Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002
data_eu 

_database_code_CSD	175743


_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Ng, Dennis K. P.'
'Lam, Chi-Keung'
'Lee, Chi-Hang'
'Li, Hung-Wing'
'Liu, Wei'
'Mak, Thomas C. W.'
'Wang, Jinzhi'

_publ_contact_author_name     	'Prof Dennis K. P. Ng'  
_publ_contact_author_address 
;
Chemistry
The Chinese University of Hong Kong
Department of Chemistry, University
Hong Kong
CHINA
;

_publ_contact_author_email       'DKPN@CUHK.EDU.HK'

_publ_section_title		
;
Formation and crystal structure of an unexpected inclusion complex
of metal-free phthalocyanine and oxalic acid
;


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C62 H76 N8 O8' 
_chemical_formula_weight          1061.31 

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            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/c 

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

_cell_length_a                    15.8962(15) 
_cell_length_b                    8.8141(9) 
_cell_length_c                    21.695(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.911(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2994.4(5) 
_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        'rhombic plate' 
_exptl_crystal_colour             green 
_exptl_crystal_size_max           '0.76'  
_exptl_crystal_size_mid           '0.23' 
_exptl_crystal_size_min           '0.21'  
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.177 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1136 
_exptl_absorpt_coefficient_mu     0.079 
_exptl_absorpt_correction_type    SADABS 
_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 1K' 
_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             13406 
_diffrn_reflns_av_R_equivalents   0.0432 
_diffrn_reflns_av_sigmaI/netI     0.0486 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          1.91 
_diffrn_reflns_theta_max          23.00 
_reflns_number_total              4160 
_reflns_number_gt                 2594 
_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^)+(0.1436P)^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        0.0030(16) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          4160 
_refine_ls_number_parameters      358 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1015 
_refine_ls_R_factor_gt            0.0686 
_refine_ls_wR_factor_ref          0.2195 
_refine_ls_wR_factor_gt           0.1996 
_refine_ls_goodness_of_fit_ref    1.002 
_refine_ls_restrained_S_all       1.002 
_refine_ls_shift/su_max           0.588 
_refine_ls_shift/su_mean          0.022 

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 
N1 N 0.62220(17) -0.0281(3) 0.49583(12) 0.0504(7) Uani 1 1 d . . . 
H1 H 0.561(3) -0.0009(16) 0.4993(2) 0.25(3) Uiso 1 1 d R . . 
O1 O 0.63255(15) 0.3163(3) 0.29127(11) 0.0694(8) Uani 1 1 d . . . 
C1 C 0.4118(2) 0.1916(4) 0.39600(14) 0.0464(8) Uani 1 1 d . . . 
N2 N 0.62989(16) 0.1164(3) 0.40187(12) 0.0510(7) Uani 1 1 d . . . 
O2 O 0.15702(15) 0.2809(3) 0.41544(13) 0.0810(9) Uani 1 1 d . . . 
C2 C 0.4268(2) 0.2771(4) 0.34196(14) 0.0470(8) Uani 1 1 d . . . 
N3 N 0.48591(16) 0.1238(3) 0.42354(12) 0.0475(7) Uani 1 1 d . . . 
C3 C 0.3723(2) 0.3632(4) 0.29884(16) 0.0608(10) Uani 1 1 d . . . 
H3B H 0.3148 0.3739 0.3015 0.073 Uiso 1 1 calc R . . 
N4 N 0.33642(17) 0.1900(3) 0.41408(12) 0.0519(8) Uani 1 1 d . . . 
C4 C 0.4069(2) 0.4328(4) 0.25162(17) 0.0672(11) Uani 1 1 d . . . 
H4C H 0.3719 0.4905 0.2217 0.081 Uiso 1 1 calc R . . 
C5 C 0.4923(2) 0.4177(4) 0.24834(17) 0.0649(11) Uani 1 1 d . . . 
H5A H 0.5130 0.4647 0.2156 0.078 Uiso 1 1 calc R . . 
C6 C 0.5485(2) 0.3356(4) 0.29155(16) 0.0526(9) Uani 1 1 d . . . 
C7 C 0.5132(2) 0.2612(4) 0.33878(14) 0.0451(8) Uani 1 1 d . . . 
C8 C 0.5490(2) 0.1621(4) 0.39039(14) 0.0456(8) Uani 1 1 d . . . 
C9 C 0.6619(2) 0.0283(4) 0.44984(15) 0.0501(9) Uani 1 1 d . . . 
C10 C 0.7485(2) -0.0259(4) 0.45954(16) 0.0568(9) Uani 1 1 d . . . 
C11 C 0.8136(2) -0.0036(5) 0.4250(2) 0.0803(13) Uani 1 1 d . . . 
H11A H 0.8058 0.0564 0.3892 0.096 Uiso 1 1 calc R . . 
C12 C 0.8897(3) -0.0741(6) 0.4463(2) 0.1010(17) Uani 1 1 d . . . 
H12A H 0.9343 -0.0617 0.4241 0.121 Uiso 1 1 calc R . . 
C13 C 0.3208(2) 0.1163(4) 0.46474(15) 0.0504(9) Uani 1 1 d . . . 
C14 C 0.2404(2) 0.1177(4) 0.48708(16) 0.0543(9) Uani 1 1 d . . . 
C15 C 0.1618(2) 0.1901(5) 0.46662(18) 0.0686(11) Uani 1 1 d . . . 
C16 C 0.0972(3) 0.1637(5) 0.5002(2) 0.0913(15) Uani 1 1 d . . . 
H16A H 0.0437 0.2066 0.4868 0.110 Uiso 1 1 calc R . . 
C17 C 0.0867(2) 0.3822(5) 0.39516(19) 0.0763(12) Uani 1 1 d . . . 
H17A H 0.0431 0.3650 0.4213 0.092 Uiso 1 1 calc R . . 
C18 C 0.1192(3) 0.5439(6) 0.4054(2) 0.0991(15) Uani 1 1 d . . . 
H18A H 0.1649 0.5592 0.3810 0.119 Uiso 1 1 calc R . . 
C19 C 0.1549(6) 0.5728(9) 0.4733(3) 0.205(4) Uani 1 1 d . . . 
H19A H 0.1995 0.5009 0.4874 0.307 Uiso 1 1 calc R . . 
H19B H 0.1104 0.5621 0.4977 0.307 Uiso 1 1 calc R . . 
H19C H 0.1778 0.6738 0.4780 0.307 Uiso 1 1 calc R . . 
C20 C 0.0506(5) 0.6607(7) 0.3851(3) 0.156(3) Uani 1 1 d . . . 
H20A H 0.0745 0.7606 0.3921 0.233 Uiso 1 1 calc R . . 
H20B H 0.0055 0.6481 0.4090 0.233 Uiso 1 1 calc R . . 
H20C H 0.0281 0.6478 0.3415 0.233 Uiso 1 1 calc R . . 
C21 C 0.0493(3) 0.3388(6) 0.3279(2) 0.0897(14) Uani 1 1 d . . . 
H21A H 0.0018 0.4081 0.3136 0.108 Uiso 1 1 calc R . . 
C22 C 0.0130(4) 0.1786(7) 0.3255(3) 0.140(2) Uani 1 1 d . . . 
H22A H -0.0273 0.1710 0.3536 0.210 Uiso 1 1 calc R . . 
H22B H 0.0585 0.1074 0.3376 0.210 Uiso 1 1 calc R . . 
H22C H -0.0152 0.1566 0.2836 0.210 Uiso 1 1 calc R . . 
C23 C 0.1124(3) 0.3553(7) 0.2841(2) 0.1139(18) Uani 1 1 d . . . 
H23A H 0.1342 0.4571 0.2864 0.171 Uiso 1 1 calc R . . 
H23B H 0.0846 0.3341 0.2421 0.171 Uiso 1 1 calc R . . 
H23C H 0.1586 0.2854 0.2959 0.171 Uiso 1 1 calc R . . 
C24 C 0.6828(3) 0.4256(5) 0.2625(2) 0.0848(14) Uani 1 1 d . . . 
H24A H 0.6443 0.4988 0.2381 0.102 Uiso 1 1 calc R . . 
C25 C 0.7287(4) 0.3381(8) 0.2194(3) 0.125(2) Uani 1 1 d . . . 
H25A H 0.7570 0.2511 0.2422 0.150 Uiso 1 1 calc R . . 
C26 C 0.7917(5) 0.4199(10) 0.1895(4) 0.195(4) Uani 1 1 d . . . 
H26A H 0.8354 0.4610 0.2212 0.293 Uiso 1 1 calc R . . 
H26B H 0.7639 0.5008 0.1643 0.293 Uiso 1 1 calc R . . 
H26C H 0.8170 0.3511 0.1636 0.293 Uiso 1 1 calc R . . 
C27 C 0.6633(6) 0.2793(9) 0.1650(3) 0.163(3) Uani 1 1 d . . . 
H27A H 0.6919 0.2218 0.1372 0.245 Uiso 1 1 calc R . . 
H27B H 0.6340 0.3634 0.1428 0.245 Uiso 1 1 calc R . . 
H27C H 0.6229 0.2155 0.1807 0.245 Uiso 1 1 calc R . . 
C28 C 0.7386(4) 0.5077(8) 0.3161(4) 0.138(2) Uani 1 1 d . . . 
H28A H 0.7708 0.5840 0.2969 0.165 Uiso 1 1 calc R . . 
C29 C 0.8048(4) 0.4012(11) 0.3532(4) 0.200(4) Uani 1 1 d . . . 
H29A H 0.8366 0.3519 0.3251 0.300 Uiso 1 1 calc R . . 
H29B H 0.7763 0.3263 0.3742 0.300 Uiso 1 1 calc R . . 
H29C H 0.8430 0.4587 0.3835 0.300 Uiso 1 1 calc R . . 
C30 C 0.6874(6) 0.5924(9) 0.3560(4) 0.191(4) Uani 1 1 d . . . 
H30A H 0.6485 0.6593 0.3304 0.286 Uiso 1 1 calc R . . 
H30B H 0.7249 0.6505 0.3866 0.286 Uiso 1 1 calc R . . 
H30C H 0.6558 0.5218 0.3769 0.286 Uiso 1 1 calc R . . 
O3 O 0.3849(5) 0.5685(10) 0.4884(3) 0.219(3) Uani 1 1 d . . . 
O4 O 0.5165(5) 0.6436(11) 0.4454(4) 0.267(5) Uani 1 1 d . . . 
C31 C 0.4574(8) 0.5363(14) 0.4789(9) 0.236(7) Uani 1 1 d . . . 
H4 H 0.5142(8) 0.6876(16) 0.3998(7) 0.014(6) Uiso 1 1 d 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 
N1 0.0481(17) 0.0600(18) 0.0434(16) 0.0102(14) 0.0086(13) 0.0089(14) 
O1 0.0626(17) 0.0727(18) 0.0766(18) 0.0291(14) 0.0222(14) 0.0066(13) 
C1 0.046(2) 0.052(2) 0.0405(19) 0.0017(15) 0.0072(15) 0.0031(16) 
N2 0.0492(17) 0.0578(18) 0.0463(17) 0.0090(14) 0.0091(13) 0.0070(14) 
O2 0.0536(15) 0.112(2) 0.0795(19) 0.0433(17) 0.0176(13) 0.0317(15) 
C2 0.051(2) 0.0493(19) 0.0398(19) 0.0042(15) 0.0059(15) 0.0046(16) 
N3 0.0448(16) 0.0566(17) 0.0418(16) 0.0047(13) 0.0094(13) 0.0044(14) 
C3 0.057(2) 0.071(2) 0.053(2) 0.0105(19) 0.0067(18) 0.0099(19) 
N4 0.0496(17) 0.0622(18) 0.0439(17) 0.0081(14) 0.0082(13) 0.0069(14) 
C4 0.066(3) 0.075(3) 0.061(2) 0.023(2) 0.0089(19) 0.015(2) 
C5 0.076(3) 0.066(2) 0.055(2) 0.0249(19) 0.016(2) 0.008(2) 
C6 0.056(2) 0.051(2) 0.052(2) 0.0051(17) 0.0113(17) 0.0057(17) 
C7 0.052(2) 0.0474(19) 0.0352(18) 0.0014(15) 0.0063(15) 0.0012(16) 
C8 0.050(2) 0.047(2) 0.0391(18) 0.0001(15) 0.0053(15) 0.0008(16) 
C9 0.0461(19) 0.059(2) 0.046(2) 0.0084(17) 0.0108(16) 0.0050(16) 
C10 0.049(2) 0.065(2) 0.058(2) 0.0158(19) 0.0145(17) 0.0077(17) 
C11 0.066(3) 0.095(3) 0.086(3) 0.039(2) 0.030(2) 0.019(2) 
C12 0.064(3) 0.127(4) 0.124(4) 0.063(3) 0.051(3) 0.032(3) 
C13 0.0462(19) 0.059(2) 0.046(2) 0.0053(17) 0.0062(16) 0.0036(17) 
C14 0.044(2) 0.065(2) 0.055(2) 0.0104(18) 0.0115(16) 0.0058(17) 
C15 0.057(2) 0.083(3) 0.068(3) 0.023(2) 0.016(2) 0.014(2) 
C16 0.056(2) 0.120(4) 0.103(3) 0.051(3) 0.030(2) 0.028(2) 
C17 0.058(2) 0.094(3) 0.078(3) 0.028(2) 0.014(2) 0.024(2) 
C18 0.111(4) 0.095(4) 0.093(4) 0.013(3) 0.022(3) 0.009(3) 
C19 0.311(11) 0.164(7) 0.121(6) -0.024(5) -0.015(6) -0.045(7) 
C20 0.181(6) 0.108(5) 0.195(7) 0.028(5) 0.079(5) 0.058(5) 
C21 0.072(3) 0.105(4) 0.088(3) 0.019(3) 0.001(3) 0.012(3) 
C22 0.141(5) 0.141(6) 0.134(5) -0.005(4) 0.012(4) -0.037(4) 
C23 0.116(4) 0.146(5) 0.079(3) 0.001(3) 0.015(3) 0.008(4) 
C24 0.075(3) 0.087(3) 0.095(3) 0.047(3) 0.021(3) -0.002(2) 
C25 0.109(4) 0.158(6) 0.128(5) 0.058(4) 0.075(4) 0.027(4) 
C26 0.180(7) 0.236(9) 0.200(8) 0.082(7) 0.118(6) 0.042(6) 
C27 0.236(9) 0.149(6) 0.127(6) 0.033(5) 0.094(6) 0.059(6) 
C28 0.120(5) 0.114(5) 0.160(6) 0.050(5) -0.025(5) -0.041(4) 
C29 0.128(5) 0.259(10) 0.193(8) 0.082(8) -0.031(5) -0.033(6) 
C30 0.284(11) 0.123(6) 0.147(7) -0.039(5) -0.011(7) 0.002(6) 
O3 0.198(6) 0.274(8) 0.182(5) -0.053(5) 0.027(5) -0.074(6) 
O4 0.172(6) 0.403(13) 0.222(8) -0.179(9) 0.025(6) -0.032(8) 
C31 0.167(10) 0.171(9) 0.334(18) -0.123(10) -0.054(11) 0.000(8) 

_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 
N1 C9 1.363(4) . ? 
N1 C13 1.375(4) 3_656 ? 
O1 C6 1.348(4) . ? 
O1 C24 1.459(4) . ? 
C1 N4 1.324(4) . ? 
C1 N3 1.363(4) . ? 
C1 C2 1.448(4) . ? 
N2 C9 1.328(4) . ? 
N2 C8 1.330(4) . ? 
O2 C15 1.360(4) . ? 
O2 C17 1.439(4) . ? 
C2 C3 1.387(5) . ? 
C2 C7 1.394(4) . ? 
N3 C8 1.373(4) . ? 
C3 C4 1.386(5) . ? 
N4 C13 1.337(4) . ? 
C4 C5 1.378(5) . ? 
C5 C6 1.382(5) . ? 
C6 C7 1.411(4) . ? 
C7 C8 1.456(4) . ? 
C9 C10 1.438(4) . ? 
C10 C11 1.393(4) . ? 
C10 C14 1.399(4) 3_656 ? 
C11 C12 1.367(6) . ? 
C12 C16 1.389(6) 3_656 ? 
C13 N1 1.375(4) 3_656 ? 
C13 C14 1.443(4) . ? 
C14 C10 1.399(4) 3_656 ? 
C14 C15 1.405(5) . ? 
C15 C16 1.378(5) . ? 
C16 C12 1.389(6) 3_656 ? 
C17 C18 1.520(6) . ? 
C17 C21 1.525(6) . ? 
C18 C19 1.507(8) . ? 
C18 C20 1.509(7) . ? 
C21 C23 1.502(6) . ? 
C21 C22 1.523(7) . ? 
C24 C25 1.496(7) . ? 
C24 C28 1.519(8) . ? 
C25 C26 1.471(8) . ? 
C25 C27 1.523(9) . ? 
C28 C30 1.488(9) . ? 
C28 C29 1.532(8) . ? 
O3 C31 1.238(13) . ? 
O4 C31 1.59(2) . ? 
C31 C31 1.63(2) 3_666 ? 

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 
C9 N1 C13 108.8(3) . 3_656 ? 
C6 O1 C24 122.3(3) . . ? 
N4 C1 N3 128.6(3) . . ? 
N4 C1 C2 122.0(3) . . ? 
N3 C1 C2 109.5(3) . . ? 
C9 N2 C8 123.5(3) . . ? 
C15 O2 C17 123.1(3) . . ? 
C3 C2 C7 121.9(3) . . ? 
C3 C2 C1 131.3(3) . . ? 
C7 C2 C1 106.8(3) . . ? 
C1 N3 C8 108.4(3) . . ? 
C4 C3 C2 117.3(3) . . ? 
C1 N4 C13 123.7(3) . . ? 
C5 C4 C3 121.0(3) . . ? 
C4 C5 C6 122.9(3) . . ? 
O1 C6 C5 126.0(3) . . ? 
O1 C6 C7 117.5(3) . . ? 
C5 C6 C7 116.4(3) . . ? 
C2 C7 C6 120.5(3) . . ? 
C2 C7 C8 106.2(3) . . ? 
C6 C7 C8 133.3(3) . . ? 
N2 C8 N3 126.7(3) . . ? 
N2 C8 C7 124.2(3) . . ? 
N3 C8 C7 109.1(3) . . ? 
N2 C9 N1 128.6(3) . . ? 
N2 C9 C10 122.5(3) . . ? 
N1 C9 C10 108.9(3) . . ? 
C11 C10 C14 121.8(3) . 3_656 ? 
C11 C10 C9 131.0(3) . . ? 
C14 C10 C9 107.2(3) 3_656 . ? 
C12 C11 C10 116.7(4) . . ? 
C11 C12 C16 122.6(4) . 3_656 ? 
N4 C13 N1 126.2(3) . 3_656 ? 
N4 C13 C14 125.0(3) . . ? 
N1 C13 C14 108.9(3) 3_656 . ? 
C10 C14 C15 120.2(3) 3_656 . ? 
C10 C14 C13 106.2(3) 3_656 . ? 
C15 C14 C13 133.5(3) . . ? 
O2 C15 C16 126.1(3) . . ? 
O2 C15 C14 116.5(3) . . ? 
C16 C15 C14 117.3(3) . . ? 
C15 C16 C12 121.3(4) . 3_656 ? 
O2 C17 C18 108.1(4) . . ? 
O2 C17 C21 106.9(3) . . ? 
C18 C17 C21 116.2(4) . . ? 
C19 C18 C20 107.6(5) . . ? 
C19 C18 C17 111.3(5) . . ? 
C20 C18 C17 112.8(5) . . ? 
C23 C21 C22 111.0(5) . . ? 
C23 C21 C17 112.9(4) . . ? 
C22 C21 C17 110.4(4) . . ? 
O1 C24 C25 106.8(4) . . ? 
O1 C24 C28 106.1(4) . . ? 
C25 C24 C28 116.2(5) . . ? 
C26 C25 C24 117.7(6) . . ? 
C26 C25 C27 104.6(6) . . ? 
C24 C25 C27 108.6(5) . . ? 
C30 C28 C24 112.3(5) . . ? 
C30 C28 C29 113.3(7) . . ? 
C24 C28 C29 111.6(6) . . ? 
O3 C31 O4 125.3(13) . . ? 
O3 C31 C31 135(3) . 3_666 ? 
O4 C31 C31 89.4(14) . 3_666 ? 

_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              23.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.452 
_refine_diff_density_min   -0.233 
_refine_diff_density_rms    0.054