# Supplementary Material (ESI) for Chemical Communications

# This journal is © The Royal Society of Chemistry 2002



data_global



_journal_coden_Cambridge      182

_journal_volume           ?

_journal_year             ? 

_journal_page_first       ?



_publ_requested_journal       'Chemical Communications'



loop_

_publ_author_name

'Julius Rebek'

'Byron W. Purse'

'Alexander Shivanyuk'



_publ_contact_author_name     	'Prof Julius Rebek'  

_publ_contact_author_address 

;

Prof Julius Rebek

Skaggs Institute for Chemical Biology

The Scripps Research Institute

10550 North Torrey Pines Road

MB-26

La Jolla

CA

92037

UNITED STATES OF AMERICA

;



_publ_contact_author_email       'JREBEK@SCRIPPS.EDU'



_publ_section_title

;

Resorcin[6]arene as a Building Block for Tubular

Crystalline State Architectures

;



data_bpas1



_database_code_CSD	193890





_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

'C36 H44 O8 S0.44'

_chemical_formula_weight          618.96



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'

'S'  'S'   0.1246   0.1234

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting            rhombohedral

_symmetry_space_group_name_H-M    R-3



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

'-y, x-y, z'

'-x+y, -x, z'

'x+2/3, y+1/3, z+1/3'

'-y+2/3, x-y+1/3, z+1/3'

'-x+y+2/3, -x+1/3, z+1/3'

'x+1/3, y+2/3, z+2/3'

'-y+1/3, x-y+2/3, z+2/3'

'-x+y+1/3, -x+2/3, z+2/3'

'-x, -y, -z'

'y, -x+y, -z'

'x-y, x, -z'

'-x+2/3, -y+1/3, -z+1/3'

'y+2/3, -x+y+1/3, -z+1/3'

'x-y+2/3, x+1/3, -z+1/3'

'-x+1/3, -y+2/3, -z+2/3'

'y+1/3, -x+y+2/3, -z+2/3'

'x-y+1/3, x+2/3, -z+2/3'



_cell_length_a                    28.453(5)

_cell_length_b                    28.453(5)

_cell_length_c                    10.024(3)

_cell_angle_alpha                 90.00

_cell_angle_beta                  90.00

_cell_angle_gamma                 120.00

_cell_volume                      7028(3)

_cell_formula_units_Z             9

_cell_measurement_temperature     293(2)

_cell_measurement_reflns_used     ?

_cell_measurement_theta_min       ?

_cell_measurement_theta_max       ?



_exptl_crystal_description        ?

_exptl_crystal_colour             ?

_exptl_crystal_size_max           ?

_exptl_crystal_size_mid           ?

_exptl_crystal_size_min           ?

_exptl_crystal_density_meas       ?

_exptl_crystal_density_diffrn     1.316

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              2980

_exptl_absorpt_coefficient_mu     0.120

_exptl_absorpt_correction_type    ?

_exptl_absorpt_correction_T_min   ?

_exptl_absorpt_correction_T_max   ?

_exptl_absorpt_process_details    ?



_exptl_special_details

;

?

;



_diffrn_ambient_temperature       293(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   ?

_diffrn_measurement_method        ?

_diffrn_detector_area_resol_mean  ?

_diffrn_standards_number          ?

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         ?

_diffrn_reflns_number             21034

_diffrn_reflns_av_R_equivalents   0.1108

_diffrn_reflns_av_sigmaI/netI     0.1198

_diffrn_reflns_limit_h_min        -37

_diffrn_reflns_limit_h_max        37

_diffrn_reflns_limit_k_min        -37

_diffrn_reflns_limit_k_max        37

_diffrn_reflns_limit_l_min        -13

_diffrn_reflns_limit_l_max        13

_diffrn_reflns_theta_min          1.43

_diffrn_reflns_theta_max          28.13

_reflns_number_total              3794

_reflns_number_gt                 2279

_reflns_threshold_expression      >2sigma(I)



_computing_data_collection        ?

_computing_cell_refinement        ?

_computing_data_reduction         ?

_computing_structure_solution     ?

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     ?

_computing_publication_material   ?



_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.

;



_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/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          3794

_refine_ls_number_parameters      188

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.2173

_refine_ls_R_factor_gt            0.1632

_refine_ls_wR_factor_ref          0.4641

_refine_ls_wR_factor_gt           0.4352

_refine_ls_goodness_of_fit_ref    1.494

_refine_ls_restrained_S_all       1.494

_refine_ls_shift/su_max           0.428

_refine_ls_shift/su_mean          0.042



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

C6 C 0.1214(2) 0.1203(2) 0.5012(6) 0.0389(14) Uani 1 1 d . . .

H6 H 0.0997 0.0854 0.5345 0.047 Uiso 1 1 calc . . .

C1 C 0.1179(3) 0.1616(3) 0.5621(6) 0.0408(15) Uani 1 1 d . . .

C5 C 0.1549(2) 0.1264(3) 0.3933(7) 0.0411(15) Uani 1 1 d . . .

C8 C 0.0574(3) 0.1011(3) 0.7513(7) 0.0450(16) Uani 1 1 d . . .

H8A H 0.0377 0.0703 0.6922 0.054 Uiso 1 1 calc R . .

H8B H 0.0885 0.0997 0.7857 0.054 Uiso 1 1 calc R . .

C2 C 0.1549(3) 0.2152(3) 0.5146(7) 0.0415(15) Uani 1 1 d . . .

C4 C 0.1864(3) 0.1790(3) 0.3439(7) 0.0449(16) Uani 1 1 d . . .

C3 C 0.1865(3) 0.2217(3) 0.4058(8) 0.0486(17) Uani 1 1 d . . .

H3 H 0.2089 0.2565 0.3729 0.058 Uiso 1 1 calc . . .

C9 C 0.0208(4) 0.0968(4) 0.8667(9) 0.063(2) Uani 1 1 d . . .

H9A H 0.0394 0.1283 0.9225 0.095 Uiso 1 1 calc R . .

H9B H 0.0117 0.0649 0.9179 0.095 Uiso 1 1 calc R . .

H9C H -0.0117 0.0946 0.8325 0.095 Uiso 1 1 calc R . .

C7 C 0.0770(2) 0.1534(3) 0.6723(7) 0.0415(15) Uani 1 1 d . . .

CZ3 C 0.1024(2) 0.3100(2) 0.1476(7) 0.0380(14) Uani 1 1 d . . .

HZ3A H 0.0910 0.2883 0.0680 0.057 Uiso 1 1 calc R . .

HZ3B H 0.1353 0.3434 0.1302 0.057 Uiso 1 1 calc R . .

HZ3C H 0.0746 0.3177 0.1750 0.057 Uiso 1 1 calc R . .

CZ4 C 0.0689(4) 0.2746(5) 0.3871(12) 0.091(3) Uani 1 1 d . . .

HZ4A H 0.0875 0.3055 0.4446 0.136 Uiso 1 1 calc R . .

HZ4B H 0.0586 0.2421 0.4371 0.136 Uiso 1 1 calc R . .

HZ4C H 0.0371 0.2734 0.3514 0.136 Uiso 1 1 calc R . .

O1 O 0.1532(2) 0.25625(18) 0.5800(6) 0.0530(14) Uani 1 1 d . . .

H1 H 0.1832 0.2837 0.5765 0.080 Uiso 1 1 calc R . .

O2 O 0.2184(2) 0.1860(2) 0.2340(6) 0.0579(14) Uani 1 1 d . . .

H2 H 0.2249 0.2139 0.1948 0.087 Uiso 1 1 calc R . .

S1 S 0.11198(8) 0.27955(7) 0.2561(2) 0.0630(8) Uani 1 1 d . . .

OZ3 O 0.2291(3) 0.2722(3) 0.1015(8) 0.093(2) Uani 1 1 d . . .

S2A S 0.22381(17) 0.26764(12) -0.0534(3) 0.0896(14) Uani 0.862(8) 1 d P . .

S2 S 0.2192(6) 0.3054(6) 0.0027(14) 0.056(5) Uani 0.138(8) 1 d P . .

OZ5 O 0.0792(4) 0.2097(3) 0.2058(13) 0.141(6) Uani 0.97(3) 1 d P . .

CT1 C 0.2868(8) 0.3145(6) -0.1213(16) 0.136(6) Uani 1 1 d . . .

CT2 C 0.1905(8) 0.3056(7) -0.0953(16) 0.134(6) Uani 1 1 d . . .



loop_

_atom_site_aniso_label

_atom_site_aniso_U_11

_atom_site_aniso_U_22

_atom_site_aniso_U_33

_atom_site_aniso_U_23

_atom_site_aniso_U_13

_atom_site_aniso_U_12

C6 0.035(3) 0.027(3) 0.047(4) 0.004(3) 0.001(3) 0.010(2)

C1 0.046(4) 0.037(3) 0.037(3) 0.004(3) -0.002(3) 0.019(3)

C5 0.033(3) 0.040(3) 0.047(4) 0.002(3) -0.001(3) 0.016(3)

C8 0.033(3) 0.042(3) 0.055(4) 0.009(3) 0.003(3) 0.015(3)

C2 0.033(3) 0.038(3) 0.051(4) -0.003(3) -0.005(3) 0.017(3)

C4 0.031(3) 0.048(4) 0.051(4) 0.007(3) 0.003(3) 0.016(3)

C3 0.029(3) 0.040(3) 0.068(5) 0.016(3) 0.004(3) 0.010(3)

C9 0.061(5) 0.074(5) 0.062(5) 0.021(4) 0.012(4) 0.040(4)

C7 0.036(3) 0.039(3) 0.047(4) 0.000(3) 0.000(3) 0.017(3)

CZ3 0.038(3) 0.010(2) 0.053(4) 0.001(2) 0.003(3) 0.002(2)

CZ4 0.059(5) 0.095(7) 0.112(9) 0.046(7) 0.024(5) 0.034(5)

O1 0.050(3) 0.031(2) 0.074(3) -0.004(2) -0.006(3) 0.018(2)

O2 0.050(3) 0.052(3) 0.067(3) 0.014(3) 0.014(3) 0.022(2)

S1 0.0549(12) 0.0341(10) 0.0875(17) 0.0060(9) -0.0036(10) 0.0130(8)

OZ3 0.107(5) 0.069(4) 0.093(5) 0.035(4) 0.020(4) 0.037(4)

S2A 0.137(3) 0.0546(17) 0.085(2) 0.0087(14) 0.029(2) 0.0538(18)

S2 0.062(9) 0.051(8) 0.047(8) 0.003(6) -0.023(6) 0.023(7)

OZ5 0.129(9) 0.049(5) 0.216(13) 0.006(5) -0.054(8) 0.023(5)

CT1 0.199(17) 0.088(9) 0.123(11) 0.045(8) 0.071(12) 0.073(10)

CT2 0.199(16) 0.135(12) 0.114(11) 0.002(9) 0.017(11) 0.119(13)



_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

C6 C1 1.371(9) . ?

C6 C5 1.394(9) . ?

C1 C2 1.433(9) . ?

C1 C7 1.535(9) . ?

C5 C4 1.394(9) . ?

C5 C7 1.550(9) 11_556 ?

C8 C9 1.519(11) . ?

C8 C7 1.524(9) . ?

C2 O1 1.361(8) . ?

C2 C3 1.366(10) . ?

C4 C3 1.363(10) . ?

C4 O2 1.380(9) . ?

C7 C5 1.550(9) 12_556 ?

CZ3 S1 1.498(6) . ?

CZ4 S1 1.753(11) . ?

S1 OZ5 1.795(9) . ?

OZ3 S2 1.489(15) . ?

OZ3 S2A 1.559(9) . ?

S2A S2 1.277(16) . ?

S2A CT1 1.750(16) . ?

S2A CT2 1.807(16) . ?

S2 CT2 1.28(2) . ?

S2 CT1 2.19(2) . ?



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

C1 C6 C5 125.2(6) . . ?

C6 C1 C2 115.7(6) . . ?

C6 C1 C7 124.3(6) . . ?

C2 C1 C7 119.9(6) . . ?

C6 C5 C4 116.2(6) . . ?

C6 C5 C7 120.8(6) . 11_556 ?

C4 C5 C7 122.9(6) . 11_556 ?

C9 C8 C7 112.1(6) . . ?

O1 C2 C3 124.8(6) . . ?

O1 C2 C1 115.5(6) . . ?

C3 C2 C1 119.6(6) . . ?

C3 C4 O2 121.9(6) . . ?

C3 C4 C5 120.6(6) . . ?

O2 C4 C5 117.5(6) . . ?

C4 C3 C2 122.3(6) . . ?

C8 C7 C1 113.8(5) . . ?

C8 C7 C5 110.5(5) . 12_556 ?

C1 C7 C5 108.0(5) . 12_556 ?

CZ3 S1 CZ4 105.6(5) . . ?

CZ3 S1 OZ5 107.0(4) . . ?

CZ4 S1 OZ5 99.6(6) . . ?

S2 OZ3 S2A 49.4(6) . . ?

S2 S2A OZ3 62.4(7) . . ?

S2 S2A CT1 91.5(9) . . ?

OZ3 S2A CT1 107.7(7) . . ?

S2 S2A CT2 45.1(8) . . ?

OZ3 S2A CT2 103.8(6) . . ?

CT1 S2A CT2 95.6(8) . . ?

S2A S2 CT2 90.0(11) . . ?

S2A S2 OZ3 68.1(8) . . ?

CT2 S2 OZ3 146.8(14) . . ?

S2A S2 CT1 52.9(7) . . ?

CT2 S2 CT1 95.0(12) . . ?

OZ3 S2 CT1 91.1(9) . . ?

S2A CT1 S2 35.6(5) . . ?

S2 CT2 S2A 44.9(9) . . ?



_diffrn_measured_fraction_theta_max    0.991

_diffrn_reflns_theta_full              28.13

_diffrn_measured_fraction_theta_full   0.991

_refine_diff_density_max    1.150

_refine_diff_density_min   -0.846

_refine_diff_density_rms    0.131

#==========================END



data_asbp3



_database_code_CSD	193891





_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

'C72 H96 O18'

_chemical_formula_weight          1249.49



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            hexagonal

_symmetry_space_group_name_H-M    R-3



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

'-y, x-y, z'

'-x+y, -x, z'

'x+2/3, y+1/3, z+1/3'

'-y+2/3, x-y+1/3, z+1/3'

'-x+y+2/3, -x+1/3, z+1/3'

'x+1/3, y+2/3, z+2/3'

'-y+1/3, x-y+2/3, z+2/3'

'-x+y+1/3, -x+2/3, z+2/3'

'-x, -y, -z'

'y, -x+y, -z'

'x-y, x, -z'

'-x+2/3, -y+1/3, -z+1/3'

'y+2/3, -x+y+1/3, -z+1/3'

'x-y+2/3, x+1/3, -z+1/3'

'-x+1/3, -y+2/3, -z+2/3'

'y+1/3, -x+y+2/3, -z+2/3'

'x-y+1/3, x+2/3, -z+2/3'



_cell_length_a                    24.7866(17)

_cell_length_b                    24.7866(17)

_cell_length_c                    9.7751(9)

_cell_angle_alpha                 90.00

_cell_angle_beta                  90.00

_cell_angle_gamma                 120.00

_cell_volume                      5201.0(7)

_cell_formula_units_Z             3

_cell_measurement_temperature     293(2)

_cell_measurement_reflns_used     ?

_cell_measurement_theta_min       ?

_cell_measurement_theta_max       ?



_exptl_crystal_description        ?

_exptl_crystal_colour             ?

_exptl_crystal_size_max           ?

_exptl_crystal_size_mid           ?

_exptl_crystal_size_min           ?

_exptl_crystal_density_meas       ?

_exptl_crystal_density_diffrn     1.197

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              2016

_exptl_absorpt_coefficient_mu     0.085

_exptl_absorpt_correction_type    ?

_exptl_absorpt_correction_T_min   ?

_exptl_absorpt_correction_T_max   ?

_exptl_absorpt_process_details    ?



_exptl_special_details

;

?

;



_diffrn_ambient_temperature       293(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   ?

_diffrn_measurement_method        ?

_diffrn_detector_area_resol_mean  ?

_diffrn_standards_number          ?

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         ?

_diffrn_reflns_number             16107

_diffrn_reflns_av_R_equivalents   0.0376

_diffrn_reflns_av_sigmaI/netI     0.0281

_diffrn_reflns_limit_h_min        -32

_diffrn_reflns_limit_h_max        32

_diffrn_reflns_limit_k_min        -32

_diffrn_reflns_limit_k_max        32

_diffrn_reflns_limit_l_min        -12

_diffrn_reflns_limit_l_max        12

_diffrn_reflns_theta_min          1.64

_diffrn_reflns_theta_max          28.02

_reflns_number_total              2796

_reflns_number_gt                 2338

_reflns_threshold_expression      >2sigma(I)



_computing_data_collection        ?

_computing_cell_refinement        ?

_computing_data_reduction         ?

_computing_structure_solution     ?

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     ?

_computing_publication_material   ?



_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.

;



_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)+(0.0679P)²+4.2186P] where P=(Fo²+2Fc²)/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          2796

_refine_ls_number_parameters      145

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.0579

_refine_ls_R_factor_gt            0.0479

_refine_ls_wR_factor_ref          0.1266

_refine_ls_wR_factor_gt           0.1194

_refine_ls_goodness_of_fit_ref    1.045

_refine_ls_restrained_S_all       1.045

_refine_ls_shift/su_max           0.001

_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 0.81286(5) 0.29975(5) 0.23079(12) 0.0144(2) Uani 1 1 d . . .

C2 C 0.87400(6) 0.31925(5) 0.19253(12) 0.0158(3) Uani 1 1 d . . .

C3 C 0.92399(5) 0.36782(6) 0.26129(13) 0.0186(3) Uani 1 1 d . . .

H3 H 0.9646 0.3788 0.2380 0.022 Uiso 1 1 calc . . .

C4 C 0.91320(6) 0.39979(6) 0.36440(13) 0.0176(3) Uani 1 1 d . . .

C5 C 0.85238(5) 0.38313(5) 0.40301(12) 0.0145(2) Uani 1 1 d . . .

C6 C 0.80402(5) 0.33248(5) 0.33666(12) 0.0144(2) Uani 1 1 d . . .

H6 H 0.7634 0.3196 0.3642 0.017 Uiso 1 1 calc . . .

C7 C 0.75638(5) 0.24699(5) 0.15935(12) 0.0152(3) Uani 1 1 d . . .

C7A C 0.72108(6) 0.27246(6) 0.07782(13) 0.0208(3) Uani 1 1 d . . .

H7A1 H 0.6847 0.2381 0.0355 0.025 Uiso 1 1 calc R . .

H7A2 H 0.7068 0.2933 0.1398 0.025 Uiso 1 1 calc R . .

C7B C 0.76171(7) 0.31806(7) -0.03252(14) 0.0298(3) Uani 1 1 d . . .

H7B1 H 0.7973 0.3526 0.0092 0.045 Uiso 1 1 calc R . .

H7B2 H 0.7381 0.3329 -0.0814 0.045 Uiso 1 1 calc R . .

H7B3 H 0.7754 0.2974 -0.0949 0.045 Uiso 1 1 calc R . .

C8 C 0.95139(12) 0.41025(12) -0.2051(2) 0.0673(6) Uani 1 1 d . . .

H8A H 0.9155 0.3702 -0.1878 0.101 Uiso 1 1 calc R . .

H8B H 0.9658 0.4114 -0.2968 0.101 Uiso 1 1 calc R . .

H8C H 0.9404 0.4421 -0.1942 0.101 Uiso 1 1 calc R . .

C9 C 1.00159(8) 0.42122(7) -0.10678(16) 0.0334(4) Uani 1 1 d . . .

C10 C 1.06083(9) 0.48227(8) -0.1133(2) 0.0476(5) Uani 1 1 d . . .

H10A H 1.0877 0.4848 -0.0397 0.071 Uiso 1 1 calc R . .

H10B H 1.0518 0.5155 -0.1052 0.071 Uiso 1 1 calc R . .

H10C H 1.0811 0.4857 -0.1991 0.071 Uiso 1 1 calc R . .

O1 O 0.88501(4) 0.29055(4) 0.08327(9) 0.0199(2) Uani 1 1 d . . .

H1 H 0.9188 0.3147 0.0488 0.030 Uiso 1 1 calc R . .

O2 O 0.96010(4) 0.44980(4) 0.42982(11) 0.0265(2) Uani 1 1 d . . .

H2 H 0.9930 0.4501 0.4178 0.040 Uiso 1 1 calc R . .

O3 O 0.99488(5) 0.38199(5) -0.02319(12) 0.0373(3) Uani 1 1 d . . .

H1X H 0.7717(7) 0.2279(7) 0.0944(15) 0.019(4) Uiso 1 1 d . . .



loop_

_atom_site_aniso_label

_atom_site_aniso_U_11

_atom_site_aniso_U_22

_atom_site_aniso_U_33

_atom_site_aniso_U_23

_atom_site_aniso_U_13

_atom_site_aniso_U_12

C1 0.0154(6) 0.0117(5) 0.0159(5) 0.0023(4) 0.0003(4) 0.0066(4)

C2 0.0182(6) 0.0130(5) 0.0172(6) 0.0019(4) 0.0029(4) 0.0086(5)

C3 0.0125(5) 0.0190(6) 0.0245(6) -0.0002(5) 0.0018(4) 0.0081(5)

C4 0.0154(6) 0.0146(6) 0.0217(6) -0.0017(4) -0.0026(4) 0.0065(5)

C5 0.0162(6) 0.0132(5) 0.0162(5) 0.0015(4) -0.0002(4) 0.0090(5)

C6 0.0135(5) 0.0138(5) 0.0170(6) 0.0024(4) 0.0008(4) 0.0076(4)

C7 0.0149(5) 0.0140(5) 0.0157(6) 0.0002(4) 0.0015(4) 0.0063(5)

C7A 0.0203(6) 0.0194(6) 0.0201(6) 0.0013(5) -0.0041(5) 0.0079(5)

C7B 0.0311(8) 0.0272(7) 0.0240(7) 0.0073(5) -0.0041(6) 0.0093(6)

C8 0.0794(16) 0.0625(14) 0.0536(13) -0.0003(11) -0.0194(11) 0.0307(13)

C9 0.0399(9) 0.0356(8) 0.0281(7) 0.0037(6) 0.0141(6) 0.0215(7)

C10 0.0428(10) 0.0385(9) 0.0597(12) 0.0185(8) 0.0234(9) 0.0189(8)

O1 0.0180(4) 0.0165(4) 0.0228(5) -0.0021(3) 0.0066(3) 0.0068(4)

O2 0.0133(4) 0.0247(5) 0.0382(6) -0.0149(4) -0.0045(4) 0.0072(4)

O3 0.0340(6) 0.0344(6) 0.0373(6) 0.0119(5) 0.0141(5) 0.0125(5)



_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 1.3919(16) . ?

C1 C6 1.3982(16) . ?

C1 C7 1.5254(16) . ?

C2 O1 1.3839(14) . ?

C2 C3 1.3946(17) . ?

C3 C4 1.3881(17) . ?

C4 O2 1.3624(15) . ?

C4 C5 1.4012(16) . ?

C5 C6 1.3888(16) . ?

C5 C7 1.5206(16) 18_545 ?

C7 C5 1.5207(16) 17 ?

C7 C7A 1.5337(17) . ?

C7A C7B 1.5222(18) . ?

C8 C9 1.486(3) . ?

C9 O3 1.2163(19) . ?

C9 C10 1.493(2) . ?



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 117.17(11) . . ?

C2 C1 C7 123.22(10) . . ?

C6 C1 C7 119.56(10) . . ?

O1 C2 C1 119.28(10) . . ?

O1 C2 C3 119.82(10) . . ?

C1 C2 C3 120.89(11) . . ?

C4 C3 C2 120.08(11) . . ?

O2 C4 C3 122.68(11) . . ?

O2 C4 C5 116.39(11) . . ?

C3 C4 C5 120.89(11) . . ?

C6 C5 C4 117.11(11) . . ?

C6 C5 C7 123.78(10) . 18_545 ?

C4 C5 C7 119.01(10) . 18_545 ?

C5 C6 C1 123.74(11) . . ?

C5 C7 C1 109.47(9) 17 . ?

C5 C7 C7A 113.97(10) 17 . ?

C1 C7 C7A 110.66(10) . . ?

C7B C7A C7 111.84(11) . . ?

O3 C9 C8 121.40(17) . . ?

O3 C9 C10 120.73(16) . . ?

C8 C9 C10 117.87(17) . . ?



_diffrn_measured_fraction_theta_max    0.998

_diffrn_reflns_theta_full              28.02

_diffrn_measured_fraction_theta_full   0.998

_refine_diff_density_max    0.403

_refine_diff_density_min   -0.201

_refine_diff_density_rms    0.050









