# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Leonard J Barbour'
_publ_contact_author_address     
;
University of Stellenbosch
SOUTH AFRICA
;

_publ_contact_author_email       LJB@SUN.AC.ZA

_publ_section_title              
;
Polymorphism of pure p-tert-butylcalix[4]arene:
subtle thermally -induced modifications
;
loop_
_publ_author_name
'Leonard J. Barbour'
'Jerry L. Atwood'
'Gareth O. Lloyd'
'Praveen K. Thallapally'

data_TBC4
_database_code_depnum_ccdc_archive 'CCDC 231714'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            2b
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 O4'
_chemical_formula_weight         648.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   12.581(2)
_cell_length_b                   26.239(2)
_cell_length_c                   12.718(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.34(2)
_cell_angle_gamma                90.00
_cell_volume                     4198.2(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8262
_exptl_absorpt_correction_T_max  0.8455
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
Data were corrected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54060
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            12369
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.86
_diffrn_reflns_theta_max         59.93
_reflns_number_total             5875
_reflns_number_gt                3470
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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.
;

_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^)+(0.0804P)^2^+0.2565P] 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     SHELXL
_refine_ls_extinction_coef       0.0027(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5875
_refine_ls_number_parameters     586
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1600
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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
O1A O 0.80851(16) 0.22861(7) -0.21147(14) 0.0607(5) Uani 1 1 d D . .
C1A C 0.7612(2) 0.27454(10) -0.23928(19) 0.0480(7) Uani 1 1 d . . .
C2A C 0.6913(2) 0.29686(10) -0.16960(18) 0.0468(7) Uani 1 1 d . . .
C3A C 0.6423(2) 0.34194(10) -0.19933(19) 0.0521(7) Uani 1 1 d . . .
H3A H 0.5953 0.3571 -0.1527 0.063 Uiso 1 1 calc R . .
C4A C 0.6601(2) 0.36560(10) -0.2956(2) 0.0527(7) Uani 1 1 d . A .
C5A C 0.7310(2) 0.34140(10) -0.36170(19) 0.0523(7) Uani 1 1 d . . .
H5A H 0.7445 0.3561 -0.4268 0.063 Uiso 1 1 calc R . .
C6A C 0.7832(2) 0.29621(10) -0.33622(18) 0.0479(7) Uani 1 1 d . . .
C7A C 0.8628(2) 0.27353(10) -0.41196(19) 0.0521(7) Uani 1 1 d . . .
H7A1 H 0.8408 0.2813 -0.4834 0.063 Uiso 1 1 calc R . .
H7A2 H 0.8630 0.2368 -0.4042 0.063 Uiso 1 1 calc R . .
C8A C 0.6050(3) 0.41441(12) -0.3280(2) 0.0748(9) Uani 1 1 d D . .
C9A C 0.6946(6) 0.4547(2) -0.3534(7) 0.122(3) Uani 0.646(9) 1 d PD A 1
H9A1 H 0.7374 0.4424 -0.4102 0.183 Uiso 0.646(9) 1 calc PR A 1
H9A2 H 0.7384 0.4597 -0.2922 0.183 Uiso 0.646(9) 1 calc PR A 1
H9A3 H 0.6623 0.4865 -0.3731 0.183 Uiso 0.646(9) 1 calc PR A 1
C10A C 0.5474(6) 0.4055(3) -0.4325(5) 0.115(3) Uani 0.646(9) 1 d PD A 1
H10A H 0.5177 0.4371 -0.4572 0.172 Uiso 0.646(9) 1 calc PR A 1
H10B H 0.4914 0.3811 -0.4227 0.172 Uiso 0.646(9) 1 calc PR A 1
H10C H 0.5968 0.3927 -0.4834 0.172 Uiso 0.646(9) 1 calc PR A 1
C11A C 0.5330(9) 0.4370(4) -0.2483(7) 0.141(5) Uani 0.646(9) 1 d PD A 1
H11A H 0.5040 0.4683 -0.2748 0.211 Uiso 0.646(9) 1 calc PR A 1
H11B H 0.5723 0.4436 -0.1848 0.211 Uiso 0.646(9) 1 calc PR A 1
H11C H 0.4762 0.4136 -0.2338 0.211 Uiso 0.646(9) 1 calc PR A 1
C12A C 0.6243(18) 0.4326(7) -0.4376(10) 0.153(10) Uani 0.354(9) 1 d PD A 2
H12A H 0.5805 0.4617 -0.4517 0.229 Uiso 0.354(9) 1 calc PR A 2
H12B H 0.6071 0.4059 -0.4864 0.229 Uiso 0.354(9) 1 calc PR A 2
H12C H 0.6977 0.4417 -0.4450 0.229 Uiso 0.354(9) 1 calc PR A 2
C13A C 0.4806(7) 0.4017(5) -0.3237(13) 0.125(6) Uani 0.354(9) 1 d PD A 2
H13A H 0.4405 0.4324 -0.3342 0.188 Uiso 0.354(9) 1 calc PR A 2
H13B H 0.4638 0.3874 -0.2563 0.188 Uiso 0.354(9) 1 calc PR A 2
H13C H 0.4630 0.3777 -0.3779 0.188 Uiso 0.354(9) 1 calc PR A 2
C14A C 0.6201(16) 0.4527(6) -0.2392(12) 0.151(10) Uani 0.354(9) 1 d PD A 2
H14A H 0.6927 0.4641 -0.2378 0.227 Uiso 0.354(9) 1 calc PR A 2
H14B H 0.6034 0.4368 -0.1734 0.227 Uiso 0.354(9) 1 calc PR A 2
H14C H 0.5739 0.4813 -0.2504 0.227 Uiso 0.354(9) 1 calc PR A 2
H1A H 0.8820(19) 0.2225(16) -0.236(3) 0.160(18) Uiso 1 1 d D . .
O1B O 1.01188(15) 0.22672(7) -0.27247(14) 0.0604(5) Uani 1 1 d D . .
C1B C 1.0442(2) 0.27122(10) -0.32220(19) 0.0480(7) Uani 1 1 d . . .
C2B C 0.9747(2) 0.29348(10) -0.39405(18) 0.0455(6) Uani 1 1 d . . .
C3B C 1.0089(2) 0.33675(10) -0.44645(19) 0.0514(7) Uani 1 1 d . . .
H3B H 0.9630 0.3520 -0.4947 0.062 Uiso 1 1 calc R . .
C4B C 1.1086(2) 0.35841(10) -0.43019(19) 0.0511(7) Uani 1 1 d . B .
C5B C 1.1737(2) 0.33439(10) -0.35670(19) 0.0520(7) Uani 1 1 d . . .
H5B H 1.2407 0.3481 -0.3438 0.062 Uiso 1 1 calc R . .
C6B C 1.1445(2) 0.29134(10) -0.30185(18) 0.0466(7) Uani 1 1 d . . .
C7B C 1.2186(2) 0.26877(11) -0.22003(18) 0.0555(7) Uani 1 1 d . . .
H7B1 H 1.2915 0.2755 -0.2401 0.067 Uiso 1 1 calc R . .
H7B2 H 1.2089 0.2321 -0.2183 0.067 Uiso 1 1 calc R . .
C8B C 1.1453(2) 0.40576(11) -0.4891(2) 0.0651(8) Uani 1 1 d D . .
C9B C 1.1707(9) 0.4485(2) -0.4128(5) 0.110(4) Uani 0.590(9) 1 d PD B 1
H9B1 H 1.1964 0.4775 -0.4510 0.165 Uiso 0.590(9) 1 calc PR B 1
H9B2 H 1.2242 0.4373 -0.3639 0.165 Uiso 0.590(9) 1 calc PR B 1
H9B3 H 1.1076 0.4577 -0.3753 0.165 Uiso 0.590(9) 1 calc PR B 1
C10B C 1.2500(5) 0.3935(2) -0.5502(6) 0.085(3) Uani 0.590(9) 1 d PD B 1
H10D H 1.2740 0.4236 -0.5858 0.127 Uiso 0.590(9) 1 calc PR B 1
H10E H 1.2363 0.3671 -0.6008 0.127 Uiso 0.590(9) 1 calc PR B 1
H10F H 1.3037 0.3823 -0.5016 0.127 Uiso 0.590(9) 1 calc PR B 1
C11B C 1.0684(6) 0.4244(3) -0.5750(6) 0.104(3) Uani 0.590(9) 1 d PD B 1
H11D H 1.0022 0.4342 -0.5437 0.157 Uiso 0.590(9) 1 calc PR B 1
H11E H 1.0561 0.3976 -0.6249 0.157 Uiso 0.590(9) 1 calc PR B 1
H11F H 1.0988 0.4533 -0.6103 0.157 Uiso 0.590(9) 1 calc PR B 1
C12B C 1.2529(9) 0.4238(6) -0.4492(13) 0.157(9) Uani 0.410(9) 1 d PD B 2
H12D H 1.2721 0.4548 -0.4846 0.235 Uiso 0.410(9) 1 calc PR B 2
H12E H 1.3054 0.3981 -0.4628 0.235 Uiso 0.410(9) 1 calc PR B 2
H12F H 1.2491 0.4300 -0.3749 0.235 Uiso 0.410(9) 1 calc PR B 2
C13B C 1.1398(13) 0.3928(5) -0.6051(6) 0.134(6) Uani 0.410(9) 1 d PD B 2
H13D H 1.1626 0.4217 -0.6456 0.201 Uiso 0.410(9) 1 calc PR B 2
H13E H 1.0679 0.3844 -0.6240 0.201 Uiso 0.410(9) 1 calc PR B 2
H13F H 1.1852 0.3643 -0.6193 0.201 Uiso 0.410(9) 1 calc PR B 2
C14B C 1.0618(9) 0.4471(3) -0.4638(12) 0.127(6) Uani 0.410(9) 1 d PD B 2
H14D H 1.0579 0.4517 -0.3890 0.191 Uiso 0.410(9) 1 calc PR B 2
H14E H 0.9936 0.4366 -0.4902 0.191 Uiso 0.410(9) 1 calc PR B 2
H14F H 1.0819 0.4786 -0.4963 0.191 Uiso 0.410(9) 1 calc PR B 2
H1B H 1.044(4) 0.222(2) -0.199(2) 0.21(2) Uiso 1 1 d D . .
O1C O 1.07743(16) 0.22344(7) -0.07149(14) 0.0613(5) Uani 1 1 d D . .
C1C C 1.1278(2) 0.26815(10) -0.04184(19) 0.0478(7) Uani 1 1 d . . .
C2C C 1.1996(2) 0.29021(10) -0.11094(19) 0.0492(7) Uani 1 1 d . . .
C3C C 1.2518(2) 0.33408(11) -0.0789(2) 0.0544(7) Uani 1 1 d . . .
H3C H 1.2995 0.3492 -0.1250 0.065 Uiso 1 1 calc R . .
C4C C 1.2361(2) 0.35670(10) 0.0191(2) 0.0529(7) Uani 1 1 d . C .
C5C C 1.1633(2) 0.33287(10) 0.08416(19) 0.0522(7) Uani 1 1 d . . .
H5C H 1.1508 0.3472 0.1499 0.063 Uiso 1 1 calc R . .
C6C C 1.1080(2) 0.28906(10) 0.05718(19) 0.0473(7) Uani 1 1 d . . .
C7C C 1.02685(19) 0.26760(11) 0.13179(18) 0.0524(7) Uani 1 1 d . . .
H7C1 H 1.0497 0.2739 0.2036 0.063 Uiso 1 1 calc R . .
H7C2 H 1.0221 0.2310 0.1220 0.063 Uiso 1 1 calc R . .
C8C C 1.2928(3) 0.40520(12) 0.0535(2) 0.0707(9) Uani 1 1 d D . .
C9C C 1.3518(5) 0.3959(3) 0.1576(4) 0.096(2) Uani 0.742(9) 1 d PD C 1
H9C1 H 1.3844 0.4270 0.1808 0.144 Uiso 0.742(9) 1 calc PR C 1
H9C2 H 1.4056 0.3705 0.1475 0.144 Uiso 0.742(9) 1 calc PR C 1
H9C3 H 1.3024 0.3844 0.2097 0.144 Uiso 0.742(9) 1 calc PR C 1
C10C C 1.3694(6) 0.4273(3) -0.0250(5) 0.116(3) Uani 0.742(9) 1 d PD C 1
H10G H 1.3918 0.4604 -0.0019 0.174 Uiso 0.742(9) 1 calc PR C 1
H10H H 1.3349 0.4301 -0.0924 0.174 Uiso 0.742(9) 1 calc PR C 1
H10I H 1.4302 0.4054 -0.0308 0.174 Uiso 0.742(9) 1 calc PR C 1
C11C C 1.2082(4) 0.44732(19) 0.0767(6) 0.110(3) Uani 0.742(9) 1 d PD C 1
H11G H 1.1618 0.4359 0.1315 0.166 Uiso 0.742(9) 1 calc PR C 1
H11H H 1.1674 0.4540 0.0142 0.166 Uiso 0.742(9) 1 calc PR C 1
H11I H 1.2435 0.4780 0.0988 0.166 Uiso 0.742(9) 1 calc PR C 1
C12C C 1.4117(8) 0.3899(7) 0.0361(16) 0.128(8) Uani 0.258(9) 1 d PD C 2
H12G H 1.4203 0.3771 -0.0341 0.192 Uiso 0.258(9) 1 calc PR C 2
H12H H 1.4315 0.3640 0.0857 0.192 Uiso 0.258(9) 1 calc PR C 2
H12I H 1.4563 0.4192 0.0460 0.192 Uiso 0.258(9) 1 calc PR C 2
C13C C 1.268(2) 0.4437(6) -0.0339(14) 0.140(11) Uani 0.258(9) 1 d PD C 2
H13G H 1.3031 0.4754 -0.0189 0.209 Uiso 0.258(9) 1 calc PR C 2
H13H H 1.1924 0.4493 -0.0375 0.209 Uiso 0.258(9) 1 calc PR C 2
H13I H 1.2922 0.4306 -0.1000 0.209 Uiso 0.258(9) 1 calc PR C 2
C14C C 1.270(3) 0.4189(9) 0.1668(11) 0.179(18) Uani 0.258(9) 1 d PD C 2
H14G H 1.3294 0.4377 0.1952 0.269 Uiso 0.258(9) 1 calc PR C 2
H14H H 1.2603 0.3883 0.2069 0.269 Uiso 0.258(9) 1 calc PR C 2
H14I H 1.2073 0.4394 0.1701 0.269 Uiso 0.258(9) 1 calc PR C 2
H1C H 1.002(2) 0.2210(19) -0.042(3) 0.19(2) Uiso 1 1 d D . .
O1D O 0.87305(15) 0.22632(7) -0.01060(15) 0.0606(5) Uani 1 1 d D . .
C1D C 0.8458(2) 0.27098(10) 0.04138(18) 0.0467(7) Uani 1 1 d . . .
C2D C 0.9181(2) 0.29121(10) 0.11428(18) 0.0472(7) Uani 1 1 d . . .
C3D C 0.8889(2) 0.33462(10) 0.16729(18) 0.0501(7) Uani 1 1 d . . .
H3D H 0.9361 0.3481 0.2165 0.060 Uiso 1 1 calc R . .
C4D C 0.7927(2) 0.35940(10) 0.1513(2) 0.0539(7) Uani 1 1 d . D .
C5D C 0.7239(2) 0.33792(10) 0.07714(19) 0.0517(7) Uani 1 1 d . . .
H5D H 0.6587 0.3535 0.0646 0.062 Uiso 1 1 calc R . .
C6D C 0.7490(2) 0.29408(10) 0.02121(18) 0.0462(7) Uani 1 1 d . . .
C7D C 0.6712(2) 0.27448(10) -0.06078(18) 0.0531(7) Uani 1 1 d . . .
H7D1 H 0.5994 0.2829 -0.0393 0.064 Uiso 1 1 calc R . .
H7D2 H 0.6765 0.2376 -0.0645 0.064 Uiso 1 1 calc R . .
C8D C 0.7665(3) 0.40774(12) 0.2119(2) 0.0695(9) Uani 1 1 d D . .
C9D C 0.7706(6) 0.3955(3) 0.3286(4) 0.096(2) Uani 0.750(11) 1 d PD D 1
H9D1 H 0.8402 0.3832 0.3469 0.143 Uiso 0.750(11) 1 calc PR D 1
H9D2 H 0.7188 0.3698 0.3444 0.143 Uiso 0.750(11) 1 calc PR D 1
H9D3 H 0.7555 0.4258 0.3682 0.143 Uiso 0.750(11) 1 calc PR D 1
C10D C 0.8537(4) 0.4481(2) 0.1879(5) 0.094(2) Uani 0.750(11) 1 d PD D 1
H10J H 0.8381 0.4791 0.2250 0.141 Uiso 0.750(11) 1 calc PR D 1
H10K H 0.8550 0.4548 0.1137 0.141 Uiso 0.750(11) 1 calc PR D 1
H10L H 0.9217 0.4354 0.2102 0.141 Uiso 0.750(11) 1 calc PR D 1
C11D C 0.6610(6) 0.4311(3) 0.1798(7) 0.118(3) Uani 0.750(11) 1 d PD D 1
H11J H 0.6549 0.4644 0.2100 0.177 Uiso 0.750(11) 1 calc PR D 1
H11K H 0.6041 0.4099 0.2046 0.177 Uiso 0.750(11) 1 calc PR D 1
H11L H 0.6573 0.4335 0.1046 0.177 Uiso 0.750(11) 1 calc PR D 1
C12D C 0.827(3) 0.4183(11) 0.313(2) 0.21(2) Uani 0.250(11) 1 d PD D 2
H12J H 0.8851 0.4409 0.2990 0.316 Uiso 0.250(11) 1 calc PR D 2
H12K H 0.8538 0.3869 0.3413 0.316 Uiso 0.250(11) 1 calc PR D 2
H12L H 0.7801 0.4338 0.3631 0.316 Uiso 0.250(11) 1 calc PR D 2
C13D C 0.745(5) 0.4507(9) 0.1320(18) 0.30(4) Uani 0.250(11) 1 d PD D 2
H13J H 0.7635 0.4829 0.1630 0.449 Uiso 0.250(11) 1 calc PR D 2
H13K H 0.6716 0.4507 0.1124 0.449 Uiso 0.250(11) 1 calc PR D 2
H13L H 0.7880 0.4453 0.0706 0.449 Uiso 0.250(11) 1 calc PR D 2
C14D C 0.6552(15) 0.3977(9) 0.260(3) 0.181(14) Uani 0.250(11) 1 d PD D 2
H14J H 0.6569 0.3663 0.2994 0.272 Uiso 0.250(11) 1 calc PR D 2
H14K H 0.6031 0.3952 0.2052 0.272 Uiso 0.250(11) 1 calc PR D 2
H14L H 0.6369 0.4252 0.3066 0.272 Uiso 0.250(11) 1 calc PR D 2
H1D H 0.839(3) 0.2239(17) -0.081(2) 0.162(18) Uiso 1 1 d 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
O1A 0.0712(15) 0.0542(12) 0.0567(12) -0.0030(9) 0.0043(10) -0.0046(10)
C1A 0.0532(17) 0.0496(16) 0.0412(16) -0.0051(13) -0.0053(13) -0.0078(13)
C2A 0.0469(16) 0.0586(17) 0.0349(14) -0.0052(13) 0.0020(12) -0.0138(14)
C3A 0.0484(17) 0.0669(19) 0.0412(16) -0.0101(14) 0.0053(13) -0.0020(14)
C4A 0.0551(18) 0.0631(18) 0.0401(16) -0.0040(13) 0.0044(13) -0.0039(14)
C5A 0.0544(18) 0.0657(19) 0.0369(15) 0.0016(13) 0.0017(13) -0.0124(15)
C6A 0.0484(16) 0.0595(18) 0.0358(15) -0.0103(13) -0.0015(12) -0.0107(14)
C7A 0.0590(18) 0.0625(17) 0.0348(14) -0.0113(13) -0.0038(12) -0.0041(14)
C8A 0.088(3) 0.071(2) 0.066(2) 0.0077(17) 0.0098(19) 0.0147(19)
C9A 0.163(8) 0.068(4) 0.136(8) 0.023(4) 0.052(6) 0.008(4)
C10A 0.126(7) 0.129(8) 0.089(6) 0.019(5) -0.007(5) 0.059(5)
C11A 0.197(11) 0.120(9) 0.106(7) 0.035(6) 0.072(8) 0.092(8)
C12A 0.23(3) 0.132(17) 0.101(12) 0.072(12) 0.059(15) 0.066(16)
C13A 0.097(10) 0.131(12) 0.147(15) -0.002(10) -0.014(9) 0.049(8)
C14A 0.20(2) 0.077(10) 0.174(18) -0.020(11) -0.056(18) 0.032(13)
O1B 0.0723(14) 0.0527(12) 0.0562(13) 0.0005(10) 0.0053(11) -0.0017(10)
C1B 0.0593(19) 0.0485(16) 0.0362(15) -0.0074(12) 0.0102(13) 0.0049(14)
C2B 0.0515(17) 0.0534(16) 0.0314(14) -0.0126(12) 0.0035(12) 0.0016(13)
C3B 0.0548(18) 0.0625(18) 0.0369(15) -0.0075(13) -0.0026(13) 0.0059(15)
C4B 0.0551(18) 0.0547(17) 0.0436(15) -0.0055(13) 0.0001(13) 0.0023(14)
C5B 0.0511(17) 0.0631(18) 0.0418(16) -0.0090(14) 0.0017(13) -0.0006(14)
C6B 0.0529(17) 0.0528(16) 0.0344(14) -0.0089(13) 0.0053(12) 0.0077(14)
C7B 0.0524(17) 0.0680(18) 0.0461(16) -0.0018(14) 0.0055(13) 0.0133(14)
C8B 0.071(2) 0.0583(19) 0.066(2) 0.0090(16) -0.0055(16) -0.0047(16)
C9B 0.180(12) 0.061(4) 0.089(5) -0.010(4) 0.001(6) -0.026(5)
C10B 0.086(5) 0.087(5) 0.082(5) 0.022(4) 0.024(4) -0.003(4)
C11B 0.121(7) 0.095(6) 0.097(7) 0.043(5) -0.029(5) -0.021(5)
C12B 0.111(11) 0.143(15) 0.22(2) 0.104(16) -0.033(12) -0.055(10)
C13B 0.201(19) 0.121(11) 0.080(8) 0.036(7) 0.037(9) -0.019(10)
C14B 0.114(10) 0.070(7) 0.198(16) 0.029(8) 0.007(10) 0.000(6)
O1C 0.0724(15) 0.0533(12) 0.0580(12) 0.0034(9) 0.0034(11) 0.0037(10)
C1C 0.0479(17) 0.0520(17) 0.0435(16) 0.0073(13) -0.0041(13) 0.0115(13)
C2C 0.0481(17) 0.0605(18) 0.0390(15) 0.0057(13) 0.0021(13) 0.0123(14)
C3C 0.0518(18) 0.072(2) 0.0398(16) 0.0128(14) 0.0046(13) 0.0050(15)
C4C 0.0556(18) 0.0626(18) 0.0405(16) 0.0051(14) 0.0026(13) 0.0040(14)
C5C 0.0553(18) 0.0683(19) 0.0329(14) 0.0057(13) 0.0026(13) 0.0086(15)
C6C 0.0483(16) 0.0565(17) 0.0372(15) 0.0100(13) -0.0020(12) 0.0103(14)
C7C 0.0586(18) 0.0622(17) 0.0364(14) 0.0149(13) 0.0009(13) 0.0028(13)
C8C 0.078(2) 0.071(2) 0.064(2) 0.0058(17) 0.0039(18) -0.0141(18)
C9C 0.112(5) 0.103(5) 0.072(4) -0.014(3) -0.017(4) -0.031(4)
C10C 0.163(7) 0.106(6) 0.079(4) -0.008(4) 0.037(5) -0.064(5)
C11C 0.118(5) 0.072(4) 0.141(7) -0.015(4) 0.011(4) 0.001(3)
C12C 0.121(15) 0.132(16) 0.131(18) 0.009(13) -0.038(12) -0.075(13)
C13C 0.16(2) 0.063(10) 0.19(2) 0.023(12) -0.05(2) -0.015(12)
C14C 0.34(5) 0.11(2) 0.082(14) -0.055(15) 0.07(2) -0.09(3)
O1D 0.0736(14) 0.0529(12) 0.0552(13) 0.0009(10) 0.0029(11) -0.0039(10)
C1D 0.0575(18) 0.0471(16) 0.0358(14) 0.0070(12) 0.0080(13) -0.0034(13)
C2D 0.0485(16) 0.0586(17) 0.0346(14) 0.0133(13) 0.0052(12) -0.0007(14)
C3D 0.0534(18) 0.0624(18) 0.0345(15) 0.0031(13) -0.0018(13) -0.0050(14)
C4D 0.0601(19) 0.0591(18) 0.0425(16) 0.0025(13) 0.0006(14) 0.0009(15)
C5D 0.0504(17) 0.0631(18) 0.0418(15) 0.0055(14) 0.0010(13) 0.0028(14)
C6D 0.0456(16) 0.0581(17) 0.0349(14) 0.0082(13) 0.0070(12) -0.0079(14)
C7D 0.0530(17) 0.0622(17) 0.0441(16) 0.0004(13) 0.0032(13) -0.0114(14)
C8D 0.079(2) 0.068(2) 0.062(2) -0.0108(17) -0.0033(17) 0.0079(18)
C9D 0.128(6) 0.111(6) 0.048(3) -0.032(3) 0.013(3) 0.008(4)
C10D 0.124(5) 0.063(3) 0.095(5) -0.011(3) -0.008(3) -0.001(3)
C11D 0.112(5) 0.103(7) 0.137(7) -0.052(5) -0.043(4) 0.056(5)
C12D 0.26(4) 0.12(3) 0.24(4) -0.12(3) -0.15(3) 0.06(2)
C13D 0.67(12) 0.058(15) 0.17(3) 0.026(16) 0.09(5) 0.10(3)
C14D 0.16(2) 0.14(2) 0.25(4) -0.12(2) -0.02(2) 0.068(19)

_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
O1A C1A 1.389(3) . ?
C1A C2A 1.383(3) . ?
C1A C6A 1.387(3) . ?
C2A C3A 1.385(3) . ?
C2A C7D 1.526(3) . ?
C3A C4A 1.392(3) . ?
C4A C5A 1.384(3) . ?
C4A C8A 1.512(4) . ?
C5A C6A 1.393(4) . ?
C6A C7A 1.515(3) . ?
C7A C2B 1.518(3) . ?
C8A C11A 1.487(6) . ?
C8A C12A 1.493(8) . ?
C8A C14A 1.523(9) . ?
C8A C10A 1.529(6) . ?
C8A C9A 1.579(6) . ?
C8A C13A 1.601(8) . ?
O1B C1B 1.390(3) . ?
C1B C2B 1.389(3) . ?
C1B C6B 1.391(3) . ?
C2B C3B 1.386(3) . ?
C3B C4B 1.392(3) . ?
C4B C5B 1.390(3) . ?
C4B C8B 1.524(4) . ?
C5B C6B 1.379(3) . ?
C6B C7B 1.513(3) . ?
C7B C2C 1.517(3) . ?
C8B C13B 1.515(8) . ?
C8B C9B 1.515(6) . ?
C8B C12B 1.518(8) . ?
C8B C11B 1.536(6) . ?
C8B C14B 1.546(8) . ?
C8B C10B 1.566(5) . ?
O1C C1C 1.384(3) . ?
C1C C2C 1.391(3) . ?
C1C C6C 1.397(3) . ?
C2C C3C 1.385(4) . ?
C3C C4C 1.396(3) . ?
C4C C5C 1.387(3) . ?
C4C C8C 1.521(4) . ?
C5C C6C 1.386(3) . ?
C6C C7C 1.507(3) . ?
C7C C2D 1.517(3) . ?
C8C C10C 1.508(5) . ?
C8C C14C 1.513(9) . ?
C8C C13C 1.533(9) . ?
C8C C9C 1.534(5) . ?
C8C C11C 1.564(5) . ?
C8C C12C 1.567(9) . ?
O1D C1D 1.389(3) . ?
C1D C6D 1.383(3) . ?
C1D C2D 1.399(3) . ?
C2D C3D 1.375(3) . ?
C3D C4D 1.388(3) . ?
C4D C5D 1.395(3) . ?
C4D C8D 1.521(4) . ?
C5D C6D 1.390(3) . ?
C6D C7D 1.516(3) . ?
C8D C11D 1.515(5) . ?
C8D C12D 1.517(10) . ?
C8D C9D 1.518(5) . ?
C8D C13D 1.540(10) . ?
C8D C10D 1.557(5) . ?
C8D C14D 1.557(10) . ?

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
C2A C1A C6A 121.8(3) . . ?
C2A C1A O1A 118.5(2) . . ?
C6A C1A O1A 119.6(2) . . ?
C1A C2A C3A 118.1(2) . . ?
C1A C2A C7D 121.9(3) . . ?
C3A C2A C7D 120.0(2) . . ?
C2A C3A C4A 123.2(3) . . ?
C5A C4A C3A 115.9(3) . . ?
C5A C4A C8A 121.2(2) . . ?
C3A C4A C8A 122.8(3) . . ?
C4A C5A C6A 123.7(2) . . ?
C1A C6A C5A 117.3(2) . . ?
C1A C6A C7A 122.7(3) . . ?
C5A C6A C7A 119.9(2) . . ?
C6A C7A C2B 112.64(19) . . ?
C11A C8A C12A 127.7(8) . . ?
C11A C8A C4A 115.6(4) . . ?
C12A C8A C4A 116.6(7) . . ?
C11A C8A C14A 46.0(7) . . ?
C12A C8A C14A 117.5(11) . . ?
C4A C8A C14A 107.6(7) . . ?
C11A C8A C10A 111.5(6) . . ?
C12A C8A C10A 46.9(8) . . ?
C4A C8A C10A 108.8(4) . . ?
C14A C8A C10A 143.4(7) . . ?
C11A C8A C9A 108.1(6) . . ?
C12A C8A C9A 58.4(9) . . ?
C4A C8A C9A 107.3(3) . . ?
C14A C8A C9A 67.9(8) . . ?
C10A C8A C9A 105.1(5) . . ?
C11A C8A C13A 57.3(6) . . ?
C12A C8A C13A 105.2(10) . . ?
C4A C8A C13A 105.1(5) . . ?
C14A C8A C13A 103.3(9) . . ?
C10A C8A C13A 62.6(6) . . ?
C9A C8A C13A 147.6(6) . . ?
C2B C1B O1B 117.9(2) . . ?
C2B C1B C6B 121.9(2) . . ?
O1B C1B C6B 120.1(2) . . ?
C3B C2B C1B 117.7(2) . . ?
C3B C2B C7A 120.0(2) . . ?
C1B C2B C7A 122.2(2) . . ?
C2B C3B C4B 123.0(3) . . ?
C5B C4B C3B 116.2(3) . . ?
C5B C4B C8B 121.4(3) . . ?
C3B C4B C8B 122.4(2) . . ?
C6B C5B C4B 123.6(3) . . ?
C5B C6B C1B 117.5(2) . . ?
C5B C6B C7B 120.3(2) . . ?
C1B C6B C7B 122.2(2) . . ?
C6B C7B C2C 112.6(2) . . ?
C13B C8B C9B 142.9(5) . . ?
C13B C8B C12B 115.6(8) . . ?
C9B C8B C12B 51.0(6) . . ?
C13B C8B C4B 106.5(5) . . ?
C9B C8B C4B 110.6(3) . . ?
C12B C8B C4B 111.3(5) . . ?
C13B C8B C11B 49.7(5) . . ?
C9B C8B C11B 110.4(5) . . ?
C12B C8B C11B 134.0(5) . . ?
C4B C8B C11B 114.7(3) . . ?
C13B C8B C14B 109.4(8) . . ?
C9B C8B C14B 59.2(5) . . ?
C12B C8B C14B 108.5(8) . . ?
C4B C8B C14B 105.1(4) . . ?
C11B C8B C14B 59.9(6) . . ?
C13B C8B C10B 60.3(6) . . ?
C9B C8B C10B 107.2(5) . . ?
C12B C8B C10B 58.7(7) . . ?
C4B C8B C10B 109.6(3) . . ?
C11B C8B C10B 103.9(4) . . ?
C14B C8B C10B 145.3(5) . . ?
O1C C1C C2C 118.6(2) . . ?
O1C C1C C6C 119.7(2) . . ?
C2C C1C C6C 121.7(3) . . ?
C3C C2C C1C 118.0(2) . . ?
C3C C2C C7B 120.0(2) . . ?
C1C C2C C7B 122.0(3) . . ?
C2C C3C C4C 123.1(3) . . ?
C5C C4C C3C 116.0(3) . . ?
C5C C4C C8C 121.0(2) . . ?
C3C C4C C8C 123.0(3) . . ?
C6C C5C C4C 124.0(2) . . ?
C5C C6C C1C 117.2(2) . . ?
C5C C6C C7C 119.7(2) . . ?
C1C C6C C7C 123.0(3) . . ?
C6C C7C C2D 111.63(19) . . ?
C10C C8C C14C 131.5(10) . . ?
C10C C8C C4C 115.6(3) . . ?
C14C C8C C4C 112.5(9) . . ?
C10C C8C C13C 52.8(8) . . ?
C14C C8C C13C 119.7(13) . . ?
C4C C8C C13C 104.5(7) . . ?
C10C C8C C9C 108.9(5) . . ?
C14C C8C C9C 46.2(13) . . ?
C4C C8C C9C 109.8(3) . . ?
C13C C8C C9C 145.7(7) . . ?
C10C C8C C11C 107.0(4) . . ?
C14C C8C C11C 61.4(13) . . ?
C4C C8C C11C 109.1(3) . . ?
C13C C8C C11C 62.2(9) . . ?
C9C C8C C11C 106.0(4) . . ?
C10C C8C C12C 52.4(7) . . ?
C14C C8C C12C 112.2(16) . . ?
C4C C8C C12C 101.0(6) . . ?
C13C C8C C12C 105.0(11) . . ?
C9C C8C C12C 67.8(7) . . ?
C11C C8C C12C 149.3(7) . . ?
C6D C1D O1D 120.0(2) . . ?
C6D C1D C2D 121.7(2) . . ?
O1D C1D C2D 118.3(2) . . ?
C3D C2D C1D 117.7(2) . . ?
C3D C2D C7C 120.7(2) . . ?
C1D C2D C7C 121.6(2) . . ?
C2D C3D C4D 123.5(2) . . ?
C3D C4D C5D 116.5(3) . . ?
C3D C4D C8D 120.5(3) . . ?
C5D C4D C8D 123.0(3) . . ?
C6D C5D C4D 122.6(3) . . ?
C1D C6D C5D 118.0(2) . . ?
C1D C6D C7D 122.9(2) . . ?
C5D C6D C7D 119.0(2) . . ?
C6D C7D C2A 112.5(2) . . ?
C11D C8D C12D 126.0(13) . . ?
C11D C8D C9D 111.9(5) . . ?
C12D C8D C9D 36.4(16) . . ?
C11D C8D C4D 113.1(3) . . ?
C12D C8D C4D 118.3(11) . . ?
C9D C8D C4D 108.2(3) . . ?
C11D C8D C13D 51.6(19) . . ?
C12D C8D C13D 120.7(18) . . ?
C9D C8D C13D 143.5(10) . . ?
C4D C8D C13D 108.2(10) . . ?
C11D C8D C10D 106.8(4) . . ?
C12D C8D C10D 72.1(16) . . ?
C9D C8D C10D 108.4(4) . . ?
C4D C8D C10D 108.3(3) . . ?
C13D C8D C10D 59(2) . . ?
C11D C8D C14D 52.1(12) . . ?
C12D C8D C14D 98.2(17) . . ?
C9D C8D C14D 66.6(14) . . ?
C4D C8D C14D 104.9(7) . . ?
C13D C8D C14D 103.5(19) . . ?
C10D C8D C14D 146.1(8) . . ?

_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_theta_full        59.93
_diffrn_measured_fraction_theta_full 0.944
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.035

data_compound_1
_database_code_depnum_ccdc_archive 'CCDC 231715'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            TBC4@130Degrees
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 O4'
_chemical_formula_weight         648.89

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           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   12.804(3)
_cell_length_b                   26.742(5)
_cell_length_c                   12.799(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.13(3)
_cell_angle_gamma                90.00
_cell_volume                     4382.5(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    403(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_type   'empirical - using SADABS'
_exptl_absorpt_correction_T_min  0.9759
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      403(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            7552
_diffrn_reflns_av_R_equivalents  0.3464
_diffrn_reflns_av_sigmaI/netI    0.5099
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         22.02
_reflns_number_total             5188
_reflns_number_gt                845
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
;

_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^)+(0.2000P)^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     SHELXL
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5188
_refine_ls_number_parameters     72
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.4833
_refine_ls_R_factor_gt           0.2373
_refine_ls_wR_factor_ref         0.6251
_refine_ls_wR_factor_gt          0.5396
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.106
_refine_ls_shift/su_mean         0.011

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
O1A O 0.7578(3) 0.22495(14) -0.1179(3) 0.084(5) Uiso 1 1 d G . .
H1A H 0.7751 0.2156 -0.0593 0.100 Uiso 1 1 calc R . .
C2A C 0.8107(3) 0.26858(16) -0.1426(3) 0.075(7) Uiso 1 1 d G . .
C3A C 0.7923(3) 0.29055(18) -0.2386(3) 0.077(7) Uiso 1 1 d G . .
C4A C 0.8476(3) 0.3336(2) -0.2653(3) 0.097(8) Uiso 1 1 d G . .
H4A H 0.8351 0.3485 -0.3298 0.116 Uiso 1 1 calc R . .
C5A C 0.9211(3) 0.3550(2) -0.1985(4) 0.094(8) Uiso 1 1 d G A .
C6A C 0.9358(3) 0.3317(2) -0.1020(4) 0.084(7) Uiso 1 1 d G . .
H6A H 0.9834 0.3457 -0.0554 0.101 Uiso 1 1 calc R . .
C7A C 0.8830(3) 0.28867(18) -0.0722(3) 0.082(7) Uiso 1 1 d G . .
C8A C 0.8998(3) 0.26773(19) 0.0376(4) 0.101(8) Uiso 1 1 d G . .
H8A1 H 0.8902 0.2318 0.0359 0.121 Uiso 1 1 calc R . .
H8A2 H 0.9712 0.2743 0.0592 0.121 Uiso 1 1 calc R . .
C9A C 0.9843(4) 0.4017(2) -0.2253(5) 0.155(12) Uiso 1 1 d G . .
C10A C 0.9565(5) 0.4231(3) -0.3322(5) 0.08(2) Uiso 0.44(3) 1 d PG A 1
H10A H 0.8832 0.4307 -0.3344 0.126 Uiso 0.44(3) 1 calc PR A 1
H10B H 0.9726 0.3989 -0.3853 0.126 Uiso 0.44(3) 1 calc PR A 1
H10C H 0.9960 0.4530 -0.3441 0.126 Uiso 0.44(3) 1 calc PR A 1
C11A C 1.0498(4) 0.3927(3) -0.3232(5) 0.22(3) Uiso 0.56(3) 1 d PG A 2
H11A H 1.0936 0.3639 -0.3126 0.329 Uiso 0.56(3) 1 calc PR A 2
H11B H 1.0926 0.4214 -0.3365 0.329 Uiso 0.56(3) 1 calc PR A 2
H11C H 1.0044 0.3869 -0.3817 0.329 Uiso 0.56(3) 1 calc PR A 2
C12A C 1.1011(4) 0.3899(3) -0.2237(5) 0.10(2) Uiso 0.44(3) 1 d PG A 1
H12A H 1.1199 0.3764 -0.1567 0.151 Uiso 0.44(3) 1 calc PR A 1
H12B H 1.1401 0.4200 -0.2361 0.151 Uiso 0.44(3) 1 calc PR A 1
H12C H 1.1167 0.3659 -0.2772 0.151 Uiso 0.44(3) 1 calc PR A 1
C13A C 1.0597(4) 0.4139(3) -0.1337(5) 0.37(6) Uiso 0.56(3) 1 d PG A 2
H13A H 1.1039 0.3856 -0.1205 0.560 Uiso 0.56(3) 1 calc PR A 2
H13B H 1.0199 0.4214 -0.0722 0.560 Uiso 0.56(3) 1 calc PR A 2
H13C H 1.1019 0.4423 -0.1518 0.560 Uiso 0.56(3) 1 calc PR A 2
C14A C 0.9629(4) 0.4428(2) -0.1425(5) 0.14(3) Uiso 0.44(3) 1 d PG A 1
H14A H 0.9800 0.4302 -0.0743 0.207 Uiso 0.44(3) 1 calc PR A 1
H14B H 0.8905 0.4520 -0.1447 0.207 Uiso 0.44(3) 1 calc PR A 1
H14C H 1.0051 0.4716 -0.1573 0.207 Uiso 0.44(3) 1 calc PR A 1
C15A C 0.9157(5) 0.4474(2) -0.2438(5) 0.17(3) Uiso 0.56(3) 1 d PG A 2
H15A H 0.8740 0.4536 -0.1829 0.248 Uiso 0.56(3) 1 calc PR A 2
H15B H 0.8708 0.4415 -0.3027 0.248 Uiso 0.56(3) 1 calc PR A 2
H15C H 0.9589 0.4760 -0.2575 0.248 Uiso 0.56(3) 1 calc PR A 2
O1B O 0.7013(3) 0.22642(14) 0.0850(3) 0.087(5) Uiso 1 1 d G . .
H1B H 0.6420 0.2182 0.1018 0.105 Uiso 1 1 calc R . .
C2B C 0.7283(3) 0.27037(16) 0.1358(3) 0.073(7) Uiso 1 1 d G . .
C3B C 0.8266(3) 0.28988(18) 0.1165(3) 0.075(7) Uiso 1 1 d G . .
C4B C 0.8545(3) 0.3335(2) 0.1698(3) 0.090(8) Uiso 1 1 d G . .
H4B H 0.9203 0.3470 0.1576 0.108 Uiso 1 1 calc R . .
C5B C 0.7890(4) 0.3579(2) 0.2400(3) 0.085(7) Uiso 1 1 d G B .
C6B C 0.6910(4) 0.3364(2) 0.2566(3) 0.096(8) Uiso 1 1 d G . .
H6B H 0.6456 0.3516 0.3035 0.115 Uiso 1 1 calc R . .
C7B C 0.6585(4) 0.29298(18) 0.2054(3) 0.078(7) Uiso 1 1 d G . .
C8B C 0.5487(4) 0.27273(19) 0.2253(3) 0.092(8) Uiso 1 1 d G . .
H8B1 H 0.5490 0.2367 0.2174 0.111 Uiso 1 1 calc R . .
H8B2 H 0.5285 0.2803 0.2965 0.111 Uiso 1 1 calc R . .
C9B C 0.8249(5) 0.4051(2) 0.2959(4) 0.119(9) Uiso 1 1 d G . .
C10B C 0.9345(5) 0.4188(3) 0.2594(5) 0.16(3) Uiso 0.51(3) 1 d PG B 3
H10D H 0.9573 0.4486 0.2945 0.236 Uiso 0.51(3) 1 calc PR B 3
H10E H 0.9337 0.4245 0.1853 0.236 Uiso 0.51(3) 1 calc PR B 3
H10F H 0.9816 0.3919 0.2752 0.236 Uiso 0.51(3) 1 calc PR B 3
C11B C 0.9237(5) 0.3939(3) 0.3584(4) 0.13(2) Uiso 0.49(3) 1 d PG B 4
H11D H 0.9465 0.4236 0.3936 0.192 Uiso 0.49(3) 1 calc PR B 4
H11E H 0.9776 0.3826 0.3119 0.192 Uiso 0.49(3) 1 calc PR B 4
H11F H 0.9094 0.3683 0.4089 0.192 Uiso 0.49(3) 1 calc PR B 4
C12B C 0.8245(5) 0.3993(3) 0.4147(4) 0.13(2) Uiso 0.51(3) 1 d PG B 3
H12D H 0.8476 0.4299 0.4465 0.199 Uiso 0.51(3) 1 calc PR B 3
H12E H 0.8707 0.3726 0.4344 0.199 Uiso 0.51(3) 1 calc PR B 3
H12F H 0.7550 0.3918 0.4378 0.199 Uiso 0.51(3) 1 calc PR B 3
C13B C 0.7413(5) 0.4262(3) 0.3687(4) 0.15(3) Uiso 0.49(3) 1 d PG B 4
H13D H 0.7673 0.4559 0.4021 0.219 Uiso 0.49(3) 1 calc PR B 4
H13E H 0.7242 0.4018 0.4208 0.219 Uiso 0.49(3) 1 calc PR B 4
H13F H 0.6800 0.4343 0.3289 0.219 Uiso 0.49(3) 1 calc PR B 4
C14B C 0.7489(5) 0.4478(2) 0.2669(4) 0.14(2) Uiso 0.51(3) 1 d PG B 3
H14D H 0.7701 0.4780 0.3014 0.216 Uiso 0.51(3) 1 calc PR B 3
H14E H 0.6795 0.4390 0.2887 0.216 Uiso 0.51(3) 1 calc PR B 3
H14F H 0.7497 0.4528 0.1927 0.216 Uiso 0.51(3) 1 calc PR B 3
C15B C 0.8494(5) 0.4451(2) 0.2124(5) 0.14(2) Uiso 0.49(3) 1 d PG B 4
H15D H 0.8723 0.4753 0.2460 0.204 Uiso 0.49(3) 1 calc PR B 4
H15E H 0.7877 0.4518 0.1721 0.204 Uiso 0.49(3) 1 calc PR B 4
H15F H 0.9036 0.4330 0.1671 0.204 Uiso 0.49(3) 1 calc PR B 4
O1C O 0.5005(3) 0.22926(14) 0.0284(3) 0.118(6) Uiso 1 1 d G . .
H1C H 0.4830 0.2203 -0.0303 0.141 Uiso 1 1 calc R . .
C2C C 0.4502(3) 0.27342(16) 0.0531(3) 0.073(6) Uiso 1 1 d G . .
C3C C 0.4694(3) 0.29518(18) 0.1505(3) 0.076(7) Uiso 1 1 d G . .
C4C C 0.4153(3) 0.3381(2) 0.1767(3) 0.087(7) Uiso 1 1 d G . .
H4C H 0.4269 0.3522 0.2420 0.104 Uiso 1 1 calc R . .
C5C C 0.3440(3) 0.3610(2) 0.1096(4) 0.106(9) Uiso 1 1 d G C .
C6C C 0.3284(3) 0.3384(2) 0.0120(4) 0.086(7) Uiso 1 1 d G . .
H6C H 0.2813 0.3529 -0.0345 0.103 Uiso 1 1 calc R . .
C7C C 0.3806(3) 0.29538(18) -0.0178(3) 0.069(6) Uiso 1 1 d G . .
C8C C 0.3606(3) 0.27305(19) -0.1251(4) 0.078(7) Uiso 1 1 d G . .
H8C1 H 0.2892 0.2801 -0.1457 0.093 Uiso 1 1 calc R . .
H8C2 H 0.3686 0.2370 -0.1212 0.093 Uiso 1 1 calc R . .
C9C C 0.2847(4) 0.4082(2) 0.1428(5) 0.136(11) Uiso 1 1 d G . .
C10C C 0.3041(5) 0.4276(3) 0.2418(5) 0.23(3) Uiso 0.67(3) 1 d PG C 5
H10G H 0.2621 0.4569 0.2523 0.344 Uiso 0.67(3) 1 calc PR C 5
H10H H 0.3766 0.4363 0.2477 0.344 Uiso 0.67(3) 1 calc PR C 5
H10I H 0.2870 0.4030 0.2936 0.344 Uiso 0.67(3) 1 calc PR C 5
C11C C 0.2230(4) 0.3957(3) 0.2468(5) 0.10(3) Uiso 0.33(3) 1 d PG C 6
H11G H 0.2709 0.3835 0.2987 0.156 Uiso 0.33(3) 1 calc PR C 6
H11H H 0.1712 0.3706 0.2327 0.156 Uiso 0.33(3) 1 calc PR C 6
H11I H 0.1895 0.4254 0.2722 0.156 Uiso 0.33(3) 1 calc PR C 6
C12C C 0.1635(4) 0.3960(3) 0.1297(5) 0.29(4) Uiso 0.67(3) 1 d PG C 5
H12G H 0.1509 0.3826 0.0612 0.434 Uiso 0.67(3) 1 calc PR C 5
H12H H 0.1236 0.4261 0.1387 0.434 Uiso 0.67(3) 1 calc PR C 5
H12I H 0.1429 0.3719 0.1813 0.434 Uiso 0.67(3) 1 calc PR C 5
C13C C 0.2094(4) 0.4269(3) 0.0640(6) 0.11(3) Uiso 0.33(3) 1 d PG C 6
H13G H 0.1755 0.4563 0.0902 0.169 Uiso 0.33(3) 1 calc PR C 6
H13H H 0.1581 0.4016 0.0500 0.169 Uiso 0.33(3) 1 calc PR C 6
H13I H 0.2459 0.4349 0.0007 0.169 Uiso 0.33(3) 1 calc PR C 6
C14C C 0.3029(5) 0.4497(2) 0.0511(5) 0.16(2) Uiso 0.67(3) 1 d PG C 5
H14G H 0.2888 0.4349 -0.0158 0.237 Uiso 0.67(3) 1 calc PR C 5
H14H H 0.3740 0.4612 0.0532 0.237 Uiso 0.67(3) 1 calc PR C 5
H14I H 0.2568 0.4775 0.0620 0.237 Uiso 0.67(3) 1 calc PR C 5
C15C C 0.3640(5) 0.4493(2) 0.1728(5) 0.16(4) Uiso 0.33(3) 1 d PG C 6
H15G H 0.4120 0.4365 0.2239 0.236 Uiso 0.33(3) 1 calc PR C 6
H15H H 0.3275 0.4775 0.2015 0.236 Uiso 0.33(3) 1 calc PR C 6
H15I H 0.4018 0.4596 0.1118 0.236 Uiso 0.33(3) 1 calc PR C 6
O1D O 0.5566(3) 0.22806(14) -0.1719(3) 0.104(5) Uiso 1 1 d G . .
H1D H 0.6144 0.2180 -0.1897 0.125 Uiso 1 1 calc R . .
C2D C 0.5328(3) 0.27124(16) -0.2257(3) 0.067(6) Uiso 1 1 d G . .
C3D C 0.4349(3) 0.29362(18) -0.2086(3) 0.061(6) Uiso 1 1 d G . .
C4D C 0.4092(3) 0.3355(2) -0.2657(3) 0.081(7) Uiso 1 1 d G . .
H4D H 0.3445 0.3504 -0.2544 0.097 Uiso 1 1 calc R . .
C5D C 0.4756(4) 0.3565(2) -0.3397(3) 0.097(8) Uiso 1 1 d G D .
C6D C 0.5722(4) 0.3338(2) -0.3528(3) 0.068(6) Uiso 1 1 d G . .
H6D H 0.6186 0.3475 -0.4007 0.081 Uiso 1 1 calc R . .
C7D C 0.6028(3) 0.29158(18) -0.2981(3) 0.062(6) Uiso 1 1 d G . .
C8D C 0.7111(4) 0.26951(19) -0.3148(3) 0.092(8) Uiso 1 1 d G . .
H8D1 H 0.7332 0.2764 -0.3858 0.111 Uiso 1 1 calc R . .
H8D2 H 0.7075 0.2335 -0.3065 0.111 Uiso 1 1 calc R . .
C9D C 0.4462(5) 0.4027(2) -0.4051(4) 0.140(11) Uiso 1 1 d G . .
C10D C 0.3374(5) 0.4221(3) -0.3798(5) 0.11(2) Uiso 0.46(4) 1 d PG D 7
H10J H 0.2870 0.3963 -0.3928 0.168 Uiso 0.46(4) 1 calc PR D 7
H10K H 0.3221 0.4506 -0.4230 0.168 Uiso 0.46(4) 1 calc PR D 7
H10L H 0.3346 0.4318 -0.3076 0.168 Uiso 0.46(4) 1 calc PR D 7
C11D C 0.3495(5) 0.3940(3) -0.4720(4) 0.42(7) Uiso 0.54(4) 1 d PG D 8
H11J H 0.3616 0.3664 -0.5184 0.634 Uiso 0.54(4) 1 calc PR D 8
H11K H 0.3347 0.4235 -0.5121 0.634 Uiso 0.54(4) 1 calc PR D 8
H11L H 0.2911 0.3866 -0.4277 0.634 Uiso 0.54(4) 1 calc PR D 8
C12D C 0.4491(5) 0.3892(3) -0.5218(4) 0.13(3) Uiso 0.46(4) 1 d PG D 7
H12J H 0.5172 0.3768 -0.5394 0.202 Uiso 0.46(4) 1 calc PR D 7
H12K H 0.4339 0.4183 -0.5627 0.202 Uiso 0.46(4) 1 calc PR D 7
H12L H 0.3978 0.3638 -0.5360 0.202 Uiso 0.46(4) 1 calc PR D 7
C13D C 0.5372(5) 0.4161(3) -0.4781(4) 0.38(6) Uiso 0.54(4) 1 d PG D 8
H13J H 0.5992 0.4217 -0.4374 0.573 Uiso 0.54(4) 1 calc PR D 8
H13K H 0.5202 0.4458 -0.5166 0.573 Uiso 0.54(4) 1 calc PR D 8
H13L H 0.5490 0.3890 -0.5259 0.573 Uiso 0.54(4) 1 calc PR D 8
C14D C 0.5252(5) 0.4443(2) -0.3840(4) 0.18(3) Uiso 0.46(4) 1 d PG D 7
H14J H 0.5942 0.4325 -0.3997 0.264 Uiso 0.46(4) 1 calc PR D 7
H14K H 0.5218 0.4539 -0.3118 0.264 Uiso 0.46(4) 1 calc PR D 7
H14L H 0.5093 0.4727 -0.4271 0.264 Uiso 0.46(4) 1 calc PR D 7
C15D C 0.4255(5) 0.4467(2) -0.3320(5) 0.25(4) Uiso 0.54(4) 1 d PG D 8
H15J H 0.4860 0.4526 -0.2893 0.380 Uiso 0.54(4) 1 calc PR D 8
H15K H 0.3669 0.4391 -0.2881 0.380 Uiso 0.54(4) 1 calc PR D 8
H15L H 0.4105 0.4761 -0.3725 0.380 Uiso 0.54(4) 1 calc PR D 8

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
O1A C2A 1.3858 . ?
C2A C3A 1.3824 . ?
C2A C7A 1.3981 . ?
C3A C4A 1.3942 . ?
C3A C8D 1.5312 . ?
C4A C5A 1.3935 . ?
C5A C6A 1.3945 . ?
C5A C9A 1.5292 . ?
C6A C7A 1.3895 . ?
C7A C8A 1.5269 . ?
C8A C3B 1.5018 . ?
C9A C15A 1.5233 . ?
C9A C10A 1.5233 . ?
C9A C11A 1.5278 . ?
C9A C12A 1.5278 . ?
C9A C14A 1.5509 . ?
C9A C13A 1.5510 . ?
O1B C2B 1.3867 . ?
C2B C3B 1.3850 . ?
C2B C7B 1.4007 . ?
C3B C4B 1.3965 . ?
C4B C5B 1.3929 . ?
C5B C6B 1.3967 . ?
C5B C9B 1.5234 . ?
C6B C7B 1.3958 . ?
C7B C8B 1.5285 . ?
C8B C3C 1.5175 . ?
C9B C10B 1.5248 . ?
C9B C11B 1.5248 . ?
C9B C12B 1.5281 . ?
C9B C13B 1.5282 . ?
C9B C15B 1.5443 . ?
C9B C14B 1.5443 . ?
O1C C2C 1.3821 . ?
C2C C3C 1.3972 . ?
C2C C7C 1.3998 . ?
C3C C4C 1.3819 . ?
C4C C5C 1.3941 . ?
C5C C6C 1.4016 . ?
C5C C9C 1.5326 . ?
C6C C7C 1.3852 . ?
C7C C8C 1.5180 . ?
C8C C3D 1.5351 . ?
C9C C10C 1.3910 . ?
C9C C13C 1.4803 . ?
C9C C15C 1.5456 . ?
C9C C11C 1.5861 . ?
C9C C12C 1.5943 . ?
C9C C14C 1.6328 . ?
O1D C2D 1.3783 . ?
C2D C7D 1.4002 . ?
C2D C3D 1.4065 . ?
C3D C4D 1.3773 . ?
C4D C5D 1.3923 . ?
C5D C6D 1.3885 . ?
C5D C9D 1.5402 . ?
C6D C7D 1.3845 . ?
C7D C8D 1.5220 . ?
C9D C11D 1.5225 . ?
C9D C10D 1.5225 . ?
C9D C15D 1.5267 . ?
C9D C14D 1.5268 . ?
C9D C13D 1.5365 . ?
C9D C12D 1.5366 . ?

_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_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
C3A C2A O1A 118.6 . . ?
C3A C2A C7A 121.4 . . ?
O1A C2A C7A 120.0 . . ?
C2A C3A C4A 118.9 . . ?
C2A C3A C8D 121.6 . . ?
C4A C3A C8D 119.5 . . ?
C5A C4A C3A 122.1 . . ?
C4A C5A C6A 116.8 . . ?
C4A C5A C9A 123.7 . . ?
C6A C5A C9A 119.5 . . ?
C7A C6A C5A 123.2 . . ?
C6A C7A C2A 117.6 . . ?
C6A C7A C8A 119.3 . . ?
C2A C7A C8A 122.9 . . ?
C3B C8A C7A 112.8 . . ?
C15A C9A C10A 55.0 . . ?
C15A C9A C11A 108.5 . . ?
C10A C9A C11A 56.7 . . ?
C15A C9A C12A 137.1 . . ?
C10A C9A C12A 108.5 . . ?
C11A C9A C12A 55.9 . . ?
C15A C9A C5A 112.6 . . ?
C10A C9A C5A 112.6 . . ?
C11A C9A C5A 110.3 . . ?
C12A C9A C5A 110.3 . . ?
C15A C9A C14A 55.6 . . ?
C10A C9A C14A 107.9 . . ?
C11A C9A C14A 140.4 . . ?
C12A C9A C14A 108.1 . . ?
C5A C9A C14A 109.3 . . ?
C15A C9A C13A 107.9 . . ?
C10A C9A C13A 138.1 . . ?
C11A C9A C13A 108.1 . . ?
C12A C9A C13A 55.0 . . ?
C5A C9A C13A 109.3 . . ?
C14A C9A C13A 56.3 . . ?
C3B C2B O1B 117.5 . . ?
C3B C2B C7B 122.1 . . ?
O1B C2B C7B 120.4 . . ?
C2B C3B C4B 117.3 . . ?
C2B C3B C8A 122.7 . . ?
C4B C3B C8A 119.9 . . ?
C5B C4B C3B 123.5 . . ?
C4B C5B C6B 116.6 . . ?
C4B C5B C9B 120.7 . . ?
C6B C5B C9B 122.7 . . ?
C7B C6B C5B 122.5 . . ?
C6B C7B C2B 117.9 . . ?
C6B C7B C8B 119.3 . . ?
C2B C7B C8B 122.8 . . ?
C3C C8B C7B 111.6 . . ?
C5B C9B C10B 109.4 . . ?
C5B C9B C11B 109.4 . . ?
C10B C9B C11B 56.3 . . ?
C5B C9B C12B 112.4 . . ?
C10B C9B C12B 109.6 . . ?
C11B C9B C12B 57.6 . . ?
C5B C9B C13B 112.4 . . ?
C10B C9B C13B 138.2 . . ?
C11B C9B C13B 109.6 . . ?
C12B C9B C13B 55.1 . . ?
C5B C9B C15B 108.1 . . ?
C10B C9B C15B 55.5 . . ?
C11B C9B C15B 109.2 . . ?
C12B C9B C15B 139.5 . . ?
C13B C9B C15B 108.1 . . ?
C5B C9B C14B 108.1 . . ?
C10B C9B C14B 109.2 . . ?
C11B C9B C14B 142.5 . . ?
C12B C9B C14B 108.1 . . ?
C13B C9B C14B 55.4 . . ?
C15B C9B C14B 56.8 . . ?
O1C C2C C3C 118.6 . . ?
O1C C2C C7C 120.5 . . ?
C3C C2C C7C 121.0 . . ?
C4C C3C C2C 118.3 . . ?
C4C C3C C8B 120.7 . . ?
C2C C3C C8B 121.0 . . ?
C3C C4C C5C 123.0 . . ?
C4C C5C C6C 116.8 . . ?
C4C C5C C9C 121.1 . . ?
C6C C5C C9C 122.1 . . ?
C7C C6C C5C 122.4 . . ?
C6C C7C C2C 118.5 . . ?
C6C C7C C8C 119.7 . . ?
C2C C7C C8C 121.8 . . ?
C7C C8C C3D 112.7 . . ?
C10C C9C C13C 127.5 . . ?
C10C C9C C5C 118.1 . . ?
C13C C9C C5C 114.3 . . ?
C10C C9C C15C 52.5 . . ?
C13C C9C C15C 110.8 . . ?
C5C C9C C15C 109.2 . . ?
C10C C9C C11C 53.3 . . ?
C13C C9C C11C 108.6 . . ?
C5C C9C C11C 107.9 . . ?
C15C C9C C11C 105.6 . . ?
C10C C9C C12C 110.1 . . ?
C13C C9C C12C 50.6 . . ?
C5C C9C C12C 106.6 . . ?
C15C C9C C12C 144.2 . . ?
C11C C9C C12C 63.8 . . ?
C10C C9C C14C 112.0 . . ?
C13C C9C C14C 51.3 . . ?
C5C C9C C14C 106.8 . . ?
C15C C9C C14C 66.4 . . ?
C11C C9C C14C 145.0 . . ?
C12C C9C C14C 101.8 . . ?
O1D C2D C7D 121.0 . . ?
O1D C2D C3D 118.3 . . ?
C7D C2D C3D 120.6 . . ?
C4D C3D C2D 118.4 . . ?
C4D C3D C8C 120.9 . . ?
C2D C3D C8C 120.7 . . ?
C3D C4D C5D 122.8 . . ?
C6D C5D C4D 116.9 . . ?
C6D C5D C9D 120.1 . . ?
C4D C5D C9D 123.0 . . ?
C7D C6D C5D 123.1 . . ?
C6D C7D C2D 118.1 . . ?
C6D C7D C8D 120.1 . . ?
C2D C7D C8D 121.8 . . ?
C7D C8D C3A 112.7 . . ?
C11D C9D C10D 55.1 . . ?
C11D C9D C15D 108.7 . . ?
C10D C9D C15D 56.4 . . ?
C11D C9D C14D 138.5 . . ?
C10D C9D C14D 108.7 . . ?
C15D C9D C14D 56.4 . . ?
C11D C9D C13D 108.1 . . ?
C10D C9D C13D 138.2 . . ?
C15D C9D C13D 109.1 . . ?
C14D C9D C13D 55.7 . . ?
C11D C9D C12D 55.8 . . ?
C10D C9D C12D 108.1 . . ?
C15D C9D C12D 141.5 . . ?
C14D C9D C12D 109.1 . . ?
C13D C9D C12D 56.3 . . ?
C11D C9D C5D 112.4 . . ?
C10D C9D C5D 112.4 . . ?
C15D C9D C5D 109.1 . . ?
C14D C9D C5D 109.1 . . ?
C13D C9D C5D 109.4 . . ?
C12D C9D C5D 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        22.02
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.127