.502(2) 0.140(2) -0.119(2) 0.204(14) Uiso 0.25 1 d P B 2
C31 C 0.4239(7) 0.3049(7) -0.0170(9) 0.104(6) Uiso 0.50 1 d P . .
C32 C 0.3767(11) 0.2253(10) 0.1707(12) 0.134(8) Uiso 0.50 1 d P . .
O33 O 0.4398(11) 0.2951(12) 0.2965(14) 0.113(9) Uiso 0.25 1 d P . .
C34 C 0.3554(14) 0.1589(12) 0.036(2) 0.074(9) Uiso 0.25 1 d P . .
C35 C 0.3262(9) 0.1514(9) 0.1186(11) 0.212(7) Uiso 1 1 d . . .
C36 C 0.2939(12) 0.2299(12) 0.1305(14) 0.131(10) Uiso 0.50 1 d P . .
C37 C 0.3157(12) 0.2786(10) 0.1529(16) 0.109(9) Uiso 0.50 1 d P . .
C38 C 0.4206(11) 0.3129(15) 0.2565(14) 0.149(9) Uiso 0.50 1 d P . .
C39 C 0.3500(11) 0.3144(12) 0.1953(13) 0.128(10) Uiso 0.50 1 d P . .
C40 C 0.3407(10) 0.2035(9) 0.1278(12) 0.125(8) Uiso 0.50 1 d P . .
C41 C 0.392(3) 0.171(2) 0.089(3) 0.141(19) Uiso 0.25 1 d P . .
C42 C 0.3865(12) 0.2709(15) 0.2008(13) 0.144(9) Uiso 0.50 1 d P . .

_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
O1 C2 1.34(4) . ?
C2 C3 1.613(17) 16 ?
C2 C3 1.613(17) . ?
C3 C6 0.78(3) . ?
C3 C14 1.08(4) . ?
C3 C8 1.10(4) . ?
C3 C7 1.57(3) . ?
C3 C10 1.57(3) . ?
C3 C4 1.85(4) . ?
O4 C9 1.174(11) . ?
C5 C9 1.64(4) . ?
C5 C8 1.53(4) . ?
C5 C8 1.53(4) 16 ?
O6 C19 1.32(2) . ?
O6 C36 1.35(3) . ?
O7 C11 1.51(3) . ?
C9 O4 1.174(11) 16 ?
C10 C15 1.35(4) . ?
C10 C37 1.53(4) . ?
C11 C34 1.02(3) . ?
C11 C34 1.02(3) 16 ?
C11 C13 1.98(7) 16 ?
C11 C13 1.98(7) . ?
C11 C22 1.55(3) . ?
C11 C22 1.55(3) 16 ?
C12 C23 0.92(4) . ?
C12 C12 1.07(7) 16 ?
C12 C13 0.58(6) . ?
C12 C28 0.93(6) . ?
C12 C13 1.20(4) 16 ?
C12 C41 1.66(7) . ?
C12 C23 1.95(7) 16 ?
C12 C34 1.85(5) . ?
C13 C34 1.29(6) . ?
C13 C13 1.02(9) 16 ?
C13 C23 0.91(5) . ?
C13 C41 1.46(8) . ?
C13 C12 1.20(4) 16 ?
C13 C22 1.87(6) . ?
C13 C34 1.80(7) 16 ?
C13 C28 1.41(7) . ?
C13 C23 1.91(7) 16 ?
C15 C37 0.54(4) . ?
C15 C36 1.21(4) . ?
C15 C18 1.51(5) . ?
C15 C19 1.51(4) . ?
C15 C14 1.51(5) . ?
C15 C39 1.81(5) . ?
C18 C39 0.59(3) . ?
C18 C37 1.07(3) . ?
C18 C25 1.06(3) . ?
C18 C42 1.62(5) . ?
C18 C27 2.01(4) . ?
C19 C36 0.65(3) . ?
C19 C20 1.34(3) . ?
C19 C40 1.39(3) . ?
C19 C37 1.69(4) . ?
C20 C40 0.81(3) . ?
C20 C27 1.17(3) . ?
C20 C32 1.21(3) . ?
C20 C36 1.52(4) . ?
C20 C35 1.89(4) . ?
C20 C42 1.89(4) . ?
C22 C34 0.80(3) . ?
C22 C35 1.12(2) . ?
C22 C41 1.32(6) . ?
C22 C40 1.90(4) . ?
C22 C23 1.81(4) . ?
C25 C42 0.85(3) . ?
C25 C39 1.27(4) . ?
C25 C38 1.48(4) . ?
C25 C27 1.48(4) . ?
C25 C37 2.03(4) . ?
C25 C33 2.06(4) . ?
O26 C33 0.64(4) . ?
O26 C38 1.46(5) . ?
C27 C32 0.88(3) . ?
C27 C42 0.92(3) . ?
C27 C40 1.72(4) . ?
O29 O2 0.92(4) . ?
O29 O33 1.33(5) . ?
O29 C38 2.00(5) . ?
C33 C38 0.88(4) . ?
C33 O33 1.64(5) . ?
C33 O2 1.97(6) . ?
C16 C26 0.94(3) 16 ?
C16 C26 0.94(3) . ?
C16 C29 1.82(5) . ?
C16 C29 1.82(5) 16 ?
C24 C30 0.78(4) . ?
C24 C31 0.94(2) . ?
C24 C29 1.23(4) . ?
C24 C31 1.58(4) 16 ?
C24 C26 1.61(4) . ?
C1 O3 0.93(3) 16 ?
C1 O3 0.93(3) . ?
C1 C28 1.45(2) . ?
O3 O8 1.17(4) . ?
O3 C28 1.68(4) . ?
O2 O33 0.72(4) . ?
O2 C38 1.29(4) . ?
C4 C7 0.86(4) . ?
C4 C4 1.35(8) 16 ?
C6 C6 1.33(7) 16 ?
C6 C14 1.58(6) . ?
C6 O10 1.68(4) . ?
C6 C7 2.04(4) . ?
O10 O10 1.02(7) 16 ?
C14 C37 1.84(5) . ?
C23 C41 0.77(5) . ?
C23 C28 1.78(6) . ?
C23 C12 1.95(7) 16 ?
C23 C34 1.59(5) . ?
C23 C13 1.91(7) 16 ?
C26 C29 0.90(4) . ?
C26 C26 1.42(6) 16 ?
C26 C30 1.90(6) . ?
C28 C12 0.93(6) 16 ?
C28 C23 1.78(6) 16 ?
C28 O3 1.68(4) 16 ?
C28 C13 1.41(7) 16 ?
C29 C30 1.16(5) . ?
C30 C31 1.64(5) . ?
C31 C31 0.73(4) 16 ?
C31 C24 1.58(4) 16 ?
C32 C40 1.29(3) . ?
C32 C42 1.36(4) . ?
O33 C38 1.26(4) . ?
C34 C41 1.46(7) . ?
C34 C34 1.56(10) 16 ?
C34 C13 1.80(7) 16 ?
C34 C35 1.92(5) . ?
C35 C40 1.36(3) . ?
C35 C41 1.80(8) . ?
C36 C37 1.31(4) . ?
C36 C40 1.85(4) . ?
C37 C39 1.36(5) . ?
C38 C42 1.64(5) . ?
C39 C42 2.01(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
_geom_angle_publ_flag
O1 C2 C3 120.1(11) . 16 ?
O1 C2 C3 120.1(11) . . ?
C3 C2 C3 119(2) 16 . ?
C6 C3 C14 114(4) . . ?
C6 C3 C8 97(3) . . ?
C14 C3 C8 149(3) . . ?
C6 C3 C7 117(3) . . ?
C14 C3 C7 129(3) . . ?
C8 C3 C7 20.0(18) . . ?
C6 C3 C10 127(3) . . ?
C14 C3 C10 13(2) . . ?
C8 C3 C10 136(2) . . ?
C7 C3 C10 116.6(17) . . ?
C6 C3 C2 8.7(19) . . ?
C14 C3 C2 106(2) . . ?
C8 C3 C2 106(2) . . ?
C7 C3 C2 125(2) . . ?
C10 C3 C2 118.2(19) . . ?
C6 C3 C4 89(3) . . ?
C14 C3 C4 157(3) . . ?
C8 C3 C4 8.1(19) . . ?
C7 C3 C4 27.6(11) . . ?
C10 C3 C4 144.0(18) . . ?
C2 C3 C4 97.7(19) . . ?
C9 C5 C8 132.9(15) . . ?
C9 C5 C8 132.9(15) . 16 ?
C8 C5 C8 93(3) . 16 ?
C19 O6 C36 28.2(13) . . ?
C3 C8 C5 148(3) . . ?
O4 C9 O4 136.2(19) . 16 ?
O4 C9 C5 111.8(10) . . ?
O4 C9 C5 111.8(10) 16 . ?
C15 C10 C3 96(2) . . ?
C15 C10 C37 20.5(17) . . ?
C3 C10 C37 111.3(19) . . ?
C34 C11 C34 99(7) . 16 ?
C34 C11 O7 130(3) . . ?
C34 C11 O7 130(3) 16 . ?
C34 C11 C13 65(4) . 16 ?
C34 C11 C13 35(3) 16 16 ?
O7 C11 C13 164.9(14) . 16 ?
C34 C11 C13 35(3) . . ?
C34 C11 C13 65(4) 16 . ?
O7 C11 C13 164.9(14) . . ?
C13 C11 C13 30(3) 16 . ?
C34 C11 C22 28(2) . . ?
C34 C11 C22 127(5) 16 . ?
O7 C11 C22 102.4(16) . . ?
C13 C11 C22 92(2) 16 . ?
C13 C11 C22 62.7(19) . . ?
C34 C11 C22 127(5) . 16 ?
C34 C11 C22 28(2) 16 16 ?
O7 C11 C22 102.4(16) . 16 ?
C13 C11 C22 62.7(19) 16 16 ?
C13 C11 C22 92(2) . 16 ?
C22 C11 C22 155(3) . 16 ?
C23 C12 C12 156(3) . 16 ?
C23 C12 C13 70(6) . . ?
C12 C12 C13 88(6) 16 . ?
C23 C12 C28 149(6) . . ?
C12 C12 C28 55(3) 16 . ?
C13 C12 C28 137(9) . . ?
C23 C12 C13 128(5) . 16 ?
C12 C12 C13 29(3) 16 16 ?
C13 C12 C13 58(7) . 16 ?
C28 C12 C13 82(4) . 16 ?
C23 C12 C41 11(3) . . ?
C12 C12 C41 145(2) 16 . ?
C13 C12 C41 60(7) . . ?
C28 C12 C41 160(5) . . ?
C13 C12 C41 117(4) 16 . ?
C23 C12 C23 145(5) . 16 ?
C12 C12 C23 11.1(16) 16 16 ?
C13 C12 C23 77(7) . 16 ?
C28 C12 C23 66(3) . 16 ?
C13 C12 C23 19(3) 16 16 ?
C41 C12 C23 134(3) . 16 ?
C23 C12 C34 59(3) . . ?
C12 C12 C34 97.7(19) 16 . ?
C13 C12 C34 13(6) . . ?
C28 C12 C34 150(5) . . ?
C13 C12 C34 69(3) 16 . ?
C41 C12 C34 49(3) . . ?
C23 C12 C34 87(3) 16 . ?
C12 C13 C34 161(9) . . ?
C12 C13 C13 92(6) . 16 ?
C34 C13 C13 102(3) . 16 ?
C12 C13 C23 73(6) . . ?
C34 C13 C23 91(6) . . ?
C13 C13 C23 163(5) 16 . ?
C12 C13 C41 100(7) . . ?
C34 C13 C41 64(4) . . ?
C13 C13 C41 163(3) 16 . ?
C23 C13 C41 27(4) . . ?
C12 C13 C12 63(7) . 16 ?
C34 C13 C12 131(5) . 16 ?
C13 C13 C12 29(3) 16 16 ?
C23 C13 C12 135(7) . 16 ?
C41 C13 C12 159(6) . 16 ?
C12 C13 C11 165(8) . . ?
C34 C13 C11 27(3) . . ?
C13 C13 C11 75.1(14) 16 . ?
C23 C13 C11 118(6) . . ?
C41 C13 C11 91(4) . . ?
C12 C13 C11 104(3) 16 . ?
C12 C13 C22 144(7) . . ?
C34 C13 C22 20(2) . . ?
C13 C13 C22 122.4(17) 16 . ?
C23 C13 C22 72(5) . . ?
C41 C13 C22 44(3) . . ?
C12 C13 C22 151(4) 16 . ?
C11 C13 C22 47.3(19) . . ?
C12 C13 C34 136(8) . 16 ?
C34 C13 C34 58(4) . 16 ?
C13 C13 C34 44(2) 16 16 ?
C23 C13 C34 147(6) . 16 ?
C41 C13 C34 121(5) . 16 ?
C12 C13 C34 73(3) 16 16 ?
C11 C13 C34 30.9(14) . 16 ?
C22 C13 C34 78(3) . 16 ?
C12 C13 C28 27(6) . . ?
C34 C13 C28 171(4) . . ?
C13 C13 C28 69(2) 16 . ?
C23 C13 C28 98(6) . . ?
C41 C13 C28 125(5) . . ?
C12 C13 C28 41(3) 16 . ?
C11 C13 C28 144(3) . . ?
C22 C13 C28 168(4) . . ?
C34 C13 C28 113(3) 16 . ?
C12 C13 C23 85(7) . 16 ?
C34 C13 C23 108(4) . 16 ?
C13 C13 C23 8(2) 16 16 ?
C23 C13 C23 155(7) . 16 ?
C41 C13 C23 163(4) . 16 ?
C12 C13 C23 23(2) 16 16 ?
C11 C13 C23 82(2) . 16 ?
C22 C13 C23 129(4) . 16 ?
C34 C13 C23 51(2) 16 16 ?
C28 C13 C23 63(3) . 16 ?
C37 C15 C36 89(6) . . ?
C37 C15 C10 99(6) . . ?
C36 C15 C10 128(3) . . ?
C37 C15 C18 30(5) . . ?
C36 C15 C18 102(3) . . ?
C10 C15 C18 110(3) . . ?
C37 C15 C19 100(6) . . ?
C36 C15 C19 24.7(18) . . ?
C10 C15 C19 145(3) . . ?
C18 C15 C19 102(3) . . ?
C37 C15 C14 120(7) . . ?
C36 C15 C14 128(3) . . ?
C10 C15 C14 22.1(19) . . ?
C18 C15 C14 125(3) . . ?
C19 C15 C14 134(3) . . ?
C37 C15 C39 30(5) . . ?
C36 C15 C39 115(3) . . ?
C10 C15 C39 92(2) . . ?
C18 C15 C39 17.5(14) . . ?
C19 C15 C39 118(3) . . ?
C14 C15 C39 108(3) . . ?
C39 C18 C37 107(6) . . ?
C39 C18 C25 96(6) . . ?
C37 C18 C25 143(4) . . ?
C39 C18 C15 112(6) . . ?
C37 C18 C15 15(2) . . ?
C25 C18 C15 149(3) . . ?
C39 C18 C42 124(6) . . ?
C37 C18 C42 125(3) . . ?
C25 C18 C42 28.6(19) . . ?
C15 C18 C42 124(3) . . ?
C39 C18 C27 137(6) . . ?
C37 C18 C27 100(3) . . ?
C25 C18 C27 46(2) . . ?
C15 C18 C27 103(2) . . ?
C42 C18 C27 26.8(12) . . ?
C36 C19 O6 79(4) . . ?
C36 C19 C20 93(4) . . ?
O6 C19 C20 137(2) . . ?
C36 C19 C40 127(4) . . ?
O6 C19 C40 128(2) . . ?
C20 C19 C40 34.7(13) . . ?
C36 C19 C15 51(4) . . ?
O6 C19 C15 98(2) . . ?
C20 C19 C15 109(2) . . ?
C40 C19 C15 134(2) . . ?
C36 C19 C37 45(4) . . ?
O6 C19 C37 110(2) . . ?
C20 C19 C37 91(2) . . ?
C40 C19 C37 120(2) . . ?
C15 C19 C37 18.5(15) . . ?
C40 C20 C27 119(4) . . ?
C40 C20 C32 76(3) . . ?
C27 C20 C32 43.1(17) . . ?
C40 C20 C19 76(3) . . ?
C27 C20 C19 135(3) . . ?
C32 C20 C19 131(3) . . ?
C40 C20 C36 101(3) . . ?
C27 C20 C36 123(3) . . ?
C32 C20 C36 144(3) . . ?
C19 C20 C36 25.3(14) . . ?
C40 C20 C35 39(2) . . ?
C27 C20 C35 123(2) . . ?
C32 C20 C35 87(2) . . ?
C19 C20 C35 96(2) . . ?
C36 C20 C35 113(2) . . ?
C40 C20 C42 113(3) . . ?
C27 C20 C42 22.4(16) . . ?
C32 C20 C42 46.0(19) . . ?
C19 C20 C42 113(2) . . ?
C36 C20 C42 108(2) . . ?
C35 C20 C42 133(2) . . ?
C34 C22 C35 175(4) . . ?
C34 C22 C41 83(4) . . ?
C35 C22 C41 95(4) . . ?
C34 C22 C13 34(3) . . ?
C35 C22 C13 145(3) . . ?
C41 C22 C13 51(3) . . ?
C34 C22 C11 37(3) . . ?
C35 C22 C11 145(3) . . ?
C41 C22 C11 119(4) . . ?
C13 C22 C11 70(3) . . ?
C34 C22 C40 131(3) . . ?
C35 C22 C40 45.0(16) . . ?
C41 C22 C40 88(3) . . ?
C13 C22 C40 128(2) . . ?
C11 C22 C40 124.2(15) . . ?
C34 C22 C23 62(3) . . ?
C35 C22 C23 117(3) . . ?
C41 C22 C23 22(3) . . ?
C13 C22 C23 28.6(17) . . ?
C11 C22 C23 98(3) . . ?
C40 C22 C23 107.3(18) . . ?
C42 C25 C18 115(4) . . ?
C42 C25 C39 141(4) . . ?
C18 C25 C39 27(2) . . ?
C42 C25 C38 84(4) . . ?
C18 C25 C38 147(3) . . ?
C39 C25 C38 125(3) . . ?
C42 C25 C27 35(3) . . ?
C18 C25 C27 103(3) . . ?
C39 C25 C27 128(3) . . ?
C38 C25 C27 107(3) . . ?
C42 C25 C37 105(3) . . ?
C18 C25 C37 18.6(19) . . ?
C39 C25 C37 41.3(19) . . ?
C38 C25 C37 166(2) . . ?
C27 C25 C37 86.5(16) . . ?
C42 C25 C33 105(4) . . ?
C18 C25 C33 127(3) . . ?
C39 C25 C33 104(2) . . ?
C38 C25 C33 22.1(16) . . ?
C27 C25 C33 129(2) . . ?
C37 C25 C33 145(2) . . ?
C33 O26 C38 19(4) . . ?
C32 C27 C42 99(4) . . ?
C32 C27 C20 71(3) . . ?
C42 C27 C20 129(4) . . ?
C32 C27 C25 127(4) . . ?
C42 C27 C25 32(2) . . ?
C20 C27 C25 119(2) . . ?
C32 C27 C40 47(2) . . ?
C42 C27 C40 120(3) . . ?
C20 C27 C40 24.4(16) . . ?
C25 C27 C40 127(2) . . ?
C32 C27 C18 119(3) . . ?
C42 C27 C18 52(3) . . ?
C20 C27 C18 88(2) . . ?
C25 C27 C18 31.0(12) . . ?
C40 C27 C18 98.1(17) . . ?
O2 O29 O33 31(3) . . ?
O2 O29 C38 30(3) . . ?
O33 O29 C38 38.3(17) . . ?
O26 C33 C38 147(7) . . ?
O26 C33 O33 161(6) . . ?
C38 C33 O33 50(3) . . ?
O26 C33 O2 176(6) . . ?
C38 C33 O2 30(3) . . ?
O33 C33 O2 20.3(14) . . ?
O26 C33 C25 109(5) . . ?
C38 C33 C25 39(3) . . ?
O33 C33 C25 87(2) . . ?
O2 C33 C25 68(2) . . ?
C26 C16 C26 98(5) 16 . ?
C26 C16 C29 105(4) 16 . ?
C26 C16 C29 8(2) . . ?
C26 C16 C29 8(2) 16 16 ?
C26 C16 C29 105(4) . 16 ?
C29 C16 C29 113(4) . 16 ?
C30 C24 C31 146(5) . . ?
C30 C24 C29 66(4) . . ?
C31 C24 C29 148(4) . . ?
C30 C24 C31 162(4) . 16 ?
C31 C24 C31 16.7(11) . 16 ?
C29 C24 C31 131(3) . 16 ?
C30 C24 C26 100(4) . . ?
C31 C24 C26 114(3) . . ?
C29 C24 C26 34(2) . . ?
C31 C24 C26 98(2) 16 . ?
O3 C1 O3 167(5) 16 . ?
O3 C1 C28 86(3) 16 . ?
O3 C1 C28 86(3) . . ?
C1 O3 O8 161(5) . . ?
C1 O3 C28 60(2) . . ?
O8 O3 C28 114(3) . . ?
O33 O2 O29 108(6) . . ?
O33 O2 C38 72(5) . . ?
O29 O2 C38 129(5) . . ?
O33 O2 C33 52(4) . . ?
O29 O2 C33 125(4) . . ?
C38 O2 C33 20.0(19) . . ?
C7 C4 C4 168(2) . 16 ?
C7 C4 C3 58(2) . . ?
C4 C4 C3 112.7(12) 16 . ?
C3 C6 C6 158(2) . 16 ?
C3 C6 C14 39(2) . . ?
C6 C6 C14 163.0(18) 16 . ?
C3 C6 O10 117(3) . . ?
C6 C6 O10 84.8(19) 16 . ?
C14 C6 O10 78(2) . . ?
C3 C6 C7 43(2) . . ?
C6 C6 C7 114.7(11) 16 . ?
C14 C6 C7 82(2) . . ?
O10 C6 C7 160(3) . . ?
O10 O10 C6 95.2(19) 16 . ?
C4 C7 C3 95(3) . . ?
C4 C7 C6 75(2) . . ?
C3 C7 C6 20.1(9) . . ?
C3 C14 C15 113(3) . . ?
C3 C14 C6 27.0(19) . . ?
C15 C14 C6 115(3) . . ?
C3 C14 C37 120(3) . . ?
C15 C14 C37 14.7(17) . . ?
C6 C14 C37 127(2) . . ?
C12 C23 C41 157(7) . . ?
C12 C23 C13 37(4) . . ?
C41 C23 C13 120(7) . . ?
C12 C23 C28 15(3) . . ?
C41 C23 C28 172(6) . . ?
C13 C23 C28 52(5) . . ?
C12 C23 C12 12.8(19) . 16 ?
C41 C23 C12 144(6) . 16 ?
C13 C23 C12 26(4) . 16 ?
C28 C23 C12 28.3(19) . 16 ?
C12 C23 C34 91(4) . . ?
C41 C23 C34 66(5) . . ?
C13 C23 C34 54(4) . . ?
C28 C23 C34 106(3) . . ?
C12 C23 C34 79(3) 16 . ?
C12 C23 C22 117(4) . . ?
C41 C23 C22 41(5) . . ?
C13 C23 C22 80(5) . . ?
C28 C23 C22 131(2) . . ?
C12 C23 C22 105(2) 16 . ?
C34 C23 C22 26.4(15) . . ?
C12 C23 C13 30(3) . 16 ?
C41 C23 C13 127(6) . 16 ?
C13 C23 C13 9(3) . 16 ?
C28 C23 C13 45(3) . 16 ?
C12 C23 C13 17(2) 16 16 ?
C34 C23 C13 61(2) . 16 ?
C22 C23 C13 87(2) . 16 ?
C29 C26 C16 163(5) . . ?
C29 C26 C26 154(3) . 16 ?
C16 C26 C26 41(3) . 16 ?
C29 C26 C24 50(3) . . ?
C16 C26 C24 144(4) . . ?
C26 C26 C24 104.1(15) 16 . ?
C29 C26 C30 26(3) . . ?
C16 C26 C30 164(3) . . ?
C26 C26 C30 127.5(17) 16 . ?
C24 C26 C30 23.7(14) . . ?
C12 C28 C12 70(6) . 16 ?
C12 C28 C1 139(7) . . ?
C12 C28 C1 139(7) 16 . ?
C12 C28 C23 15(3) . . ?
C12 C28 C23 86(4) 16 . ?
C1 C28 C23 126(3) . . ?
C12 C28 C23 86(4) . 16 ?
C12 C28 C23 15(3) 16 16 ?
C1 C28 C23 126(3) . 16 ?
C23 C28 C23 101(4) . 16 ?
C12 C28 O3 107(4) . 16 ?
C12 C28 O3 159(10) 16 16 ?
C1 C28 O3 33.7(13) . 16 ?
C23 C28 O3 93(2) . 16 ?
C23 C28 O3 155(6) 16 16 ?
C12 C28 O3 159(10) . . ?
C12 C28 O3 107(4) 16 . ?
C1 C28 O3 33.7(13) . . ?
C23 C28 O3 155(6) . . ?
C23 C28 O3 93(2) 16 . ?
O3 C28 O3 67(3) 16 . ?
C12 C28 C13 16(3) . . ?
C12 C28 C13 57(4) 16 . ?
C1 C28 C13 156(6) . . ?
C23 C28 C13 30.4(19) . . ?
C23 C28 C13 72(3) 16 . ?
O3 C28 C13 123(3) 16 . ?
O3 C28 C13 161(8) . . ?
C12 C28 C13 57(4) . 16 ?
C12 C28 C13 16(3) 16 16 ?
C1 C28 C13 156(6) . 16 ?
C23 C28 C13 72(3) . 16 ?
C23 C28 C13 30.4(19) 16 16 ?
O3 C28 C13 161(8) 16 16 ?
O3 C28 C13 123(3) . 16 ?
C13 C28 C13 42(4) . 16 ?
C26 C29 C24 97(4) . . ?
C26 C29 C30 134(6) . . ?
C24 C29 C30 38(3) . . ?
C26 C29 C16 9(2) . . ?
C24 C29 C16 104(4) . . ?
C30 C29 C16 141(5) . . ?
C24 C30 C29 76(5) . . ?
C24 C30 C31 19(3) . . ?
C29 C30 C31 95(4) . . ?
C24 C30 C26 56(4) . . ?
C29 C30 C26 20(3) . . ?
C31 C30 C26 75(2) . . ?
C31 C31 C24 141.5(17) 16 . ?
C31 C31 C30 156.3(17) 16 . ?
C24 C31 C30 15(2) . . ?
C31 C31 C24 21.8(10) 16 16 ?
C24 C31 C24 120(3) . 16 ?
C30 C31 C24 135(2) . 16 ?
C27 C32 C20 66(3) . . ?
C27 C32 C40 103(3) . . ?
C20 C32 C40 37.7(16) . . ?
C27 C32 C42 42(2) . . ?
C20 C32 C42 94(3) . . ?
C40 C32 C42 122(3) . . ?
O2 O33 C38 76(4) . . ?
O2 O33 O29 41(4) . . ?
C38 O33 O29 101(3) . . ?
O2 O33 C33 107(5) . . ?
C38 O33 C33 32.3(17) . . ?
O29 O33 C33 123(2) . . ?
C22 C34 C11 115(5) . . ?
C22 C34 C13 125(5) . . ?
C11 C34 C13 117(5) . . ?
C22 C34 C41 64(4) . . ?
C11 C34 C41 177(4) . . ?
C13 C34 C41 64(4) . . ?
C22 C34 C34 156(3) . 16 ?
C11 C34 C34 40(3) . 16 ?
C13 C34 C34 78(3) . 16 ?
C41 C34 C34 140(3) . 16 ?
C22 C34 C13 158(4) . 16 ?
C11 C34 C13 84(5) . 16 ?
C13 C34 C13 33(3) . 16 ?
C41 C34 C13 97(4) . 16 ?
C34 C34 C13 44(2) 16 16 ?
C22 C34 C23 92(4) . . ?
C11 C34 C23 152(5) . . ?
C13 C34 C23 35(3) . . ?
C41 C34 C23 29(2) . . ?
C34 C34 C23 112(2) 16 . ?
C13 C34 C23 68(2) 16 . ?
C22 C34 C35 3(2) . . ?
C11 C34 C35 116(3) . . ?
C13 C34 C35 125(4) . . ?
C41 C34 C35 63(4) . . ?
C34 C34 C35 156.7(12) 16 . ?
C13 C34 C35 158(3) 16 . ?
C23 C34 C35 91(3) . . ?
C22 C34 C12 121(4) . . ?
C11 C34 C12 122(5) . . ?
C13 C34 C12 6(3) . . ?
C41 C34 C12 59(3) . . ?
C34 C34 C12 82.3(19) 16 . ?
C13 C34 C12 38.1(15) 16 . ?
C23 C34 C12 30.0(16) . . ?
C35 C34 C12 121(2) . . ?
C22 C35 C40 100(2) . . ?
C22 C35 C41 47(2) . . ?
C40 C35 C41 91(2) . . ?
C22 C35 C20 121(2) . . ?
C40 C35 C20 22.1(13) . . ?
C41 C35 C20 108(2) . . ?
C22 C35 C34 2.0(17) . . ?
C40 C35 C34 98(2) . . ?
C41 C35 C34 46(2) . . ?
C20 C35 C34 119.6(16) . . ?
C19 C36 C15 104(5) . . ?
C19 C36 C37 114(5) . . ?
C15 C36 C37 24(2) . . ?
C19 C36 O6 73(4) . . ?
C15 C36 O6 113(3) . . ?
C37 C36 O6 136(3) . . ?
C19 C36 C20 61(3) . . ?
C15 C36 C20 116(3) . . ?
C37 C36 C20 100(2) . . ?
O6 C36 C20 119(3) . . ?
C19 C36 C40 36(3) . . ?
C15 C36 C40 119(3) . . ?
C37 C36 C40 113(2) . . ?
O6 C36 C40 97(2) . . ?
C20 C36 C40 25.6(12) . . ?
C15 C37 C18 135(7) . . ?
C15 C37 C39 139(7) . . ?
C18 C37 C39 24(2) . . ?
C15 C37 C36 67(6) . . ?
C18 C37 C36 126(3) . . ?
C39 C37 C36 147(3) . . ?
C15 C37 C10 60(6) . . ?
C18 C37 C10 127(3) . . ?
C39 C37 C10 105(2) . . ?
C36 C37 C10 108(3) . . ?
C15 C37 C19 62(6) . . ?
C18 C37 C19 114(3) . . ?
C39 C37 C19 138(3) . . ?
C36 C37 C19 20.6(15) . . ?
C10 C37 C19 116(3) . . ?
C15 C37 C14 45(6) . . ?
C18 C37 C14 131(3) . . ?
C39 C37 C14 113(2) . . ?
C36 C37 C14 100(3) . . ?
C10 C37 C14 16.3(15) . . ?
C19 C37 C14 103(2) . . ?
C15 C37 C25 142(6) . . ?
C18 C37 C25 18.5(19) . . ?
C39 C37 C25 38.0(19) . . ?
C36 C37 C25 109(2) . . ?
C10 C37 C25 143(2) . . ?
C19 C37 C25 101.0(17) . . ?
C14 C37 C25 149(2) . . ?
C33 C38 O33 98(4) . . ?
C33 C38 O2 130(5) . . ?
O33 C38 O2 32.6(19) . . ?
C33 C38 C25 119(4) . . ?
O33 C38 C25 137(3) . . ?
O2 C38 C25 109(3) . . ?
C33 C38 C42 147(4) . . ?
O33 C38 C42 115(3) . . ?
O2 C38 C42 83(3) . . ?
C25 C38 C42 31.3(13) . . ?
C33 C38 O26 14(3) . . ?
O33 C38 O26 111(3) . . ?
O2 C38 O26 143(4) . . ?
C25 C38 O26 105(2) . . ?
C42 C38 O26 134(3) . . ?
C33 C38 O29 126(4) . . ?
O33 C38 O29 41(2) . . ?
O2 C38 O29 21.1(19) . . ?
C25 C38 O29 115(3) . . ?
C42 C38 O29 84(2) . . ?
O26 C38 O29 138(3) . . ?
C18 C39 C37 49(5) . . ?
C18 C39 C25 57(5) . . ?
C37 C39 C25 101(3) . . ?
C18 C39 C15 51(5) . . ?
C37 C39 C15 11.4(18) . . ?
C25 C39 C15 106(3) . . ?
C18 C39 C42 42(5) . . ?
C37 C39 C42 89(2) . . ?
C25 C39 C42 15.4(16) . . ?
C15 C39 C42 92(2) . . ?
C20 C40 C35 119(3) . . ?
C20 C40 C32 66(3) . . ?
C35 C40 C32 112(2) . . ?
C20 C40 C19 69(3) . . ?
C35 C40 C19 125(2) . . ?
C32 C40 C19 120(3) . . ?
C20 C40 C27 36(2) . . ?
C35 C40 C27 123(2) . . ?
C32 C40 C27 29.7(14) . . ?
C19 C40 C27 96(2) . . ?
C20 C40 C22 154(3) . . ?
C35 C40 C22 35.5(12) . . ?
C32 C40 C22 121(2) . . ?
C19 C40 C22 117.2(19) . . ?
C27 C40 C22 147.0(19) . . ?
C20 C40 C36 54(3) . . ?
C35 C40 C36 125(2) . . ?
C32 C40 C36 111(2) . . ?
C19 C40 C36 16.3(14) . . ?
C27 C40 C36 83.3(18) . . ?
C22 C40 C36 128.7(17) . . ?
C23 C41 C22 117(6) . . ?
C23 C41 C13 33(4) . . ?
C22 C41 C13 85(4) . . ?
C23 C41 C34 85(5) . . ?
C22 C41 C34 33.2(19) . . ?
C13 C41 C34 53(3) . . ?
C23 C41 C12 13(4) . . ?
C22 C41 C12 105(4) . . ?
C13 C41 C12 20(2) . . ?
C34 C41 C12 73(3) . . ?
C23 C41 C35 153(7) . . ?
C22 C41 C35 38(2) . . ?
C13 C41 C35 122(4) . . ?
C34 C41 C35 71(3) . . ?
C12 C41 C35 142(4) . . ?
C25 C42 C27 113(5) . . ?
C25 C42 C32 147(4) . . ?
C27 C42 C32 39(2) . . ?
C25 C42 C38 64(3) . . ?
C27 C42 C38 135(4) . . ?
C32 C42 C38 145(3) . . ?
C25 C42 C18 37(2) . . ?
C27 C42 C18 101(3) . . ?
C32 C42 C18 118(3) . . ?
C38 C42 C18 97(3) . . ?
C25 C42 C20 107(3) . . ?
C27 C42 C20 29(2) . . ?
C32 C42 C20 39.8(16) . . ?
C38 C42 C20 160(2) . . ?
C18 C42 C20 81.3(19) . . ?
C25 C42 C39 23(3) . . ?
C27 C42 C39 109(3) . . ?
C32 C42 C39 131(2) . . ?
C38 C42 C39 84(2) . . ?
C18 C42 C39 14.0(15) . . ?
C20 C42 C39 93.3(17) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        17.76
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.108

#==END