Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Zheming Wang' _publ_contact_author_email zmw@pku.edu.cn _publ_section_title ; Erbium-Formate Frameworks Templated by Diammonium Cations: Syntheses, Structures, Structural Transition and Magnetic Properties ; loop_ _publ_author_name 'Zheming Wang' 'Mengyuan Li' 'Bin Liu' 'Bingwu Wang' 'Song Gao' M.Kurmoo #### End of 2 at 290 K #### data_CCDC812093-1-at-160K _database_code_depnum_ccdc_archive 'CCDC 789449' #TrackingRef '- DT-ART-12-2011-010241.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Er2 N2 O16' _chemical_formula_weight 784.84 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 orthorhombic _symmetry_space_group_name_H-M 'P na2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.0939(3) _cell_length_b 13.3115(2) _cell_length_c 8.5775(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2065.95(7) _cell_formula_units_Z 4 _cell_measurement_temperature 160 _cell_measurement_reflns_used 18843 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description column _exptl_crystal_colour pink _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 8.153 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.150 0 -1 0 0.190 1 0 2 0.080 -1 0 -2 0.090 -1 0 2 0.090 1 0 -2 0.090 1 -4 3 0.120 0 6 1 0.140 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.155 _exptl_absorpt_correction_T_max 0.327 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 160 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31386 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4684 _reflns_number_gt 3800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction (Numerical): P. Coppens, in Crystallographic Computing, edited by F. R. Ahmed, S. R. Hall, C. P. Huber, pp255-270, 1970, Copenhagen: Munksgaard. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+1.3053P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 174(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 4684 _refine_ls_number_parameters 285 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Er1 Er 0.601024(16) 0.37458(3) 0.25264(4) 0.02263(14) Uani 1 1 d . . . Er2 Er 0.393797(16) 0.12491(3) 0.75236(4) 0.02240(14) Uani 1 1 d . . . O1 O 0.5639(3) 0.2941(5) 0.4811(10) 0.0380(16) Uani 1 1 d . . . O2 O 0.4971(4) 0.2108(4) 0.6521(10) 0.0324(16) Uani 1 1 d . . . O3 O 0.6480(3) 0.2057(4) 0.2333(11) 0.0388(18) Uani 1 1 d . . . O4 O 0.6478(3) 0.0415(4) 0.2819(11) 0.043(2) Uani 1 1 d . . . O5 O 0.7032(9) 0.3864(5) 0.4205(13) 0.040(2) Uani 1 1 d . . . O6 O 0.7957(8) 0.3811(4) 0.5815(14) 0.036(2) Uani 1 1 d . . . O7 O 0.7011(7) 0.3660(4) 0.0910(13) 0.032(2) Uani 1 1 d . . . O8 O 0.7915(9) 0.3678(5) -0.0761(14) 0.042(3) Uani 1 1 d . . . O9 O 0.6477(3) 0.5433(4) 0.2382(8) 0.0297(14) Uani 1 1 d . . . O10 O 0.6475(3) 0.7076(4) 0.1959(8) 0.0303(15) Uani 1 1 d . . . O11 O 0.5034(4) 0.4671(4) 0.3384(10) 0.0329(16) Uani 1 1 d . . . O12 O 0.4343(3) 0.5532(4) 0.5077(9) 0.0327(14) Uani 1 1 d . . . O13 O 0.5018(4) 0.2798(4) 0.1533(10) 0.0327(15) Uani 1 1 d . . . O14 O 0.4271(3) 0.2159(4) -0.0269(9) 0.0347(15) Uani 1 1 d . . . O15 O 0.4971(3) 0.0406(4) 0.8496(9) 0.0274(14) Uani 1 1 d . . . O16 O 0.5719(3) -0.0372(5) 1.0164(10) 0.0376(16) Uani 1 1 d . . . C1 C 0.5102(7) 0.2468(9) 0.5206(13) 0.027(2) Uani 1 1 d . . . H1 H 0.4737 0.2357 0.4428 0.032 Uiso 1 1 calc R . . C2 C 0.6155(5) 0.1186(7) 0.2629(18) 0.041(3) Uani 1 1 d . . . H2 H 0.5631 0.1175 0.2694 0.049 Uiso 1 1 calc R . . C3 C 0.7325(6) 0.3542(7) 0.5250(13) 0.041(2) Uiso 1 1 d . . . H3 H 0.7079 0.3012 0.5778 0.050 Uiso 1 1 calc R . . C4 C 0.7330(6) 0.3952(7) -0.0391(12) 0.039(2) Uani 1 1 d . . . H4 H 0.7073 0.4405 -0.1055 0.047 Uiso 1 1 calc R . . C5 C 0.6165(6) 0.6217(7) 0.2141(12) 0.035(3) Uani 1 1 d . . . H5 H 0.5641 0.6198 0.2081 0.041 Uiso 1 1 calc R . . C6 C 0.4932(8) 0.5069(10) 0.4672(16) 0.038(3) Uani 1 1 d . . . H6 H 0.5320 0.5028 0.5415 0.045 Uiso 1 1 calc R . . C7 C 0.4881(6) 0.2486(8) 0.0203(13) 0.026(2) Uani 1 1 d . . . H7 H 0.5275 0.2496 -0.0528 0.031 Uiso 1 1 calc R . . C8 C 0.5105(7) 0.0009(10) 0.9749(14) 0.034(3) Uani 1 1 d . . . H8 H 0.4713 -0.0017 1.0484 0.041 Uiso 1 1 calc R . . C9 C 0.8335(5) 0.5717(7) 0.1882(12) 0.044(2) Uani 1 1 d . . . H9A H 0.7954 0.5997 0.1198 0.065 Uiso 1 1 calc R . . H9B H 0.8535 0.5102 0.1417 0.065 Uiso 1 1 calc R . . H9C H 0.8734 0.6209 0.2014 0.065 Uiso 1 1 calc R . . C10 C 0.7751(6) 0.6408(6) 0.4276(12) 0.038(2) Uani 1 1 d . . . H10A H 0.7482 0.6851 0.3544 0.045 Uiso 1 1 calc R . . H10B H 0.8183 0.6780 0.4683 0.045 Uiso 1 1 calc R . . C11 C 0.7243(6) 0.6106(7) 0.5625(13) 0.046(2) Uani 1 1 d . . . H11A H 0.6808 0.5739 0.5216 0.055 Uiso 1 1 calc R . . H11B H 0.7511 0.5657 0.6350 0.055 Uiso 1 1 calc R . . C12 C 0.6678(6) 0.6809(8) 0.8014(12) 0.054(3) Uani 1 1 d . . . H12A H 0.6219 0.6426 0.7891 0.080 Uiso 1 1 calc R . . H12B H 0.6572 0.7444 0.8549 0.080 Uiso 1 1 calc R . . H12C H 0.7031 0.6417 0.8631 0.080 Uiso 1 1 calc R . . N1 N 0.8004(4) 0.5478(6) 0.3443(10) 0.0444(18) Uani 1 1 d . . . H1A H 0.7608 0.5053 0.3309 0.053 Uiso 1 1 calc R . . H1B H 0.8349 0.5151 0.4046 0.053 Uiso 1 1 calc R . . N2 N 0.6997(4) 0.7021(5) 0.6463(9) 0.0397(17) Uani 1 1 d . . . H2A H 0.7394 0.7446 0.6581 0.048 Uiso 1 1 calc R . . H2B H 0.6649 0.7348 0.5866 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0250(2) 0.0217(2) 0.0212(2) 0.00022(11) 0.0014(3) 0.00015(14) Er2 0.0250(2) 0.0212(2) 0.0210(2) -0.00049(11) 0.0064(3) -0.00031(14) O1 0.034(3) 0.053(4) 0.027(3) 0.011(3) 0.000(3) -0.010(3) O2 0.033(4) 0.032(3) 0.032(4) 0.006(3) 0.004(3) 0.003(3) O3 0.029(3) 0.019(3) 0.068(5) 0.001(3) 0.001(4) -0.004(2) O4 0.027(3) 0.028(3) 0.074(6) -0.008(3) -0.002(3) -0.003(2) O5 0.046(5) 0.049(4) 0.024(5) -0.002(3) -0.002(4) -0.009(4) O6 0.023(4) 0.044(4) 0.041(6) -0.018(3) -0.005(4) -0.015(3) O7 0.023(4) 0.039(4) 0.034(5) 0.011(3) 0.012(3) 0.004(3) O8 0.039(6) 0.045(5) 0.041(6) 0.008(3) 0.003(5) 0.008(3) O9 0.029(3) 0.027(3) 0.033(3) -0.005(3) -0.005(3) -0.002(2) O10 0.031(3) 0.018(3) 0.041(4) 0.000(2) 0.002(2) -0.005(2) O11 0.030(4) 0.036(4) 0.033(4) -0.009(3) 0.006(3) 0.008(3) O12 0.040(4) 0.029(3) 0.028(3) -0.002(3) 0.007(3) 0.008(2) O13 0.035(4) 0.033(3) 0.030(4) -0.002(3) -0.002(3) -0.002(3) O14 0.031(3) 0.041(3) 0.032(4) -0.016(3) 0.003(3) -0.002(3) O15 0.030(3) 0.029(3) 0.023(3) 0.000(3) -0.002(3) 0.003(3) O16 0.034(3) 0.051(4) 0.028(4) -0.002(3) -0.004(3) 0.013(3) C1 0.026(6) 0.034(4) 0.020(4) 0.013(4) -0.003(4) 0.008(4) C2 0.026(3) 0.034(5) 0.063(8) 0.007(4) -0.008(6) 0.006(4) C4 0.054(5) 0.034(4) 0.030(5) -0.005(3) 0.003(4) 0.000(4) C5 0.024(3) 0.041(6) 0.038(7) -0.023(4) -0.001(4) 0.009(4) C6 0.033(6) 0.031(5) 0.049(7) 0.018(5) 0.009(6) 0.005(4) C7 0.026(6) 0.029(4) 0.023(4) -0.012(4) 0.006(4) 0.006(4) C8 0.030(7) 0.040(5) 0.032(6) -0.017(5) -0.003(5) 0.007(4) C9 0.041(5) 0.049(5) 0.040(5) 0.006(4) 0.003(4) -0.007(4) C10 0.051(5) 0.029(4) 0.034(5) 0.003(4) -0.004(4) -0.006(4) C11 0.049(6) 0.046(5) 0.043(5) -0.011(4) -0.002(5) 0.001(4) C12 0.044(5) 0.077(7) 0.039(5) 0.000(5) -0.006(4) -0.017(5) N1 0.041(4) 0.054(5) 0.038(4) 0.001(4) 0.001(3) -0.010(3) N2 0.034(4) 0.051(4) 0.035(4) 0.009(3) 0.000(3) -0.002(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 Er1 O11 2.276(6) . ? Er1 O7 2.283(12) . ? Er1 O1 2.332(8) . ? Er1 O5 2.349(15) . ? Er1 O13 2.354(6) . ? Er1 O12 2.397(7) 2_664 ? Er1 O9 2.402(6) . ? Er1 O3 2.409(6) . ? Er2 O6 2.303(13) 3_455 ? Er2 O14 2.327(7) 1_556 ? Er2 O15 2.335(6) . ? Er2 O4 2.353(6) 2_655 ? Er2 O2 2.354(6) . ? Er2 O8 2.366(15) 3_456 ? Er2 O10 2.401(6) 2_665 ? Er2 O16 2.418(8) 2_654 ? O1 C1 1.207(15) . ? O2 C1 1.248(13) . ? O3 C2 1.326(11) . ? O4 C2 1.192(11) . ? O4 Er2 2.353(6) 2_654 ? O5 C3 1.126(16) . ? O6 C3 1.293(16) . ? O6 Er2 2.303(13) 3 ? O7 C4 1.316(14) . ? O8 C4 1.165(18) . ? O8 Er2 2.366(15) 3_554 ? O9 C5 1.205(10) . ? O10 C5 1.282(11) . ? O10 Er2 2.401(6) 2_664 ? O11 C6 1.239(16) . ? O12 C6 1.279(15) . ? O12 Er1 2.397(7) 2_665 ? O13 C7 1.239(13) . ? O14 C7 1.254(14) . ? O14 Er2 2.327(7) 1_554 ? O15 C8 1.221(15) . ? O16 C8 1.271(15) . ? O16 Er2 2.418(8) 2_655 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 N1 1.502(11) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.501(11) . ? C10 C11 1.531(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.483(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N2 1.478(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? 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 O11 Er1 O7 147.0(3) . . ? O11 Er1 O1 75.7(3) . . ? O7 Er1 O1 135.7(3) . . ? O11 Er1 O5 112.1(3) . . ? O7 Er1 O5 75.6(2) . . ? O1 Er1 O5 75.1(3) . . ? O11 Er1 O13 79.35(16) . . ? O7 Er1 O13 111.0(3) . . ? O1 Er1 O13 80.7(2) . . ? O5 Er1 O13 149.1(3) . . ? O11 Er1 O12 81.9(3) . 2_664 ? O7 Er1 O12 72.5(3) . 2_664 ? O1 Er1 O12 147.55(17) . 2_664 ? O5 Er1 O12 136.1(3) . 2_664 ? O13 Er1 O12 72.2(2) . 2_664 ? O11 Er1 O9 77.5(2) . . ? O7 Er1 O9 74.7(2) . . ? O1 Er1 O9 125.0(3) . . ? O5 Er1 O9 72.1(3) . . ? O13 Er1 O9 138.7(2) . . ? O12 Er1 O9 71.0(2) 2_664 . ? O11 Er1 O3 143.3(2) . . ? O7 Er1 O3 68.4(2) . . ? O1 Er1 O3 74.4(3) . . ? O5 Er1 O3 80.0(3) . . ? O13 Er1 O3 75.2(2) . . ? O12 Er1 O3 114.1(3) 2_664 . ? O9 Er1 O3 138.1(2) . . ? O6 Er2 O14 137.4(3) 3_455 1_556 ? O6 Er2 O15 145.8(2) 3_455 . ? O14 Er2 O15 75.6(2) 1_556 . ? O6 Er2 O4 77.8(3) 3_455 2_655 ? O14 Er2 O4 119.0(3) 1_556 2_655 ? O15 Er2 O4 76.4(2) . 2_655 ? O6 Er2 O2 113.3(3) 3_455 . ? O14 Er2 O2 80.7(2) 1_556 . ? O15 Er2 O2 74.25(15) . . ? O4 Er2 O2 138.6(2) 2_655 . ? O6 Er2 O8 78.2(2) 3_455 3_456 ? O14 Er2 O8 71.1(3) 1_556 3_456 ? O15 Er2 O8 115.1(4) . 3_456 ? O4 Er2 O8 73.8(2) 2_655 3_456 ? O2 Er2 O8 145.9(2) . 3_456 ? O6 Er2 O10 70.4(2) 3_455 2_665 ? O14 Er2 O10 76.2(2) 1_556 2_665 ? O15 Er2 O10 140.2(2) . 2_665 ? O4 Er2 O10 142.81(19) 2_655 2_665 ? O2 Er2 O10 73.9(2) . 2_665 ? O8 Er2 O10 81.0(3) 3_456 2_665 ? O6 Er2 O16 69.4(3) 3_455 2_654 ? O14 Er2 O16 149.98(16) 1_556 2_654 ? O15 Er2 O16 82.0(2) . 2_654 ? O4 Er2 O16 73.6(3) 2_655 2_654 ? O2 Er2 O16 74.0(2) . 2_654 ? O8 Er2 O16 137.8(3) 3_456 2_654 ? O10 Er2 O16 111.1(3) 2_665 2_654 ? C1 O1 Er1 135.1(7) . . ? C1 O2 Er2 131.9(7) . . ? C2 O3 Er1 130.3(6) . . ? C2 O4 Er2 129.7(6) . 2_654 ? C3 O5 Er1 146.4(11) . . ? C3 O6 Er2 155.6(8) . 3 ? C4 O7 Er1 148.1(9) . . ? C4 O8 Er2 150.2(9) . 3_554 ? C5 O9 Er1 130.8(6) . . ? C5 O10 Er2 131.8(6) . 2_664 ? C6 O11 Er1 129.4(7) . . ? C6 O12 Er1 130.8(8) . 2_665 ? C7 O13 Er1 131.7(7) . . ? C7 O14 Er2 132.2(6) . 1_554 ? C8 O15 Er2 132.9(7) . . ? C8 O16 Er2 130.6(7) . 2_655 ? O1 C1 O2 127.4(11) . . ? O1 C1 H1 116.3 . . ? O2 C1 H1 116.3 . . ? O4 C2 O3 124.2(9) . . ? O4 C2 H2 117.9 . . ? O3 C2 H2 117.9 . . ? O5 C3 O6 127.5(13) . . ? O5 C3 H3 116.2 . . ? O6 C3 H3 116.2 . . ? O8 C4 O7 122.5(12) . . ? O8 C4 H4 118.7 . . ? O7 C4 H4 118.7 . . ? O9 C5 O10 126.0(9) . . ? O9 C5 H5 117.0 . . ? O10 C5 H5 117.0 . . ? O11 C6 O12 124.9(12) . . ? O11 C6 H6 117.6 . . ? O12 C6 H6 117.6 . . ? O13 C7 O14 126.2(10) . . ? O13 C7 H7 116.9 . . ? O14 C7 H7 116.9 . . ? O15 C8 O16 126.3(11) . . ? O15 C8 H8 116.9 . . ? O16 C8 H8 116.9 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 109.0(6) . . ? N1 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N1 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C10 109.3(7) . . ? N2 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? N2 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 N1 C9 111.8(7) . . ? C10 N1 H1A 109.3 . . ? C9 N1 H1A 109.3 . . ? C10 N1 H1B 109.3 . . ? C9 N1 H1B 109.3 . . ? H1A N1 H1B 107.9 . . ? C12 N2 C11 113.4(7) . . ? C12 N2 H2A 108.9 . . ? C11 N2 H2A 108.9 . . ? C12 N2 H2B 108.9 . . ? C11 N2 H2B 108.9 . . ? H2A N2 H2B 107.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O5 0.92 2.04 2.852(14) 145.6 . N1 H1A O9 0.92 2.25 2.909(10) 127.8 . N1 H1B O6 0.92 2.45 3.011(13) 119.8 . N1 H1B O16 0.92 2.06 2.967(11) 167.5 4_654 N2 H2A O3 0.92 2.20 2.855(10) 127.7 4_655 N2 H2A O7 0.92 2.03 2.865(12) 151.0 4_655 N2 H2B O8 0.92 2.39 2.920(11) 116.7 4_655 N2 H2B O14 0.92 2.04 2.943(10) 167.6 2_665 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.305 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.161 #### End of 1 at 290 K #### data_CCDC789450-2-at-290K _database_code_depnum_ccdc_archive 'CCDC 789450' #TrackingRef '- DT-ART-12-2011-010241.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H26 Er2 N2 O16' _chemical_formula_weight 812.89 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.7325(2) _cell_length_b 12.9990(2) _cell_length_c 12.7787(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.9751(6) _cell_angle_gamma 90.00 _cell_volume 2364.11(6) _cell_formula_units_Z 4 _cell_measurement_temperature 290 _cell_measurement_reflns_used 15829 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 7.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.258 _exptl_absorpt_correction_T_max 0.570 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995, 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 290 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28351 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2714 _reflns_number_gt 2216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00135(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2714 _refine_ls_number_parameters 169 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.092 _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 Er1 Er 0.264767(12) 0.431931(12) 0.188853(13) 0.02274(9) Uani 1 1 d . . . O1 O 0.1162(3) 0.4526(3) 0.2322(3) 0.0589(10) Uani 1 1 d . . . O2 O 0.1165(3) 0.4770(6) 0.0693(3) 0.124(2) Uani 1 1 d . . . O31 O 0.2933(7) 0.3095(5) 0.0685(6) 0.0508(19) Uani 0.50 1 d PD . . O32 O 0.2776(7) 0.1804(5) -0.0464(6) 0.055(2) Uani 0.50 1 d PD . . O4 O 0.3126(2) 0.4427(2) 0.3797(2) 0.0410(8) Uani 1 1 d . . . O5 O 0.3122(2) 0.4820(2) 0.5476(2) 0.0388(7) Uani 1 1 d . . . O6 O 0.2435(3) 0.2711(2) 0.2546(3) 0.0603(11) Uani 1 1 d . . . O7 O 0.2268(2) 0.1058(2) 0.2751(3) 0.0477(8) Uani 1 1 d . . . O8 O 0.4238(3) 0.4142(3) 0.2321(3) 0.0703(13) Uani 1 1 d . . . C1 C 0.0761(4) 0.4768(4) 0.1392(5) 0.0519(13) Uani 1 1 d . . . H1 H 0.0130 0.4954 0.1227 0.062 Uiso 1 1 calc R . . C2 C 0.2500 0.2500 0.0000 0.057(2) Uani 1 2 d SD . . H2 H 0.1847(15) 0.266(4) -0.027(4) 0.069 Uiso 0.50 1 d PD . . C3 C 0.2765(3) 0.4825(3) 0.4468(3) 0.0325(10) Uani 1 1 d . . . H3 H 0.2188 0.5152 0.4211 0.039 Uiso 1 1 calc R . . C4 C 0.2702(4) 0.1818(3) 0.2597(3) 0.0427(12) Uani 1 1 d . . . H4 H 0.3301 0.1705 0.2509 0.051 Uiso 1 1 calc R . . C5 C 0.5000 0.3737(7) 0.2500 0.0535(19) Uani 1 2 d S . . H5 H 0.5000 0.3022 0.2500 0.064 Uiso 1 2 calc SR . . N1 N 0.4473(3) 0.3221(3) 0.5974(4) 0.0619(12) Uani 1 1 d D . . H1A H 0.4102 0.3786 0.5941 0.074 Uiso 1 1 calc R . . C6 C 0.5073(8) 0.3143(9) 0.7059(5) 0.191(6) Uani 1 1 d D . . H6A H 0.5422 0.2513 0.7047 0.230 Uiso 1 1 calc R . . H6B H 0.5525 0.3694 0.7098 0.230 Uiso 1 1 calc R . . C7 C 0.5132(5) 0.3411(7) 0.5284(7) 0.137(4) Uani 1 1 d D . . H7A H 0.5514 0.4001 0.5552 0.206 Uiso 1 1 calc R . . H7B H 0.4780 0.3535 0.4551 0.206 Uiso 1 1 calc R . . H7C H 0.5528 0.2821 0.5306 0.206 Uiso 1 1 calc R . . C8 C 0.3865(4) 0.2332(4) 0.5596(5) 0.0662(15) Uani 1 1 d D . . H8A H 0.3462 0.2474 0.4891 0.099 Uiso 1 1 calc R . . H8B H 0.3489 0.2198 0.6093 0.099 Uiso 1 1 calc R . . H8C H 0.4245 0.1740 0.5557 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.03325(13) 0.01677(12) 0.01934(11) -0.00220(7) 0.00885(8) -0.00193(7) O1 0.041(2) 0.085(3) 0.053(2) 0.011(2) 0.0143(19) 0.0134(19) O2 0.037(2) 0.291(7) 0.042(2) 0.033(4) 0.004(2) -0.002(3) O31 0.079(6) 0.038(4) 0.042(4) -0.025(3) 0.028(4) -0.015(4) O32 0.101(7) 0.030(4) 0.036(4) -0.027(3) 0.022(5) -0.012(4) O4 0.050(2) 0.052(2) 0.0222(15) -0.0056(13) 0.0107(15) 0.0087(15) O5 0.051(2) 0.0435(19) 0.0230(15) -0.0019(14) 0.0122(14) 0.0127(15) O6 0.109(3) 0.0167(17) 0.065(2) 0.0053(15) 0.040(2) 0.0003(17) O7 0.068(2) 0.0201(16) 0.054(2) 0.0095(16) 0.0140(17) -0.0039(15) O8 0.037(2) 0.122(4) 0.056(3) 0.015(2) 0.0198(19) 0.022(2) C1 0.036(3) 0.062(3) 0.055(3) 0.007(3) 0.007(3) 0.000(2) C2 0.084(6) 0.046(4) 0.051(5) -0.004(4) 0.034(5) -0.022(4) C3 0.044(3) 0.028(2) 0.027(2) 0.0003(18) 0.012(2) 0.0033(19) C4 0.066(3) 0.029(3) 0.035(3) 0.000(2) 0.017(2) -0.003(2) C5 0.041(5) 0.073(6) 0.048(4) 0.000 0.014(3) 0.000 N1 0.050(3) 0.054(3) 0.072(3) 0.006(2) -0.001(2) 0.020(2) C6 0.169(11) 0.285(14) 0.107(9) -0.078(9) 0.013(10) -0.028(12) C7 0.072(5) 0.202(10) 0.150(8) 0.076(7) 0.052(5) 0.005(6) C8 0.070(4) 0.053(3) 0.070(4) 0.003(3) 0.008(3) 0.004(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 Er1 O8 2.276(4) . ? Er1 O32 2.291(6) 7 ? Er1 O7 2.303(3) 4 ? Er1 O6 2.305(3) . ? Er1 O31 2.326(7) . ? Er1 O4 2.361(3) . ? Er1 O5 2.377(3) 6_565 ? Er1 O2 2.393(4) . ? Er1 O1 2.408(4) . ? Er1 C1 2.749(5) . ? O1 C1 1.223(6) . ? O2 C1 1.195(6) . ? O31 O32 1.018(10) 7 ? O31 C2 1.218(7) . ? O32 O31 1.018(10) 7 ? O32 C2 1.208(7) . ? O32 Er1 2.291(6) 7 ? O4 C3 1.233(5) . ? O5 C3 1.260(4) . ? O5 Er1 2.377(3) 6_566 ? O6 C4 1.222(5) . ? O7 C4 1.220(5) . ? O7 Er1 2.303(3) 4_545 ? O8 C5 1.206(5) . ? C1 H1 0.9300 . ? C2 O32 1.208(7) 7 ? C2 O31 1.218(7) 7 ? C2 H2 0.957(15) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 O8 1.206(5) 2_655 ? C5 H5 0.9300 . ? N1 C6 1.442(9) . ? N1 C8 1.466(6) . ? N1 C7 1.492(7) . ? N1 H1A 0.9100 . ? C6 C6 1.201(13) 2_656 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 O8 Er1 O32 100.4(3) . 7 ? O8 Er1 O7 92.98(14) . 4 ? O32 Er1 O7 140.7(2) 7 4 ? O8 Er1 O6 92.74(15) . . ? O32 Er1 O6 71.1(2) 7 . ? O7 Er1 O6 145.37(12) 4 . ? O8 Er1 O31 75.0(2) . . ? O32 Er1 O31 25.5(2) 7 . ? O7 Er1 O31 142.6(2) 4 . ? O6 Er1 O31 71.6(2) . . ? O8 Er1 O4 75.04(13) . . ? O32 Er1 O4 143.7(2) 7 . ? O7 Er1 O4 75.46(11) 4 . ? O6 Er1 O4 73.14(12) . . ? O31 Er1 O4 131.8(2) . . ? O8 Er1 O5 75.28(13) . 6_565 ? O32 Er1 O5 76.7(2) 7 6_565 ? O7 Er1 O5 71.24(11) 4 6_565 ? O6 Er1 O5 142.96(11) . 6_565 ? O31 Er1 O5 71.4(2) . 6_565 ? O4 Er1 O5 133.51(11) . 6_565 ? O8 Er1 O2 153.19(15) . . ? O32 Er1 O2 68.4(3) 7 . ? O7 Er1 O2 83.1(2) 4 . ? O6 Er1 O2 105.52(19) . . ? O31 Er1 O2 92.1(3) . . ? O4 Er1 O2 128.64(14) . . ? O5 Er1 O2 78.38(14) 6_565 . ? O8 Er1 O1 153.60(15) . . ? O32 Er1 O1 100.2(3) 7 . ? O7 Er1 O1 81.35(12) 4 . ? O6 Er1 O1 78.49(13) . . ? O31 Er1 O1 124.0(2) . . ? O4 Er1 O1 78.58(12) . . ? O5 Er1 O1 125.81(12) 6_565 . ? O2 Er1 O1 52.08(14) . . ? O8 Er1 C1 173.54(15) . . ? O32 Er1 C1 84.3(3) 7 . ? O7 Er1 C1 80.61(14) 4 . ? O6 Er1 C1 93.00(15) . . ? O31 Er1 C1 109.7(3) . . ? O4 Er1 C1 103.86(14) . . ? O5 Er1 C1 101.70(14) 6_565 . ? O2 Er1 C1 25.71(14) . . ? O1 Er1 C1 26.39(13) . . ? C1 O1 Er1 92.6(3) . . ? C1 O2 Er1 94.0(3) . . ? O32 O31 C2 64.7(6) 7 . ? O32 O31 Er1 75.4(6) 7 . ? C2 O31 Er1 139.4(6) . . ? O31 O32 C2 65.7(6) 7 . ? O31 O32 Er1 79.2(6) 7 7 ? C2 O32 Er1 144.1(7) . 7 ? C3 O4 Er1 132.5(3) . . ? C3 O5 Er1 130.3(3) . 6_566 ? C4 O6 Er1 144.1(3) . . ? C4 O7 Er1 145.4(3) . 4_545 ? C5 O8 Er1 159.9(5) . . ? O2 C1 O1 121.2(5) . . ? O2 C1 Er1 60.2(3) . . ? O1 C1 Er1 61.0(3) . . ? O2 C1 H1 119.4 . . ? O1 C1 H1 119.4 . . ? Er1 C1 H1 177.2 . . ? O32 C2 O32 180.0(6) 7 . ? O32 C2 O31 130.4(4) 7 7 ? O32 C2 O31 49.6(4) . 7 ? O32 C2 O31 49.6(4) 7 . ? O32 C2 O31 130.4(4) . . ? O31 C2 O31 180.0(7) 7 . ? O32 C2 H2 65.0(17) 7 . ? O32 C2 H2 115.0(16) . . ? O31 C2 H2 65.7(17) 7 . ? O31 C2 H2 114.3(17) . . ? O4 C3 O5 124.6(4) . . ? O4 C3 H3 117.7 . . ? O5 C3 H3 117.7 . . ? O7 C4 O6 127.1(5) . . ? O7 C4 H4 116.4 . . ? O6 C4 H4 116.4 . . ? O8 C5 O8 128.3(9) . 2_655 ? O8 C5 H5 115.8 . . ? O8 C5 H5 115.8 2_655 . ? C6 N1 C8 115.6(6) . . ? C6 N1 C7 104.4(6) . . ? C8 N1 C7 111.9(5) . . ? C6 N1 H1A 108.2 . . ? C8 N1 H1A 108.2 . . ? C7 N1 H1A 108.2 . . ? C6 C6 N1 133.4(15) 2_656 . ? C6 C6 H6A 103.9 2_656 . ? N1 C6 H6A 103.9 . . ? C6 C6 H6B 103.9 2_656 . ? N1 C6 H6B 103.9 . . ? H6A C6 H6B 105.4 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O5 0.91 1.95 2.834(5) 163.6 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.344 _refine_diff_density_min -1.157 _refine_diff_density_rms 0.125 #### End of 1 at 160 K #### data_CCDC812094-2-at-160K _database_code_depnum_ccdc_archive 'CCDC 812093' #TrackingRef '- DT-ART-12-2011-010241.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H26 Er2 N2 O16' _chemical_formula_weight 812.89 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 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6163(2) _cell_length_b 26.0625(3) _cell_length_c 12.67840(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.0459(5) _cell_angle_gamma 90.00 _cell_volume 4664.10(9) _cell_formula_units_Z 8 _cell_measurement_temperature 160 _cell_measurement_reflns_used 48906 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 7.227 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.070 0 -1 0 0.170 0 0 1 0.040 0 0 -1 0.040 3 0 -1 0.130 -3 0 1 0.090 3 -14 -1 0.125 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.226 _exptl_absorpt_correction_T_max 0.576 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 160 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 109815 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10694 _reflns_number_gt 6124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction (Numerical): P. Coppens, in Crystallographic Computing, edited by F. R. Ahmed, S. R. Hall, C. P. Huber, pp255-270, 1970, Copenhagen: Munksgaard. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000074(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10694 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 Er1 Er 0.225334(19) 0.465375(12) 0.30476(2) 0.01273(8) Uani 1 1 d . . . Er2 Er 0.248742(19) 0.215814(13) 0.181509(19) 0.01347(8) Uani 1 1 d . . . Er3 Er 0.718310(19) 0.214368(12) 0.303951(19) 0.01322(8) Uani 1 1 d . . . Er4 Er 0.756206(19) 0.465271(12) 0.19186(2) 0.01257(8) Uani 1 1 d . . . O1 O 0.3756(3) 0.4707(2) 0.4341(4) 0.0488(15) Uani 1 1 d . . . O2 O 0.3750(3) 0.48310(17) 0.2659(3) 0.0272(12) Uani 1 1 d . . . O3 O 0.1036(3) 0.25512(18) 0.0685(3) 0.0325(12) Uani 1 1 d . . . O4 O 0.1017(3) 0.22478(17) 0.2283(3) 0.0258(11) Uani 1 1 d . . . O5 O 0.8689(3) 0.2203(2) 0.4281(4) 0.0476(15) Uani 1 1 d . . . O6 O 0.8660(3) 0.23475(17) 0.2609(3) 0.0284(12) Uani 1 1 d . . . O7 O 0.6114(3) 0.5004(2) 0.0761(4) 0.0400(13) Uani 1 1 d . . . O8 O 0.6090(3) 0.47633(18) 0.2400(4) 0.0298(12) Uani 1 1 d . . . O9 O 0.2637(3) 0.38480(16) 0.2519(3) 0.0244(11) Uani 1 1 d . . . O10 O 0.2667(3) 0.30108(16) 0.2304(3) 0.0227(11) Uani 1 1 d . . . O11 O 0.4005(3) 0.19241(18) 0.2122(4) 0.0376(13) Uani 1 1 d . . . O12 O 0.5538(3) 0.20886(19) 0.2594(3) 0.0330(12) Uani 1 1 d . . . O13 O 0.7033(3) 0.30205(16) 0.2692(3) 0.0269(12) Uani 1 1 d . . . O14 O 0.7255(3) 0.38471(16) 0.2543(3) 0.0245(11) Uani 1 1 d . . . O15 O 0.2154(3) 0.55303(16) 0.2663(3) 0.0228(11) Uani 1 1 d . . . O16 O 0.2468(3) 0.63508(17) 0.2586(4) 0.0279(12) Uani 1 1 d . . . O17 O 0.1870(3) 0.46793(17) 0.1125(3) 0.0211(10) Uani 1 1 d . . . O18 O 0.1914(3) 0.49103(16) -0.0533(3) 0.0195(11) Uani 1 1 d . . . O19 O 0.1841(3) 0.51278(16) 0.4448(3) 0.0214(11) Uani 1 1 d . . . O20 O 0.1884(3) 0.53382(17) 0.6154(3) 0.0225(10) Uani 1 1 d . . . O21 O 0.0631(3) 0.45692(17) 0.2467(3) 0.0280(11) Uani 1 1 d . . . O22 O -0.0894(3) 0.44186(18) 0.2253(3) 0.0353(13) Uani 1 1 d . . . O23 O 0.1922(3) 0.40598(17) 0.4273(3) 0.0328(12) Uani 1 1 d . . . O24 O 0.2023(3) 0.33819(17) 0.5326(3) 0.0358(12) Uani 1 1 d . . . O25 O 0.3026(3) 0.21706(17) 0.3761(3) 0.0199(10) Uani 1 1 d . . . O26 O 0.3022(3) 0.24204(16) 0.5425(3) 0.0209(11) Uani 1 1 d . . . O27 O 0.2285(3) 0.13384(17) 0.2441(4) 0.0260(11) Uani 1 1 d . . . O28 O 0.2292(3) 0.05014(16) 0.2603(3) 0.0237(11) Uani 1 1 d . . . O29 O 0.6977(3) 0.15262(17) 0.4274(4) 0.0351(13) Uani 1 1 d . . . O30 O 0.7227(4) 0.08902(17) 0.5450(4) 0.0462(15) Uani 1 1 d . . . O31 O 0.6776(3) 0.25930(16) 0.4464(3) 0.0214(11) Uani 1 1 d . . . O32 O 0.6722(3) 0.28028(17) 0.6127(3) 0.0228(10) Uani 1 1 d . . . C1 C 0.4174(4) 0.4838(3) 0.3637(5) 0.0270(17) Uani 1 1 d . . . H1 H 0.4818 0.4942 0.3856 0.032 Uiso 1 1 calc R . . C2 C 0.0623(4) 0.2468(3) 0.1417(5) 0.0261(17) Uani 1 1 d . . . H2 H -0.0015 0.2578 0.1306 0.031 Uiso 1 1 calc R . . C3 C 0.9085(5) 0.2341(3) 0.3578(5) 0.0255(17) Uani 1 1 d . . . H3 H 0.9730 0.2444 0.3793 0.031 Uiso 1 1 calc R . . C4 C 0.5695(5) 0.4952(2) 0.1482(5) 0.0259(16) Uani 1 1 d . . . H4 H 0.5053 0.5057 0.1339 0.031 Uiso 1 1 calc R . . C5 C 0.2261(5) 0.3413(2) 0.2425(5) 0.0175(15) Uani 1 1 d . . . H5 H 0.1618 0.3391 0.2447 0.021 Uiso 1 1 calc R . . C6 C 0.4857(5) 0.1811(3) 0.2270(5) 0.033(2) Uani 1 1 d . . . H6 H 0.4989 0.1466 0.2110 0.039 Uiso 1 1 calc R . . C7 C 0.7516(4) 0.3398(2) 0.2543(4) 0.0193(17) Uani 1 1 d . . . H7 H 0.8121 0.3333 0.2423 0.023 Uiso 1 1 calc R . . C8 C 0.2680(5) 0.5891(2) 0.2575(5) 0.0206(16) Uani 1 1 d . . . H8 H 0.3291 0.5809 0.2494 0.025 Uiso 1 1 calc R . . C9 C 0.2252(4) 0.4896(2) 0.0477(5) 0.0135(14) Uani 1 1 d . . . H9 H 0.2841 0.5063 0.0771 0.016 Uiso 1 1 calc R . . C10 C 0.2163(4) 0.5094(2) 0.5465(5) 0.0209(16) Uani 1 1 d . . . H10 H 0.2667 0.4858 0.5727 0.025 Uiso 1 1 calc R . . C11 C -0.0043(4) 0.4308(3) 0.2523(5) 0.0240(18) Uani 1 1 d . . . H11 H 0.0105 0.3973 0.2813 0.029 Uiso 1 1 calc R . . C12 C 0.2370(5) 0.3751(3) 0.4951(5) 0.0256(16) Uani 1 1 d . . . H12 H 0.3035 0.3801 0.5206 0.031 Uiso 1 1 calc R . . C13 C 0.2659(4) 0.2404(2) 0.4403(5) 0.0183(15) Uani 1 1 d . . . H13 H 0.2078 0.2579 0.4113 0.022 Uiso 1 1 calc R . . C14 C 0.2656(5) 0.0918(3) 0.2489(5) 0.0230(17) Uani 1 1 d . . . H14 H 0.3292 0.0909 0.2433 0.028 Uiso 1 1 calc R . . C15 C 0.7480(5) 0.1267(3) 0.5024(5) 0.0270(15) Uani 1 1 d . . . H15 H 0.8122 0.1371 0.5294 0.032 Uiso 1 1 calc R . . C16 C 0.7077(4) 0.2571(2) 0.5474(5) 0.0198(15) Uani 1 1 d . . . H16 H 0.7617 0.2362 0.5767 0.024 Uiso 1 1 calc R . . N1 N 0.5481(4) 0.3418(2) 0.3730(5) 0.0326(15) Uani 1 1 d . . . H1A H 0.5935 0.3180 0.3658 0.039 Uiso 1 1 calc R . . N2 N 0.4357(4) 0.3420(2) 0.0661(5) 0.0329(15) Uani 1 1 d . . . H2A H 0.3979 0.3159 0.0277 0.039 Uiso 1 1 calc R . . C17 C 0.5050(4) 0.3646(3) 0.2585(5) 0.035(2) Uani 1 1 d . . . H17A H 0.4526 0.3882 0.2612 0.042 Uiso 1 1 calc R . . H17B H 0.5539 0.3845 0.2348 0.042 Uiso 1 1 calc R . . C18 C 0.4689(5) 0.3227(3) 0.1794(6) 0.044(2) Uani 1 1 d . . . H18A H 0.5199 0.2972 0.1832 0.053 Uiso 1 1 calc R . . H18B H 0.4159 0.3051 0.1997 0.053 Uiso 1 1 calc R . . C19 C 0.5978(5) 0.3823(3) 0.4452(5) 0.0375(19) Uani 1 1 d . . . H19A H 0.6422 0.3996 0.4108 0.056 Uiso 1 1 calc R . . H19B H 0.6328 0.3673 0.5148 0.056 Uiso 1 1 calc R . . H19C H 0.5517 0.4072 0.4582 0.056 Uiso 1 1 calc R . . C20 C 0.4800(5) 0.3143(3) 0.4199(6) 0.060(3) Uani 1 1 d . . . H20A H 0.4486 0.2874 0.3691 0.089 Uiso 1 1 calc R . . H20B H 0.4324 0.3384 0.4322 0.089 Uiso 1 1 calc R . . H20C H 0.5135 0.2986 0.4894 0.089 Uiso 1 1 calc R . . C21 C 0.5143(5) 0.3477(4) 0.0130(6) 0.072(3) Uani 1 1 d . . . H21A H 0.4893 0.3607 -0.0615 0.108 Uiso 1 1 calc R . . H21B H 0.5443 0.3143 0.0104 0.108 Uiso 1 1 calc R . . H21C H 0.5611 0.3719 0.0549 0.108 Uiso 1 1 calc R . . C22 C 0.3735(5) 0.3876(3) 0.0516(5) 0.0337(18) Uani 1 1 d . . . H22A H 0.3559 0.3977 -0.0255 0.051 Uiso 1 1 calc R . . H22B H 0.4072 0.4159 0.0961 0.051 Uiso 1 1 calc R . . H22C H 0.3162 0.3794 0.0747 0.051 Uiso 1 1 calc R . . N3 N 0.0693(4) 0.6006(2) 0.3988(4) 0.0271(14) Uani 1 1 d . . . H3A H 0.1065 0.5718 0.3974 0.032 Uiso 1 1 calc R . . N4 N -0.0520(4) 0.5840(2) 0.0985(4) 0.0277(14) Uani 1 1 d . . . H4A H -0.0952 0.5580 0.0704 0.033 Uiso 1 1 calc R . . C23 C 0.0283(4) 0.6180(3) 0.2817(5) 0.0271(17) Uani 1 1 d . . . H23A H -0.0152 0.6472 0.2799 0.032 Uiso 1 1 calc R . . H23B H 0.0799 0.6293 0.2497 0.032 Uiso 1 1 calc R . . C24 C -0.0238(4) 0.5747(3) 0.2175(5) 0.0310(18) Uani 1 1 d . . . H24A H 0.0166 0.5437 0.2322 0.037 Uiso 1 1 calc R . . H24B H -0.0813 0.5677 0.2425 0.037 Uiso 1 1 calc R . . C25 C 0.1316(5) 0.6414(3) 0.4602(5) 0.039(2) Uani 1 1 d . . . H25A H 0.1798 0.6504 0.4220 0.059 Uiso 1 1 calc R . . H25B H 0.1628 0.6290 0.5338 0.059 Uiso 1 1 calc R . . H25C H 0.0936 0.6718 0.4655 0.059 Uiso 1 1 calc R . . C26 C -0.0052(5) 0.5861(3) 0.4544(6) 0.050(2) Uani 1 1 d . . . H26A H -0.0452 0.5590 0.4125 0.075 Uiso 1 1 calc R . . H26B H -0.0442 0.6161 0.4590 0.075 Uiso 1 1 calc R . . H26C H 0.0249 0.5735 0.5281 0.075 Uiso 1 1 calc R . . C27 C 0.0268(5) 0.5760(3) 0.0463(6) 0.051(2) Uani 1 1 d . . . H27A H 0.0044 0.5829 -0.0322 0.076 Uiso 1 1 calc R . . H27B H 0.0491 0.5405 0.0577 0.076 Uiso 1 1 calc R . . H27C H 0.0789 0.5994 0.0790 0.076 Uiso 1 1 calc R . . C28 C -0.1043(5) 0.6318(3) 0.0644(5) 0.0335(18) Uani 1 1 d . . . H28A H -0.1190 0.6349 -0.0153 0.050 Uiso 1 1 calc R . . H28B H -0.0654 0.6610 0.0982 0.050 Uiso 1 1 calc R . . H28C H -0.1633 0.6314 0.0875 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01892(17) 0.00905(18) 0.01102(16) 0.00093(12) 0.00537(12) 0.00112(12) Er2 0.01821(16) 0.00982(17) 0.01321(16) -0.00150(13) 0.00556(12) -0.00114(13) Er3 0.01904(16) 0.00995(17) 0.01103(14) 0.00129(13) 0.00457(11) 0.00128(13) Er4 0.01744(16) 0.00943(18) 0.01145(17) -0.00147(12) 0.00484(12) -0.00171(12) O1 0.019(3) 0.094(5) 0.030(3) -0.002(3) 0.000(2) 0.006(3) O2 0.020(3) 0.035(3) 0.023(3) 0.005(2) 0.001(2) -0.004(2) O3 0.027(3) 0.040(3) 0.029(3) 0.003(2) 0.003(2) 0.004(2) O4 0.018(2) 0.030(3) 0.029(3) 0.003(2) 0.006(2) 0.007(2) O5 0.022(3) 0.090(5) 0.029(3) 0.001(3) 0.004(2) -0.001(3) O6 0.019(3) 0.040(3) 0.026(3) 0.003(2) 0.006(2) -0.005(2) O7 0.026(3) 0.063(4) 0.029(3) 0.004(3) 0.004(2) -0.002(3) O8 0.021(3) 0.035(3) 0.035(3) 0.011(2) 0.011(2) 0.011(2) O9 0.040(3) 0.008(3) 0.031(3) -0.005(2) 0.020(2) -0.003(2) O10 0.030(3) 0.014(3) 0.024(2) -0.006(2) 0.005(2) 0.000(2) O11 0.023(3) 0.054(4) 0.037(3) 0.014(3) 0.010(2) -0.001(2) O12 0.022(3) 0.044(3) 0.032(3) 0.001(3) 0.004(2) -0.006(3) O13 0.043(3) 0.011(3) 0.029(3) 0.001(2) 0.013(2) -0.002(2) O14 0.037(3) 0.010(3) 0.027(3) 0.004(2) 0.010(2) 0.000(2) O15 0.034(3) 0.013(3) 0.022(2) 0.006(2) 0.008(2) -0.002(2) O16 0.052(3) 0.005(3) 0.036(3) -0.002(2) 0.027(2) -0.007(2) O17 0.027(3) 0.024(3) 0.013(2) 0.000(2) 0.0064(19) -0.001(2) O18 0.024(3) 0.021(3) 0.014(2) 0.001(2) 0.0058(19) -0.006(2) O19 0.034(3) 0.020(3) 0.012(2) -0.0036(19) 0.008(2) 0.000(2) O20 0.029(3) 0.023(3) 0.014(2) -0.005(2) 0.004(2) 0.004(2) O21 0.014(2) 0.039(3) 0.030(3) 0.005(2) 0.005(2) -0.006(2) O22 0.022(3) 0.055(4) 0.032(3) 0.006(3) 0.013(2) 0.004(2) O23 0.050(3) 0.028(3) 0.026(3) 0.008(2) 0.019(2) 0.008(2) O24 0.053(3) 0.026(3) 0.031(3) 0.016(2) 0.016(2) 0.011(2) O25 0.024(2) 0.025(3) 0.011(2) -0.001(2) 0.0048(18) 0.008(2) O26 0.027(3) 0.021(3) 0.017(2) 0.000(2) 0.010(2) 0.008(2) O27 0.038(3) 0.006(3) 0.036(3) 0.001(2) 0.014(2) 0.002(2) O28 0.033(3) 0.009(3) 0.029(3) 0.004(2) 0.007(2) -0.004(2) O29 0.056(4) 0.027(3) 0.029(3) 0.011(2) 0.023(3) 0.010(2) O30 0.092(5) 0.022(3) 0.030(3) 0.012(2) 0.026(3) 0.018(3) O31 0.026(3) 0.023(3) 0.015(2) -0.001(2) 0.007(2) 0.007(2) O32 0.028(3) 0.029(3) 0.010(2) -0.001(2) 0.0029(18) 0.010(2) C1 0.013(4) 0.034(5) 0.031(4) 0.003(4) -0.001(3) 0.005(3) C2 0.017(4) 0.028(4) 0.031(4) -0.002(3) 0.003(3) 0.001(3) C3 0.018(4) 0.032(5) 0.025(4) -0.001(3) 0.002(3) 0.000(3) C4 0.019(4) 0.021(4) 0.036(4) 0.003(3) 0.003(3) -0.001(3) C5 0.016(3) 0.018(4) 0.020(4) -0.002(3) 0.008(3) -0.003(3) C6 0.029(5) 0.030(5) 0.040(5) -0.003(4) 0.011(4) -0.007(3) C7 0.029(4) 0.021(5) 0.010(4) -0.005(3) 0.008(3) 0.001(3) C8 0.025(4) 0.014(4) 0.025(4) 0.006(3) 0.008(3) -0.001(3) C9 0.011(3) 0.014(4) 0.015(3) 0.005(3) 0.002(3) 0.000(3) C10 0.027(4) 0.018(4) 0.018(4) 0.000(3) 0.005(3) 0.002(3) C11 0.016(4) 0.029(5) 0.029(4) 0.006(3) 0.008(3) 0.003(3) C12 0.036(4) 0.017(3) 0.024(4) 0.010(3) 0.007(3) 0.007(3) C13 0.026(4) 0.011(4) 0.020(4) 0.006(3) 0.012(3) 0.001(3) C14 0.027(4) 0.031(5) 0.014(4) 0.003(3) 0.011(3) -0.003(3) C15 0.045(4) 0.019(4) 0.023(4) 0.005(3) 0.020(3) 0.013(3) C16 0.024(4) 0.022(4) 0.013(3) 0.002(3) 0.005(3) 0.002(3) N1 0.020(3) 0.032(4) 0.046(4) 0.003(3) 0.009(3) 0.011(3) N2 0.024(3) 0.030(4) 0.045(4) -0.012(3) 0.008(3) -0.012(3) C17 0.037(5) 0.031(5) 0.041(5) -0.005(4) 0.018(4) 0.002(3) C18 0.025(4) 0.034(5) 0.070(6) -0.007(4) 0.010(4) 0.001(3) C19 0.046(5) 0.032(5) 0.033(4) 0.006(4) 0.008(4) 0.012(4) C20 0.031(5) 0.073(7) 0.071(6) 0.038(5) 0.006(4) -0.008(4) C21 0.028(5) 0.145(10) 0.049(6) -0.034(6) 0.021(4) -0.007(5) C22 0.028(4) 0.037(5) 0.036(4) 0.001(4) 0.008(3) 0.003(3) N3 0.027(3) 0.030(4) 0.025(3) 0.003(3) 0.008(3) 0.011(3) N4 0.017(3) 0.033(4) 0.029(3) -0.008(3) 0.000(3) -0.008(3) C23 0.030(4) 0.031(5) 0.023(4) 0.000(3) 0.012(3) 0.000(3) C24 0.026(4) 0.017(4) 0.049(5) -0.001(3) 0.008(3) 0.002(3) C25 0.049(5) 0.038(5) 0.025(4) -0.007(4) 0.002(4) 0.008(4) C26 0.034(5) 0.077(7) 0.041(5) 0.028(4) 0.013(4) 0.014(4) C27 0.030(5) 0.076(6) 0.050(5) -0.025(5) 0.018(4) 0.002(4) C28 0.035(4) 0.027(5) 0.032(4) 0.002(3) -0.003(3) 0.003(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 Er1 O21 2.304(4) . ? Er1 O9 2.317(4) . ? Er1 O23 2.331(4) . ? Er1 O15 2.333(4) . ? Er1 O17 2.356(4) . ? Er1 O19 2.366(4) . ? Er1 O1 2.380(4) . ? Er1 O2 2.409(4) . ? Er1 C1 2.753(6) . ? Er2 O11 2.234(5) . ? Er2 O10 2.304(4) . ? Er2 O24 2.311(4) 4_565 ? Er2 O27 2.325(4) . ? Er2 O26 2.375(4) 4_565 ? Er2 O4 2.385(4) . ? Er2 O25 2.387(4) . ? Er2 O3 2.454(4) . ? Er2 C2 2.760(6) . ? Er3 O16 2.317(4) 2_645 ? Er3 O29 2.318(4) . ? Er3 O13 2.327(4) . ? Er3 O12 2.327(4) . ? Er3 O32 2.346(4) 4_565 ? Er3 O5 2.355(4) . ? Er3 O31 2.355(4) . ? Er3 O6 2.419(4) . ? Er3 C3 2.733(6) . ? Er4 O22 2.269(4) 1_655 ? Er4 O30 2.288(4) 4_565 ? Er4 O28 2.289(4) 2_655 ? Er4 O14 2.328(4) . ? Er4 O20 2.366(4) 3_666 ? Er4 O18 2.381(4) 3_665 ? Er4 O8 2.402(4) . ? Er4 O7 2.421(5) . ? Er4 C4 2.752(7) . ? O1 C1 1.252(7) . ? O2 C1 1.234(7) . ? O3 C2 1.249(7) . ? O4 C2 1.241(7) . ? O5 C3 1.235(7) . ? O6 C3 1.225(7) . ? O7 C4 1.232(7) . ? O8 C4 1.257(7) . ? O9 C5 1.252(7) . ? O10 C5 1.233(7) . ? O11 C6 1.247(7) . ? O12 C6 1.214(7) . ? O13 C7 1.253(6) . ? O14 C7 1.232(6) . ? O15 C8 1.238(7) . ? O16 C8 1.238(7) . ? O16 Er3 2.317(4) 2_655 ? O17 C9 1.242(6) . ? O18 C9 1.248(6) . ? O18 Er4 2.381(4) 3_665 ? O19 C10 1.256(6) . ? O20 C10 1.233(6) . ? O20 Er4 2.366(4) 3_666 ? O21 C11 1.214(7) . ? O22 C11 1.236(6) . ? O22 Er4 2.269(4) 1_455 ? O23 C12 1.233(7) . ? O24 C12 1.239(7) . ? O24 Er2 2.311(4) 4_566 ? O25 C13 1.244(6) . ? O26 C13 1.267(6) . ? O26 Er2 2.375(4) 4_566 ? O27 C14 1.218(7) . ? O28 C14 1.233(7) . ? O28 Er4 2.289(4) 2_645 ? O29 C15 1.241(7) . ? O30 C15 1.224(8) . ? O30 Er4 2.288(4) 4_566 ? O31 C16 1.243(6) . ? O32 C16 1.243(6) . ? O32 Er3 2.346(4) 4_566 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N1 C19 1.462(8) . ? N1 C20 1.471(8) . ? N1 C17 1.544(8) . ? N1 H1A 0.9300 . ? N2 C22 1.478(8) . ? N2 C18 1.480(8) . ? N2 C21 1.482(8) . ? N2 H2A 0.9300 . ? C17 C18 1.485(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N3 C25 1.483(8) . ? N3 C26 1.491(8) . ? N3 C23 1.518(7) . ? N3 H3A 0.9300 . ? N4 C28 1.467(7) . ? N4 C24 1.476(7) . ? N4 C27 1.485(7) . ? N4 H4A 0.9300 . ? C23 C24 1.480(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 O21 Er1 O9 97.30(16) . . ? O21 Er1 O23 76.99(15) . . ? O9 Er1 O23 72.45(14) . . ? O21 Er1 O15 91.35(15) . . ? O9 Er1 O15 146.52(14) . . ? O23 Er1 O15 140.99(15) . . ? O21 Er1 O17 73.97(14) . . ? O9 Er1 O17 74.73(15) . . ? O23 Er1 O17 132.34(15) . . ? O15 Er1 O17 76.77(14) . . ? O21 Er1 O19 81.25(14) . . ? O9 Er1 O19 144.90(14) . . ? O23 Er1 O19 73.10(14) . . ? O15 Er1 O19 68.35(14) . . ? O17 Er1 O19 136.32(14) . . ? O21 Er1 O1 156.21(16) . . ? O9 Er1 O1 90.19(17) . . ? O23 Er1 O1 83.90(17) . . ? O15 Er1 O1 94.76(17) . . ? O17 Er1 O1 129.81(15) . . ? O19 Er1 O1 79.72(16) . . ? O21 Er1 O2 150.14(15) . . ? O9 Er1 O2 79.28(15) . . ? O23 Er1 O2 128.34(15) . . ? O15 Er1 O2 77.31(15) . . ? O17 Er1 O2 76.54(14) . . ? O19 Er1 O2 118.39(15) . . ? O1 Er1 O2 53.49(15) . . ? O21 Er1 C1 174.78(18) . . ? O9 Er1 C1 86.00(18) . . ? O23 Er1 C1 107.94(18) . . ? O15 Er1 C1 83.70(18) . . ? O17 Er1 C1 103.16(17) . . ? O19 Er1 C1 98.39(17) . . ? O1 Er1 C1 27.01(16) . . ? O2 Er1 C1 26.61(15) . . ? O11 Er2 O10 100.24(16) . . ? O11 Er2 O24 92.49(17) . 4_565 ? O10 Er2 O24 142.76(15) . 4_565 ? O11 Er2 O27 84.16(16) . . ? O10 Er2 O27 144.13(14) . . ? O24 Er2 O27 71.51(15) 4_565 . ? O11 Er2 O26 75.66(15) . 4_565 ? O10 Er2 O26 73.56(14) . 4_565 ? O24 Er2 O26 76.04(14) 4_565 4_565 ? O27 Er2 O26 140.72(15) . 4_565 ? O11 Er2 O4 154.31(15) . . ? O10 Er2 O4 83.44(15) . . ? O24 Er2 O4 99.82(16) 4_565 . ? O27 Er2 O4 78.60(15) . . ? O26 Er2 O4 129.12(14) 4_565 . ? O11 Er2 O25 77.16(14) . . ? O10 Er2 O25 74.02(15) . . ? O24 Er2 O25 143.20(15) 4_565 . ? O27 Er2 O25 72.35(15) . . ? O26 Er2 O25 132.60(14) 4_565 . ? O4 Er2 O25 79.53(13) . . ? O11 Er2 O3 152.11(15) . . ? O10 Er2 O3 77.03(15) . . ? O24 Er2 O3 75.60(16) 4_565 . ? O27 Er2 O3 114.55(16) . . ? O26 Er2 O3 77.00(14) 4_565 . ? O4 Er2 O3 53.57(14) . . ? O25 Er2 O3 126.92(14) . . ? O11 Er2 C2 178.69(18) . . ? O10 Er2 C2 78.77(17) . . ? O24 Er2 C2 87.83(18) 4_565 . ? O27 Er2 C2 97.15(18) . . ? O26 Er2 C2 103.20(17) 4_565 . ? O4 Er2 C2 26.66(15) . . ? O25 Er2 C2 103.32(16) . . ? O3 Er2 C2 26.91(14) . . ? O16 Er3 O29 71.97(14) 2_645 . ? O16 Er3 O13 146.05(14) 2_645 . ? O29 Er3 O13 141.92(15) . . ? O16 Er3 O12 99.63(17) 2_645 . ? O29 Er3 O12 79.27(16) . . ? O13 Er3 O12 88.51(16) . . ? O16 Er3 O32 74.28(16) 2_645 4_565 ? O29 Er3 O32 133.31(16) . 4_565 ? O13 Er3 O32 76.02(15) . 4_565 ? O12 Er3 O32 75.60(14) . 4_565 ? O16 Er3 O5 92.12(17) 2_645 . ? O29 Er3 O5 81.80(17) . . ? O13 Er3 O5 95.02(17) . . ? O12 Er3 O5 153.33(16) . . ? O32 Er3 O5 130.90(15) 4_565 . ? O16 Er3 O31 145.88(14) 2_645 . ? O29 Er3 O31 74.01(15) . . ? O13 Er3 O31 68.07(14) . . ? O12 Er3 O31 76.45(15) . . ? O32 Er3 O31 134.50(14) 4_565 . ? O5 Er3 O31 80.40(15) . . ? O16 Er3 O6 80.21(15) 2_645 . ? O29 Er3 O6 125.79(15) . . ? O13 Er3 O6 77.73(15) . . ? O12 Er3 O6 152.25(15) . . ? O32 Er3 O6 77.73(14) 4_565 . ? O5 Er3 O6 53.32(15) . . ? O31 Er3 O6 118.82(15) . . ? O16 Er3 C3 87.33(18) 2_645 . ? O29 Er3 C3 105.31(18) . . ? O13 Er3 C3 84.39(18) . . ? O12 Er3 C3 172.66(18) . . ? O32 Er3 C3 104.35(17) 4_565 . ? O5 Er3 C3 26.80(15) . . ? O31 Er3 C3 99.09(17) . . ? O6 Er3 C3 26.62(15) . . ? O22 Er4 O30 88.75(18) 1_655 4_565 ? O22 Er4 O28 100.99(16) 1_655 2_655 ? O30 Er4 O28 143.01(15) 4_565 2_655 ? O22 Er4 O14 87.96(16) 1_655 . ? O30 Er4 O14 72.50(15) 4_565 . ? O28 Er4 O14 142.60(15) 2_655 . ? O22 Er4 O20 75.69(15) 1_655 3_666 ? O30 Er4 O20 142.19(16) 4_565 3_666 ? O28 Er4 O20 74.54(15) 2_655 3_666 ? O14 Er4 O20 72.70(15) . 3_666 ? O22 Er4 O18 76.80(14) 1_655 3_665 ? O30 Er4 O18 74.78(15) 4_565 3_665 ? O28 Er4 O18 72.99(14) 2_655 3_665 ? O14 Er4 O18 144.05(14) . 3_665 ? O20 Er4 O18 131.90(14) 3_666 3_665 ? O22 Er4 O8 153.92(15) 1_655 . ? O30 Er4 O8 105.32(18) 4_565 . ? O28 Er4 O8 81.08(16) 2_655 . ? O14 Er4 O8 75.94(15) . . ? O20 Er4 O8 79.94(14) 3_666 . ? O18 Er4 O8 127.68(14) 3_665 . ? O22 Er4 O7 152.34(15) 1_655 . ? O30 Er4 O7 76.82(18) 4_565 . ? O28 Er4 O7 78.55(16) 2_655 . ? O14 Er4 O7 109.38(16) . . ? O20 Er4 O7 129.27(15) 3_666 . ? O18 Er4 O7 76.69(15) 3_665 . ? O8 Er4 O7 53.74(15) . . ? O22 Er4 C4 178.79(18) 1_655 . ? O30 Er4 C4 91.1(2) 4_565 . ? O28 Er4 C4 78.40(17) 2_655 . ? O14 Er4 C4 93.16(18) . . ? O20 Er4 C4 105.10(17) 3_666 . ? O18 Er4 C4 102.01(17) 3_665 . ? O8 Er4 C4 27.16(15) . . ? O7 Er4 C4 26.58(15) . . ? C1 O1 Er1 93.3(4) . . ? C1 O2 Er1 92.4(4) . . ? C2 O3 Er2 90.3(4) . . ? C2 O4 Er2 93.8(4) . . ? C3 O5 Er3 94.0(4) . . ? C3 O6 Er3 91.2(4) . . ? C4 O7 Er4 91.9(4) . . ? C4 O8 Er4 92.1(4) . . ? C5 O9 Er1 135.7(4) . . ? C5 O10 Er2 145.9(4) . . ? C6 O11 Er2 177.5(5) . . ? C6 O12 Er3 145.5(5) . . ? C7 O13 Er3 140.3(4) . . ? C7 O14 Er4 140.4(4) . . ? C8 O15 Er1 139.1(5) . . ? C8 O16 Er3 141.4(4) . 2_655 ? C9 O17 Er1 132.1(4) . . ? C9 O18 Er4 130.8(4) . 3_665 ? C10 O19 Er1 129.3(4) . . ? C10 O20 Er4 130.5(4) . 3_666 ? C11 O21 Er1 144.9(5) . . ? C11 O22 Er4 174.6(4) . 1_455 ? C12 O23 Er1 137.1(5) . . ? C12 O24 Er2 136.4(5) . 4_566 ? C13 O25 Er2 126.9(4) . . ? C13 O26 Er2 130.1(4) . 4_566 ? C14 O27 Er2 138.6(5) . . ? C14 O28 Er4 150.2(5) . 2_645 ? C15 O29 Er3 137.8(5) . . ? C15 O30 Er4 146.1(5) . 4_566 ? C16 O31 Er3 132.4(4) . . ? C16 O32 Er3 131.3(4) . 4_566 ? O2 C1 O1 120.1(6) . . ? O2 C1 Er1 60.9(3) . . ? O1 C1 Er1 59.6(3) . . ? O2 C1 H1 119.9 . . ? O1 C1 H1 119.9 . . ? Er1 C1 H1 173.2 . . ? O4 C2 O3 122.3(6) . . ? O4 C2 Er2 59.5(3) . . ? O3 C2 Er2 62.8(3) . . ? O4 C2 H2 118.8 . . ? O3 C2 H2 118.8 . . ? Er2 C2 H2 178.0 . . ? O6 C3 O5 121.1(6) . . ? O6 C3 Er3 62.2(3) . . ? O5 C3 Er3 59.2(3) . . ? O6 C3 H3 119.4 . . ? O5 C3 H3 119.4 . . ? Er3 C3 H3 173.9 . . ? O7 C4 O8 122.2(6) . . ? O7 C4 Er4 61.5(4) . . ? O8 C4 Er4 60.7(3) . . ? O7 C4 H4 118.9 . . ? O8 C4 H4 118.9 . . ? Er4 C4 H4 179.3 . . ? O10 C5 O9 124.7(6) . . ? O10 C5 H5 117.7 . . ? O9 C5 H5 117.7 . . ? O12 C6 O11 127.5(8) . . ? O12 C6 H6 116.2 . . ? O11 C6 H6 116.2 . . ? O14 C7 O13 124.0(6) . . ? O14 C7 H7 118.0 . . ? O13 C7 H7 118.0 . . ? O16 C8 O15 124.9(7) . . ? O16 C8 H8 117.6 . . ? O15 C8 H8 117.6 . . ? O17 C9 O18 124.5(5) . . ? O17 C9 H9 117.8 . . ? O18 C9 H9 117.8 . . ? O20 C10 O19 125.9(6) . . ? O20 C10 H10 117.1 . . ? O19 C10 H10 117.1 . . ? O21 C11 O22 128.7(7) . . ? O21 C11 H11 115.6 . . ? O22 C11 H11 115.6 . . ? O23 C12 O24 125.3(7) . . ? O23 C12 H12 117.4 . . ? O24 C12 H12 117.4 . . ? O25 C13 O26 123.3(6) . . ? O25 C13 H13 118.4 . . ? O26 C13 H13 118.4 . . ? O27 C14 O28 126.7(7) . . ? O27 C14 H14 116.7 . . ? O28 C14 H14 116.7 . . ? O30 C15 O29 126.0(8) . . ? O30 C15 H15 117.0 . . ? O29 C15 H15 117.0 . . ? O31 C16 O32 124.5(6) . . ? O31 C16 H16 117.8 . . ? O32 C16 H16 117.8 . . ? C19 N1 C20 112.2(6) . . ? C19 N1 C17 108.9(5) . . ? C20 N1 C17 114.5(5) . . ? C19 N1 H1A 106.9 . . ? C20 N1 H1A 106.9 . . ? C17 N1 H1A 106.9 . . ? C22 N2 C18 115.5(5) . . ? C22 N2 C21 112.8(6) . . ? C18 N2 C21 112.2(6) . . ? C22 N2 H2A 105.1 . . ? C18 N2 H2A 105.1 . . ? C21 N2 H2A 105.1 . . ? C18 C17 N1 109.8(7) . . ? C18 C17 H17A 109.7 . . ? N1 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? N1 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N2 C18 C17 112.0(6) . . ? N2 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N2 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 N3 C26 111.0(5) . . ? C25 N3 C23 109.5(5) . . ? C26 N3 C23 112.7(5) . . ? C25 N3 H3A 107.8 . . ? C26 N3 H3A 107.8 . . ? C23 N3 H3A 107.8 . . ? C28 N4 C24 115.2(5) . . ? C28 N4 C27 113.1(6) . . ? C24 N4 C27 112.9(5) . . ? C28 N4 H4A 104.8 . . ? C24 N4 H4A 104.8 . . ? C27 N4 H4A 104.8 . . ? C24 C23 N3 109.1(6) . . ? C24 C23 H23A 109.9 . . ? N3 C23 H23A 109.9 . . ? C24 C23 H23B 109.9 . . ? N3 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N4 C24 C23 113.9(5) . . ? N4 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? N4 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O31 0.93 2.06 2.855(7) 142.7 . N1 H1A O13 0.93 2.29 3.082(7) 142.2 . N2 H2A O26 0.93 2.10 2.897(7) 142.9 4_565 N2 H2A O25 0.93 2.23 3.086(7) 152.3 4_565 N3 H3A O19 0.93 1.91 2.809(7) 160.9 . N3 H3A O15 0.93 2.63 3.283(7) 128.0 . N4 H4A O18 0.93 1.87 2.773(6) 162.8 3_565 N4 H4A O17 0.93 2.45 3.184(6) 135.5 3_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.231 _refine_diff_density_min -2.224 _refine_diff_density_rms 0.199 #### End of 2 at 160 K #### # Attachment '- DT-ART-12-2011-010241.cif' data_CCDC789449-1-at-290K _database_code_depnum_ccdc_archive 'CCDC 812094' #TrackingRef '- DT-ART-12-2011-010241.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Er2 N2 O16' _chemical_formula_weight 784.84 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 orthorhombic _symmetry_space_group_name_H-M 'P na2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.1266(3) _cell_length_b 13.3611(2) _cell_length_c 8.5791(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2077.78(7) _cell_formula_units_Z 4 _cell_measurement_temperature 290 _cell_measurement_reflns_used 18193 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description column _exptl_crystal_colour pink _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 8.107 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.150 0 -1 0 0.190 1 0 2 0.080 -1 0 -2 0.090 -1 0 2 0.090 1 0 -2 0.090 1 -4 3 0.120 0 6 1 0.140 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.156 _exptl_absorpt_correction_T_max 0.330 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 290 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31663 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4695 _reflns_number_gt 3654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction (Numerical): P. Coppens, in Crystallographic Computing, edited by F. R. Ahmed, S. R. Hall, C. P. Huber, pp255-270, 1970, Copenhagen: Munksgaard. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.9762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 115(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 4695 _refine_ls_number_parameters 285 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 Er1 Er 0.600931(16) 0.37468(3) 0.25300(4) 0.02653(15) Uani 1 1 d . . . Er2 Er 0.393684(16) 0.12462(3) 0.75275(4) 0.02633(15) Uani 1 1 d . . . O1 O 0.5631(4) 0.2992(5) 0.4794(11) 0.0488(18) Uani 1 1 d . . . O2 O 0.4947(4) 0.2101(4) 0.6442(9) 0.0377(17) Uani 1 1 d . . . O3 O 0.6484(4) 0.2045(4) 0.2479(10) 0.0378(15) Uani 1 1 d . . . O4 O 0.6481(4) 0.0405(4) 0.2919(9) 0.0393(18) Uani 1 1 d . . . O5 O 0.7001(7) 0.3858(5) 0.4208(11) 0.040(2) Uani 1 1 d . . . O6 O 0.7921(9) 0.3826(5) 0.5697(19) 0.069(4) Uani 1 1 d . . . O7 O 0.7037(9) 0.3652(5) 0.0859(16) 0.055(3) Uani 1 1 d . . . O8 O 0.7941(7) 0.3695(4) -0.0779(11) 0.040(2) Uani 1 1 d . . . O9 O 0.6478(4) 0.5405(4) 0.2484(14) 0.059(2) Uani 1 1 d . . . O10 O 0.6480(4) 0.7058(4) 0.2090(12) 0.053(3) Uani 1 1 d . . . O11 O 0.5030(4) 0.4701(4) 0.3304(9) 0.0392(16) Uani 1 1 d . . . O12 O 0.4357(4) 0.5491(5) 0.5072(11) 0.0426(16) Uani 1 1 d . . . O13 O 0.5045(5) 0.2805(5) 0.1440(10) 0.0427(18) Uani 1 1 d . . . O14 O 0.4270(4) 0.2098(5) -0.0260(11) 0.0500(18) Uani 1 1 d . . . O15 O 0.4971(4) 0.0375(4) 0.8435(9) 0.0376(16) Uani 1 1 d . . . O16 O 0.5706(4) -0.0334(4) 1.0170(10) 0.0390(16) Uani 1 1 d . . . C1 C 0.5086(8) 0.2484(12) 0.5228(19) 0.048(3) Uani 1 1 d . . . H1 H 0.4728 0.2391 0.4465 0.057 Uiso 1 1 calc R . . C2 C 0.6172(6) 0.1294(7) 0.265(2) 0.050(3) Uani 1 1 d . . . H2 H 0.5660 0.1314 0.2583 0.060 Uiso 1 1 calc R . . C3 C 0.7356(8) 0.3561(9) 0.5266(16) 0.063(3) Uiso 1 1 d . . . H3 H 0.7147 0.3038 0.5829 0.076 Uiso 1 1 calc R . . C4 C 0.7324(6) 0.3947(6) -0.0330(11) 0.037(2) Uani 1 1 d . . . H4 H 0.7060 0.4394 -0.0946 0.045 Uiso 1 1 calc R . . C5 C 0.6171(6) 0.6300(7) 0.2127(13) 0.040(3) Uani 1 1 d . . . H5 H 0.5670 0.6306 0.1892 0.048 Uiso 1 1 calc R . . C6 C 0.4903(8) 0.5081(9) 0.4692(13) 0.041(3) Uani 1 1 d . . . H6 H 0.5274 0.5022 0.5434 0.049 Uiso 1 1 calc R . . C7 C 0.4894(7) 0.2463(11) 0.0213(18) 0.044(3) Uani 1 1 d . . . H7 H 0.5275 0.2455 -0.0514 0.053 Uiso 1 1 calc R . . C8 C 0.5127(7) -0.0001(9) 0.9776(13) 0.035(3) Uani 1 1 d . . . H8 H 0.4750 -0.0012 1.0510 0.042 Uiso 1 1 calc R . . C9 C 0.8354(6) 0.5718(9) 0.1901(13) 0.063(3) Uani 1 1 d . . . H9A H 0.8001 0.5998 0.1189 0.095 Uiso 1 1 calc R . . H9B H 0.8556 0.5115 0.1467 0.095 Uiso 1 1 calc R . . H9C H 0.8744 0.6191 0.2074 0.095 Uiso 1 1 calc R . . C10 C 0.7763(6) 0.6400(7) 0.4281(13) 0.049(2) Uani 1 1 d . . . H10A H 0.7522 0.6867 0.3580 0.059 Uiso 1 1 calc R . . H10B H 0.8196 0.6724 0.4712 0.059 Uiso 1 1 calc R . . C11 C 0.7225(6) 0.6103(7) 0.5619(14) 0.051(2) Uani 1 1 d . . . H11A H 0.6794 0.5772 0.5189 0.062 Uiso 1 1 calc R . . H11B H 0.7467 0.5642 0.6327 0.062 Uiso 1 1 calc R . . C12 C 0.6638(7) 0.6803(10) 0.7965(13) 0.071(3) Uani 1 1 d . . . H12A H 0.6193 0.6430 0.7788 0.107 Uiso 1 1 calc R . . H12B H 0.6521 0.7423 0.8471 0.107 Uiso 1 1 calc R . . H12C H 0.6965 0.6420 0.8614 0.107 Uiso 1 1 calc R . . N1 N 0.7984(5) 0.5486(6) 0.3414(11) 0.054(2) Uani 1 1 d . . . H1A H 0.7581 0.5112 0.3228 0.065 Uiso 1 1 calc R . . H1B H 0.8292 0.5123 0.4010 0.065 Uiso 1 1 calc R . . N2 N 0.6999(5) 0.7008(6) 0.6466(11) 0.052(2) Uani 1 1 d . . . H2A H 0.7401 0.7390 0.6638 0.063 Uiso 1 1 calc R . . H2B H 0.6688 0.7362 0.5862 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0289(2) 0.0255(2) 0.0252(2) 0.00058(12) 0.0010(3) 0.00033(15) Er2 0.0289(2) 0.0248(2) 0.0253(2) -0.00030(12) 0.0075(3) -0.00058(15) O1 0.057(5) 0.050(4) 0.039(4) 0.004(3) 0.006(4) -0.011(3) O2 0.046(4) 0.038(4) 0.030(3) 0.006(3) 0.001(3) -0.004(3) O3 0.038(3) 0.019(3) 0.056(4) 0.001(3) -0.003(4) -0.004(2) O4 0.040(4) 0.031(3) 0.048(5) 0.004(3) -0.002(3) -0.001(3) O5 0.038(5) 0.058(5) 0.024(4) 0.002(3) -0.011(3) -0.005(3) O6 0.042(6) 0.039(5) 0.126(12) -0.029(4) 0.026(7) -0.020(3) O7 0.055(6) 0.038(4) 0.073(8) 0.015(4) -0.005(5) 0.010(4) O8 0.040(5) 0.055(5) 0.026(4) 0.011(3) 0.023(4) 0.013(3) O9 0.039(4) 0.033(3) 0.103(7) 0.000(4) -0.011(6) -0.004(3) O10 0.043(4) 0.014(3) 0.101(7) -0.007(3) 0.005(4) -0.005(3) O11 0.038(4) 0.040(4) 0.040(4) -0.002(3) 0.007(3) 0.008(3) O12 0.039(4) 0.053(4) 0.036(4) -0.020(3) 0.002(3) 0.009(3) O13 0.052(5) 0.042(4) 0.034(4) -0.009(3) -0.005(3) -0.009(3) O14 0.039(4) 0.066(4) 0.045(5) -0.011(3) -0.001(3) -0.010(3) O15 0.037(4) 0.036(4) 0.040(4) 0.000(3) -0.009(3) 0.000(3) O16 0.038(4) 0.048(3) 0.031(4) 0.013(3) -0.004(3) 0.010(3) C1 0.030(6) 0.055(6) 0.057(7) 0.014(6) 0.012(5) -0.003(5) C2 0.033(4) 0.040(5) 0.078(10) -0.016(5) 0.014(6) -0.001(5) C4 0.056(5) 0.026(4) 0.029(5) 0.004(3) 0.005(4) 0.004(4) C5 0.027(3) 0.043(6) 0.050(9) 0.010(4) -0.008(4) -0.001(4) C6 0.058(9) 0.036(5) 0.028(6) 0.000(5) -0.011(5) -0.015(5) C7 0.032(6) 0.051(6) 0.049(6) -0.011(6) -0.008(5) -0.011(4) C8 0.043(9) 0.035(5) 0.027(5) -0.007(5) 0.005(4) -0.012(4) C9 0.055(6) 0.085(8) 0.050(6) 0.000(6) 0.013(5) -0.014(5) C10 0.045(5) 0.052(5) 0.049(6) 0.002(4) -0.006(4) -0.013(4) C11 0.049(6) 0.050(5) 0.055(6) -0.009(4) 0.001(5) 0.004(4) C12 0.053(6) 0.117(10) 0.043(6) 0.005(6) 0.002(4) -0.015(6) N1 0.051(5) 0.059(5) 0.052(5) 0.007(4) -0.002(4) -0.011(4) N2 0.048(5) 0.060(5) 0.050(5) 0.013(4) -0.003(4) -0.004(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 Er1 O11 2.283(7) . ? Er1 O1 2.294(9) . ? Er1 O5 2.308(10) . ? Er1 O13 2.348(7) . ? Er1 O7 2.354(17) . ? Er1 O9 2.373(6) . ? Er1 O3 2.431(5) . ? Er1 O12 2.434(8) 2_664 ? Er2 O14 2.294(9) 1_556 ? Er2 O8 2.318(9) 3_456 ? Er2 O15 2.340(7) . ? Er2 O2 2.351(7) . ? Er2 O4 2.356(6) 2_655 ? Er2 O10 2.418(6) 2_665 ? Er2 O6 2.422(17) 3_455 ? Er2 O16 2.449(8) 2_654 ? O1 C1 1.256(16) . ? O2 C1 1.187(16) . ? O3 C2 1.160(11) . ? O4 C2 1.335(11) . ? O4 Er2 2.356(6) 2_654 ? O5 C3 1.181(16) . ? O6 C3 1.15(2) . ? O6 Er2 2.422(17) 3 ? O7 C4 1.211(18) . ? O8 C4 1.230(16) . ? O8 Er2 2.318(9) 3_554 ? O9 C5 1.355(10) . ? O10 C5 1.159(10) . ? O10 Er2 2.418(6) 2_664 ? O11 C6 1.316(13) . ? O12 C6 1.177(16) . ? O12 Er1 2.434(8) 2_665 ? O13 C7 1.179(15) . ? O14 C7 1.297(14) . ? O14 Er2 2.294(9) 1_554 ? O15 C8 1.286(13) . ? O16 C8 1.188(15) . ? O16 Er2 2.449(8) 2_655 ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 N1 1.494(12) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N1 1.485(12) . ? C10 C11 1.558(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.469(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.469(13) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? 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 O11 Er1 O1 76.5(3) . . ? O11 Er1 O5 112.8(3) . . ? O1 Er1 O5 74.5(3) . . ? O11 Er1 O13 80.58(18) . . ? O1 Er1 O13 83.0(3) . . ? O5 Er1 O13 149.6(3) . . ? O11 Er1 O7 145.3(3) . . ? O1 Er1 O7 136.8(3) . . ? O5 Er1 O7 76.5(3) . . ? O13 Er1 O7 108.5(4) . . ? O11 Er1 O9 76.2(3) . . ? O1 Er1 O9 122.1(4) . . ? O5 Er1 O9 70.8(3) . . ? O13 Er1 O9 139.5(3) . . ? O7 Er1 O9 75.9(3) . . ? O11 Er1 O3 143.3(2) . . ? O1 Er1 O3 73.1(3) . . ? O5 Er1 O3 78.2(2) . . ? O13 Er1 O3 75.8(2) . . ? O7 Er1 O3 70.1(3) . . ? O9 Er1 O3 138.3(2) . . ? O11 Er1 O12 78.8(3) . 2_664 ? O1 Er1 O12 146.75(19) . 2_664 ? O5 Er1 O12 136.5(3) . 2_664 ? O13 Er1 O12 71.1(3) . 2_664 ? O7 Er1 O12 73.2(4) . 2_664 ? O9 Er1 O12 72.1(3) . 2_664 ? O3 Er1 O12 118.2(3) . 2_664 ? O14 Er2 O8 70.7(3) 1_556 3_456 ? O14 Er2 O15 76.2(3) 1_556 . ? O8 Er2 O15 115.6(4) 3_456 . ? O14 Er2 O2 83.2(3) 1_556 . ? O8 Er2 O2 147.0(2) 3_456 . ? O15 Er2 O2 75.48(16) . . ? O14 Er2 O4 115.5(3) 1_556 2_655 ? O8 Er2 O4 72.1(2) 3_456 2_655 ? O15 Er2 O4 75.2(2) . 2_655 ? O2 Er2 O4 139.6(2) . 2_655 ? O14 Er2 O10 75.3(3) 1_556 2_665 ? O8 Er2 O10 79.7(3) 3_456 2_665 ? O15 Er2 O10 140.2(2) . 2_665 ? O2 Er2 O10 74.2(3) . 2_665 ? O4 Er2 O10 143.0(2) 2_655 2_665 ? O14 Er2 O6 139.2(3) 1_556 3_455 ? O8 Er2 O6 79.4(3) 3_456 3_455 ? O15 Er2 O6 143.6(3) . 3_455 ? O2 Er2 O6 110.8(4) . 3_455 ? O4 Er2 O6 79.1(3) 2_655 3_455 ? O10 Er2 O6 72.5(2) 2_665 3_455 ? O14 Er2 O16 149.39(18) 1_556 2_654 ? O8 Er2 O16 137.8(3) 3_456 2_654 ? O15 Er2 O16 79.4(2) . 2_654 ? O2 Er2 O16 73.0(2) . 2_654 ? O4 Er2 O16 74.7(2) 2_655 2_654 ? O10 Er2 O16 114.9(3) 2_665 2_654 ? O6 Er2 O16 69.2(3) 3_455 2_654 ? C1 O1 Er1 136.4(9) . . ? C1 O2 Er2 136.2(9) . . ? C2 O3 Er1 129.4(7) . . ? C2 O4 Er2 132.4(7) . 2_654 ? C3 O5 Er1 151.8(10) . . ? C3 O6 Er2 151.2(12) . 3 ? C4 O7 Er1 146.7(10) . . ? C4 O8 Er2 153.5(7) . 3_554 ? C5 O9 Er1 132.9(6) . . ? C5 O10 Er2 131.6(7) . 2_664 ? C6 O11 Er1 128.0(7) . . ? C6 O12 Er1 131.6(8) . 2_665 ? C7 O13 Er1 137.3(9) . . ? C7 O14 Er2 132.5(8) . 1_554 ? C8 O15 Er2 131.9(7) . . ? C8 O16 Er2 130.9(7) . 2_655 ? O2 C1 O1 131.2(15) . . ? O2 C1 H1 114.4 . . ? O1 C1 H1 114.4 . . ? O3 C2 O4 126.0(10) . . ? O3 C2 H2 117.0 . . ? O4 C2 H2 117.0 . . ? O6 C3 O5 129.1(15) . . ? O6 C3 H3 115.5 . . ? O5 C3 H3 115.5 . . ? O7 C4 O8 124.4(12) . . ? O7 C4 H4 117.8 . . ? O8 C4 H4 117.8 . . ? O10 C5 O9 125.4(9) . . ? O10 C5 H5 117.3 . . ? O9 C5 H5 117.3 . . ? O12 C6 O11 125.3(11) . . ? O12 C6 H6 117.3 . . ? O11 C6 H6 117.3 . . ? O13 C7 O14 128.8(13) . . ? O13 C7 H7 115.6 . . ? O14 C7 H7 115.6 . . ? O16 C8 O15 126.5(10) . . ? O16 C8 H8 116.7 . . ? O15 C8 H8 116.7 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 109.2(7) . . ? N1 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? N1 C10 H10B 109.8 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N2 C11 C10 109.2(7) . . ? N2 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? N2 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 N1 C9 112.7(8) . . ? C10 N1 H1A 109.1 . . ? C9 N1 H1A 109.1 . . ? C10 N1 H1B 109.1 . . ? C9 N1 H1B 109.1 . . ? H1A N1 H1B 107.8 . . ? C12 N2 C11 113.7(8) . . ? C12 N2 H2A 108.8 . . ? C11 N2 H2A 108.8 . . ? C12 N2 H2B 108.8 . . ? C11 N2 H2B 108.8 . . ? H2A N2 H2B 107.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O5 0.90 2.15 2.893(13) 139.5 . N1 H1A O9 0.90 2.13 2.846(11) 135.4 . N1 H1B O6 0.90 2.36 2.961(15) 124.6 . N1 H1B O16 0.90 2.16 3.019(11) 159.6 4_654 N2 H2A O3 0.90 2.20 2.884(11) 132.8 4_655 N2 H2A O7 0.90 2.08 2.854(14) 143.3 4_655 N2 H2B O8 0.90 2.37 2.966(11) 124.0 4_655 N2 H2B O14 0.90 2.11 2.986(11) 163.1 2_665 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.261 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.153