# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _audit_creation_method 'SHELXL-97 plus manual editing' _journal_coden_Cambridge 440 loop_ _publ_author_name 'Klinowski, J.' 'Almeida, F. A.' 'Bond, Andrew D.' 'Khimyak, Yaroslav Z.' _publ_contact_author_name 'Prof Jacek Klinowski' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW U.K. ; _publ_requested_journal 'New Journal of Chemistry' _publ_contact_author_email jk18@cam.ac.uk _publ_contact_author_fax '(01223) 336362' _publ_contact_author_phone '(01223) 336509' _publ_section_title ; Synthesis and characterisation of a new layered compound of trimesic acid ; data_jk0101 _database_code_CSD 176116 _chemical_name_systematic ? _chemical_name_common ; trimesic acid, 1,2-bis(4-pyridyl)ethane, 4:1 co-crystal hydrate ; _chemical_melting_point ? _chemical_formula_moiety '(C9 H6 O6)4, C12 H12 N2, H2 O' _chemical_formula_sum 'C48 H38 N2 O25' _chemical_formula_weight 1042.80 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' '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' 'H' 'H' 0.0000 0.0000 '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 12.4048(8) _cell_length_b 12.9345(7) _cell_length_c 15.5773(10) _cell_angle_alpha 93.282(3) _cell_angle_beta 107.930(3) _cell_angle_gamma 106.375(3) _cell_volume 2252.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 11530 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 16999 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 24.97 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.974 _reflns_number_total 7712 _reflns_number_gt 4374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All hydrogens not bound to carbon were located from difference Fourier maps and refined with a single isotropic displacement parameter common to all of these hydrogens. O-H or N-H distance restraints were not applied, except for those hydrogens associated with the water molecule; the O-H distances in this case were restrained to 0.84(1)\%A. All hydrogens bound to carbon were placed geometrically and allowed to ride during subsequent refinement with an isotropic displacement parameter fixed at 1.2 times Ueq for the carbon to which they are attached. ; _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^)+(0.0728P)^2^+0.0983P] 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 7712 _refine_ls_number_parameters 710 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.770 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.069 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_1 O -0.4486(2) 0.96073(19) -0.87615(16) 0.0515(6) Uani 1 1 d . . . O2_1 O -0.6025(2) 0.82439(18) -0.87003(17) 0.0520(7) Uani 1 1 d . . . H2O_1 H -0.657(4) 0.849(3) -0.919(3) 0.108(5) Uiso 1 1 d . . . O3_1 O -0.55345(17) 0.54702(15) -0.67112(14) 0.0334(5) Uani 1 1 d . . . O4_1 O -0.36879(17) 0.56333(16) -0.58349(15) 0.0377(5) Uani 1 1 d . . . O5_1 O -0.02955(18) 0.87005(16) -0.55877(14) 0.0366(5) Uani 1 1 d . . . O6_1 O -0.04503(18) 0.99833(16) -0.64808(14) 0.0361(5) Uani 1 1 d . . . H6O_1 H 0.069(4) 1.040(3) -0.612(3) 0.108(5) Uiso 1 1 d . . . C1_1 C -0.4128(2) 0.8412(2) -0.76795(19) 0.0229(7) Uani 1 1 d . . . C2_1 C -0.4629(2) 0.7449(2) -0.73860(19) 0.0242(7) Uani 1 1 d . . . H2_1 H -0.5461 0.7074 -0.7652 0.029 Uiso 1 1 calc R . . C3_1 C -0.3923(2) 0.7033(2) -0.67076(19) 0.0230(7) Uani 1 1 d . . . C4_1 C -0.2715(2) 0.7597(2) -0.63174(19) 0.0246(7) Uani 1 1 d . . . H4_1 H -0.2228 0.7320 -0.5851 0.029 Uiso 1 1 calc R . . C5_1 C -0.2204(2) 0.8561(2) -0.65966(19) 0.0234(7) Uani 1 1 d . . . C6_1 C -0.2918(2) 0.8969(2) -0.72848(19) 0.0252(7) Uani 1 1 d . . . H6_1 H -0.2575 0.9626 -0.7481 0.030 Uiso 1 1 calc R . . C7_1 C -0.4882(3) 0.8825(2) -0.8435(2) 0.0324(8) Uani 1 1 d . . . C8_1 C -0.4440(3) 0.5970(2) -0.6402(2) 0.0267(7) Uani 1 1 d . . . C9_1 C -0.0903(3) 0.9115(2) -0.6190(2) 0.0270(7) Uani 1 1 d . . . O1_2 O -0.4066(2) -0.04434(19) -0.28140(16) 0.0516(6) Uani 1 1 d . . . O2_2 O -0.2472(2) 0.09158(19) -0.27645(18) 0.0501(7) Uani 1 1 d . . . H2O_2 H -0.199(4) 0.061(4) -0.233(3) 0.108(5) Uiso 1 1 d . . . O3_2 O -0.27047(18) 0.37775(16) -0.47011(15) 0.0384(6) Uani 1 1 d . . . O4_2 O -0.45288(18) 0.37874(17) -0.54934(15) 0.0401(6) Uani 1 1 d . . . H4O_2 H -0.416(4) 0.455(4) -0.575(3) 0.108(5) Uiso 1 1 d . . . O5_2 O -0.81129(19) 0.08215(17) -0.58130(15) 0.0409(6) Uani 1 1 d . . . O6_2 O -0.79822(18) -0.05352(17) -0.49980(15) 0.0388(5) Uani 1 1 d . . . H6O_2 H -0.909(4) -0.087(3) -0.528(3) 0.108(5) Uiso 1 1 d . . . C1_2 C -0.4314(2) 0.0897(2) -0.37699(19) 0.0241(7) Uani 1 1 d . . . C2_2 C -0.3755(2) 0.1848(2) -0.40422(19) 0.0246(7) Uani 1 1 d . . . H2_2 H -0.2917 0.2185 -0.3766 0.029 Uiso 1 1 calc R . . C3_2 C -0.4406(2) 0.2314(2) -0.47130(19) 0.0242(7) Uani 1 1 d . . . C4_2 C -0.5632(2) 0.1819(2) -0.51115(19) 0.0261(7) Uani 1 1 d . . . H4_2 H -0.6086 0.2133 -0.5568 0.031 Uiso 1 1 calc R . . C5_2 C -0.6196(2) 0.0865(2) -0.48438(19) 0.0237(7) Uani 1 1 d . . . C6_2 C -0.5539(2) 0.0404(2) -0.41724(19) 0.0256(7) Uani 1 1 d . . . H6_2 H -0.5927 -0.0246 -0.3990 0.031 Uiso 1 1 calc R . . C7_2 C -0.3629(3) 0.0378(2) -0.3065(2) 0.0289(7) Uani 1 1 d . . . C8_2 C -0.3789(3) 0.3359(2) -0.4969(2) 0.0271(7) Uani 1 1 d . . . C9_2 C -0.7511(3) 0.0359(2) -0.5253(2) 0.0276(7) Uani 1 1 d . . . O1_3 O -0.86783(19) 0.44139(18) -0.78471(15) 0.0460(6) Uani 1 1 d . . . O2_3 O -0.73208(19) 0.60167(18) -0.77113(17) 0.0466(6) Uani 1 1 d . . . H2O_3 H -0.678(4) 0.564(4) -0.736(3) 0.108(5) Uiso 1 1 d . . . O3_3 O -0.80182(19) 0.85746(17) -0.98251(16) 0.0461(6) Uani 1 1 d . . . O4_3 O -0.98973(17) 0.84696(16) -1.05861(14) 0.0356(5) Uani 1 1 d . . . O5_3 O -1.31949(18) 0.54334(16) -1.05929(15) 0.0393(6) Uani 1 1 d . . . O6_3 O -1.29492(18) 0.41362(17) -0.97376(15) 0.0374(6) Uani 1 1 d . . . H6O_3 H -1.385(4) 0.384(3) -1.002(3) 0.108(5) Uiso 1 1 d . . . C1_3 C -0.9253(2) 0.5755(2) -0.86970(19) 0.0228(7) Uani 1 1 d . . . C2_3 C -0.8818(3) 0.6717(2) -0.90216(19) 0.0266(7) Uani 1 1 d . . . H2_3 H -0.7987 0.7104 -0.8796 0.032 Uiso 1 1 calc R . . C3_3 C -0.9581(2) 0.7115(2) -0.96674(19) 0.0238(7) Uani 1 1 d . . . C4_3 C -1.0795(2) 0.6545(2) -0.99801(19) 0.0244(7) Uani 1 1 d . . . H4_3 H -1.1329 0.6815 -1.0416 0.029 Uiso 1 1 calc R . . C5_3 C -1.1243(2) 0.5586(2) -0.96657(19) 0.0240(7) Uani 1 1 d . . . C6_3 C -1.0464(2) 0.5188(2) -0.90218(18) 0.0252(7) Uani 1 1 d . . . H6_3 H -1.0763 0.4531 -0.8807 0.030 Uiso 1 1 calc R . . C7_3 C -0.8406(3) 0.5319(2) -0.8043(2) 0.0272(7) Uani 1 1 d . . . C8_3 C -0.9100(3) 0.8127(2) -1.0032(2) 0.0289(7) Uani 1 1 d . . . C9_3 C -1.2543(3) 0.5036(2) -1.0030(2) 0.0270(7) Uani 1 1 d . . . O1_4 O 0.0611(2) 0.4403(2) -0.36627(19) 0.0654(8) Uani 1 1 d . . . O2_4 O -0.09832(19) 0.32732(19) -0.34852(17) 0.0503(7) Uani 1 1 d . . . H2O_4 H -0.157(4) 0.353(3) -0.401(3) 0.108(5) Uiso 1 1 d . . . O3_4 O -0.07305(18) 0.02968(16) -0.16617(15) 0.0383(5) Uani 1 1 d . . . O4_4 O 0.10869(18) 0.02026(17) -0.09899(16) 0.0440(6) Uani 1 1 d . . . H4O_4 H 0.059(4) -0.058(4) -0.080(3) 0.108(5) Uiso 1 1 d . . . O5_4 O 0.46719(17) 0.33336(16) -0.04830(14) 0.0335(5) Uani 1 1 d . . . O6_4 O 0.45049(18) 0.46918(16) -0.12915(15) 0.0363(5) Uani 1 1 d . . . H6O_4 H 0.557(4) 0.504(3) -0.099(3) 0.108(5) Uiso 1 1 d . . . C1_4 C 0.0868(2) 0.3216(2) -0.25608(19) 0.0235(7) Uani 1 1 d . . . C2_4 C 0.0307(2) 0.2249(2) -0.23094(19) 0.0262(7) Uani 1 1 d . . . H2_4 H -0.0533 0.1921 -0.2579 0.031 Uiso 1 1 calc R . . C3_4 C 0.0966(2) 0.1757(2) -0.16667(19) 0.0223(6) Uani 1 1 d . . . C4_4 C 0.2195(2) 0.2262(2) -0.12542(19) 0.0247(7) Uani 1 1 d . . . H4_4 H 0.2652 0.1934 -0.0813 0.030 Uiso 1 1 calc R . . C5_4 C 0.2753(2) 0.3248(2) -0.14878(19) 0.0232(7) Uani 1 1 d . . . C6_4 C 0.2084(2) 0.3708(2) -0.21507(19) 0.0247(7) Uani 1 1 d . . . H6_4 H 0.2467 0.4368 -0.2324 0.030 Uiso 1 1 calc R . . C7_4 C 0.0166(3) 0.3703(2) -0.3287(2) 0.0293(7) Uani 1 1 d . . . C8_4 C 0.0369(3) 0.0686(2) -0.1432(2) 0.0278(7) Uani 1 1 d . . . C9_4 C 0.4063(2) 0.3769(2) -0.1043(2) 0.0243(7) Uani 1 1 d . . . N1_1 N 0.0526(3) 0.3124(2) 0.3490(2) 0.0433(7) Uani 1 1 d . . . H1N_1 H 0.143(4) 0.338(3) 0.363(3) 0.108(5) Uiso 1 1 d . . . N2_1 N -0.7499(3) 0.1585(3) 0.1284(2) 0.0685(10) Uani 1 1 d . . . H2N_1 H -0.830(4) 0.114(4) 0.112(3) 0.108(5) Uiso 1 1 d . . . C10_1 C -0.0188(3) 0.2472(3) 0.2702(3) 0.0471(9) Uani 1 1 d . . . H10_1 H 0.0157 0.2234 0.2293 0.057 Uiso 1 1 calc R . . C11_1 C -0.1393(3) 0.2145(3) 0.2474(3) 0.0462(9) Uani 1 1 d . . . H11_1 H -0.1883 0.1684 0.1911 0.055 Uiso 1 1 calc R . . C12_1 C -0.1910(3) 0.2484(3) 0.3067(2) 0.0378(8) Uani 1 1 d . . . C13_1 C -0.1158(3) 0.3143(3) 0.3882(2) 0.0431(9) Uani 1 1 d . . . H13_1 H -0.1481 0.3382 0.4306 0.052 Uiso 1 1 calc R . . C14_1 C 0.0065(3) 0.3454(3) 0.4081(2) 0.0470(9) Uani 1 1 d . . . H14_1 H 0.0580 0.3906 0.4643 0.056 Uiso 1 1 calc R . . C15_1 C -0.3241(3) 0.2175(3) 0.2815(2) 0.0429(9) Uani 1 1 d . . . H15A_1 H -0.3447 0.2235 0.3377 0.051 Uiso 1 1 calc R . . H15B_1 H -0.3609 0.1406 0.2509 0.051 Uiso 1 1 calc R . . C16_1 C -0.3754(3) 0.2916(3) 0.2173(3) 0.0568(11) Uani 1 1 d . . . H16A_1 H -0.3484 0.3668 0.2508 0.068 Uiso 1 1 calc R . . H16B_1 H -0.3455 0.2940 0.1652 0.068 Uiso 1 1 calc R . . C17_1 C -0.6893(4) 0.1150(3) 0.0897(3) 0.0573(11) Uani 1 1 d . . . H17_1 H -0.7298 0.0519 0.0443 0.069 Uiso 1 1 calc R . . C18_1 C -0.5686(3) 0.1598(3) 0.1143(2) 0.0463(9) Uani 1 1 d . . . H18_1 H -0.5256 0.1297 0.0844 0.056 Uiso 1 1 calc R . . C19_1 C -0.5087(3) 0.2490(2) 0.1828(2) 0.0373(8) Uani 1 1 d . . . C20_1 C -0.5760(3) 0.2922(3) 0.2190(3) 0.0508(10) Uani 1 1 d . . . H20_1 H -0.5383 0.3558 0.2641 0.061 Uiso 1 1 calc R . . C21_1 C -0.69568(16) 0.24638(16) 0.19195(14) 0.0688(12) Uani 1 1 d . . . H21_1 H -0.7412 0.2773 0.2186 0.083 Uiso 1 1 calc R . . O100_1 O 0.28766(16) 0.37147(16) 0.38758(14) 0.0458(6) Uani 1 1 d RD . . H100_1 H 0.3358 0.4217 0.3756 0.055 Uiso 1 1 d RD . . H101_1 H 0.3185 0.3798 0.4446 0.055 Uiso 1 1 d RD . . 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_1 0.0480(15) 0.0477(15) 0.0570(16) 0.0293(13) 0.0108(13) 0.0159(13) O2_1 0.0308(15) 0.0435(14) 0.0631(18) 0.0213(12) -0.0072(12) 0.0064(12) O3_1 0.0194(12) 0.0304(12) 0.0434(13) 0.0137(10) 0.0036(10) 0.0034(10) O4_1 0.0207(12) 0.0376(13) 0.0477(14) 0.0237(11) 0.0006(11) 0.0073(10) O5_1 0.0202(12) 0.0428(13) 0.0357(13) 0.0102(11) 0.0004(10) 0.0024(10) O6_1 0.0252(12) 0.0301(12) 0.0424(14) 0.0073(10) 0.0064(11) -0.0022(10) C1_1 0.0217(17) 0.0226(16) 0.0247(17) 0.0030(13) 0.0061(14) 0.0097(14) C2_1 0.0167(16) 0.0258(16) 0.0262(17) 0.0009(13) 0.0030(14) 0.0062(13) C3_1 0.0182(16) 0.0257(16) 0.0240(16) 0.0035(13) 0.0064(13) 0.0060(13) C4_1 0.0208(17) 0.0280(17) 0.0208(16) 0.0013(13) 0.0023(13) 0.0071(14) C5_1 0.0208(16) 0.0229(16) 0.0248(17) 0.0001(13) 0.0082(14) 0.0047(14) C6_1 0.0263(18) 0.0174(15) 0.0301(18) 0.0003(13) 0.0108(15) 0.0035(13) C7_1 0.032(2) 0.0263(18) 0.038(2) 0.0112(15) 0.0073(16) 0.0104(16) C8_1 0.0222(18) 0.0256(17) 0.0274(18) 0.0041(14) 0.0044(15) 0.0044(15) C9_1 0.0227(17) 0.0280(18) 0.0251(18) -0.0031(14) 0.0048(15) 0.0053(15) O1_2 0.0367(14) 0.0493(15) 0.0568(16) 0.0303(13) 0.0052(12) 0.0027(12) O2_2 0.0233(14) 0.0510(15) 0.0693(18) 0.0340(13) 0.0051(12) 0.0081(12) O3_2 0.0219(13) 0.0389(13) 0.0507(15) 0.0226(11) 0.0064(11) 0.0074(10) O4_2 0.0220(12) 0.0371(13) 0.0536(15) 0.0249(11) 0.0013(11) 0.0069(10) O5_2 0.0212(12) 0.0413(13) 0.0484(15) 0.0084(11) 0.0004(11) 0.0044(11) O6_2 0.0210(12) 0.0372(13) 0.0453(14) 0.0059(11) 0.0061(11) -0.0048(10) C1_2 0.0229(17) 0.0223(16) 0.0247(17) 0.0019(13) 0.0066(14) 0.0056(14) C2_2 0.0160(15) 0.0245(16) 0.0302(17) 0.0036(13) 0.0047(14) 0.0052(13) C3_2 0.0190(16) 0.0248(16) 0.0276(17) 0.0023(13) 0.0058(14) 0.0076(14) C4_2 0.0244(17) 0.0267(17) 0.0260(17) 0.0035(13) 0.0045(14) 0.0107(14) C5_2 0.0215(16) 0.0247(16) 0.0235(17) 0.0004(13) 0.0069(14) 0.0066(14) C6_2 0.0269(18) 0.0245(16) 0.0252(17) 0.0045(13) 0.0111(14) 0.0053(14) C7_2 0.0234(18) 0.0286(18) 0.0319(19) 0.0093(15) 0.0076(15) 0.0047(15) C8_2 0.0198(18) 0.0288(17) 0.0296(18) 0.0085(14) 0.0042(14) 0.0068(15) C9_2 0.0240(17) 0.0257(17) 0.0284(18) 0.0018(14) 0.0058(15) 0.0043(15) O1_3 0.0383(14) 0.0405(14) 0.0503(15) 0.0217(12) 0.0042(12) 0.0079(12) O2_3 0.0213(13) 0.0412(14) 0.0663(17) 0.0218(12) 0.0010(12) 0.0058(11) O3_3 0.0229(14) 0.0370(13) 0.0655(17) 0.0242(12) 0.0010(12) 0.0022(11) O4_3 0.0239(12) 0.0289(12) 0.0471(14) 0.0160(10) 0.0021(11) 0.0069(10) O5_3 0.0198(12) 0.0400(13) 0.0463(14) 0.0116(11) 0.0010(11) 0.0018(11) O6_3 0.0209(12) 0.0380(13) 0.0430(14) 0.0105(11) 0.0050(11) -0.0007(10) C1_3 0.0183(16) 0.0230(16) 0.0240(16) 0.0045(13) 0.0055(14) 0.0035(13) C2_3 0.0197(16) 0.0264(17) 0.0300(18) 0.0014(14) 0.0059(14) 0.0052(14) C3_3 0.0200(17) 0.0183(15) 0.0292(17) 0.0036(13) 0.0060(14) 0.0027(13) C4_3 0.0235(17) 0.0239(16) 0.0234(17) 0.0012(13) 0.0030(14) 0.0098(14) C5_3 0.0191(16) 0.0242(16) 0.0244(17) -0.0004(13) 0.0049(14) 0.0037(13) C6_3 0.0281(18) 0.0235(16) 0.0230(17) 0.0050(13) 0.0097(14) 0.0053(14) C7_3 0.0226(18) 0.0272(18) 0.0286(18) 0.0068(14) 0.0060(15) 0.0057(15) C8_3 0.0238(19) 0.0232(16) 0.0324(19) 0.0055(14) 0.0023(15) 0.0039(15) C9_3 0.0267(18) 0.0264(17) 0.0233(17) 0.0013(14) 0.0048(15) 0.0059(15) O1_4 0.0341(15) 0.0697(18) 0.086(2) 0.0514(16) 0.0100(15) 0.0105(13) O2_4 0.0189(13) 0.0588(15) 0.0642(17) 0.0360(13) 0.0026(12) 0.0060(11) O3_4 0.0195(13) 0.0381(13) 0.0497(14) 0.0211(11) 0.0038(11) 0.0035(10) O4_4 0.0210(12) 0.0382(13) 0.0627(16) 0.0280(12) 0.0011(11) 0.0047(11) O5_4 0.0206(11) 0.0359(12) 0.0353(13) 0.0062(10) 0.0026(10) 0.0033(10) O6_4 0.0219(12) 0.0270(12) 0.0497(15) 0.0080(10) 0.0039(11) 0.0005(10) C1_4 0.0196(17) 0.0225(16) 0.0276(17) 0.0045(13) 0.0076(14) 0.0057(13) C2_4 0.0177(16) 0.0283(17) 0.0286(17) 0.0017(14) 0.0049(14) 0.0050(14) C3_4 0.0198(16) 0.0206(15) 0.0219(16) 0.0024(13) 0.0035(13) 0.0036(13) C4_4 0.0185(17) 0.0276(17) 0.0240(17) 0.0019(13) 0.0018(14) 0.0075(14) C5_4 0.0188(16) 0.0212(16) 0.0262(17) -0.0018(13) 0.0078(14) 0.0019(13) C6_4 0.0243(17) 0.0208(15) 0.0292(17) 0.0040(13) 0.0103(14) 0.0061(14) C7_4 0.0218(19) 0.0247(17) 0.0387(19) 0.0117(15) 0.0075(15) 0.0048(14) C8_4 0.0189(18) 0.0290(17) 0.0288(18) 0.0089(14) 0.0011(14) 0.0045(15) C9_4 0.0196(17) 0.0255(17) 0.0256(17) -0.0006(14) 0.0073(14) 0.0050(14) N1_1 0.0289(16) 0.0498(18) 0.051(2) 0.0170(16) 0.0124(16) 0.0113(15) N2_1 0.0285(19) 0.092(3) 0.060(2) 0.011(2) 0.0037(19) -0.006(2) C10_1 0.038(2) 0.053(2) 0.051(2) 0.0077(19) 0.018(2) 0.0117(19) C11_1 0.037(2) 0.047(2) 0.052(2) 0.0088(18) 0.0149(19) 0.0089(18) C12_1 0.0280(19) 0.0381(19) 0.046(2) 0.0169(17) 0.0106(18) 0.0091(16) C13_1 0.030(2) 0.050(2) 0.048(2) 0.0097(18) 0.0125(18) 0.0122(17) C14_1 0.036(2) 0.052(2) 0.045(2) 0.0079(18) 0.0048(19) 0.0106(18) C15_1 0.0283(19) 0.041(2) 0.057(2) 0.0162(17) 0.0135(18) 0.0068(16) C16_1 0.034(2) 0.052(2) 0.082(3) 0.034(2) 0.014(2) 0.0116(18) C17_1 0.065(3) 0.037(2) 0.041(2) 0.0119(18) -0.011(2) 0.002(2) C18_1 0.055(3) 0.045(2) 0.043(2) 0.0192(18) 0.012(2) 0.024(2) C19_1 0.0284(19) 0.0297(18) 0.050(2) 0.0215(17) 0.0081(17) 0.0064(16) C20_1 0.036(2) 0.050(2) 0.054(2) -0.0008(18) -0.0005(19) 0.0126(19) C21_1 0.039(3) 0.111(4) 0.052(3) -0.003(3) 0.009(2) 0.026(3) O100_1 0.0279(13) 0.0486(14) 0.0546(15) 0.0191(12) 0.0057(12) 0.0096(11) _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_1 C7_1 1.206(3) . ? O2_1 C7_1 1.323(4) . ? O2_1 H2O_1 0.98(5) . ? O3_1 C8_1 1.249(3) . ? O4_1 C8_1 1.267(3) . ? O4_1 H4O_2 1.39(5) . ? O5_1 C9_1 1.259(3) . ? O6_1 C9_1 1.281(3) . ? O6_1 H6O_1 1.28(5) . ? C1_1 C6_1 1.386(4) . ? C1_1 C2_1 1.397(4) . ? C1_1 C7_1 1.491(4) . ? C2_1 C3_1 1.391(4) . ? C2_1 H2_1 0.9500 . ? C3_1 C4_1 1.385(4) . ? C3_1 C8_1 1.515(4) . ? C4_1 C5_1 1.391(4) . ? C4_1 H4_1 0.9500 . ? C5_1 C6_1 1.399(4) . ? C5_1 C9_1 1.478(4) . ? C6_1 H6_1 0.9500 . ? O1_2 C7_2 1.195(3) . ? O2_2 C7_2 1.322(4) . ? O2_2 H2O_2 0.94(5) . ? O3_2 C8_2 1.223(3) . ? O4_2 C8_2 1.300(3) . ? O4_2 H4O_2 1.12(5) . ? O5_2 C9_2 1.260(3) . ? O6_2 C9_2 1.285(3) . ? O6_2 H6O_2 1.24(5) . ? C1_2 C6_2 1.389(4) . ? C1_2 C2_2 1.392(4) . ? C1_2 C7_2 1.487(4) . ? C2_2 C3_2 1.390(4) . ? C2_2 H2_2 0.9500 . ? C3_2 C4_2 1.390(4) . ? C3_2 C8_2 1.497(4) . ? C4_2 C5_2 1.392(4) . ? C4_2 H4_2 0.9500 . ? C5_2 C6_2 1.391(4) . ? C5_2 C9_2 1.485(4) . ? C6_2 H6_2 0.9500 . ? O1_3 C7_3 1.208(3) . ? O2_3 C7_3 1.314(3) . ? O2_3 H2O_3 0.99(5) . ? O3_3 C8_3 1.230(3) . ? O4_3 C8_3 1.298(3) . ? O5_3 C9_3 1.240(3) . ? O6_3 C9_3 1.299(3) . ? O6_3 H6O_3 1.01(5) . ? C1_3 C6_3 1.385(4) . ? C1_3 C2_3 1.399(4) . ? C1_3 C7_3 1.484(4) . ? C2_3 C3_3 1.385(4) . ? C2_3 H2_3 0.9500 . ? C3_3 C4_3 1.390(4) . ? C3_3 C8_3 1.499(4) . ? C4_3 C5_3 1.391(4) . ? C4_3 H4_3 0.9500 . ? C5_3 C6_3 1.395(4) . ? C5_3 C9_3 1.473(4) . ? C6_3 H6_3 0.9500 . ? O1_4 C7_4 1.202(3) . ? O2_4 C7_4 1.304(3) . ? O2_4 H2O_4 1.05(5) . ? O3_4 C8_4 1.238(3) . ? O4_4 C8_4 1.283(3) . ? O4_4 H4O_4 1.13(5) . ? O5_4 C9_4 1.240(3) . ? O6_4 C9_4 1.301(3) . ? O6_4 H6O_4 1.19(5) . ? C1_4 C6_4 1.381(4) . ? C1_4 C2_4 1.391(4) . ? C1_4 C7_4 1.490(4) . ? C2_4 C3_4 1.392(4) . ? C2_4 H2_4 0.9500 . ? C3_4 C4_4 1.397(4) . ? C3_4 C8_4 1.499(4) . ? C4_4 C5_4 1.395(4) . ? C4_4 H4_4 0.9500 . ? C5_4 C6_4 1.389(4) . ? C5_4 C9_4 1.487(4) . ? C6_4 H6_4 0.9500 . ? N1_1 C14_1 1.331(4) . ? N1_1 C10_1 1.340(4) . ? N1_1 H1N_1 1.03(4) . ? N2_1 C17_1 1.312(5) . ? N2_1 C21_1 1.325(4) . ? N2_1 H2N_1 0.95(5) . ? C10_1 C11_1 1.356(4) . ? C10_1 H10_1 0.9500 . ? C11_1 C12_1 1.390(4) . ? C11_1 H11_1 0.9500 . ? C12_1 C13_1 1.381(4) . ? C12_1 C15_1 1.500(4) . ? C13_1 C14_1 1.382(4) . ? C13_1 H13_1 0.9500 . ? C14_1 H14_1 0.9500 . ? C15_1 C16_1 1.544(5) . ? C15_1 H15A_1 0.9900 . ? C15_1 H15B_1 0.9900 . ? C16_1 C19_1 1.495(4) . ? C16_1 H16A_1 0.9900 . ? C16_1 H16B_1 0.9900 . ? C17_1 C18_1 1.363(5) . ? C17_1 H17_1 0.9500 . ? C18_1 C19_1 1.381(4) . ? C18_1 H18_1 0.9500 . ? C19_1 C20_1 1.358(4) . ? C20_1 C21_1 1.350(4) . ? C20_1 H20_1 0.9500 . ? C21_1 H21_1 0.9500 . ? O100_1 H100_1 0.8230 . ? O100_1 H101_1 0.8385 . ? 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 C7_1 O2_1 H2O_1 117(3) . . ? C8_1 O4_1 H4O_2 112.3(17) . . ? C9_1 O6_1 H6O_1 115(2) . . ? C6_1 C1_1 C2_1 119.9(3) . . ? C6_1 C1_1 C7_1 119.9(3) . . ? C2_1 C1_1 C7_1 120.2(3) . . ? C3_1 C2_1 C1_1 120.6(3) . . ? C3_1 C2_1 H2_1 119.7 . . ? C1_1 C2_1 H2_1 119.7 . . ? C4_1 C3_1 C2_1 119.0(3) . . ? C4_1 C3_1 C8_1 119.5(3) . . ? C2_1 C3_1 C8_1 121.5(3) . . ? C3_1 C4_1 C5_1 121.1(3) . . ? C3_1 C4_1 H4_1 119.4 . . ? C5_1 C4_1 H4_1 119.4 . . ? C4_1 C5_1 C6_1 119.5(3) . . ? C4_1 C5_1 C9_1 119.5(3) . . ? C6_1 C5_1 C9_1 120.9(3) . . ? C1_1 C6_1 C5_1 119.8(3) . . ? C1_1 C6_1 H6_1 120.1 . . ? C5_1 C6_1 H6_1 120.1 . . ? O1_1 C7_1 O2_1 124.2(3) . . ? O1_1 C7_1 C1_1 123.3(3) . . ? O2_1 C7_1 C1_1 112.5(3) . . ? O3_1 C8_1 O4_1 123.8(3) . . ? O3_1 C8_1 C3_1 120.9(3) . . ? O4_1 C8_1 C3_1 115.4(3) . . ? O5_1 C9_1 O6_1 123.4(3) . . ? O5_1 C9_1 C5_1 118.4(3) . . ? O6_1 C9_1 C5_1 118.1(3) . . ? C7_2 O2_2 H2O_2 116(3) . . ? C8_2 O4_2 H4O_2 119(2) . . ? C9_2 O6_2 H6O_2 116(2) . . ? C6_2 C1_2 C2_2 119.7(3) . . ? C6_2 C1_2 C7_2 118.8(3) . . ? C2_2 C1_2 C7_2 121.5(3) . . ? C3_2 C2_2 C1_2 120.8(3) . . ? C3_2 C2_2 H2_2 119.6 . . ? C1_2 C2_2 H2_2 119.6 . . ? C4_2 C3_2 C2_2 119.3(3) . . ? C4_2 C3_2 C8_2 121.0(3) . . ? C2_2 C3_2 C8_2 119.8(3) . . ? C3_2 C4_2 C5_2 120.1(3) . . ? C3_2 C4_2 H4_2 119.9 . . ? C5_2 C4_2 H4_2 119.9 . . ? C6_2 C5_2 C4_2 120.3(3) . . ? C6_2 C5_2 C9_2 119.8(3) . . ? C4_2 C5_2 C9_2 119.9(3) . . ? C1_2 C6_2 C5_2 119.8(3) . . ? C1_2 C6_2 H6_2 120.1 . . ? C5_2 C6_2 H6_2 120.1 . . ? O1_2 C7_2 O2_2 123.8(3) . . ? O1_2 C7_2 C1_2 124.1(3) . . ? O2_2 C7_2 C1_2 112.1(3) . . ? O3_2 C8_2 O4_2 123.5(3) . . ? O3_2 C8_2 C3_2 123.5(3) . . ? O4_2 C8_2 C3_2 112.9(3) . . ? O5_2 C9_2 O6_2 123.1(3) . . ? O5_2 C9_2 C5_2 119.6(3) . . ? O6_2 C9_2 C5_2 117.3(3) . . ? C7_3 O2_3 H2O_3 108(3) . . ? C8_3 O4_3 H4O_4 111.5(18) . . ? C9_3 O6_3 H6O_3 110(3) . . ? C6_3 C1_3 C2_3 119.8(3) . . ? C6_3 C1_3 C7_3 120.4(3) . . ? C2_3 C1_3 C7_3 119.7(3) . . ? C3_3 C2_3 C1_3 121.0(3) . . ? C3_3 C2_3 H2_3 119.5 . . ? C1_3 C2_3 H2_3 119.5 . . ? C2_3 C3_3 C4_3 118.6(3) . . ? C2_3 C3_3 C8_3 120.5(3) . . ? C4_3 C3_3 C8_3 120.9(3) . . ? C3_3 C4_3 C5_3 121.2(3) . . ? C3_3 C4_3 H4_3 119.4 . . ? C5_3 C4_3 H4_3 119.4 . . ? C4_3 C5_3 C6_3 119.7(3) . . ? C4_3 C5_3 C9_3 117.6(3) . . ? C6_3 C5_3 C9_3 122.7(3) . . ? C1_3 C6_3 C5_3 119.7(3) . . ? C1_3 C6_3 H6_3 120.1 . . ? C5_3 C6_3 H6_3 120.1 . . ? O1_3 C7_3 O2_3 123.6(3) . . ? O1_3 C7_3 C1_3 123.7(3) . . ? O2_3 C7_3 C1_3 112.7(3) . . ? O3_3 C8_3 O4_3 123.5(3) . . ? O3_3 C8_3 C3_3 121.1(3) . . ? O4_3 C8_3 C3_3 115.4(3) . . ? O5_3 C9_3 O6_3 123.0(3) . . ? O5_3 C9_3 C5_3 119.9(3) . . ? O6_3 C9_3 C5_3 117.1(3) . . ? C7_4 O2_4 H2O_4 119(2) . . ? C9_4 O6_4 H6O_4 114(2) . . ? C6_4 C1_4 C2_4 119.7(3) . . ? C6_4 C1_4 C7_4 120.1(3) . . ? C2_4 C1_4 C7_4 120.2(3) . . ? C1_4 C2_4 C3_4 120.5(3) . . ? C1_4 C2_4 H2_4 119.7 . . ? C3_4 C2_4 H2_4 119.7 . . ? C2_4 C3_4 C4_4 119.3(3) . . ? C2_4 C3_4 C8_4 120.4(3) . . ? C4_4 C3_4 C8_4 120.3(2) . . ? C5_4 C4_4 C3_4 120.2(3) . . ? C5_4 C4_4 H4_4 119.9 . . ? C3_4 C4_4 H4_4 119.9 . . ? C6_4 C5_4 C4_4 119.6(3) . . ? C6_4 C5_4 C9_4 121.1(3) . . ? C4_4 C5_4 C9_4 119.2(3) . . ? C1_4 C6_4 C5_4 120.6(3) . . ? C1_4 C6_4 H6_4 119.7 . . ? C5_4 C6_4 H6_4 119.7 . . ? O1_4 C7_4 O2_4 123.6(3) . . ? O1_4 C7_4 C1_4 123.7(3) . . ? O2_4 C7_4 C1_4 112.8(3) . . ? O3_4 C8_4 O4_4 123.0(3) . . ? O3_4 C8_4 C3_4 122.4(2) . . ? O4_4 C8_4 C3_4 114.6(3) . . ? O5_4 C9_4 O6_4 123.6(3) . . ? O5_4 C9_4 C5_4 121.3(3) . . ? O6_4 C9_4 C5_4 115.1(3) . . ? C14_1 N1_1 C10_1 120.5(3) . . ? C14_1 N1_1 H1N_1 120(2) . . ? C10_1 N1_1 H1N_1 120(2) . . ? C17_1 N2_1 C21_1 121.1(3) . . ? C17_1 N2_1 H2N_1 112(3) . . ? C21_1 N2_1 H2N_1 126(3) . . ? N1_1 C10_1 C11_1 121.4(3) . . ? N1_1 C10_1 H10_1 119.3 . . ? C11_1 C10_1 H10_1 119.3 . . ? C10_1 C11_1 C12_1 120.0(3) . . ? C10_1 C11_1 H11_1 120.0 . . ? C12_1 C11_1 H11_1 120.0 . . ? C13_1 C12_1 C11_1 117.7(3) . . ? C13_1 C12_1 C15_1 121.1(3) . . ? C11_1 C12_1 C15_1 121.1(3) . . ? C12_1 C13_1 C14_1 120.1(3) . . ? C12_1 C13_1 H13_1 119.9 . . ? C14_1 C13_1 H13_1 119.9 . . ? N1_1 C14_1 C13_1 120.3(3) . . ? N1_1 C14_1 H14_1 119.8 . . ? C13_1 C14_1 H14_1 119.8 . . ? C12_1 C15_1 C16_1 111.4(3) . . ? C12_1 C15_1 H15A_1 109.3 . . ? C16_1 C15_1 H15A_1 109.3 . . ? C12_1 C15_1 H15B_1 109.3 . . ? C16_1 C15_1 H15B_1 109.3 . . ? H15A_1 C15_1 H15B_1 108.0 . . ? C19_1 C16_1 C15_1 110.1(3) . . ? C19_1 C16_1 H16A_1 109.6 . . ? C15_1 C16_1 H16A_1 109.6 . . ? C19_1 C16_1 H16B_1 109.6 . . ? C15_1 C16_1 H16B_1 109.6 . . ? H16A_1 C16_1 H16B_1 108.1 . . ? N2_1 C17_1 C18_1 120.4(4) . . ? N2_1 C17_1 H17_1 119.8 . . ? C18_1 C17_1 H17_1 119.8 . . ? C17_1 C18_1 C19_1 120.0(3) . . ? C17_1 C18_1 H18_1 120.0 . . ? C19_1 C18_1 H18_1 120.0 . . ? C20_1 C19_1 C18_1 117.1(3) . . ? C20_1 C19_1 C16_1 122.3(3) . . ? C18_1 C19_1 C16_1 120.5(3) . . ? C21_1 C20_1 C19_1 121.1(3) . . ? C21_1 C20_1 H20_1 119.5 . . ? C19_1 C20_1 H20_1 119.5 . . ? N2_1 C21_1 C20_1 120.2(3) . . ? N2_1 C21_1 H21_1 119.9 . . ? C20_1 C21_1 H21_1 119.9 . . ? H100_1 O100_1 H101_1 100.7 . . ? 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 C6_1 C1_1 C2_1 C3_1 -0.8(4) . . . . ? C7_1 C1_1 C2_1 C3_1 177.3(2) . . . . ? C1_1 C2_1 C3_1 C4_1 0.9(4) . . . . ? C1_1 C2_1 C3_1 C8_1 -177.9(2) . . . . ? C2_1 C3_1 C4_1 C5_1 -0.4(4) . . . . ? C8_1 C3_1 C4_1 C5_1 178.4(2) . . . . ? C3_1 C4_1 C5_1 C6_1 -0.2(4) . . . . ? C3_1 C4_1 C5_1 C9_1 -177.5(2) . . . . ? C2_1 C1_1 C6_1 C5_1 0.2(4) . . . . ? C7_1 C1_1 C6_1 C5_1 -177.9(2) . . . . ? C4_1 C5_1 C6_1 C1_1 0.2(4) . . . . ? C9_1 C5_1 C6_1 C1_1 177.5(2) . . . . ? C6_1 C1_1 C7_1 O1_1 3.5(4) . . . . ? C2_1 C1_1 C7_1 O1_1 -174.6(3) . . . . ? C6_1 C1_1 C7_1 O2_1 -176.2(2) . . . . ? C2_1 C1_1 C7_1 O2_1 5.8(4) . . . . ? C4_1 C3_1 C8_1 O3_1 176.6(2) . . . . ? C2_1 C3_1 C8_1 O3_1 -4.6(4) . . . . ? C4_1 C3_1 C8_1 O4_1 -4.3(4) . . . . ? C2_1 C3_1 C8_1 O4_1 174.4(2) . . . . ? C4_1 C5_1 C9_1 O5_1 -1.1(4) . . . . ? C6_1 C5_1 C9_1 O5_1 -178.4(2) . . . . ? C4_1 C5_1 C9_1 O6_1 177.9(2) . . . . ? C6_1 C5_1 C9_1 O6_1 0.6(4) . . . . ? C6_2 C1_2 C2_2 C3_2 0.0(4) . . . . ? C7_2 C1_2 C2_2 C3_2 179.0(2) . . . . ? C1_2 C2_2 C3_2 C4_2 0.2(4) . . . . ? C1_2 C2_2 C3_2 C8_2 177.8(2) . . . . ? C2_2 C3_2 C4_2 C5_2 -0.4(4) . . . . ? C8_2 C3_2 C4_2 C5_2 -178.0(2) . . . . ? C3_2 C4_2 C5_2 C6_2 0.4(4) . . . . ? C3_2 C4_2 C5_2 C9_2 178.2(2) . . . . ? C2_2 C1_2 C6_2 C5_2 0.0(4) . . . . ? C7_2 C1_2 C6_2 C5_2 -179.0(2) . . . . ? C4_2 C5_2 C6_2 C1_2 -0.2(4) . . . . ? C9_2 C5_2 C6_2 C1_2 -178.0(2) . . . . ? C6_2 C1_2 C7_2 O1_2 -0.3(4) . . . . ? C2_2 C1_2 C7_2 O1_2 -179.3(3) . . . . ? C6_2 C1_2 C7_2 O2_2 177.9(2) . . . . ? C2_2 C1_2 C7_2 O2_2 -1.1(4) . . . . ? C4_2 C3_2 C8_2 O3_2 -173.4(3) . . . . ? C2_2 C3_2 C8_2 O3_2 9.1(4) . . . . ? C4_2 C3_2 C8_2 O4_2 7.8(4) . . . . ? C2_2 C3_2 C8_2 O4_2 -169.7(2) . . . . ? C6_2 C5_2 C9_2 O5_2 175.0(2) . . . . ? C4_2 C5_2 C9_2 O5_2 -2.8(4) . . . . ? C6_2 C5_2 C9_2 O6_2 -3.9(4) . . . . ? C4_2 C5_2 C9_2 O6_2 178.4(2) . . . . ? C6_3 C1_3 C2_3 C3_3 -0.2(4) . . . . ? C7_3 C1_3 C2_3 C3_3 176.7(2) . . . . ? C1_3 C2_3 C3_3 C4_3 0.9(4) . . . . ? C1_3 C2_3 C3_3 C8_3 -178.0(2) . . . . ? C2_3 C3_3 C4_3 C5_3 -0.9(4) . . . . ? C8_3 C3_3 C4_3 C5_3 177.9(2) . . . . ? C3_3 C4_3 C5_3 C6_3 0.3(4) . . . . ? C3_3 C4_3 C5_3 C9_3 179.8(2) . . . . ? C2_3 C1_3 C6_3 C5_3 -0.5(4) . . . . ? C7_3 C1_3 C6_3 C5_3 -177.3(2) . . . . ? C4_3 C5_3 C6_3 C1_3 0.4(4) . . . . ? C9_3 C5_3 C6_3 C1_3 -179.0(2) . . . . ? C6_3 C1_3 C7_3 O1_3 9.5(4) . . . . ? C2_3 C1_3 C7_3 O1_3 -167.3(3) . . . . ? C6_3 C1_3 C7_3 O2_3 -171.6(2) . . . . ? C2_3 C1_3 C7_3 O2_3 11.6(4) . . . . ? C2_3 C3_3 C8_3 O3_3 5.9(4) . . . . ? C4_3 C3_3 C8_3 O3_3 -172.9(3) . . . . ? C2_3 C3_3 C8_3 O4_3 -175.4(2) . . . . ? C4_3 C3_3 C8_3 O4_3 5.7(4) . . . . ? C4_3 C5_3 C9_3 O5_3 -0.4(4) . . . . ? C6_3 C5_3 C9_3 O5_3 179.1(3) . . . . ? C4_3 C5_3 C9_3 O6_3 179.4(2) . . . . ? C6_3 C5_3 C9_3 O6_3 -1.1(4) . . . . ? C6_4 C1_4 C2_4 C3_4 -1.8(4) . . . . ? C7_4 C1_4 C2_4 C3_4 176.5(2) . . . . ? C1_4 C2_4 C3_4 C4_4 2.0(4) . . . . ? C1_4 C2_4 C3_4 C8_4 -176.9(2) . . . . ? C2_4 C3_4 C4_4 C5_4 -0.2(4) . . . . ? C8_4 C3_4 C4_4 C5_4 178.7(2) . . . . ? C3_4 C4_4 C5_4 C6_4 -1.7(4) . . . . ? C3_4 C4_4 C5_4 C9_4 -179.8(2) . . . . ? C2_4 C1_4 C6_4 C5_4 -0.1(4) . . . . ? C7_4 C1_4 C6_4 C5_4 -178.5(2) . . . . ? C4_4 C5_4 C6_4 C1_4 1.9(4) . . . . ? C9_4 C5_4 C6_4 C1_4 179.9(2) . . . . ? C6_4 C1_4 C7_4 O1_4 13.4(4) . . . . ? C2_4 C1_4 C7_4 O1_4 -165.0(3) . . . . ? C6_4 C1_4 C7_4 O2_4 -167.9(3) . . . . ? C2_4 C1_4 C7_4 O2_4 13.8(4) . . . . ? C2_4 C3_4 C8_4 O3_4 -13.2(4) . . . . ? C4_4 C3_4 C8_4 O3_4 167.9(3) . . . . ? C2_4 C3_4 C8_4 O4_4 165.8(3) . . . . ? C4_4 C3_4 C8_4 O4_4 -13.1(4) . . . . ? C6_4 C5_4 C9_4 O5_4 -176.5(2) . . . . ? C4_4 C5_4 C9_4 O5_4 1.5(4) . . . . ? C6_4 C5_4 C9_4 O6_4 2.9(4) . . . . ? C4_4 C5_4 C9_4 O6_4 -179.1(2) . . . . ? C14_1 N1_1 C10_1 C11_1 1.1(5) . . . . ? N1_1 C10_1 C11_1 C12_1 -0.2(5) . . . . ? C10_1 C11_1 C12_1 C13_1 -0.8(5) . . . . ? C10_1 C11_1 C12_1 C15_1 177.3(3) . . . . ? C11_1 C12_1 C13_1 C14_1 0.8(5) . . . . ? C15_1 C12_1 C13_1 C14_1 -177.3(3) . . . . ? C10_1 N1_1 C14_1 C13_1 -1.1(5) . . . . ? C12_1 C13_1 C14_1 N1_1 0.1(5) . . . . ? C13_1 C12_1 C15_1 C16_1 97.7(4) . . . . ? C11_1 C12_1 C15_1 C16_1 -80.2(4) . . . . ? C12_1 C15_1 C16_1 C19_1 171.8(3) . . . . ? C21_1 N2_1 C17_1 C18_1 0.0(6) . . . . ? N2_1 C17_1 C18_1 C19_1 2.4(5) . . . . ? C17_1 C18_1 C19_1 C20_1 -3.8(5) . . . . ? C17_1 C18_1 C19_1 C16_1 173.4(3) . . . . ? C15_1 C16_1 C19_1 C20_1 100.3(4) . . . . ? C15_1 C16_1 C19_1 C18_1 -76.8(4) . . . . ? C18_1 C19_1 C20_1 C21_1 3.0(5) . . . . ? C16_1 C19_1 C20_1 C21_1 -174.2(3) . . . . ? C17_1 N2_1 C21_1 C20_1 -0.9(5) . . . . ? C19_1 C20_1 C21_1 N2_1 -0.7(5) . . . . ? 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 ### within HxBTC layers O6_1 H6O_1 O5_2 1.28(5) 1.35(5) 2.628(3) 175(4) 1_665 O6_2 H6O_2 O5_1 1.24(5) 1.36(5) 2.594(3) 177(4) 1_445 O2_1 H2O_1 O3_3 0.98(5) 1.80(5) 2.717(3) 154(4) . O2_3 H2O_3 O3_1 0.99(5) 1.65(5) 2.592(3) 159(4) . O6_4 H6O_4 O5_3 1.19(5) 1.39(5) 2.583(3) 176(4) 1_756 O6_3 H6O_3 O5_4 1.01(5) 1.66(5) 2.676(3) 179(4) 1_354 O4_2 H4O_2 O4_1 1.12(5) 1.39(5) 2.481(3) 164(4) . O2_4 H2O_4 O3_2 1.05(5) 1.62(5) 2.648(3) 165(4) . O2_2 H2O_2 O3_4 0.94(5) 1.76(5) 2.666(3) 161(4) . O4_4 H4O_4 O4_3 1.13(5) 1.32(5) 2.450(3) 174(4) 1_646 ### between layers, involving one end of BPEH cation N2_1 H2N_1 O3_4 0.95(5) 2.26(5) 3.006(4) 135(4) 2_455 N2_1 H2N_1 O4_3 0.95(5) 2.34(5) 3.053(4) 131(4) 2_364 C17_1 H17_1 O3_3 0.95 2.38 3.208(4) 145.0 1_546 C17_1 H17_1 O4_4 0.95 2.42 3.122(4) 130.8 1_455 ### between layers, involving other end of BPEH and H2O N1_1 H1N_1 O100_1 1.03(4) 1.63(5) 2.658(3) 177(4) . O100_1 H100_1 O3_1 0.82 2.13 2.950(3) 173.4 1_656 O100_1 H101_1 O4_1 0.84 2.08 2.894(3) 162.3 2_565 ### C-H...O between double layers C10_1 H10_1 O4_3 0.95 2.65 3.490(4) 147.4 2_464 C13_1 H13_1 O3_3 0.95 2.60 3.539(4) 170.1 1_556 C14_1 H14_1 O1_4 0.95 2.67 3.448(5) 140.0 1_556 C20_1 H20_1 O4_2 0.95 2.74 3.433(4) 130.9 1_556 C20_1 H20_1 O3_1 0.95 2.70 3.522(4) 145.8 1_556