# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Fu, Zhiyong' 'Zhang, Jie' 'Zeng, Yu' 'Tan, Yi' 'Liao, Shijun' 'Chen, Hengjun' 'Dai, Jingcao' _publ_contact_author_name 'Fu, Zhiyong' _publ_contact_author_email zyfu@scut.edu.cn _publ_section_title ; Synthesis and Structure of a Mixed Crystal Containing Tris (4-pyridiniumyl)-1, 3, 5-triazine and Benzenetetracarboxylate Ions: Constructing New Photochromic Molecular System via Self-assembly ; data_1 _database_code_depnum_ccdc_archive 'CCDC 838462' #TrackingRef 'compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H27 N6 O17.50' _chemical_formula_weight 847.66 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 7.8884(16) _cell_length_b 9.6713(19) _cell_length_c 25.380(5) _cell_angle_alpha 82.76(3) _cell_angle_beta 89.58(2) _cell_angle_gamma 68.29(3) _cell_volume 1782.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3850 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 25.35 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.128 _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 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14374 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6412 _reflns_number_gt 3850 _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^)+(0.1122P)^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 6412 _refine_ls_number_parameters 586 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.051 _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 -0.1123(4) 0.4173(3) 0.17424(15) 0.0929(10) Uani 1 1 d . . . O2 O 0.1657(4) 0.3536(3) 0.14371(11) 0.0669(7) Uani 1 1 d D . . O3 O -0.2736(3) 0.1568(3) 0.02149(9) 0.0609(7) Uani 1 1 d . . . O4 O -0.1580(4) -0.0858(3) 0.02262(9) 0.0623(7) Uani 1 1 d . . . O5 O 0.0372(4) -0.3089(2) 0.07638(10) 0.0675(8) Uani 1 1 d . . . O6 O 0.1703(4) -0.3728(2) 0.15529(9) 0.0645(7) Uani 1 1 d . . . O7 O 0.3388(3) -0.0779(2) 0.25373(8) 0.0474(6) Uani 1 1 d . . . O8 O 0.1988(4) 0.1700(2) 0.24799(9) 0.0665(8) Uani 1 1 d . . . O9 O 0.5582(3) -0.2872(2) 0.36278(9) 0.0558(6) Uani 1 1 d . . . O10 O 0.5179(3) -0.0548(2) 0.32814(8) 0.0513(6) Uani 1 1 d . . . O11 O 0.6872(4) -0.4721(3) 0.48426(10) 0.0715(8) Uani 1 1 d . . . O12 O 0.8950(3) -0.4860(2) 0.42384(8) 0.0472(5) Uani 1 1 d . . . O13 O 0.8456(3) -0.1619(2) 0.60050(8) 0.0520(6) Uani 1 1 d . . . O14 O 0.8707(3) 0.0523(2) 0.57326(9) 0.0528(6) Uani 1 1 d . . . O15 O 0.7690(3) 0.23996(19) 0.49494(9) 0.0517(6) Uani 1 1 d . . . O16 O 0.5699(3) 0.29740(18) 0.42802(8) 0.0438(5) Uani 1 1 d . . . O17 O 0.1990(19) 0.4167(14) 0.0143(5) 0.383(8) Uani 1 1 d . . . H9 H 0.1346 0.4695 -0.0196 0.460 Uiso 1 1 d R . . H10 H 0.2493 0.4323 0.0415 0.460 Uiso 1 1 d R . . O18 O 0.541(3) -0.511(2) 0.0235(6) 0.249(7) Uiso 0.50 1 d P . . C1 C 0.5522(5) -0.2513(3) 0.09650(12) 0.0495(8) Uani 1 1 d . . . H1A H 0.5698 -0.3457 0.0874 0.059 Uiso 1 1 calc R . . C2 C 0.6358(4) -0.2392(3) 0.14157(11) 0.0427(7) Uani 1 1 d . . . H2A H 0.7093 -0.3250 0.1634 0.051 Uiso 1 1 calc R . . C3 C 0.4162(4) 0.0096(3) 0.07666(11) 0.0411(7) Uani 1 1 d . . . H3A H 0.3406 0.0931 0.0542 0.049 Uiso 1 1 calc R . . C4 C 0.4980(4) 0.0285(3) 0.12137(11) 0.0386(7) Uani 1 1 d . . . H4A H 0.4785 0.1243 0.1293 0.046 Uiso 1 1 calc R . . C5 C 0.6104(4) -0.0978(3) 0.15455(10) 0.0336(6) Uani 1 1 d . . . C6 C 0.7018(4) -0.0810(3) 0.20284(10) 0.0326(6) Uani 1 1 d . . . C7 C 0.7566(4) 0.0678(3) 0.25625(10) 0.0330(6) Uani 1 1 d . . . C8 C 0.9018(4) -0.1831(3) 0.27271(10) 0.0318(6) Uani 1 1 d . . . C9 C 0.7144(4) 0.2182(3) 0.27289(11) 0.0355(6) Uani 1 1 d . . . C10 C 0.5791(4) 0.3441(3) 0.24565(13) 0.0450(7) Uani 1 1 d . . . H10A H 0.5153 0.3356 0.2163 0.054 Uiso 1 1 calc R . . C11 C 0.5416(5) 0.4807(3) 0.26281(14) 0.0504(8) Uani 1 1 d . . . H11A H 0.4531 0.5661 0.2446 0.061 Uiso 1 1 calc R . . C12 C 0.8091(4) 0.2338(3) 0.31601(11) 0.0430(7) Uani 1 1 d . . . H12A H 0.9031 0.1512 0.3337 0.052 Uiso 1 1 calc R . . C13 C 0.7623(5) 0.3734(3) 0.33245(13) 0.0492(8) Uani 1 1 d . . . H13A H 0.8217 0.3851 0.3621 0.059 Uiso 1 1 calc R . . C14 C 1.0342(4) -0.3165(3) 0.30574(10) 0.0335(6) Uani 1 1 d . . . C15 C 1.0682(4) -0.4608(3) 0.29372(11) 0.0377(7) Uani 1 1 d . . . H15A H 1.0101 -0.4746 0.2642 0.045 Uiso 1 1 calc R . . C16 C 1.1879(4) -0.5825(3) 0.32574(11) 0.0409(7) Uani 1 1 d . . . H16A H 1.2113 -0.6795 0.3183 0.049 Uiso 1 1 calc R . . C17 C 1.1241(4) -0.2982(3) 0.34949(11) 0.0402(7) Uani 1 1 d . . . H17A H 1.1038 -0.2027 0.3580 0.048 Uiso 1 1 calc R . . C18 C 1.2436(4) -0.4232(3) 0.38004(12) 0.0445(7) Uani 1 1 d . . . H18A H 1.3058 -0.4126 0.4093 0.053 Uiso 1 1 calc R . . C19 C 0.1279(4) 0.0432(3) 0.18284(10) 0.0329(6) Uani 1 1 d . . . C20 C 0.1372(4) -0.0934(3) 0.16971(10) 0.0325(6) Uani 1 1 d . . . H20A H 0.2058 -0.1793 0.1923 0.039 Uiso 1 1 calc R . . C21 C 0.0513(4) -0.1113(3) 0.12498(11) 0.0337(6) Uani 1 1 d . . . C22 C -0.0566(4) 0.0206(3) 0.09126(11) 0.0376(6) Uani 1 1 d . . . C23 C -0.0660(4) 0.1588(3) 0.10465(11) 0.0410(7) Uani 1 1 d . . . H23A H -0.1374 0.2455 0.0828 0.049 Uiso 1 1 calc R . . C24 C 0.0256(4) 0.1739(3) 0.14890(11) 0.0389(7) Uani 1 1 d . . . C25 C 0.0149(5) 0.3275(3) 0.15783(13) 0.0521(9) Uani 1 1 d . . . C26 C -0.1692(4) 0.0315(3) 0.04213(11) 0.0424(7) Uani 1 1 d . . . C27 C 0.0888(5) -0.2746(3) 0.11852(12) 0.0443(7) Uani 1 1 d . . . C28 C 0.2272(4) 0.0505(3) 0.23196(11) 0.0382(7) Uani 1 1 d . . . C29 C 0.6500(4) -0.1384(3) 0.41433(10) 0.0290(6) Uani 1 1 d . . . C30 C 0.7357(4) -0.2536(3) 0.45558(10) 0.0299(6) Uani 1 1 d . . . C31 C 0.7894(4) -0.2188(3) 0.50211(10) 0.0299(6) Uani 1 1 d . . . H31A H 0.8419 -0.2959 0.5298 0.036 Uiso 1 1 calc R . . C32 C 0.7685(3) -0.0728(2) 0.50941(10) 0.0283(6) Uani 1 1 d . . . C33 C 0.6920(3) 0.0427(2) 0.46656(10) 0.0280(6) Uani 1 1 d . . . C34 C 0.6311(4) 0.0065(3) 0.42135(10) 0.0298(6) Uani 1 1 d . . . H34A H 0.5741 0.0836 0.3940 0.036 Uiso 1 1 calc R . . C35 C 0.5715(4) -0.1649(3) 0.36488(11) 0.0352(6) Uani 1 1 d . . . C36 C 0.7785(4) -0.4157(3) 0.45130(11) 0.0357(6) Uani 1 1 d . . . C37 C 0.8307(4) -0.0625(3) 0.56468(10) 0.0354(6) Uani 1 1 d . . . C38 C 0.6718(4) 0.2051(3) 0.46337(11) 0.0326(6) Uani 1 1 d . . . N1 N 0.4448(4) -0.1281(3) 0.06524(10) 0.0440(6) Uani 1 1 d . . . N2 N 0.6311(4) 0.4919(3) 0.30541(11) 0.0504(7) Uani 1 1 d . . . H2 H 0.606(6) 0.584(5) 0.3173(16) 0.078(12) Uiso 1 1 d . . . N3 N 1.2707(4) -0.5591(3) 0.36795(10) 0.0424(6) Uani 1 1 d . . . H3 H 1.358(5) -0.636(4) 0.3900(14) 0.066(10) Uiso 1 1 d . . . N4 N 0.8799(3) -0.0487(2) 0.28622(9) 0.0359(5) Uani 1 1 d . . . N5 N 0.8134(3) -0.2056(2) 0.23191(9) 0.0344(5) Uani 1 1 d . . . N6 N 0.6672(3) 0.0587(2) 0.21320(9) 0.0358(5) Uani 1 1 d . . . H1 H 0.382(6) -0.135(4) 0.0344(17) 0.080(12) Uiso 1 1 d . . . H4 H 0.151(12) 0.451(4) 0.143(4) 0.22(4) Uiso 1 1 d D . . H5 H -0.049(7) -0.200(6) 0.047(2) 0.106(15) Uiso 1 1 d . . . H6 H 0.421(6) -0.066(4) 0.2884(18) 0.087(12) Uiso 1 1 d . . . H7 H 0.719(7) -0.575(6) 0.482(2) 0.116(16) Uiso 1 1 d . . . H8 H 0.835(6) 0.126(5) 0.5436(19) 0.095(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.085(2) 0.0470(14) 0.149(3) -0.0327(16) 0.041(2) -0.0207(14) O2 0.0724(18) 0.0448(13) 0.0897(19) -0.0161(12) 0.0118(14) -0.0270(12) O3 0.0648(16) 0.0601(14) 0.0522(14) 0.0030(11) -0.0262(12) -0.0194(11) O4 0.0715(17) 0.0643(14) 0.0480(13) -0.0130(11) -0.0226(12) -0.0195(12) O5 0.101(2) 0.0465(12) 0.0562(15) -0.0175(11) -0.0211(14) -0.0246(12) O6 0.095(2) 0.0346(11) 0.0609(15) -0.0050(10) -0.0221(14) -0.0206(11) O7 0.0566(14) 0.0432(11) 0.0386(11) -0.0055(9) -0.0194(10) -0.0137(9) O8 0.099(2) 0.0443(12) 0.0508(14) -0.0157(10) -0.0268(13) -0.0169(12) O9 0.0760(17) 0.0324(10) 0.0572(14) -0.0129(9) -0.0242(12) -0.0154(10) O10 0.0735(16) 0.0528(12) 0.0334(11) 0.0051(9) -0.0205(11) -0.0332(11) O11 0.118(2) 0.0395(12) 0.0779(17) -0.0265(11) 0.0429(16) -0.0489(14) O12 0.0559(14) 0.0291(9) 0.0527(13) -0.0129(9) 0.0008(11) -0.0087(9) O13 0.0826(17) 0.0416(11) 0.0317(11) 0.0041(9) -0.0148(10) -0.0256(10) O14 0.0874(18) 0.0392(11) 0.0391(12) -0.0033(9) -0.0208(11) -0.0319(11) O15 0.0704(15) 0.0288(9) 0.0608(13) 0.0018(9) -0.0297(12) -0.0259(9) O16 0.0538(13) 0.0230(8) 0.0493(12) 0.0044(8) -0.0154(10) -0.0108(8) O17 0.453(18) 0.382(15) 0.339(14) -0.249(12) 0.015(13) -0.120(14) C1 0.059(2) 0.0407(15) 0.0481(18) -0.0133(13) -0.0121(16) -0.0146(14) C2 0.0496(19) 0.0341(13) 0.0382(16) -0.0071(12) -0.0135(14) -0.0074(12) C3 0.0399(17) 0.0484(16) 0.0310(15) 0.0011(12) -0.0100(13) -0.0136(13) C4 0.0391(17) 0.0354(14) 0.0357(15) -0.0029(11) -0.0026(13) -0.0078(12) C5 0.0308(15) 0.0372(13) 0.0295(14) -0.0085(11) -0.0020(11) -0.0075(11) C6 0.0354(15) 0.0301(12) 0.0294(14) -0.0068(10) -0.0001(11) -0.0077(11) C7 0.0361(16) 0.0311(13) 0.0292(14) -0.0051(10) -0.0004(12) -0.0092(11) C8 0.0368(16) 0.0323(13) 0.0255(13) -0.0061(10) -0.0012(11) -0.0110(11) C9 0.0412(17) 0.0342(13) 0.0328(14) -0.0090(11) 0.0021(12) -0.0145(11) C10 0.0502(19) 0.0336(14) 0.0478(17) -0.0087(12) -0.0029(14) -0.0105(12) C11 0.056(2) 0.0340(14) 0.059(2) -0.0106(13) -0.0006(16) -0.0122(13) C12 0.0528(19) 0.0418(15) 0.0375(16) -0.0106(12) -0.0017(14) -0.0193(13) C13 0.064(2) 0.0488(17) 0.0459(18) -0.0194(14) 0.0054(16) -0.0302(16) C14 0.0348(15) 0.0353(13) 0.0283(14) -0.0011(11) -0.0027(11) -0.0114(11) C15 0.0399(17) 0.0352(14) 0.0358(15) -0.0050(11) -0.0043(13) -0.0113(12) C16 0.0478(18) 0.0318(13) 0.0396(16) 0.0000(12) -0.0021(13) -0.0122(12) C17 0.0461(18) 0.0384(14) 0.0347(15) -0.0069(12) -0.0090(13) -0.0131(12) C18 0.0478(19) 0.0464(16) 0.0361(16) 0.0003(13) -0.0078(14) -0.0155(13) C19 0.0350(16) 0.0332(13) 0.0281(14) -0.0032(10) -0.0002(12) -0.0101(11) C20 0.0379(16) 0.0283(12) 0.0295(14) -0.0010(10) -0.0038(12) -0.0111(11) C21 0.0341(16) 0.0358(13) 0.0325(14) -0.0058(11) -0.0009(12) -0.0139(11) C22 0.0396(17) 0.0420(14) 0.0291(14) -0.0022(11) -0.0034(12) -0.0135(12) C23 0.0441(18) 0.0357(14) 0.0346(15) 0.0002(12) -0.0084(13) -0.0064(12) C24 0.0453(18) 0.0319(13) 0.0347(15) -0.0021(11) -0.0040(13) -0.0095(12) C25 0.066(2) 0.0303(15) 0.0515(19) -0.0040(13) -0.0007(17) -0.0090(15) C26 0.0421(18) 0.0508(17) 0.0330(15) -0.0020(13) -0.0062(13) -0.0168(14) C27 0.055(2) 0.0370(15) 0.0443(17) -0.0107(13) -0.0011(15) -0.0188(13) C28 0.0434(17) 0.0397(15) 0.0321(15) -0.0045(12) -0.0049(13) -0.0163(12) C29 0.0311(15) 0.0287(12) 0.0281(13) -0.0059(10) -0.0023(11) -0.0112(10) C30 0.0346(15) 0.0228(11) 0.0319(14) -0.0030(10) -0.0011(11) -0.0104(10) C31 0.0368(15) 0.0225(11) 0.0286(13) 0.0000(10) -0.0057(11) -0.0098(10) C32 0.0294(14) 0.0230(11) 0.0301(13) -0.0039(10) -0.0025(11) -0.0068(10) C33 0.0298(14) 0.0240(12) 0.0288(13) -0.0046(10) -0.0007(11) -0.0079(10) C34 0.0364(15) 0.0227(11) 0.0278(13) 0.0018(10) -0.0045(11) -0.0098(10) C35 0.0382(16) 0.0312(13) 0.0347(15) -0.0078(11) -0.0038(12) -0.0102(11) C36 0.0487(18) 0.0252(12) 0.0336(14) -0.0041(11) -0.0032(13) -0.0138(12) C37 0.0440(17) 0.0266(12) 0.0309(14) -0.0057(11) -0.0085(12) -0.0070(11) C38 0.0364(16) 0.0220(12) 0.0385(15) -0.0019(11) -0.0028(12) -0.0105(10) N1 0.0445(15) 0.0521(14) 0.0343(13) -0.0075(11) -0.0071(12) -0.0160(11) N2 0.0591(18) 0.0395(14) 0.0630(18) -0.0218(13) 0.0141(14) -0.0259(13) N3 0.0450(15) 0.0366(13) 0.0367(13) 0.0067(10) -0.0060(11) -0.0086(11) N4 0.0393(14) 0.0341(11) 0.0330(12) -0.0073(9) -0.0050(10) -0.0111(10) N5 0.0365(13) 0.0320(11) 0.0312(12) -0.0059(9) -0.0075(10) -0.0078(9) N6 0.0405(14) 0.0308(11) 0.0327(12) -0.0084(9) -0.0046(10) -0.0079(9) _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 C25 1.173(4) . ? O2 C25 1.341(4) . ? O3 C26 1.236(4) . ? O4 C26 1.267(4) . ? O5 C27 1.271(4) . ? O6 C27 1.233(3) . ? O7 C28 1.284(3) . ? O8 C28 1.216(3) . ? O9 C35 1.233(3) . ? O10 C35 1.267(3) . ? O11 C36 1.297(4) . ? O12 C36 1.200(4) . ? O13 C37 1.210(3) . ? O14 C37 1.304(3) . ? O15 C38 1.270(3) . ? O16 C38 1.235(3) . ? O18 O18 1.32(3) 2_645 ? C1 N1 1.339(4) . ? C1 C2 1.364(4) . ? C2 C5 1.389(4) . ? C3 N1 1.335(4) . ? C3 C4 1.374(4) . ? C4 C5 1.392(3) . ? C5 C6 1.483(4) . ? C6 N5 1.332(3) . ? C6 N6 1.336(3) . ? C7 N4 1.334(3) . ? C7 N6 1.334(3) . ? C7 C9 1.483(4) . ? C8 N5 1.336(3) . ? C8 N4 1.336(3) . ? C8 C14 1.484(3) . ? C9 C12 1.384(4) . ? C9 C10 1.392(4) . ? C10 C11 1.370(4) . ? C11 N2 1.333(4) . ? C12 C13 1.380(4) . ? C13 N2 1.338(4) . ? C14 C17 1.386(4) . ? C14 C15 1.393(4) . ? C15 C16 1.373(4) . ? C16 N3 1.344(4) . ? C17 C18 1.372(4) . ? C18 N3 1.327(4) . ? C19 C20 1.378(4) . ? C19 C24 1.404(4) . ? C19 C28 1.500(4) . ? C20 C21 1.388(4) . ? C21 C22 1.419(4) . ? C21 C27 1.526(4) . ? C22 C23 1.396(4) . ? C22 C26 1.506(4) . ? C23 C24 1.392(4) . ? C24 C25 1.502(4) . ? C29 C34 1.387(3) . ? C29 C30 1.398(3) . ? C29 C35 1.495(3) . ? C30 C31 1.379(3) . ? C30 C36 1.495(3) . ? C31 C32 1.396(3) . ? C32 C33 1.414(3) . ? C32 C37 1.516(3) . ? C33 C34 1.380(3) . ? C33 C38 1.510(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 N1 C1 C2 120.4(3) . . ? C1 C2 C5 119.5(2) . . ? N1 C3 C4 120.3(2) . . ? C3 C4 C5 119.1(2) . . ? C2 C5 C4 119.0(2) . . ? C2 C5 C6 120.7(2) . . ? C4 C5 C6 120.3(2) . . ? N5 C6 N6 125.3(2) . . ? N5 C6 C5 117.6(2) . . ? N6 C6 C5 117.1(2) . . ? N4 C7 N6 125.0(2) . . ? N4 C7 C9 117.0(2) . . ? N6 C7 C9 118.0(2) . . ? N5 C8 N4 124.8(2) . . ? N5 C8 C14 118.1(2) . . ? N4 C8 C14 117.1(2) . . ? C12 C9 C10 119.6(2) . . ? C12 C9 C7 120.0(2) . . ? C10 C9 C7 120.5(2) . . ? C11 C10 C9 118.8(3) . . ? N2 C11 C10 120.4(3) . . ? C13 C12 C9 119.1(3) . . ? N2 C13 C12 119.6(3) . . ? C17 C14 C15 119.3(2) . . ? C17 C14 C8 119.9(2) . . ? C15 C14 C8 120.8(2) . . ? C16 C15 C14 119.6(3) . . ? N3 C16 C15 118.9(2) . . ? C18 C17 C14 118.9(3) . . ? N3 C18 C17 120.2(3) . . ? C20 C19 C24 118.4(2) . . ? C20 C19 C28 120.3(2) . . ? C24 C19 C28 121.2(2) . . ? C19 C20 C21 124.4(2) . . ? C20 C21 C22 117.5(2) . . ? C20 C21 C27 114.1(2) . . ? C22 C21 C27 128.4(2) . . ? C23 C22 C21 118.0(2) . . ? C23 C22 C26 114.3(2) . . ? C21 C22 C26 127.7(2) . . ? C24 C23 C22 123.5(2) . . ? C23 C24 C19 118.1(2) . . ? C23 C24 C25 119.1(2) . . ? C19 C24 C25 122.8(2) . . ? O1 C25 O2 123.0(3) . . ? O1 C25 C24 124.3(4) . . ? O2 C25 C24 112.8(3) . . ? O3 C26 O4 120.7(3) . . ? O3 C26 C22 118.7(3) . . ? O4 C26 C22 120.5(3) . . ? O6 C27 O5 120.7(2) . . ? O6 C27 C21 118.3(2) . . ? O5 C27 C21 121.0(2) . . ? O8 C28 O7 125.7(3) . . ? O8 C28 C19 120.6(2) . . ? O7 C28 C19 113.7(2) . . ? C34 C29 C30 117.8(2) . . ? C34 C29 C35 119.6(2) . . ? C30 C29 C35 122.5(2) . . ? C31 C30 C29 119.4(2) . . ? C31 C30 C36 117.5(2) . . ? C29 C30 C36 123.1(2) . . ? C30 C31 C32 122.8(2) . . ? C31 C32 C33 118.0(2) . . ? C31 C32 C37 112.8(2) . . ? C33 C32 C37 129.2(2) . . ? C34 C33 C32 118.2(2) . . ? C34 C33 C38 114.4(2) . . ? C32 C33 C38 127.4(2) . . ? C33 C34 C29 123.7(2) . . ? O9 C35 O10 124.7(2) . . ? O9 C35 C29 119.5(2) . . ? O10 C35 C29 115.8(2) . . ? O12 C36 O11 125.0(2) . . ? O12 C36 C30 123.0(3) . . ? O11 C36 C30 111.6(3) . . ? O13 C37 O14 120.2(2) . . ? O13 C37 C32 119.8(2) . . ? O14 C37 C32 120.0(2) . . ? O16 C38 O15 122.3(2) . . ? O16 C38 C33 118.8(2) . . ? O15 C38 C33 118.7(2) . . ? C3 N1 C1 121.8(3) . . ? C11 N2 C13 122.4(3) . . ? C18 N3 C16 123.0(2) . . ? C7 N4 C8 115.1(2) . . ? C6 N5 C8 114.9(2) . . ? C7 N6 C6 114.7(2) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.599 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.066 # Attachment '- compound1b.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 850279' #TrackingRef '- compound1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H27 N6 O17.50' _chemical_formula_weight 847.66 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 7.8201(14) _cell_length_b 9.6697(18) _cell_length_c 25.351(5) _cell_angle_alpha 82.651(3) _cell_angle_beta 89.211(3) _cell_angle_gamma 68.329(3) _cell_volume 1765.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6358 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.129 _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 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13063 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6358 _reflns_number_gt 4677 _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^)+(0.0946P)^2^+1.1062P] 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 6358 _refine_ls_number_parameters 591 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.059 _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 -0.6130(3) 0.4185(3) 0.17636(11) 0.0572(7) Uani 1 1 d . . . O2 O -0.3311(3) 0.3567(2) 0.14462(9) 0.0424(5) Uani 1 1 d D . . O3 O -0.7721(3) 0.1610(2) 0.02158(8) 0.0371(5) Uani 1 1 d . . . O4 O -0.6566(3) -0.0831(2) 0.02290(8) 0.0377(5) Uani 1 1 d . . . O5 O -0.4647(3) -0.3073(2) 0.07718(8) 0.0412(5) Uani 1 1 d . . . O6 O -0.3288(3) -0.3714(2) 0.15622(8) 0.0405(5) Uani 1 1 d . . . O7 O -0.1589(3) -0.0788(2) 0.25444(7) 0.0300(4) Uani 1 1 d . . . O8 O -0.2972(3) 0.1710(2) 0.24849(8) 0.0386(5) Uani 1 1 d . . . O9 O 0.0568(3) -0.2886(2) 0.36374(7) 0.0320(5) Uani 1 1 d . . . O10 O 0.0216(3) -0.0562(2) 0.32832(7) 0.0310(5) Uani 1 1 d . . . O11 O 0.1880(3) -0.4737(2) 0.48562(8) 0.0399(5) Uani 1 1 d . . . O12 O 0.3971(2) -0.48689(19) 0.42330(7) 0.0273(4) Uani 1 1 d . . . O13 O 0.3447(3) -0.1627(2) 0.60123(7) 0.0322(5) Uani 1 1 d . . . O14 O 0.3705(3) 0.0529(2) 0.57386(8) 0.0319(5) Uani 1 1 d . . . O15 O 0.2692(3) 0.24080(19) 0.49517(8) 0.0318(5) Uani 1 1 d . . . O16 O 0.0710(2) 0.29696(18) 0.42774(7) 0.0262(4) Uani 1 1 d . . . O17 O -0.2952(11) 0.3971(7) 0.0223(2) 0.203(3) Uani 1 1 d D . . H9 H -0.4139 0.4167 0.0344 0.304 Uiso 1 1 d RD . . H10 H -0.2940 0.4813 -0.0015 0.304 Uiso 1 1 d R . . O18 O 0.0656(16) -0.5141(8) 0.0207(3) 0.135(4) Uani 0.50 1 d P . . C1 C 0.0516(4) -0.2512(3) 0.09554(11) 0.0304(6) Uani 1 1 d . . . H1A H 0.0684 -0.3454 0.0865 0.036 Uiso 1 1 calc R . . C2 C 0.1360(4) -0.2395(3) 0.14095(10) 0.0266(6) Uani 1 1 d . . . H2A H 0.2098 -0.3252 0.1628 0.032 Uiso 1 1 calc R . . C3 C -0.0832(3) 0.0114(3) 0.07572(10) 0.0255(6) Uani 1 1 d . . . H3A H -0.1581 0.0952 0.0532 0.031 Uiso 1 1 calc R . . C4 C -0.0017(3) 0.0291(3) 0.12056(10) 0.0237(6) Uani 1 1 d . . . H4A H -0.0207 0.1247 0.1286 0.028 Uiso 1 1 calc R . . C5 C 0.1096(3) -0.0970(3) 0.15396(10) 0.0213(5) Uani 1 1 d . . . C6 C 0.2010(3) -0.0803(3) 0.20247(10) 0.0205(5) Uani 1 1 d . . . C7 C 0.2572(3) 0.0675(3) 0.25578(9) 0.0210(5) Uani 1 1 d . . . C8 C 0.4015(3) -0.1826(3) 0.27194(9) 0.0198(5) Uani 1 1 d . . . C9 C 0.2147(3) 0.2192(3) 0.27211(10) 0.0230(5) Uani 1 1 d . . . C10 C 0.0782(4) 0.3449(3) 0.24524(11) 0.0278(6) Uani 1 1 d . . . H10A H 0.0141 0.3365 0.2159 0.033 Uiso 1 1 calc R . . C11 C 0.0392(4) 0.4824(3) 0.26264(11) 0.0306(6) Uani 1 1 d . . . H11A H -0.0505 0.5679 0.2448 0.037 Uiso 1 1 calc R . . C12 C 0.3092(4) 0.2348(3) 0.31559(10) 0.0256(6) Uani 1 1 d . . . H12A H 0.4029 0.1521 0.3334 0.031 Uiso 1 1 calc R . . C13 C 0.2624(4) 0.3740(3) 0.33192(11) 0.0297(6) Uani 1 1 d . . . H13A H 0.3227 0.3853 0.3615 0.036 Uiso 1 1 calc R . . C14 C 0.5342(3) -0.3167(3) 0.30512(9) 0.0210(5) Uani 1 1 d . . . C15 C 0.5677(3) -0.4613(3) 0.29314(10) 0.0226(5) Uani 1 1 d . . . H15A H 0.5096 -0.4751 0.2636 0.027 Uiso 1 1 calc R . . C16 C 0.6867(3) -0.5826(3) 0.32528(10) 0.0242(6) Uani 1 1 d . . . H16A H 0.7090 -0.6795 0.3180 0.029 Uiso 1 1 calc R . . C17 C 0.6255(4) -0.2985(3) 0.34879(10) 0.0244(6) Uani 1 1 d . . . H17A H 0.6064 -0.2031 0.3571 0.029 Uiso 1 1 calc R . . C18 C 0.7448(4) -0.4240(3) 0.37956(10) 0.0263(6) Uani 1 1 d . . . H18A H 0.8073 -0.4138 0.4089 0.032 Uiso 1 1 calc R . . C19 C -0.3708(3) 0.0451(3) 0.18305(9) 0.0212(5) Uani 1 1 d . . . C20 C -0.3606(3) -0.0921(3) 0.17033(9) 0.0205(5) Uani 1 1 d . . . H20A H -0.2919 -0.1779 0.1930 0.025 Uiso 1 1 calc R . . C21 C -0.4477(3) -0.1094(3) 0.12522(10) 0.0227(5) Uani 1 1 d . . . C22 C -0.5547(3) 0.0234(3) 0.09180(10) 0.0251(6) Uani 1 1 d . . . C23 C -0.5637(4) 0.1616(3) 0.10530(10) 0.0271(6) Uani 1 1 d . . . H23A H -0.6344 0.2485 0.0835 0.033 Uiso 1 1 calc R . . C24 C -0.4724(4) 0.1755(3) 0.14969(10) 0.0265(6) Uani 1 1 d . . . C25 C -0.4823(4) 0.3296(3) 0.15932(12) 0.0350(7) Uani 1 1 d . . . C26 C -0.6676(4) 0.0347(3) 0.04233(10) 0.0270(6) Uani 1 1 d . . . C27 C -0.4116(4) -0.2729(3) 0.11962(11) 0.0271(6) Uani 1 1 d . . . C28 C -0.2703(3) 0.0510(3) 0.23284(10) 0.0233(5) Uani 1 1 d . . . C29 C 0.1512(3) -0.1393(3) 0.41495(9) 0.0189(5) Uani 1 1 d . . . C30 C 0.2368(3) -0.2546(3) 0.45602(9) 0.0187(5) Uani 1 1 d . . . C31 C 0.2908(3) -0.2197(3) 0.50288(9) 0.0197(5) Uani 1 1 d . . . H31A H 0.3432 -0.2966 0.5306 0.024 Uiso 1 1 calc R . . C32 C 0.2695(3) -0.0733(3) 0.50989(9) 0.0184(5) Uani 1 1 d . . . C33 C 0.1926(3) 0.0420(3) 0.46708(9) 0.0177(5) Uani 1 1 d . . . C34 C 0.1326(3) 0.0056(3) 0.42133(9) 0.0183(5) Uani 1 1 d . . . H34A H 0.0775 0.0821 0.3937 0.022 Uiso 1 1 calc R . . C35 C 0.0718(3) -0.1657(3) 0.36545(10) 0.0208(5) Uani 1 1 d . . . C36 C 0.2804(4) -0.4171(3) 0.45190(10) 0.0220(5) Uani 1 1 d . . . C37 C 0.3314(3) -0.0627(3) 0.56554(10) 0.0210(5) Uani 1 1 d . . . C38 C 0.1721(3) 0.2053(3) 0.46326(10) 0.0206(5) Uani 1 1 d . . . N1 N -0.0548(3) -0.1274(3) 0.06423(9) 0.0263(5) Uani 1 1 d . . . N2 N 0.1308(3) 0.4927(3) 0.30540(9) 0.0302(5) Uani 1 1 d . . . N3 N 0.7708(3) -0.5603(2) 0.36734(9) 0.0253(5) Uani 1 1 d . . . N4 N 0.3814(3) -0.0482(2) 0.28543(8) 0.0224(5) Uani 1 1 d . . . N5 N 0.3123(3) -0.2054(2) 0.23156(8) 0.0219(5) Uani 1 1 d . . . N6 N 0.1666(3) 0.0594(2) 0.21274(8) 0.0220(5) Uani 1 1 d . . . H2 H 0.099(5) 0.592(4) 0.3195(16) 0.065(11) Uiso 1 1 d . . . H3 H 0.857(5) -0.637(4) 0.3901(13) 0.044(9) Uiso 1 1 d . . . H5 H -0.553(6) -0.200(5) 0.0515(17) 0.077(13) Uiso 1 1 d . . . H6 H -0.066(6) -0.065(5) 0.2925(19) 0.093(14) Uiso 1 1 d . . . H7 H 0.212(7) -0.575(6) 0.478(2) 0.113(18) Uiso 1 1 d . . . H8 H 0.340(5) 0.130(5) 0.5471(16) 0.066(12) Uiso 1 1 d . . . H1 H -0.113(4) -0.142(3) 0.0327(13) 0.041(8) Uiso 1 1 d . . . H4 H -0.353(7) 0.458(3) 0.148(2) 0.112(18) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0534(15) 0.0325(13) 0.0860(19) -0.0181(12) 0.0241(14) -0.0137(11) O2 0.0444(13) 0.0347(12) 0.0540(14) -0.0116(10) 0.0046(10) -0.0196(10) O3 0.0396(12) 0.0392(12) 0.0292(10) 0.0006(9) -0.0144(9) -0.0118(10) O4 0.0405(12) 0.0420(12) 0.0282(10) -0.0082(9) -0.0125(9) -0.0107(10) O5 0.0559(14) 0.0326(12) 0.0359(11) -0.0135(9) -0.0127(10) -0.0140(10) O6 0.0568(14) 0.0244(10) 0.0368(12) -0.0026(9) -0.0148(10) -0.0110(10) O7 0.0366(11) 0.0260(10) 0.0258(10) -0.0032(8) -0.0112(8) -0.0094(8) O8 0.0551(13) 0.0283(11) 0.0309(11) -0.0099(9) -0.0152(9) -0.0109(10) O9 0.0410(11) 0.0221(10) 0.0339(11) -0.0092(8) -0.0118(9) -0.0104(8) O10 0.0441(12) 0.0320(11) 0.0221(9) 0.0014(8) -0.0111(8) -0.0213(9) O11 0.0645(15) 0.0265(11) 0.0408(12) -0.0135(9) 0.0200(10) -0.0285(10) O12 0.0299(10) 0.0203(9) 0.0299(10) -0.0073(8) 0.0004(8) -0.0058(8) O13 0.0512(13) 0.0262(10) 0.0203(9) 0.0006(8) -0.0069(8) -0.0164(9) O14 0.0524(13) 0.0231(10) 0.0246(10) -0.0020(8) -0.0131(9) -0.0190(9) O15 0.0442(12) 0.0182(9) 0.0362(11) 0.0007(8) -0.0164(9) -0.0159(8) O16 0.0316(10) 0.0157(9) 0.0285(10) 0.0018(7) -0.0094(8) -0.0066(8) O17 0.330(9) 0.195(6) 0.125(4) -0.101(4) 0.019(5) -0.121(6) O18 0.265(13) 0.053(4) 0.075(5) -0.025(4) 0.036(6) -0.041(6) C1 0.0329(15) 0.0261(14) 0.0319(15) -0.0093(12) -0.0050(12) -0.0087(12) C2 0.0272(14) 0.0228(13) 0.0249(13) -0.0032(11) -0.0078(11) -0.0032(11) C3 0.0218(13) 0.0296(14) 0.0209(13) 0.0011(11) -0.0036(10) -0.0061(11) C4 0.0233(13) 0.0215(13) 0.0240(13) -0.0033(10) -0.0017(10) -0.0053(10) C5 0.0182(12) 0.0236(13) 0.0199(12) -0.0047(10) -0.0008(10) -0.0047(10) C6 0.0192(12) 0.0213(13) 0.0195(12) -0.0051(10) -0.0002(10) -0.0049(10) C7 0.0201(12) 0.0229(13) 0.0182(12) -0.0035(10) 0.0006(10) -0.0057(10) C8 0.0204(12) 0.0225(13) 0.0166(12) -0.0046(10) 0.0012(10) -0.0073(10) C9 0.0254(13) 0.0241(13) 0.0213(12) -0.0066(10) 0.0031(10) -0.0102(11) C10 0.0295(14) 0.0233(14) 0.0279(14) -0.0051(11) -0.0025(11) -0.0058(11) C11 0.0315(15) 0.0236(14) 0.0358(15) -0.0050(12) 0.0020(12) -0.0086(12) C12 0.0283(14) 0.0259(14) 0.0237(13) -0.0051(11) -0.0023(11) -0.0107(11) C13 0.0349(15) 0.0349(16) 0.0276(14) -0.0118(12) 0.0044(12) -0.0201(13) C14 0.0204(12) 0.0241(13) 0.0181(12) -0.0015(10) 0.0002(10) -0.0082(10) C15 0.0227(13) 0.0249(13) 0.0208(12) -0.0040(10) -0.0013(10) -0.0091(11) C16 0.0268(14) 0.0204(13) 0.0246(13) -0.0026(10) 0.0002(11) -0.0080(11) C17 0.0281(14) 0.0232(13) 0.0219(13) -0.0045(10) -0.0035(10) -0.0088(11) C18 0.0268(14) 0.0315(15) 0.0201(12) -0.0031(11) -0.0029(10) -0.0102(11) C19 0.0206(12) 0.0235(13) 0.0187(12) -0.0029(10) -0.0003(10) -0.0072(10) C20 0.0197(12) 0.0208(13) 0.0186(12) -0.0008(10) -0.0021(10) -0.0054(10) C21 0.0207(13) 0.0266(14) 0.0213(13) -0.0044(10) 0.0013(10) -0.0091(10) C22 0.0208(13) 0.0323(15) 0.0209(13) -0.0014(11) -0.0013(10) -0.0091(11) C23 0.0290(14) 0.0247(14) 0.0206(13) 0.0006(11) -0.0039(11) -0.0026(11) C24 0.0287(14) 0.0224(13) 0.0243(13) -0.0029(11) 0.0002(11) -0.0048(11) C25 0.0425(18) 0.0242(15) 0.0334(15) -0.0010(12) -0.0013(13) -0.0076(13) C26 0.0243(14) 0.0365(16) 0.0209(13) -0.0044(12) -0.0011(11) -0.0119(12) C27 0.0270(14) 0.0284(15) 0.0276(14) -0.0086(12) -0.0008(11) -0.0107(11) C28 0.0241(13) 0.0264(14) 0.0197(12) -0.0040(11) -0.0023(10) -0.0092(11) C29 0.0188(12) 0.0192(12) 0.0199(12) -0.0044(10) 0.0008(9) -0.0079(10) C30 0.0204(12) 0.0162(12) 0.0200(12) -0.0042(10) 0.0008(9) -0.0069(10) C31 0.0225(13) 0.0166(12) 0.0192(12) 0.0015(9) -0.0017(10) -0.0074(10) C32 0.0186(12) 0.0179(12) 0.0192(12) -0.0032(10) -0.0007(9) -0.0071(10) C33 0.0172(12) 0.0160(12) 0.0203(12) -0.0028(9) -0.0020(9) -0.0062(9) C34 0.0184(12) 0.0159(12) 0.0185(12) 0.0009(9) -0.0032(9) -0.0050(9) C35 0.0208(12) 0.0194(13) 0.0218(13) -0.0051(10) -0.0014(10) -0.0062(10) C36 0.0278(13) 0.0173(12) 0.0211(12) -0.0002(10) -0.0074(11) -0.0090(11) C37 0.0236(13) 0.0164(12) 0.0213(13) -0.0036(10) -0.0030(10) -0.0050(10) C38 0.0217(13) 0.0172(12) 0.0235(13) -0.0025(10) -0.0013(10) -0.0077(10) N1 0.0252(12) 0.0329(13) 0.0206(11) -0.0047(10) -0.0048(9) -0.0098(10) N2 0.0349(13) 0.0255(12) 0.0357(13) -0.0118(10) 0.0085(11) -0.0154(10) N3 0.0253(12) 0.0238(12) 0.0214(11) 0.0037(9) -0.0027(9) -0.0048(9) N4 0.0235(11) 0.0226(11) 0.0210(10) -0.0051(9) -0.0012(9) -0.0077(9) N5 0.0209(11) 0.0202(11) 0.0224(11) -0.0047(9) -0.0039(9) -0.0041(9) N6 0.0235(11) 0.0202(11) 0.0215(11) -0.0069(9) -0.0021(8) -0.0059(9) _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 C25 1.185(4) . ? O2 C25 1.340(4) . ? O3 C26 1.243(3) . ? O4 C26 1.272(3) . ? O5 C27 1.283(3) . ? O6 C27 1.234(3) . ? O7 C28 1.289(3) . ? O8 C28 1.218(3) . ? O9 C35 1.244(3) . ? O10 C35 1.268(3) . ? O11 C36 1.307(3) . ? O12 C36 1.211(3) . ? O13 C37 1.212(3) . ? O14 C37 1.305(3) . ? O15 C38 1.276(3) . ? O16 C38 1.233(3) . ? O18 O18 1.408(19) 2_545 ? C1 N1 1.339(3) . ? C1 C2 1.372(4) . ? C2 C5 1.398(4) . ? C3 N1 1.347(3) . ? C3 C4 1.371(4) . ? C4 C5 1.390(3) . ? C5 C6 1.486(3) . ? C6 N5 1.333(3) . ? C6 N6 1.336(3) . ? C7 N4 1.328(3) . ? C7 N6 1.335(3) . ? C7 C9 1.491(3) . ? C8 N5 1.332(3) . ? C8 N4 1.338(3) . ? C8 C14 1.489(3) . ? C9 C12 1.390(4) . ? C9 C10 1.390(4) . ? C10 C11 1.379(4) . ? C11 N2 1.342(4) . ? C12 C13 1.375(4) . ? C13 N2 1.334(4) . ? C14 C17 1.390(3) . ? C14 C15 1.398(3) . ? C15 C16 1.370(4) . ? C16 N3 1.341(3) . ? C17 C18 1.376(4) . ? C18 N3 1.333(3) . ? C19 C20 1.379(3) . ? C19 C24 1.393(4) . ? C19 C28 1.514(3) . ? C20 C21 1.398(3) . ? C21 C22 1.419(4) . ? C21 C27 1.525(4) . ? C22 C23 1.398(4) . ? C22 C26 1.513(4) . ? C23 C24 1.388(4) . ? C24 C25 1.515(4) . ? C29 C34 1.385(3) . ? C29 C30 1.395(3) . ? C29 C35 1.498(3) . ? C30 C31 1.387(3) . ? C30 C36 1.497(3) . ? C31 C32 1.397(3) . ? C32 C33 1.413(3) . ? C32 C37 1.526(3) . ? C33 C34 1.389(3) . ? C33 C38 1.518(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 N1 C1 C2 120.3(2) . . ? C1 C2 C5 119.1(2) . . ? N1 C3 C4 120.0(2) . . ? C3 C4 C5 119.5(2) . . ? C4 C5 C2 119.1(2) . . ? C4 C5 C6 120.4(2) . . ? C2 C5 C6 120.5(2) . . ? N5 C6 N6 125.5(2) . . ? N5 C6 C5 117.4(2) . . ? N6 C6 C5 117.0(2) . . ? N4 C7 N6 125.5(2) . . ? N4 C7 C9 117.2(2) . . ? N6 C7 C9 117.3(2) . . ? N5 C8 N4 125.3(2) . . ? N5 C8 C14 117.8(2) . . ? N4 C8 C14 116.9(2) . . ? C12 C9 C10 119.4(2) . . ? C12 C9 C7 119.7(2) . . ? C10 C9 C7 120.8(2) . . ? C11 C10 C9 119.0(2) . . ? N2 C11 C10 119.9(3) . . ? C13 C12 C9 119.2(2) . . ? N2 C13 C12 120.1(2) . . ? C17 C14 C15 119.3(2) . . ? C17 C14 C8 119.8(2) . . ? C15 C14 C8 120.8(2) . . ? C16 C15 C14 119.4(2) . . ? N3 C16 C15 119.4(2) . . ? C18 C17 C14 118.9(2) . . ? N3 C18 C17 120.0(2) . . ? C20 C19 C24 119.4(2) . . ? C20 C19 C28 119.3(2) . . ? C24 C19 C28 121.3(2) . . ? C19 C20 C21 123.6(2) . . ? C20 C21 C22 117.1(2) . . ? C20 C21 C27 113.4(2) . . ? C22 C21 C27 129.5(2) . . ? C23 C22 C21 118.5(2) . . ? C23 C22 C26 114.3(2) . . ? C21 C22 C26 127.1(2) . . ? C24 C23 C22 123.2(2) . . ? C23 C24 C19 118.1(2) . . ? C23 C24 C25 119.3(2) . . ? C19 C24 C25 122.6(2) . . ? O1 C25 O2 123.7(3) . . ? O1 C25 C24 123.2(3) . . ? O2 C25 C24 113.0(2) . . ? O3 C26 O4 121.0(2) . . ? O3 C26 C22 118.6(2) . . ? O4 C26 C22 120.3(2) . . ? O6 C27 O5 120.7(2) . . ? O6 C27 C21 119.0(2) . . ? O5 C27 C21 120.4(2) . . ? O8 C28 O7 126.3(2) . . ? O8 C28 C19 120.1(2) . . ? O7 C28 C19 113.6(2) . . ? C34 C29 C30 118.5(2) . . ? C34 C29 C35 119.0(2) . . ? C30 C29 C35 122.4(2) . . ? C31 C30 C29 119.3(2) . . ? C31 C30 C36 117.2(2) . . ? C29 C30 C36 123.5(2) . . ? C30 C31 C32 122.4(2) . . ? C31 C32 C33 118.2(2) . . ? C31 C32 C37 112.5(2) . . ? C33 C32 C37 129.2(2) . . ? C34 C33 C32 118.3(2) . . ? C34 C33 C38 113.7(2) . . ? C32 C33 C38 127.9(2) . . ? C29 C34 C33 123.1(2) . . ? O9 C35 O10 125.1(2) . . ? O9 C35 C29 119.2(2) . . ? O10 C35 C29 115.7(2) . . ? O12 C36 O11 125.5(2) . . ? O12 C36 C30 122.8(2) . . ? O11 C36 C30 111.5(2) . . ? O13 C37 O14 121.1(2) . . ? O13 C37 C32 119.3(2) . . ? O14 C37 C32 119.6(2) . . ? O16 C38 O15 122.4(2) . . ? O16 C38 C33 119.1(2) . . ? O15 C38 C33 118.4(2) . . ? C1 N1 C3 122.0(2) . . ? C13 N2 C11 122.4(2) . . ? C18 N3 C16 122.9(2) . . ? C7 N4 C8 114.6(2) . . ? C6 N5 C8 114.5(2) . . ? C7 N6 C6 114.3(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.920 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.065