Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_02bckm 
_database_code_CSD            163266

_journal_coden_Cambridge 182 
_journal_volume           ?
_journal_year             ? 
_journal_page_first       ?

_publ_requested_journal       'Chemical Communications'


loop_
_publ_author_name  
'Chi-Keung Lam'
'Thomas C. W. Mak'

_publ_contact_author_name     	'Prof Thomas C W Mak'  
_publ_contact_author_address 
;
Prof Thomas C W Mak
The Chinese University of Hong Kong
Department of Chemistry
Shatin
New Territories
Hong Kong
SAR, 
P R CHINA
;

_publ_contact_author_email       'TCWMAK@CUHK.EDU.HK'

_publ_section_title
;
Rhodizonate and croconate dianions as divergent hydrogen-bond
acceptors in the self-assembly of supramolecular structures
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             
'bis(tetra-n-butyl)ammonium rhodizonate-phenylurea (1/4)'
_chemical_melting_point           ? 
_chemical_formula_moiety          '[(n-C4H9)4N]2C6O6.4C6H5NHCONH2 '
_chemical_formula_sum 
'C66 H104 N10 O10' 
_chemical_formula_weight          1197.59 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 

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

_cell_length_a                    8.9555(6) 
_cell_length_b                    13.1902(9) 
_cell_length_c                    31.649(2) 
_cell_angle_alpha                 85.813(2) 
_cell_angle_beta                  82.838(2) 
_cell_angle_gamma                 73.879(2) 
_cell_volume                      3560.6(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        Block 
_exptl_crystal_colour             'deep orange red' 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.117 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1300 
_exptl_absorpt_coefficient_mu     0.076 
_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   'Bruker Smart CCD 1000' 
_diffrn_measurement_method        'omega scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             16078 
_diffrn_reflns_av_R_equivalents   0.0373 
_diffrn_reflns_av_sigmaI/netI     0.0665 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -34 
_diffrn_reflns_limit_l_max        34 
_diffrn_reflns_theta_min          1.61 
_diffrn_reflns_theta_max          22.54 
_reflns_number_total              9336 
_reflns_number_gt                 3855 
_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^)+(0.0969P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          9336 
_refine_ls_number_parameters      775 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1396 
_refine_ls_R_factor_gt            0.0588 
_refine_ls_wR_factor_ref          0.1865 
_refine_ls_wR_factor_gt           0.1548 
_refine_ls_goodness_of_fit_ref    0.867 
_refine_ls_restrained_S_all       0.867 
_refine_ls_shift/su_max           0.024 
_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 
O1 O 0.2438(4) 0.8829(2) 0.19142(10) 0.1382(12) Uani 1 1 d . . . 
O2 O 0.4418(3) 0.6994(2) 0.16325(9) 0.1059(9) Uani 1 1 d . . . 
O3 O 0.6266(4) 0.5726(2) 0.21693(9) 0.1267(10) Uani 1 1 d . . . 
O4 O 0.6540(4) 0.6420(2) 0.29214(11) 0.1511(13) Uani 1 1 d . . . 
O5 O 0.4739(3) 0.8285(2) 0.31905(9) 0.1090(9) Uani 1 1 d . . . 
O6 O 0.2605(4) 0.9475(2) 0.26980(8) 0.1318(11) Uani 1 1 d . . . 
C1 C 0.3394(5) 0.8280(3) 0.21445(14) 0.0886(12) Uani 1 1 d . . . 
C2 C 0.4430(5) 0.7286(3) 0.19979(14) 0.0813(11) Uani 1 1 d . . . 
C3 C 0.5460(5) 0.6621(3) 0.22836(14) 0.0941(13) Uani 1 1 d . . . 
C4 C 0.5570(5) 0.6978(3) 0.26885(14) 0.0937(12) Uani 1 1 d . . . 
C5 C 0.4617(5) 0.7973(3) 0.28335(14) 0.0828(11) Uani 1 1 d . . . 
C6 C 0.3491(5) 0.8622(3) 0.25656(13) 0.0893(12) Uani 1 1 d . . . 
N1 N 0.7224(4) 0.0129(3) 0.35684(12) 0.1117(11) Uani 1 1 d . . . 
C7 C 0.6173(5) 0.0321(4) 0.32051(16) 0.1237(15) Uani 1 1 d . . . 
H7C H 0.6036 -0.0352 0.3139 0.148 Uiso 1 1 calc R . . 
H7D H 0.5151 0.0764 0.3308 0.148 Uiso 1 1 calc R . . 
C8 C 0.6747(6) 0.0825(5) 0.27999(18) 0.166(2) Uani 1 1 d . . . 
H8B H 0.7792 0.0417 0.2698 0.199 Uiso 1 1 calc R . . 
H8C H 0.6783 0.1534 0.2851 0.199 Uiso 1 1 calc R . . 
C9 C 0.5619(9) 0.0865(6) 0.2467(2) 0.203(3) Uani 1 1 d . . . 
H9C H 0.5391 0.0186 0.2480 0.244 Uiso 1 1 calc R . . 
H9D H 0.4647 0.1387 0.2552 0.244 Uiso 1 1 calc R . . 
C10 C 0.6056(10) 0.1084(8) 0.2066(3) 0.286(5) Uani 1 1 d . . . 
H10B H 0.5263 0.1053 0.1893 0.428 Uiso 1 1 calc R . . 
H10C H 0.7018 0.0577 0.1972 0.428 Uiso 1 1 calc R . . 
H10D H 0.6206 0.1779 0.2039 0.428 Uiso 1 1 calc R . . 
C11 C 0.8830(5) -0.0582(5) 0.34329(16) 0.1354(17) Uani 1 1 d . . . 
H11A H 0.9308 -0.0232 0.3195 0.163 Uiso 1 1 calc R . . 
H11B H 0.9463 -0.0656 0.3666 0.163 Uiso 1 1 calc R . . 
C12 C 0.8896(7) -0.1671(5) 0.33037(19) 0.174(2) Uani 1 1 d . . . 
H12A H 0.8330 -0.2010 0.3526 0.209 Uiso 1 1 calc R . . 
H12B H 0.8401 -0.1620 0.3044 0.209 Uiso 1 1 calc R . . 
C13 C 1.0558(9) -0.2318(7) 0.3232(3) 0.255(4) Uani 1 1 d . . . 
H13A H 1.1117 -0.1922 0.3033 0.305 Uiso 1 1 calc R . . 
H13B H 1.1003 -0.2382 0.3500 0.305 Uiso 1 1 calc R . . 
C14 C 1.0839(11) -0.3227(7) 0.3097(3) 0.292(5) Uani 1 1 d . . . 
H14A H 1.1947 -0.3546 0.3067 0.437 Uiso 1 1 calc R . . 
H14B H 1.0451 -0.3185 0.2825 0.437 Uiso 1 1 calc R . . 
H14C H 1.0334 -0.3647 0.3294 0.437 Uiso 1 1 calc R . . 
C15 C 0.7431(6) 0.1170(4) 0.36981(15) 0.1273(16) Uani 1 1 d . . . 
H15A H 0.8158 0.1013 0.3912 0.153 Uiso 1 1 calc R . . 
H15B H 0.7907 0.1491 0.3451 0.153 Uiso 1 1 calc R . . 
C16 C 0.5949(7) 0.1980(4) 0.38738(17) 0.1477(18) Uani 1 1 d . . . 
H16A H 0.5162 0.2085 0.3678 0.177 Uiso 1 1 calc R . . 
H16B H 0.5542 0.1712 0.4144 0.177 Uiso 1 1 calc R . . 
C17 C 0.6251(8) 0.2994(5) 0.3934(2) 0.188(3) Uani 1 1 d . . . 
H17A H 0.6631 0.3262 0.3660 0.225 Uiso 1 1 calc R . . 
H17B H 0.7077 0.2872 0.4118 0.225 Uiso 1 1 calc R . . 
C18 C 0.4894(9) 0.3814(5) 0.4118(2) 0.233(4) Uani 1 1 d . . . 
H18A H 0.5191 0.4453 0.4139 0.349 Uiso 1 1 calc R . . 
H18B H 0.4539 0.3577 0.4397 0.349 Uiso 1 1 calc R . . 
H18C H 0.4066 0.3947 0.3939 0.349 Uiso 1 1 calc R . . 
C19 C 0.6417(5) -0.0391(3) 0.39323(15) 0.1118(14) Uani 1 1 d . . . 
H19A H 0.5391 0.0081 0.4011 0.134 Uiso 1 1 calc R . . 
H19B H 0.6262 -0.1028 0.3831 0.134 Uiso 1 1 calc R . . 
C20 C 0.7235(6) -0.0678(4) 0.43205(16) 0.1410(17) Uani 1 1 d . . . 
H20A H 0.7297 -0.0042 0.4445 0.169 Uiso 1 1 calc R . . 
H20B H 0.8292 -0.1109 0.4246 0.169 Uiso 1 1 calc R . . 
C21 C 0.6377(7) -0.1278(5) 0.46411(19) 0.162(2) Uani 1 1 d . . . 
H21A H 0.5360 -0.0813 0.4734 0.194 Uiso 1 1 calc R . . 
H21B H 0.6203 -0.1859 0.4500 0.194 Uiso 1 1 calc R . . 
C22 C 0.7152(8) -0.1693(6) 0.5008(2) 0.223(3) Uani 1 1 d . . . 
H22A H 0.6531 -0.2066 0.5192 0.334 Uiso 1 1 calc R . . 
H22B H 0.7297 -0.1124 0.5156 0.334 Uiso 1 1 calc R . . 
H22C H 0.8152 -0.2169 0.4921 0.334 Uiso 1 1 calc R . . 
N2 N 0.7712(4) 0.5248(3) 0.85654(11) 0.1023(10) Uani 1 1 d . . . 
C23 C 0.6866(5) 0.4762(3) 0.89306(13) 0.1034(13) Uani 1 1 d . . . 
H23A H 0.5818 0.5224 0.8988 0.124 Uiso 1 1 calc R . . 
H23B H 0.6768 0.4096 0.8843 0.124 Uiso 1 1 calc R . . 
C24 C 0.7622(7) 0.4564(4) 0.93356(17) 0.1516(19) Uani 1 1 d . . . 
H24A H 0.7651 0.5231 0.9439 0.182 Uiso 1 1 calc R . . 
H24B H 0.8691 0.4133 0.9279 0.182 Uiso 1 1 calc R . . 
C25 C 0.6712(8) 0.3986(5) 0.9689(2) 0.181(3) Uani 1 1 d . . . 
H25A H 0.6989 0.4072 0.9968 0.217 Uiso 1 1 calc R . . 
H25B H 0.5594 0.4285 0.9687 0.217 Uiso 1 1 calc R . . 
C26 C 0.7120(9) 0.2935(6) 0.9600(2) 0.237(3) Uani 1 1 d . . . 
H26A H 0.6548 0.2570 0.9805 0.356 Uiso 1 1 calc R . . 
H26B H 0.8221 0.2639 0.9615 0.356 Uiso 1 1 calc R . . 
H26C H 0.6877 0.2860 0.9319 0.356 Uiso 1 1 calc R . . 
C27 C 0.7943(5) 0.6289(4) 0.86825(14) 0.1176(15) Uani 1 1 d . . . 
H27A H 0.8672 0.6139 0.8896 0.141 Uiso 1 1 calc R . . 
H27B H 0.8429 0.6590 0.8432 0.141 Uiso 1 1 calc R . . 
C28 C 0.6480(6) 0.7122(4) 0.88516(16) 0.1325(16) Uani 1 1 d . . . 
H28A H 0.5664 0.7193 0.8668 0.159 Uiso 1 1 calc R . . 
H28B H 0.6107 0.6903 0.9135 0.159 Uiso 1 1 calc R . . 
C29 C 0.6836(6) 0.8172(4) 0.88677(17) 0.1526(19) Uani 1 1 d . . . 
H29A H 0.7704 0.8076 0.9035 0.183 Uiso 1 1 calc R . . 
H29B H 0.7170 0.8391 0.8581 0.183 Uiso 1 1 calc R . . 
C30 C 0.5532(7) 0.9022(4) 0.9047(2) 0.202(3) Uani 1 1 d . . . 
H30A H 0.5848 0.9663 0.9035 0.304 Uiso 1 1 calc R . . 
H30B H 0.5232 0.8837 0.9338 0.304 Uiso 1 1 calc R . . 
H30C H 0.4660 0.9125 0.8885 0.304 Uiso 1 1 calc R . . 
C31 C 0.6717(5) 0.5414(3) 0.81932(14) 0.1100(13) Uani 1 1 d . . . 
H31A H 0.6569 0.4737 0.8137 0.132 Uiso 1 1 calc R . . 
H31B H 0.5694 0.5874 0.8285 0.132 Uiso 1 1 calc R . . 
C32 C 0.7321(6) 0.5870(4) 0.77814(16) 0.1439(18) Uani 1 1 d . . . 
H32A H 0.8373 0.5451 0.7691 0.173 Uiso 1 1 calc R . . 
H32B H 0.7361 0.6585 0.7821 0.173 Uiso 1 1 calc R . . 
C33 C 0.6255(8) 0.5880(5) 0.74422(19) 0.181(2) Uani 1 1 d . . . 
H33A H 0.6163 0.5168 0.7426 0.217 Uiso 1 1 calc R . . 
H33B H 0.5222 0.6324 0.7535 0.217 Uiso 1 1 calc R . . 
C34 C 0.6725(9) 0.6236(6) 0.7028(2) 0.247(4) Uani 1 1 d . . . 
H34A H 0.5978 0.6209 0.6840 0.370 Uiso 1 1 calc R . . 
H34B H 0.7733 0.5791 0.6928 0.370 Uiso 1 1 calc R . . 
H34C H 0.6785 0.6949 0.7036 0.370 Uiso 1 1 calc R . . 
C35 C 0.9315(5) 0.4540(4) 0.84436(15) 0.1212(15) Uani 1 1 d . . . 
H35A H 0.9906 0.4446 0.8687 0.145 Uiso 1 1 calc R . . 
H35B H 0.9834 0.4898 0.8217 0.145 Uiso 1 1 calc R . . 
C36 C 0.9385(6) 0.3461(4) 0.82970(17) 0.1494(19) Uani 1 1 d . . . 
H36A H 0.8927 0.3530 0.8031 0.179 Uiso 1 1 calc R . . 
H36B H 0.8800 0.3108 0.8508 0.179 Uiso 1 1 calc R . . 
C37 C 1.1081(8) 0.2825(6) 0.8236(3) 0.234(4) Uani 1 1 d . . . 
H37A H 1.1662 0.3244 0.8056 0.281 Uiso 1 1 calc R . . 
H37B H 1.1480 0.2720 0.8512 0.281 Uiso 1 1 calc R . . 
C38 C 1.1376(9) 0.1909(7) 0.8071(3) 0.251(4) Uani 1 1 d . . . 
H38A H 1.2477 0.1570 0.8059 0.376 Uiso 1 1 calc R . . 
H38B H 1.1062 0.1999 0.7789 0.376 Uiso 1 1 calc R . . 
H38C H 1.0809 0.1481 0.8244 0.376 Uiso 1 1 calc R . . 
O7 O 0.8680(3) 0.4354(2) 0.07967(9) 0.1094(9) Uani 1 1 d . . . 
N3 N 0.7238(3) 0.4462(2) 0.14350(10) 0.0924(9) Uani 1 1 d . . . 
H3A H 0.7655 0.3811 0.1505 0.111 Uiso 1 1 calc R . . 
H3B H 0.6533 0.4852 0.1609 0.111 Uiso 1 1 calc R . . 
N4 N 0.6920(3) 0.5912(3) 0.09849(10) 0.0847(9) Uani 1 1 d . . . 
H4A H 0.6143 0.6178 0.1169 0.102 Uiso 1 1 calc R . . 
C39 C 0.7690(5) 0.4870(3) 0.10534(14) 0.0810(11) Uani 1 1 d . . . 
C40 C 0.8290(5) 0.6279(3) 0.02869(14) 0.0947(12) Uani 1 1 d . . . 
H40A H 0.8782 0.5566 0.0252 0.114 Uiso 1 1 calc R . . 
C41 C 0.8591(5) 0.7018(5) -0.00209(14) 0.1114(14) Uani 1 1 d . . . 
H41A H 0.9302 0.6794 -0.0258 0.134 Uiso 1 1 calc R . . 
C42 C 0.7867(7) 0.8064(5) 0.00157(16) 0.1345(18) Uani 1 1 d . . . 
H42A H 0.8083 0.8556 -0.0192 0.161 Uiso 1 1 calc R . . 
C43 C 0.6813(7) 0.8376(4) 0.03655(19) 0.1444(19) Uani 1 1 d . . . 
H43A H 0.6295 0.9089 0.0392 0.173 Uiso 1 1 calc R . . 
C44 C 0.6504(5) 0.7653(4) 0.06800(15) 0.1171(15) Uani 1 1 d . . . 
H44A H 0.5783 0.7881 0.0915 0.140 Uiso 1 1 calc R . . 
C45 C 0.7265(4) 0.6598(3) 0.06452(13) 0.0809(10) Uani 1 1 d . . . 
O8 O 0.9798(3) 0.2823(2) 0.30299(8) 0.1058(9) Uani 1 1 d . . . 
N5 N 0.8396(4) 0.3963(2) 0.25735(10) 0.1109(11) Uani 1 1 d . . . 
H5A H 0.8610 0.3501 0.2381 0.133 Uiso 1 1 calc R . . 
H5B H 0.7814 0.4589 0.2524 0.133 Uiso 1 1 calc R . . 
N6 N 0.8554(4) 0.4512(2) 0.32186(10) 0.1014(10) Uani 1 1 d . . . 
H6A H 0.7975 0.5097 0.3122 0.122 Uiso 1 1 calc R . . 
C46 C 0.8965(5) 0.3709(3) 0.29488(13) 0.0851(11) Uani 1 1 d . . . 
C47 C 0.8200(8) 0.5418(4) 0.38427(16) 0.167(2) Uani 1 1 d . . . 
H47A H 0.7497 0.5973 0.3713 0.200 Uiso 1 1 calc R . . 
C48 C 0.8514(13) 0.5483(6) 0.4257(2) 0.258(5) Uani 1 1 d . . . 
H48A H 0.7999 0.6080 0.4410 0.310 Uiso 1 1 calc R . . 
C49 C 0.9574(14) 0.4678(8) 0.4441(2) 0.272(5) Uani 1 1 d . . . 
H49A H 0.9800 0.4739 0.4715 0.326 Uiso 1 1 calc R . . 
C50 C 1.0301(9) 0.3791(5) 0.4228(2) 0.185(3) Uani 1 1 d . . . 
H50A H 1.1008 0.3234 0.4356 0.222 Uiso 1 1 calc R . . 
C51 C 0.9978(6) 0.3733(4) 0.38274(16) 0.1294(16) Uani 1 1 d . . . 
H51A H 1.0484 0.3127 0.3679 0.155 Uiso 1 1 calc R . . 
C52 C 0.8937(6) 0.4527(4) 0.36306(14) 0.1007(13) Uani 1 1 d . . . 
O9 O 0.0896(4) 1.0915(2) 0.41112(8) 0.1186(10) Uani 1 1 d . . . 
N7 N 0.1961(3) 1.0838(2) 0.34281(11) 0.0973(10) Uani 1 1 d . . . 
H7A H 0.1509 1.1491 0.3371 0.117 Uiso 1 1 calc R . . 
H7B H 0.2562 1.0454 0.3233 0.117 Uiso 1 1 calc R . . 
N8 N 0.2533(3) 0.9379(3) 0.38666(10) 0.0849(9) Uani 1 1 d . . . 
H8A H 0.3144 0.9116 0.3647 0.102 Uiso 1 1 calc R . . 
C53 C 0.1727(5) 1.0416(3) 0.38238(15) 0.0812(11) Uani 1 1 d . . . 
C54 C 0.3358(6) 0.7652(4) 0.41764(15) 0.1237(15) Uani 1 1 d . . . 
H54A H 0.3938 0.7443 0.3917 0.148 Uiso 1 1 calc R . . 
C55 C 0.3371(8) 0.6917(4) 0.4513(2) 0.170(2) Uani 1 1 d . . . 
H55A H 0.3964 0.6221 0.4480 0.205 Uiso 1 1 calc R . . 
C56 C 0.2502(9) 0.7223(5) 0.48953(19) 0.167(2) Uani 1 1 d . . . 
H56A H 0.2493 0.6729 0.5120 0.200 Uiso 1 1 calc R . . 
C57 C 0.1668(6) 0.8231(5) 0.49444(17) 0.1396(18) Uani 1 1 d . . . 
H57A H 0.1087 0.8431 0.5204 0.168 Uiso 1 1 calc R . . 
C58 C 0.1662(5) 0.8973(4) 0.46138(16) 0.1094(13) Uani 1 1 d . . . 
H58A H 0.1092 0.9671 0.4655 0.131 Uiso 1 1 calc R . . 
C59 C 0.2494(4) 0.8693(3) 0.42203(14) 0.0843(11) Uani 1 1 d . . . 
O10 O -0.0872(3) 1.2479(2) 0.18904(8) 0.1076(9) Uani 1 1 d . . . 
N9 N 0.0680(4) 1.1338(2) 0.23223(11) 0.1174(12) Uani 1 1 d . . . 
H9A H 0.0553 1.1808 0.2508 0.141 Uiso 1 1 calc R . . 
H9B H 0.1262 1.0709 0.2366 0.141 Uiso 1 1 calc R . . 
N10 N 0.0301(4) 1.0785(2) 0.16876(10) 0.0994(10) Uani 1 1 d . . . 
H10A H 0.0918 1.0199 0.1769 0.119 Uiso 1 1 calc R . . 
C60 C -0.0031(5) 1.1587(3) 0.19637(14) 0.0912(11) Uani 1 1 d . . . 
C61 C -0.1131(6) 1.1650(3) 0.10848(15) 0.1256(16) Uani 1 1 d . . . 
H61A H -0.1428 1.2299 0.1213 0.151 Uiso 1 1 calc R . . 
C62 C -0.1606(6) 1.1575(4) 0.06951(15) 0.1252(15) Uani 1 1 d . . . 
H62A H -0.2226 1.2171 0.0564 0.150 Uiso 1 1 calc R . . 
C63 C -0.1187(7) 1.0658(5) 0.05017(16) 0.1328(17) Uani 1 1 d . . . 
H63A H -0.1520 1.0610 0.0239 0.159 Uiso 1 1 calc R . . 
C64 C -0.0280(8) 0.9807(4) 0.06913(18) 0.160(2) Uani 1 1 d . . . 
H64A H 0.0016 0.9167 0.0557 0.192 Uiso 1 1 calc R . . 
C65 C 0.0236(6) 0.9859(3) 0.10896(15) 0.1289(17) Uani 1 1 d . . . 
H65A H 0.0884 0.9267 0.1215 0.155 Uiso 1 1 calc R . . 
C66 C -0.0233(5) 1.0792(3) 0.12862(13) 0.0860(11) 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 
O1 0.151(3) 0.095(2) 0.144(3) -0.0225(19) -0.049(2) 0.026(2) 
O2 0.102(2) 0.102(2) 0.109(2) -0.0324(17) -0.0009(17) -0.0169(16) 
O3 0.156(3) 0.0797(19) 0.122(2) -0.0211(17) -0.0192(19) 0.0115(19) 
O4 0.183(3) 0.103(2) 0.137(3) -0.013(2) -0.049(3) 0.028(2) 
O5 0.116(2) 0.103(2) 0.097(2) -0.0244(17) 0.0012(17) -0.0128(16) 
O6 0.159(3) 0.0872(19) 0.116(2) -0.0269(17) -0.019(2) 0.0292(19) 
C1 0.092(3) 0.060(3) 0.097(3) -0.006(2) -0.005(3) 0.005(2) 
C2 0.079(3) 0.064(3) 0.095(3) -0.007(2) 0.008(3) -0.017(2) 
C3 0.099(3) 0.062(3) 0.108(4) -0.015(3) 0.014(3) -0.008(2) 
C4 0.100(3) 0.070(3) 0.094(3) -0.002(3) 0.002(3) -0.002(3) 
C5 0.083(3) 0.064(3) 0.090(3) -0.014(2) 0.012(3) -0.009(2) 
C6 0.096(3) 0.059(2) 0.095(3) -0.014(2) 0.010(3) 0.002(2) 
N1 0.081(3) 0.131(3) 0.127(3) 0.009(3) -0.017(2) -0.036(2) 
C7 0.099(3) 0.149(4) 0.129(4) 0.003(3) -0.034(3) -0.036(3) 
C8 0.128(4) 0.236(6) 0.133(5) 0.031(4) -0.037(4) -0.046(4) 
C9 0.212(8) 0.258(8) 0.141(5) 0.012(6) -0.053(6) -0.056(6) 
C10 0.224(9) 0.447(15) 0.183(7) -0.032(9) -0.019(7) -0.084(9) 
C11 0.077(4) 0.169(5) 0.152(4) -0.005(4) -0.015(3) -0.020(4) 
C12 0.124(5) 0.186(6) 0.189(6) -0.038(5) 0.013(4) -0.009(5) 
C13 0.169(7) 0.226(9) 0.360(11) -0.136(8) 0.096(7) -0.062(7) 
C14 0.257(10) 0.242(10) 0.377(13) -0.095(9) 0.086(9) -0.101(9) 
C15 0.127(4) 0.134(4) 0.147(4) 0.009(3) -0.038(3) -0.072(4) 
C16 0.142(5) 0.133(4) 0.180(5) 0.006(4) -0.034(4) -0.053(4) 
C17 0.242(8) 0.144(5) 0.209(6) -0.013(5) -0.030(6) -0.102(6) 
C18 0.290(10) 0.134(5) 0.275(9) -0.045(6) -0.008(7) -0.058(6) 
C19 0.086(3) 0.126(4) 0.127(4) 0.011(3) -0.008(3) -0.040(3) 
C20 0.125(4) 0.180(5) 0.126(4) 0.036(4) -0.026(4) -0.061(4) 
C21 0.151(5) 0.179(5) 0.155(5) 0.040(4) -0.024(4) -0.052(4) 
C22 0.193(7) 0.274(8) 0.206(7) 0.090(6) -0.056(6) -0.084(6) 
N2 0.076(2) 0.119(3) 0.120(3) -0.002(2) -0.012(2) -0.039(2) 
C23 0.086(3) 0.128(3) 0.107(3) 0.003(3) -0.015(3) -0.047(3) 
C24 0.169(5) 0.184(5) 0.128(4) 0.024(4) -0.045(4) -0.086(4) 
C25 0.205(6) 0.132(5) 0.206(7) -0.020(5) -0.047(5) -0.033(5) 
C26 0.273(9) 0.224(8) 0.239(8) 0.052(7) -0.100(7) -0.091(7) 
C27 0.095(4) 0.120(4) 0.155(4) -0.006(3) -0.029(3) -0.053(3) 
C28 0.111(4) 0.131(4) 0.164(4) -0.010(3) -0.024(3) -0.042(4) 
C29 0.151(5) 0.128(4) 0.193(5) -0.028(4) -0.014(4) -0.057(4) 
C30 0.161(6) 0.149(5) 0.291(8) -0.079(5) -0.001(5) -0.023(4) 
C31 0.090(3) 0.139(4) 0.115(3) -0.004(3) -0.020(3) -0.049(3) 
C32 0.120(4) 0.190(5) 0.125(4) 0.027(4) -0.017(4) -0.054(4) 
C33 0.202(6) 0.224(7) 0.128(5) 0.047(5) -0.044(5) -0.082(5) 
C34 0.271(9) 0.283(9) 0.181(7) 0.039(6) -0.048(7) -0.069(7) 
C35 0.079(3) 0.128(4) 0.156(4) -0.010(3) -0.010(3) -0.028(3) 
C36 0.112(4) 0.146(5) 0.175(5) -0.029(4) 0.011(4) -0.016(4) 
C37 0.164(7) 0.171(6) 0.367(11) -0.137(7) 0.089(6) -0.064(6) 
C38 0.209(8) 0.253(9) 0.294(10) -0.038(8) 0.057(7) -0.100(7) 
O7 0.106(2) 0.0942(19) 0.109(2) -0.0242(16) 0.0063(17) 0.0012(17) 
N3 0.086(2) 0.084(2) 0.100(2) -0.0115(19) -0.0020(19) -0.0121(17) 
N4 0.072(2) 0.078(2) 0.096(2) -0.0166(19) 0.0018(18) -0.0089(19) 
C39 0.069(3) 0.082(3) 0.092(3) -0.024(3) -0.010(2) -0.015(2) 
C40 0.096(3) 0.096(3) 0.092(3) -0.020(3) -0.007(3) -0.023(3) 
C41 0.122(4) 0.120(4) 0.095(3) -0.016(3) -0.004(3) -0.039(3) 
C42 0.176(5) 0.118(5) 0.116(4) -0.020(3) 0.015(4) -0.061(4) 
C43 0.200(6) 0.085(3) 0.138(4) -0.007(4) 0.011(4) -0.033(4) 
C44 0.143(4) 0.086(3) 0.111(4) -0.016(3) 0.016(3) -0.022(3) 
C45 0.077(3) 0.077(3) 0.091(3) -0.024(3) -0.010(2) -0.020(2) 
O8 0.137(2) 0.0719(17) 0.0937(19) -0.0088(15) -0.0340(17) 0.0059(17) 
N5 0.140(3) 0.080(2) 0.098(3) -0.0159(19) -0.046(2) 0.012(2) 
N6 0.137(3) 0.075(2) 0.083(2) -0.0111(19) -0.023(2) -0.007(2) 
C46 0.099(3) 0.068(3) 0.084(3) -0.010(2) -0.016(2) -0.011(2) 
C47 0.296(8) 0.102(4) 0.098(4) -0.023(3) -0.024(4) -0.041(4) 
C48 0.487(16) 0.148(6) 0.125(6) -0.046(5) -0.065(7) -0.038(8) 
C49 0.525(18) 0.192(8) 0.115(6) -0.029(6) -0.116(8) -0.083(10) 
C50 0.298(9) 0.161(6) 0.118(5) 0.000(4) -0.069(5) -0.081(6) 
C51 0.168(5) 0.132(4) 0.093(4) -0.016(3) -0.046(3) -0.031(4) 
C52 0.142(4) 0.080(3) 0.082(3) -0.009(3) -0.010(3) -0.033(3) 
O9 0.138(3) 0.102(2) 0.094(2) -0.0311(17) -0.0089(18) 0.0079(18) 
N7 0.102(2) 0.087(2) 0.093(2) -0.0173(19) 0.000(2) -0.0093(18) 
N8 0.085(2) 0.089(2) 0.077(2) -0.017(2) -0.0047(18) -0.0144(19) 
C53 0.072(3) 0.080(3) 0.091(3) -0.027(3) -0.022(2) -0.010(2) 
C54 0.155(4) 0.096(3) 0.104(4) -0.010(3) -0.005(3) -0.008(3) 
C55 0.245(7) 0.101(4) 0.134(5) 0.003(4) 0.001(5) -0.007(4) 
C56 0.235(7) 0.131(5) 0.113(5) 0.005(4) -0.002(4) -0.023(5) 
C57 0.160(5) 0.137(5) 0.103(4) -0.012(4) -0.002(3) -0.012(4) 
C58 0.107(3) 0.117(4) 0.095(3) -0.008(3) -0.015(3) -0.013(3) 
C59 0.077(3) 0.090(3) 0.086(3) -0.023(3) -0.016(2) -0.013(2) 
O10 0.147(3) 0.0687(17) 0.0941(19) -0.0112(15) -0.0375(17) 0.0038(17) 
N9 0.146(3) 0.082(2) 0.107(3) -0.0185(19) -0.045(2) 0.015(2) 
N10 0.123(3) 0.063(2) 0.105(3) -0.0131(19) -0.021(2) -0.0079(18) 
C60 0.106(3) 0.072(3) 0.091(3) -0.007(3) -0.018(3) -0.013(3) 
C61 0.176(5) 0.086(3) 0.109(4) -0.017(3) -0.052(3) -0.006(3) 
C62 0.160(5) 0.119(4) 0.099(4) -0.006(3) -0.035(3) -0.034(3) 
C63 0.184(5) 0.123(4) 0.099(4) -0.015(4) -0.019(4) -0.048(4) 
C64 0.263(7) 0.100(4) 0.114(5) -0.030(3) -0.028(5) -0.033(4) 
C65 0.200(5) 0.083(3) 0.098(3) -0.017(3) -0.017(3) -0.025(3) 
C66 0.109(3) 0.076(3) 0.078(3) -0.014(2) -0.003(2) -0.034(2) 

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

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
O1 C1 1.234(4) . ? 
O2 C2 1.247(4) . ? 
O3 C3 1.252(4) . ? 
O4 C4 1.251(4) . ? 
O5 C5 1.258(4) . ? 
O6 C6 1.250(4) . ? 
C1 C2 1.449(5) . ? 
C1 C6 1.458(5) . ? 
C2 C3 1.443(5) . ? 
C3 C4 1.421(5) . ? 
C4 C5 1.424(5) . ? 
C5 C6 1.447(5) . ? 
N1 C19 1.507(5) . ? 
N1 C11 1.512(5) . ? 
N1 C15 1.526(5) . ? 
N1 C7 1.539(5) . ? 
C7 C8 1.501(6) . ? 
C8 C9 1.537(7) . ? 
C9 C10 1.316(8) . ? 
C11 C12 1.505(6) . ? 
C12 C13 1.494(8) . ? 
C13 C14 1.251(8) . ? 
C15 C16 1.526(6) . ? 
C16 C17 1.466(6) . ? 
C17 C18 1.474(7) . ? 
C19 C20 1.480(5) . ? 
C20 C21 1.508(6) . ? 
C21 C22 1.423(7) . ? 
N2 C35 1.500(5) . ? 
N2 C23 1.504(4) . ? 
N2 C27 1.523(5) . ? 
N2 C31 1.532(5) . ? 
C23 C24 1.496(5) . ? 
C24 C25 1.577(7) . ? 
C25 C26 1.373(7) . ? 
C27 C28 1.523(5) . ? 
C28 C29 1.511(6) . ? 
C29 C30 1.464(6) . ? 
C31 C32 1.498(5) . ? 
C32 C33 1.521(7) . ? 
C33 C34 1.413(7) . ? 
C35 C36 1.511(5) . ? 
C36 C37 1.514(7) . ? 
C37 C38 1.297(7) . ? 
O7 C39 1.214(4) . ? 
N3 C39 1.348(4) . ? 
N4 C39 1.372(4) . ? 
N4 C45 1.414(4) . ? 
C40 C45 1.379(5) . ? 
C40 C41 1.383(5) . ? 
C41 C42 1.359(5) . ? 
C42 C43 1.370(5) . ? 
C43 C44 1.384(5) . ? 
C44 C45 1.375(5) . ? 
O8 C46 1.228(4) . ? 
N5 C46 1.335(4) . ? 
N6 C46 1.351(4) . ? 
N6 C52 1.392(5) . ? 
C47 C52 1.357(5) . ? 
C47 C48 1.388(8) . ? 
C48 C49 1.362(10) . ? 
C49 C50 1.352(9) . ? 
C50 C51 1.348(6) . ? 
C51 C52 1.365(6) . ? 
O9 C53 1.209(4) . ? 
N7 C53 1.349(4) . ? 
N8 C53 1.363(4) . ? 
N8 C59 1.391(4) . ? 
C54 C59 1.384(5) . ? 
C54 C55 1.385(6) . ? 
C55 C56 1.377(6) . ? 
C56 C57 1.341(6) . ? 
C57 C58 1.379(6) . ? 
C58 C59 1.388(5) . ? 
O10 C60 1.232(4) . ? 
N9 C60 1.346(4) . ? 
N10 C60 1.366(4) . ? 
N10 C66 1.411(4) . ? 
C61 C66 1.361(5) . ? 
C61 C62 1.373(5) . ? 
C62 C63 1.333(5) . ? 
C63 C64 1.341(6) . ? 
C64 C65 1.408(6) . ? 
C65 C66 1.355(5) . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
O1 C1 C2 120.1(4) . . ? 
O1 C1 C6 120.5(4) . . ? 
C2 C1 C6 119.4(4) . . ? 
O2 C2 C3 120.0(4) . . ? 
O2 C2 C1 120.8(4) . . ? 
C3 C2 C1 119.2(4) . . ? 
O3 C3 C4 120.4(4) . . ? 
O3 C3 C2 119.2(4) . . ? 
C4 C3 C2 120.5(4) . . ? 
O4 C4 C3 119.7(4) . . ? 
O4 C4 C5 118.9(4) . . ? 
C3 C4 C5 121.4(4) . . ? 
O5 C5 C4 120.8(4) . . ? 
O5 C5 C6 120.1(3) . . ? 
C4 C5 C6 119.1(4) . . ? 
O6 C6 C5 119.5(4) . . ? 
O6 C6 C1 120.4(4) . . ? 
C5 C6 C1 120.1(4) . . ? 
C19 N1 C11 110.2(4) . . ? 
C19 N1 C15 111.1(3) . . ? 
C11 N1 C15 107.8(4) . . ? 
C19 N1 C7 106.0(3) . . ? 
C11 N1 C7 111.1(3) . . ? 
C15 N1 C7 110.6(3) . . ? 
C8 C7 N1 116.1(4) . . ? 
C7 C8 C9 108.4(5) . . ? 
C10 C9 C8 118.5(7) . . ? 
C12 C11 N1 116.5(4) . . ? 
C13 C12 C11 110.1(6) . . ? 
C14 C13 C12 118.8(9) . . ? 
C16 C15 N1 116.3(4) . . ? 
C17 C16 C15 111.5(5) . . ? 
C16 C17 C18 115.2(6) . . ? 
C20 C19 N1 116.1(4) . . ? 
C19 C20 C21 110.4(5) . . ? 
C22 C21 C20 115.1(5) . . ? 
C35 N2 C23 111.1(3) . . ? 
C35 N2 C27 106.3(3) . . ? 
C23 N2 C27 111.5(3) . . ? 
C35 N2 C31 110.5(3) . . ? 
C23 N2 C31 106.6(3) . . ? 
C27 N2 C31 110.8(3) . . ? 
C24 C23 N2 115.4(4) . . ? 
C23 C24 C25 111.6(5) . . ? 
C26 C25 C24 107.9(6) . . ? 
C28 C27 N2 116.5(4) . . ? 
C29 C28 C27 110.2(4) . . ? 
C30 C29 C28 115.1(5) . . ? 
C32 C31 N2 117.6(4) . . ? 
C31 C32 C33 109.6(4) . . ? 
C34 C33 C32 116.2(6) . . ? 
N2 C35 C36 116.1(4) . . ? 
C35 C36 C37 108.4(5) . . ? 
C38 C37 C36 116.9(7) . . ? 
C39 N4 C45 127.1(3) . . ? 
O7 C39 N3 122.7(4) . . ? 
O7 C39 N4 123.8(4) . . ? 
N3 C39 N4 113.5(4) . . ? 
C45 C40 C41 120.2(4) . . ? 
C42 C41 C40 121.4(4) . . ? 
C41 C42 C43 118.4(5) . . ? 
C42 C43 C44 121.3(5) . . ? 
C45 C44 C43 120.0(4) . . ? 
C44 C45 C40 118.7(4) . . ? 
C44 C45 N4 116.6(4) . . ? 
C40 C45 N4 124.7(4) . . ? 
C46 N6 C52 129.1(4) . . ? 
O8 C46 N5 121.7(4) . . ? 
O8 C46 N6 124.5(4) . . ? 
N5 C46 N6 113.8(4) . . ? 
C52 C47 C48 118.7(6) . . ? 
C49 C48 C47 120.3(7) . . ? 
C50 C49 C48 120.7(7) . . ? 
C51 C50 C49 118.4(7) . . ? 
C50 C51 C52 122.6(5) . . ? 
C47 C52 C51 119.2(5) . . ? 
C47 C52 N6 115.6(5) . . ? 
C51 C52 N6 125.2(4) . . ? 
C53 N8 C59 128.3(3) . . ? 
O9 C53 N7 123.0(4) . . ? 
O9 C53 N8 123.7(4) . . ? 
N7 C53 N8 113.3(4) . . ? 
C59 C54 C55 120.9(5) . . ? 
C56 C55 C54 119.6(5) . . ? 
C57 C56 C55 120.2(6) . . ? 
C56 C57 C58 120.7(5) . . ? 
C57 C58 C59 120.9(5) . . ? 
C54 C59 C58 117.6(4) . . ? 
C54 C59 N8 117.4(4) . . ? 
C58 C59 N8 125.0(4) . . ? 
C60 N10 C66 128.6(3) . . ? 
O10 C60 N9 121.8(4) . . ? 
O10 C60 N10 123.6(4) . . ? 
N9 C60 N10 114.5(4) . . ? 
C66 C61 C62 121.1(4) . . ? 
C63 C62 C61 120.8(5) . . ? 
C62 C63 C64 119.1(5) . . ? 
C63 C64 C65 121.6(5) . . ? 
C66 C65 C64 118.5(5) . . ? 
C65 C66 C61 118.9(4) . . ? 
C65 C66 N10 115.6(4) . . ? 
C61 C66 N10 125.4(4) . . ? 

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 
O1 C1 C2 O2 3.1(6) . . . . ? 
C6 C1 C2 O2 -177.0(3) . . . . ? 
O1 C1 C2 C3 -175.6(4) . . . . ? 
C6 C1 C2 C3 4.3(5) . . . . ? 
O2 C2 C3 O3 -4.2(6) . . . . ? 
C1 C2 C3 O3 174.4(3) . . . . ? 
O2 C2 C3 C4 175.3(3) . . . . ? 
C1 C2 C3 C4 -6.1(5) . . . . ? 
O3 C3 C4 O4 4.0(6) . . . . ? 
C2 C3 C4 O4 -175.5(4) . . . . ? 
O3 C3 C4 C5 -177.2(3) . . . . ? 
C2 C3 C4 C5 3.3(6) . . . . ? 
O4 C4 C5 O5 -0.4(6) . . . . ? 
C3 C4 C5 O5 -179.2(4) . . . . ? 
O4 C4 C5 C6 -179.9(4) . . . . ? 
C3 C4 C5 C6 1.3(5) . . . . ? 
O5 C5 C6 O6 -2.5(6) . . . . ? 
C4 C5 C6 O6 177.0(3) . . . . ? 
O5 C5 C6 C1 177.5(3) . . . . ? 
C4 C5 C6 C1 -3.0(5) . . . . ? 
O1 C1 C6 O6 0.0(6) . . . . ? 
C2 C1 C6 O6 -179.8(3) . . . . ? 
O1 C1 C6 C5 -180.0(4) . . . . ? 
C2 C1 C6 C5 0.2(5) . . . . ? 
C19 N1 C7 C8 -179.2(4) . . . . ? 
C11 N1 C7 C8 -59.5(5) . . . . ? 
C15 N1 C7 C8 60.2(5) . . . . ? 
N1 C7 C8 C9 175.3(5) . . . . ? 
C7 C8 C9 C10 -166.8(8) . . . . ? 
C19 N1 C11 C12 56.8(6) . . . . ? 
C15 N1 C11 C12 178.2(4) . . . . ? 
C7 N1 C11 C12 -60.4(6) . . . . ? 
N1 C11 C12 C13 -172.9(5) . . . . ? 
C11 C12 C13 C14 -175.6(10) . . . . ? 
C19 N1 C15 C16 -55.4(5) . . . . ? 
C11 N1 C15 C16 -176.2(4) . . . . ? 
C7 N1 C15 C16 62.2(5) . . . . ? 
N1 C15 C16 C17 -172.4(4) . . . . ? 
C15 C16 C17 C18 -177.8(5) . . . . ? 
C11 N1 C19 C20 58.4(5) . . . . ? 
C15 N1 C19 C20 -61.0(5) . . . . ? 
C7 N1 C19 C20 178.7(4) . . . . ? 
N1 C19 C20 C21 -174.8(4) . . . . ? 
C19 C20 C21 C22 173.5(5) . . . . ? 
C35 N2 C23 C24 61.4(5) . . . . ? 
C27 N2 C23 C24 -57.0(5) . . . . ? 
C31 N2 C23 C24 -178.1(4) . . . . ? 
N2 C23 C24 C25 -176.2(4) . . . . ? 
C23 C24 C25 C26 78.7(7) . . . . ? 
C35 N2 C27 C28 -175.5(4) . . . . ? 
C23 N2 C27 C28 -54.3(5) . . . . ? 
C31 N2 C27 C28 64.3(5) . . . . ? 
N2 C27 C28 C29 -168.5(4) . . . . ? 
C27 C28 C29 C30 -176.9(5) . . . . ? 
C35 N2 C31 C32 -57.8(5) . . . . ? 
C23 N2 C31 C32 -178.6(4) . . . . ? 
C27 N2 C31 C32 59.8(5) . . . . ? 
N2 C31 C32 C33 174.8(4) . . . . ? 
C31 C32 C33 C34 -176.6(6) . . . . ? 
C23 N2 C35 C36 60.7(5) . . . . ? 
C27 N2 C35 C36 -177.7(4) . . . . ? 
C31 N2 C35 C36 -57.4(5) . . . . ? 
N2 C35 C36 C37 -173.8(5) . . . . ? 
C35 C36 C37 C38 -173.6(7) . . . . ? 
C45 N4 C39 O7 -9.3(6) . . . . ? 
C45 N4 C39 N3 171.1(3) . . . . ? 
C45 C40 C41 C42 -1.4(7) . . . . ? 
C40 C41 C42 C43 -0.6(7) . . . . ? 
C41 C42 C43 C44 1.2(8) . . . . ? 
C42 C43 C44 C45 0.1(8) . . . . ? 
C43 C44 C45 C40 -2.1(6) . . . . ? 
C43 C44 C45 N4 178.2(4) . . . . ? 
C41 C40 C45 C44 2.7(6) . . . . ? 
C41 C40 C45 N4 -177.6(4) . . . . ? 
C39 N4 C45 C44 -169.4(4) . . . . ? 
C39 N4 C45 C40 10.9(6) . . . . ? 
C52 N6 C46 O8 -0.8(7) . . . . ? 
C52 N6 C46 N5 -179.9(4) . . . . ? 
C52 C47 C48 C49 1.7(14) . . . . ? 
C47 C48 C49 C50 -2.0(18) . . . . ? 
C48 C49 C50 C51 1.4(15) . . . . ? 
C49 C50 C51 C52 -0.7(10) . . . . ? 
C48 C47 C52 C51 -1.0(9) . . . . ? 
C48 C47 C52 N6 179.4(6) . . . . ? 
C50 C51 C52 C47 0.5(8) . . . . ? 
C50 C51 C52 N6 -179.9(5) . . . . ? 
C46 N6 C52 C47 -172.5(4) . . . . ? 
C46 N6 C52 C51 7.9(7) . . . . ? 
C59 N8 C53 O9 4.6(6) . . . . ? 
C59 N8 C53 N7 -176.1(3) . . . . ? 
C59 C54 C55 C56 0.6(9) . . . . ? 
C54 C55 C56 C57 -1.1(10) . . . . ? 
C55 C56 C57 C58 0.3(10) . . . . ? 
C56 C57 C58 C59 1.2(8) . . . . ? 
C55 C54 C59 C58 0.8(7) . . . . ? 
C55 C54 C59 N8 -179.5(5) . . . . ? 
C57 C58 C59 C54 -1.7(6) . . . . ? 
C57 C58 C59 N8 178.6(4) . . . . ? 
C53 N8 C59 C54 176.3(4) . . . . ? 
C53 N8 C59 C58 -4.0(6) . . . . ? 
C66 N10 C60 O10 -1.3(6) . . . . ? 
C66 N10 C60 N9 -179.2(4) . . . . ? 
C66 C61 C62 C63 -0.6(8) . . . . ? 
C61 C62 C63 C64 -0.6(8) . . . . ? 
C62 C63 C64 C65 0.2(9) . . . . ? 
C63 C64 C65 C66 1.4(8) . . . . ? 
C64 C65 C66 C61 -2.5(7) . . . . ? 
C64 C65 C66 N10 178.9(4) . . . . ? 
C62 C61 C66 C65 2.2(7) . . . . ? 
C62 C61 C66 N10 -179.4(4) . . . . ? 
C60 N10 C66 C65 -177.1(4) . . . . ? 
C60 N10 C66 C61 4.5(7) . . . . ? 

loop_ 
_geom_hbond_atom_site_label_D 
_geom_hbond_atom_site_label_H 
_geom_hbond_atom_site_label_A 
_geom_hbond_distance_DH 
_geom_hbond_distance_HA 
_geom_hbond_distance_DA 
_geom_hbond_angle_DHA 
_geom_hbond_site_symmetry_A 
N3 H3A O10  0.86 2.26 3.063(4) 154.9 1_645 
N3 H3B O3  0.86 2.14 2.863(4) 141.5 . 
N4 H4A O2  0.86 2.11 2.960(4) 171.5 . 
N5 H5A O10  0.86 2.05 2.913(4) 176.1 1_645 
N5 H5B O3  0.86 2.10 2.897(4) 153.3 . 
N6 H6A O4  0.86 1.97 2.834(4) 176.6 . 
N7 H7A O8  0.86 2.29 3.083(4) 153.5 1_465 
N7 H7B O6  0.86 2.19 2.933(4) 144.1 . 
N8 H8A O5  0.86 2.04 2.895(4) 170.5 . 
N9 H9A O8  0.86 2.13 2.969(4) 166.5 1_465 
N9 H9B O6  0.86 2.04 2.856(4) 157.0 . 
N10 H10A O1  0.86 2.00 2.857(4) 175.6 . 

_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              22.54 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.251 
_refine_diff_density_min   -0.120 
_refine_diff_density_rms    0.029 


data_02ckm 
_database_code_CSD            163267
_journal_coden_Cambridge 182 
_journal_volume           ?
_journal_year             ? 
_journal_page_first       ?

_publ_requested_journal       'Chemical Communications'


loop_
_publ_author_name  
'Chi-Keung Lam'
'Thomas C. W. Mak'

_publ_contact_author_name     	'Prof Thomas C W Mak'  
_publ_contact_author_address 
;
Prof Thomas C W Mak
The Chinese University of Hong Kong
Department of Chemistry
Shatin
New Territories
Hong Kong
SAR, 
P R CHINA
;

_publ_contact_author_email       'TCWMAK@CUHK.EDU.HK'

_publ_section_title
;
Rhodizonate and croconate dianions as divergent hydrogen-bond
acceptors in the self-assembly of supramolecular structures
; 

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C65 H104 N10 O9' 
_chemical_formula_weight          1169.58 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 

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

_cell_length_a                    8.7478(9) 
_cell_length_b                    13.1937(13) 
_cell_length_c                    17.1799(17) 
_cell_angle_alpha                 70.147(2) 
_cell_angle_beta                  86.368(2) 
_cell_angle_gamma                 70.806(2) 
_cell_volume                      1758.7(3) 
_cell_formula_units_Z             1 
_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     1.104 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              636 
_exptl_absorpt_coefficient_mu     0.074 
_exptl_absorpt_correction_type    none 
_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   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             9038 
_diffrn_reflns_av_R_equivalents   0.0307 
_diffrn_reflns_av_sigmaI/netI     0.0414 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.74 
_diffrn_reflns_theta_max          24.04 
_reflns_number_total              5489 
_reflns_number_gt                 2909 
_reflns_threshold_expression      >2sigma(I) 

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

_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^)+(0.0980P)^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        0.007(2) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          5489 
_refine_ls_number_parameters      425 
_refine_ls_number_restraints      27 
_refine_ls_R_factor_all           0.0990 
_refine_ls_R_factor_gt            0.0563 
_refine_ls_wR_factor_ref          0.1834 
_refine_ls_wR_factor_gt           0.1619 
_refine_ls_goodness_of_fit_ref    0.992 
_refine_ls_restrained_S_all       1.009 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 

loop_ 
_atom_site_label 
_atom_site_type_symbol 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_adp_type 
_atom_site_occupancy 
_atom_site_symmetry_multiplicity 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
O1 O 0.5162(5) 0.7057(4) 0.4394(2) 0.1155(14) Uani 0.50 1 d PD . . 
O2 O 0.6328(5) 0.5392(4) 0.6033(3) 0.1204(14) Uani 0.50 1 d PD . . 
O3 O 0.5621(5) 0.3325(3) 0.6127(2) 0.1216(16) Uani 0.50 1 d PD . . 
O4 O 0.3909(6) 0.3796(4) 0.4602(3) 0.1330(17) Uani 0.50 1 d PD . . 
O5 O 0.3702(4) 0.6089(3) 0.3497(2) 0.0876(10) Uani 0.50 1 d PD . . 
C1 C 0.5021(12) 0.6101(8) 0.4645(12) 0.075(3) Uani 0.50 1 d PD . . 
C2 C 0.5669(13) 0.5279(18) 0.5458(11) 0.078(4) Uani 0.50 1 d PD . . 
C3 C 0.5344(18) 0.4242(10) 0.5543(9) 0.080(4) Uani 0.50 1 d PD . . 
C4 C 0.4510(17) 0.4431(18) 0.4773(15) 0.093(6) Uani 0.50 1 d PD . . 
C5 C 0.4339(12) 0.5568(19) 0.4214(7) 0.073(3) Uani 0.50 1 d PD . . 
N1 N 0.5510(3) 0.85271(17) 0.51625(13) 0.1109(8) Uani 1 1 d . . . 
H1A H 0.5118 0.9194 0.4797 0.133 Uiso 1 1 calc R . . 
H1B H 0.5557 0.7932 0.5048 0.133 Uiso 1 1 calc R . . 
O6 O 0.6002(3) 0.92465(15) 0.60979(11) 0.1156(7) Uani 1 1 d . . . 
C6 C 0.6049(4) 0.8415(2) 0.59115(16) 0.0896(8) Uani 1 1 d . . . 
N2 N 0.6662(3) 0.73194(17) 0.64255(12) 0.0921(7) Uani 1 1 d . . . 
H2A H 0.6659 0.6808 0.6222 0.110 Uiso 1 1 calc R . . 
C7 C 0.7299(3) 0.6909(2) 0.72449(16) 0.0858(7) Uani 1 1 d . . . 
C8 C 0.7477(4) 0.5800(3) 0.76929(18) 0.1125(10) Uani 1 1 d . . . 
H8A H 0.7177 0.5355 0.7453 0.135 Uiso 1 1 calc R . . 
C9 C 0.8097(6) 0.5340(4) 0.8498(2) 0.1545(15) Uani 1 1 d . . . 
H9A H 0.8203 0.4585 0.8802 0.185 Uiso 1 1 calc R . . 
C10 C 0.8561(6) 0.5978(5) 0.8855(2) 0.1589(17) Uani 1 1 d . . . 
H10A H 0.9001 0.5657 0.9397 0.191 Uiso 1 1 calc R . . 
C11 C 0.8376(5) 0.7078(4) 0.8417(2) 0.1387(13) Uani 1 1 d . . . 
H11A H 0.8661 0.7522 0.8664 0.166 Uiso 1 1 calc R . . 
C12 C 0.7768(4) 0.7548(3) 0.76065(18) 0.1144(10) Uani 1 1 d . . . 
H12A H 0.7676 0.8301 0.7304 0.137 Uiso 1 1 calc R . . 
N3 N 0.3893(3) 0.91025(18) 0.30651(13) 0.0935(7) Uani 1 1 d . . . 
H3A H 0.3759 0.9717 0.3171 0.112 Uiso 1 1 calc R . . 
H3B H 0.3897 0.8489 0.3459 0.112 Uiso 1 1 calc R . . 
O7 O 0.4101(3) 0.99427(17) 0.17047(12) 0.1321(8) Uani 1 1 d . . . 
C13 C 0.4097(3) 0.9100(2) 0.22824(17) 0.0816(7) Uani 1 1 d . . . 
N4 N 0.4308(2) 0.80731(17) 0.22027(11) 0.0778(6) Uani 1 1 d . . . 
H4A H 0.4275 0.7535 0.2652 0.093 Uiso 1 1 calc R . . 
C14 C 0.4572(3) 0.7775(2) 0.14823(14) 0.0759(7) Uani 1 1 d . . . 
C15 C 0.4680(3) 0.8512(2) 0.07088(15) 0.0958(8) Uani 1 1 d . . . 
H15 H 0.4566 0.9265 0.0637 0.115 Uiso 1 1 calc R . . 
C16 C 0.4956(4) 0.8137(3) 0.00419(19) 0.1205(11) Uani 1 1 d . . . 
H16 H 0.5028 0.8643 -0.0479 0.145 Uiso 1 1 calc R . . 
C17 C 0.5126(5) 0.7046(4) 0.0126(2) 0.1340(12) Uani 1 1 d . . . 
H17 H 0.5330 0.6802 -0.0330 0.161 Uiso 1 1 calc R . . 
C18 C 0.4994(5) 0.6303(3) 0.0895(2) 0.1356(13) Uani 1 1 d . . . 
H18 H 0.5085 0.5556 0.0960 0.163 Uiso 1 1 calc R . . 
C19 C 0.4725(4) 0.6673(2) 0.15658(17) 0.1035(9) Uani 1 1 d . . . 
H19 H 0.4647 0.6167 0.2085 0.124 Uiso 1 1 calc R . . 
N5 N 0.0802(3) 0.1567(2) 0.70840(14) 0.1006(7) Uani 1 1 d . . . 
C20 C 0.1497(4) 0.2550(4) 0.6755(2) 0.1241(11) Uani 1 1 d . . . 
H20A H 0.2261 0.2471 0.7175 0.149 Uiso 1 1 calc R . . 
H20B H 0.2099 0.2475 0.6272 0.149 Uiso 1 1 calc R . . 
C21 C 0.0255(5) 0.3750(4) 0.6515(3) 0.1533(14) Uani 1 1 d . . . 
H21A H -0.0356 0.3817 0.6997 0.184 Uiso 1 1 calc R . . 
H21B H -0.0500 0.3828 0.6092 0.184 Uiso 1 1 calc R . . 
C22 C 0.0929(6) 0.4773(5) 0.6187(3) 0.1792(19) Uani 1 1 d . . . 
H22A H 0.1636 0.4684 0.5740 0.215 Uiso 1 1 calc R . . 
H22B H 0.0038 0.5481 0.5972 0.215 Uiso 1 1 calc R . . 
C23 C 0.1798(7) 0.4815(5) 0.6832(4) 0.208(2) Uani 1 1 d . . . 
H23A H 0.2169 0.5463 0.6631 0.312 Uiso 1 1 calc R . . 
H23B H 0.2713 0.4130 0.7025 0.312 Uiso 1 1 calc R . . 
H23C H 0.1105 0.4882 0.7281 0.312 Uiso 1 1 calc R . . 
C24 C -0.0116(3) 0.1633(3) 0.78495(17) 0.1017(9) Uani 1 1 d . . . 
H24A H -0.1028 0.2336 0.7695 0.122 Uiso 1 1 calc R . . 
H24B H -0.0552 0.1007 0.8037 0.122 Uiso 1 1 calc R . . 
C25 C 0.0832(4) 0.1590(3) 0.85660(19) 0.1273(11) Uani 1 1 d . . . 
H25A H 0.1279 0.2210 0.8392 0.153 Uiso 1 1 calc R . . 
H25B H 0.1727 0.0877 0.8745 0.153 Uiso 1 1 calc R . . 
C26 C -0.0242(4) 0.1686(3) 0.92809(19) 0.1301(12) Uani 1 1 d . . . 
H26A H -0.1179 0.2369 0.9081 0.156 Uiso 1 1 calc R . . 
H26B H -0.0630 0.1038 0.9469 0.156 Uiso 1 1 calc R . . 
C27 C 0.0545(6) 0.1732(4) 0.9988(2) 0.1737(17) Uani 1 1 d . . . 
H27A H -0.0207 0.1777 1.0417 0.261 Uiso 1 1 calc R . . 
H27B H 0.0889 0.2392 0.9816 0.261 Uiso 1 1 calc R . . 
H27C H 0.1470 0.1057 1.0195 0.261 Uiso 1 1 calc R . . 
C28 C 0.2197(3) 0.0460(3) 0.72710(19) 0.1122(10) Uani 1 1 d . . . 
H28A H 0.2745 0.0452 0.6763 0.135 Uiso 1 1 calc R . . 
H28B H 0.2964 0.0449 0.7660 0.135 Uiso 1 1 calc R . . 
C29 C 0.1761(4) -0.0619(3) 0.7623(2) 0.1204(11) Uani 1 1 d . . . 
H29A H 0.1288 -0.0651 0.8154 0.144 Uiso 1 1 calc R . . 
H29B H 0.0953 -0.0602 0.7253 0.144 Uiso 1 1 calc R . . 
C30 C 0.3216(5) -0.1672(4) 0.7738(3) 0.1526(15) Uani 1 1 d . . . 
H30A H 0.3670 -0.1639 0.7203 0.183 Uiso 1 1 calc R . . 
H30B H 0.4031 -0.1668 0.8093 0.183 Uiso 1 1 calc R . . 
C31 C 0.2867(6) -0.2758(4) 0.8101(3) 0.1784(18) Uani 1 1 d . . . 
H31A H 0.3851 -0.3386 0.8166 0.268 Uiso 1 1 calc R . . 
H31B H 0.2101 -0.2789 0.7740 0.268 Uiso 1 1 calc R . . 
H31C H 0.2422 -0.2803 0.8632 0.268 Uiso 1 1 calc R . . 
C32 C -0.0414(3) 0.1661(3) 0.64484(17) 0.1079(9) Uani 1 1 d . . . 
H32A H -0.0858 0.1044 0.6683 0.129 Uiso 1 1 calc R . . 
H32B H -0.1299 0.2370 0.6358 0.129 Uiso 1 1 calc R . . 
C33 C 0.0221(4) 0.1624(3) 0.56141(19) 0.1281(11) Uani 1 1 d . . . 
H33A H 0.1066 0.0900 0.5685 0.154 Uiso 1 1 calc R . . 
H33B H 0.0684 0.2229 0.5369 0.154 Uiso 1 1 calc R . . 
C34 C -0.1151(5) 0.1770(4) 0.5047(2) 0.1511(14) Uani 1 1 d . . . 
H34A H -0.1616 0.1168 0.5303 0.181 Uiso 1 1 calc R . . 
H34B H -0.1991 0.2492 0.4985 0.181 Uiso 1 1 calc R . . 
C35 C -0.0629(6) 0.1738(4) 0.4210(2) 0.1860(19) Uani 1 1 d . . . 
H35A H -0.1539 0.1814 0.3885 0.279 Uiso 1 1 calc R . . 
H35B H 0.0205 0.1026 0.4266 0.279 Uiso 1 1 calc R . . 
H35C H -0.0217 0.2355 0.3940 0.279 Uiso 1 1 calc R . . 

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 
O1 0.181(4) 0.078(3) 0.099(3) -0.025(2) 0.002(3) -0.060(3) 
O2 0.154(4) 0.112(3) 0.091(3) -0.038(3) -0.037(3) -0.027(3) 
O3 0.195(5) 0.069(3) 0.065(2) -0.007(2) 0.001(3) -0.012(3) 
O4 0.238(6) 0.082(3) 0.094(3) -0.025(3) -0.017(3) -0.072(3) 
O5 0.111(3) 0.084(2) 0.058(2) -0.0144(19) -0.0054(18) -0.0276(19) 
C1 0.097(5) 0.060(7) 0.063(7) -0.020(6) 0.006(4) -0.019(4) 
C2 0.090(5) 0.063(10) 0.072(6) -0.020(6) -0.014(4) -0.014(5) 
C3 0.129(9) 0.049(7) 0.053(8) -0.022(4) 0.017(6) -0.014(5) 
C4 0.131(9) 0.058(8) 0.094(13) -0.041(9) 0.015(8) -0.022(6) 
C5 0.092(5) 0.075(9) 0.061(7) -0.038(7) 0.019(4) -0.026(4) 
N1 0.174(3) 0.0748(14) 0.0834(14) -0.0194(11) -0.0363(15) -0.0396(14) 
O6 0.187(2) 0.0745(12) 0.0881(12) -0.0280(10) -0.0270(12) -0.0392(12) 
C6 0.116(2) 0.0747(18) 0.0775(17) -0.0243(14) -0.0091(15) -0.0300(15) 
N2 0.1247(19) 0.0715(13) 0.0778(13) -0.0245(11) -0.0175(12) -0.0259(12) 
C7 0.0888(19) 0.0828(18) 0.0766(16) -0.0296(15) -0.0016(13) -0.0127(14) 
C8 0.137(3) 0.087(2) 0.092(2) -0.0185(16) -0.0113(18) -0.0177(18) 
C9 0.200(4) 0.117(3) 0.097(2) -0.005(2) -0.028(3) -0.014(3) 
C10 0.183(4) 0.158(4) 0.089(2) -0.024(3) -0.039(2) -0.007(3) 
C11 0.157(3) 0.152(3) 0.098(2) -0.045(2) -0.036(2) -0.027(3) 
C12 0.135(3) 0.112(2) 0.0905(19) -0.0332(17) -0.0257(18) -0.0283(19) 
N3 0.1234(19) 0.0907(14) 0.0809(14) -0.0279(11) 0.0168(12) -0.0567(13) 
O7 0.225(3) 0.0929(14) 0.0852(13) -0.0093(11) 0.0031(14) -0.0814(15) 
C13 0.0917(19) 0.0744(17) 0.0790(18) -0.0120(15) -0.0046(13) -0.0403(14) 
N4 0.0912(15) 0.0786(14) 0.0609(11) -0.0101(10) 0.0014(10) -0.0379(11) 
C14 0.0725(16) 0.0768(17) 0.0703(16) -0.0102(13) -0.0027(11) -0.0282(12) 
C15 0.121(2) 0.104(2) 0.0686(16) -0.0169(15) 0.0034(14) -0.0576(17) 
C16 0.157(3) 0.135(3) 0.0773(19) -0.0231(19) 0.0162(18) -0.072(2) 
C17 0.181(4) 0.142(3) 0.090(2) -0.048(2) 0.023(2) -0.060(3) 
C18 0.191(4) 0.107(2) 0.108(3) -0.044(2) 0.016(2) -0.041(2) 
C19 0.133(3) 0.087(2) 0.0816(18) -0.0180(15) 0.0057(16) -0.0342(17) 
N5 0.0650(14) 0.142(2) 0.1020(16) -0.0520(15) 0.0110(12) -0.0337(15) 
C20 0.086(2) 0.178(4) 0.126(2) -0.058(2) 0.0226(19) -0.063(3) 
C21 0.127(3) 0.169(4) 0.173(4) -0.051(3) 0.016(3) -0.068(3) 
C22 0.139(4) 0.265(6) 0.159(4) -0.072(4) 0.020(3) -0.101(4) 
C23 0.153(4) 0.229(5) 0.230(6) -0.059(4) 0.012(4) -0.067(4) 
C24 0.0704(18) 0.141(2) 0.106(2) -0.0573(18) 0.0180(15) -0.0363(16) 
C25 0.101(2) 0.188(3) 0.115(2) -0.073(2) 0.0116(19) -0.054(2) 
C26 0.122(3) 0.171(3) 0.112(2) -0.067(2) 0.016(2) -0.049(2) 
C27 0.169(4) 0.254(5) 0.128(3) -0.103(3) 0.014(3) -0.069(3) 
C28 0.0698(19) 0.160(3) 0.109(2) -0.056(2) 0.0130(16) -0.030(2) 
C29 0.088(2) 0.150(3) 0.121(2) -0.059(2) 0.0087(18) -0.023(2) 
C30 0.107(3) 0.170(4) 0.152(3) -0.061(3) 0.000(2) -0.001(3) 
C31 0.163(4) 0.136(4) 0.199(4) -0.052(3) 0.002(3) -0.005(3) 
C32 0.082(2) 0.146(3) 0.102(2) -0.0492(18) -0.0022(16) -0.0352(17) 
C33 0.116(3) 0.169(3) 0.103(2) -0.055(2) 0.007(2) -0.043(2) 
C34 0.141(3) 0.201(4) 0.115(3) -0.074(3) -0.007(2) -0.038(3) 
C35 0.217(5) 0.221(5) 0.126(3) -0.080(3) 0.001(3) -0.056(4) 

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

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
O1 C1 1.233(10) . ? 
O1 O3 1.461(6) 2_666 ? 
O1 O4 1.778(6) 2_666 ? 
O1 C3 1.87(2) 2_666 ? 
O2 O4 1.211(5) 2_666 ? 
O2 C2 1.248(16) . ? 
O2 C4 1.52(2) 2_666 ? 
O2 C5 1.73(2) 2_666 ? 
O3 C3 1.242(12) . ? 
O3 C1 1.33(2) 2_666 ? 
O3 C5 1.39(2) 2_666 ? 
O3 O5 1.434(6) 2_666 ? 
O3 O1 1.461(6) 2_666 ? 
O4 O2 1.211(5) 2_666 ? 
O4 C4 1.242(16) . ? 
O4 C2 1.36(2) 2_666 ? 
O4 C1 1.71(2) 2_666 ? 
O4 O1 1.778(6) 2_666 ? 
O5 C5 1.250(12) . ? 
O5 O3 1.434(6) 2_666 ? 
O5 C3 1.75(2) 2_666 ? 
C1 C3 0.787(11) 2_666 ? 
C1 C4 1.022(19) 2_666 ? 
C1 O3 1.33(2) 2_666 ? 
C1 C5 1.443(10) . ? 
C1 C2 1.455(13) . ? 
C1 O4 1.71(2) 2_666 ? 
C2 C4 0.44(2) 2_666 ? 
C2 C5 1.07(2) 2_666 ? 
C2 O4 1.36(2) 2_666 ? 
C2 C3 1.445(12) . ? 
C2 C3 1.80(2) 2_666 ? 
C3 C5 0.666(13) 2_666 ? 
C3 C1 0.787(11) 2_666 ? 
C3 C4 1.458(12) . ? 
C3 C4 1.69(2) 2_666 ? 
C3 O5 1.75(2) 2_666 ? 
C3 C2 1.80(2) 2_666 ? 
C3 O1 1.87(2) 2_666 ? 
C4 C2 0.44(2) 2_666 ? 
C4 C1 1.022(19) 2_666 ? 
C4 C5 1.445(13) . ? 
C4 O2 1.52(2) 2_666 ? 
C4 C3 1.69(2) 2_666 ? 
C5 C3 0.666(13) 2_666 ? 
C5 C2 1.07(2) 2_666 ? 
C5 O3 1.39(2) 2_666 ? 
C5 O2 1.73(2) 2_666 ? 
N1 C6 1.342(3) . ? 
O6 C6 1.230(3) . ? 
C6 N2 1.357(3) . ? 
N2 C7 1.403(3) . ? 
C7 C8 1.363(4) . ? 
C7 C12 1.371(4) . ? 
C8 C9 1.372(5) . ? 
C9 C10 1.362(6) . ? 
C10 C11 1.348(5) . ? 
C11 C12 1.377(4) . ? 
N3 C13 1.346(3) . ? 
O7 C13 1.214(3) . ? 
C13 N4 1.359(3) . ? 
N4 C14 1.405(3) . ? 
C14 C19 1.373(3) . ? 
C14 C15 1.374(3) . ? 
C15 C16 1.374(4) . ? 
C16 C17 1.355(4) . ? 
C17 C18 1.376(4) . ? 
C18 C19 1.377(4) . ? 
N5 C24 1.510(3) . ? 
N5 C28 1.511(4) . ? 
N5 C32 1.519(3) . ? 
N5 C20 1.532(4) . ? 
C20 C21 1.530(5) . ? 
C21 C22 1.565(5) . ? 
C22 C23 1.409(6) . ? 
C24 C25 1.503(4) . ? 
C25 C26 1.513(4) . ? 
C26 C27 1.462(5) . ? 
C28 C29 1.511(4) . ? 
C29 C30 1.508(5) . ? 
C30 C31 1.481(5) . ? 
C32 C33 1.514(4) . ? 
C33 C34 1.516(5) . ? 
C34 C35 1.490(5) . ? 

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 O1 O3 58.7(10) . 2_666 ? 
C1 O1 O4 66.4(10) . 2_666 ? 
O3 O1 O4 125.0(4) 2_666 2_666 ? 
C1 O1 C3 17.2(7) . 2_666 ? 
O3 O1 C3 41.4(6) 2_666 2_666 ? 
O4 O1 C3 83.6(6) 2_666 2_666 ? 
O4 O2 C2 67.0(11) 2_666 . ? 
O4 O2 C4 52.7(8) 2_666 2_666 ? 
C2 O2 C4 14.5(11) . 2_666 ? 
O4 O2 C5 104.7(6) 2_666 2_666 ? 
C2 O2 C5 37.7(10) . 2_666 ? 
C4 O2 C5 52.2(6) 2_666 2_666 ? 
C3 O3 C1 35.3(8) . 2_666 ? 
C3 O3 C5 28.6(9) . 2_666 ? 
C1 O3 C5 64.0(5) 2_666 2_666 ? 
C3 O3 O5 81.2(12) . 2_666 ? 
C1 O3 O5 116.5(6) 2_666 2_666 ? 
C5 O3 O5 52.6(5) 2_666 2_666 ? 
C3 O3 O1 87.4(12) . 2_666 ? 
C1 O3 O1 52.1(6) 2_666 2_666 ? 
C5 O3 O1 116.0(5) 2_666 2_666 ? 
O5 O3 O1 168.6(4) 2_666 2_666 ? 
O2 O4 C4 76.5(13) 2_666 . ? 
O2 O4 C2 57.8(9) 2_666 2_666 ? 
C4 O4 C2 18.9(12) . 2_666 ? 
O2 O4 C1 112.7(6) 2_666 2_666 ? 
C4 O4 C1 36.3(12) . 2_666 ? 
C2 O4 C1 55.2(7) 2_666 2_666 ? 
O2 O4 O1 153.4(5) 2_666 2_666 ? 
C4 O4 O1 77.6(13) . 2_666 ? 
C2 O4 O1 96.5(8) 2_666 2_666 ? 
C1 O4 O1 41.3(4) 2_666 2_666 ? 
C5 O5 O3 61.9(10) . 2_666 ? 
C5 O5 C3 17.3(8) . 2_666 ? 
O3 O5 C3 44.6(6) 2_666 2_666 ? 
C3 C1 C4 106.6(17) 2_666 2_666 ? 
C3 C1 O1 135(2) 2_666 . ? 
C4 C1 O1 118.2(19) 2_666 . ? 
C3 C1 O3 65.9(14) 2_666 2_666 ? 
C4 C1 O3 172.4(16) 2_666 2_666 ? 
O1 C1 O3 69.3(8) . 2_666 ? 
C3 C1 C5 6.2(12) 2_666 . ? 
C4 C1 C5 112.6(11) 2_666 . ? 
O1 C1 C5 129(2) . . ? 
O3 C1 C5 59.8(15) 2_666 . ? 
C3 C1 C2 102.5(16) 2_666 . ? 
C4 C1 C2 4.1(13) 2_666 . ? 
O1 C1 C2 122.3(19) . . ? 
O3 C1 C2 168.3(17) 2_666 . ? 
C5 C1 C2 108.6(13) . . ? 
C3 C1 O4 152.4(16) 2_666 2_666 ? 
C4 C1 O4 46.0(12) 2_666 2_666 ? 
O1 C1 O4 72.3(8) . 2_666 ? 
O3 C1 O4 141.4(8) 2_666 2_666 ? 
C5 C1 O4 158.1(15) . 2_666 ? 
C2 C1 O4 50.0(12) . 2_666 ? 
C4 C2 C5 143(4) 2_666 2_666 ? 
C4 C2 O2 120(5) 2_666 . ? 
C5 C2 O2 96.6(18) 2_666 . ? 
C4 C2 O4 66(4) 2_666 2_666 ? 
C5 C2 O4 151.7(18) 2_666 2_666 ? 
O2 C2 O4 55.2(7) . 2_666 ? 
C4 C2 C3 117(4) 2_666 . ? 
C5 C2 C3 25.6(8) 2_666 . ? 
O2 C2 C3 122(2) . . ? 
O4 C2 C3 175.7(15) 2_666 . ? 
C4 C2 C1 10(3) 2_666 . ? 
C5 C2 C1 133.5(14) 2_666 . ? 
O2 C2 C1 130(2) . . ? 
O4 C2 C1 74.9(16) 2_666 . ? 
C3 C2 C1 108.0(11) . . ? 
C4 C2 C3 35(3) 2_666 2_666 ? 
C5 C2 C3 108.2(12) 2_666 2_666 ? 
O2 C2 C3 155(2) . 2_666 ? 
O4 C2 C3 100.1(18) 2_666 2_666 ? 
C3 C2 C3 82.7(9) . 2_666 ? 
C1 C2 C3 25.3(5) . 2_666 ? 
C5 C3 C1 166(3) 2_666 2_666 ? 
C5 C3 O3 88(3) 2_666 . ? 
C1 C3 O3 79(2) 2_666 . ? 
C5 C3 C2 43.8(17) 2_666 . ? 
C1 C3 C2 149.4(14) 2_666 . ? 
O3 C3 C2 132(2) . . ? 
C5 C3 C4 150.8(19) 2_666 . ? 
C1 C3 C4 42.2(13) 2_666 . ? 
O3 C3 C4 121(2) . . ? 
C2 C3 C4 107.2(8) . . ? 
C5 C3 C4 57.1(17) 2_666 2_666 ? 
C1 C3 C4 136.1(18) 2_666 2_666 ? 
O3 C3 C4 145(3) . 2_666 ? 
C2 C3 C4 13.4(9) . 2_666 ? 
C4 C3 C4 93.9(9) . 2_666 ? 
C5 C3 O5 34(2) 2_666 2_666 ? 
C1 C3 O5 133.0(17) 2_666 2_666 ? 
O3 C3 O5 54.2(8) . 2_666 ? 
C2 C3 O5 77.6(16) . 2_666 ? 
C4 C3 O5 175.1(16) . 2_666 ? 
C4 C3 O5 90.9(19) 2_666 2_666 ? 
C5 C3 C2 141(2) 2_666 2_666 ? 
C1 C3 C2 52.2(13) 2_666 2_666 ? 
O3 C3 C2 131(2) . 2_666 ? 
C2 C3 C2 97.3(9) . 2_666 ? 
C4 C3 C2 9.9(9) . 2_666 ? 
C4 C3 C2 83.9(8) 2_666 2_666 ? 
O5 C3 C2 174.6(16) 2_666 2_666 ? 
C5 C3 O1 139(3) 2_666 2_666 ? 
C1 C3 O1 27.6(14) 2_666 2_666 ? 
O3 C3 O1 51.1(8) . 2_666 ? 
C2 C3 O1 176.9(17) . 2_666 ? 
C4 C3 O1 69.9(16) . 2_666 ? 
C4 C3 O1 164(2) 2_666 2_666 ? 
O5 C3 O1 105.3(6) 2_666 2_666 ? 
C2 C3 O1 79.8(16) 2_666 2_666 ? 
C2 C4 C1 166(4) 2_666 2_666 ? 
C2 C4 O4 96(5) 2_666 . ? 
C1 C4 O4 98(2) 2_666 . ? 
C2 C4 C5 27(3) 2_666 . ? 
C1 C4 C5 140.0(14) 2_666 . ? 
O4 C4 C5 122(2) . . ? 
C2 C4 C3 135(4) 2_666 . ? 
C1 C4 C3 31.2(7) 2_666 . ? 
O4 C4 C3 129(2) . . ? 
C5 C4 C3 108.9(10) . . ? 
C2 C4 O2 45(4) 2_666 2_666 ? 
C1 C4 O2 148.3(19) 2_666 2_666 ? 
O4 C4 O2 50.9(8) . 2_666 ? 
C5 C4 O2 71.6(17) . 2_666 ? 
C3 C4 O2 178.8(11) . 2_666 ? 
C2 C4 C3 49(3) 2_666 2_666 ? 
C1 C4 C3 117.3(13) 2_666 2_666 ? 
O4 C4 C3 145(3) . 2_666 ? 
C5 C4 C3 22.8(6) . 2_666 ? 
C3 C4 C3 86.1(9) . 2_666 ? 
O2 C4 C3 94(2) 2_666 2_666 ? 
C3 C5 C2 111(2) 2_666 2_666 ? 
C3 C5 O5 129(3) 2_666 . ? 
C2 C5 O5 120.3(18) 2_666 . ? 
C3 C5 O3 63(2) 2_666 2_666 ? 
C2 C5 O3 173.8(13) 2_666 2_666 ? 
O5 C5 O3 65.6(9) . 2_666 ? 
C3 C5 C1 7.3(14) 2_666 . ? 
C2 C5 C1 117.8(12) 2_666 . ? 
O5 C5 C1 122(2) . . ? 
O3 C5 C1 56.2(14) 2_666 . ? 
C3 C5 C4 100(2) 2_666 . ? 
C2 C5 C4 10.6(13) 2_666 . ? 
O5 C5 C4 131(2) . . ? 
O3 C5 C4 163.5(16) 2_666 . ? 
C1 C5 C4 107.3(12) . . ? 
C3 C5 O2 156(3) 2_666 2_666 ? 
C2 C5 O2 45.6(12) 2_666 2_666 ? 
O5 C5 O2 74.7(8) . 2_666 ? 
O3 C5 O2 140.3(8) 2_666 2_666 ? 
C1 C5 O2 163.4(17) . 2_666 ? 
C4 C5 O2 56.2(14) . 2_666 ? 
O6 C6 N1 121.9(2) . . ? 
O6 C6 N2 123.9(2) . . ? 
N1 C6 N2 114.2(2) . . ? 
C6 N2 C7 128.7(2) . . ? 
C8 C7 C12 119.1(3) . . ? 
C8 C7 N2 116.9(3) . . ? 
C12 C7 N2 124.0(3) . . ? 
C7 C8 C9 120.1(4) . . ? 
C10 C9 C8 120.6(4) . . ? 
C11 C10 C9 119.5(3) . . ? 
C10 C11 C12 120.5(4) . . ? 
C7 C12 C11 120.1(3) . . ? 
O7 C13 N3 122.5(2) . . ? 
O7 C13 N4 123.5(3) . . ? 
N3 C13 N4 114.0(2) . . ? 
C13 N4 C14 128.5(2) . . ? 
C19 C14 C15 118.5(3) . . ? 
C19 C14 N4 117.2(2) . . ? 
C15 C14 N4 124.3(2) . . ? 
C16 C15 C14 120.0(3) . . ? 
C17 C16 C15 121.4(3) . . ? 
C16 C17 C18 119.2(3) . . ? 
C17 C18 C19 119.6(3) . . ? 
C14 C19 C18 121.2(3) . . ? 
C24 N5 C28 111.1(2) . . ? 
C24 N5 C32 106.3(2) . . ? 
C28 N5 C32 110.9(2) . . ? 
C24 N5 C20 110.3(2) . . ? 
C28 N5 C20 108.0(2) . . ? 
C32 N5 C20 110.3(2) . . ? 
C21 C20 N5 115.7(3) . . ? 
C20 C21 C22 116.9(4) . . ? 
C23 C22 C21 110.1(4) . . ? 
C25 C24 N5 116.2(2) . . ? 
C24 C25 C26 110.6(3) . . ? 
C27 C26 C25 114.6(3) . . ? 
C29 C28 N5 116.1(2) . . ? 
C30 C29 C28 112.0(3) . . ? 
C31 C30 C29 114.4(4) . . ? 
C33 C32 N5 116.4(2) . . ? 
C32 C33 C34 109.7(3) . . ? 
C35 C34 C33 113.3(4) . . ? 

_diffrn_measured_fraction_theta_max    0.993 
_diffrn_reflns_theta_full              24.04 
_diffrn_measured_fraction_theta_full   0.993 
_refine_diff_density_max    0.176 
_refine_diff_density_min   -0.137 
_refine_diff_density_rms    0.029