# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c:\users\nick\desktop\xrayfi~1\nch83(~1\p-1 _database_code_depnum_ccdc_archive 'CCDC 914681' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cl3 Gd N4 O10' _chemical_formula_weight 728.08 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8714(5) _cell_length_b 11.1470(6) _cell_length_c 14.5317(8) _cell_angle_alpha 102.922(3) _cell_angle_beta 93.887(2) _cell_angle_gamma 91.677(2) _cell_volume 1395.96(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 2.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.9 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34764 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 30.64 _reflns_number_total 8145 _reflns_number_gt 7464 _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. The asymmetric unit contains the entire cluster as well as two water molecules and three chloride ions. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20, H21, H22, H23, H24, H25, H26, H27 and H28 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. The hydrogen atoms for the lattice water molecules (O9 and O10) were omitted due to uncertainties in thier position. ; _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^)+(0.0221P)^2^+1.0449P] 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 8145 _refine_ls_number_parameters 363 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0516 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _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 Gd1 Gd 1.317224(10) 0.202604(8) -0.199367(6) 0.01311(3) Uani 1 1 d . . . O8 O 1.35186(17) 0.40270(14) -0.08867(11) 0.0203(3) Uani 1 1 d D . . O4 O 1.45115(16) 0.11165(13) -0.33112(10) 0.0170(3) Uani 1 1 d . . . O1 O 1.40181(16) 0.01454(13) -0.17338(10) 0.0186(3) Uani 1 1 d . . . O3 O 1.33603(17) 0.34578(13) -0.29111(10) 0.0190(3) Uani 1 1 d . . . O2 O 1.20705(16) 0.16793(13) -0.06585(10) 0.0183(3) Uani 1 1 d . . . O6 O 1.13866(17) 0.05599(14) -0.30077(11) 0.0219(3) Uani 1 1 d D . . O7 O 1.57955(18) 0.24403(15) -0.14324(12) 0.0257(3) Uani 1 1 d D . . O5 O 1.06403(17) 0.28870(14) -0.18774(12) 0.0237(3) Uani 1 1 d D . . N2 N 1.0057(2) 0.27997(16) 0.03967(12) 0.0185(3) Uani 1 1 d D . . N1 N 1.1358(2) 0.10816(16) 0.06438(12) 0.0185(3) Uani 1 1 d D . . C5 C 1.0470(2) 0.20385(18) 0.09554(14) 0.0170(4) Uani 1 1 d . . . N4 N 1.5974(2) -0.09016(16) -0.37343(12) 0.0184(3) Uani 1 1 d D . . N3 N 1.6375(2) 0.08702(16) -0.43267(12) 0.0175(3) Uani 1 1 d D . . C14 C 1.6740(2) -0.02865(19) -0.42644(14) 0.0172(4) Uani 1 1 d . . . C6 C 0.9925(2) 0.2234(2) 0.18609(14) 0.0203(4) Uani 1 1 d . . . H6 H 1.0187 0.1704 0.2269 0.024 Uiso 1 1 calc R . . C2 C 1.3817(2) -0.05127(18) -0.11442(14) 0.0166(4) Uani 1 1 d . . . C13 C 1.5336(2) 0.16098(19) -0.38155(13) 0.0162(4) Uani 1 1 d . . . C1 C 1.4577(3) -0.17246(19) -0.13115(16) 0.0229(4) Uani 1 1 d . . . H1 H 1.5637 -0.1594 -0.1431 0.034 Uiso 1 1 calc R . . H3 H 1.4059 -0.2296 -0.1861 0.034 Uiso 1 1 calc R . . H2 H 1.4531 -0.2073 -0.0751 0.034 Uiso 1 1 calc R . . C4 C 1.2141(2) 0.08661(18) -0.01727(14) 0.0162(4) Uani 1 1 d . . . C9 C 0.9132(3) 0.3745(2) 0.06714(16) 0.0233(4) Uani 1 1 d . . . H9 H 0.8858 0.4256 0.0250 0.028 Uiso 1 1 calc R . . C12 C 1.5306(2) 0.28245(19) -0.39211(14) 0.0176(4) Uani 1 1 d . . . H14 H 1.5996 0.3084 -0.4318 0.021 Uiso 1 1 calc R . . C3 C 1.2929(2) -0.02103(19) -0.03714(14) 0.0182(4) Uani 1 1 d . . . H4 H 1.2862 -0.0766 0.0035 0.022 Uiso 1 1 calc R . . C8 C 0.8598(3) 0.3962(2) 0.15436(17) 0.0252(5) Uani 1 1 d . . . H8 H 0.7954 0.4623 0.1740 0.030 Uiso 1 1 calc R . . C7 C 0.9016(3) 0.3192(2) 0.21479(16) 0.0242(5) Uani 1 1 d . . . H7 H 0.8664 0.3337 0.2764 0.029 Uiso 1 1 calc R . . C10 C 1.4363(3) 0.4946(2) -0.36550(17) 0.0281(5) Uani 1 1 d . . . H11 H 1.4589 0.5549 -0.3054 0.042 Uiso 1 1 calc R . . H13 H 1.3380 0.5104 -0.3944 0.042 Uiso 1 1 calc R . . H12 H 1.5150 0.5016 -0.4084 0.042 Uiso 1 1 calc R . . C17 C 1.7464(3) -0.2633(2) -0.41081(17) 0.0265(5) Uani 1 1 d . . . H18 H 1.7709 -0.3436 -0.4045 0.032 Uiso 1 1 calc R . . C15 C 1.7920(2) -0.0865(2) -0.47588(15) 0.0224(4) Uani 1 1 d . . . H16 H 1.8470 -0.0458 -0.5148 0.027 Uiso 1 1 calc R . . C18 C 1.6315(3) -0.2045(2) -0.36495(16) 0.0228(4) Uani 1 1 d . . . H19 H 1.5745 -0.2445 -0.3265 0.027 Uiso 1 1 calc R . . C11 C 1.4318(2) 0.36721(18) -0.34757(14) 0.0174(4) Uani 1 1 d . . . C16 C 1.8273(3) -0.2028(2) -0.46737(17) 0.0264(5) Uani 1 1 d . . . H17 H 1.9076 -0.2424 -0.5003 0.032 Uiso 1 1 calc R . . Cl2 Cl 0.83613(5) 0.06947(5) -0.20413(4) 0.01908(10) Uani 1 1 d . . . Cl1 Cl 1.22960(6) -0.19769(5) -0.40455(4) 0.02274(11) Uani 1 1 d . . . Cl3 Cl 1.66851(7) 0.52239(6) -0.12501(4) 0.03277(13) Uani 1 1 d . . . O9 O 1.1227(2) -0.45051(18) -0.53582(14) 0.0438(5) Uani 1 1 d . . . O10 O 0.8831(3) 0.4145(3) -0.28488(17) 0.0732(8) Uani 1 1 d . . . H26 H 0.998(3) 0.234(3) -0.186(3) 0.088 Uiso 1 1 d D . . H15 H 1.690(4) 0.115(4) -0.473(2) 0.088 Uiso 1 1 d D . . H5 H 1.142(5) 0.054(3) 0.100(2) 0.088 Uiso 1 1 d D . . H22 H 1.640(4) 0.189(3) -0.161(3) 0.088 Uiso 1 1 d D . . H20 H 1.524(3) -0.050(3) -0.344(3) 0.088 Uiso 1 1 d D . . H27 H 1.052(2) 0.050(4) -0.282(3) 0.088 Uiso 1 1 d D . . H28 H 1.168(5) -0.0137(19) -0.327(3) 0.088 Uiso 1 1 d D . . H24 H 1.336(5) 0.413(4) -0.0312(10) 0.088 Uiso 1 1 d D . . H10 H 1.045(4) 0.264(4) -0.0156(15) 0.088 Uiso 1 1 d D . . H23 H 1.424(3) 0.448(3) -0.098(3) 0.088 Uiso 1 1 d D . . H25 H 1.031(5) 0.335(3) -0.222(3) 0.088 Uiso 1 1 d D . . H21 H 1.618(4) 0.3151(17) -0.138(3) 0.088 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 Gd1 0.01370(5) 0.01236(5) 0.01352(5) 0.00267(3) 0.00370(3) 0.00085(3) O8 0.0211(7) 0.0183(7) 0.0198(7) 0.0004(6) 0.0030(6) -0.0007(6) O4 0.0192(7) 0.0155(7) 0.0174(7) 0.0041(5) 0.0071(5) 0.0006(6) O1 0.0217(7) 0.0171(7) 0.0188(7) 0.0053(6) 0.0074(6) 0.0044(6) O3 0.0227(7) 0.0178(7) 0.0189(7) 0.0072(6) 0.0072(6) 0.0043(6) O2 0.0212(7) 0.0177(7) 0.0182(7) 0.0068(6) 0.0065(6) 0.0037(6) O6 0.0178(7) 0.0214(8) 0.0237(8) -0.0018(6) 0.0058(6) -0.0022(6) O7 0.0166(7) 0.0206(8) 0.0367(9) -0.0002(7) 0.0006(6) 0.0031(6) O5 0.0173(7) 0.0192(8) 0.0355(9) 0.0078(7) 0.0020(6) 0.0012(6) N2 0.0173(8) 0.0208(9) 0.0197(8) 0.0080(7) 0.0055(7) 0.0036(7) N1 0.0212(9) 0.0196(9) 0.0175(8) 0.0075(7) 0.0073(7) 0.0051(7) C5 0.0163(9) 0.0160(9) 0.0195(10) 0.0054(8) 0.0031(7) -0.0002(8) N4 0.0199(9) 0.0173(8) 0.0177(8) 0.0025(7) 0.0035(7) 0.0014(7) N3 0.0171(8) 0.0207(9) 0.0158(8) 0.0048(7) 0.0060(6) 0.0029(7) C14 0.0157(9) 0.0199(10) 0.0144(9) 0.0010(8) -0.0010(7) -0.0003(8) C6 0.0237(11) 0.0224(10) 0.0169(9) 0.0075(8) 0.0053(8) 0.0029(8) C2 0.0154(9) 0.0145(9) 0.0190(9) 0.0022(7) -0.0003(7) 0.0003(7) C13 0.0159(9) 0.0196(10) 0.0121(9) 0.0017(7) 0.0021(7) -0.0007(8) C1 0.0262(11) 0.0184(10) 0.0251(11) 0.0049(8) 0.0069(9) 0.0050(9) C4 0.0156(9) 0.0178(9) 0.0148(9) 0.0030(7) 0.0025(7) -0.0014(7) C9 0.0222(11) 0.0218(10) 0.0301(11) 0.0130(9) 0.0060(9) 0.0063(9) C12 0.0190(10) 0.0186(10) 0.0157(9) 0.0040(8) 0.0049(7) -0.0016(8) C3 0.0207(10) 0.0179(10) 0.0177(9) 0.0062(8) 0.0050(8) 0.0011(8) C8 0.0227(11) 0.0224(11) 0.0323(12) 0.0063(9) 0.0121(9) 0.0077(9) C7 0.0249(11) 0.0271(11) 0.0213(10) 0.0045(9) 0.0092(9) 0.0042(9) C10 0.0426(14) 0.0182(10) 0.0275(12) 0.0098(9) 0.0140(10) 0.0040(10) C17 0.0263(12) 0.0209(11) 0.0304(12) 0.0023(9) -0.0018(9) 0.0056(9) C15 0.0177(10) 0.0276(11) 0.0203(10) 0.0014(9) 0.0037(8) 0.0016(9) C18 0.0247(11) 0.0183(10) 0.0252(11) 0.0050(8) 0.0009(9) 0.0017(8) C11 0.0205(10) 0.0163(9) 0.0155(9) 0.0041(7) 0.0018(7) -0.0005(8) C16 0.0191(10) 0.0287(12) 0.0290(12) 0.0005(9) 0.0026(9) 0.0075(9) Cl2 0.0160(2) 0.0197(2) 0.0233(2) 0.00764(19) 0.00436(18) 0.00229(18) Cl1 0.0254(3) 0.0200(2) 0.0228(2) 0.00305(19) 0.0097(2) -0.0024(2) Cl3 0.0403(3) 0.0316(3) 0.0226(3) -0.0019(2) 0.0094(2) -0.0139(3) O9 0.0580(13) 0.0326(10) 0.0383(11) 0.0028(8) 0.0021(9) 0.0033(9) O10 0.102(2) 0.0774(18) 0.0469(14) 0.0204(13) 0.0127(14) 0.0448(16) _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 Gd1 O3 2.3062(14) . ? Gd1 O2 2.3323(13) . ? Gd1 O1 2.3469(14) . ? Gd1 O4 2.3699(13) . ? Gd1 O7 2.4095(16) . ? Gd1 O6 2.4097(15) . ? Gd1 O8 2.4383(15) . ? Gd1 O5 2.4699(16) . ? O8 H24 0.838(10) . ? O8 H23 0.835(10) . ? O4 C13 1.267(2) . ? O1 C2 1.264(2) . ? O3 C11 1.273(2) . ? O2 C4 1.268(2) . ? O6 H27 0.837(10) . ? O6 H28 0.841(10) . ? O7 H22 0.838(10) . ? O7 H21 0.838(10) . ? O5 H26 0.840(10) . ? O5 H25 0.839(10) . ? N2 C5 1.341(3) . ? N2 C9 1.360(3) . ? N2 H10 0.881(10) . ? N1 C5 1.358(3) . ? N1 C4 1.393(2) . ? N1 H5 0.878(10) . ? C5 C6 1.406(3) . ? N4 C14 1.343(3) . ? N4 C18 1.349(3) . ? N4 H20 0.875(10) . ? N3 C14 1.359(3) . ? N3 C13 1.394(3) . ? N3 H15 0.877(10) . ? C14 C15 1.401(3) . ? C6 C7 1.364(3) . ? C6 H6 0.9500 . ? C2 C3 1.401(3) . ? C2 C1 1.506(3) . ? C13 C12 1.397(3) . ? C1 H1 0.9800 . ? C1 H3 0.9800 . ? C1 H2 0.9800 . ? C4 C3 1.391(3) . ? C9 C8 1.357(3) . ? C9 H9 0.9500 . ? C12 C11 1.390(3) . ? C12 H14 0.9500 . ? C3 H4 0.9500 . ? C8 C7 1.399(3) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? C10 C11 1.500(3) . ? C10 H11 0.9800 . ? C10 H13 0.9800 . ? C10 H12 0.9800 . ? C17 C18 1.359(3) . ? C17 C16 1.395(3) . ? C17 H18 0.9500 . ? C15 C16 1.372(3) . ? C15 H16 0.9500 . ? C18 H19 0.9500 . ? C16 H17 0.9500 . ? 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 O3 Gd1 O2 141.98(5) . . ? O3 Gd1 O1 145.21(5) . . ? O2 Gd1 O1 72.71(5) . . ? O3 Gd1 O4 73.06(5) . . ? O2 Gd1 O4 144.66(5) . . ? O1 Gd1 O4 72.81(5) . . ? O3 Gd1 O7 90.26(6) . . ? O2 Gd1 O7 102.46(6) . . ? O1 Gd1 O7 75.02(5) . . ? O4 Gd1 O7 75.73(5) . . ? O3 Gd1 O6 99.47(5) . . ? O2 Gd1 O6 90.52(5) . . ? O1 Gd1 O6 77.93(5) . . ? O4 Gd1 O6 74.93(5) . . ? O7 Gd1 O6 144.73(5) . . ? O3 Gd1 O8 74.09(5) . . ? O2 Gd1 O8 77.16(5) . . ? O1 Gd1 O8 126.35(5) . . ? O4 Gd1 O8 131.31(5) . . ? O7 Gd1 O8 69.50(5) . . ? O6 Gd1 O8 145.77(5) . . ? O3 Gd1 O5 79.35(5) . . ? O2 Gd1 O5 69.05(5) . . ? O1 Gd1 O5 130.25(5) . . ? O4 Gd1 O5 132.06(5) . . ? O7 Gd1 O5 143.38(5) . . ? O6 Gd1 O5 71.89(5) . . ? O8 Gd1 O5 73.88(5) . . ? Gd1 O8 H24 123(3) . . ? Gd1 O8 H23 115(3) . . ? H24 O8 H23 113(4) . . ? C13 O4 Gd1 130.28(13) . . ? C2 O1 Gd1 136.64(13) . . ? C11 O3 Gd1 133.62(13) . . ? C4 O2 Gd1 136.00(13) . . ? Gd1 O6 H27 117(3) . . ? Gd1 O6 H28 119(3) . . ? H27 O6 H28 111(4) . . ? Gd1 O7 H22 118(3) . . ? Gd1 O7 H21 119(3) . . ? H22 O7 H21 113(4) . . ? Gd1 O5 H26 111(3) . . ? Gd1 O5 H25 123(3) . . ? H26 O5 H25 110(4) . . ? C5 N2 C9 122.58(18) . . ? C5 N2 H10 114(3) . . ? C9 N2 H10 123(3) . . ? C5 N1 C4 127.22(17) . . ? C5 N1 H5 115(3) . . ? C4 N1 H5 118(3) . . ? N2 C5 N1 120.78(18) . . ? N2 C5 C6 118.36(18) . . ? N1 C5 C6 120.83(18) . . ? C14 N4 C18 122.46(18) . . ? C14 N4 H20 115(3) . . ? C18 N4 H20 123(3) . . ? C14 N3 C13 127.34(17) . . ? C14 N3 H15 112(3) . . ? C13 N3 H15 120(3) . . ? N4 C14 N3 120.90(18) . . ? N4 C14 C15 118.60(19) . . ? N3 C14 C15 120.49(19) . . ? C7 C6 C5 119.5(2) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? O1 C2 C3 125.15(19) . . ? O1 C2 C1 116.40(17) . . ? C3 C2 C1 118.43(18) . . ? O4 C13 N3 117.19(18) . . ? O4 C13 C12 126.63(19) . . ? N3 C13 C12 116.18(17) . . ? C2 C1 H1 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? H3 C1 H2 109.5 . . ? O2 C4 C3 126.42(18) . . ? O2 C4 N1 116.52(18) . . ? C3 C4 N1 117.06(18) . . ? C8 C9 N2 120.4(2) . . ? C8 C9 H9 119.8 . . ? N2 C9 H9 119.8 . . ? C11 C12 C13 123.34(18) . . ? C11 C12 H14 118.3 . . ? C13 C12 H14 118.3 . . ? C4 C3 C2 122.96(18) . . ? C4 C3 H4 118.5 . . ? C2 C3 H4 118.5 . . ? C9 C8 C7 118.5(2) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C6 C7 C8 120.7(2) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C11 C10 H11 109.5 . . ? C11 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? C11 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? H13 C10 H12 109.5 . . ? C18 C17 C16 118.4(2) . . ? C18 C17 H18 120.8 . . ? C16 C17 H18 120.8 . . ? C16 C15 C14 119.2(2) . . ? C16 C15 H16 120.4 . . ? C14 C15 H16 120.4 . . ? N4 C18 C17 120.8(2) . . ? N4 C18 H19 119.6 . . ? C17 C18 H19 119.6 . . ? O3 C11 C12 124.98(18) . . ? O3 C11 C10 116.20(18) . . ? C12 C11 C10 118.82(18) . . ? C15 C16 C17 120.6(2) . . ? C15 C16 H17 119.7 . . ? C17 C16 H17 119.7 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 30.64 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.234 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.099 data_10c:\users\nick\desktop\honour~1\er(no3~1\p21c _database_code_depnum_ccdc_archive 'CCDC 914682' #TrackingRef '10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H24 Er N7 O14' _chemical_formula_weight 741.71 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.0075(6) _cell_length_b 14.8207(7) _cell_length_c 13.9166(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.653(2) _cell_angle_gamma 90.00 _cell_volume 2617.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour pink _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 3.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_T_max 0.720 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26852 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 30.51 _reflns_number_total 7929 _reflns_number_gt 5503 _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. The asymmetric unit contains the entire cluster as well as one nitrate ion. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20 and H24 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. ; _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^)+(0.0310P)^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 7929 _refine_ls_number_parameters 397 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.002 _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 Er1 Er 0.747793(14) 0.089061(12) 0.278206(14) 0.01804(6) Uani 1 1 d . . . O2 O 0.7525(2) -0.05687(19) 0.2204(2) 0.0245(6) Uani 1 1 d . . . O4 O 0.8599(2) 0.20907(17) 0.3359(2) 0.0237(7) Uani 1 1 d . . . O3 O 0.6540(2) 0.21819(18) 0.2332(2) 0.0255(7) Uani 1 1 d . . . O5 O 0.8245(3) 0.1152(2) 0.1431(2) 0.0298(7) Uani 1 1 d D . . O6 O 0.5612(2) 0.05500(19) 0.2680(2) 0.0236(7) Uani 1 1 d . . . O1 O 0.9186(2) 0.03616(18) 0.3390(2) 0.0215(6) Uani 1 1 d . . . N7 N 0.9111(3) -0.4113(2) 0.3141(3) 0.0243(8) Uani 1 1 d . . . O7 O 0.6058(2) 0.05836(19) 0.1278(2) 0.0244(7) Uani 1 1 d . . . N1 N 0.7669(3) -0.2102(2) 0.2228(2) 0.0210(8) Uani 1 1 d D . . H5 H 0.8061 -0.2572 0.2456 0.025 Uiso 1 1 calc RD . . N3 N 0.9417(3) 0.3439(2) 0.3729(3) 0.0207(8) Uani 1 1 d D . . O9 O 0.7123(2) 0.1233(2) 0.4375(2) 0.0252(7) Uani 1 1 d . . . N4 N 1.0544(3) 0.2216(2) 0.4308(3) 0.0215(8) Uani 1 1 d D . . O13 O 0.9797(2) -0.4650(2) 0.3601(2) 0.0295(7) Uani 1 1 d . . . C11 C 0.6669(3) 0.3024(3) 0.2464(3) 0.0219(9) Uani 1 1 d . . . C10 C 0.5713(3) 0.3619(3) 0.2104(3) 0.0255(10) Uani 1 1 d . . . H12 H 0.5731 0.3861 0.1453 0.038 Uiso 1 1 calc R . . H13 H 0.5720 0.4118 0.2567 0.038 Uiso 1 1 calc R . . H11 H 0.5070 0.3262 0.2060 0.038 Uiso 1 1 calc R . . C13 C 0.8515(3) 0.2935(3) 0.3308(3) 0.0200(9) Uani 1 1 d . . . O10 O 0.7282(2) -0.01839(19) 0.4100(2) 0.0260(7) Uani 1 1 d . . . N6 N 0.7013(3) 0.0422(3) 0.4644(3) 0.0258(8) Uani 1 1 d . . . C4 C 0.8096(3) -0.1250(3) 0.2505(3) 0.0227(9) Uani 1 1 d . . . O12 O 0.9378(3) -0.3347(2) 0.2932(3) 0.0408(9) Uani 1 1 d . . . C15 C 1.1172(3) 0.3700(3) 0.4668(3) 0.0218(9) Uani 1 1 d . . . H16 H 1.1079 0.4335 0.4603 0.026 Uiso 1 1 calc R . . C1 C 1.0751(3) -0.0468(3) 0.3976(3) 0.0284(10) Uani 1 1 d . . . H1 H 1.1170 -0.0045 0.3678 0.043 Uiso 1 1 calc R . . H2 H 1.1015 -0.1083 0.3931 0.043 Uiso 1 1 calc R . . H3 H 1.0808 -0.0310 0.4669 0.043 Uiso 1 1 calc R . . C2 C 0.9613(3) -0.0418(3) 0.3435(3) 0.0218(9) Uani 1 1 d . . . C14 C 1.0361(3) 0.3117(3) 0.4228(3) 0.0198(9) Uani 1 1 d . . . C3 C 0.9128(3) -0.1210(3) 0.3070(3) 0.0230(9) Uani 1 1 d . . . N5 N 0.5318(3) 0.0558(2) 0.1750(3) 0.0245(8) Uani 1 1 d . . . O11 O 0.6684(3) 0.0239(2) 0.5373(2) 0.0404(9) Uani 1 1 d . . . C16 C 1.2108(3) 0.3348(3) 0.5196(3) 0.0252(10) Uani 1 1 d . . . H17 H 1.2655 0.3743 0.5507 0.030 Uiso 1 1 calc R . . O14 O 0.8176(3) -0.4355(2) 0.2906(3) 0.0397(9) Uani 1 1 d . . . O8 O 0.4395(2) 0.0532(2) 0.1324(2) 0.0368(8) Uani 1 1 d . . . C12 C 0.7619(3) 0.3433(3) 0.2912(3) 0.0238(10) Uani 1 1 d . . . N2 N 0.6104(3) -0.1588(2) 0.1191(3) 0.0214(8) Uani 1 1 d D . . C5 C 0.6708(3) -0.2277(3) 0.1642(3) 0.0199(9) Uani 1 1 d . . . C6 C 0.6331(3) -0.3155(3) 0.1466(3) 0.0222(9) Uani 1 1 d . . . H6 H 0.6729 -0.3653 0.1779 0.027 Uiso 1 1 calc R . . C17 C 1.2260(3) 0.2417(3) 0.5276(3) 0.0254(10) Uani 1 1 d . . . H18 H 1.2903 0.2172 0.5639 0.030 Uiso 1 1 calc R . . C18 C 1.1459(3) 0.1866(3) 0.4819(3) 0.0261(10) Uani 1 1 d . . . H19 H 1.1548 0.1230 0.4861 0.031 Uiso 1 1 calc R . . C19 C 0.8109(5) 0.1851(4) 0.0740(4) 0.0613(19) Uani 1 1 d . . . H22 H 0.7710 0.2342 0.0958 0.092 Uiso 1 1 calc R . . H23 H 0.7723 0.1625 0.0101 0.092 Uiso 1 1 calc R . . H21 H 0.8800 0.2076 0.0677 0.092 Uiso 1 1 calc R . . C9 C 0.5162(3) -0.1715(3) 0.0568(3) 0.0247(10) Uani 1 1 d . . . H9 H 0.4769 -0.1211 0.0265 0.030 Uiso 1 1 calc R . . C8 C 0.4775(3) -0.2566(3) 0.0374(3) 0.0289(10) Uani 1 1 d . . . H8 H 0.4113 -0.2663 -0.0063 0.035 Uiso 1 1 calc R . . C7 C 0.5368(4) -0.3290(3) 0.0829(3) 0.0287(10) Uani 1 1 d . . . H7 H 0.5107 -0.3887 0.0699 0.034 Uiso 1 1 calc R . . H14 H 0.768(3) 0.402(3) 0.293(3) 0.014(11) Uiso 1 1 d . . . H15 H 0.940(4) 0.4027(8) 0.367(3) 0.032(13) Uiso 1 1 d D . . H10 H 0.644(3) -0.1074(18) 0.133(4) 0.041(15) Uiso 1 1 d D . . H4 H 0.957(4) -0.177(3) 0.320(3) 0.037(14) Uiso 1 1 d . . . H20 H 1.005(2) 0.184(2) 0.401(3) 0.021(12) Uiso 1 1 d D . . H24 H 0.8882(15) 0.100(4) 0.154(5) 0.08(2) 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 Er1 0.01679(9) 0.01460(9) 0.02135(10) 0.00118(8) 0.00119(7) 0.00084(8) O2 0.0261(16) 0.0150(13) 0.0296(17) -0.0000(13) -0.0003(13) 0.0080(13) O4 0.0210(16) 0.0122(14) 0.0356(18) 0.0019(12) 0.0017(13) -0.0011(12) O3 0.0276(17) 0.0123(14) 0.0331(18) 0.0020(12) -0.0009(14) 0.0026(12) O5 0.0230(18) 0.039(2) 0.0276(18) 0.0083(14) 0.0071(15) -0.0028(15) O6 0.0218(16) 0.0237(15) 0.0246(17) 0.0034(13) 0.0033(13) -0.0018(12) O1 0.0196(15) 0.0166(15) 0.0260(16) 0.0016(12) -0.0001(12) 0.0021(12) N7 0.028(2) 0.0165(17) 0.030(2) -0.0015(16) 0.0098(16) 0.0046(16) O7 0.0222(16) 0.0229(15) 0.0268(17) 0.0004(13) 0.0023(13) 0.0028(12) N1 0.0190(19) 0.0171(17) 0.0236(19) 0.0026(15) -0.0023(15) 0.0040(14) N3 0.0215(19) 0.0109(17) 0.029(2) 0.0018(15) 0.0037(16) 0.0028(14) O9 0.0255(17) 0.0212(15) 0.0273(18) -0.0013(13) 0.0024(14) 0.0019(13) N4 0.0195(18) 0.0184(18) 0.026(2) 0.0009(15) 0.0031(15) -0.0003(15) O13 0.0288(18) 0.0209(16) 0.0359(19) 0.0042(14) 0.0011(15) 0.0062(13) C11 0.026(2) 0.020(2) 0.020(2) 0.0037(17) 0.0069(18) 0.0085(18) C10 0.021(2) 0.021(2) 0.033(3) 0.0020(19) 0.003(2) 0.0063(18) C13 0.023(2) 0.018(2) 0.019(2) -0.0023(16) 0.0058(18) -0.0008(17) O10 0.0290(17) 0.0183(15) 0.0301(18) 0.0008(13) 0.0049(14) 0.0031(13) N6 0.0206(19) 0.030(2) 0.026(2) 0.0028(17) 0.0031(16) 0.0032(16) C4 0.023(2) 0.023(2) 0.022(2) 0.0056(18) 0.0047(19) -0.0011(18) O12 0.054(2) 0.0179(17) 0.054(2) 0.0089(16) 0.0197(19) 0.0010(16) C15 0.021(2) 0.017(2) 0.027(2) -0.0028(18) 0.0063(19) -0.0005(17) C1 0.024(2) 0.022(2) 0.037(3) 0.003(2) 0.003(2) 0.0047(19) C2 0.022(2) 0.025(2) 0.020(2) 0.0029(18) 0.0079(18) -0.0002(18) C14 0.022(2) 0.018(2) 0.020(2) 0.0013(17) 0.0062(17) 0.0015(17) C3 0.020(2) 0.022(2) 0.025(2) 0.0003(18) 0.0025(18) 0.0073(18) N5 0.024(2) 0.0147(17) 0.032(2) 0.0037(15) -0.0012(17) -0.0009(15) O11 0.043(2) 0.053(2) 0.0291(19) 0.0091(17) 0.0158(17) 0.0048(18) C16 0.023(2) 0.030(2) 0.022(2) -0.0061(19) 0.0043(18) -0.0088(19) O14 0.0230(18) 0.039(2) 0.052(2) -0.0062(17) -0.0032(16) 0.0013(15) O8 0.0165(16) 0.045(2) 0.043(2) 0.0086(17) -0.0065(15) -0.0012(14) C12 0.025(2) 0.016(2) 0.029(3) 0.0025(18) 0.0039(19) -0.0003(18) N2 0.0163(18) 0.0216(19) 0.024(2) 0.0014(16) 0.0004(15) 0.0006(15) C5 0.024(2) 0.019(2) 0.017(2) 0.0009(17) 0.0043(17) -0.0003(17) C6 0.018(2) 0.020(2) 0.027(2) 0.0016(18) 0.0027(18) -0.0016(17) C17 0.020(2) 0.032(3) 0.024(2) 0.0027(19) 0.0042(19) 0.0020(19) C18 0.026(2) 0.024(2) 0.028(3) 0.0049(19) 0.006(2) 0.0035(19) C19 0.055(4) 0.078(5) 0.056(4) 0.028(4) 0.025(3) 0.028(3) C9 0.018(2) 0.033(2) 0.021(2) 0.0055(19) -0.0006(18) 0.0033(18) C8 0.022(2) 0.035(3) 0.026(2) 0.002(2) -0.0035(19) -0.0065(19) C7 0.028(2) 0.024(2) 0.035(3) -0.000(2) 0.009(2) -0.0075(19) _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 Er1 O3 2.282(3) . ? Er1 O2 2.313(3) . ? Er1 O4 2.329(3) . ? Er1 O1 2.334(3) . ? Er1 O5 2.346(3) . ? Er1 O9 2.416(3) . ? Er1 O6 2.453(3) . ? Er1 O10 2.484(3) . ? Er1 O7 2.511(3) . ? O2 C4 1.269(5) . ? O4 C13 1.257(5) . ? O3 C11 1.267(5) . ? O5 C19 1.398(6) . ? O5 H24 0.840(10) . ? O6 N5 1.267(4) . ? O1 C2 1.278(5) . ? N7 O14 1.241(5) . ? N7 O12 1.241(4) . ? N7 O13 1.260(4) . ? O7 N5 1.278(5) . ? N1 C5 1.359(5) . ? N1 C4 1.400(5) . ? N1 H5 0.8800 . ? N3 C14 1.359(5) . ? N3 C13 1.405(5) . ? N3 H15 0.875(10) . ? O9 N6 1.277(5) . ? N4 C18 1.349(5) . ? N4 C14 1.357(5) . ? N4 H20 0.883(10) . ? C11 C12 1.396(6) . ? C11 C10 1.517(5) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H11 0.9800 . ? C13 C12 1.387(6) . ? O10 N6 1.272(4) . ? N6 O11 1.215(5) . ? C4 C3 1.401(6) . ? C15 C16 1.380(6) . ? C15 C14 1.396(6) . ? C15 H16 0.9500 . ? C1 C2 1.508(6) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 C3 1.376(6) . ? C3 H4 1.01(5) . ? N5 O8 1.218(4) . ? C16 C17 1.395(6) . ? C16 H17 0.9500 . ? C12 H14 0.88(4) . ? N2 C9 1.349(5) . ? N2 C5 1.356(5) . ? N2 H10 0.880(10) . ? C5 C6 1.394(5) . ? C6 C7 1.382(6) . ? C6 H6 0.9500 . ? C17 C18 1.365(6) . ? C17 H18 0.9500 . ? C18 H19 0.9500 . ? C19 H22 0.9800 . ? C19 H23 0.9800 . ? C19 H21 0.9800 . ? C9 C8 1.363(6) . ? C9 H9 0.9500 . ? C8 C7 1.390(6) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? 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 O3 Er1 O2 137.90(10) . . ? O3 Er1 O4 73.19(10) . . ? O2 Er1 O4 140.51(10) . . ? O3 Er1 O1 142.23(10) . . ? O2 Er1 O1 73.51(10) . . ? O4 Er1 O1 69.92(9) . . ? O3 Er1 O5 86.38(11) . . ? O2 Er1 O5 80.05(11) . . ? O4 Er1 O5 78.82(11) . . ? O1 Er1 O5 78.90(11) . . ? O3 Er1 O9 82.98(10) . . ? O2 Er1 O9 122.74(10) . . ? O4 Er1 O9 75.76(10) . . ? O1 Er1 O9 95.53(10) . . ? O5 Er1 O9 154.34(11) . . ? O3 Er1 O6 72.19(10) . . ? O2 Er1 O6 83.62(10) . . ? O4 Er1 O6 135.58(10) . . ? O1 Er1 O6 143.48(10) . . ? O5 Er1 O6 125.24(11) . . ? O9 Er1 O6 73.17(10) . . ? O3 Er1 O10 127.26(10) . . ? O2 Er1 O10 70.86(10) . . ? O4 Er1 O10 113.12(10) . . ? O1 Er1 O10 76.14(10) . . ? O5 Er1 O10 145.90(11) . . ? O9 Er1 O10 52.12(9) . . ? O6 Er1 O10 69.54(10) . . ? O3 Er1 O7 70.84(10) . . ? O2 Er1 O7 67.14(10) . . ? O4 Er1 O7 135.78(10) . . ? O1 Er1 O7 135.20(10) . . ? O5 Er1 O7 74.11(11) . . ? O9 Er1 O7 123.33(10) . . ? O6 Er1 O7 51.44(10) . . ? O10 Er1 O7 108.88(10) . . ? C4 O2 Er1 133.4(3) . . ? C13 O4 Er1 134.5(3) . . ? C11 O3 Er1 137.8(3) . . ? C19 O5 Er1 131.4(3) . . ? C19 O5 H24 107(4) . . ? Er1 O5 H24 113(4) . . ? N5 O6 Er1 97.5(2) . . ? C2 O1 Er1 133.7(3) . . ? O14 N7 O12 120.7(4) . . ? O14 N7 O13 119.7(4) . . ? O12 N7 O13 119.6(4) . . ? N5 O7 Er1 94.4(2) . . ? C5 N1 C4 126.4(3) . . ? C5 N1 H5 116.8 . . ? C4 N1 H5 116.8 . . ? C14 N3 C13 127.2(3) . . ? C14 N3 H15 113(3) . . ? C13 N3 H15 119(3) . . ? N6 O9 Er1 97.3(2) . . ? C18 N4 C14 122.7(4) . . ? C18 N4 H20 118(3) . . ? C14 N4 H20 119(3) . . ? O3 C11 C12 124.7(4) . . ? O3 C11 C10 116.9(4) . . ? C12 C11 C10 118.5(4) . . ? C11 C10 H12 109.5 . . ? C11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C11 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? O4 C13 C12 127.4(4) . . ? O4 C13 N3 116.8(4) . . ? C12 C13 N3 115.8(4) . . ? N6 O10 Er1 94.2(2) . . ? O11 N6 O10 122.2(4) . . ? O11 N6 O9 122.5(4) . . ? O10 N6 O9 115.3(3) . . ? O2 C4 N1 117.3(4) . . ? O2 C4 C3 124.9(4) . . ? N1 C4 C3 117.8(4) . . ? C16 C15 C14 119.5(4) . . ? C16 C15 H16 120.2 . . ? C14 C15 H16 120.2 . . ? C2 C1 H1 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? O1 C2 C3 126.5(4) . . ? O1 C2 C1 115.9(4) . . ? C3 C2 C1 117.6(4) . . ? N4 C14 N3 120.7(4) . . ? N4 C14 C15 118.1(4) . . ? N3 C14 C15 121.2(4) . . ? C2 C3 C4 123.3(4) . . ? C2 C3 H4 116(3) . . ? C4 C3 H4 120(3) . . ? O8 N5 O6 122.7(4) . . ? O8 N5 O7 121.6(4) . . ? O6 N5 O7 115.7(3) . . ? C15 C16 C17 120.6(4) . . ? C15 C16 H17 119.7 . . ? C17 C16 H17 119.7 . . ? C13 C12 C11 122.1(4) . . ? C13 C12 H14 117(3) . . ? C11 C12 H14 120(3) . . ? C9 N2 C5 123.0(4) . . ? C9 N2 H10 127(3) . . ? C5 N2 H10 110(3) . . ? N2 C5 N1 119.9(4) . . ? N2 C5 C6 118.4(4) . . ? N1 C5 C6 121.6(4) . . ? C7 C6 C5 118.8(4) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C18 C17 C16 118.3(4) . . ? C18 C17 H18 120.8 . . ? C16 C17 H18 120.8 . . ? N4 C18 C17 120.7(4) . . ? N4 C18 H19 119.6 . . ? C17 C18 H19 119.6 . . ? O5 C19 H22 109.5 . . ? O5 C19 H23 109.5 . . ? H22 C19 H23 109.5 . . ? O5 C19 H21 109.5 . . ? H22 C19 H21 109.5 . . ? H23 C19 H21 109.5 . . ? N2 C9 C8 120.0(4) . . ? N2 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C8 C7 118.7(4) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C6 C7 C8 121.0(4) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.964 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.169 data_11c:\users\nick\desktop\honour~1\y(paah~1\p-1 _database_code_depnum_ccdc_archive 'CCDC 914683' #TrackingRef '11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H12 N5 O12 Y' _chemical_formula_weight 471.15 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' Y Y -2.7962 3.5667 '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 7.4349(15) _cell_length_b 10.630(2) _cell_length_c 11.657(2) _cell_angle_alpha 68.02(3) _cell_angle_beta 88.31(3) _cell_angle_gamma 87.44(3) _cell_volume 853.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour clear _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 3.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_T_max 0.705 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10436 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.1072 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3852 _reflns_number_gt 3394 _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. The asymmetric unit contains the entire cluster. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H12, H17, H30 and H36 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. ; _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^)+(0.0000P)^2^+4.4432P] 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 3852 _refine_ls_number_parameters 257 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_restrained_S_all 1.274 _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 Y1 Y 0.57630(8) 0.80093(6) 0.73966(6) 0.01144(18) Uani 1 1 d . . . O2 O 0.6221(6) 1.0305(5) 0.6683(4) 0.0252(11) Uani 1 1 d . . . O3 O 0.3650(7) 0.8546(5) 0.5846(5) 0.0278(12) Uani 1 1 d D . . O4 O 0.7252(7) 0.8392(5) 0.5389(5) 0.0310(12) Uani 1 1 d . . . O5 O 0.7023(7) 0.8352(5) 0.9008(5) 0.0275(12) Uani 1 1 d . . . O6 O 0.2960(7) 0.6908(5) 0.8372(5) 0.0308(12) Uani 1 1 d . . . O7 O 0.6716(8) 0.5839(5) 0.8973(5) 0.0368(14) Uani 1 1 d . . . O8 O 0.3290(7) 0.8934(5) 0.8363(5) 0.0314(13) Uani 1 1 d . . . O1 O 0.0937(7) 0.7766(6) 0.9314(5) 0.0392(14) Uani 1 1 d . . . O9 O 1.0171(7) 0.8317(7) 0.5075(6) 0.0488(17) Uani 1 1 d . . . N3 N 0.2318(8) 0.7850(6) 0.8707(6) 0.0273(14) Uani 1 1 d . . . N4 N 0.8865(9) 0.8216(7) 0.5782(7) 0.0336(16) Uani 1 1 d . . . O10 O 0.9044(7) 0.7888(6) 0.6944(5) 0.0352(13) Uani 1 1 d . . . O12 O 0.5864(8) 0.5790(5) 0.7231(5) 0.0353(13) Uani 1 1 d . . . N8 N 0.7661(8) 0.9159(6) 1.0500(6) 0.0261(14) Uani 1 1 d D . . C9 C 0.6514(10) 1.1150(7) 0.7226(7) 0.0260(16) Uani 1 1 d . . . C10 C 0.6920(10) 1.0765(7) 0.8465(7) 0.0285(17) Uani 1 1 d . . . H10 H 0.7033 1.1458 0.8786 0.034 Uiso 1 1 calc R . . O11 O 0.6341(10) 0.3875(6) 0.8813(6) 0.059(2) Uani 1 1 d . . . N13 N 0.6329(9) 0.5116(6) 0.8373(7) 0.0356(17) Uani 1 1 d . . . C14 C 0.8003(10) 0.7915(7) 1.1429(7) 0.0245(16) Uani 1 1 d . . . C15 C 0.7177(9) 0.9391(7) 0.9285(7) 0.0251(16) Uani 1 1 d . . . C17 C 0.6443(11) 1.2645(7) 0.6422(7) 0.0333(19) Uani 1 1 d . . . H17A H 0.7513 1.2862 0.5882 0.050 Uiso 1 1 calc R . . H17B H 0.6411 1.3181 0.6948 0.050 Uiso 1 1 calc R . . H17C H 0.5360 1.2861 0.5916 0.050 Uiso 1 1 calc R . . N1 N 0.8175(9) 0.6780(6) 1.1169(6) 0.0278(14) Uani 1 1 d D . . C2 C 0.8550(11) 0.5521(8) 1.2035(8) 0.0343(19) Uani 1 1 d . . . H2 H 0.8687 0.4756 1.1802 0.041 Uiso 1 1 calc R . . C3 C 0.8205(11) 0.7801(8) 1.2648(7) 0.0327(19) Uani 1 1 d . . . H3 H 0.8111 0.8583 1.2859 0.039 Uiso 1 1 calc R . . C4 C 0.8726(12) 0.5375(8) 1.3232(8) 0.041(2) Uani 1 1 d . . . H4 H 0.8968 0.4504 1.3851 0.049 Uiso 1 1 calc R . . C5 C 0.8546(12) 0.6528(9) 1.3548(8) 0.041(2) Uani 1 1 d . . . H5 H 0.8658 0.6433 1.4386 0.049 Uiso 1 1 calc R . . H12 H 0.378(12) 0.895(8) 0.5075(16) 0.049 Uiso 1 1 d D . . H17 H 0.263(5) 0.825(8) 0.611(8) 0.049 Uiso 1 1 d D . . H30 H 0.836(12) 0.671(9) 1.045(4) 0.049 Uiso 1 1 d D . . H36 H 0.769(12) 0.983(6) 1.077(8) 0.049 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 Y1 0.0118(3) 0.0134(3) 0.0104(3) -0.0059(2) -0.0020(2) 0.0005(2) O2 0.028(3) 0.031(3) 0.019(3) -0.012(2) 0.001(2) -0.003(2) O3 0.021(3) 0.041(3) 0.019(3) -0.008(3) 0.001(2) -0.006(2) O4 0.026(3) 0.046(3) 0.024(3) -0.016(3) -0.003(2) 0.000(2) O5 0.030(3) 0.030(3) 0.026(3) -0.015(2) -0.006(2) 0.004(2) O6 0.039(3) 0.026(3) 0.034(3) -0.018(2) 0.000(3) -0.001(2) O7 0.050(4) 0.035(3) 0.032(3) -0.021(3) -0.015(3) 0.005(3) O8 0.030(3) 0.030(3) 0.039(3) -0.018(3) 0.002(3) -0.006(2) O1 0.027(3) 0.059(4) 0.034(3) -0.020(3) 0.005(3) -0.003(3) O9 0.024(3) 0.089(5) 0.047(4) -0.041(4) 0.008(3) -0.007(3) N3 0.027(3) 0.035(4) 0.019(3) -0.009(3) -0.001(3) -0.002(3) N4 0.025(4) 0.046(4) 0.038(4) -0.024(4) -0.007(3) 0.003(3) O10 0.033(3) 0.051(3) 0.025(3) -0.019(3) -0.009(3) 0.006(3) O12 0.053(4) 0.032(3) 0.021(3) -0.011(2) -0.011(3) 0.009(3) N8 0.035(4) 0.025(3) 0.023(3) -0.014(3) -0.005(3) -0.000(3) C9 0.028(4) 0.023(4) 0.025(4) -0.007(3) -0.001(3) 0.002(3) C10 0.038(4) 0.026(4) 0.022(4) -0.008(3) -0.004(3) -0.004(3) O11 0.109(6) 0.025(3) 0.044(4) -0.013(3) -0.015(4) 0.010(3) N13 0.050(4) 0.026(4) 0.036(4) -0.019(3) -0.009(3) 0.010(3) C14 0.024(4) 0.028(4) 0.025(4) -0.014(3) -0.002(3) 0.001(3) C15 0.020(4) 0.034(4) 0.026(4) -0.017(4) -0.002(3) 0.004(3) C17 0.047(5) 0.029(4) 0.024(4) -0.011(4) 0.002(4) -0.002(4) N1 0.035(4) 0.026(3) 0.023(4) -0.011(3) -0.004(3) -0.005(3) C2 0.046(5) 0.027(4) 0.029(5) -0.010(4) -0.006(4) 0.002(4) C3 0.039(5) 0.035(4) 0.026(4) -0.015(4) -0.009(4) 0.004(4) C4 0.058(6) 0.027(4) 0.035(5) -0.009(4) -0.007(4) -0.000(4) C5 0.051(5) 0.047(5) 0.020(4) -0.008(4) -0.013(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O5 2.277(5) . ? Y1 O2 2.303(5) . ? Y1 O3 2.319(5) . ? Y1 O12 2.435(5) . ? Y1 O7 2.441(5) . ? Y1 O4 2.458(5) . ? Y1 O6 2.467(5) . ? Y1 O8 2.482(5) . ? Y1 O10 2.488(5) . ? O2 C9 1.306(8) . ? O3 H12 0.843(10) . ? O3 H17 0.840(10) . ? O4 N4 1.277(8) . ? O5 C15 1.273(8) . ? O6 N3 1.275(8) . ? O7 N13 1.264(8) . ? O8 N3 1.312(8) . ? O1 N3 1.217(8) . ? O9 N4 1.236(9) . ? N4 O10 1.276(8) . ? O12 N13 1.302(8) . ? N8 C14 1.378(9) . ? N8 C15 1.399(9) . ? N8 H36 0.881(10) . ? C9 C10 1.385(10) . ? C9 C17 1.512(10) . ? C10 C15 1.423(10) . ? C10 H10 0.9500 . ? O11 N13 1.223(8) . ? C14 N1 1.349(9) . ? C14 C3 1.392(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N1 C2 1.364(10) . ? N1 H30 0.881(10) . ? C2 C4 1.355(11) . ? C2 H2 0.9500 . ? C3 C5 1.385(11) . ? C3 H3 0.9500 . ? C4 C5 1.405(12) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? 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 O5 Y1 O2 75.07(18) . . ? O5 Y1 O3 151.56(19) . . ? O2 Y1 O3 85.80(18) . . ? O5 Y1 O12 121.94(18) . . ? O2 Y1 O12 154.11(18) . . ? O3 Y1 O12 83.79(19) . . ? O5 Y1 O7 69.91(17) . . ? O2 Y1 O7 142.81(17) . . ? O3 Y1 O7 131.38(18) . . ? O12 Y1 O7 52.70(17) . . ? O5 Y1 O4 125.02(18) . . ? O2 Y1 O4 78.52(18) . . ? O3 Y1 O4 69.50(17) . . ? O12 Y1 O4 75.64(18) . . ? O7 Y1 O4 111.97(18) . . ? O5 Y1 O6 101.07(18) . . ? O2 Y1 O6 125.41(17) . . ? O3 Y1 O6 72.99(18) . . ? O12 Y1 O6 73.58(18) . . ? O7 Y1 O6 74.43(19) . . ? O4 Y1 O6 133.30(17) . . ? O5 Y1 O8 74.22(17) . . ? O2 Y1 O8 75.49(17) . . ? O3 Y1 O8 80.81(18) . . ? O12 Y1 O8 125.72(18) . . ? O7 Y1 O8 105.82(19) . . ? O4 Y1 O8 141.61(18) . . ? O6 Y1 O8 52.15(16) . . ? O5 Y1 O10 77.36(18) . . ? O2 Y1 O10 82.88(18) . . ? O3 Y1 O10 121.48(18) . . ? O12 Y1 O10 82.50(19) . . ? O7 Y1 O10 77.74(19) . . ? O4 Y1 O10 51.99(17) . . ? O6 Y1 O10 150.74(18) . . ? O8 Y1 O10 147.80(17) . . ? C9 O2 Y1 133.7(4) . . ? Y1 O3 H12 130(6) . . ? Y1 O3 H17 113(6) . . ? H12 O3 H17 117(9) . . ? N4 O4 Y1 96.6(4) . . ? C15 O5 Y1 133.7(5) . . ? N3 O6 Y1 97.5(4) . . ? N13 O7 Y1 96.2(4) . . ? N3 O8 Y1 95.8(4) . . ? O1 N3 O6 123.8(6) . . ? O1 N3 O8 121.7(6) . . ? O6 N3 O8 114.5(6) . . ? O9 N4 O10 122.2(6) . . ? O9 N4 O4 121.5(7) . . ? O10 N4 O4 116.2(6) . . ? N4 O10 Y1 95.1(4) . . ? N13 O12 Y1 95.4(4) . . ? C14 N8 C15 126.6(6) . . ? C14 N8 H36 112(6) . . ? C15 N8 H36 121(6) . . ? O2 C9 C10 124.5(6) . . ? O2 C9 C17 116.8(6) . . ? C10 C9 C17 118.7(7) . . ? C9 C10 C15 123.7(7) . . ? C9 C10 H10 118.1 . . ? C15 C10 H10 118.1 . . ? O11 N13 O7 123.9(7) . . ? O11 N13 O12 121.1(6) . . ? O7 N13 O12 115.0(6) . . ? N1 C14 N8 120.4(7) . . ? N1 C14 C3 118.5(7) . . ? N8 C14 C3 121.1(7) . . ? O5 C15 N8 116.9(6) . . ? O5 C15 C10 125.7(7) . . ? N8 C15 C10 117.4(6) . . ? C9 C17 H17A 109.5 . . ? C9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 N1 C2 123.7(7) . . ? C14 N1 H30 129(6) . . ? C2 N1 H30 106(6) . . ? C4 C2 N1 119.1(7) . . ? C4 C2 H2 120.4 . . ? N1 C2 H2 120.4 . . ? C5 C3 C14 118.8(7) . . ? C5 C3 H3 120.6 . . ? C14 C3 H3 120.6 . . ? C2 C4 C5 119.2(8) . . ? C2 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C3 C5 C4 120.6(8) . . ? C3 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.731 _refine_diff_density_min -2.414 _refine_diff_density_rms 0.150 data_2c:\users\nick\desktop\ _database_code_depnum_ccdc_archive 'CCDC 914684' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cl3 N4 O10 Tb' _chemical_formula_weight 729.75 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8490(18) _cell_length_b 11.157(2) _cell_length_c 14.564(3) _cell_angle_alpha 103.13(3) _cell_angle_beta 93.56(3) _cell_angle_gamma 91.72(3) _cell_volume 1396.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 2.874 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71090 _diffrn_radiation_type synchrotron _diffrn_radiation_source '3BM1 dipole' _diffrn_radiation_monochromator 'double crystal' _diffrn_measurement_device_type synchrotron _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28286 _diffrn_reflns_av_R_equivalents 0.1334 _diffrn_reflns_av_sigmaI/netI 0.1234 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 30.88 _reflns_number_total 7446 _reflns_number_gt 7111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. The crystal was run on the Australian synchrotron in which we were restricted to only one 185 degree phi scan. The asymmetric unit contains the entire cluster as well as two water molecules and three chloride ions. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20, H21, H22, H23, H24, H25, H26, H27 and H28 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. The hydrogen atoms for the lattice water molecules (O9 and O10) were omitted due to uncertainties in thier position. ; _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^)+(0.0100P)^2^+2.2318P] 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 7446 _refine_ls_number_parameters 363 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.003 _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 Tb1 Tb 0.31943(2) 0.201343(14) 0.301578(10) 0.01696(9) Uani 1 1 d . . . Cl1 Cl 0.23321(14) -0.19781(9) 0.09737(7) 0.0269(2) Uani 1 1 d . . . Cl2 Cl -0.16383(13) 0.06776(9) 0.29498(7) 0.0229(2) Uani 1 1 d . . . O3 O 0.3374(4) 0.3430(3) 0.2105(2) 0.0236(6) Uani 1 1 d . . . O1 O 0.4050(4) 0.0145(3) 0.3273(2) 0.0232(6) Uani 1 1 d . . . O4 O 0.4537(4) 0.1101(3) 0.1700(2) 0.0209(6) Uani 1 1 d . . . O2 O 0.2088(4) 0.1681(3) 0.4343(2) 0.0243(6) Uani 1 1 d . . . O6 O 0.1425(4) 0.0553(3) 0.2021(2) 0.0253(6) Uani 1 1 d D . . N1 N 0.1361(5) 0.1087(3) 0.5644(2) 0.0218(7) Uani 1 1 d D . . O8 O 0.3515(4) 0.4011(3) 0.4114(2) 0.0245(6) Uani 1 1 d D . . C12 C 0.5318(5) 0.2809(4) 0.1077(3) 0.0199(7) Uani 1 1 d . . . H14 H 0.6003 0.3072 0.0677 0.024 Uiso 1 1 calc R . . N2 N 0.0068(5) 0.2809(3) 0.5389(3) 0.0222(7) Uani 1 1 d D . . C3 C 0.2930(6) -0.0221(4) 0.4634(3) 0.0223(8) Uani 1 1 d . . . H4 H 0.2851 -0.0777 0.5036 0.027 Uiso 1 1 calc R . . C14 C 0.6767(6) -0.0308(4) 0.0720(3) 0.0218(8) Uani 1 1 d . . . C13 C 0.5356(5) 0.1588(4) 0.1185(3) 0.0189(7) Uani 1 1 d . . . N3 N 0.6390(5) 0.0854(3) 0.0662(2) 0.0217(7) Uani 1 1 d D . . O7 O 0.5804(5) 0.2444(3) 0.3562(3) 0.0305(7) Uani 1 1 d D . . C9 C -0.0865(6) 0.3766(4) 0.5669(3) 0.0266(9) Uani 1 1 d . . . H9 H -0.1149 0.4270 0.5247 0.032 Uiso 1 1 calc R . . C4 C 0.2158(5) 0.0867(4) 0.4831(3) 0.0198(7) Uani 1 1 d . . . C6 C -0.0066(6) 0.2257(4) 0.6867(3) 0.0262(9) Uani 1 1 d . . . H6 H 0.0198 0.1727 0.7272 0.031 Uiso 1 1 calc R . . N4 N 0.5996(5) -0.0929(3) 0.1257(3) 0.0207(6) Uani 1 1 d D . . C2 C 0.3823(5) -0.0519(4) 0.3855(3) 0.0211(8) Uani 1 1 d . . . C5 C 0.0451(5) 0.2056(4) 0.5956(3) 0.0196(7) Uani 1 1 d . . . C15 C 0.7924(5) -0.0885(4) 0.0207(3) 0.0253(8) Uani 1 1 d . . . H16 H 0.8457 -0.0481 -0.0192 0.030 Uiso 1 1 calc R . . C7 C -0.0959(6) 0.3233(4) 0.7161(3) 0.0273(9) Uani 1 1 d . . . H7 H -0.1293 0.3397 0.7783 0.033 Uiso 1 1 calc R . . C8 C -0.1384(6) 0.3993(4) 0.6550(3) 0.0288(9) Uani 1 1 d . . . H8 H -0.2025 0.4657 0.6748 0.035 Uiso 1 1 calc R . . C1 C 0.4580(6) -0.1741(4) 0.3678(3) 0.0269(9) Uani 1 1 d . . . H2 H 0.4074 -0.2301 0.3119 0.040 Uiso 1 1 calc R . . H3 H 0.4507 -0.2102 0.4229 0.040 Uiso 1 1 calc R . . H1 H 0.5649 -0.1612 0.3572 0.040 Uiso 1 1 calc R . . C10 C 0.4344(7) 0.4922(4) 0.1343(3) 0.0313(11) Uani 1 1 d . . . H12 H 0.3313 0.5133 0.1175 0.047 Uiso 1 1 calc R . . H13 H 0.4982 0.4938 0.0819 0.047 Uiso 1 1 calc R . . H11 H 0.4761 0.5521 0.1910 0.047 Uiso 1 1 calc R . . C11 C 0.4309(5) 0.3653(4) 0.1536(3) 0.0195(7) Uani 1 1 d . . . C18 C 0.6345(6) -0.2074(4) 0.1340(3) 0.0270(9) Uani 1 1 d . . . H19 H 0.5789 -0.2472 0.1731 0.032 Uiso 1 1 calc R . . C16 C 0.8284(6) -0.2057(4) 0.0288(3) 0.0289(9) Uani 1 1 d . . . H17 H 0.9080 -0.2456 -0.0053 0.035 Uiso 1 1 calc R . . C17 C 0.7496(7) -0.2661(4) 0.0862(3) 0.0306(10) Uani 1 1 d . . . H18 H 0.7753 -0.3462 0.0920 0.037 Uiso 1 1 calc R . . Cl3 Cl 0.66627(16) 0.52387(11) 0.37383(8) 0.0322(3) Uani 1 1 d . . . O9 O 0.1194(6) -0.4501(3) -0.0355(3) 0.0382(9) Uani 1 1 d . . . O10 O -0.1214(8) 0.4076(5) 0.2141(3) 0.0602(16) Uani 1 1 d . . . O5 O 0.0653(4) 0.2869(3) 0.3134(3) 0.0254(6) Uani 1 1 d D . . H10 H 0.031(8) 0.261(6) 0.4796(18) 0.031 Uiso 1 1 d D . . H5 H 0.131(8) 0.061(5) 0.605(4) 0.031 Uiso 1 1 d D . . H15 H 0.677(8) 0.106(6) 0.017(3) 0.031 Uiso 1 1 d D . . H20 H 0.528(6) -0.056(5) 0.159(4) 0.031 Uiso 1 1 d D . . H22 H 0.654(5) 0.199(5) 0.350(5) 0.031 Uiso 1 1 d D . . H21 H 0.614(8) 0.318(2) 0.373(5) 0.031 Uiso 1 1 d D . . H28 H 0.200(7) -0.004(4) 0.187(5) 0.031 Uiso 1 1 d D . . H27 H 0.053(3) 0.059(6) 0.218(5) 0.031 Uiso 1 1 d D . . H26 H 0.014(7) 0.221(4) 0.311(5) 0.031 Uiso 1 1 d D . . H25 H 0.024(7) 0.351(4) 0.305(5) 0.031 Uiso 1 1 d D . . H23 H 0.424(5) 0.434(5) 0.390(5) 0.031 Uiso 1 1 d D . . H24 H 0.359(8) 0.403(6) 0.4695(12) 0.031 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 Tb1 0.02012(15) 0.01997(12) 0.01070(11) 0.00225(7) 0.00441(7) 0.00222(7) Cl1 0.0323(7) 0.0273(4) 0.0203(4) 0.0026(3) 0.0093(4) -0.0020(4) Cl2 0.0198(6) 0.0283(4) 0.0221(4) 0.0079(3) 0.0051(3) 0.0035(3) O3 0.033(2) 0.0242(13) 0.0145(12) 0.0037(10) 0.0064(11) 0.0049(11) O1 0.0278(19) 0.0250(13) 0.0182(13) 0.0062(10) 0.0073(11) 0.0048(11) O4 0.0227(18) 0.0239(12) 0.0165(12) 0.0041(10) 0.0064(10) 0.0025(10) O2 0.032(2) 0.0248(13) 0.0174(13) 0.0057(10) 0.0062(11) 0.0077(11) O6 0.0227(19) 0.0283(14) 0.0220(14) -0.0017(11) 0.0070(11) 0.0017(11) N1 0.025(2) 0.0267(15) 0.0158(14) 0.0070(12) 0.0084(12) 0.0053(13) O8 0.0288(19) 0.0269(13) 0.0149(12) -0.0018(10) 0.0043(11) 0.0011(11) C12 0.019(2) 0.0263(17) 0.0152(15) 0.0057(13) 0.0046(13) -0.0002(13) N2 0.021(2) 0.0293(16) 0.0194(15) 0.0098(13) 0.0063(13) 0.0063(13) C3 0.026(2) 0.0248(17) 0.0169(16) 0.0056(13) 0.0045(14) 0.0027(14) C14 0.026(2) 0.0260(17) 0.0118(15) 0.0003(13) 0.0021(13) -0.0002(14) C13 0.019(2) 0.0243(16) 0.0115(14) 0.0012(12) -0.0003(12) 0.0014(13) N3 0.026(2) 0.0262(15) 0.0127(13) 0.0035(11) 0.0068(12) 0.0026(13) O7 0.027(2) 0.0246(14) 0.0359(18) -0.0019(12) 0.0023(14) 0.0062(12) C9 0.023(3) 0.034(2) 0.027(2) 0.0113(16) 0.0119(16) 0.0080(16) C4 0.021(2) 0.0261(17) 0.0120(15) 0.0037(13) 0.0023(13) -0.0009(14) C6 0.034(3) 0.0298(19) 0.0153(16) 0.0049(14) 0.0038(15) 0.0024(16) N4 0.017(2) 0.0263(15) 0.0183(15) 0.0031(12) 0.0064(12) 0.0032(12) C2 0.027(2) 0.0216(15) 0.0134(15) 0.0020(12) 0.0024(13) -0.0002(14) C5 0.016(2) 0.0274(17) 0.0166(16) 0.0066(13) 0.0054(13) 0.0008(13) C15 0.018(2) 0.035(2) 0.0214(18) 0.0034(15) 0.0027(14) 0.0060(16) C7 0.032(3) 0.0308(19) 0.0207(18) 0.0061(15) 0.0111(16) 0.0041(16) C8 0.029(3) 0.033(2) 0.027(2) 0.0093(17) 0.0115(17) 0.0098(17) C1 0.033(3) 0.0237(17) 0.0239(19) 0.0032(14) 0.0027(16) 0.0091(16) C10 0.051(3) 0.0235(18) 0.0227(19) 0.0089(15) 0.0127(19) 0.0047(18) C11 0.021(2) 0.0236(16) 0.0132(15) 0.0033(12) 0.0024(13) 0.0013(13) C18 0.030(3) 0.0262(18) 0.0232(19) 0.0027(15) 0.0025(16) 0.0016(16) C16 0.027(3) 0.035(2) 0.0210(19) -0.0033(16) 0.0015(16) 0.0109(17) C17 0.036(3) 0.0277(19) 0.025(2) -0.0005(15) -0.0031(18) 0.0098(17) Cl3 0.0388(8) 0.0353(5) 0.0196(4) -0.0004(4) 0.0089(4) -0.0057(4) O9 0.054(3) 0.0316(16) 0.0259(17) 0.0005(13) 0.0015(16) 0.0026(16) O10 0.085(4) 0.073(3) 0.028(2) 0.015(2) 0.013(2) 0.042(3) O5 0.0221(19) 0.0249(13) 0.0303(16) 0.0073(12) 0.0044(12) 0.0053(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 Tb1 O3 2.290(3) . ? Tb1 O2 2.318(3) . ? Tb1 O1 2.339(3) . ? Tb1 O4 2.364(3) . ? Tb1 O6 2.387(4) . ? Tb1 O7 2.393(4) . ? Tb1 O8 2.427(3) . ? Tb1 O5 2.470(4) . ? O3 C11 1.265(5) . ? O1 C2 1.268(5) . ? O4 C13 1.269(5) . ? O2 C4 1.275(5) . ? O6 H28 0.840(10) . ? O6 H27 0.838(10) . ? N1 C5 1.378(5) . ? N1 C4 1.392(5) . ? N1 H5 0.880(10) . ? O8 H23 0.839(10) . ? O8 H24 0.841(10) . ? C12 C11 1.404(6) . ? C12 C13 1.408(5) . ? C12 H14 0.9500 . ? N2 C5 1.341(5) . ? N2 C9 1.373(6) . ? N2 H10 0.883(10) . ? C3 C4 1.392(6) . ? C3 C2 1.406(6) . ? C3 H4 0.9500 . ? C14 N4 1.357(5) . ? C14 N3 1.368(5) . ? C14 C15 1.392(6) . ? C13 N3 1.391(5) . ? N3 H15 0.880(10) . ? O7 H22 0.836(10) . ? O7 H21 0.839(10) . ? C9 C8 1.361(6) . ? C9 H9 0.9500 . ? C6 C7 1.369(6) . ? C6 C5 1.402(6) . ? C6 H6 0.9500 . ? N4 C18 1.354(5) . ? N4 H20 0.876(10) . ? C2 C1 1.513(6) . ? C15 C16 1.385(6) . ? C15 H16 0.9500 . ? C7 C8 1.405(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C1 H1 0.9800 . ? C10 C11 1.504(6) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H11 0.9800 . ? C18 C17 1.368(7) . ? C18 H19 0.9500 . ? C16 C17 1.392(8) . ? C16 H17 0.9500 . ? C17 H18 0.9500 . ? O5 H26 0.841(10) . ? O5 H25 0.840(10) . ? 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 O3 Tb1 O2 141.65(11) . . ? O3 Tb1 O1 145.21(11) . . ? O2 Tb1 O1 73.04(11) . . ? O3 Tb1 O4 73.16(11) . . ? O2 Tb1 O4 144.85(10) . . ? O1 Tb1 O4 72.72(11) . . ? O3 Tb1 O6 99.53(12) . . ? O2 Tb1 O6 90.37(12) . . ? O1 Tb1 O6 77.97(12) . . ? O4 Tb1 O6 74.99(12) . . ? O3 Tb1 O7 89.99(14) . . ? O2 Tb1 O7 102.85(14) . . ? O1 Tb1 O7 75.27(12) . . ? O4 Tb1 O7 75.76(12) . . ? O6 Tb1 O7 144.97(11) . . ? O3 Tb1 O8 74.05(11) . . ? O2 Tb1 O8 76.91(11) . . ? O1 Tb1 O8 126.52(12) . . ? O4 Tb1 O8 131.61(12) . . ? O6 Tb1 O8 145.37(12) . . ? O7 Tb1 O8 69.66(12) . . ? O3 Tb1 O5 79.17(12) . . ? O2 Tb1 O5 68.93(12) . . ? O1 Tb1 O5 130.41(12) . . ? O4 Tb1 O5 131.90(12) . . ? O6 Tb1 O5 71.76(12) . . ? O7 Tb1 O5 143.27(11) . . ? O8 Tb1 O5 73.62(12) . . ? C11 O3 Tb1 134.6(3) . . ? C2 O1 Tb1 136.3(3) . . ? C13 O4 Tb1 130.6(3) . . ? C4 O2 Tb1 135.8(3) . . ? Tb1 O6 H28 99(5) . . ? Tb1 O6 H27 115(5) . . ? H28 O6 H27 133(7) . . ? C5 N1 C4 127.3(3) . . ? C5 N1 H5 106(5) . . ? C4 N1 H5 126(5) . . ? Tb1 O8 H23 102(5) . . ? Tb1 O8 H24 118(4) . . ? H23 O8 H24 116(7) . . ? C11 C12 C13 122.6(4) . . ? C11 C12 H14 118.7 . . ? C13 C12 H14 118.7 . . ? C5 N2 C9 121.4(4) . . ? C5 N2 H10 118(4) . . ? C9 N2 H10 120(4) . . ? C4 C3 C2 121.9(4) . . ? C4 C3 H4 119.0 . . ? C2 C3 H4 119.0 . . ? N4 C14 N3 120.7(4) . . ? N4 C14 C15 119.0(4) . . ? N3 C14 C15 120.3(4) . . ? O4 C13 N3 117.8(4) . . ? O4 C13 C12 126.5(4) . . ? N3 C13 C12 115.7(4) . . ? C14 N3 C13 127.1(4) . . ? C14 N3 H15 111(4) . . ? C13 N3 H15 121(5) . . ? Tb1 O7 H22 130(5) . . ? Tb1 O7 H21 120(5) . . ? H22 O7 H21 108(7) . . ? C8 C9 N2 120.1(4) . . ? C8 C9 H9 120.0 . . ? N2 C9 H9 120.0 . . ? O2 C4 C3 127.0(4) . . ? O2 C4 N1 116.3(4) . . ? C3 C4 N1 116.7(3) . . ? C7 C6 C5 118.7(4) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C18 N4 C14 122.4(4) . . ? C18 N4 H20 119(4) . . ? C14 N4 H20 119(4) . . ? O1 C2 C3 125.7(4) . . ? O1 C2 C1 116.2(4) . . ? C3 C2 C1 118.2(4) . . ? N2 C5 N1 119.9(4) . . ? N2 C5 C6 120.2(4) . . ? N1 C5 C6 119.9(4) . . ? C16 C15 C14 118.8(4) . . ? C16 C15 H16 120.6 . . ? C14 C15 H16 120.6 . . ? C6 C7 C8 120.5(4) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C2 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C2 C1 H1 109.5 . . ? H2 C1 H1 109.5 . . ? H3 C1 H1 109.5 . . ? C11 C10 H12 109.5 . . ? C11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C11 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? O3 C11 C12 124.9(4) . . ? O3 C11 C10 117.4(4) . . ? C12 C11 C10 117.7(4) . . ? N4 C18 C17 120.3(4) . . ? N4 C18 H19 119.8 . . ? C17 C18 H19 119.8 . . ? C15 C16 C17 121.0(4) . . ? C15 C16 H17 119.5 . . ? C17 C16 H17 119.5 . . ? C18 C17 C16 118.5(4) . . ? C18 C17 H18 120.7 . . ? C16 C17 H18 120.7 . . ? Tb1 O5 H26 99(5) . . ? Tb1 O5 H25 138(5) . . ? H26 O5 H25 121(7) . . ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 30.88 _diffrn_measured_fraction_theta_full 0.846 _refine_diff_density_max 3.914 _refine_diff_density_min -3.647 _refine_diff_density_rms 0.206 data_3c:\users\nick\desktop\ _database_code_depnum_ccdc_archive 'CCDC 914685' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cl3 Dy N4 O10' _chemical_formula_weight 733.33 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 8.8460(18) _cell_length_b 11.148(2) _cell_length_c 14.527(3) _cell_angle_alpha 102.85(3) _cell_angle_beta 93.52(3) _cell_angle_gamma 91.86(3) _cell_volume 1392.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_absorpt_coefficient_mu 3.025 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type synchrotron _diffrn_radiation_source '3BM1 dipole' _diffrn_radiation_monochromator 'double crystal' _diffrn_measurement_device_type synchrotron _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11894 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 28.69 _reflns_number_total 5957 _reflns_number_gt 5850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. The crystal was run on the Australian synchrotron in which we were restricted to only one 185 degree phi scan. The asymmetric unit contains the entire cluster as well as two water molecules and three chloride ions. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20, H21, H22, H23, H24, H25, H26, H27 and H28 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. The hydrogen atoms for the lattice water molecules (O9 and O10) were omitted due to uncertainties in thier position. ; _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^)+(0.0079P)^2^+3.5624P] 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 5957 _refine_ls_number_parameters 363 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _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 Dy1 Dy 0.820205(15) 0.200890(12) 0.301306(9) 0.01188(7) Uani 1 1 d . . . O3 O 0.8377(3) 0.3419(2) 0.21116(16) 0.0172(5) Uani 1 1 d . . . O4 O 0.9538(3) 0.1101(2) 0.17041(16) 0.0161(4) Uani 1 1 d . . . O1 O 0.9049(3) 0.0153(2) 0.32711(17) 0.0186(5) Uani 1 1 d . . . O2 O 0.7104(3) 0.1676(2) 0.43337(16) 0.0173(5) Uani 1 1 d . . . N1 N 0.6349(4) 0.1092(3) 0.5637(2) 0.0184(6) Uani 1 1 d D . . N3 N 1.1398(3) 0.0854(3) 0.0660(2) 0.0170(5) Uani 1 1 d D . . C17 C 1.2490(4) -0.2654(3) 0.0863(3) 0.0237(7) Uani 1 1 d . . . H18 H 1.2738 -0.3458 0.0921 0.028 Uiso 1 1 calc R . . N2 N 0.5054(4) 0.2814(3) 0.5376(2) 0.0179(6) Uani 1 1 d D . . C3 C 0.7935(4) -0.0218(3) 0.4631(2) 0.0176(6) Uani 1 1 d . . . H4 H 0.7855 -0.0773 0.5038 0.021 Uiso 1 1 calc R . . C13 C 1.0360(4) 0.1589(3) 0.1186(2) 0.0158(6) Uani 1 1 d . . . C6 C 0.4926(4) 0.2268(3) 0.6857(2) 0.0208(7) Uani 1 1 d . . . H6 H 0.5182 0.1742 0.7269 0.025 Uiso 1 1 calc R . . N4 N 1.1004(3) -0.0924(3) 0.1257(2) 0.0168(5) Uani 1 1 d D . . C15 C 1.2934(4) -0.0880(3) 0.0204(2) 0.0204(7) Uani 1 1 d . . . H16 H 1.3469 -0.0473 -0.0194 0.024 Uiso 1 1 calc R . . C4 C 0.7161(4) 0.0870(3) 0.4825(2) 0.0166(6) Uani 1 1 d . . . C2 C 0.8833(4) -0.0521(3) 0.3852(2) 0.0156(6) Uani 1 1 d . . . C7 C 0.4025(5) 0.3234(4) 0.7139(3) 0.0243(7) Uani 1 1 d . . . H7 H 0.3679 0.3392 0.7759 0.029 Uiso 1 1 calc R . . C14 C 1.1764(4) -0.0304(3) 0.0718(2) 0.0162(6) Uani 1 1 d . . . C8 C 0.3600(4) 0.4000(4) 0.6525(3) 0.0235(7) Uani 1 1 d . . . H8 H 0.2956 0.4662 0.6716 0.028 Uiso 1 1 calc R . . C10 C 0.9320(5) 0.4919(3) 0.1350(3) 0.0227(7) Uani 1 1 d . . . H12 H 0.8332 0.5050 0.1054 0.034 Uiso 1 1 calc R . . H13 H 1.0114 0.5008 0.0925 0.034 Uiso 1 1 calc R . . H11 H 0.9517 0.5530 0.1949 0.034 Uiso 1 1 calc R . . C9 C 0.4147(4) 0.3759(3) 0.5644(3) 0.0212(7) Uani 1 1 d . . . H9 H 0.3884 0.4263 0.5216 0.025 Uiso 1 1 calc R . . C1 C 0.9583(4) -0.1730(3) 0.3676(3) 0.0209(7) Uani 1 1 d . . . H2 H 0.9046 -0.2302 0.3136 0.031 Uiso 1 1 calc R . . H3 H 0.9554 -0.2075 0.4240 0.031 Uiso 1 1 calc R . . H1 H 1.0640 -0.1604 0.3539 0.031 Uiso 1 1 calc R . . C18 C 1.1340(4) -0.2068(3) 0.1338(3) 0.0212(7) Uani 1 1 d . . . H19 H 1.0775 -0.2470 0.1727 0.025 Uiso 1 1 calc R . . C5 C 0.5472(4) 0.2059(3) 0.5944(2) 0.0159(6) Uani 1 1 d . . . C12 C 1.0323(4) 0.2807(3) 0.1075(2) 0.0147(6) Uani 1 1 d . . . H14 H 1.1004 0.3072 0.0671 0.018 Uiso 1 1 calc R . . C11 C 0.9317(4) 0.3648(3) 0.1537(2) 0.0156(6) Uani 1 1 d . . . C16 C 1.3293(4) -0.2045(4) 0.0288(3) 0.0251(7) Uani 1 1 d . . . H17 H 1.4095 -0.2439 -0.0048 0.030 Uiso 1 1 calc R . . Cl2 Cl 0.33663(9) 0.06692(7) 0.29479(6) 0.01773(15) Uani 1 1 d . . . Cl1 Cl 0.73347(10) -0.19840(8) 0.09816(6) 0.02116(16) Uani 1 1 d . . . Cl3 Cl 1.16763(11) 0.52398(8) 0.37422(6) 0.02553(18) Uani 1 1 d . . . O6 O 0.6443(3) 0.0556(2) 0.20185(18) 0.0195(5) Uani 1 1 d D . . O8 O 0.8519(3) 0.3998(2) 0.41136(17) 0.0189(5) Uani 1 1 d D . . O5 O 0.5686(3) 0.2860(2) 0.31277(19) 0.0194(5) Uani 1 1 d D . . O7 O 1.0808(3) 0.2434(2) 0.3564(2) 0.0229(5) Uani 1 1 d D . . O9 O 0.6225(4) -0.4508(3) -0.0353(2) 0.0315(6) Uani 1 1 d . . . O10 O 0.3777(6) 0.4075(4) 0.2145(2) 0.0561(12) Uani 1 1 d . . . H5 H 0.647(9) 0.061(6) 0.603(4) 0.067 Uiso 1 1 d D . . H15 H 1.195(7) 0.127(6) 0.034(5) 0.067 Uiso 1 1 d D . . H20 H 1.029(6) -0.062(7) 0.163(4) 0.067 Uiso 1 1 d D . . H10 H 0.536(9) 0.271(7) 0.480(2) 0.067 Uiso 1 1 d D . . H24 H 0.849(9) 0.405(7) 0.4696(13) 0.067 Uiso 1 1 d D . . H22 H 1.145(7) 0.190(5) 0.339(5) 0.067 Uiso 1 1 d D . . H26 H 0.502(7) 0.230(5) 0.311(5) 0.067 Uiso 1 1 d D . . H27 H 0.556(3) 0.043(8) 0.217(5) 0.067 Uiso 1 1 d D . . H21 H 1.110(9) 0.316(3) 0.358(5) 0.067 Uiso 1 1 d D . . H28 H 0.674(9) -0.014(3) 0.175(5) 0.067 Uiso 1 1 d D . . H23 H 0.934(4) 0.431(7) 0.400(5) 0.067 Uiso 1 1 d D . . H25 H 0.528(8) 0.340(5) 0.289(5) 0.067 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 Dy1 0.01236(9) 0.01038(9) 0.01318(9) 0.00238(5) 0.00392(5) 0.00086(6) O3 0.0215(12) 0.0138(10) 0.0173(11) 0.0044(8) 0.0059(9) 0.0028(10) O4 0.0180(11) 0.0132(10) 0.0178(11) 0.0034(8) 0.0059(8) 0.0014(10) O1 0.0226(12) 0.0157(11) 0.0186(11) 0.0050(9) 0.0069(9) 0.0008(10) O2 0.0189(11) 0.0170(11) 0.0184(11) 0.0073(9) 0.0052(8) 0.0043(10) N1 0.0228(14) 0.0176(13) 0.0168(13) 0.0059(10) 0.0076(10) 0.0025(12) N3 0.0167(13) 0.0172(13) 0.0174(13) 0.0034(10) 0.0059(10) 0.0019(12) C17 0.0224(18) 0.0188(15) 0.0279(18) 0.0006(13) -0.0015(13) 0.0078(15) N2 0.0190(14) 0.0187(13) 0.0178(13) 0.0067(11) 0.0051(10) 0.0020(12) C3 0.0200(16) 0.0152(14) 0.0188(15) 0.0060(11) 0.0033(12) 0.0026(13) C13 0.0150(14) 0.0171(14) 0.0143(14) 0.0015(11) 0.0020(10) -0.0005(13) C6 0.0236(17) 0.0189(15) 0.0210(16) 0.0061(12) 0.0050(12) 0.0014(14) N4 0.0157(13) 0.0162(12) 0.0189(13) 0.0032(10) 0.0039(10) 0.0057(11) C15 0.0152(15) 0.0250(17) 0.0192(15) 0.0007(12) 0.0029(12) 0.0031(14) C4 0.0148(15) 0.0193(15) 0.0143(14) 0.0010(11) 0.0025(11) -0.0037(13) C2 0.0149(15) 0.0130(13) 0.0177(14) 0.0013(11) 0.0003(11) 0.0014(13) C7 0.0249(18) 0.0269(18) 0.0219(17) 0.0054(14) 0.0092(13) 0.0015(16) C14 0.0137(14) 0.0195(15) 0.0135(13) -0.0002(11) 0.0002(11) 0.0020(13) C8 0.0202(17) 0.0214(16) 0.0312(18) 0.0078(14) 0.0097(13) 0.0058(15) C10 0.0285(19) 0.0170(15) 0.0252(17) 0.0081(13) 0.0085(13) 0.0036(15) C9 0.0172(16) 0.0203(16) 0.0288(18) 0.0095(13) 0.0056(13) 0.0058(14) C1 0.0242(17) 0.0158(14) 0.0232(16) 0.0042(12) 0.0046(13) 0.0048(14) C18 0.0224(17) 0.0164(15) 0.0239(16) 0.0025(12) 0.0009(13) 0.0013(14) C5 0.0132(14) 0.0153(14) 0.0210(15) 0.0073(12) 0.0040(11) 0.0014(13) C12 0.0155(15) 0.0129(13) 0.0168(14) 0.0058(11) 0.0019(11) 0.0011(12) C11 0.0174(15) 0.0139(14) 0.0147(14) 0.0013(11) 0.0001(11) 0.0023(13) C16 0.0187(17) 0.0300(19) 0.0225(17) -0.0034(14) 0.0011(12) 0.0070(16) Cl2 0.0144(3) 0.0172(3) 0.0230(4) 0.0066(3) 0.0046(3) 0.0020(3) Cl1 0.0235(4) 0.0172(3) 0.0228(4) 0.0028(3) 0.0093(3) -0.0018(3) Cl3 0.0285(4) 0.0240(4) 0.0215(4) -0.0008(3) 0.0071(3) -0.0069(4) O6 0.0149(11) 0.0191(11) 0.0231(12) -0.0001(9) 0.0067(9) 0.0016(10) O8 0.0206(12) 0.0156(11) 0.0178(11) -0.0019(9) 0.0015(9) -0.0018(10) O5 0.0136(11) 0.0166(11) 0.0288(13) 0.0063(9) 0.0017(9) 0.0011(10) O7 0.0164(12) 0.0168(11) 0.0335(14) 0.0010(10) 0.0020(10) 0.0038(10) O9 0.0461(18) 0.0216(13) 0.0244(13) 0.0002(10) 0.0025(12) 0.0011(13) O10 0.092(3) 0.056(2) 0.0279(16) 0.0170(15) 0.0127(18) 0.046(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O3 2.266(2) . ? Dy1 O2 2.299(2) . ? Dy1 O1 2.322(3) . ? Dy1 O4 2.353(2) . ? Dy1 O6 2.377(3) . ? Dy1 O7 2.390(3) . ? Dy1 O8 2.425(3) . ? Dy1 O5 2.448(3) . ? O3 C11 1.273(4) . ? O4 C13 1.271(4) . ? O1 C2 1.267(4) . ? O2 C4 1.267(4) . ? N1 C5 1.358(5) . ? N1 C4 1.398(4) . ? N1 H5 0.878(10) . ? N3 C14 1.361(4) . ? N3 C13 1.398(4) . ? N3 H15 0.879(10) . ? C17 C18 1.366(5) . ? C17 C16 1.398(6) . ? C17 H18 0.9500 . ? N2 C5 1.347(4) . ? N2 C9 1.347(5) . ? N2 H10 0.877(10) . ? C3 C4 1.395(5) . ? C3 C2 1.408(5) . ? C3 H4 0.9500 . ? C13 C12 1.404(4) . ? C6 C7 1.364(6) . ? C6 C5 1.413(5) . ? C6 H6 0.9500 . ? N4 C14 1.348(4) . ? N4 C18 1.348(4) . ? N4 H20 0.880(10) . ? C15 C16 1.377(6) . ? C15 C14 1.402(5) . ? C15 H16 0.9500 . ? C2 C1 1.500(5) . ? C7 C8 1.409(5) . ? C7 H7 0.9500 . ? C8 C9 1.370(5) . ? C8 H8 0.9500 . ? C10 C11 1.501(5) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H11 0.9800 . ? C9 H9 0.9500 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C1 H1 0.9800 . ? C18 H19 0.9500 . ? C12 C11 1.403(5) . ? C12 H14 0.9500 . ? C16 H17 0.9500 . ? O6 H27 0.839(10) . ? O6 H28 0.839(10) . ? O8 H24 0.837(10) . ? O8 H23 0.838(10) . ? O5 H26 0.840(10) . ? O5 H25 0.838(10) . ? O7 H22 0.840(10) . ? O7 H21 0.839(10) . ? 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 O3 Dy1 O2 141.37(9) . . ? O3 Dy1 O1 145.40(9) . . ? O2 Dy1 O1 73.13(9) . . ? O3 Dy1 O4 73.54(9) . . ? O2 Dy1 O4 144.76(8) . . ? O1 Dy1 O4 72.53(9) . . ? O3 Dy1 O6 99.46(9) . . ? O2 Dy1 O6 90.63(9) . . ? O1 Dy1 O6 77.96(9) . . ? O4 Dy1 O6 74.74(9) . . ? O3 Dy1 O7 90.33(10) . . ? O2 Dy1 O7 102.58(10) . . ? O1 Dy1 O7 75.07(9) . . ? O4 Dy1 O7 75.88(9) . . ? O6 Dy1 O7 144.81(9) . . ? O3 Dy1 O8 74.11(9) . . ? O2 Dy1 O8 76.57(9) . . ? O1 Dy1 O8 126.42(9) . . ? O4 Dy1 O8 131.97(9) . . ? O6 Dy1 O8 145.40(9) . . ? O7 Dy1 O8 69.79(10) . . ? O3 Dy1 O5 78.83(9) . . ? O2 Dy1 O5 69.03(9) . . ? O1 Dy1 O5 130.59(9) . . ? O4 Dy1 O5 131.95(9) . . ? O6 Dy1 O5 71.99(9) . . ? O7 Dy1 O5 143.19(9) . . ? O8 Dy1 O5 73.41(9) . . ? C11 O3 Dy1 134.5(2) . . ? C13 O4 Dy1 130.5(2) . . ? C2 O1 Dy1 136.9(2) . . ? C4 O2 Dy1 136.3(2) . . ? C5 N1 C4 127.2(3) . . ? C5 N1 H5 114(5) . . ? C4 N1 H5 118(5) . . ? C14 N3 C13 127.0(3) . . ? C14 N3 H15 120(5) . . ? C13 N3 H15 112(5) . . ? C18 C17 C16 118.5(3) . . ? C18 C17 H18 120.7 . . ? C16 C17 H18 120.7 . . ? C5 N2 C9 122.9(3) . . ? C5 N2 H10 121(5) . . ? C9 N2 H10 116(5) . . ? C4 C3 C2 122.2(3) . . ? C4 C3 H4 118.9 . . ? C2 C3 H4 118.9 . . ? O4 C13 N3 117.9(3) . . ? O4 C13 C12 126.3(3) . . ? N3 C13 C12 115.7(3) . . ? C7 C6 C5 119.2(3) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C14 N4 C18 122.7(3) . . ? C14 N4 H20 125(5) . . ? C18 N4 H20 112(5) . . ? C16 C15 C14 118.8(3) . . ? C16 C15 H16 120.6 . . ? C14 C15 H16 120.6 . . ? O2 C4 C3 126.6(3) . . ? O2 C4 N1 116.3(3) . . ? C3 C4 N1 117.1(3) . . ? O1 C2 C3 124.7(3) . . ? O1 C2 C1 116.6(3) . . ? C3 C2 C1 118.7(3) . . ? C6 C7 C8 121.0(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? N4 C14 N3 121.0(3) . . ? N4 C14 C15 118.8(3) . . ? N3 C14 C15 120.1(3) . . ? C9 C8 C7 117.8(4) . . ? C9 C8 H8 121.1 . . ? C7 C8 H8 121.1 . . ? C11 C10 H12 109.5 . . ? C11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C11 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? N2 C9 C8 120.7(3) . . ? N2 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C2 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C2 C1 H1 109.5 . . ? H2 C1 H1 109.5 . . ? H3 C1 H1 109.5 . . ? N4 C18 C17 120.4(3) . . ? N4 C18 H19 119.8 . . ? C17 C18 H19 119.8 . . ? N2 C5 N1 121.1(3) . . ? N2 C5 C6 118.3(3) . . ? N1 C5 C6 120.5(3) . . ? C13 C12 C11 122.5(3) . . ? C13 C12 H14 118.7 . . ? C11 C12 H14 118.7 . . ? O3 C11 C12 124.9(3) . . ? O3 C11 C10 116.3(3) . . ? C12 C11 C10 118.8(3) . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H17 119.6 . . ? C17 C16 H17 119.6 . . ? Dy1 O6 H27 122(6) . . ? Dy1 O6 H28 119(6) . . ? H27 O6 H28 106(8) . . ? Dy1 O8 H24 120(6) . . ? Dy1 O8 H23 105(5) . . ? H24 O8 H23 110(7) . . ? Dy1 O5 H26 110(6) . . ? Dy1 O5 H25 132(6) . . ? H26 O5 H25 107(7) . . ? Dy1 O7 H22 120(5) . . ? Dy1 O7 H21 113(6) . . ? H22 O7 H21 115(8) . . ? 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 O2 Dy1 O3 C11 158.2(3) . . . . ? O1 Dy1 O3 C11 -16.2(4) . . . . ? O4 Dy1 O3 C11 -27.8(3) . . . . ? O6 Dy1 O3 C11 -98.7(3) . . . . ? O7 Dy1 O3 C11 47.4(3) . . . . ? O8 Dy1 O3 C11 116.2(3) . . . . ? O5 Dy1 O3 C11 -168.1(3) . . . . ? O3 Dy1 O4 C13 27.0(3) . . . . ? O2 Dy1 O4 C13 -159.5(3) . . . . ? O1 Dy1 O4 C13 -146.1(3) . . . . ? O6 Dy1 O4 C13 132.0(3) . . . . ? O7 Dy1 O4 C13 -67.6(3) . . . . ? O8 Dy1 O4 C13 -22.5(3) . . . . ? O5 Dy1 O4 C13 84.5(3) . . . . ? O3 Dy1 O1 C2 178.3(3) . . . . ? O2 Dy1 O1 C2 2.0(3) . . . . ? O4 Dy1 O1 C2 -170.0(3) . . . . ? O6 Dy1 O1 C2 -92.4(3) . . . . ? O7 Dy1 O1 C2 110.4(3) . . . . ? O8 Dy1 O1 C2 60.3(3) . . . . ? O5 Dy1 O1 C2 -39.2(4) . . . . ? O3 Dy1 O2 C4 -174.1(3) . . . . ? O1 Dy1 O2 C4 2.6(3) . . . . ? O4 Dy1 O2 C4 15.9(4) . . . . ? O6 Dy1 O2 C4 79.8(3) . . . . ? O7 Dy1 O2 C4 -67.4(3) . . . . ? O8 Dy1 O2 C4 -132.7(3) . . . . ? O5 Dy1 O2 C4 150.2(3) . . . . ? Dy1 O4 C13 N3 159.8(2) . . . . ? Dy1 O4 C13 C12 -21.2(5) . . . . ? C14 N3 C13 O4 -8.3(5) . . . . ? C14 N3 C13 C12 172.5(3) . . . . ? Dy1 O2 C4 C3 -5.1(5) . . . . ? Dy1 O2 C4 N1 175.6(2) . . . . ? C2 C3 C4 O2 3.0(6) . . . . ? C2 C3 C4 N1 -177.8(3) . . . . ? C5 N1 C4 O2 1.9(5) . . . . ? C5 N1 C4 C3 -177.4(3) . . . . ? Dy1 O1 C2 C3 -3.9(5) . . . . ? Dy1 O1 C2 C1 175.4(2) . . . . ? C4 C3 C2 O1 1.3(5) . . . . ? C4 C3 C2 C1 -177.9(3) . . . . ? C5 C6 C7 C8 1.8(6) . . . . ? C18 N4 C14 N3 -179.5(3) . . . . ? C18 N4 C14 C15 1.3(5) . . . . ? C13 N3 C14 N4 6.9(5) . . . . ? C13 N3 C14 C15 -174.0(3) . . . . ? C16 C15 C14 N4 -1.8(5) . . . . ? C16 C15 C14 N3 179.1(3) . . . . ? C6 C7 C8 C9 -1.3(6) . . . . ? C5 N2 C9 C8 0.1(6) . . . . ? C7 C8 C9 N2 0.3(6) . . . . ? C14 N4 C18 C17 -0.2(5) . . . . ? C16 C17 C18 N4 -0.6(5) . . . . ? C9 N2 C5 N1 177.8(3) . . . . ? C9 N2 C5 C6 0.3(5) . . . . ? C4 N1 C5 N2 13.2(5) . . . . ? C4 N1 C5 C6 -169.4(3) . . . . ? C7 C6 C5 N2 -1.3(5) . . . . ? C7 C6 C5 N1 -178.8(3) . . . . ? O4 C13 C12 C11 -0.7(5) . . . . ? N3 C13 C12 C11 178.4(3) . . . . ? Dy1 O3 C11 C12 21.2(5) . . . . ? Dy1 O3 C11 C10 -159.0(2) . . . . ? C13 C12 C11 O3 1.8(5) . . . . ? C13 C12 C11 C10 -178.0(3) . . . . ? C14 C15 C16 C17 1.1(5) . . . . ? C18 C17 C16 C15 0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.831 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.831 _refine_diff_density_max 1.278 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.139 data_4c:\users\nick\desktop\xrd\honour~1\ho_cl_~1\p-1 _database_code_depnum_ccdc_archive 'CCDC 914686' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cl3 Ho N4 O10' _chemical_formula_weight 735.76 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8700(18) _cell_length_b 11.120(2) _cell_length_c 14.439(3) _cell_angle_alpha 102.36(3) _cell_angle_beta 93.95(3) _cell_angle_gamma 91.96(3) _cell_volume 1386.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 3.198 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71086 _diffrn_radiation_type synchrotron _diffrn_radiation_source '3BM1 dipole' _diffrn_radiation_monochromator 'double crystal' _diffrn_measurement_device_type synchrotron _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11496 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 28.57 _reflns_number_total 5758 _reflns_number_gt 5461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. The crystal was run on the Australian synchrotron in which we were restricted to only one 185 degree phi scan. The asymmetric unit contains the entire cluster as well as two water molecules and three chloride ions. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20, H21, H22, H23, H24, H25, H26, H27 and H28 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. The hydrogen atoms for the lattice water molecules (O9 and O10) were omitted due to uncertainties in thier position. ; _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^)+(0.0182P)^2^+2.0392P] 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 5758 _refine_ls_number_parameters 364 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _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 Ho1 Ho 0.823066(14) 0.200869(11) 0.300818(9) 0.01872(6) Uani 1 1 d . . . O3 O 0.8381(3) 0.3435(2) 0.21095(17) 0.0244(4) Uani 1 1 d . . . O2 O 0.7130(3) 0.1673(2) 0.43242(17) 0.0258(5) Uani 1 1 d . . . C2 C 0.8852(3) -0.0521(3) 0.3864(2) 0.0228(6) Uani 1 1 d . . . O1 O 0.9076(3) 0.0152(2) 0.32756(17) 0.0246(4) Uani 1 1 d . . . N2 N 0.5060(3) 0.2783(3) 0.5333(2) 0.0248(5) Uani 1 1 d D . . C3 C 0.7944(3) -0.0225(3) 0.4623(2) 0.0241(6) Uani 1 1 d . . . H4 H 0.7849 -0.0788 0.5029 0.029 Uiso 1 1 calc R . . O6 O 0.6478(3) 0.0555(2) 0.20252(18) 0.0277(5) Uani 1 1 d D . . N4 N 1.0990(3) -0.0901(2) 0.1274(2) 0.0241(5) Uani 1 1 d D . . C13 C 1.0340(3) 0.1603(3) 0.1190(2) 0.0220(6) Uani 1 1 d . . . O4 O 0.9526(2) 0.1113(2) 0.16997(16) 0.0226(4) Uani 1 1 d . . . O5 O 0.5743(3) 0.2869(2) 0.3096(2) 0.0303(5) Uani 1 1 d D . . O7 O 1.0810(3) 0.2421(2) 0.35456(19) 0.0300(5) Uani 1 1 d D . . O8 O 0.8564(3) 0.3966(2) 0.41079(17) 0.0265(5) Uani 1 1 d D . . C5 C 0.5469(3) 0.2036(3) 0.5917(2) 0.0226(6) Uani 1 1 d . . . C8 C 0.3582(4) 0.3959(3) 0.6469(3) 0.0300(7) Uani 1 1 d . . . H8 H 0.2933 0.4616 0.6650 0.036 Uiso 1 1 calc R . . C9 C 0.4129(4) 0.3727(3) 0.5591(3) 0.0290(7) Uani 1 1 d . . . H9 H 0.3860 0.4229 0.5155 0.035 Uiso 1 1 calc R . . C4 C 0.7167(3) 0.0864(3) 0.4817(2) 0.0201(5) Uani 1 1 d . . . N3 N 1.1368(3) 0.0876(3) 0.0668(2) 0.0239(5) Uani 1 1 d D . . C16 C 1.3295(4) -0.2009(3) 0.0331(3) 0.0326(7) Uani 1 1 d . . . H17 H 1.4098 -0.2397 -0.0001 0.039 Uiso 1 1 calc R . . C1 C 0.9596(4) -0.1742(3) 0.3696(3) 0.0271(6) Uani 1 1 d . . . H2 H 0.9108 -0.2290 0.3123 0.041 Uiso 1 1 calc R . . H3 H 0.9491 -0.2119 0.4244 0.041 Uiso 1 1 calc R . . H1 H 1.0671 -0.1609 0.3613 0.041 Uiso 1 1 calc R . . C6 C 0.4921(4) 0.2244(3) 0.6827(2) 0.0263(6) Uani 1 1 d . . . H6 H 0.5188 0.1726 0.7251 0.032 Uiso 1 1 calc R . . C18 C 1.1335(4) -0.2050(3) 0.1375(3) 0.0285(6) Uani 1 1 d . . . H19 H 1.0772 -0.2452 0.1768 0.034 Uiso 1 1 calc R . . C17 C 1.2496(4) -0.2629(3) 0.0912(3) 0.0326(7) Uani 1 1 d . . . H18 H 1.2754 -0.3428 0.0982 0.039 Uiso 1 1 calc R . . C15 C 1.2926(4) -0.0851(3) 0.0239(2) 0.0272(6) Uani 1 1 d . . . H16 H 1.3463 -0.0438 -0.0159 0.033 Uiso 1 1 calc R . . C7 C 0.3999(4) 0.3202(3) 0.7097(3) 0.0291(7) Uani 1 1 d . . . H7 H 0.3640 0.3355 0.7714 0.035 Uiso 1 1 calc R . . C12 C 1.0315(4) 0.2831(3) 0.1069(2) 0.0237(6) Uani 1 1 d . . . H14 H 1.0989 0.3095 0.0661 0.028 Uiso 1 1 calc R . . C14 C 1.1745(3) -0.0284(3) 0.0740(2) 0.0231(6) Uani 1 1 d . . . C10 C 0.9354(5) 0.4952(3) 0.1358(3) 0.0349(8) Uani 1 1 d . . . H12 H 0.8356 0.5117 0.1092 0.052 Uiso 1 1 calc R . . H13 H 1.0111 0.5029 0.0907 0.052 Uiso 1 1 calc R . . H11 H 0.9618 0.5547 0.1958 0.052 Uiso 1 1 calc R . . C11 C 0.9323(4) 0.3668(3) 0.1535(2) 0.0243(6) Uani 1 1 d . . . Cl2 Cl 0.34070(8) 0.07054(7) 0.29461(6) 0.02497(15) Uani 1 1 d . . . Cl1 Cl 0.73171(9) -0.19948(7) 0.09793(6) 0.02840(16) Uani 1 1 d . . . Cl3 Cl 1.17206(10) 0.52097(8) 0.37480(6) 0.03446(18) Uani 1 1 d . . . O9 O 0.6241(5) -0.4499(3) -0.0351(3) 0.0581(9) Uani 1 1 d . . . O10 O 0.3941(7) 0.4179(5) 0.2139(3) 0.0862(15) Uani 1 1 d . . . N1 N 0.6356(3) 0.1075(2) 0.5625(2) 0.0238(5) Uani 1 1 d D . . H15 H 1.181(5) 0.120(4) 0.024(2) 0.029 Uiso 1 1 d D . . H20 H 1.028(3) -0.058(4) 0.163(3) 0.029 Uiso 1 1 d D . . H24 H 0.845(5) 0.406(4) 0.4691(10) 0.029 Uiso 1 1 d D . . H28 H 0.685(5) -0.012(2) 0.179(3) 0.029 Uiso 1 1 d D . . H10 H 0.552(4) 0.265(4) 0.4799(17) 0.029 Uiso 1 1 d D . . H26 H 0.505(4) 0.235(3) 0.314(3) 0.029 Uiso 1 1 d D . . H21 H 1.120(5) 0.3134(18) 0.360(3) 0.029 Uiso 1 1 d D . . H25 H 0.551(5) 0.329(3) 0.269(2) 0.029 Uiso 1 1 d D . . H22 H 1.139(4) 0.185(3) 0.336(3) 0.029 Uiso 1 1 d D . . H23 H 0.938(3) 0.432(4) 0.405(3) 0.029 Uiso 1 1 d D . . H5 H 0.648(5) 0.057(3) 0.601(3) 0.029 Uiso 1 1 d D . . H27 H 0.559(2) 0.049(5) 0.218(4) 0.042(13) 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 Ho1 0.01861(8) 0.01657(8) 0.02051(9) 0.00195(5) 0.00443(5) 0.00157(4) O3 0.0303(11) 0.0209(10) 0.0239(11) 0.0070(8) 0.0072(8) 0.0034(8) O2 0.0292(11) 0.0238(10) 0.0256(11) 0.0041(9) 0.0120(9) 0.0052(8) C2 0.0215(13) 0.0199(13) 0.0254(15) 0.0021(11) 0.0001(11) -0.0002(10) O1 0.0290(11) 0.0215(10) 0.0248(11) 0.0061(8) 0.0078(8) 0.0031(8) N2 0.0233(12) 0.0265(13) 0.0267(14) 0.0086(11) 0.0064(10) 0.0026(10) C3 0.0248(14) 0.0202(13) 0.0277(15) 0.0056(11) 0.0030(11) 0.0022(11) O6 0.0225(10) 0.0263(11) 0.0316(12) -0.0012(9) 0.0081(9) -0.0005(8) N4 0.0240(12) 0.0222(12) 0.0248(13) 0.0008(10) 0.0046(10) 0.0031(9) C13 0.0213(13) 0.0226(13) 0.0198(13) -0.0006(11) 0.0032(10) -0.0006(10) O4 0.0245(10) 0.0207(9) 0.0229(11) 0.0038(8) 0.0066(8) 0.0009(8) O5 0.0246(11) 0.0223(10) 0.0450(15) 0.0089(10) 0.0035(10) 0.0016(8) O7 0.0225(10) 0.0217(10) 0.0419(14) -0.0018(10) 0.0008(9) 0.0045(8) O8 0.0269(11) 0.0240(10) 0.0261(11) -0.0010(9) 0.0044(9) 0.0009(8) C5 0.0202(13) 0.0239(13) 0.0244(15) 0.0058(12) 0.0046(11) 0.0010(11) C8 0.0281(15) 0.0285(15) 0.0363(18) 0.0100(14) 0.0106(13) 0.0074(12) C9 0.0269(15) 0.0263(15) 0.0353(18) 0.0088(13) 0.0054(12) 0.0041(12) C4 0.0209(12) 0.0235(13) 0.0171(13) 0.0060(11) 0.0047(10) -0.0006(10) N3 0.0220(11) 0.0253(12) 0.0241(13) 0.0035(10) 0.0054(9) 0.0018(9) C16 0.0259(15) 0.0343(17) 0.0355(18) 0.0012(14) 0.0045(13) 0.0086(13) C1 0.0283(15) 0.0224(14) 0.0308(16) 0.0045(12) 0.0056(12) 0.0052(11) C6 0.0287(15) 0.0260(14) 0.0244(15) 0.0047(12) 0.0050(12) 0.0031(12) C18 0.0301(15) 0.0225(14) 0.0311(17) 0.0020(12) 0.0020(12) 0.0014(12) C17 0.0311(16) 0.0251(15) 0.0393(19) 0.0021(14) -0.0008(14) 0.0070(12) C15 0.0218(13) 0.0340(16) 0.0261(15) 0.0056(13) 0.0055(11) 0.0034(12) C7 0.0305(15) 0.0298(15) 0.0276(16) 0.0045(13) 0.0096(12) 0.0041(12) C12 0.0264(14) 0.0218(13) 0.0227(14) 0.0039(11) 0.0046(11) -0.0018(11) C14 0.0202(12) 0.0261(14) 0.0213(14) 0.0018(11) 0.0007(10) 0.0004(11) C10 0.052(2) 0.0229(15) 0.0337(19) 0.0096(14) 0.0162(16) 0.0044(14) C11 0.0292(14) 0.0219(13) 0.0210(14) 0.0029(11) 0.0027(11) 0.0008(11) Cl2 0.0219(3) 0.0245(3) 0.0294(4) 0.0067(3) 0.0054(3) 0.0032(2) Cl1 0.0313(4) 0.0247(3) 0.0290(4) 0.0030(3) 0.0110(3) -0.0010(3) Cl3 0.0397(4) 0.0313(4) 0.0292(4) -0.0008(3) 0.0082(3) -0.0074(3) O9 0.072(2) 0.0418(17) 0.054(2) -0.0028(15) 0.0010(17) 0.0010(16) O10 0.108(4) 0.092(3) 0.060(3) 0.013(2) 0.007(2) 0.049(3) N1 0.0267(12) 0.0230(12) 0.0235(13) 0.0071(10) 0.0067(10) 0.0046(10) _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 Ho1 O3 2.260(2) . ? Ho1 O2 2.289(2) . ? Ho1 O1 2.320(2) . ? Ho1 O4 2.335(2) . ? Ho1 O7 2.362(2) . ? Ho1 O6 2.363(2) . ? Ho1 O8 2.399(2) . ? Ho1 O5 2.435(2) . ? O3 C11 1.275(4) . ? O2 C4 1.260(4) . ? C2 O1 1.267(4) . ? C2 C3 1.395(4) . ? C2 C1 1.510(4) . ? N2 C5 1.346(4) . ? N2 C9 1.362(4) . ? N2 H10 0.884(10) . ? C3 C4 1.400(4) . ? C3 H4 0.9500 . ? O6 H28 0.840(10) . ? O6 H27 0.840(10) . ? N4 C14 1.335(4) . ? N4 C18 1.360(4) . ? N4 H20 0.879(10) . ? C13 O4 1.257(4) . ? C13 N3 1.392(4) . ? C13 C12 1.413(4) . ? O5 H26 0.839(10) . ? O5 H25 0.839(10) . ? O7 H21 0.839(10) . ? O7 H22 0.839(10) . ? O8 H24 0.840(10) . ? O8 H23 0.836(10) . ? C5 N1 1.360(4) . ? C5 C6 1.408(5) . ? C8 C9 1.365(5) . ? C8 C7 1.403(5) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C4 N1 1.394(4) . ? N3 C14 1.367(4) . ? N3 H15 0.882(10) . ? C16 C15 1.371(5) . ? C16 C17 1.406(6) . ? C16 H17 0.9500 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C1 H1 0.9800 . ? C6 C7 1.371(5) . ? C6 H6 0.9500 . ? C18 C17 1.370(5) . ? C18 H19 0.9500 . ? C17 H18 0.9500 . ? C15 C14 1.405(4) . ? C15 H16 0.9500 . ? C7 H7 0.9500 . ? C12 C11 1.401(4) . ? C12 H14 0.9500 . ? C10 C11 1.504(5) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H11 0.9800 . ? N1 H5 0.880(10) . ? 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 O3 Ho1 O2 140.43(8) . . ? O3 Ho1 O1 146.03(8) . . ? O2 Ho1 O1 73.45(8) . . ? O3 Ho1 O4 74.03(8) . . ? O2 Ho1 O4 145.07(8) . . ? O1 Ho1 O4 72.71(8) . . ? O3 Ho1 O7 90.43(9) . . ? O2 Ho1 O7 103.45(9) . . ? O1 Ho1 O7 74.94(9) . . ? O4 Ho1 O7 75.79(9) . . ? O3 Ho1 O6 100.04(9) . . ? O2 Ho1 O6 89.97(9) . . ? O1 Ho1 O6 77.61(9) . . ? O4 Ho1 O6 74.56(8) . . ? O7 Ho1 O6 144.30(8) . . ? O3 Ho1 O8 74.14(9) . . ? O2 Ho1 O8 76.28(9) . . ? O1 Ho1 O8 125.86(9) . . ? O4 Ho1 O8 132.31(8) . . ? O7 Ho1 O8 69.90(9) . . ? O6 Ho1 O8 145.80(8) . . ? O3 Ho1 O5 77.44(9) . . ? O2 Ho1 O5 69.41(9) . . ? O1 Ho1 O5 131.33(8) . . ? O4 Ho1 O5 130.91(9) . . ? O7 Ho1 O5 143.54(8) . . ? O6 Ho1 O5 72.14(8) . . ? O8 Ho1 O5 73.71(9) . . ? C11 O3 Ho1 133.6(2) . . ? C4 O2 Ho1 136.49(19) . . ? O1 C2 C3 124.6(3) . . ? O1 C2 C1 116.5(3) . . ? C3 C2 C1 118.8(3) . . ? C2 O1 Ho1 136.4(2) . . ? C5 N2 C9 122.3(3) . . ? C5 N2 H10 114(3) . . ? C9 N2 H10 124(3) . . ? C2 C3 C4 123.0(3) . . ? C2 C3 H4 118.5 . . ? C4 C3 H4 118.5 . . ? Ho1 O6 H28 114(3) . . ? Ho1 O6 H27 120(4) . . ? H28 O6 H27 114(5) . . ? C14 N4 C18 122.9(3) . . ? C14 N4 H20 124(3) . . ? C18 N4 H20 113(3) . . ? O4 C13 N3 117.9(3) . . ? O4 C13 C12 126.9(3) . . ? N3 C13 C12 115.2(3) . . ? C13 O4 Ho1 130.25(19) . . ? Ho1 O5 H26 114(3) . . ? Ho1 O5 H25 116(3) . . ? H26 O5 H25 112(4) . . ? Ho1 O7 H21 119(3) . . ? Ho1 O7 H22 116(3) . . ? H21 O7 H22 115(4) . . ? Ho1 O8 H24 123(3) . . ? Ho1 O8 H23 111(3) . . ? H24 O8 H23 108(4) . . ? N2 C5 N1 120.8(3) . . ? N2 C5 C6 118.7(3) . . ? N1 C5 C6 120.5(3) . . ? C9 C8 C7 118.5(3) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? N2 C9 C8 120.6(3) . . ? N2 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? O2 C4 N1 116.9(3) . . ? O2 C4 C3 125.9(3) . . ? N1 C4 C3 117.2(3) . . ? C14 N3 C13 126.8(3) . . ? C14 N3 H15 117(3) . . ? C13 N3 H15 116(3) . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H17 119.7 . . ? C17 C16 H17 119.7 . . ? C2 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C2 C1 H1 109.5 . . ? H2 C1 H1 109.5 . . ? H3 C1 H1 109.5 . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? N4 C18 C17 120.0(4) . . ? N4 C18 H19 120.0 . . ? C17 C18 H19 120.0 . . ? C18 C17 C16 118.3(3) . . ? C18 C17 H18 120.8 . . ? C16 C17 H18 120.8 . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H16 120.4 . . ? C14 C15 H16 120.4 . . ? C6 C7 C8 120.6(3) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C11 C12 C13 121.8(3) . . ? C11 C12 H14 119.1 . . ? C13 C12 H14 119.1 . . ? N4 C14 N3 120.8(3) . . ? N4 C14 C15 119.0(3) . . ? N3 C14 C15 120.2(3) . . ? C11 C10 H12 109.5 . . ? C11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C11 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? O3 C11 C12 125.3(3) . . ? O3 C11 C10 116.3(3) . . ? C12 C11 C10 118.5(3) . . ? C5 N1 C4 126.8(3) . . ? C5 N1 H5 116(3) . . ? C4 N1 H5 117(3) . . ? _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 28.57 _diffrn_measured_fraction_theta_full 0.815 _refine_diff_density_max 1.095 _refine_diff_density_min -1.656 _refine_diff_density_rms 0.093 data_5c:\users\nick\desktop\xrayfi~1\nc278(~1\p-1 _database_code_depnum_ccdc_archive 'CCDC 914687' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cl3 Er N4 O10' _chemical_formula_weight 738.09 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8067(5) _cell_length_b 11.1745(7) _cell_length_c 14.5412(9) _cell_angle_alpha 103.075(2) _cell_angle_beta 93.297(2) _cell_angle_gamma 91.942(2) _cell_volume 1389.98(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour pink _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 726 _exptl_absorpt_coefficient_mu 3.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.9 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20990 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8118 _reflns_number_gt 7295 _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. The asymmetric unit contains the entire cluster as well as two water molecules and three chloride ions. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20, H21, H22, H23, H24, H25, H26, H27 and H28 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. The hydrogen atoms for the lattice water molecules (O9 and O10) were omitted due to uncertainties in thier position. ; _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^)+(0.0239P)^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 8118 _refine_ls_number_parameters 375 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.003 _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 Er1 Er 1.321271(11) 0.200695(10) -0.198523(6) 0.01117(4) Uani 1 1 d . . . O8 O 1.3516(2) 0.39647(17) -0.08980(11) 0.0177(4) Uani 1 1 d D . . O4 O 1.45404(18) 0.11070(15) -0.32878(10) 0.0143(3) Uani 1 1 d . . . O1 O 1.40686(18) 0.01684(15) -0.17404(11) 0.0162(4) Uani 1 1 d . . . O3 O 1.33671(19) 0.34219(15) -0.28715(10) 0.0158(4) Uani 1 1 d . . . O2 O 1.21167(18) 0.16971(15) -0.06668(10) 0.0150(3) Uani 1 1 d . . . O6 O 1.14728(19) 0.05581(17) -0.29607(12) 0.0180(4) Uani 1 1 d D . . O7 O 1.5793(2) 0.24261(19) -0.14443(13) 0.0220(4) Uani 1 1 d D . . O5 O 1.0717(2) 0.28399(17) -0.18819(12) 0.0179(4) Uani 1 1 d D . . N2 N 1.0052(2) 0.2822(2) 0.03799(13) 0.0159(4) Uani 1 1 d D . . N1 N 1.1348(2) 0.11091(19) 0.06297(13) 0.0160(4) Uani 1 1 d D . . C5 C 1.0462(3) 0.2067(2) 0.09413(15) 0.0139(5) Uani 1 1 d . . . N4 N 1.6023(2) -0.09107(19) -0.37405(13) 0.0157(4) Uani 1 1 d D . . N3 N 1.6394(2) 0.08622(19) -0.43334(13) 0.0149(4) Uani 1 1 d D . . C14 C 1.6770(3) -0.0287(2) -0.42836(15) 0.0144(5) Uani 1 1 d . . . C6 C 0.9924(3) 0.2284(2) 0.18533(15) 0.0171(5) Uani 1 1 d . . . H6 H 1.0192 0.1769 0.2268 0.021 Uiso 1 1 calc R . . C2 C 1.3845(3) -0.0504(2) -0.11600(15) 0.0145(5) Uani 1 1 d . . . C13 C 1.5359(2) 0.1598(2) -0.38055(14) 0.0124(5) Uani 1 1 d . . . C1 C 1.4590(3) -0.1714(2) -0.13364(17) 0.0196(5) Uani 1 1 d . . . H3 H 1.4087 -0.2269 -0.1899 0.029 Uiso 1 1 calc R . . H2 H 1.4501 -0.2078 -0.0788 0.029 Uiso 1 1 calc R . . H1 H 1.5668 -0.1585 -0.1438 0.029 Uiso 1 1 calc R . . C4 C 1.2160(3) 0.0878(2) -0.01844(15) 0.0140(5) Uani 1 1 d . . . C9 C 0.9132(3) 0.3770(2) 0.06496(17) 0.0192(5) Uani 1 1 d . . . H9 H 0.8864 0.4273 0.0225 0.023 Uiso 1 1 calc R . . C12 C 1.5317(3) 0.2811(2) -0.39106(15) 0.0143(5) Uani 1 1 d . . . H14 H 1.6003 0.3075 -0.4314 0.017 Uiso 1 1 calc R . . C3 C 1.2935(3) -0.0200(2) -0.03842(15) 0.0161(5) Uani 1 1 d . . . H4 H 1.2848 -0.0756 0.0019 0.019 Uiso 1 1 calc R . . C8 C 0.8594(3) 0.4003(2) 0.15282(17) 0.0211(6) Uani 1 1 d . . . H8 H 0.7949 0.4665 0.1724 0.025 Uiso 1 1 calc R . . C7 C 0.9011(3) 0.3245(2) 0.21360(17) 0.0208(6) Uani 1 1 d . . . H7 H 0.8654 0.3400 0.2754 0.025 Uiso 1 1 calc R . . C10 C 1.4318(3) 0.4915(2) -0.36380(17) 0.0228(6) Uani 1 1 d . . . H13 H 1.3324 0.5045 -0.3929 0.034 Uiso 1 1 calc R . . H12 H 1.5113 0.5001 -0.4067 0.034 Uiso 1 1 calc R . . H11 H 1.4520 0.5527 -0.3040 0.034 Uiso 1 1 calc R . . C17 C 1.7504(3) -0.2642(3) -0.41542(17) 0.0224(6) Uani 1 1 d . . . H18 H 1.7751 -0.3447 -0.4104 0.027 Uiso 1 1 calc R . . C15 C 1.7943(3) -0.0877(3) -0.48061(16) 0.0191(5) Uani 1 1 d . . . H16 H 1.8478 -0.0474 -0.5208 0.023 Uiso 1 1 calc R . . C18 C 1.6371(3) -0.2061(2) -0.36692(17) 0.0201(5) Uani 1 1 d . . . H19 H 1.5816 -0.2463 -0.3275 0.024 Uiso 1 1 calc R . . C11 C 1.4315(3) 0.3649(2) -0.34512(15) 0.0141(5) Uani 1 1 d . . . C16 C 1.8303(3) -0.2032(3) -0.47311(17) 0.0227(6) Uani 1 1 d . . . H17 H 1.9105 -0.2425 -0.5074 0.027 Uiso 1 1 calc R . . Cl2 Cl 0.83820(6) 0.06667(6) -0.20307(4) 0.01693(12) Uani 1 1 d . . . Cl1 Cl 1.23376(7) -0.19822(6) -0.40119(4) 0.02006(13) Uani 1 1 d . . . Cl3 Cl 1.66879(7) 0.52208(6) -0.12507(4) 0.02478(15) Uani 1 1 d . . . O9 O 1.1231(2) -0.45006(18) -0.53474(13) 0.0298(5) Uani 1 1 d . . . O10 O 0.8807(3) 0.4055(2) -0.28605(14) 0.0505(7) Uani 1 1 d . . . H5 H 1.145(3) 0.0559(19) 0.0962(16) 0.020(7) Uiso 1 1 d D . . H15 H 1.684(3) 0.118(2) -0.4744(15) 0.022(7) Uiso 1 1 d D . . H25 H 1.038(3) 0.334(2) -0.217(2) 0.037(9) Uiso 1 1 d D . . H23 H 1.428(2) 0.437(2) -0.099(2) 0.027(8) Uiso 1 1 d D . . H10 H 1.038(3) 0.265(3) -0.0189(10) 0.032(8) Uiso 1 1 d D . . H26 H 1.008(3) 0.227(2) -0.186(2) 0.033(9) Uiso 1 1 d D . . H24 H 1.343(4) 0.404(3) -0.0321(8) 0.049(10) Uiso 1 1 d D . . H27 H 1.060(2) 0.049(3) -0.277(2) 0.054(11) Uiso 1 1 d D . . H21 H 1.605(4) 0.3174(12) -0.134(3) 0.060(13) Uiso 1 1 d D . . H20 H 1.530(2) -0.051(2) -0.3434(18) 0.034(9) Uiso 1 1 d D . . H28 H 1.173(3) -0.0142(14) -0.323(2) 0.035(9) Uiso 1 1 d D . . H22 H 1.642(3) 0.188(2) -0.162(2) 0.046(10) 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 Er1 0.01165(6) 0.01041(6) 0.01165(5) 0.00224(4) 0.00343(4) 0.00113(4) O8 0.0185(9) 0.0160(10) 0.0171(8) 0.0003(7) 0.0034(7) -0.0011(7) O4 0.0152(8) 0.0126(9) 0.0162(7) 0.0040(7) 0.0059(6) 0.0016(7) O1 0.0178(9) 0.0150(10) 0.0168(7) 0.0049(7) 0.0047(7) 0.0026(7) O3 0.0202(9) 0.0131(9) 0.0155(7) 0.0043(7) 0.0073(7) 0.0037(7) O2 0.0164(8) 0.0147(9) 0.0159(7) 0.0061(7) 0.0054(6) 0.0040(7) O6 0.0141(9) 0.0156(10) 0.0212(8) -0.0028(7) 0.0052(7) -0.0010(7) O7 0.0143(9) 0.0152(11) 0.0337(10) -0.0002(9) -0.0008(8) 0.0044(8) O5 0.0147(9) 0.0144(10) 0.0261(9) 0.0073(8) 0.0015(7) 0.0022(7) N2 0.0140(10) 0.0191(12) 0.0159(9) 0.0058(8) 0.0034(8) 0.0021(8) N1 0.0211(11) 0.0136(11) 0.0162(9) 0.0077(8) 0.0064(8) 0.0050(9) C5 0.0134(11) 0.0120(13) 0.0165(10) 0.0033(9) 0.0016(9) -0.0000(9) N4 0.0160(10) 0.0139(12) 0.0165(9) 0.0014(8) 0.0018(8) 0.0048(8) N3 0.0148(10) 0.0161(12) 0.0150(9) 0.0045(8) 0.0064(8) 0.0042(8) C14 0.0115(11) 0.0177(14) 0.0125(9) 0.0003(9) -0.0009(8) 0.0031(9) C6 0.0202(12) 0.0175(14) 0.0142(10) 0.0041(9) 0.0043(9) 0.0013(10) C2 0.0132(11) 0.0137(13) 0.0151(10) 0.0008(9) -0.0010(9) -0.0018(9) C13 0.0100(10) 0.0156(13) 0.0107(9) 0.0013(9) 0.0003(8) 0.0014(9) C1 0.0228(13) 0.0135(14) 0.0227(11) 0.0038(10) 0.0035(10) 0.0038(10) C4 0.0124(11) 0.0184(14) 0.0120(9) 0.0050(9) 0.0019(8) -0.0013(9) C9 0.0152(12) 0.0195(15) 0.0256(12) 0.0097(10) 0.0039(10) 0.0045(10) C12 0.0149(11) 0.0155(13) 0.0130(9) 0.0033(9) 0.0041(9) 0.0005(9) C3 0.0205(12) 0.0129(13) 0.0163(10) 0.0054(9) 0.0034(9) 0.0035(10) C8 0.0165(12) 0.0211(15) 0.0271(12) 0.0057(11) 0.0081(10) 0.0061(10) C7 0.0210(13) 0.0228(15) 0.0197(11) 0.0047(10) 0.0091(10) 0.0033(11) C10 0.0312(15) 0.0176(15) 0.0228(11) 0.0088(10) 0.0083(11) 0.0054(11) C17 0.0225(13) 0.0166(15) 0.0248(12) -0.0015(11) -0.0046(11) 0.0090(11) C15 0.0129(11) 0.0258(16) 0.0162(10) -0.0006(10) 0.0016(9) 0.0028(10) C18 0.0221(13) 0.0166(14) 0.0209(11) 0.0031(10) -0.0008(10) 0.0027(11) C11 0.0174(12) 0.0134(13) 0.0112(9) 0.0024(9) -0.0007(9) -0.0005(10) C16 0.0158(12) 0.0259(16) 0.0222(12) -0.0035(11) -0.0013(10) 0.0091(11) Cl2 0.0131(3) 0.0177(3) 0.0219(3) 0.0075(2) 0.0039(2) 0.0020(2) Cl1 0.0227(3) 0.0160(3) 0.0215(3) 0.0027(2) 0.0086(2) -0.0009(2) Cl3 0.0272(3) 0.0252(4) 0.0190(3) -0.0010(2) 0.0065(2) -0.0077(3) O9 0.0430(12) 0.0208(11) 0.0259(9) 0.0049(8) 0.0049(9) 0.0048(9) O10 0.0795(18) 0.0514(16) 0.0256(10) 0.0133(10) 0.0074(11) 0.0376(14) _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 Er1 O3 2.2599(16) . ? Er1 O2 2.2842(14) . ? Er1 O1 2.3066(17) . ? Er1 O4 2.3321(14) . ? Er1 O6 2.3503(17) . ? Er1 O7 2.3578(19) . ? Er1 O8 2.3883(17) . ? Er1 O5 2.4149(18) . ? O8 H23 0.830(10) . ? O8 H24 0.832(10) . ? O4 C13 1.269(2) . ? O1 C2 1.269(3) . ? O3 C11 1.279(2) . ? O2 C4 1.273(3) . ? O6 H27 0.839(10) . ? O6 H28 0.836(10) . ? O7 H21 0.835(10) . ? O7 H22 0.841(10) . ? O5 H25 0.828(10) . ? O5 H26 0.841(10) . ? N2 C5 1.344(3) . ? N2 C9 1.356(3) . ? N2 H10 0.876(10) . ? N1 C5 1.356(3) . ? N1 C4 1.397(3) . ? N1 H5 0.868(10) . ? C5 C6 1.406(3) . ? N4 C14 1.349(3) . ? N4 C18 1.357(3) . ? N4 H20 0.879(10) . ? N3 C14 1.354(3) . ? N3 C13 1.394(3) . ? N3 H15 0.865(10) . ? C14 C15 1.410(3) . ? C6 C7 1.365(3) . ? C6 H6 0.9500 . ? C2 C3 1.407(3) . ? C2 C1 1.499(3) . ? C13 C12 1.399(3) . ? C1 H3 0.9800 . ? C1 H2 0.9800 . ? C1 H1 0.9800 . ? C4 C3 1.386(3) . ? C9 C8 1.361(3) . ? C9 H9 0.9500 . ? C12 C11 1.394(3) . ? C12 H14 0.9500 . ? C3 H4 0.9500 . ? C8 C7 1.398(4) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? C10 C11 1.500(3) . ? C10 H13 0.9800 . ? C10 H12 0.9800 . ? C10 H11 0.9800 . ? C17 C18 1.353(3) . ? C17 C16 1.399(4) . ? C17 H18 0.9500 . ? C15 C16 1.366(4) . ? C15 H16 0.9500 . ? C18 H19 0.9500 . ? C16 H17 0.9500 . ? 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 O3 Er1 O2 140.26(6) . . ? O3 Er1 O1 145.75(5) . . ? O2 Er1 O1 73.87(5) . . ? O3 Er1 O4 74.17(6) . . ? O2 Er1 O4 145.25(6) . . ? O1 Er1 O4 72.26(5) . . ? O3 Er1 O6 99.95(6) . . ? O2 Er1 O6 90.74(6) . . ? O1 Er1 O6 77.59(6) . . ? O4 Er1 O6 74.69(5) . . ? O3 Er1 O7 90.76(7) . . ? O2 Er1 O7 102.38(6) . . ? O1 Er1 O7 74.82(6) . . ? O4 Er1 O7 76.00(6) . . ? O6 Er1 O7 144.55(7) . . ? O3 Er1 O8 73.72(6) . . ? O2 Er1 O8 75.96(6) . . ? O1 Er1 O8 126.58(6) . . ? O4 Er1 O8 132.18(5) . . ? O6 Er1 O8 145.46(6) . . ? O7 Er1 O8 69.98(6) . . ? O3 Er1 O5 77.88(6) . . ? O2 Er1 O5 69.29(6) . . ? O1 Er1 O5 131.06(6) . . ? O4 Er1 O5 131.32(6) . . ? O6 Er1 O5 71.91(6) . . ? O7 Er1 O5 143.54(7) . . ? O8 Er1 O5 73.58(6) . . ? Er1 O8 H23 113(2) . . ? Er1 O8 H24 121(2) . . ? H23 O8 H24 110(3) . . ? C13 O4 Er1 130.26(15) . . ? C2 O1 Er1 136.41(15) . . ? C11 O3 Er1 133.80(16) . . ? C4 O2 Er1 135.72(15) . . ? Er1 O6 H27 117(2) . . ? Er1 O6 H28 122(2) . . ? H27 O6 H28 108(3) . . ? Er1 O7 H21 113(3) . . ? Er1 O7 H22 119(2) . . ? H21 O7 H22 121(3) . . ? Er1 O5 H25 126(2) . . ? Er1 O5 H26 109(2) . . ? H25 O5 H26 113(3) . . ? C5 N2 C9 123.01(19) . . ? C5 N2 H10 116(2) . . ? C9 N2 H10 121(2) . . ? C5 N1 C4 127.9(2) . . ? C5 N1 H5 118.5(18) . . ? C4 N1 H5 113.6(18) . . ? N2 C5 N1 120.84(19) . . ? N2 C5 C6 118.2(2) . . ? N1 C5 C6 121.0(2) . . ? C14 N4 C18 122.8(2) . . ? C14 N4 H20 114(2) . . ? C18 N4 H20 123(2) . . ? C14 N3 C13 127.66(18) . . ? C14 N3 H15 116.7(19) . . ? C13 N3 H15 115.6(19) . . ? N4 C14 N3 121.05(19) . . ? N4 C14 C15 117.8(2) . . ? N3 C14 C15 121.1(2) . . ? C7 C6 C5 119.3(2) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? O1 C2 C3 124.6(2) . . ? O1 C2 C1 116.78(19) . . ? C3 C2 C1 118.6(2) . . ? O4 C13 N3 117.4(2) . . ? O4 C13 C12 126.4(2) . . ? N3 C13 C12 116.18(18) . . ? C2 C1 H3 109.5 . . ? C2 C1 H2 109.5 . . ? H3 C1 H2 109.5 . . ? C2 C1 H1 109.5 . . ? H3 C1 H1 109.5 . . ? H2 C1 H1 109.5 . . ? O2 C4 C3 126.56(19) . . ? O2 C4 N1 115.8(2) . . ? C3 C4 N1 117.6(2) . . ? N2 C9 C8 120.1(2) . . ? N2 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C12 C13 123.02(19) . . ? C11 C12 H14 118.5 . . ? C13 C12 H14 118.5 . . ? C4 C3 C2 122.7(2) . . ? C4 C3 H4 118.7 . . ? C2 C3 H4 118.7 . . ? C9 C8 C7 118.5(2) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.7 . . ? C6 C7 C8 120.9(2) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C11 C10 H13 109.5 . . ? C11 C10 H12 109.5 . . ? H13 C10 H12 109.5 . . ? C11 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? C18 C17 C16 118.6(3) . . ? C18 C17 H18 120.7 . . ? C16 C17 H18 120.7 . . ? C16 C15 C14 119.5(2) . . ? C16 C15 H16 120.2 . . ? C14 C15 H16 120.2 . . ? C17 C18 N4 120.6(2) . . ? C17 C18 H19 119.7 . . ? N4 C18 H19 119.7 . . ? O3 C11 C12 124.7(2) . . ? O3 C11 C10 116.3(2) . . ? C12 C11 C10 118.99(19) . . ? C15 C16 C17 120.7(2) . . ? C15 C16 H17 119.7 . . ? C17 C16 H17 119.7 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.905 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.127 data_6c:\users\nick\desktop\ _database_code_depnum_ccdc_archive 'CCDC 914688' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H32 Cl3 N4 O10 Y' _chemical_formula_weight 659.74 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8190(18) _cell_length_b 11.149(2) _cell_length_c 14.491(3) _cell_angle_alpha 102.91(3) _cell_angle_beta 93.47(3) _cell_angle_gamma 91.88(3) _cell_volume 1384.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour clear _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 2.450 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71086 _diffrn_radiation_type synchrotron _diffrn_radiation_source '3BM1 dipole' _diffrn_radiation_monochromator 'double crystal' _diffrn_measurement_device_type synchrotron _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8682 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4297 _reflns_number_gt 4141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. The crystal was run on the Australian synchrotron in which we were restricted to only one 185 degree phi scan. The asymmetric unit contains the entire cluster as well as two water molecules and three chloride ions. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20, H21, H22, H23, H24, H25, H26, H27 and H28 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. The hydrogen atoms for the lattice water molecules (O9 and O10) were omitted due to uncertainties in thier position. ; _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^)+(0.0404P)^2^+1.1770P] 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 4297 _refine_ls_number_parameters 363 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _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 Y1 Y 0.32162(2) 0.70085(2) 0.801452(16) 0.01781(10) Uani 1 1 d . . . O2 O 0.2119(2) 0.66841(17) 0.93344(13) 0.0241(4) Uani 1 1 d . . . O3 O 0.3375(2) 0.84278(17) 0.71153(13) 0.0230(4) Uani 1 1 d . . . O4 O 0.45426(19) 0.61076(16) 0.67053(13) 0.0211(4) Uani 1 1 d . . . O1 O 0.4071(2) 0.51560(17) 0.82688(13) 0.0240(4) Uani 1 1 d . . . O7 O 0.5803(2) 0.74266(19) 0.85572(15) 0.0285(4) Uani 1 1 d D . . O5 O 0.0714(2) 0.78494(18) 0.81113(15) 0.0264(4) Uani 1 1 d D . . N1 N 0.1350(2) 0.6091(2) 1.06338(16) 0.0229(5) Uani 1 1 d D . . N4 N 0.6013(2) 0.4084(2) 0.62610(16) 0.0223(5) Uani 1 1 d D . . N3 N 0.6391(2) 0.5863(2) 0.56650(15) 0.0216(5) Uani 1 1 d D . . C13 C 0.5355(3) 0.6599(2) 0.61916(17) 0.0195(5) Uani 1 1 d . . . C6 C -0.0078(3) 0.7267(3) 1.1847(2) 0.0250(6) Uani 1 1 d . . . H6 H 0.0182 0.6745 1.2263 0.030 Uiso 1 1 calc R . . N2 N 0.0052(2) 0.7806(2) 1.03690(17) 0.0240(5) Uani 1 1 d D . . C2 C 0.3843(3) 0.4484(2) 0.88475(18) 0.0208(5) Uani 1 1 d . . . C4 C 0.2160(3) 0.5873(2) 0.98197(18) 0.0216(5) Uani 1 1 d . . . C9 C -0.0871(3) 0.8760(3) 1.0640(2) 0.0279(6) Uani 1 1 d . . . H9 H -0.1144 0.9262 1.0212 0.033 Uiso 1 1 calc R . . C18 C 0.6355(3) 0.2936(3) 0.6344(2) 0.0274(6) Uani 1 1 d . . . H19 H 0.5794 0.2537 0.6737 0.033 Uiso 1 1 calc R . . C1 C 0.4597(3) 0.3268(3) 0.8675(2) 0.0272(6) Uani 1 1 d . . . H1 H 0.5667 0.3397 0.8559 0.041 Uiso 1 1 calc R . . H3 H 0.4081 0.2703 0.8121 0.041 Uiso 1 1 calc R . . H2 H 0.4534 0.2914 0.9233 0.041 Uiso 1 1 calc R . . C12 C 0.5320(3) 0.7816(2) 0.60850(18) 0.0216(5) Uani 1 1 d . . . H14 H 0.6010 0.8080 0.5684 0.026 Uiso 1 1 calc R . . C14 C 0.6767(3) 0.4704(2) 0.57232(18) 0.0206(5) Uani 1 1 d . . . C5 C 0.0464(3) 0.7053(2) 1.09402(19) 0.0220(5) Uani 1 1 d . . . C16 C 0.8293(3) 0.2959(3) 0.5282(2) 0.0291(6) Uani 1 1 d . . . H17 H 0.9088 0.2562 0.4936 0.035 Uiso 1 1 calc R . . C8 C -0.1407(3) 0.8999(3) 1.1523(2) 0.0297(6) Uani 1 1 d . . . H8 H -0.2047 0.9665 1.1718 0.036 Uiso 1 1 calc R . . C7 C -0.0987(3) 0.8238(3) 1.2132(2) 0.0278(6) Uani 1 1 d . . . H7 H -0.1337 0.8395 1.2753 0.033 Uiso 1 1 calc R . . C11 C 0.4318(3) 0.8657(2) 0.65418(18) 0.0209(5) Uani 1 1 d . . . C10 C 0.4330(3) 0.9935(3) 0.6357(2) 0.0301(6) Uani 1 1 d . . . H11 H 0.4547 1.0543 0.6957 0.045 Uiso 1 1 calc R . . H13 H 0.3335 1.0075 0.6071 0.045 Uiso 1 1 calc R . . H12 H 0.5117 1.0017 0.5923 0.045 Uiso 1 1 calc R . . C17 C 0.7503(3) 0.2351(3) 0.5864(2) 0.0303(6) Uani 1 1 d . . . H18 H 0.7759 0.1549 0.5924 0.036 Uiso 1 1 calc R . . O8 O 0.3531(2) 0.89780(18) 0.91111(13) 0.0248(4) Uani 1 1 d D . . O6 O 0.1473(2) 0.55524(17) 0.70338(14) 0.0251(4) Uani 1 1 d D . . C3 C 0.2938(3) 0.4789(3) 0.96239(19) 0.0236(5) Uani 1 1 d . . . H4 H 0.2853 0.4234 1.0031 0.028 Uiso 1 1 calc R . . C15 C 0.7936(3) 0.4121(3) 0.52056(19) 0.0260(6) Uani 1 1 d . . . H16 H 0.8474 0.4528 0.4806 0.031 Uiso 1 1 calc R . . Cl2 Cl -0.16163(6) 0.56789(6) 0.79579(5) 0.02391(15) Uani 1 1 d . . . Cl1 Cl 0.23322(7) 0.30143(6) 0.59838(5) 0.02736(16) Uani 1 1 d . . . Cl3 Cl 0.66889(8) 1.02239(7) 0.87429(5) 0.03262(17) Uani 1 1 d . . . O9 O 0.1220(3) 0.0509(2) 0.46550(17) 0.0425(5) Uani 1 1 d . . . O10 O -0.1163(4) 0.9089(3) 0.71456(19) 0.0685(9) Uani 1 1 d . . . H20 H 0.531(4) 0.446(4) 0.661(3) 0.082 Uiso 1 1 d D . . H15 H 0.683(5) 0.622(4) 0.526(3) 0.082 Uiso 1 1 d D . . H5 H 0.137(6) 0.552(4) 1.097(3) 0.082 Uiso 1 1 d D . . H26 H 0.005(4) 0.730(3) 0.812(4) 0.082 Uiso 1 1 d D . . H22 H 0.640(5) 0.692(4) 0.829(3) 0.082 Uiso 1 1 d D . . H10 H 0.042(5) 0.765(5) 0.9802(17) 0.082 Uiso 1 1 d D . . H23 H 0.431(4) 0.938(4) 0.903(4) 0.082 Uiso 1 1 d D . . H28 H 0.176(6) 0.483(2) 0.684(4) 0.082 Uiso 1 1 d D . . H25 H 0.044(6) 0.835(4) 0.780(3) 0.082 Uiso 1 1 d D . . H21 H 0.614(6) 0.8147(19) 0.860(4) 0.082 Uiso 1 1 d D . . H27 H 0.060(3) 0.553(5) 0.723(4) 0.082 Uiso 1 1 d D . . H24 H 0.336(6) 0.909(5) 0.9689(12) 0.082 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 Y1 0.01653(14) 0.01813(15) 0.01959(15) 0.00470(10) 0.00512(9) 0.00265(9) O2 0.0253(9) 0.0251(10) 0.0248(9) 0.0093(8) 0.0092(7) 0.0056(7) O3 0.0247(9) 0.0216(10) 0.0247(9) 0.0078(8) 0.0071(7) 0.0039(7) O4 0.0209(8) 0.0204(9) 0.0235(9) 0.0060(8) 0.0083(7) 0.0028(7) O1 0.0259(9) 0.0239(10) 0.0238(9) 0.0070(8) 0.0072(7) 0.0038(7) O7 0.0195(9) 0.0261(11) 0.0385(11) 0.0045(10) 0.0015(8) 0.0040(7) O5 0.0192(9) 0.0232(10) 0.0386(11) 0.0097(9) 0.0047(8) 0.0029(7) N1 0.0240(11) 0.0242(12) 0.0235(11) 0.0095(10) 0.0070(9) 0.0049(9) N4 0.0214(10) 0.0219(12) 0.0231(11) 0.0032(10) 0.0037(8) 0.0046(8) N3 0.0206(10) 0.0231(12) 0.0216(11) 0.0049(10) 0.0059(8) 0.0029(8) C13 0.0170(11) 0.0241(14) 0.0160(12) 0.0017(11) 0.0013(9) 0.0008(9) C6 0.0256(13) 0.0259(14) 0.0246(13) 0.0066(12) 0.0051(10) 0.0030(10) N2 0.0215(10) 0.0258(12) 0.0272(12) 0.0096(10) 0.0066(9) 0.0035(9) C2 0.0184(11) 0.0208(13) 0.0228(13) 0.0046(11) -0.0008(9) -0.0013(9) C4 0.0179(11) 0.0267(14) 0.0211(12) 0.0074(12) 0.0021(9) -0.0013(10) C9 0.0227(13) 0.0283(15) 0.0365(15) 0.0139(13) 0.0066(11) 0.0051(10) C18 0.0279(13) 0.0237(14) 0.0306(14) 0.0063(12) 0.0005(11) 0.0018(10) C1 0.0282(13) 0.0252(15) 0.0296(14) 0.0072(12) 0.0068(11) 0.0065(11) C12 0.0213(12) 0.0230(13) 0.0212(12) 0.0062(11) 0.0050(9) -0.0016(10) C14 0.0188(11) 0.0226(13) 0.0184(12) 0.0011(11) -0.0010(9) 0.0017(9) C5 0.0177(12) 0.0235(14) 0.0254(13) 0.0070(12) 0.0017(10) -0.0009(10) C16 0.0223(13) 0.0317(16) 0.0294(14) -0.0017(13) -0.0002(11) 0.0080(11) C8 0.0252(13) 0.0276(15) 0.0390(16) 0.0104(13) 0.0109(11) 0.0065(11) C7 0.0271(13) 0.0291(15) 0.0271(14) 0.0041(13) 0.0094(11) 0.0041(11) C11 0.0223(12) 0.0234(14) 0.0165(12) 0.0041(11) 0.0007(9) 0.0000(10) C10 0.0396(16) 0.0239(14) 0.0298(15) 0.0093(13) 0.0115(12) 0.0056(11) C17 0.0295(14) 0.0254(15) 0.0343(15) 0.0030(13) -0.0011(12) 0.0086(11) O8 0.0259(9) 0.0224(10) 0.0243(9) 0.0006(8) 0.0054(7) 0.0011(7) O6 0.0199(9) 0.0247(10) 0.0281(10) -0.0009(9) 0.0073(7) 0.0002(7) C3 0.0237(12) 0.0245(14) 0.0244(13) 0.0086(12) 0.0042(10) 0.0016(10) C15 0.0200(12) 0.0324(16) 0.0241(13) 0.0024(12) 0.0032(10) 0.0037(10) Cl2 0.0191(3) 0.0253(3) 0.0293(3) 0.0091(3) 0.0057(2) 0.0035(2) Cl1 0.0285(3) 0.0256(4) 0.0289(3) 0.0057(3) 0.0109(3) -0.0001(2) Cl3 0.0356(4) 0.0327(4) 0.0278(3) 0.0024(3) 0.0087(3) -0.0064(3) O9 0.0516(13) 0.0358(13) 0.0401(13) 0.0078(11) 0.0055(10) 0.0052(10) O10 0.101(2) 0.072(2) 0.0389(14) 0.0191(14) 0.0109(14) 0.0456(18) _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 Y1 O3 2.2695(18) . ? Y1 O2 2.2883(18) . ? Y1 O1 2.3191(19) . ? Y1 O4 2.3390(19) . ? Y1 O6 2.358(2) . ? Y1 O7 2.364(2) . ? Y1 O8 2.402(2) . ? Y1 O5 2.4252(19) . ? O2 C4 1.263(3) . ? O3 C11 1.270(3) . ? O4 C13 1.260(3) . ? O1 C2 1.263(3) . ? O7 H22 0.836(10) . ? O7 H21 0.836(10) . ? O5 H26 0.837(10) . ? O5 H25 0.831(10) . ? N1 C5 1.357(3) . ? N1 C4 1.395(3) . ? N1 H5 0.880(10) . ? N4 C14 1.342(3) . ? N4 C18 1.353(4) . ? N4 H20 0.882(10) . ? N3 C14 1.363(3) . ? N3 C13 1.395(3) . ? N3 H15 0.882(10) . ? C13 C12 1.400(4) . ? C6 C7 1.372(4) . ? C6 C5 1.399(4) . ? C6 H6 0.9500 . ? N2 C5 1.348(3) . ? N2 C9 1.363(4) . ? N2 H10 0.884(10) . ? C2 C3 1.406(4) . ? C2 C1 1.506(4) . ? C4 C3 1.391(4) . ? C9 C8 1.363(4) . ? C9 H9 0.9500 . ? C18 C17 1.363(4) . ? C18 H19 0.9500 . ? C1 H1 0.9800 . ? C1 H3 0.9800 . ? C1 H2 0.9800 . ? C12 C11 1.396(4) . ? C12 H14 0.9500 . ? C14 C15 1.403(4) . ? C16 C15 1.370(4) . ? C16 C17 1.397(4) . ? C16 H17 0.9500 . ? C8 C7 1.398(4) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? C11 C10 1.507(4) . ? C10 H11 0.9800 . ? C10 H13 0.9800 . ? C10 H12 0.9800 . ? C17 H18 0.9500 . ? O8 H23 0.839(10) . ? O8 H24 0.843(10) . ? O6 H28 0.842(10) . ? O6 H27 0.840(10) . ? C3 H4 0.9500 . ? C15 H16 0.9500 . ? 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 O3 Y1 O2 140.76(7) . . ? O3 Y1 O1 145.70(6) . . ? O2 Y1 O1 73.45(7) . . ? O3 Y1 O4 73.84(7) . . ? O2 Y1 O4 145.04(6) . . ? O1 Y1 O4 72.52(7) . . ? O3 Y1 O6 99.94(7) . . ? O2 Y1 O6 90.41(7) . . ? O1 Y1 O6 77.51(7) . . ? O4 Y1 O6 74.68(7) . . ? O3 Y1 O7 90.62(7) . . ? O2 Y1 O7 102.65(7) . . ? O1 Y1 O7 74.91(7) . . ? O4 Y1 O7 75.91(7) . . ? O6 Y1 O7 144.43(7) . . ? O3 Y1 O8 73.98(7) . . ? O2 Y1 O8 76.32(7) . . ? O1 Y1 O8 126.34(7) . . ? O4 Y1 O8 132.05(7) . . ? O6 Y1 O8 145.70(7) . . ? O7 Y1 O8 69.87(7) . . ? O3 Y1 O5 77.93(7) . . ? O2 Y1 O5 69.50(7) . . ? O1 Y1 O5 131.01(7) . . ? O4 Y1 O5 131.14(7) . . ? O6 Y1 O5 71.94(7) . . ? O7 Y1 O5 143.62(7) . . ? O8 Y1 O5 73.79(7) . . ? C4 O2 Y1 136.25(17) . . ? C11 O3 Y1 133.96(16) . . ? C13 O4 Y1 130.20(16) . . ? C2 O1 Y1 136.48(16) . . ? Y1 O7 H22 115(4) . . ? Y1 O7 H21 116(4) . . ? H22 O7 H21 111(5) . . ? Y1 O5 H26 111(4) . . ? Y1 O5 H25 122(4) . . ? H26 O5 H25 114(5) . . ? C5 N1 C4 127.1(2) . . ? C5 N1 H5 116(3) . . ? C4 N1 H5 117(3) . . ? C14 N4 C18 123.0(2) . . ? C14 N4 H20 118(3) . . ? C18 N4 H20 119(3) . . ? C14 N3 C13 127.3(2) . . ? C14 N3 H15 119(3) . . ? C13 N3 H15 113(3) . . ? O4 C13 N3 117.3(2) . . ? O4 C13 C12 126.7(2) . . ? N3 C13 C12 116.0(2) . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C5 N2 C9 122.6(2) . . ? C5 N2 H10 117(3) . . ? C9 N2 H10 121(3) . . ? O1 C2 C3 124.7(2) . . ? O1 C2 C1 116.7(2) . . ? C3 C2 C1 118.6(2) . . ? O2 C4 C3 126.4(2) . . ? O2 C4 N1 116.6(2) . . ? C3 C4 N1 116.9(2) . . ? N2 C9 C8 120.4(3) . . ? N2 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N4 C18 C17 120.3(3) . . ? N4 C18 H19 119.9 . . ? C17 C18 H19 119.9 . . ? C2 C1 H1 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? H3 C1 H2 109.5 . . ? C11 C12 C13 122.9(2) . . ? C11 C12 H14 118.5 . . ? C13 C12 H14 118.5 . . ? N4 C14 N3 121.1(2) . . ? N4 C14 C15 118.3(2) . . ? N3 C14 C15 120.6(2) . . ? N2 C5 N1 120.8(2) . . ? N2 C5 C6 118.4(2) . . ? N1 C5 C6 120.8(2) . . ? C15 C16 C17 120.8(3) . . ? C15 C16 H17 119.6 . . ? C17 C16 H17 119.6 . . ? C9 C8 C7 118.1(3) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C6 C7 C8 121.0(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? O3 C11 C12 124.6(2) . . ? O3 C11 C10 116.4(2) . . ? C12 C11 C10 119.1(2) . . ? C11 C10 H11 109.5 . . ? C11 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? C11 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? H13 C10 H12 109.5 . . ? C18 C17 C16 118.3(3) . . ? C18 C17 H18 120.8 . . ? C16 C17 H18 120.8 . . ? Y1 O8 H23 113(4) . . ? Y1 O8 H24 123(4) . . ? H23 O8 H24 112(5) . . ? Y1 O6 H28 118(4) . . ? Y1 O6 H27 115(4) . . ? H28 O6 H27 111(5) . . ? C4 C3 C2 122.6(2) . . ? C4 C3 H4 118.7 . . ? C2 C3 H4 118.7 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 H16 120.4 . . ? C14 C15 H16 120.4 . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 0.382 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.056 data_7c:\users\nick\desktop\xrd\honour~1\tb(no3~1\p21c _database_code_depnum_ccdc_archive 'CCDC 914689' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H24 N7 O14 Tb' _chemical_formula_weight 733.37 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.0909(18) _cell_length_b 14.851(3) _cell_length_c 13.916(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.875(4) _cell_angle_gamma 90.00 _cell_volume 2637.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 2.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.9 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9058 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.1216 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4210 _reflns_number_gt 3311 _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. The asymmetric unit contains the entire cluster as well as one nitrate ion. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20 and H24 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. The ISOR command was used to constrain the anisotropic thermal parameters for O1, O6 and C14 to prevent them from going NPD. ; _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^)+(0.0000P)^2^+69.3169P] 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 4210 _refine_ls_number_parameters 376 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.1998 _refine_ls_wR_factor_gt 0.1857 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.116 _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 Tb1 Tb 0.74671(6) 0.08911(4) 0.77844(5) 0.0200(2) Uani 1 1 d . . . N4 N 1.0534(10) 0.2217(8) 0.9321(8) 0.022(3) Uani 1 1 d D . . H20 H 1.0030 0.1844 0.9048 0.027 Uiso 1 1 calc RD . . N2 N 0.6116(10) -0.1590(8) 0.6189(8) 0.024(3) Uani 1 1 d D . . H10 H 0.6348 -0.1036 0.6307 0.029 Uiso 1 1 calc RD . . C14 C 1.0360(11) 0.3105(9) 0.9233(9) 0.016(3) Uani 1 1 d U . . C1 C 1.0754(14) -0.0479(11) 0.8976(12) 0.042(5) Uani 1 1 d . . . H1 H 1.1124 0.0067 0.8852 0.064 Uiso 1 1 calc R . . H2 H 1.1077 -0.1006 0.8741 0.064 Uiso 1 1 calc R . . H3 H 1.0796 -0.0538 0.9685 0.064 Uiso 1 1 calc R . . C10 C 0.5746(12) 0.3628(10) 0.7117(10) 0.025(3) Uani 1 1 d . . . H12 H 0.5708 0.3807 0.6433 0.037 Uiso 1 1 calc R . . H13 H 0.5805 0.4166 0.7534 0.037 Uiso 1 1 calc R . . H11 H 0.5111 0.3295 0.7158 0.037 Uiso 1 1 calc R . . C11 C 0.6683(14) 0.3041(10) 0.7465(11) 0.032(4) Uani 1 1 d . . . C13 C 0.8549(12) 0.2953(9) 0.8317(10) 0.019(3) Uani 1 1 d . . . C4 C 0.8106(12) -0.1248(10) 0.7509(10) 0.023(3) Uani 1 1 d . . . C2 C 0.9630(12) -0.0418(10) 0.8443(10) 0.023(3) Uani 1 1 d . . . C7 C 0.5386(15) -0.3295(10) 0.5839(11) 0.035(4) Uani 1 1 d . . . H7 H 0.5126 -0.3890 0.5703 0.041 Uiso 1 1 calc R . . C17 C 1.2235(11) 0.2406(9) 1.0283(10) 0.023(3) Uani 1 1 d . . . H18 H 1.2863 0.2158 1.0668 0.027 Uiso 1 1 calc R . . C18 C 1.1457(12) 0.1873(9) 0.9816(10) 0.023(3) Uani 1 1 d . . . H19 H 1.1557 0.1239 0.9832 0.028 Uiso 1 1 calc R . . C12 C 0.7607(12) 0.3440(9) 0.7920(10) 0.026(4) Uani 1 1 d . . . H14 H 0.7624 0.4078 0.7976 0.031 Uiso 1 1 calc R . . C5 C 0.6719(12) -0.2270(10) 0.6632(9) 0.022(3) Uani 1 1 d . . . C8 C 0.4795(14) -0.2568(11) 0.5395(11) 0.033(4) Uani 1 1 d . . . H8 H 0.4128 -0.2666 0.4970 0.040 Uiso 1 1 calc R . . C3 C 0.9142(14) -0.1211(10) 0.8060(10) 0.031(4) Uani 1 1 d . . . H4 H 0.9530 -0.1756 0.8177 0.038 Uiso 1 1 calc R . . C16 C 1.2096(13) 0.3335(10) 1.0188(10) 0.028(4) Uani 1 1 d . . . H17 H 1.2657 0.3717 1.0493 0.034 Uiso 1 1 calc R . . C6 C 0.6314(11) -0.3168(10) 0.6455(11) 0.025(3) Uani 1 1 d . . . H6 H 0.6702 -0.3666 0.6773 0.029 Uiso 1 1 calc R . . O2 O 0.7538(9) -0.0582(6) 0.7196(8) 0.029(2) Uani 1 1 d . . . O4 O 0.8580(8) 0.2099(6) 0.8362(7) 0.023(2) Uani 1 1 d . . . O3 O 0.6542(8) 0.2210(7) 0.7318(7) 0.030(3) Uani 1 1 d . . . O5 O 0.8238(9) 0.1162(7) 0.6411(8) 0.032(3) Uani 1 1 d D . . O7 O 0.6034(9) 0.0581(7) 0.6263(7) 0.029(3) Uani 1 1 d . . . N1 N 0.7696(11) -0.2090(8) 0.7223(8) 0.029(3) Uani 1 1 d D . . H5 H 0.8097 -0.2557 0.7438 0.034 Uiso 1 1 calc RD . . O9 O 0.7099(9) 0.1214(7) 0.9413(7) 0.035(3) Uani 1 1 d . . . O10 O 0.7272(9) -0.0210(7) 0.9104(7) 0.030(3) Uani 1 1 d . . . N3 N 0.9443(10) 0.3445(8) 0.8728(8) 0.025(3) Uani 1 1 d D . . H15 H 0.9406 0.4033 0.8652 0.030 Uiso 1 1 calc RD . . O6 O 0.5572(8) 0.0565(7) 0.7671(7) 0.028(2) Uani 1 1 d U . . N5 N 0.5268(10) 0.0576(8) 0.6750(9) 0.025(3) Uani 1 1 d . . . O11 O 0.6681(10) 0.0215(8) 1.0381(8) 0.043(3) Uani 1 1 d . . . O8 O 0.4349(10) 0.0536(8) 0.6312(8) 0.047(3) Uani 1 1 d . . . N6 N 0.7001(10) 0.0382(9) 0.9654(9) 0.026(3) Uani 1 1 d . . . O13 O 0.9823(9) -0.4638(7) 0.8605(8) 0.031(3) Uani 1 1 d . . . O12 O 0.9434(11) -0.3343(7) 0.7943(9) 0.046(3) Uani 1 1 d . . . C15 C 1.1208(12) 0.3712(10) 0.9685(11) 0.026(3) Uani 1 1 d . . . H16 H 1.1133 0.4347 0.9627 0.031 Uiso 1 1 calc R . . C9 C 0.5174(14) -0.1714(10) 0.5570(11) 0.034(4) Uani 1 1 d . . . H9 H 0.4780 -0.1213 0.5262 0.040 Uiso 1 1 calc R . . C19 C 0.811(2) 0.1847(16) 0.5722(17) 0.074(8) Uani 1 1 d . . . H23 H 0.7906 0.1590 0.5058 0.110 Uiso 1 1 calc R . . H21 H 0.8773 0.2174 0.5788 0.110 Uiso 1 1 calc R . . H22 H 0.7566 0.2261 0.5830 0.110 Uiso 1 1 calc R . . N7 N 0.9120(12) -0.4099(8) 0.8136(9) 0.034(3) Uani 1 1 d . . . O14 O 0.8189(9) -0.4344(9) 0.7900(9) 0.045(3) Uani 1 1 d . . . O1 O 0.9194(7) 0.0351(6) 0.8382(6) 0.0133(19) Uani 1 1 d U . . H24 H 0.884(5) 0.093(9) 0.651(10) 0.016 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 Tb1 0.0244(4) 0.0113(3) 0.0226(4) 0.0007(3) 0.0013(3) 0.0007(3) N4 0.024(7) 0.014(6) 0.028(6) 0.006(5) 0.003(5) 0.001(5) N2 0.033(8) 0.018(6) 0.020(6) -0.001(5) 0.005(6) 0.004(5) C14 0.016(6) 0.021(6) 0.016(5) -0.003(4) 0.014(5) -0.001(5) C1 0.055(13) 0.014(8) 0.043(10) -0.003(7) -0.021(9) 0.013(8) C10 0.022(9) 0.031(9) 0.023(7) 0.002(6) 0.007(6) 0.006(7) C11 0.040(11) 0.019(8) 0.028(8) -0.003(6) -0.009(7) 0.003(7) C13 0.021(9) 0.020(8) 0.019(7) 0.000(5) 0.012(6) -0.004(6) C4 0.025(9) 0.030(8) 0.021(7) -0.006(6) 0.019(7) -0.009(7) C2 0.031(10) 0.022(8) 0.019(7) 0.008(6) 0.014(6) 0.006(7) C7 0.061(13) 0.015(8) 0.029(8) -0.001(6) 0.011(8) -0.004(7) C17 0.020(9) 0.021(8) 0.023(7) 0.007(6) -0.004(6) -0.002(6) C18 0.031(10) 0.013(7) 0.022(7) -0.006(6) -0.000(6) 0.004(6) C12 0.035(10) 0.008(7) 0.030(8) 0.006(6) -0.003(7) 0.003(6) C5 0.023(9) 0.032(8) 0.009(6) 0.008(6) 0.001(6) 0.007(6) C8 0.035(11) 0.037(10) 0.027(8) 0.006(7) 0.004(7) 0.001(8) C3 0.060(13) 0.007(7) 0.023(8) 0.003(6) -0.000(8) 0.008(7) C16 0.031(10) 0.031(9) 0.022(7) 0.003(6) 0.005(7) -0.011(7) C6 0.012(8) 0.026(8) 0.035(8) 0.006(6) 0.003(7) -0.007(6) O2 0.038(7) 0.014(5) 0.034(6) -0.002(4) 0.003(5) 0.010(5) O4 0.020(6) 0.019(5) 0.028(5) 0.001(4) 0.003(4) 0.012(4) O3 0.028(7) 0.022(6) 0.035(6) -0.001(5) -0.005(5) 0.005(5) O5 0.019(7) 0.031(6) 0.044(6) 0.008(5) -0.001(5) -0.001(5) O7 0.026(7) 0.025(6) 0.032(6) -0.006(4) -0.000(5) -0.005(5) N1 0.045(9) 0.017(6) 0.020(6) -0.001(5) -0.002(6) 0.009(6) O9 0.052(8) 0.021(6) 0.026(6) -0.001(4) -0.001(5) 0.015(5) O10 0.043(7) 0.016(5) 0.026(5) -0.003(4) -0.001(5) 0.009(5) N3 0.040(9) 0.010(6) 0.020(6) 0.002(5) -0.004(6) -0.006(5) O6 0.022(5) 0.023(5) 0.036(5) 0.002(4) -0.001(4) -0.019(4) N5 0.024(8) 0.019(6) 0.023(6) 0.005(5) -0.013(6) -0.002(5) O11 0.049(9) 0.048(8) 0.032(6) 0.011(6) 0.009(6) 0.003(6) O8 0.054(9) 0.043(8) 0.036(7) 0.011(5) -0.007(6) 0.001(6) N6 0.019(8) 0.035(8) 0.028(7) 0.018(6) 0.015(6) 0.010(6) O13 0.041(7) 0.014(5) 0.038(6) 0.013(4) 0.005(5) 0.005(5) O12 0.070(10) 0.014(6) 0.061(8) 0.008(5) 0.027(7) 0.003(6) C15 0.029(10) 0.014(7) 0.033(8) -0.001(6) 0.005(7) -0.000(6) C9 0.054(12) 0.020(8) 0.023(8) -0.002(6) 0.000(8) 0.009(7) C19 0.09(2) 0.067(16) 0.076(16) 0.033(13) 0.051(15) 0.041(14) N7 0.061(11) 0.011(6) 0.032(7) -0.008(6) 0.014(7) -0.009(7) O14 0.016(7) 0.056(9) 0.058(8) -0.011(6) -0.002(6) -0.004(5) O1 0.005(4) 0.010(4) 0.023(4) 0.000(3) -0.000(3) 0.001(3) _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 Tb1 O3 2.318(10) . ? Tb1 O4 2.337(10) . ? Tb1 O2 2.345(9) . ? Tb1 O1 2.368(9) . ? Tb1 O5 2.385(12) . ? Tb1 O9 2.467(11) . ? Tb1 O6 2.498(10) . ? Tb1 O10 2.514(10) . ? Tb1 O7 2.538(10) . ? Tb1 N6 2.902(11) . ? Tb1 N5 2.954(13) . ? N4 C14 1.340(17) . ? N4 C18 1.351(18) . ? N4 H20 0.8800 . ? N2 C5 1.344(18) . ? N2 C9 1.35(2) . ? N2 H10 0.8800 . ? C14 N3 1.347(18) . ? C14 C15 1.46(2) . ? C1 C2 1.49(2) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C10 C11 1.49(2) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H11 0.9800 . ? C11 O3 1.258(18) . ? C11 C12 1.37(2) . ? C13 O4 1.270(16) . ? C13 N3 1.390(18) . ? C13 C12 1.43(2) . ? C4 O2 1.255(18) . ? C4 N1 1.383(19) . ? C4 C3 1.40(2) . ? C2 O1 1.271(16) . ? C2 C3 1.39(2) . ? C7 C6 1.34(2) . ? C7 C8 1.39(2) . ? C7 H7 0.9500 . ? C17 C18 1.34(2) . ? C17 C16 1.39(2) . ? C17 H18 0.9500 . ? C18 H19 0.9500 . ? C12 H14 0.9500 . ? C5 N1 1.384(19) . ? C5 C6 1.44(2) . ? C8 C9 1.36(2) . ? C8 H8 0.9500 . ? C3 H4 0.9500 . ? C16 C15 1.34(2) . ? C16 H17 0.9500 . ? C6 H6 0.9500 . ? O5 C19 1.38(2) . ? O5 H24 0.840(10) . ? O7 N5 1.330(17) . ? N1 H5 0.8800 . ? O9 N6 1.295(16) . ? O10 N6 1.267(16) . ? N3 H15 0.8800 . ? O6 N5 1.254(15) . ? N5 O8 1.223(17) . ? O11 N6 1.205(15) . ? O13 N7 1.282(17) . ? O12 N7 1.246(17) . ? C15 H16 0.9500 . ? C9 H9 0.9500 . ? C19 H23 0.9800 . ? C19 H21 0.9800 . ? C19 H22 0.9800 . ? N7 O14 1.244(17) . ? 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 O3 Tb1 O4 72.2(3) . . ? O3 Tb1 O2 138.5(4) . . ? O4 Tb1 O2 140.0(4) . . ? O3 Tb1 O1 141.5(3) . . ? O4 Tb1 O1 70.5(3) . . ? O2 Tb1 O1 72.4(3) . . ? O3 Tb1 O5 85.5(4) . . ? O4 Tb1 O5 78.7(4) . . ? O2 Tb1 O5 79.7(4) . . ? O1 Tb1 O5 78.3(3) . . ? O3 Tb1 O9 84.1(3) . . ? O4 Tb1 O9 76.7(4) . . ? O2 Tb1 O9 122.2(4) . . ? O1 Tb1 O9 96.3(3) . . ? O5 Tb1 O9 155.1(4) . . ? O3 Tb1 O6 72.3(4) . . ? O4 Tb1 O6 134.8(3) . . ? O2 Tb1 O6 85.0(4) . . ? O1 Tb1 O6 144.4(3) . . ? O5 Tb1 O6 125.0(3) . . ? O9 Tb1 O6 72.6(4) . . ? O3 Tb1 O10 128.5(4) . . ? O4 Tb1 O10 113.9(3) . . ? O2 Tb1 O10 70.5(3) . . ? O1 Tb1 O10 76.5(3) . . ? O5 Tb1 O10 145.5(4) . . ? O9 Tb1 O10 51.9(3) . . ? O6 Tb1 O10 70.1(3) . . ? O3 Tb1 O7 71.2(3) . . ? O4 Tb1 O7 135.6(3) . . ? O2 Tb1 O7 67.6(3) . . ? O1 Tb1 O7 134.5(3) . . ? O5 Tb1 O7 74.2(4) . . ? O9 Tb1 O7 122.9(4) . . ? O6 Tb1 O7 51.2(3) . . ? O10 Tb1 O7 108.3(3) . . ? O3 Tb1 N6 105.7(4) . . ? O4 Tb1 N6 97.5(4) . . ? O2 Tb1 N6 95.9(4) . . ? O1 Tb1 N6 88.4(3) . . ? O5 Tb1 N6 166.7(4) . . ? O9 Tb1 N6 26.4(4) . . ? O6 Tb1 N6 66.5(3) . . ? O10 Tb1 N6 25.8(3) . . ? O7 Tb1 N6 115.9(4) . . ? O3 Tb1 N5 66.8(3) . . ? O4 Tb1 N5 138.9(3) . . ? O2 Tb1 N5 78.0(4) . . ? O1 Tb1 N5 150.2(3) . . ? O5 Tb1 N5 100.2(4) . . ? O9 Tb1 N5 96.3(4) . . ? O6 Tb1 N5 24.8(3) . . ? O10 Tb1 N5 90.4(3) . . ? O7 Tb1 N5 26.7(3) . . ? N6 Tb1 N5 91.1(4) . . ? C14 N4 C18 122.2(13) . . ? C14 N4 H20 118.9 . . ? C18 N4 H20 118.9 . . ? C5 N2 C9 123.4(14) . . ? C5 N2 H10 118.3 . . ? C9 N2 H10 118.3 . . ? N4 C14 N3 122.0(12) . . ? N4 C14 C15 118.1(13) . . ? N3 C14 C15 119.8(12) . . ? C2 C1 H1 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C11 C10 H12 109.5 . . ? C11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C11 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? O3 C11 C12 125.6(14) . . ? O3 C11 C10 116.1(14) . . ? C12 C11 C10 118.3(14) . . ? O4 C13 N3 119.4(13) . . ? O4 C13 C12 122.6(13) . . ? N3 C13 C12 117.8(12) . . ? O2 C4 N1 116.8(14) . . ? O2 C4 C3 125.7(14) . . ? N1 C4 C3 117.3(14) . . ? O1 C2 C3 125.0(15) . . ? O1 C2 C1 117.8(13) . . ? C3 C2 C1 117.2(14) . . ? C6 C7 C8 120.8(15) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C18 C17 C16 118.0(14) . . ? C18 C17 H18 121.0 . . ? C16 C17 H18 121.0 . . ? C17 C18 N4 121.5(13) . . ? C17 C18 H19 119.3 . . ? N4 C18 H19 119.3 . . ? C11 C12 C13 123.8(13) . . ? C11 C12 H14 118.1 . . ? C13 C12 H14 118.1 . . ? N2 C5 N1 119.8(14) . . ? N2 C5 C6 117.5(14) . . ? N1 C5 C6 122.6(13) . . ? C9 C8 C7 119.9(16) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C2 C3 C4 123.4(14) . . ? C2 C3 H4 118.3 . . ? C4 C3 H4 118.3 . . ? C15 C16 C17 122.9(14) . . ? C15 C16 H17 118.6 . . ? C17 C16 H17 118.6 . . ? C7 C6 C5 119.4(14) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C4 O2 Tb1 132.9(10) . . ? C13 O4 Tb1 137.6(9) . . ? C11 O3 Tb1 137.3(10) . . ? C19 O5 Tb1 132.3(11) . . ? C19 O5 H24 112(10) . . ? Tb1 O5 H24 110(10) . . ? N5 O7 Tb1 94.4(7) . . ? C4 N1 C5 126.4(13) . . ? C4 N1 H5 116.8 . . ? C5 N1 H5 116.8 . . ? N6 O9 Tb1 95.9(8) . . ? N6 O10 Tb1 94.5(7) . . ? C14 N3 C13 126.0(12) . . ? C14 N3 H15 117.0 . . ? C13 N3 H15 117.0 . . ? N5 O6 Tb1 98.4(9) . . ? O8 N5 O6 124.2(14) . . ? O8 N5 O7 121.0(12) . . ? O6 N5 O7 114.7(12) . . ? O8 N5 Tb1 173.7(10) . . ? O6 N5 Tb1 56.8(7) . . ? O7 N5 Tb1 58.9(6) . . ? O11 N6 O10 124.2(13) . . ? O11 N6 O9 119.2(13) . . ? O10 N6 O9 116.6(11) . . ? O11 N6 Tb1 171.6(10) . . ? O10 N6 Tb1 59.7(6) . . ? O9 N6 Tb1 57.7(6) . . ? C16 C15 C14 117.1(14) . . ? C16 C15 H16 121.5 . . ? C14 C15 H16 121.5 . . ? N2 C9 C8 118.9(14) . . ? N2 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? O5 C19 H23 109.5 . . ? O5 C19 H21 109.5 . . ? H23 C19 H21 109.5 . . ? O5 C19 H22 109.5 . . ? H23 C19 H22 109.5 . . ? H21 C19 H22 109.5 . . ? O14 N7 O12 123.9(15) . . ? O14 N7 O13 120.2(13) . . ? O12 N7 O13 116.0(15) . . ? C2 O1 Tb1 135.1(9) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 2.077 _refine_diff_density_min -2.847 _refine_diff_density_rms 0.226 data_8c:\users\nick\desktop\ _database_code_depnum_ccdc_archive 'CCDC 914690' #TrackingRef '8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H24 Dy N7 O14' _chemical_formula_weight 736.95 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.090(3) _cell_length_b 14.792(3) _cell_length_c 13.965(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.88(3) _cell_angle_gamma 90.00 _cell_volume 2636.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 2.917 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type synchrotron _diffrn_radiation_source '3BM1 dipole' _diffrn_radiation_monochromator 'double crystal' _diffrn_measurement_device_type synchrotron _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23485 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.77 _reflns_number_total 6654 _reflns_number_gt 5539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. The crystal was run on the Australian synchrotron in which we were restricted to only one 185 degree phi scan. The asymmetric unit contains the entire cluster as well as one nitrate ion. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20 and H24 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. ; _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^)+(0.0608P)^2^+3.0223P] 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 6654 _refine_ls_number_parameters 428 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _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 Dy1 Dy 0.747242(14) 0.088287(12) 0.778433(15) 0.02960(9) Uani 1 1 d . . . O4 O 0.8605(3) 0.2087(2) 0.8368(3) 0.0382(7) Uani 1 1 d . . . O9 O 0.7116(3) 0.1229(2) 0.9385(3) 0.0416(8) Uani 1 1 d . . . O2 O 0.7514(2) -0.0581(2) 0.7223(2) 0.0374(7) Uani 1 1 d . . . O7 O 0.6037(3) 0.0579(3) 0.6287(3) 0.0422(8) Uani 1 1 d . . . O3 O 0.6555(3) 0.2198(2) 0.7338(3) 0.0433(8) Uani 1 1 d . . . O1 O 0.9180(2) 0.0336(2) 0.8395(3) 0.0337(7) Uani 1 1 d . . . N1 N 0.7673(3) -0.2120(3) 0.7212(3) 0.0330(8) Uani 1 1 d D . . N4 N 1.0541(3) 0.2207(3) 0.9302(3) 0.0365(8) Uani 1 1 d D . . O10 O 0.7260(3) -0.0190(2) 0.9108(3) 0.0407(8) Uani 1 1 d . . . C13 C 0.8536(3) 0.2937(3) 0.8320(4) 0.0331(9) Uani 1 1 d . . . N2 N 0.6103(3) -0.1594(2) 0.6184(3) 0.0319(8) Uani 1 1 d D . . C11 C 0.6690(4) 0.3037(3) 0.7468(4) 0.0355(9) Uani 1 1 d . . . O6 O 0.5580(3) 0.0560(2) 0.7669(3) 0.0398(7) Uani 1 1 d . . . O5 O 0.8244(3) 0.1157(3) 0.6431(3) 0.0496(9) Uani 1 1 d D . . N3 N 0.9429(3) 0.3434(3) 0.8728(3) 0.0359(8) Uani 1 1 d D . . N6 N 0.7004(3) 0.0416(3) 0.9644(3) 0.0421(10) Uani 1 1 d . . . C15 C 1.1174(4) 0.3698(3) 0.9682(4) 0.0390(10) Uani 1 1 d . . . C4 C 0.8088(3) -0.1268(3) 0.7500(3) 0.0296(8) Uani 1 1 d . . . C10 C 0.5744(4) 0.3638(3) 0.7110(4) 0.0442(12) Uani 1 1 d . . . H12 H 0.5745 0.3859 0.6449 0.066 Uiso 1 1 calc R . . H13 H 0.5772 0.4152 0.7558 0.066 Uiso 1 1 calc R . . H11 H 0.5102 0.3291 0.7093 0.066 Uiso 1 1 calc R . . C5 C 0.6704(3) -0.2288(3) 0.6620(3) 0.0313(8) Uani 1 1 d . . . C1 C 1.0741(3) -0.0496(3) 0.8975(4) 0.0401(11) Uani 1 1 d . . . H1 H 1.1152 -0.0079 0.8665 0.060 Uiso 1 1 calc R . . H2 H 1.0999 -0.1114 0.8935 0.060 Uiso 1 1 calc R . . H3 H 1.0813 -0.0328 0.9665 0.060 Uiso 1 1 calc R . . C8 C 0.4781(4) -0.2569(4) 0.5359(4) 0.0442(11) Uani 1 1 d . . . C12 C 0.7640(4) 0.3448(3) 0.7908(4) 0.0385(10) Uani 1 1 d . . . C2 C 0.9610(3) -0.0446(3) 0.8453(4) 0.0343(9) Uani 1 1 d . . . C14 C 1.0369(4) 0.3111(3) 0.9231(4) 0.0341(9) Uani 1 1 d . . . C7 C 0.5373(4) -0.3299(4) 0.5808(5) 0.0452(12) Uani 1 1 d . . . C9 C 0.5164(4) -0.1720(3) 0.5559(4) 0.0380(10) Uani 1 1 d . . . C3 C 0.9116(3) -0.1237(3) 0.8064(4) 0.0332(9) Uani 1 1 d . . . C18 C 1.1467(4) 0.1861(3) 0.9823(4) 0.0411(11) Uani 1 1 d . . . C6 C 0.6329(4) -0.3169(3) 0.6437(4) 0.0391(10) Uani 1 1 d . . . C17 C 1.2250(4) 0.2404(4) 1.0272(4) 0.0413(11) Uani 1 1 d . . . C16 C 1.2107(4) 0.3341(4) 1.0207(4) 0.0414(11) Uani 1 1 d . . . O13 O 0.9784(3) -0.4660(2) 0.8597(3) 0.0496(10) Uani 1 1 d . . . N7 N 0.9126(4) -0.4108(3) 0.8126(4) 0.0458(10) Uani 1 1 d . . . N5 N 0.5306(3) 0.0569(3) 0.6742(3) 0.0389(9) Uani 1 1 d . . . O8 O 0.4379(3) 0.0538(3) 0.6310(4) 0.0590(11) Uani 1 1 d . . . O11 O 0.6677(3) 0.0238(3) 1.0370(3) 0.0599(11) Uani 1 1 d . . . O12 O 0.9400(4) -0.3368(3) 0.7896(4) 0.0714(14) Uani 1 1 d . . . O14 O 0.8184(3) -0.4327(4) 0.7901(4) 0.0704(14) Uani 1 1 d . . . C19 C 0.8093(7) 0.1777(9) 0.5714(8) 0.130(5) Uani 1 1 d . . . H23 H 0.7660 0.1517 0.5113 0.194 Uiso 1 1 calc R . . H21 H 0.8771 0.1962 0.5592 0.194 Uiso 1 1 calc R . . H22 H 0.7737 0.2304 0.5913 0.194 Uiso 1 1 calc R . . H5 H 0.791(9) -0.268(3) 0.729(9) 0.155 Uiso 1 1 d D . . H15 H 0.936(10) 0.4022(14) 0.877(10) 0.155 Uiso 1 1 d D . . H24 H 0.8897(16) 0.116(8) 0.664(10) 0.155 Uiso 1 1 d D . . H6 H 0.670(4) -0.365(4) 0.668(4) 0.031(13) Uiso 1 1 d . . . H17 H 1.270(4) 0.375(3) 1.056(4) 0.023(11) Uiso 1 1 d . . . H18 H 1.298(4) 0.214(4) 1.068(4) 0.038(14) Uiso 1 1 d . . . H19 H 1.154(5) 0.119(4) 0.981(5) 0.048(16) Uiso 1 1 d . . . H9 H 0.481(5) -0.115(4) 0.527(5) 0.053(17) Uiso 1 1 d . . . H7 H 0.513(6) -0.402(5) 0.579(6) 0.07(2) Uiso 1 1 d . . . H8 H 0.412(6) -0.265(5) 0.487(6) 0.07(2) Uiso 1 1 d . . . H16 H 1.100(4) 0.428(4) 0.968(4) 0.034(14) Uiso 1 1 d . . . H4 H 0.950(6) -0.184(5) 0.825(6) 0.07(2) Uiso 1 1 d . . . H14 H 0.757(4) 0.423(3) 0.788(4) 0.025(13) Uiso 1 1 d . . . H20 H 1.002(3) 0.185(3) 0.902(3) 0.029 Uiso 1 1 d D . . H10 H 0.638(4) -0.1049(16) 0.628(4) 0.029 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 Dy1 0.02566(11) 0.02358(12) 0.03574(14) 0.00194(7) -0.00130(8) 0.00178(6) O4 0.0346(15) 0.0243(14) 0.051(2) 0.0016(14) 0.0001(14) 0.0014(12) O9 0.0369(16) 0.0405(18) 0.044(2) -0.0012(16) 0.0015(15) 0.0039(14) O2 0.0325(16) 0.0313(16) 0.041(2) -0.0020(13) -0.0066(14) 0.0062(12) O7 0.0330(16) 0.0422(18) 0.046(2) 0.0028(16) -0.0019(15) 0.0049(14) O3 0.0342(16) 0.0302(16) 0.057(2) 0.0053(15) -0.0076(15) 0.0016(12) O1 0.0273(13) 0.0280(14) 0.0400(18) 0.0013(13) -0.0046(12) 0.0027(11) N1 0.0306(17) 0.0284(18) 0.036(2) -0.0023(15) -0.0008(15) 0.0024(13) N4 0.0314(18) 0.0316(19) 0.043(2) 0.0063(16) 0.0015(16) -0.0009(14) O10 0.0398(17) 0.0325(16) 0.046(2) 0.0037(14) 0.0021(15) 0.0056(13) C13 0.031(2) 0.031(2) 0.036(2) -0.0004(17) 0.0037(17) -0.0009(16) N2 0.0278(16) 0.0289(17) 0.035(2) 0.0022(15) -0.0014(14) 0.0003(13) C11 0.035(2) 0.034(2) 0.038(3) 0.0029(19) 0.0074(18) 0.0037(17) O6 0.0338(15) 0.0383(17) 0.043(2) 0.0042(15) -0.0007(14) -0.0014(13) O5 0.0403(19) 0.060(2) 0.046(2) 0.0097(19) 0.0031(17) -0.0053(17) N3 0.0325(18) 0.0295(17) 0.044(2) 0.0026(16) 0.0043(16) 0.0001(15) N6 0.0291(18) 0.054(3) 0.041(2) 0.006(2) 0.0034(16) 0.0043(17) C15 0.034(2) 0.037(2) 0.044(3) -0.003(2) 0.0037(19) -0.0026(18) C4 0.0306(19) 0.0274(19) 0.028(2) -0.0011(16) 0.0004(16) 0.0022(15) C10 0.038(2) 0.039(2) 0.053(3) 0.006(2) 0.005(2) 0.012(2) C5 0.0270(18) 0.034(2) 0.031(2) 0.0015(17) 0.0025(16) 0.0006(16) C1 0.029(2) 0.038(2) 0.046(3) -0.006(2) -0.0066(19) 0.0052(18) C8 0.035(2) 0.044(3) 0.047(3) 0.002(2) -0.006(2) -0.003(2) C12 0.037(2) 0.031(2) 0.046(3) 0.0025(19) 0.005(2) 0.0012(17) C2 0.0306(19) 0.034(2) 0.035(2) 0.0009(18) 0.0004(17) 0.0020(17) C14 0.033(2) 0.031(2) 0.038(2) 0.0046(18) 0.0076(18) -0.0002(16) C7 0.038(2) 0.038(2) 0.055(3) 0.001(2) 0.000(2) -0.0096(19) C9 0.033(2) 0.040(2) 0.034(2) 0.002(2) -0.0066(18) 0.0008(18) C3 0.0295(19) 0.0278(19) 0.038(2) 0.0002(18) -0.0022(17) 0.0039(16) C18 0.037(2) 0.038(2) 0.046(3) 0.011(2) 0.003(2) 0.0035(19) C6 0.034(2) 0.034(2) 0.046(3) 0.004(2) 0.001(2) -0.0005(18) C17 0.037(2) 0.052(3) 0.033(2) 0.004(2) 0.0039(19) 0.003(2) C16 0.035(2) 0.052(3) 0.034(2) -0.004(2) 0.0008(19) -0.003(2) O13 0.0396(18) 0.0336(17) 0.069(3) 0.0057(17) -0.0018(18) 0.0072(14) N7 0.048(2) 0.036(2) 0.053(3) 0.0037(19) 0.011(2) 0.0127(17) N5 0.0275(17) 0.0316(18) 0.049(3) 0.0072(18) -0.0092(16) 0.0004(14) O8 0.0311(17) 0.066(3) 0.068(3) 0.012(2) -0.0133(18) -0.0046(17) O11 0.045(2) 0.084(3) 0.053(3) 0.012(2) 0.0145(19) 0.009(2) O12 0.089(3) 0.037(2) 0.094(4) 0.017(2) 0.032(3) 0.005(2) O14 0.041(2) 0.080(3) 0.080(4) -0.012(3) -0.006(2) 0.013(2) C19 0.077(5) 0.226(14) 0.102(7) 0.101(9) 0.053(5) 0.071(7) _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 Dy1 O3 2.298(3) . ? Dy1 O2 2.308(4) . ? Dy1 O4 2.344(3) . ? Dy1 O1 2.351(3) . ? Dy1 O5 2.368(4) . ? Dy1 O9 2.438(4) . ? Dy1 O6 2.492(3) . ? Dy1 O10 2.499(4) . ? Dy1 O7 2.521(4) . ? O4 C13 1.262(6) . ? O9 N6 1.274(6) . ? O2 C4 1.272(5) . ? O7 N5 1.261(6) . ? O3 C11 1.261(6) . ? O1 C2 1.281(5) . ? N1 C5 1.373(5) . ? N1 C4 1.396(6) . ? N1 H5 0.880(10) . ? N4 C14 1.356(6) . ? N4 C18 1.366(6) . ? N4 H20 0.880(10) . ? O10 N6 1.260(6) . ? C13 N3 1.390(6) . ? C13 C12 1.405(6) . ? N2 C9 1.353(6) . ? N2 C5 1.353(6) . ? N2 H10 0.880(10) . ? C11 C12 1.397(7) . ? C11 C10 1.516(6) . ? O6 N5 1.264(6) . ? O5 C19 1.338(9) . ? O5 H24 0.839(10) . ? N3 C14 1.360(6) . ? N3 H15 0.878(10) . ? N6 O11 1.214(6) . ? C15 C16 1.381(7) . ? C15 C14 1.402(6) . ? C15 H16 0.89(5) . ? C4 C3 1.401(6) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H11 0.9800 . ? C5 C6 1.395(6) . ? C1 C2 1.499(6) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C8 C9 1.358(7) . ? C8 C7 1.394(7) . ? C8 H8 0.99(8) . ? C12 H14 1.16(5) . ? C2 C3 1.388(6) . ? C7 C6 1.373(7) . ? C7 H7 1.11(7) . ? C9 H9 1.00(7) . ? C3 H4 1.03(7) . ? C18 C17 1.343(7) . ? C18 H19 0.99(6) . ? C6 H6 0.89(5) . ? C17 C16 1.400(8) . ? C17 H18 1.07(6) . ? C16 H17 1.01(5) . ? O13 N7 1.261(5) . ? N7 O12 1.218(6) . ? N7 O14 1.245(7) . ? N5 O8 1.229(5) . ? C19 H23 0.9800 . ? C19 H21 0.9800 . ? C19 H22 0.9800 . ? 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 O3 Dy1 O2 138.83(12) . . ? O3 Dy1 O4 72.71(12) . . ? O2 Dy1 O4 140.35(11) . . ? O3 Dy1 O1 141.87(11) . . ? O2 Dy1 O1 73.00(10) . . ? O4 Dy1 O1 70.06(11) . . ? O3 Dy1 O5 85.90(15) . . ? O2 Dy1 O5 80.98(14) . . ? O4 Dy1 O5 78.34(14) . . ? O1 Dy1 O5 78.95(13) . . ? O3 Dy1 O9 82.84(14) . . ? O2 Dy1 O9 122.18(13) . . ? O4 Dy1 O9 75.94(13) . . ? O1 Dy1 O9 95.78(12) . . ? O5 Dy1 O9 153.99(15) . . ? O3 Dy1 O6 72.13(12) . . ? O2 Dy1 O6 84.06(11) . . ? O4 Dy1 O6 135.29(12) . . ? O1 Dy1 O6 143.93(11) . . ? O5 Dy1 O6 125.14(13) . . ? O9 Dy1 O6 73.09(12) . . ? O3 Dy1 O10 126.92(13) . . ? O2 Dy1 O10 70.76(12) . . ? O4 Dy1 O10 113.04(13) . . ? O1 Dy1 O10 76.51(11) . . ? O5 Dy1 O10 146.83(14) . . ? O9 Dy1 O10 51.63(12) . . ? O6 Dy1 O10 69.72(11) . . ? O3 Dy1 O7 71.22(12) . . ? O2 Dy1 O7 67.71(11) . . ? O4 Dy1 O7 136.08(12) . . ? O1 Dy1 O7 135.41(12) . . ? O5 Dy1 O7 74.93(13) . . ? O9 Dy1 O7 122.59(12) . . ? O6 Dy1 O7 50.64(13) . . ? O10 Dy1 O7 108.39(12) . . ? C13 O4 Dy1 135.0(3) . . ? N6 O9 Dy1 96.9(3) . . ? C4 O2 Dy1 134.8(3) . . ? N5 O7 Dy1 95.4(3) . . ? C11 O3 Dy1 138.2(3) . . ? C2 O1 Dy1 134.6(3) . . ? C5 N1 C4 125.8(4) . . ? C5 N1 H5 99(8) . . ? C4 N1 H5 135(8) . . ? C14 N4 C18 121.5(4) . . ? C14 N4 H20 117(3) . . ? C18 N4 H20 121(3) . . ? N6 O10 Dy1 94.3(3) . . ? O4 C13 N3 117.5(4) . . ? O4 C13 C12 126.9(4) . . ? N3 C13 C12 115.6(4) . . ? C9 N2 C5 122.6(4) . . ? C9 N2 H10 120(4) . . ? C5 N2 H10 117(4) . . ? O3 C11 C12 125.0(4) . . ? O3 C11 C10 116.8(4) . . ? C12 C11 C10 118.1(4) . . ? N5 O6 Dy1 96.7(3) . . ? C19 O5 Dy1 134.1(5) . . ? C19 O5 H24 103(9) . . ? Dy1 O5 H24 108(10) . . ? C14 N3 C13 127.4(4) . . ? C14 N3 H15 114(9) . . ? C13 N3 H15 118(9) . . ? O11 N6 O10 122.1(5) . . ? O11 N6 O9 121.8(5) . . ? O10 N6 O9 116.1(4) . . ? C16 C15 C14 119.3(5) . . ? C16 C15 H16 124(4) . . ? C14 C15 H16 116(4) . . ? O2 C4 N1 117.9(4) . . ? O2 C4 C3 125.0(4) . . ? N1 C4 C3 117.1(4) . . ? C11 C10 H12 109.5 . . ? C11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C11 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? N2 C5 N1 120.0(4) . . ? N2 C5 C6 118.7(4) . . ? N1 C5 C6 121.3(4) . . ? C2 C1 H1 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C9 C8 C7 118.8(4) . . ? C9 C8 H8 119(4) . . ? C7 C8 H8 122(4) . . ? C11 C12 C13 121.7(4) . . ? C11 C12 H14 111(2) . . ? C13 C12 H14 127(2) . . ? O1 C2 C3 125.2(4) . . ? O1 C2 C1 116.6(4) . . ? C3 C2 C1 118.2(4) . . ? N4 C14 N3 120.0(4) . . ? N4 C14 C15 118.8(4) . . ? N3 C14 C15 121.2(4) . . ? C6 C7 C8 121.0(5) . . ? C6 C7 H7 112(4) . . ? C8 C7 H7 127(4) . . ? N2 C9 C8 120.1(4) . . ? N2 C9 H9 114(4) . . ? C8 C9 H9 126(4) . . ? C2 C3 C4 123.6(4) . . ? C2 C3 H4 118(4) . . ? C4 C3 H4 118(4) . . ? C17 C18 N4 121.2(5) . . ? C17 C18 H19 123(4) . . ? N4 C18 H19 116(4) . . ? C7 C6 C5 118.8(5) . . ? C7 C6 H6 118(3) . . ? C5 C6 H6 123(3) . . ? C18 C17 C16 119.0(5) . . ? C18 C17 H18 122(3) . . ? C16 C17 H18 119(3) . . ? C15 C16 C17 120.2(5) . . ? C15 C16 H17 121(3) . . ? C17 C16 H17 119(3) . . ? O12 N7 O14 120.1(5) . . ? O12 N7 O13 120.8(5) . . ? O14 N7 O13 119.1(5) . . ? O8 N5 O7 122.0(5) . . ? O8 N5 O6 121.7(5) . . ? O7 N5 O6 116.2(4) . . ? O5 C19 H23 109.5 . . ? O5 C19 H21 109.5 . . ? H23 C19 H21 109.5 . . ? O5 C19 H22 109.5 . . ? H23 C19 H22 109.5 . . ? H21 C19 H22 109.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.745 _refine_diff_density_min -1.808 _refine_diff_density_rms 0.145 data_9c:\users\nick\desktop\honour~1\ho(no3~1\p21c _database_code_depnum_ccdc_archive 'CCDC 914691' #TrackingRef '9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H24 Ho N7 O14' _chemical_formula_weight 739.38 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 13.0407(9) _cell_length_b 14.8401(9) _cell_length_c 13.9335(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.721(2) _cell_angle_gamma 90.00 _cell_volume 2630.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 3.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.481 _exptl_absorpt_correction_T_max 0.539 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8630 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.1133 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4466 _reflns_number_gt 3452 _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. The asymmetric unit contains the entire cluster as well as one nitrate ion. All non H-atoms are refined anisotropically and H-atoms are placed in calculated positions, except for H5, H10, H15, H20 and H24 which were refined with the DFIX card and the thermal parameters fixed to 1.2 times that of the bonded heteroatom. ; _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^)+(0.0000P)^2^+7.3621P] 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 4466 _refine_ls_number_parameters 382 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.001 _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 Ho1 Ho 0.74742(4) 0.08889(3) 0.77822(3) 0.01859(16) Uani 1 1 d . . . O9 O 0.7111(5) 0.1225(5) 0.9390(5) 0.0272(17) Uani 1 1 d . . . O7 O 0.6054(6) 0.0577(4) 0.6269(5) 0.0248(16) Uani 1 1 d . . . O2 O 0.7528(5) -0.0567(4) 0.7196(5) 0.0246(16) Uani 1 1 d . . . O3 O 0.6530(5) 0.2190(4) 0.7321(4) 0.0234(16) Uani 1 1 d . . . O4 O 0.8597(5) 0.2090(4) 0.8365(5) 0.0241(16) Uani 1 1 d . . . N1 N 0.7680(6) -0.2102(5) 0.7217(5) 0.0216(19) Uani 1 1 d D . . H5 H 0.8082 -0.2568 0.7436 0.026 Uiso 1 1 calc RD . . O5 O 0.8257(6) 0.1163(5) 0.6435(5) 0.0306(18) Uani 1 1 d D . . N4 N 1.0537(7) 0.2214(5) 0.9314(6) 0.0193(18) Uani 1 1 d D . . O1 O 0.9187(5) 0.0357(4) 0.8380(5) 0.0226(16) Uani 1 1 d . . . N3 N 0.9423(7) 0.3442(5) 0.8729(6) 0.024(2) Uani 1 1 d D . . H15 H 0.9377 0.4031 0.8665 0.029 Uiso 1 1 calc RD . . N6 N 0.7006(7) 0.0410(6) 0.9658(6) 0.026(2) Uani 1 1 d . . . O10 O 0.7273(6) -0.0190(4) 0.9112(5) 0.0264(17) Uani 1 1 d . . . O6 O 0.5587(5) 0.0550(5) 0.7680(5) 0.0296(17) Uani 1 1 d . . . C13 C 0.8518(8) 0.2947(6) 0.8306(6) 0.016(2) Uani 1 1 d . . . C10 C 0.5710(8) 0.3624(6) 0.7106(7) 0.024(2) Uani 1 1 d . . . H12 H 0.5688 0.3817 0.6429 0.036 Uiso 1 1 calc R . . H13 H 0.5755 0.4155 0.7532 0.036 Uiso 1 1 calc R . . H11 H 0.5071 0.3284 0.7127 0.036 Uiso 1 1 calc R . . O8 O 0.4386(6) 0.0542(5) 0.6323(5) 0.039(2) Uani 1 1 d . . . O11 O 0.6669(6) 0.0228(5) 1.0386(5) 0.038(2) Uani 1 1 d . . . C14 C 1.0369(8) 0.3108(7) 0.9231(7) 0.025(2) Uani 1 1 d . . . C11 C 0.6672(8) 0.3027(7) 0.7465(7) 0.022(2) Uani 1 1 d . . . N2 N 0.6105(7) -0.1592(6) 0.6195(6) 0.024(2) Uani 1 1 d D . . C5 C 0.6715(7) -0.2287(7) 0.6644(6) 0.018(2) Uani 1 1 d . . . C4 C 0.8096(8) -0.1255(7) 0.7492(7) 0.022(2) Uani 1 1 d . . . C2 C 0.9606(8) -0.0412(7) 0.8434(7) 0.022(2) Uani 1 1 d . . . N5 N 0.5314(7) 0.0562(5) 0.6738(6) 0.026(2) Uani 1 1 d . . . C8 C 0.4787(8) -0.2577(7) 0.5376(7) 0.028(2) Uani 1 1 d . . . H8 H 0.4130 -0.2676 0.4935 0.034 Uiso 1 1 calc R . . C15 C 1.1186(8) 0.3697(6) 0.9673(7) 0.021(2) Uani 1 1 d . . . H16 H 1.1102 0.4332 0.9609 0.025 Uiso 1 1 calc R . . C17 C 1.2257(9) 0.2396(7) 1.0274(7) 0.030(3) Uani 1 1 d . . . H18 H 1.2901 0.2150 1.0631 0.036 Uiso 1 1 calc R . . C7 C 0.5382(9) -0.3291(7) 0.5840(7) 0.027(2) Uani 1 1 d . . . H7 H 0.5119 -0.3887 0.5726 0.032 Uiso 1 1 calc R . . C9 C 0.5176(8) -0.1727(7) 0.5573(7) 0.028(3) Uani 1 1 d . . . H9 H 0.4784 -0.1225 0.5267 0.033 Uiso 1 1 calc R . . C16 C 1.2099(8) 0.3334(7) 1.0196(7) 0.026(2) Uani 1 1 d . . . H17 H 1.2645 0.3725 1.0517 0.032 Uiso 1 1 calc R . . C1 C 1.0758(8) -0.0473(7) 0.8973(7) 0.028(3) Uani 1 1 d . . . H1 H 1.1181 -0.0069 0.8659 0.043 Uiso 1 1 calc R . . H2 H 1.1006 -0.1093 0.8945 0.043 Uiso 1 1 calc R . . H3 H 1.0827 -0.0294 0.9662 0.043 Uiso 1 1 calc R . . C6 C 0.6336(8) -0.3152(7) 0.6457(7) 0.024(2) Uani 1 1 d . . . H6 H 0.6739 -0.3650 0.6758 0.029 Uiso 1 1 calc R . . C3 C 0.9123(8) -0.1226(6) 0.8069(6) 0.020(2) Uani 1 1 d . . . H4 H 0.9503 -0.1773 0.8218 0.024 Uiso 1 1 calc R . . C12 C 0.7612(8) 0.3434(6) 0.7919(7) 0.025(2) Uani 1 1 d . . . H14 H 0.7637 0.4073 0.7968 0.030 Uiso 1 1 calc R . . C19 C 0.8127(10) 0.1856(9) 0.5760(9) 0.054(4) Uani 1 1 d . . . H23 H 0.7731 0.1637 0.5122 0.081 Uiso 1 1 calc R . . H21 H 0.8817 0.2073 0.5692 0.081 Uiso 1 1 calc R . . H22 H 0.7741 0.2350 0.5986 0.081 Uiso 1 1 calc R . . N7 N 0.9119(7) -0.4107(6) 0.8132(6) 0.027(2) Uani 1 1 d . . . O13 O 0.9805(5) -0.4647(4) 0.8602(5) 0.0276(17) Uani 1 1 d . . . O14 O 0.8179(7) -0.4351(5) 0.7906(6) 0.041(2) Uani 1 1 d . . . O12 O 0.9388(7) -0.3339(5) 0.7925(6) 0.048(2) Uani 1 1 d . . . C18 C 1.1459(8) 0.1860(7) 0.9822(7) 0.027(2) Uani 1 1 d . . . H19 H 1.1543 0.1224 0.9859 0.032 Uiso 1 1 calc R . . H10 H 0.644(7) -0.108(4) 0.619(7) 0.032 Uiso 1 1 d D . . H20 H 1.007(6) 0.185(5) 0.896(6) 0.032 Uiso 1 1 d D . . H24 H 0.838(8) 0.078(5) 0.603(6) 0.032 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 Ho1 0.0172(3) 0.0155(3) 0.0222(2) 0.0012(2) 0.00243(18) 0.0011(2) O9 0.018(4) 0.032(4) 0.030(4) -0.003(3) 0.004(3) 0.005(3) O7 0.023(4) 0.027(4) 0.028(4) 0.000(3) 0.012(3) -0.001(3) O2 0.021(4) 0.019(4) 0.031(4) -0.001(3) 0.001(3) 0.008(3) O3 0.026(4) 0.012(4) 0.026(3) 0.004(3) -0.006(3) -0.003(3) O4 0.020(4) 0.011(4) 0.040(4) 0.005(3) 0.005(3) 0.000(3) N1 0.020(5) 0.017(5) 0.026(4) 0.004(4) 0.001(4) 0.001(4) O5 0.034(5) 0.027(4) 0.029(4) -0.001(3) 0.004(4) -0.012(4) N4 0.019(5) 0.014(5) 0.024(4) 0.008(3) 0.002(4) 0.002(4) O1 0.022(4) 0.014(4) 0.031(4) 0.001(3) 0.004(3) 0.007(3) N3 0.027(6) 0.014(4) 0.032(5) 0.005(4) 0.009(4) -0.002(4) N6 0.018(5) 0.030(5) 0.025(4) 0.006(4) -0.003(4) 0.000(4) O10 0.024(4) 0.024(4) 0.030(4) -0.004(3) 0.005(3) 0.005(3) O6 0.017(4) 0.034(4) 0.039(4) 0.009(3) 0.009(4) 0.002(3) C13 0.025(6) 0.012(5) 0.013(4) -0.001(4) 0.008(4) -0.002(4) C10 0.020(6) 0.019(6) 0.035(6) -0.000(5) 0.010(5) -0.003(5) O8 0.024(5) 0.043(5) 0.044(4) 0.009(4) -0.002(4) -0.003(4) O11 0.023(5) 0.063(6) 0.034(4) 0.005(4) 0.020(4) -0.000(4) C14 0.018(6) 0.028(6) 0.030(5) 0.001(5) 0.011(5) -0.017(5) C11 0.023(6) 0.024(6) 0.024(5) 0.002(4) 0.012(5) 0.005(5) N2 0.018(5) 0.025(5) 0.027(4) -0.002(4) 0.001(4) -0.005(4) C5 0.010(5) 0.028(6) 0.017(4) -0.000(4) 0.002(4) 0.004(4) C4 0.022(6) 0.025(6) 0.018(5) -0.009(4) 0.002(5) 0.000(5) C2 0.023(6) 0.023(6) 0.024(5) -0.002(4) 0.011(5) -0.000(5) N5 0.025(6) 0.017(5) 0.030(5) 0.001(4) -0.006(4) 0.000(4) C8 0.017(6) 0.033(6) 0.033(5) 0.007(5) 0.003(5) -0.008(5) C15 0.018(6) 0.016(5) 0.028(5) -0.008(4) 0.005(5) -0.002(4) C17 0.028(7) 0.045(7) 0.017(5) -0.000(5) 0.004(5) 0.012(6) C7 0.029(7) 0.020(6) 0.031(5) -0.007(5) 0.008(5) 0.007(5) C9 0.019(6) 0.043(7) 0.023(5) 0.011(5) 0.008(5) 0.011(5) C16 0.020(6) 0.038(7) 0.026(5) -0.005(5) 0.013(5) -0.009(5) C1 0.026(7) 0.029(6) 0.027(5) 0.000(5) -0.002(5) 0.002(5) C6 0.032(7) 0.018(6) 0.023(5) -0.001(4) 0.005(5) 0.002(5) C3 0.024(6) 0.016(5) 0.020(5) -0.004(4) 0.003(4) 0.008(4) C12 0.032(7) 0.004(5) 0.039(6) -0.003(4) 0.009(5) 0.007(5) C19 0.030(8) 0.076(10) 0.065(8) 0.026(8) 0.031(7) 0.020(7) N7 0.024(6) 0.028(5) 0.029(4) -0.005(4) 0.007(4) 0.009(5) O13 0.020(4) 0.024(4) 0.035(4) 0.006(3) -0.002(3) 0.009(3) O14 0.030(5) 0.044(5) 0.046(5) -0.003(4) 0.001(4) 0.002(4) O12 0.074(7) 0.015(4) 0.058(5) 0.019(4) 0.023(5) 0.003(4) C18 0.019(6) 0.029(6) 0.034(6) 0.005(5) 0.006(5) 0.008(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 Ho1 O3 2.304(6) . ? Ho1 O2 2.316(6) . ? Ho1 O4 2.336(6) . ? Ho1 O1 2.342(7) . ? Ho1 O5 2.362(7) . ? Ho1 O9 2.441(6) . ? Ho1 O6 2.486(7) . ? Ho1 O10 2.506(6) . ? Ho1 O7 2.524(7) . ? O9 N6 1.282(10) . ? O7 N5 1.279(10) . ? O2 C4 1.276(11) . ? O3 C11 1.266(11) . ? O4 C13 1.277(10) . ? N1 C5 1.362(11) . ? N1 C4 1.389(12) . ? N1 H5 0.8800 . ? O5 C19 1.378(13) . ? O5 H24 0.837(10) . ? N4 C14 1.346(12) . ? N4 C18 1.359(12) . ? N4 H20 0.881(10) . ? O1 C2 1.261(11) . ? N3 C14 1.369(13) . ? N3 C13 1.405(12) . ? N3 H15 0.8800 . ? N6 O11 1.222(10) . ? N6 O10 1.268(10) . ? O6 N5 1.282(10) . ? C13 C12 1.389(13) . ? C10 C11 1.527(13) . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H11 0.9800 . ? O8 N5 1.221(11) . ? C14 C15 1.411(13) . ? C11 C12 1.388(14) . ? N2 C9 1.340(13) . ? N2 C5 1.367(12) . ? N2 H10 0.879(10) . ? C5 C6 1.379(13) . ? C4 C3 1.402(13) . ? C2 C3 1.405(13) . ? C2 C1 1.527(14) . ? C8 C9 1.365(14) . ? C8 C7 1.386(13) . ? C8 H8 0.9500 . ? C15 C16 1.363(14) . ? C15 H16 0.9500 . ? C17 C18 1.351(14) . ? C17 C16 1.407(14) . ? C17 H18 0.9500 . ? C7 C6 1.363(14) . ? C7 H7 0.9500 . ? C9 H9 0.9500 . ? C16 H17 0.9500 . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C6 H6 0.9500 . ? C3 H4 0.9500 . ? C12 H14 0.9500 . ? C19 H23 0.9800 . ? C19 H21 0.9800 . ? C19 H22 0.9800 . ? N7 O12 1.244(10) . ? N7 O14 1.250(11) . ? N7 O13 1.272(10) . ? C18 H19 0.9500 . ? 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 O3 Ho1 O2 137.7(2) . . ? O3 Ho1 O4 73.3(2) . . ? O2 Ho1 O4 140.2(2) . . ? O3 Ho1 O1 142.3(2) . . ? O2 Ho1 O1 73.2(2) . . ? O4 Ho1 O1 70.0(2) . . ? O3 Ho1 O5 86.1(2) . . ? O2 Ho1 O5 80.1(2) . . ? O4 Ho1 O5 78.3(2) . . ? O1 Ho1 O5 78.2(2) . . ? O3 Ho1 O9 83.4(2) . . ? O2 Ho1 O9 122.8(2) . . ? O4 Ho1 O9 76.0(2) . . ? O1 Ho1 O9 96.0(2) . . ? O5 Ho1 O9 154.1(2) . . ? O3 Ho1 O6 72.1(2) . . ? O2 Ho1 O6 84.1(2) . . ? O4 Ho1 O6 135.4(2) . . ? O1 Ho1 O6 143.8(2) . . ? O5 Ho1 O6 125.8(2) . . ? O9 Ho1 O6 72.8(2) . . ? O3 Ho1 O10 127.2(2) . . ? O2 Ho1 O10 71.4(2) . . ? O4 Ho1 O10 113.0(2) . . ? O1 Ho1 O10 76.6(2) . . ? O5 Ho1 O10 146.3(2) . . ? O9 Ho1 O10 51.6(2) . . ? O6 Ho1 O10 69.5(2) . . ? O3 Ho1 O7 70.8(2) . . ? O2 Ho1 O7 66.9(2) . . ? O4 Ho1 O7 136.0(2) . . ? O1 Ho1 O7 134.6(2) . . ? O5 Ho1 O7 74.6(2) . . ? O9 Ho1 O7 123.3(2) . . ? O6 Ho1 O7 51.7(2) . . ? O10 Ho1 O7 108.9(2) . . ? N6 O9 Ho1 97.4(5) . . ? N5 O7 Ho1 94.2(5) . . ? C4 O2 Ho1 133.9(6) . . ? C11 O3 Ho1 136.7(7) . . ? C13 O4 Ho1 134.6(6) . . ? C5 N1 C4 126.8(8) . . ? C5 N1 H5 116.6 . . ? C4 N1 H5 116.6 . . ? C19 O5 Ho1 131.4(7) . . ? C19 O5 H24 93(7) . . ? Ho1 O5 H24 127(7) . . ? C14 N4 C18 122.3(9) . . ? C14 N4 H20 118(7) . . ? C18 N4 H20 119(7) . . ? C2 O1 Ho1 133.9(7) . . ? C14 N3 C13 127.2(8) . . ? C14 N3 H15 116.4 . . ? C13 N3 H15 116.4 . . ? O11 N6 O10 122.6(9) . . ? O11 N6 O9 122.1(9) . . ? O10 N6 O9 115.3(7) . . ? N6 O10 Ho1 94.7(5) . . ? N5 O6 Ho1 96.0(6) . . ? O4 C13 C12 126.4(9) . . ? O4 C13 N3 116.4(9) . . ? C12 C13 N3 117.0(8) . . ? C11 C10 H12 109.5 . . ? C11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C11 C10 H11 109.5 . . ? H12 C10 H11 109.5 . . ? H13 C10 H11 109.5 . . ? N4 C14 N3 120.7(9) . . ? N4 C14 C15 118.7(10) . . ? N3 C14 C15 120.5(9) . . ? O3 C11 C12 125.7(9) . . ? O3 C11 C10 115.9(9) . . ? C12 C11 C10 118.4(9) . . ? C9 N2 C5 122.4(9) . . ? C9 N2 H10 120(7) . . ? C5 N2 H10 115(7) . . ? N1 C5 N2 119.1(9) . . ? N1 C5 C6 123.0(9) . . ? N2 C5 C6 117.9(9) . . ? O2 C4 N1 118.2(9) . . ? O2 C4 C3 125.0(9) . . ? N1 C4 C3 116.8(9) . . ? O1 C2 C3 127.1(10) . . ? O1 C2 C1 116.7(9) . . ? C3 C2 C1 116.2(9) . . ? O8 N5 O7 122.6(8) . . ? O8 N5 O6 120.4(9) . . ? O7 N5 O6 116.9(8) . . ? C9 C8 C7 117.9(10) . . ? C9 C8 H8 121.0 . . ? C7 C8 H8 121.0 . . ? C16 C15 C14 118.4(10) . . ? C16 C15 H16 120.8 . . ? C14 C15 H16 120.8 . . ? C18 C17 C16 117.5(10) . . ? C18 C17 H18 121.2 . . ? C16 C17 H18 121.2 . . ? C6 C7 C8 121.2(10) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? N2 C9 C8 120.7(10) . . ? N2 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C15 C16 C17 121.9(10) . . ? C15 C16 H17 119.1 . . ? C17 C16 H17 119.1 . . ? C2 C1 H1 109.5 . . ? C2 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? C2 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C7 C6 C5 119.9(9) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C4 C3 C2 122.0(9) . . ? C4 C3 H4 119.0 . . ? C2 C3 H4 119.0 . . ? C11 C12 C13 122.7(9) . . ? C11 C12 H14 118.6 . . ? C13 C12 H14 118.6 . . ? O5 C19 H23 109.5 . . ? O5 C19 H21 109.5 . . ? H23 C19 H21 109.5 . . ? O5 C19 H22 109.5 . . ? H23 C19 H22 109.5 . . ? H21 C19 H22 109.5 . . ? O12 N7 O14 121.3(9) . . ? O12 N7 O13 119.6(9) . . ? O14 N7 O13 119.1(9) . . ? C17 C18 N4 121.2(10) . . ? C17 C18 H19 119.4 . . ? N4 C18 H19 119.4 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.937 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.183