# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2001

data_global

_journal_coden_Cambridge      0440

_publ_contact_author  'Takehiko Yamato'
_publ_contact_author_email; yamatot@cc.saga-u.ac.jp
_publ_contact_author_fax; + 81(0)952/28-8591
_publ_contact_author_phone; + 81(0)952/28-8679
_publ_contact_author_address
; 
Department of Applied Chemistry, 
Faculty of Science and Engineering, 
Saga University, Honjo-machi 1, 
Saga-shi, Saga 840-8502, 
Japan
;

_publ_section_title         Cif-file

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


_audit_creation_date               05-10-00
_audit_creation_method         from_MolEN_master_file_using_cif_in
_audit_update_record
; ?
;

# 1. SUBMISSION DETAILS

_publ_contact_author     'Prof. Takehiko Yamato'

_publ_contact_author_phone        '+81-952-28-8679'
_publ_contact_author_fax           '+81-952-28-8591'
_publ_contact_author_email        yamatot@cc.saga-u.ac.jp

_publ_requested_journal           'New Journal of Chemistry'
_publ_requested_coeditor_name     ? 

_publ_contact_letter
;
?
;

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

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic     ? 

_journal_date_to_coeditor         ? 
_journal_date_from_coeditor       ? 
_journal_date_accepted            ? 

_journal_date_printers_first      ? 
_journal_date_printers_final      ? 
_journal_date_proofs_out          ? 
_journal_date_proofs_in           ? 

_journal_coeditor_name            ? 
_journal_coeditor_code            ? 
_journal_coeditor_notes
; ?
;

_journal_techeditor_code          ? 
_journal_techeditor_notes
; ?
;

_journal_coden_ASTM               ? 
_journal_name_full                ? 
_journal_year                     ? 
_journal_volume                   ? 
_journal_issue                    ? 
_journal_page_first               ? 
_journal_page_last                ? 

_journal_suppl_publ_number        ? 
_journal_suppl_publ_pages         ? 

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


# 3. TITLE AND AUTHOR LIST

_publ_section_title
;
Medium-sized cyclophanes. Part 56
5-tert-Butyl-8-substituted [2.2]metaparacyclophane-1,9-dienes. 
Preparation, X-ray diffraction studies, and their treatment 
with Lewis acid and protic acid
;
loop_
_publ_author_name
_publ_author_address
' Yamato, Takehiko '
;
Department of Applied Chemistry, 
Faculty of Science and Engineering, 
Saga University, Honjo-
machi 1, Saga-shi, Saga 840-8505, Japan 
;
' Noda Kozo '
;
Department of Applied Chemistry, 
Faculty of Science and Engineering, 
Saga University, Honjo-
machi 1, Saga-shi, Saga 840-8505, 
Japan 
;
' Tsuzuki, Hirohisa'
;
Center of Environmental Analysis, 
Tohwa Institute for Science, Tohwa University, 
1-1-1, Chikushigaoka, Minami-ku, Fukuoka-shi, 
Fukuoka 815-8510, Japan 
;
#===================================================================

# 4. TEXT

_publ_section_abstract
;
? 
;
_publ_section_comment
;
? 
;

_publ_section_exptl_prep ?
_publ_section_exptl_refinement
;
SIR92 and SHELXL-93 were used for structure solution and refinement, 
respectively.  All H atoms were located at ideal positions (SHELXL-93) and were 
included in refinement, but restrained to ride on the atom to which they are 
bonded.  Isotropic thermal factors of H atoms were held fixed to 1.3 times 
U~eq~ of the riding atoms.  
;

_publ_section_references
;
Altomare, M. C., Burla, M., Camalli, G., Cascarano, C., Giacovazzo, 
A., Guagliardi, G. & Polidori, J. (1994). SIR92. J. Appl. Cryst. 27, 
435.

Hall, S. R. & du Boulay, D. (1995). Xtal_GX. University of 
Western Australia, Austaralia. 

Sheldrick, G. M. (1993). SHELXL-93. University of G\"ottingen, 
Germany.
;

_publ_section_figure_captions
;
? 
;

_publ_section_acknowledgements
;
The authors are grateful to authors of SIR92, SHELXL-93, and Xtal_GX 
for their permission to use their programs.  Acknowledgements are 
also due to Dr. H. Uekusa and Prof. Y. Ohashi, Tokyo Institute of 
Technology, for their kind instructions on using these programs. 
;

#===================================================================
data_5-tert-butyl-8-cyanometaparacyclophane-1,9-diene

_database_code_CSD	156030

#===================================================================
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
5-tert-butyl-8-cyanometaparacyclophane-1,9-diene
; 
_chemical_name_common         5-tert-butyl-8-cyanometaparacyclophane-1,9-diene 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C21 H19 N1' 
_chemical_formula_weight          285.39

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'    .0181    .0091 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'    .0000    .0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'    .0311    .0180 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    p212121 

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

_cell_length_a                    15.684(2) 
_cell_length_b                    18.7370(10) 
_cell_length_c                    11.044(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3245.5(10) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       21 
_cell_measurement_theta_max       43 

_exptl_crystal_description        prism 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.168 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1216 
_exptl_absorpt_coefficient_mu     0.511 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.7842 
_exptl_absorpt_correction_T_max   0.9047 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       296(2) 
_diffrn_radiation_wavelength      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   FR590 
_diffrn_measurement_method \q/2\q
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   120 
_diffrn_standards_decay_%         -0.01 
_diffrn_reflns_number             11604 
_diffrn_reflns_av_R_equivalents   0.0635 
_diffrn_reflns_av_sigmaI/netI     0.0633 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.68 
_diffrn_reflns_theta_max          65.01 
_reflns_number_total              5512 
_reflns_number_gt                 4573 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'CAD4 Enraf-Nonius software' 
_computing_cell_refinement        'CAD4 Enraf-Nonius software'  
_computing_data_reduction         'MolEN  Enraf-Nonius software'
_computing_structure_solution     
;SIR97 (Altomare, Burla, Camalli, Cascarano, Giacovazzo,
Guagliardi & Polidori, 1997) 
;
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Xtal_GX (Hall & Boulay, 1995)' 
_computing_publication_material   'SHELXL-97 (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^)+(0.0677P)^2^+0.2803P] 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     riding 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0074(5) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    1.3(8) 
_refine_ls_number_reflns          5512 
_refine_ls_number_parameters      398 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0594 
_refine_ls_R_factor_gt            0.0436 
_refine_ls_wR_factor_ref          0.1287 
_refine_ls_wR_factor_gt           0.1170 
_refine_ls_goodness_of_fit_ref    1.044 
_refine_ls_restrained_S_all       1.044 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full                .50 
_diffrn_measured_fraction_theta_full    .000 
_refine_diff_density_max     .284 
_refine_diff_density_min    -.228 
_refine_diff_density_rms     .038

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 
C01 C 0.46830(18) 0.56838(18) 0.8071(2) 0.0702(7) Uani 1 1 d . . . 
H01 H 0.4557 0.5716 0.8892 0.091 Uiso 1 1 calc R . . 
C02 C 0.44039(16) 0.61776(16) 0.7305(2) 0.0639(7) Uani 1 1 d . . . 
H02 H 0.4121 0.6574 0.7616 0.083 Uiso 1 1 calc R . . 
C03 C 0.45253(14) 0.61243(13) 0.5957(2) 0.0498(5) Uani 1 1 d . . . 
C04 C 0.38298(14) 0.60624(14) 0.5201(2) 0.0586(6) Uani 1 1 d . . . 
H04 H 0.3289 0.6147 0.5515 0.076 Uiso 1 1 calc R . . 
C05 C 0.39078(14) 0.58771(13) 0.3977(2) 0.0564(6) Uani 1 1 d . . . 
C06 C 0.47066(15) 0.56748(13) 0.3580(2) 0.0522(5) Uani 1 1 d . . . 
H06 H 0.4760 0.5500 0.2796 0.068 Uiso 1 1 calc R . . 
C07 C 0.54283(13) 0.57191(12) 0.42882(19) 0.0450(5) Uani 1 1 d . . . 
C08 C 0.53393(12) 0.60400(11) 0.54400(19) 0.0424(5) Uani 1 1 d . . . 
C09 C 0.62370(14) 0.53652(14) 0.3920(2) 0.0514(6) Uani 1 1 d . . . 
H09 H 0.6497 0.5512 0.3205 0.067 Uiso 1 1 calc R . . 
C10 C 0.66048(15) 0.48518(15) 0.4556(2) 0.0583(6) Uani 1 1 d . . . 
H10 H 0.7094 0.4627 0.4271 0.076 Uiso 1 1 calc R . . 
C11 C 0.62233(15) 0.46413(13) 0.5732(2) 0.0537(6) Uani 1 1 d . . . 
C12 C 0.53760(16) 0.44280(13) 0.5766(2) 0.0580(6) Uani 1 1 d . . . 
H12 H 0.5160 0.4135 0.5159 0.075 Uiso 1 1 calc R . . 
C13 C 0.48566(17) 0.46479(14) 0.6691(2) 0.0615(6) Uani 1 1 d . . . 
H13 H 0.4288 0.4509 0.6713 0.080 Uiso 1 1 calc R . . 
C14 C 0.51934(18) 0.50861(15) 0.7607(2) 0.0609(7) Uani 1 1 d . . . 
C15 C 0.60701(19) 0.50916(17) 0.7750(2) 0.0672(7) Uani 1 1 d . . . 
H15 H 0.6309 0.5245 0.8476 0.087 Uiso 1 1 calc R . . 
C16 C 0.65915(17) 0.48683(16) 0.6813(2) 0.0639(7) Uani 1 1 d . . . 
H16 H 0.7181 0.4870 0.6904 0.083 Uiso 1 1 calc R . . 
C17 C 0.31240(17) 0.58485(17) 0.3143(3) 0.0761(9) Uani 1 1 d . . . 
C18 C 0.3383(3) 0.5975(3) 0.1817(4) 0.144(2) Uani 1 1 d . . . 
H18A H 0.3631 0.6441 0.1739 0.187 Uiso 1 1 calc R . . 
H18B H 0.2888 0.5943 0.1309 0.187 Uiso 1 1 calc R . . 
H18C H 0.3791 0.5621 0.1576 0.187 Uiso 1 1 calc R . . 
C19 C 0.2752(4) 0.5141(3) 0.3234(9) 0.268(6) Uani 1 1 d . . . 
H19A H 0.2261 0.5112 0.2718 0.349 Uiso 1 1 calc R . . 
H19B H 0.2586 0.5052 0.4057 0.349 Uiso 1 1 calc R . . 
H19C H 0.3164 0.4791 0.2988 0.349 Uiso 1 1 calc R . . 
C20 C 0.2502(3) 0.6428(3) 0.3433(4) 0.143(2) Uani 1 1 d . . . 
H20A H 0.2776 0.6884 0.3354 0.187 Uiso 1 1 calc R . . 
H20B H 0.2300 0.6370 0.4247 0.187 Uiso 1 1 calc R . . 
H20C H 0.2029 0.6403 0.2882 0.187 Uiso 1 1 calc R . . 
C21 C 0.60715(15) 0.63225(13) 0.6040(2) 0.0514(5) Uani 1 1 d . . . 
C31 C 0.55704(16) 0.76308(15) -0.0820(2) 0.0594(6) Uani 1 1 d . . . 
H31 H 0.5393 0.7676 -0.1620 0.077 Uiso 1 1 calc R . . 
C32 C 0.50211(14) 0.74214(15) 0.0033(2) 0.0558(6) Uani 1 1 d . . . 
H32 H 0.4475 0.7282 -0.0194 0.073 Uiso 1 1 calc R . . 
C33 C 0.52591(12) 0.74054(13) 0.1349(2) 0.0467(5) Uani 1 1 d . . . 
C34 C 0.48736(13) 0.78648(14) 0.2153(2) 0.0540(6) Uani 1 1 d . . . 
H34 H 0.4389 0.8112 0.1908 0.070 Uiso 1 1 calc R . . 
C35 C 0.51815(14) 0.79730(13) 0.3318(2) 0.0527(6) Uani 1 1 d . . . 
C36 C 0.59561(15) 0.76547(13) 0.3622(2) 0.0524(5) Uani 1 1 d . . . 
H36 H 0.6201 0.7759 0.4368 0.068 Uiso 1 1 calc R . . 
C37 C 0.63739(13) 0.71885(12) 0.28488(19) 0.0455(5) Uani 1 1 d . . . 
C38 C 0.59567(12) 0.70012(12) 0.17595(19) 0.0421(5) Uani 1 1 d . . . 
C39 C 0.72729(14) 0.69830(14) 0.3096(2) 0.0551(6) Uani 1 1 d . . . 
H39 H 0.7396 0.6723 0.3792 0.072 Uiso 1 1 calc R . . 
C40 C 0.79098(14) 0.71602(14) 0.2352(3) 0.0586(6) Uani 1 1 d . . . 
H40 H 0.8471 0.7051 0.2552 0.076 Uiso 1 1 calc R . . 
C41 C 0.77089(12) 0.75324(13) 0.1206(2) 0.0514(6) Uani 1 1 d . . . 
C42 C 0.72534(13) 0.81762(12) 0.1245(2) 0.0518(6) Uani 1 1 d . . . 
H42 H 0.7377 0.8516 0.1833 0.067 Uiso 1 1 calc R . . 
C43 C 0.66249(14) 0.83003(13) 0.0408(2) 0.0538(6) Uani 1 1 d . . . 
H43 H 0.6312 0.8722 0.0433 0.070 Uiso 1 1 calc R . . 
C44 C 0.64585(15) 0.77888(14) -0.0483(2) 0.0538(6) Uani 1 1 d . . . 
C45 C 0.70855(15) 0.72855(15) -0.0724(2) 0.0586(6) Uani 1 1 d . . . 
H45 H 0.7083 0.7036 -0.1452 0.076 Uiso 1 1 calc R . . 
C46 C 0.77130(14) 0.71583(15) 0.0126(2) 0.0581(6) Uani 1 1 d . . . 
H46 H 0.8136 0.6823 -0.0027 0.075 Uiso 1 1 calc R . . 
C47 C 0.47380(18) 0.84900(15) 0.4203(3) 0.0681(7) Uani 1 1 d . . . 
C48 C 0.3824(3) 0.8594(4) 0.3907(5) 0.190(3) Uani 1 1 d . . . 
H48A H 0.3772 0.8768 0.3093 0.247 Uiso 1 1 calc R . . 
H48B H 0.3580 0.8935 0.4457 0.247 Uiso 1 1 calc R . . 
H48C H 0.3528 0.8148 0.3981 0.247 Uiso 1 1 calc R . . 
C49 C 0.4819(4) 0.8222(2) 0.5491(3) 0.141(2) Uani 1 1 d . . . 
H49A H 0.5410 0.8161 0.5687 0.183 Uiso 1 1 calc R . . 
H49B H 0.4529 0.7773 0.5567 0.183 Uiso 1 1 calc R . . 
H49C H 0.4569 0.8562 0.6035 0.183 Uiso 1 1 calc R . . 
C50 C 0.5193(3) 0.9197(2) 0.4159(4) 0.1242(17) Uani 1 1 d . . . 
H50A H 0.5784 0.9128 0.4352 0.161 Uiso 1 1 calc R . . 
H50B H 0.4941 0.9517 0.4736 0.161 Uiso 1 1 calc R . . 
H50C H 0.5144 0.9396 0.3361 0.161 Uiso 1 1 calc R . . 
C51 C 0.62194(13) 0.63804(13) 0.11065(19) 0.0455(5) Uani 1 1 d . . . 
N01 N 0.66365(15) 0.66290(15) 0.6437(2) 0.0752(7) Uani 1 1 d . . . 
N02 N 0.63669(14) 0.58402(12) 0.06558(19) 0.0616(5) 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 
C01 0.0785(17) 0.090(2) 0.0420(13) -0.0055(14) 0.0183(13) -0.0011(16) 
C02 0.0618(14) 0.0767(19) 0.0533(15) -0.0163(13) 0.0138(12) 0.0085(13) 
C03 0.0518(11) 0.0470(12) 0.0507(13) -0.0041(10) 0.0017(10) 0.0055(10) 
C04 0.0445(11) 0.0611(15) 0.0702(16) -0.0009(13) 0.0001(11) 0.0096(11) 
C05 0.0524(12) 0.0498(13) 0.0669(15) -0.0005(12) -0.0158(12) 0.0053(10) 
C06 0.0598(13) 0.0531(13) 0.0437(12) -0.0033(11) -0.0089(10) 0.0079(11) 
C07 0.0495(11) 0.0449(11) 0.0407(11) 0.0060(9) -0.0011(9) 0.0025(9) 
C08 0.0452(10) 0.0401(11) 0.0419(11) 0.0000(9) -0.0019(9) 0.0011(9) 
C09 0.0501(12) 0.0636(15) 0.0405(12) 0.0002(10) 0.0061(9) 0.0042(10) 
C10 0.0496(12) 0.0735(17) 0.0519(13) -0.0066(13) 0.0043(11) 0.0153(11) 
C11 0.0578(13) 0.0483(13) 0.0551(14) 0.0077(11) -0.0010(11) 0.0138(10) 
C12 0.0700(15) 0.0416(12) 0.0624(15) 0.0037(11) 0.0008(12) -0.0030(11) 
C13 0.0693(15) 0.0537(14) 0.0614(16) 0.0114(12) 0.0127(13) -0.0097(11) 
C14 0.0784(17) 0.0628(16) 0.0414(13) 0.0134(11) 0.0101(12) -0.0001(13) 
C15 0.0793(17) 0.0803(19) 0.0421(13) 0.0108(13) -0.0081(12) 0.0059(15) 
C16 0.0594(14) 0.0754(18) 0.0569(15) 0.0109(14) -0.0099(12) 0.0156(12) 
C17 0.0637(15) 0.0703(19) 0.094(2) 0.0071(17) -0.0354(16) 0.0042(13) 
C18 0.114(3) 0.224(6) 0.093(3) -0.007(4) -0.054(2) 0.032(3) 
C19 0.225(7) 0.135(5) 0.445(13) 0.137(6) -0.259(8) -0.104(4) 
C20 0.112(3) 0.194(5) 0.125(4) -0.018(4) -0.054(3) 0.086(3) 
C21 0.0542(12) 0.0523(13) 0.0476(12) -0.0029(11) 0.0018(10) -0.0030(10) 
C31 0.0690(14) 0.0658(16) 0.0436(13) 0.0072(12) -0.0158(11) 0.0044(12) 
C32 0.0450(11) 0.0662(16) 0.0564(14) -0.0071(12) -0.0180(10) 0.0061(11) 
C33 0.0356(9) 0.0543(13) 0.0504(12) -0.0019(10) -0.0034(9) -0.0028(9) 
C34 0.0377(10) 0.0630(15) 0.0612(15) -0.0058(12) 0.0053(10) 0.0007(10) 
C35 0.0505(11) 0.0526(13) 0.0551(14) -0.0057(11) 0.0157(11) -0.0060(10) 
C36 0.0624(13) 0.0571(14) 0.0376(11) -0.0053(10) 0.0029(10) -0.0060(11) 
C37 0.0478(11) 0.0512(13) 0.0377(11) 0.0022(9) -0.0028(9) -0.0037(9) 
C38 0.0400(10) 0.0479(12) 0.0384(11) 0.0006(9) 0.0005(9) -0.0035(8) 
C39 0.0548(12) 0.0618(15) 0.0487(13) 0.0023(11) -0.0195(11) 0.0034(11) 
C40 0.0403(11) 0.0628(16) 0.0729(16) -0.0012(13) -0.0179(11) 0.0022(10) 
C41 0.0355(9) 0.0557(14) 0.0631(14) -0.0006(12) 0.0006(10) -0.0066(9) 
C42 0.0468(11) 0.0480(13) 0.0604(14) -0.0001(11) -0.0039(10) -0.0100(9) 
C43 0.0566(12) 0.0481(13) 0.0568(14) 0.0107(11) 0.0003(11) -0.0009(10) 
C44 0.0641(13) 0.0575(14) 0.0397(11) 0.0114(10) -0.0011(11) -0.0044(11) 
C45 0.0653(14) 0.0648(16) 0.0458(12) 0.0019(12) 0.0135(11) -0.0092(12) 
C46 0.0464(11) 0.0612(15) 0.0666(16) 0.0020(13) 0.0146(11) 0.0006(11) 
C47 0.0749(16) 0.0616(16) 0.0680(16) -0.0102(14) 0.0318(14) -0.0032(13) 
C48 0.085(3) 0.291(8) 0.195(5) -0.149(6) 0.024(3) 0.044(4) 
C49 0.249(6) 0.091(3) 0.082(3) 0.001(2) 0.087(3) 0.029(3) 
C50 0.175(4) 0.064(2) 0.134(3) -0.021(2) 0.078(3) -0.015(2) 
C51 0.0464(11) 0.0520(14) 0.0381(10) 0.0048(10) -0.0030(9) -0.0009(9) 
N01 0.0723(14) 0.0920(18) 0.0612(13) -0.0113(13) -0.0045(11) -0.0252(13) 
N02 0.0781(14) 0.0536(12) 0.0530(12) -0.0061(10) -0.0011(10) 0.0005(10) 

_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 
C01 C02 1.328(4) . ? 
C01 C14 1.469(4) . ? 
C02 C03 1.505(4) . ? 
C03 C04 1.378(3) . ? 
C03 C08 1.407(3) . ? 
C04 C05 1.401(4) . ? 
C05 C06 1.380(3) . ? 
C05 C17 1.537(3) . ? 
C06 C07 1.378(3) . ? 
C07 C08 1.414(3) . ? 
C07 C09 1.488(3) . ? 
C08 C21 1.428(3) . ? 
C09 C10 1.324(3) . ? 
C10 C11 1.484(3) . ? 
C11 C12 1.388(4) . ? 
C11 C16 1.392(4) . ? 
C12 C13 1.370(4) . ? 
C13 C14 1.406(4) . ? 
C14 C15 1.384(4) . ? 
C15 C16 1.384(4) . ? 
C17 C19 1.451(5) . ? 
C17 C20 1.495(5) . ? 
C17 C18 1.538(6) . ? 
C21 N01 1.143(3) . ? 
C31 C32 1.336(4) . ? 
C31 C44 1.472(3) . ? 
C32 C33 1.501(3) . ? 
C33 C34 1.377(3) . ? 
C33 C38 1.406(3) . ? 
C34 C35 1.388(3) . ? 
C35 C36 1.394(3) . ? 
C35 C47 1.542(3) . ? 
C36 C37 1.386(3) . ? 
C37 C38 1.414(3) . ? 
C37 C39 1.487(3) . ? 
C38 C51 1.429(3) . ? 
C39 C40 1.336(4) . ? 
C40 C41 1.479(4) . ? 
C41 C46 1.384(4) . ? 
C41 C42 1.403(3) . ? 
C42 C43 1.371(3) . ? 
C43 C44 1.398(4) . ? 
C44 C45 1.388(4) . ? 
C45 C46 1.381(4) . ? 
C47 C48 1.483(5) . ? 
C47 C50 1.505(5) . ? 
C47 C49 1.514(5) . ? 
C51 N02 1.152(3) . ? 

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 
C02 C01 C14 119.3(2) . . ? 
C01 C02 C03 122.8(2) . . ? 
C04 C03 C08 117.6(2) . . ? 
C04 C03 C02 120.3(2) . . ? 
C08 C03 C02 121.6(2) . . ? 
C03 C04 C05 122.4(2) . . ? 
C06 C05 C04 117.0(2) . . ? 
C06 C05 C17 121.7(2) . . ? 
C04 C05 C17 121.1(2) . . ? 
C07 C06 C05 123.3(2) . . ? 
C06 C07 C08 117.05(19) . . ? 
C06 C07 C09 121.2(2) . . ? 
C08 C07 C09 121.33(19) . . ? 
C03 C08 C07 120.14(19) . . ? 
C03 C08 C21 120.0(2) . . ? 
C07 C08 C21 119.74(19) . . ? 
C10 C09 C07 123.4(2) . . ? 
C09 C10 C11 118.8(2) . . ? 
C12 C11 C16 117.5(2) . . ? 
C12 C11 C10 119.1(2) . . ? 
C16 C11 C10 120.1(2) . . ? 
C13 C12 C11 120.2(3) . . ? 
C12 C13 C14 119.3(2) . . ? 
C15 C14 C13 117.4(3) . . ? 
C15 C14 C01 119.7(3) . . ? 
C13 C14 C01 119.4(2) . . ? 
C16 C15 C14 119.9(3) . . ? 
C15 C16 C11 119.2(2) . . ? 
C19 C17 C20 112.7(5) . . ? 
C19 C17 C05 108.2(3) . . ? 
C20 C17 C05 111.6(3) . . ? 
C19 C17 C18 108.2(5) . . ? 
C20 C17 C18 105.3(4) . . ? 
C05 C17 C18 110.7(3) . . ? 
N01 C21 C08 171.0(3) . . ? 
C32 C31 C44 119.4(2) . . ? 
C31 C32 C33 121.9(2) . . ? 
C34 C33 C38 118.1(2) . . ? 
C34 C33 C32 120.2(2) . . ? 
C38 C33 C32 121.1(2) . . ? 
C33 C34 C35 122.4(2) . . ? 
C34 C35 C36 117.6(2) . . ? 
C34 C35 C47 121.5(2) . . ? 
C36 C35 C47 120.6(2) . . ? 
C37 C36 C35 122.2(2) . . ? 
C36 C37 C38 117.5(2) . . ? 
C36 C37 C39 119.9(2) . . ? 
C38 C37 C39 122.1(2) . . ? 
C33 C38 C37 120.1(2) . . ? 
C33 C38 C51 120.01(19) . . ? 
C37 C38 C51 119.86(19) . . ? 
C40 C39 C37 122.1(2) . . ? 
C39 C40 C41 118.99(19) . . ? 
C46 C41 C42 117.6(2) . . ? 
C46 C41 C40 119.9(2) . . ? 
C42 C41 C40 119.2(2) . . ? 
C43 C42 C41 119.4(2) . . ? 
C42 C43 C44 119.5(2) . . ? 
C45 C44 C43 117.9(2) . . ? 
C45 C44 C31 119.0(2) . . ? 
C43 C44 C31 119.5(2) . . ? 
C46 C45 C44 119.5(2) . . ? 
C45 C46 C41 119.7(2) . . ? 
C48 C47 C50 109.6(4) . . ? 
C48 C47 C49 109.4(4) . . ? 
C50 C47 C49 106.4(4) . . ? 
C48 C47 C35 112.3(3) . . ? 
C50 C47 C35 108.6(2) . . ? 
C49 C47 C35 110.5(3) . . ? 
N02 C51 C38 172.5(2) . . ? 

loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
C14 C01 C02 C03 5.1(4) . . . . ? 
C01 C02 C03 C04 115.7(3) . . . . ? 
C01 C02 C03 C08 -55.7(4) . . . . ? 
C08 C03 C04 C05 4.1(4) . . . . ? 
C02 C03 C04 C05 -167.6(3) . . . . ? 
C03 C04 C05 C06 7.4(4) . . . . ? 
C03 C04 C05 C17 -177.0(2) . . . . ? 
C04 C05 C06 C07 -6.9(4) . . . . ? 
C17 C05 C06 C07 177.5(2) . . . . ? 
C05 C06 C07 C08 -5.0(4) . . . . ? 
C05 C06 C07 C09 167.7(2) . . . . ? 
C04 C03 C08 C07 -16.5(3) . . . . ? 
C02 C03 C08 C07 155.1(2) . . . . ? 
C04 C03 C08 C21 159.2(2) . . . . ? 
C02 C03 C08 C21 -29.2(4) . . . . ? 
C06 C07 C08 C03 17.0(3) . . . . ? 
C09 C07 C08 C03 -155.7(2) . . . . ? 
C06 C07 C08 C21 -158.8(2) . . . . ? 
C09 C07 C08 C21 28.6(3) . . . . ? 
C06 C07 C09 C10 -117.5(3) . . . . ? 
C08 C07 C09 C10 54.8(3) . . . . ? 
C07 C09 C10 C11 -3.5(4) . . . . ? 
C09 C10 C11 C12 56.0(3) . . . . ? 
C09 C10 C11 C16 -103.1(3) . . . . ? 
C16 C11 C12 C13 20.8(3) . . . . ? 
C10 C11 C12 C13 -138.8(3) . . . . ? 
C11 C12 C13 C14 -0.5(4) . . . . ? 
C12 C13 C14 C15 -20.0(4) . . . . ? 
C12 C13 C14 C01 139.0(3) . . . . ? 
C02 C01 C14 C15 101.6(3) . . . . ? 
C02 C01 C14 C13 -56.9(4) . . . . ? 
C13 C14 C15 C16 20.2(4) . . . . ? 
C01 C14 C15 C16 -138.8(3) . . . . ? 
C14 C15 C16 C11 0.1(4) . . . . ? 
C12 C11 C16 C15 -20.6(4) . . . . ? 
C10 C11 C16 C15 138.8(3) . . . . ? 
C06 C05 C17 C19 88.0(6) . . . . ? 
C04 C05 C17 C19 -87.4(6) . . . . ? 
C06 C05 C17 C20 -147.4(4) . . . . ? 
C04 C05 C17 C20 37.2(4) . . . . ? 
C06 C05 C17 C18 -30.4(4) . . . . ? 
C04 C05 C17 C18 154.1(3) . . . . ? 
C03 C08 C21 N01 -89.0(17) . . . . ? 
C07 C08 C21 N01 86.7(17) . . . . ? 
C44 C31 C32 C33 5.7(4) . . . . ? 
C31 C32 C33 C34 113.2(3) . . . . ? 
C31 C32 C33 C38 -57.6(4) . . . . ? 
C38 C33 C34 C35 4.1(3) . . . . ? 
C32 C33 C34 C35 -167.0(2) . . . . ? 
C33 C34 C35 C36 6.5(4) . . . . ? 
C33 C34 C35 C47 -179.9(2) . . . . ? 
C34 C35 C36 C37 -6.3(3) . . . . ? 
C47 C35 C36 C37 -179.9(2) . . . . ? 
C35 C36 C37 C38 -4.5(3) . . . . ? 
C35 C36 C37 C39 167.3(2) . . . . ? 
C34 C33 C38 C37 -15.3(3) . . . . ? 
C32 C33 C38 C37 155.7(2) . . . . ? 
C34 C33 C38 C51 161.7(2) . . . . ? 
C32 C33 C38 C51 -27.3(3) . . . . ? 
C36 C37 C38 C33 15.4(3) . . . . ? 
C39 C37 C38 C33 -156.2(2) . . . . ? 
C36 C37 C38 C51 -161.6(2) . . . . ? 
C39 C37 C38 C51 26.8(3) . . . . ? 
C36 C37 C39 C40 -115.1(3) . . . . ? 
C38 C37 C39 C40 56.3(3) . . . . ? 
C37 C39 C40 C41 -4.0(4) . . . . ? 
C39 C40 C41 C46 -102.7(3) . . . . ? 
C39 C40 C41 C42 56.4(3) . . . . ? 
C46 C41 C42 C43 21.0(3) . . . . ? 
C40 C41 C42 C43 -138.6(2) . . . . ? 
C41 C42 C43 C44 -1.1(3) . . . . ? 
C42 C43 C44 C45 -19.3(3) . . . . ? 
C42 C43 C44 C31 139.3(2) . . . . ? 
C32 C31 C44 C45 101.7(3) . . . . ? 
C32 C31 C44 C43 -56.7(3) . . . . ? 
C43 C44 C45 C46 19.9(3) . . . . ? 
C31 C44 C45 C46 -138.8(2) . . . . ? 
C44 C45 C46 C41 0.1(4) . . . . ? 
C42 C41 C46 C45 -20.5(3) . . . . ? 
C40 C41 C46 C45 139.0(2) . . . . ? 
C34 C35 C47 C48 24.4(5) . . . . ? 
C36 C35 C47 C48 -162.2(4) . . . . ? 
C34 C35 C47 C50 -96.9(4) . . . . ? 
C36 C35 C47 C50 76.5(4) . . . . ? 
C34 C35 C47 C49 146.8(3) . . . . ? 
C36 C35 C47 C49 -39.9(4) . . . . ? 
C33 C38 C51 N02 -87.3(18) . . . . ? 
C37 C38 C51 N02 89.7(18) . . . . ?