# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chuan-De Wu' _publ_contact_author_email CDWU@ZJU.EDU.CN _publ_section_title ; Formation of a 2D Supramolecular Nanowater Framework via Metal-Organic Unit Templating ; loop_ _publ_author_name 'Chuan-De Wu.' 'Guo-Qiang Kong.' 'Qing-Guo Meng.' 'Si-Tang Yan.' ; Xiu-Li Yang ; # Attachment 'NiWater.cif' data_Ni _database_code_depnum_ccdc_archive 'CCDC 742358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H61 N5 Ni2 O24' _chemical_formula_weight 1101.35 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' Ni Ni 0.3393 1.1124 '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 10.2608(8) _cell_length_b 11.4119(8) _cell_length_c 13.314(2) _cell_angle_alpha 110.270(7) _cell_angle_beta 107.369(7) _cell_angle_gamma 100.928(5) _cell_volume 1318.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 20611 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 27.72 _exptl_crystal_description Bloc _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 578 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 0.909 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20611 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.72 _reflns_number_total 6096 _reflns_number_gt 3837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0532P)^2^+0.0279P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6096 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Ni1 Ni 0.17292(4) 0.30374(4) 0.36729(3) 0.03182(13) Uani 1 1 d . . . O1 O 0.3931(2) 0.1690(2) 0.26437(16) 0.0414(5) Uani 1 1 d . . . O2 O 0.30275(18) 0.19433(18) 0.40055(14) 0.0297(4) Uani 1 1 d . . . O3 O 0.5284(2) 0.40088(18) 0.65309(15) 0.0355(5) Uani 1 1 d . . . O4 O 0.6218(2) 0.32707(19) 0.52224(17) 0.0391(5) Uani 1 1 d . . . O5 O 0.0645(2) 0.4383(2) 0.3442(2) 0.0637(7) Uani 1 1 d . . . H5B H -0.0364 0.4202 0.3173 0.096 Uiso 1 1 d . . . H5C H 0.0871 0.4636 0.4067 0.096 Uiso 1 1 d . . . O6 O 0.3199(2) 0.46777(19) 0.52022(15) 0.0348(5) Uani 1 1 d . . . H6A H 0.3979 0.4581 0.5641 0.052 Uiso 1 1 d . . . H6B H 0.3642 0.5288 0.4925 0.052 Uiso 1 1 d . . . O7 O 0.27235(19) 0.35475(18) 0.26650(15) 0.0334(5) Uani 1 1 d . . . H7A H 0.3262 0.2978 0.2621 0.050 Uiso 1 1 d . . . H7B H 0.3493 0.4334 0.2981 0.050 Uiso 1 1 d . . . O101 O 0.3864(3) 0.3321(3) 0.9530(3) 0.0949(10) Uani 1 1 d . . . H10D H 0.4490 0.3844 1.0212 0.142 Uiso 1 1 d . . . H10E H 0.4012 0.3662 0.9073 0.142 Uiso 1 1 d . . . O102 O 0.4937(3) -0.1319(3) 0.0468(2) 0.0858(9) Uani 1 1 d . . . H10J H 0.5408 -0.1835 0.0539 0.129 Uiso 1 1 d . . . H10K H 0.5526 -0.0583 0.0794 0.129 Uiso 1 1 d . . . O103 O 0.6089(3) 0.1576(3) 0.1834(2) 0.0681(7) Uani 1 1 d . . . H10H H 0.5224 0.1745 0.1908 0.102 Uiso 1 1 d . . . H10I H 0.5608 0.1586 0.1122 0.102 Uiso 1 1 d . . . O104 O 0.4178(3) 0.4748(3) 0.8223(2) 0.0765(8) Uani 1 1 d . . . H10F H 0.4539 0.4458 0.7753 0.115 Uiso 1 1 d . . . H10G H 0.3652 0.5119 0.7934 0.115 Uiso 1 1 d . . . O105 O -0.2177(2) 0.4255(2) 0.30242(19) 0.0596(7) Uani 1 1 d . . . H10B H -0.2404 0.4525 0.3583 0.089 Uiso 1 1 d . . . H10C H -0.2716 0.3407 0.2597 0.089 Uiso 1 1 d . . . N1 N 0.0684(3) 0.2456(2) 0.4637(2) 0.0390(6) Uani 1 1 d . . . N2 N 0.0218(3) 0.1434(3) 0.2157(2) 0.0435(6) Uani 1 1 d . . . N3 N 0.0382(9) 0.4899(7) 0.1108(7) 0.169(3) Uani 0.50 1 d P . . C20 C 0.0382(9) 0.4899(7) 0.1108(7) 0.169(3) Uani 0.50 1 d P . . H20A H 0.0612 0.4817 0.1806 0.203 Uiso 0.50 1 calc PR . . C1 C 0.5611(3) 0.3109(3) 0.5869(2) 0.0302(6) Uani 1 1 d . . . C2 C 0.5344(3) 0.1796(3) 0.5924(2) 0.0271(6) Uani 1 1 d . . . C3 C 0.5750(3) 0.1815(3) 0.7010(2) 0.0364(7) Uani 1 1 d . . . H3A H 0.5922 0.2585 0.7652 0.044 Uiso 1 1 calc R . . C4 C 0.4921(3) 0.0575(2) 0.4919(2) 0.0239(6) Uani 1 1 d . . . C5 C 0.4093(3) -0.0693(3) 0.2839(2) 0.0373(7) Uani 1 1 d . . . H5A H 0.3821 -0.0728 0.2094 0.045 Uiso 1 1 calc R . . C6 C 0.4329(3) 0.0456(3) 0.3755(2) 0.0273(6) Uani 1 1 d . . . C7 C 0.3756(3) 0.1466(3) 0.3459(2) 0.0296(6) Uani 1 1 d . . . C8 C 0.1398(4) 0.2293(3) 0.5566(3) 0.0512(9) Uani 1 1 d . . . H8A H 0.2389 0.2456 0.5794 0.061 Uiso 1 1 calc R . . C9 C 0.0730(5) 0.1894(5) 0.6201(4) 0.0784(13) Uani 1 1 d . . . H9A H 0.1265 0.1804 0.6854 0.094 Uiso 1 1 calc R . . C10 C -0.0729(5) 0.1631(5) 0.5863(4) 0.0900(15) Uani 1 1 d . . . H10A H -0.1200 0.1365 0.6284 0.108 Uiso 1 1 calc R . . C11 C -0.1485(4) 0.1766(5) 0.4895(4) 0.0819(14) Uani 1 1 d . . . H11A H -0.2482 0.1573 0.4635 0.098 Uiso 1 1 calc R . . C12 C -0.0739(4) 0.2191(4) 0.4318(4) 0.0653(11) Uani 1 1 d . . . H12A H -0.1253 0.2300 0.3670 0.078 Uiso 1 1 calc R . . C13 C -0.0580(4) 0.1564(5) 0.1235(3) 0.0656(11) Uani 1 1 d . . . H13A H -0.0457 0.2404 0.1259 0.079 Uiso 1 1 calc R . . C14 C -0.1602(5) 0.0468(6) 0.0228(3) 0.0866(16) Uani 1 1 d . . . H14A H -0.2146 0.0576 -0.0411 0.104 Uiso 1 1 calc R . . C15 C -0.1786(5) -0.0746(6) 0.0200(4) 0.0917(17) Uani 1 1 d . . . H15A H -0.2473 -0.1482 -0.0455 0.110 Uiso 1 1 calc R . . C16 C -0.0964(5) -0.0892(4) 0.1132(3) 0.0811(13) Uani 1 1 d . . . H16A H -0.1070 -0.1724 0.1121 0.097 Uiso 1 1 calc R . . C17 C 0.0020(4) 0.0216(4) 0.2085(3) 0.0576(10) Uani 1 1 d . . . H17A H 0.0585 0.0112 0.2719 0.069 Uiso 1 1 calc R . . C18 C -0.0814(11) 0.5194(9) 0.0610(10) 0.185(4) Uani 1 1 d . . . H18A H -0.1376 0.5344 0.1062 0.222 Uiso 1 1 d . . . C19 C 0.1197(9) 0.4739(8) 0.0449(11) 0.178(5) Uani 1 1 d . . . H19A H 0.2102 0.4571 0.0672 0.214 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 Ni1 0.0303(2) 0.0289(2) 0.0408(2) 0.01985(18) 0.01299(16) 0.01181(17) O1 0.0642(14) 0.0431(13) 0.0391(11) 0.0275(11) 0.0284(11) 0.0325(12) O2 0.0338(10) 0.0308(11) 0.0319(9) 0.0170(9) 0.0147(8) 0.0167(9) O3 0.0461(12) 0.0206(11) 0.0354(10) 0.0082(9) 0.0136(9) 0.0134(10) O4 0.0471(12) 0.0304(12) 0.0533(12) 0.0250(11) 0.0284(11) 0.0144(10) O5 0.0522(15) 0.0698(18) 0.1015(18) 0.0599(16) 0.0345(14) 0.0374(14) O6 0.0386(11) 0.0300(12) 0.0399(11) 0.0180(9) 0.0163(9) 0.0130(10) O7 0.0362(11) 0.0268(12) 0.0388(10) 0.0182(9) 0.0117(9) 0.0110(9) O101 0.106(2) 0.072(2) 0.096(2) 0.0403(19) 0.0302(19) 0.0147(19) O102 0.109(2) 0.078(2) 0.0858(19) 0.0358(17) 0.0522(18) 0.0392(19) O103 0.0712(17) 0.078(2) 0.0645(15) 0.0278(15) 0.0361(14) 0.0337(16) O104 0.099(2) 0.095(2) 0.0582(15) 0.0399(16) 0.0393(15) 0.0535(19) O105 0.0601(15) 0.0627(17) 0.0625(15) 0.0237(13) 0.0304(13) 0.0303(14) N1 0.0395(14) 0.0345(16) 0.0551(15) 0.0239(13) 0.0263(13) 0.0166(13) N2 0.0339(14) 0.0514(19) 0.0419(14) 0.0275(14) 0.0068(12) 0.0060(14) N3 0.131(6) 0.115(5) 0.218(7) 0.045(5) 0.025(6) 0.072(5) C20 0.131(6) 0.115(5) 0.218(7) 0.045(5) 0.025(6) 0.072(5) C1 0.0294(15) 0.0224(16) 0.0328(14) 0.0123(13) 0.0047(12) 0.0076(13) C2 0.0297(14) 0.0228(15) 0.0294(14) 0.0116(12) 0.0109(12) 0.0103(13) C3 0.0520(19) 0.0272(17) 0.0289(14) 0.0094(13) 0.0143(13) 0.0184(15) C4 0.0262(13) 0.0218(15) 0.0296(13) 0.0137(12) 0.0138(11) 0.0105(12) C5 0.0567(19) 0.0344(18) 0.0266(14) 0.0172(14) 0.0143(14) 0.0227(16) C6 0.0335(15) 0.0238(16) 0.0304(14) 0.0147(12) 0.0152(12) 0.0113(13) C7 0.0337(15) 0.0224(16) 0.0266(14) 0.0093(12) 0.0062(12) 0.0080(13) C8 0.047(2) 0.061(3) 0.0496(19) 0.0276(19) 0.0222(17) 0.0149(18) C9 0.080(3) 0.109(4) 0.080(3) 0.066(3) 0.046(2) 0.033(3) C10 0.094(3) 0.123(4) 0.127(4) 0.089(4) 0.087(3) 0.053(3) C11 0.057(3) 0.104(4) 0.138(4) 0.080(3) 0.065(3) 0.041(3) C12 0.048(2) 0.076(3) 0.107(3) 0.061(3) 0.043(2) 0.036(2) C13 0.048(2) 0.094(3) 0.056(2) 0.045(2) 0.0103(18) 0.019(2) C14 0.053(3) 0.149(5) 0.042(2) 0.044(3) 0.0045(19) 0.017(3) C15 0.060(3) 0.116(5) 0.050(3) 0.014(3) 0.014(2) -0.017(3) C16 0.089(3) 0.059(3) 0.056(2) 0.010(2) 0.019(2) -0.013(3) C17 0.058(2) 0.046(2) 0.048(2) 0.0192(19) 0.0071(17) -0.0041(19) C18 0.135(7) 0.142(7) 0.229(10) 0.030(8) 0.049(7) 0.074(6) C19 0.106(6) 0.111(6) 0.223(10) 0.019(7) -0.011(7) 0.060(5) _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 Ni1 O2 2.0472(17) . ? Ni1 O7 2.0769(19) . ? Ni1 N2 2.079(3) . ? Ni1 N1 2.092(2) . ? Ni1 O6 2.0928(19) . ? Ni1 O5 2.112(2) . ? O1 C7 1.251(3) . ? O2 C7 1.261(3) . ? O3 C1 1.275(3) . ? O4 C1 1.245(3) . ? O5 H5B 0.9429 . ? O5 H5C 0.7233 . ? O6 H6A 0.8906 . ? O6 H6B 0.9931 . ? O7 H7A 0.9275 . ? O7 H7B 0.9367 . ? O101 H10D 0.8510 . ? O101 H10E 0.8618 . ? O102 H10J 0.8413 . ? O102 H10K 0.8112 . ? O103 H10H 0.9684 . ? O103 H10I 0.9334 . ? O104 H10F 0.8252 . ? O104 H10G 0.8330 . ? O105 H10B 0.8216 . ? O105 H10C 0.8907 . ? N1 C8 1.331(4) . ? N1 C12 1.333(4) . ? N2 C17 1.331(4) . ? N2 C13 1.332(4) . ? N3 C18 1.373(10) . ? N3 C19 1.375(12) . ? C1 C2 1.503(4) . ? C2 C3 1.371(3) . ? C2 C4 1.432(3) . ? C3 C5 1.395(4) 2_656 ? C3 H3A 0.9300 . ? C4 C6 1.432(3) . ? C4 C4 1.432(5) 2_656 ? C5 C6 1.365(4) . ? C5 C3 1.395(4) 2_656 ? C5 H5A 0.9300 . ? C6 C7 1.504(4) . ? C8 C9 1.374(5) . ? C8 H8A 0.9300 . ? C9 C10 1.367(6) . ? C9 H9A 0.9300 . ? C10 C11 1.367(6) . ? C10 H10A 0.9300 . ? C11 C12 1.372(5) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.401(6) . ? C13 H13A 0.9300 . ? C14 C15 1.348(7) . ? C14 H14A 0.9300 . ? C15 C16 1.360(6) . ? C15 H15A 0.9300 . ? C16 C17 1.366(5) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.379(13) 2_565 ? C18 H18A 0.9468 . ? C19 C18 1.379(13) 2_565 ? C19 H19A 0.9641 . ? 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 O2 Ni1 O7 91.87(7) . . ? O2 Ni1 N2 92.20(9) . . ? O7 Ni1 N2 88.20(9) . . ? O2 Ni1 N1 87.73(8) . . ? O7 Ni1 N1 177.92(9) . . ? N2 Ni1 N1 89.77(10) . . ? O2 Ni1 O6 89.44(7) . . ? O7 Ni1 O6 92.49(7) . . ? N2 Ni1 O6 178.20(8) . . ? N1 Ni1 O6 89.55(9) . . ? O2 Ni1 O5 172.39(9) . . ? O7 Ni1 O5 84.48(8) . . ? N2 Ni1 O5 94.35(10) . . ? N1 Ni1 O5 96.16(9) . . ? O6 Ni1 O5 84.07(9) . . ? C7 O2 Ni1 129.08(16) . . ? Ni1 O5 H5B 125.5 . . ? Ni1 O5 H5C 82.8 . . ? H5B O5 H5C 103.1 . . ? Ni1 O6 H6A 118.4 . . ? Ni1 O6 H6B 104.4 . . ? H6A O6 H6B 101.1 . . ? Ni1 O7 H7A 98.3 . . ? Ni1 O7 H7B 121.7 . . ? H7A O7 H7B 97.3 . . ? H10D O101 H10E 106.5 . . ? H10J O102 H10K 106.2 . . ? H10H O103 H10I 77.7 . . ? H10F O104 H10G 104.6 . . ? H10B O105 H10C 106.6 . . ? C8 N1 C12 117.3(3) . . ? C8 N1 Ni1 121.7(2) . . ? C12 N1 Ni1 121.0(2) . . ? C17 N2 C13 117.4(3) . . ? C17 N2 Ni1 119.8(2) . . ? C13 N2 Ni1 122.8(3) . . ? C18 N3 C19 111.7(8) . . ? O4 C1 O3 124.0(3) . . ? O4 C1 C2 117.4(2) . . ? O3 C1 C2 118.5(2) . . ? C3 C2 C4 119.7(2) . . ? C3 C2 C1 117.1(2) . . ? C4 C2 C1 122.4(2) . . ? C2 C3 C5 120.7(2) . 2_656 ? C2 C3 H3A 119.6 . . ? C5 C3 H3A 119.6 2_656 . ? C6 C4 C4 118.6(3) . 2_656 ? C6 C4 C2 122.4(2) . . ? C4 C4 C2 119.0(3) 2_656 . ? C6 C5 C3 121.6(2) . 2_656 ? C6 C5 H5A 119.2 . . ? C3 C5 H5A 119.2 2_656 . ? C5 C6 C4 119.6(2) . . ? C5 C6 C7 116.4(2) . . ? C4 C6 C7 123.5(2) . . ? O1 C7 O2 125.1(2) . . ? O1 C7 C6 118.8(2) . . ? O2 C7 C6 115.8(2) . . ? N1 C8 C9 122.6(3) . . ? N1 C8 H8A 118.7 . . ? C9 C8 H8A 118.7 . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C11 119.0(4) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C10 C11 C12 118.4(4) . . ? C10 C11 H11A 120.8 . . ? C12 C11 H11A 120.8 . . ? N1 C12 C11 123.4(4) . . ? N1 C12 H12A 118.3 . . ? C11 C12 H12A 118.3 . . ? N2 C13 C14 121.6(4) . . ? N2 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C15 C14 C13 119.0(4) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C14 C15 C16 119.9(4) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C17 118.3(5) . . ? C15 C16 H16A 120.8 . . ? C17 C16 H16A 120.8 . . ? N2 C17 C16 123.7(4) . . ? N2 C17 H17A 118.1 . . ? C16 C17 H17A 118.1 . . ? N3 C18 C19 124.5(9) . 2_565 ? N3 C18 H18A 113.5 . . ? C19 C18 H18A 122.0 2_565 . ? N3 C19 C18 123.7(8) . 2_565 ? N3 C19 H19A 124.0 . . ? C18 C19 H19A 112.2 2_565 . ? 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 O5 H5B O105 0.94 1.83 2.745(3) 164.2 . O5 H5C O6 0.72 2.40 2.816(3) 118.6 . O6 H6A O3 0.89 1.88 2.754(2) 165.6 . O6 H6B O4 0.99 1.71 2.597(3) 147.0 2_666 O7 H7A O1 0.93 1.74 2.646(3) 164.3 . O7 H7B O3 0.94 1.83 2.751(3) 168.5 2_666 O101 H10D O104 0.85 1.98 2.830(4) 171.9 2_667 O101 H10E O104 0.86 1.96 2.807(4) 166.6 . O102 H10J O101 0.84 1.96 2.793(4) 168.4 2_656 O102 H10K O103 0.81 2.22 2.949(4) 149.1 . O103 H10H O1 0.97 1.87 2.742(3) 147.8 . O103 H10I O102 0.93 1.92 2.815(4) 160.9 2_655 O104 H10F O3 0.83 1.95 2.766(3) 169.2 . O104 H10G O105 0.83 2.08 2.903(3) 170.6 2_566 O105 H10B O6 0.82 2.04 2.851(3) 169.8 2_566 O105 H10C O103 0.89 1.93 2.814(4) 173.4 1_455 N3 H20A O5 0.93 2.39 3.301(9) 167.4 . C20 H20A O5 0.93 2.39 3.301(9) 167.4 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.72 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.533 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.064