# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Wen-Jie Lu' 'Lin-Ping Zhang' 'Hai-Bin Song' 'Quan-Ming Wang' 'Thomas C. W. Mak' _publ_contact_author_name 'Prof Thomas C W Mak' _publ_contact_author_address ; The Chinese University of Hong Kong Department of Chemistry Shatin New Territories Hong Kong SAR, P R CHINA ; _publ_contact_author_email 'TCWMAK@CUHK.EDU.HK' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Novel lanthanide (III) coordination networks ; data_compound_1 _database_code_CSD 170489 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Cl3 Er N6 O19' _chemical_formula_weight 1132.33 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' '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 Hexagonal _symmetry_space_group_name_H-M R-3c _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 24.030(15) _cell_length_b 24.030(15) _cell_length_c 12.815(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6409(9) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block-like _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3402 _exptl_absorpt_coefficient_mu 2.238 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14135 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.21 _reflns_number_total 1759 _reflns_number_gt 1060 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+62.9538P] 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 1759 _refine_ls_number_parameters 109 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1844 _refine_ls_wR_factor_gt 0.1565 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.077 _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 0.3333 0.6667 0.4167 0.0381(3) Uani 1 6 d S . . O1W O 0.3333 0.6667 0.1667 0.20(2) Uani 1 6 d S . . O1 O 0.2800(2) 0.5815(3) 0.3127(6) 0.0544(16) Uani 1 1 d . . . N1 N 0.2174(3) 0.5442(3) 0.2948(6) 0.0553(19) Uani 1 1 d . . . C1 C 0.1923(4) 0.4800(4) 0.2913(11) 0.079(4) Uani 1 1 d . . . H1A H 0.2185 0.4625 0.3037 0.095 Uiso 1 1 calc R . . C2 C 0.1277(5) 0.4398(5) 0.2693(16) 0.128(7) Uani 1 1 d . . . H2A H 0.1114 0.3958 0.2629 0.153 Uiso 1 1 calc R . . C3 C 0.0862(5) 0.4657(6) 0.2565(19) 0.162(10) Uani 1 1 d D . . C4 C 0.1157(5) 0.5321(5) 0.2654(15) 0.116(6) Uani 1 1 d . . . H4A H 0.0900 0.5509 0.2606 0.139 Uiso 1 1 calc R . . C5 C 0.1815(4) 0.5723(5) 0.2810(10) 0.069(3) Uani 1 1 d . . . H5A H 0.1998 0.6168 0.2819 0.083 Uiso 1 1 calc R . . C6 C 0.0212(5) 0.4286(8) 0.2024(7) 0.057(5) Uani 0.50 1 d PD . . C7 C 0.0185(7) 0.4257(12) 0.2999(8) 0.125(13) Uani 0.50 1 d PD . . Cl1 Cl 0.10034(16) 0.6667 0.4167 0.1019(17) Uani 1 2 d SD . . O2 O 0.1454(7) 0.6804(7) 0.3394(13) 0.228(9) Uani 1 1 d D . . O3 O 0.0476(5) 0.6105(7) 0.3860(15) 0.333(14) Uani 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 0.0184(3) 0.0184(3) 0.0775(6) 0.000 0.000 0.00920(14) O1W 0.048(8) 0.048(8) 0.49(8) 0.000 0.000 0.024(4) O1 0.021(2) 0.033(3) 0.102(5) -0.012(3) -0.009(3) 0.008(2) N1 0.026(3) 0.032(3) 0.104(6) -0.010(4) -0.014(3) 0.011(3) C1 0.031(5) 0.029(4) 0.174(12) -0.007(6) -0.009(6) 0.012(4) C2 0.031(5) 0.033(5) 0.31(2) -0.029(9) -0.025(8) 0.007(4) C3 0.028(5) 0.046(6) 0.41(3) -0.044(11) -0.050(10) 0.013(5) C4 0.032(5) 0.045(6) 0.27(2) -0.013(9) -0.037(8) 0.017(5) C5 0.039(5) 0.035(4) 0.135(10) -0.008(5) -0.018(5) 0.019(4) C6 0.021(7) 0.053(11) 0.085(14) -0.019(10) -0.026(8) 0.009(7) C7 0.09(2) 0.09(2) 0.19(4) -0.01(2) -0.09(2) 0.037(18) Cl1 0.0507(14) 0.101(4) 0.171(5) 0.045(3) 0.0226(16) 0.0504(18) O2 0.157(13) 0.156(14) 0.32(2) 0.017(14) 0.119(15) 0.040(11) O3 0.040(6) 0.35(3) 0.47(3) -0.11(3) 0.016(12) -0.004(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 Er1 O1 2.232(6) 12 ? Er1 O1 2.232(6) 3_565 ? Er1 O1 2.232(6) . ? Er1 O1 2.232(6) 2_665 ? Er1 O1 2.232(6) 10_455 ? Er1 O1 2.232(6) 11_565 ? O1 N1 1.330(8) . ? N1 C1 1.346(10) . ? N1 C5 1.349(11) . ? C1 C2 1.387(13) . ? C2 C3 1.425(16) . ? C3 C4 1.390(15) . ? C3 C7 1.521(10) . ? C3 C6 1.524(9) . ? C4 C5 1.395(13) . ? C6 C7 0.828(17) 6 ? C6 C7 1.251(13) . ? C6 C6 1.506(10) 6 ? C7 C6 0.828(17) 6 ? C7 C7 1.492(10) 6 ? Cl1 O3 1.368(9) 11_565 ? Cl1 O3 1.368(9) . ? Cl1 O2 1.381(9) 11_565 ? Cl1 O2 1.381(9) . ? 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 O1 Er1 O1 166.7(3) 12 3_565 ? O1 Er1 O1 102.0(3) 12 . ? O1 Er1 O1 88.0(3) 3_565 . ? O1 Er1 O1 83.6(3) 12 2_665 ? O1 Er1 O1 88.0(3) 3_565 2_665 ? O1 Er1 O1 88.0(3) . 2_665 ? O1 Er1 O1 88.0(3) 12 10_455 ? O1 Er1 O1 101.9(3) 3_565 10_455 ? O1 Er1 O1 83.6(3) . 10_455 ? O1 Er1 O1 166.7(3) 2_665 10_455 ? O1 Er1 O1 88.0(3) 12 11_565 ? O1 Er1 O1 83.6(3) 3_565 11_565 ? O1 Er1 O1 166.7(3) . 11_565 ? O1 Er1 O1 102.0(3) 2_665 11_565 ? O1 Er1 O1 88.0(3) 10_455 11_565 ? N1 O1 Er1 131.2(5) . . ? O1 N1 C1 119.2(7) . . ? O1 N1 C5 118.4(7) . . ? C1 N1 C5 122.4(7) . . ? N1 C1 C2 120.7(9) . . ? C1 C2 C3 120.1(9) . . ? C4 C3 C2 115.2(8) . . ? C4 C3 C7 117.8(16) . . ? C2 C3 C7 116.2(16) . . ? C4 C3 C6 119.6(13) . . ? C2 C3 C6 122.2(12) . . ? C7 C3 C6 48.5(5) . . ? C3 C4 C5 123.9(10) . . ? N1 C5 C4 117.4(9) . . ? C7 C6 C7 89.3(6) 6 . ? C7 C6 C6 56.2(9) 6 6 ? C7 C6 C6 33.3(8) . 6 ? C7 C6 C3 154.8(9) 6 . ? C7 C6 C3 65.6(6) . . ? C6 C6 C3 98.7(11) 6 . ? C6 C7 C6 90.5(6) 6 . ? C6 C7 C7 57.0(9) 6 6 ? C6 C7 C7 33.7(8) . 6 ? C6 C7 C3 155.1(14) 6 . ? C6 C7 C3 65.9(6) . . ? C7 C7 C3 99.5(12) 6 . ? O3 Cl1 O3 128.6(17) 11_565 . ? O3 Cl1 O2 105.0(8) 11_565 11_565 ? O3 Cl1 O2 108.5(9) . 11_565 ? O3 Cl1 O2 108.5(9) 11_565 . ? O3 Cl1 O2 105.0(8) . . ? O2 Cl1 O2 96.6(19) 11_565 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.904 _refine_diff_density_min -1.198 _refine_diff_density_rms 0.165 #========================================END data_compound_2 _database_code_CSD 170490 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Cl3 N6 O19 Yb' _chemical_formula_weight 1138.12 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' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3c _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 23.9937(11) _cell_length_b 23.9937(11) _cell_length_c 12.8101(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6386.7(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3414 _exptl_absorpt_coefficient_mu 2.471 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10675 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.98 _reflns_number_total 1720 _reflns_number_gt 1043 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+36.6142P] 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 1720 _refine_ls_number_parameters 109 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1863 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.074 _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 Yb1 Yb 0.3333 0.6667 0.4167 0.0414(3) Uani 1 6 d S . . O1W O 0.3333 0.6667 0.1667 0.069(5) Uani 1 6 d S . . O1 O 0.2808(2) 0.5822(3) 0.3133(6) 0.0571(16) Uani 1 1 d . . . N1 N 0.2182(3) 0.5449(3) 0.2944(6) 0.0551(19) Uani 1 1 d . . . C1 C 0.1928(4) 0.4808(4) 0.2911(11) 0.081(4) Uani 1 1 d . . . H1A H 0.2191 0.4631 0.3029 0.097 Uiso 1 1 calc R . . C2 C 0.1280(5) 0.4405(5) 0.2702(16) 0.129(7) Uani 1 1 d . . . H2A H 0.1116 0.3963 0.2652 0.154 Uiso 1 1 calc R . . C3 C 0.0865(5) 0.4657(5) 0.2566(18) 0.164(9) Uani 1 1 d D . . C4 C 0.1165(4) 0.5326(5) 0.2661(14) 0.112(6) Uani 1 1 d . . . H4A H 0.0908 0.5514 0.2619 0.135 Uiso 1 1 calc R . . C5 C 0.1824(4) 0.5730(4) 0.2815(10) 0.070(3) Uani 1 1 d . . . H5A H 0.2008 0.6175 0.2827 0.084 Uiso 1 1 calc R . . C6 C 0.0215(5) 0.4289(8) 0.2027(7) 0.055(5) Uani 0.50 1 d PD . . C7 C 0.0186(7) 0.4256(11) 0.2998(8) 0.120(12) Uani 0.50 1 d PD . . Cl1 Cl 0.10008(15) 0.6667 0.4167 0.1018(17) Uani 1 2 d SD . . O2 O 0.1454(7) 0.6810(6) 0.3414(14) 0.220(8) Uani 1 1 d D . . O3 O 0.0481(5) 0.6132(9) 0.3850(15) 0.331(14) Uani 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 Yb1 0.0217(3) 0.0217(3) 0.0809(6) 0.000 0.000 0.01084(15) O1W 0.026(4) 0.026(4) 0.154(17) 0.000 0.000 0.013(2) O1 0.023(2) 0.032(3) 0.108(5) -0.011(3) -0.009(3) 0.008(2) N1 0.027(3) 0.034(3) 0.100(6) -0.012(3) -0.013(3) 0.011(3) C1 0.035(4) 0.036(4) 0.168(12) -0.010(6) -0.014(5) 0.015(4) C2 0.034(5) 0.032(5) 0.31(2) -0.030(8) -0.032(8) 0.005(4) C3 0.034(5) 0.045(6) 0.41(3) -0.039(11) -0.046(10) 0.014(5) C4 0.033(5) 0.057(7) 0.250(18) -0.027(9) -0.033(7) 0.025(5) C5 0.034(4) 0.037(4) 0.139(10) -0.008(5) -0.018(5) 0.017(4) C6 0.025(7) 0.054(10) 0.079(13) -0.014(9) -0.024(8) 0.014(7) C7 0.09(2) 0.083(18) 0.16(3) -0.010(19) -0.09(2) 0.029(17) Cl1 0.0511(13) 0.100(3) 0.170(5) 0.045(3) 0.0224(16) 0.0501(16) O2 0.147(12) 0.146(12) 0.31(2) 0.017(13) 0.116(14) 0.030(10) O3 0.043(6) 0.33(2) 0.50(4) -0.11(2) 0.016(12) 0.002(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 Yb1 O1 2.213(6) 12 ? Yb1 O1 2.213(6) 3_565 ? Yb1 O1 2.213(6) . ? Yb1 O1 2.213(6) 2_665 ? Yb1 O1 2.213(6) 10_455 ? Yb1 O1 2.213(6) 11_565 ? O1 N1 1.330(7) . ? N1 C5 1.339(10) . ? N1 C1 1.344(10) . ? C1 C2 1.387(12) . ? C2 C3 1.410(16) . ? C3 C4 1.396(15) . ? C3 C6 1.522(9) . ? C3 C7 1.524(10) . ? C4 C5 1.396(12) . ? C6 C7 0.835(16) 6 ? C6 C7 1.246(13) . ? C6 C6 1.506(10) 6 ? C7 C6 0.835(16) 6 ? C7 C7 1.492(10) 6 ? Cl1 O3 1.329(12) 11_565 ? Cl1 O3 1.329(12) . ? Cl1 O2 1.363(11) 11_565 ? Cl1 O2 1.363(11) . ? 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 O1 Yb1 O1 167.1(3) 12 3_565 ? O1 Yb1 O1 101.7(3) 12 . ? O1 Yb1 O1 87.9(3) 3_565 . ? O1 Yb1 O1 84.0(3) 12 2_665 ? O1 Yb1 O1 87.9(3) 3_565 2_665 ? O1 Yb1 O1 87.9(3) . 2_665 ? O1 Yb1 O1 87.9(3) 12 10_455 ? O1 Yb1 O1 101.7(3) 3_565 10_455 ? O1 Yb1 O1 84.0(3) . 10_455 ? O1 Yb1 O1 167.2(3) 2_665 10_455 ? O1 Yb1 O1 87.9(3) 12 11_565 ? O1 Yb1 O1 84.0(3) 3_565 11_565 ? O1 Yb1 O1 167.1(3) . 11_565 ? O1 Yb1 O1 101.7(3) 2_665 11_565 ? O1 Yb1 O1 87.9(3) 10_455 11_565 ? N1 O1 Yb1 131.2(5) . . ? O1 N1 C5 118.4(6) . . ? O1 N1 C1 119.2(7) . . ? C5 N1 C1 122.4(7) . . ? N1 C1 C2 120.7(9) . . ? C1 C2 C3 120.8(9) . . ? C4 C3 C2 114.5(8) . . ? C4 C3 C6 119.7(12) . . ? C2 C3 C6 123.0(12) . . ? C4 C3 C7 117.9(15) . . ? C2 C3 C7 116.4(15) . . ? C6 C3 C7 48.3(5) . . ? C3 C4 C5 124.3(9) . . ? N1 C5 C4 117.2(8) . . ? C7 C6 C7 89.3(6) 6 . ? C7 C6 C6 55.9(8) 6 6 ? C7 C6 C6 33.7(8) . 6 ? C7 C6 C3 155.1(9) 6 . ? C7 C6 C3 65.9(6) . . ? C6 C6 C3 99.3(10) 6 . ? C6 C7 C6 90.5(6) 6 . ? C6 C7 C7 56.7(8) 6 6 ? C6 C7 C7 34.0(8) . 6 ? C6 C7 C3 154.9(13) 6 . ? C6 C7 C3 65.7(6) . . ? C7 C7 C3 99.7(12) 6 . ? O3 Cl1 O3 125.9(18) 11_565 . ? O3 Cl1 O2 105.8(8) 11_565 11_565 ? O3 Cl1 O2 109.9(9) . 11_565 ? O3 Cl1 O2 109.9(9) 11_565 . ? O3 Cl1 O2 105.8(8) . . ? O2 Cl1 O2 95.5(18) 11_565 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.800 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.162 #=======================================END data_compound_3 _database_code_CSD 170491 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H23 Er N6 O13' _chemical_formula_weight 698.68 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 P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3115(17) _cell_length_b 15.243(3) _cell_length_c 19.580(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.797(4) _cell_angle_gamma 90.00 _cell_volume 2472.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block-like _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 3.473 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16642 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.1223 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.08 _reflns_number_total 5963 _reflns_number_gt 3023 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^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 5963 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _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 0.43118(5) 0.62442(3) 0.762118(19) 0.03768(14) Uani 1 1 d . . . O1 O -0.1629(8) 0.0112(4) 0.2917(3) 0.0516(17) Uani 1 1 d . . . N1 N -0.0861(9) 0.0695(5) 0.3330(4) 0.0420(18) Uani 1 1 d . . . O2 O 0.3349(10) 0.5890(5) 0.6546(3) 0.074(2) Uani 1 1 d . . . N2 N 0.2679(9) 0.5256(5) 0.6163(4) 0.048(2) Uani 1 1 d . . . O3 O 0.3806(8) 0.7651(4) 0.7272(3) 0.0568(18) Uani 1 1 d . . . N3 N 0.4377(9) 0.8122(5) 0.6773(4) 0.0428(18) Uani 1 1 d . . . C1 C -0.0801(12) 0.0593(6) 0.4005(5) 0.054(3) Uani 1 1 d . . . H1A H -0.1283 0.0108 0.4192 0.065 Uiso 1 1 calc R . . C2 C -0.0005(13) 0.1221(7) 0.4436(5) 0.064(3) Uani 1 1 d . . . H2A H 0.0060 0.1131 0.4908 0.077 Uiso 1 1 calc R . . C3 C 0.0672(13) 0.1956(7) 0.4191(5) 0.058(3) Uani 1 1 d . . . C4 C 0.0541(13) 0.2041(6) 0.3475(5) 0.062(3) Uani 1 1 d . . . H4A H 0.0985 0.2528 0.3275 0.075 Uiso 1 1 calc R . . C5 C -0.0234(12) 0.1412(6) 0.3065(5) 0.056(3) Uani 1 1 d . . . H5A H -0.0324 0.1489 0.2592 0.067 Uiso 1 1 calc R . . C6 C 0.1540(13) 0.2622(7) 0.4664(6) 0.069(3) Uani 1 1 d . . . H6A H 0.1976 0.2336 0.5082 0.082 Uiso 1 1 calc R . . H6B H 0.2430 0.2879 0.4443 0.082 Uiso 1 1 calc R . . C7 C 0.0383(13) 0.3324(7) 0.4832(6) 0.071(3) Uani 1 1 d . . . H7A H -0.0511 0.3067 0.5049 0.085 Uiso 1 1 calc R . . H7B H -0.0045 0.3614 0.4414 0.085 Uiso 1 1 calc R . . C8 C 0.1786(13) 0.4643(7) 0.6420(5) 0.067(3) Uani 1 1 d . . . H8A H 0.1656 0.4638 0.6888 0.081 Uiso 1 1 calc R . . C9 C 0.1050(13) 0.4015(7) 0.6006(5) 0.065(3) Uani 1 1 d . . . H9A H 0.0401 0.3596 0.6192 0.078 Uiso 1 1 calc R . . C10 C 0.1256(14) 0.3995(7) 0.5315(5) 0.067(3) Uani 1 1 d . . . C11 C 0.2236(16) 0.4635(8) 0.5084(5) 0.080(4) Uani 1 1 d . . . H11A H 0.2428 0.4638 0.4622 0.096 Uiso 1 1 calc R . . C12 C 0.2924(13) 0.5252(7) 0.5492(5) 0.063(3) Uani 1 1 d . . . H12A H 0.3571 0.5679 0.5314 0.075 Uiso 1 1 calc R . . C13 C 0.4142(12) 0.7862(6) 0.6124(5) 0.057(3) Uani 1 1 d . . . H13A H 0.3641 0.7326 0.6023 0.069 Uiso 1 1 calc R . . C14 C 0.4619(12) 0.8365(7) 0.5604(5) 0.056(3) Uani 1 1 d . . . H14A H 0.4458 0.8166 0.5154 0.067 Uiso 1 1 calc R . . C15 C 0.5349(10) 0.9179(6) 0.5741(5) 0.044(2) Uani 1 1 d . . . C16 C 0.5642(12) 0.9399(7) 0.6424(5) 0.055(3) Uani 1 1 d . . . H16A H 0.6177 0.9921 0.6541 0.066 Uiso 1 1 calc R . . C17 C 0.5164(12) 0.8871(6) 0.6930(5) 0.054(3) Uani 1 1 d . . . H17A H 0.5386 0.9032 0.7386 0.065 Uiso 1 1 calc R . . C18 C 0.5751(11) 0.9762(6) 0.5157(5) 0.052(2) Uani 1 1 d . . . H18A H 0.6206 0.9410 0.4809 0.062 Uiso 1 1 calc R . . H18B H 0.6555 1.0189 0.5324 0.062 Uiso 1 1 calc R . . N4 N 0.1500(14) 0.6549(6) 0.8303(5) 0.068(3) Uani 1 1 d . . . O4 O 0.2902(10) 0.6653(5) 0.8606(4) 0.070(2) Uani 1 1 d . . . O5 O 0.1407(8) 0.6405(5) 0.7706(4) 0.069(2) Uani 1 1 d . . . O6 O 0.0306(12) 0.6647(7) 0.8630(6) 0.129(4) Uani 1 1 d . . . N5 N 0.6497(10) 0.6681(7) 0.8789(5) 0.061(2) Uani 1 1 d . . . O7 O 0.6084(9) 0.7246(5) 0.8324(4) 0.070(2) Uani 1 1 d . . . O8 O 0.6048(9) 0.5911(5) 0.8661(4) 0.074(2) Uani 1 1 d . . . O9 O 0.7233(10) 0.6904(6) 0.9327(4) 0.097(3) Uani 1 1 d . . . N6 N 0.7149(12) 0.5763(6) 0.6966(4) 0.058(2) Uani 1 1 d . . . O10 O 0.6419(10) 0.5236(5) 0.7334(4) 0.080(2) Uani 1 1 d . . . O11 O 0.6576(8) 0.6557(4) 0.6938(4) 0.064(2) Uani 1 1 d . . . O12 O 0.8320(10) 0.5560(6) 0.6678(4) 0.091(3) Uani 1 1 d . . . O1W O 0.408(2) 0.6264(11) 0.3850(8) 0.099(6) Uani 0.50 1 d P . . O2W O 0.395(3) 0.6575(11) 0.4381(9) 0.112(7) Uani 0.50 1 d P . . 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 0.0490(2) 0.0308(2) 0.0331(2) 0.0060(2) 0.00243(15) -0.0006(2) O1 0.063(4) 0.033(3) 0.058(4) -0.017(3) 0.002(3) 0.002(3) N1 0.045(5) 0.039(4) 0.043(4) -0.007(4) 0.011(4) 0.004(4) O2 0.109(6) 0.070(5) 0.041(4) -0.003(4) -0.009(4) -0.039(5) N2 0.056(5) 0.042(5) 0.046(5) -0.004(4) -0.001(4) -0.012(4) O3 0.082(5) 0.039(4) 0.053(4) 0.016(3) 0.022(4) 0.008(3) N3 0.050(5) 0.036(4) 0.042(4) 0.010(4) 0.002(4) 0.003(4) C1 0.075(7) 0.040(6) 0.051(6) -0.002(5) 0.026(5) 0.002(5) C2 0.096(8) 0.058(7) 0.040(5) -0.017(6) 0.008(5) 0.008(7) C3 0.071(7) 0.044(6) 0.062(7) -0.015(5) 0.014(6) -0.002(5) C4 0.086(8) 0.041(6) 0.063(7) -0.005(5) 0.025(6) -0.013(6) C5 0.078(7) 0.053(7) 0.038(5) -0.003(5) 0.018(5) 0.000(5) C6 0.073(8) 0.060(7) 0.074(8) -0.016(6) 0.008(6) 0.006(6) C7 0.063(7) 0.067(7) 0.083(8) -0.024(7) 0.012(6) -0.007(6) C8 0.081(8) 0.072(8) 0.049(6) -0.015(6) 0.004(6) -0.020(7) C9 0.064(7) 0.066(8) 0.067(7) -0.009(6) 0.018(6) -0.022(6) C10 0.077(8) 0.066(8) 0.058(6) -0.033(6) 0.002(6) -0.004(6) C11 0.122(11) 0.077(9) 0.043(6) -0.021(6) 0.023(7) -0.030(8) C12 0.089(9) 0.055(7) 0.045(6) 0.002(5) 0.009(6) -0.009(6) C13 0.077(8) 0.031(5) 0.060(6) 0.012(5) -0.011(6) -0.007(5) C14 0.072(7) 0.055(6) 0.038(5) 0.003(5) -0.008(5) -0.002(6) C15 0.033(5) 0.040(5) 0.058(6) 0.007(5) -0.003(5) 0.000(4) C16 0.061(7) 0.053(6) 0.051(6) 0.005(5) 0.000(5) -0.011(5) C17 0.072(7) 0.048(6) 0.041(5) 0.004(5) 0.000(5) 0.003(5) C18 0.056(7) 0.048(6) 0.050(6) 0.013(5) 0.007(5) 0.006(5) N4 0.075(8) 0.054(6) 0.074(7) -0.005(5) -0.003(6) 0.016(5) O4 0.070(5) 0.084(6) 0.058(4) -0.021(4) 0.014(4) 0.001(4) O5 0.045(4) 0.077(6) 0.081(5) 0.023(5) -0.019(4) -0.003(4) O6 0.092(7) 0.127(9) 0.178(10) -0.020(8) 0.074(8) 0.020(6) N5 0.046(5) 0.079(7) 0.057(6) -0.012(5) -0.001(5) -0.003(5) O7 0.094(6) 0.053(5) 0.058(4) 0.001(4) -0.010(4) -0.009(4) O8 0.069(5) 0.065(5) 0.082(5) 0.016(4) -0.032(4) -0.002(4) O9 0.080(6) 0.152(9) 0.055(5) -0.019(5) -0.021(4) -0.018(6) N6 0.073(7) 0.054(6) 0.048(5) -0.016(5) 0.008(5) 0.002(5) O10 0.099(6) 0.061(5) 0.085(6) 0.017(4) 0.045(5) 0.029(5) O11 0.064(5) 0.051(4) 0.077(5) 0.025(4) 0.015(4) 0.007(4) O12 0.082(6) 0.113(8) 0.082(6) -0.015(5) 0.029(5) 0.006(6) O1W 0.151(16) 0.080(12) 0.061(10) -0.020(10) -0.013(11) 0.049(12) O2W 0.21(2) 0.052(10) 0.072(11) 0.037(9) 0.019(14) 0.021(12) _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 O2 2.254(6) . ? Er1 O3 2.278(6) . ? Er1 O1 2.302(6) 4_666 ? Er1 O4 2.419(6) . ? Er1 O10 2.431(7) . ? Er1 O11 2.445(7) . ? Er1 O5 2.446(7) . ? Er1 O8 2.448(7) . ? Er1 O7 2.461(7) . ? Er1 N4 2.825(11) . ? Er1 N6 2.872(10) . ? Er1 N5 2.876(9) . ? O1 N1 1.328(8) . ? O1 Er1 2.302(6) 4_565 ? N1 C1 1.328(11) . ? N1 C5 1.335(11) . ? O2 N2 1.317(9) . ? N2 C8 1.320(12) . ? N2 C12 1.347(11) . ? O3 N3 1.331(8) . ? N3 C13 1.331(11) . ? N3 C17 1.340(11) . ? C1 C2 1.405(13) . ? C2 C3 1.358(13) . ? C3 C4 1.404(13) . ? C3 C6 1.516(13) . ? C4 C5 1.375(13) . ? C6 C7 1.493(13) . ? C7 C10 1.534(13) . ? C8 C9 1.366(13) . ? C9 C10 1.377(13) . ? C10 C11 1.373(14) . ? C11 C12 1.333(13) . ? C13 C14 1.360(12) . ? C14 C15 1.397(13) . ? C15 C16 1.381(12) . ? C15 C18 1.506(12) . ? C16 C17 1.361(12) . ? C18 C18 1.529(17) 3_676 ? N4 O5 1.186(10) . ? N4 O6 1.234(11) . ? N4 O4 1.272(11) . ? N5 O9 1.221(10) . ? N5 O8 1.250(10) . ? N5 O7 1.279(10) . ? N6 O12 1.206(10) . ? N6 O10 1.267(10) . ? N6 O11 1.300(10) . ? O1W O2W 1.155(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Er1 O3 84.4(3) . . ? O2 Er1 O1 85.3(2) . 4_666 ? O3 Er1 O1 149.6(2) . 4_666 ? O2 Er1 O4 130.4(3) . . ? O3 Er1 O4 84.7(2) . . ? O1 Er1 O4 80.4(2) 4_666 . ? O2 Er1 O10 80.7(3) . . ? O3 Er1 O10 130.1(2) . . ? O1 Er1 O10 75.9(2) 4_666 . ? O4 Er1 O10 138.9(3) . . ? O2 Er1 O11 76.4(3) . . ? O3 Er1 O11 77.5(2) . . ? O1 Er1 O11 127.3(2) 4_666 . ? O4 Er1 O11 146.3(3) . . ? O10 Er1 O11 52.7(2) . . ? O2 Er1 O5 79.2(3) . . ? O3 Er1 O5 76.6(2) . . ? O1 Er1 O5 73.4(2) 4_666 . ? O4 Er1 O5 51.2(3) . . ? O10 Er1 O5 144.4(3) . . ? O11 Er1 O5 145.8(2) . . ? O2 Er1 O8 149.9(3) . . ? O3 Er1 O8 121.7(3) . . ? O1 Er1 O8 78.1(2) 4_666 . ? O4 Er1 O8 71.5(3) . . ? O10 Er1 O8 71.1(3) . . ? O11 Er1 O8 93.9(3) . . ? O5 Er1 O8 118.7(3) . . ? O2 Er1 O7 145.1(2) . . ? O3 Er1 O7 70.8(2) . . ? O1 Er1 O7 128.1(2) 4_666 . ? O4 Er1 O7 72.6(3) . . ? O10 Er1 O7 96.5(3) . . ? O11 Er1 O7 74.5(2) . . ? O5 Er1 O7 116.6(3) . . ? O8 Er1 O7 51.7(2) . . ? O2 Er1 N4 103.8(3) . . ? O3 Er1 N4 81.3(2) . . ? O1 Er1 N4 73.5(2) 4_666 . ? O4 Er1 N4 26.6(2) . . ? O10 Er1 N4 148.6(3) . . ? O11 Er1 N4 158.7(2) . . ? O5 Er1 N4 24.7(2) . . ? O8 Er1 N4 95.4(3) . . ? O7 Er1 N4 96.5(3) . . ? O2 Er1 N6 76.2(3) . . ? O3 Er1 N6 104.1(3) . . ? O1 Er1 N6 101.1(2) 4_666 . ? O4 Er1 N6 153.1(3) . . ? O10 Er1 N6 26.0(2) . . ? O11 Er1 N6 26.8(2) . . ? O5 Er1 N6 155.2(3) . . ? O8 Er1 N6 82.5(3) . . ? O7 Er1 N6 86.2(2) . . ? N4 Er1 N6 174.5(3) . . ? O2 Er1 N5 161.6(3) . . ? O3 Er1 N5 96.3(3) . . ? O1 Er1 N5 102.3(3) 4_666 . ? O4 Er1 N5 67.8(3) . . ? O10 Er1 N5 84.9(3) . . ? O11 Er1 N5 85.7(2) . . ? O5 Er1 N5 118.9(3) . . ? O8 Er1 N5 25.6(2) . . ? O7 Er1 N5 26.3(2) . . ? N4 Er1 N5 94.5(3) . . ? N6 Er1 N5 85.8(2) . . ? N1 O1 Er1 126.7(5) . 4_565 ? C1 N1 O1 120.2(8) . . ? C1 N1 C5 120.0(8) . . ? O1 N1 C5 119.6(7) . . ? N2 O2 Er1 143.8(6) . . ? O2 N2 C8 121.9(8) . . ? O2 N2 C12 117.8(8) . . ? C8 N2 C12 120.3(9) . . ? N3 O3 Er1 131.3(5) . . ? C13 N3 O3 120.5(8) . . ? C13 N3 C17 120.1(8) . . ? O3 N3 C17 119.3(7) . . ? N1 C1 C2 119.7(9) . . ? C3 C2 C1 122.5(9) . . ? C2 C3 C4 115.5(9) . . ? C2 C3 C6 121.8(10) . . ? C4 C3 C6 122.8(10) . . ? C5 C4 C3 120.8(9) . . ? N1 C5 C4 121.5(9) . . ? C7 C6 C3 109.4(9) . . ? C6 C7 C10 109.4(9) . . ? N2 C8 C9 120.5(10) . . ? C8 C9 C10 120.9(10) . . ? C11 C10 C9 115.7(10) . . ? C11 C10 C7 122.2(10) . . ? C9 C10 C7 122.0(11) . . ? C12 C11 C10 122.7(10) . . ? C11 C12 N2 119.8(10) . . ? N3 C13 C14 121.3(9) . . ? C13 C14 C15 120.4(9) . . ? C16 C15 C14 116.1(9) . . ? C16 C15 C18 123.9(9) . . ? C14 C15 C18 119.9(9) . . ? C17 C16 C15 121.5(9) . . ? N3 C17 C16 120.3(9) . . ? C15 C18 C18 111.2(9) . 3_676 ? O5 N4 O6 123.0(12) . . ? O5 N4 O4 117.6(10) . . ? O6 N4 O4 119.3(11) . . ? O5 N4 Er1 59.5(6) . . ? O6 N4 Er1 176.2(9) . . ? O4 N4 Er1 58.6(5) . . ? N4 O4 Er1 94.8(6) . . ? N4 O5 Er1 95.9(7) . . ? O9 N5 O8 123.6(11) . . ? O9 N5 O7 120.7(10) . . ? O8 N5 O7 115.6(9) . . ? O9 N5 Er1 170.9(7) . . ? O8 N5 Er1 57.7(5) . . ? O7 N5 Er1 58.4(5) . . ? N5 O7 Er1 95.3(6) . . ? N5 O8 Er1 96.7(6) . . ? O12 N6 O10 123.2(10) . . ? O12 N6 O11 121.8(10) . . ? O10 N6 O11 115.0(8) . . ? O12 N6 Er1 178.6(7) . . ? O10 N6 Er1 57.2(5) . . ? O11 N6 Er1 57.9(5) . . ? N6 O10 Er1 96.8(6) . . ? N6 O11 Er1 95.3(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.000 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.162 #=========================================END data_compound_4 _database_code_CSD 170492 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H23 N6 O13 Yb' _chemical_formula_weight 704.46 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' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3329(15) _cell_length_b 15.215(3) _cell_length_c 19.602(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.882(4) _cell_angle_gamma 90.00 _cell_volume 2476.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 3.854 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.453 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16387 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.09 _reflns_number_total 5968 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^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 5968 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Yb1 Yb 0.42992(4) 0.62437(2) 0.761364(14) 0.03071(11) Uani 1 1 d . . . O1 O -0.1624(6) 0.0095(4) 0.2906(3) 0.0453(14) Uani 1 1 d . . . N1 N -0.0872(7) 0.0696(4) 0.3325(3) 0.0371(14) Uani 1 1 d . . . O2 O 0.3345(8) 0.5896(4) 0.6544(3) 0.0646(19) Uani 1 1 d . . . N2 N 0.2676(8) 0.5251(5) 0.6163(3) 0.0410(16) Uani 1 1 d . . . O3 O 0.3798(7) 0.7636(4) 0.7278(3) 0.0463(14) Uani 1 1 d . . . N3 N 0.4371(7) 0.8122(4) 0.6776(3) 0.0380(15) Uani 1 1 d . . . C1 C -0.0808(9) 0.0587(6) 0.4006(4) 0.046(2) Uani 1 1 d . . . H1A H -0.1277 0.0093 0.4185 0.055 Uiso 1 1 calc R . . C2 C -0.0061(11) 0.1195(6) 0.4444(4) 0.053(2) Uani 1 1 d . . . H2A H -0.0044 0.1108 0.4915 0.064 Uiso 1 1 calc R . . C3 C 0.0665(10) 0.1933(6) 0.4198(4) 0.051(2) Uani 1 1 d . . . C4 C 0.0544(11) 0.2037(6) 0.3477(4) 0.056(2) Uani 1 1 d . . . H4A H 0.0981 0.2534 0.3288 0.067 Uiso 1 1 calc R . . C5 C -0.0205(10) 0.1417(6) 0.3052(4) 0.049(2) Uani 1 1 d . . . H5A H -0.0256 0.1490 0.2579 0.059 Uiso 1 1 calc R . . C6 C 0.1539(11) 0.2598(7) 0.4661(5) 0.067(3) Uani 1 1 d . . . H6A H 0.2416 0.2854 0.4434 0.080 Uiso 1 1 calc R . . H6B H 0.1989 0.2313 0.5077 0.080 Uiso 1 1 calc R . . C7 C 0.0382(11) 0.3309(7) 0.4837(5) 0.062(3) Uani 1 1 d . . . H7A H -0.0508 0.3047 0.5052 0.075 Uiso 1 1 calc R . . H7B H -0.0051 0.3598 0.4420 0.075 Uiso 1 1 calc R . . C8 C 0.1760(10) 0.4644(6) 0.6414(4) 0.054(2) Uani 1 1 d . . . H8A H 0.1612 0.4647 0.6879 0.065 Uiso 1 1 calc R . . C9 C 0.1026(11) 0.4012(6) 0.6005(4) 0.056(3) Uani 1 1 d . . . H9A H 0.0385 0.3591 0.6194 0.067 Uiso 1 1 calc R . . C10 C 0.1221(11) 0.3990(6) 0.5321(4) 0.051(2) Uani 1 1 d . . . C11 C 0.2198(12) 0.4638(7) 0.5081(5) 0.068(3) Uani 1 1 d . . . H11A H 0.2342 0.4657 0.4616 0.082 Uiso 1 1 calc R . . C12 C 0.2940(11) 0.5235(6) 0.5495(4) 0.056(2) Uani 1 1 d . . . H12A H 0.3637 0.5639 0.5323 0.067 Uiso 1 1 calc R . . C13 C 0.4096(10) 0.7857(5) 0.6118(4) 0.047(2) Uani 1 1 d . . . H13A H 0.3565 0.7329 0.6018 0.056 Uiso 1 1 calc R . . C14 C 0.4601(10) 0.8365(6) 0.5598(4) 0.050(2) Uani 1 1 d . . . H14A H 0.4446 0.8170 0.5147 0.060 Uiso 1 1 calc R . . C15 C 0.5340(8) 0.9168(6) 0.5742(4) 0.0375(18) Uani 1 1 d . . . C16 C 0.5648(10) 0.9397(6) 0.6428(4) 0.049(2) Uani 1 1 d . . . H16A H 0.6193 0.9917 0.6541 0.059 Uiso 1 1 calc R . . C17 C 0.5165(10) 0.8870(6) 0.6938(4) 0.049(2) Uani 1 1 d . . . H17A H 0.5386 0.9030 0.7394 0.059 Uiso 1 1 calc R . . C18 C 0.5757(9) 0.9762(6) 0.5159(4) 0.044(2) Uani 1 1 d . . . H18A H 0.6220 0.9413 0.4810 0.052 Uiso 1 1 calc R . . H18B H 0.6552 1.0192 0.5329 0.052 Uiso 1 1 calc R . . N4 N 0.1493(11) 0.6561(6) 0.8297(5) 0.068(2) Uani 1 1 d . . . O4 O 0.2911(8) 0.6649(5) 0.8592(3) 0.0637(18) Uani 1 1 d . . . O5 O 0.1409(7) 0.6395(5) 0.7692(4) 0.0618(18) Uani 1 1 d . . . O6 O 0.0300(10) 0.6644(7) 0.8620(5) 0.121(4) Uani 1 1 d . . . N5 N 0.6498(8) 0.6664(6) 0.8778(3) 0.0511(19) Uani 1 1 d . . . O7 O 0.6093(7) 0.7236(4) 0.8322(3) 0.0591(17) Uani 1 1 d . . . O8 O 0.6030(8) 0.5897(5) 0.8648(3) 0.0683(19) Uani 1 1 d . . . O9 O 0.7222(8) 0.6870(6) 0.9319(3) 0.087(3) Uani 1 1 d . . . N6 N 0.7123(9) 0.5789(6) 0.6967(3) 0.0533(19) Uani 1 1 d . . . O10 O 0.6392(8) 0.5230(5) 0.7322(3) 0.0704(19) Uani 1 1 d . . . O11 O 0.6569(7) 0.6557(4) 0.6936(3) 0.0519(15) Uani 1 1 d . . . O12 O 0.8289(8) 0.5571(6) 0.6677(3) 0.078(2) Uani 1 1 d . . . O1W O 0.407(2) 0.6267(11) 0.3867(8) 0.094(5) Uani 0.50 1 d P . . O1W' O 0.400(2) 0.6597(10) 0.4401(8) 0.105(6) Uani 0.50 1 d P . . 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 Yb1 0.04256(19) 0.02751(17) 0.02188(15) 0.00559(15) 0.00168(11) -0.00122(16) O1 0.046(3) 0.042(3) 0.047(3) -0.012(3) -0.003(2) 0.003(3) N1 0.042(4) 0.033(4) 0.036(3) -0.005(3) 0.001(3) 0.007(3) O2 0.104(5) 0.059(4) 0.028(3) -0.003(3) -0.011(3) -0.027(4) N2 0.054(4) 0.039(4) 0.028(3) -0.006(3) -0.001(3) -0.002(3) O3 0.066(4) 0.038(3) 0.037(3) 0.019(3) 0.016(3) 0.006(3) N3 0.045(4) 0.035(4) 0.034(3) 0.010(3) 0.004(3) 0.006(3) C1 0.059(5) 0.041(5) 0.039(4) 0.001(4) 0.020(4) 0.003(4) C2 0.081(6) 0.049(5) 0.031(4) -0.008(4) 0.010(4) 0.001(5) C3 0.057(5) 0.048(6) 0.049(5) -0.021(4) 0.011(4) 0.003(4) C4 0.078(6) 0.037(5) 0.055(5) -0.005(4) 0.016(5) -0.012(5) C5 0.068(6) 0.043(6) 0.038(4) -0.008(4) 0.010(4) 0.002(4) C6 0.070(6) 0.061(7) 0.066(6) -0.026(5) -0.010(5) 0.008(5) C7 0.063(6) 0.060(7) 0.064(6) -0.019(5) 0.006(5) -0.007(5) C8 0.065(6) 0.060(6) 0.038(4) -0.012(4) 0.002(4) -0.020(5) C9 0.071(6) 0.058(7) 0.039(4) -0.009(4) 0.011(4) -0.028(5) C10 0.062(5) 0.043(6) 0.048(5) -0.016(4) 0.001(4) -0.006(4) C11 0.095(8) 0.070(8) 0.041(5) -0.010(5) 0.017(5) -0.020(6) C12 0.083(6) 0.059(6) 0.026(4) -0.004(4) 0.014(4) -0.025(5) C13 0.062(5) 0.034(5) 0.041(4) 0.013(4) -0.016(4) -0.008(4) C14 0.068(6) 0.047(5) 0.033(4) 0.002(4) -0.011(4) -0.008(5) C15 0.034(4) 0.044(5) 0.034(4) 0.013(4) 0.001(3) 0.005(4) C16 0.062(5) 0.039(5) 0.046(5) -0.002(4) -0.002(4) -0.002(4) C17 0.069(6) 0.043(6) 0.034(4) 0.009(4) 0.005(4) -0.003(4) C18 0.046(4) 0.045(5) 0.040(4) 0.023(4) -0.001(3) -0.001(4) N4 0.067(6) 0.051(5) 0.090(7) 0.013(5) 0.023(5) 0.012(4) O4 0.063(4) 0.077(5) 0.053(4) -0.018(4) 0.016(3) 0.000(4) O5 0.045(3) 0.068(5) 0.070(4) 0.020(4) -0.006(3) 0.003(3) O6 0.074(5) 0.150(10) 0.147(8) -0.012(7) 0.058(6) 0.019(5) N5 0.040(4) 0.077(6) 0.035(4) -0.004(4) -0.001(3) 0.003(4) O7 0.079(4) 0.049(4) 0.047(3) 0.005(3) -0.008(3) -0.013(3) O8 0.069(4) 0.063(5) 0.069(4) 0.017(4) -0.021(3) -0.009(4) O9 0.069(4) 0.152(8) 0.035(3) -0.016(4) -0.014(3) -0.013(5) N6 0.062(5) 0.062(6) 0.037(4) -0.020(4) 0.006(3) 0.002(4) O10 0.090(5) 0.055(4) 0.072(4) 0.022(4) 0.036(4) 0.014(4) O11 0.054(4) 0.051(4) 0.052(4) 0.015(3) 0.013(3) 0.002(3) O12 0.077(5) 0.102(7) 0.060(4) -0.017(4) 0.027(4) 0.018(4) O1W 0.130(13) 0.081(12) 0.067(9) -0.028(9) -0.004(9) 0.047(10) O1W' 0.205(19) 0.048(9) 0.065(10) 0.028(8) 0.031(11) 0.038(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 Yb1 O2 2.241(5) . ? Yb1 O3 2.246(5) . ? Yb1 O1 2.268(5) 4_666 ? Yb1 O4 2.403(6) . ? Yb1 O10 2.432(7) . ? Yb1 O5 2.437(6) . ? Yb1 O8 2.443(6) . ? Yb1 O11 2.450(6) . ? Yb1 O7 2.467(6) . ? Yb1 N4 2.833(9) . ? Yb1 N6 2.851(8) . ? Yb1 N5 2.875(7) . ? O1 N1 1.348(8) . ? O1 Yb1 2.268(5) 4_565 ? N1 C1 1.342(9) . ? N1 C5 1.360(10) . ? O2 N2 1.326(8) . ? N2 C8 1.320(10) . ? N2 C12 1.346(9) . ? O3 N3 1.352(7) . ? N3 C17 1.341(10) . ? N3 C13 1.352(9) . ? C1 C2 1.374(11) . ? C2 C3 1.382(12) . ? C3 C4 1.419(11) . ? C3 C6 1.505(12) . ? C4 C5 1.373(11) . ? C6 C7 1.507(13) . ? C7 C10 1.533(12) . ? C8 C9 1.363(11) . ? C9 C10 1.365(11) . ? C10 C11 1.386(13) . ? C11 C12 1.335(12) . ? C13 C14 1.374(11) . ? C14 C15 1.386(12) . ? C15 C16 1.390(10) . ? C15 C18 1.521(10) . ? C16 C17 1.369(11) . ? C18 C18 1.539(14) 3_676 ? N4 O5 1.208(10) . ? N4 O6 1.230(10) . ? N4 O4 1.277(10) . ? N5 O9 1.216(8) . ? N5 O8 1.250(10) . ? N5 O7 1.272(9) . ? N6 O12 1.212(8) . ? N6 O11 1.255(10) . ? N6 O10 1.285(9) . ? O1W O1W' 1.166(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Yb1 O3 84.7(2) . . ? O2 Yb1 O1 85.6(2) . 4_666 ? O3 Yb1 O1 149.5(2) . 4_666 ? O2 Yb1 O4 130.6(3) . . ? O3 Yb1 O4 84.3(2) . . ? O1 Yb1 O4 80.3(2) 4_666 . ? O2 Yb1 O10 80.5(3) . . ? O3 Yb1 O10 130.4(2) . . ? O1 Yb1 O10 75.9(2) 4_666 . ? O4 Yb1 O10 138.9(2) . . ? O2 Yb1 O5 78.9(3) . . ? O3 Yb1 O5 76.7(2) . . ? O1 Yb1 O5 73.2(2) 4_666 . ? O4 Yb1 O5 51.7(2) . . ? O10 Yb1 O5 143.8(3) . . ? O2 Yb1 O8 149.6(3) . . ? O3 Yb1 O8 121.9(2) . . ? O1 Yb1 O8 77.6(2) 4_666 . ? O4 Yb1 O8 71.5(2) . . ? O10 Yb1 O8 71.0(2) . . ? O5 Yb1 O8 119.0(2) . . ? O2 Yb1 O11 76.5(2) . . ? O3 Yb1 O11 77.9(2) . . ? O1 Yb1 O11 127.3(2) 4_666 . ? O4 Yb1 O11 146.1(2) . . ? O10 Yb1 O11 52.7(2) . . ? O5 Yb1 O11 146.0(2) . . ? O8 Yb1 O11 93.6(2) . . ? O2 Yb1 O7 145.1(2) . . ? O3 Yb1 O7 71.1(2) . . ? O1 Yb1 O7 127.56(19) 4_666 . ? O4 Yb1 O7 72.8(2) . . ? O10 Yb1 O7 96.2(2) . . ? O5 Yb1 O7 117.5(2) . . ? O8 Yb1 O7 51.6(2) . . ? O11 Yb1 O7 74.2(2) . . ? O2 Yb1 N4 104.0(3) . . ? O3 Yb1 N4 80.6(2) . . ? O1 Yb1 N4 73.9(2) 4_666 . ? O4 Yb1 N4 26.6(2) . . ? O10 Yb1 N4 148.9(2) . . ? O5 Yb1 N4 25.1(2) . . ? O8 Yb1 N4 95.6(3) . . ? O11 Yb1 N4 158.4(2) . . ? O7 Yb1 N4 96.6(3) . . ? O2 Yb1 N6 76.5(2) . . ? O3 Yb1 N6 103.8(2) . . ? O1 Yb1 N6 101.8(2) 4_666 . ? O4 Yb1 N6 152.7(2) . . ? O10 Yb1 N6 26.7(2) . . ? O5 Yb1 N6 155.3(2) . . ? O8 Yb1 N6 82.3(2) . . ? O11 Yb1 N6 26.0(2) . . ? O7 Yb1 N6 85.1(2) . . ? N4 Yb1 N6 175.6(2) . . ? O2 Yb1 N5 161.2(2) . . ? O3 Yb1 N5 96.5(2) . . ? O1 Yb1 N5 101.9(2) 4_666 . ? O4 Yb1 N5 68.1(2) . . ? O10 Yb1 N5 84.6(2) . . ? O5 Yb1 N5 119.7(2) . . ? O8 Yb1 N5 25.6(2) . . ? O11 Yb1 N5 85.3(2) . . ? O7 Yb1 N5 26.2(2) . . ? N4 Yb1 N5 94.7(3) . . ? N6 Yb1 N5 84.98(19) . . ? N1 O1 Yb1 127.8(4) . 4_565 ? C1 N1 O1 120.0(7) . . ? C1 N1 C5 120.6(7) . . ? O1 N1 C5 119.4(6) . . ? N2 O2 Yb1 143.1(5) . . ? C8 N2 O2 122.5(6) . . ? C8 N2 C12 119.8(7) . . ? O2 N2 C12 117.8(7) . . ? N3 O3 Yb1 131.4(4) . . ? C17 N3 O3 119.3(6) . . ? C17 N3 C13 121.3(7) . . ? O3 N3 C13 119.3(7) . . ? N1 C1 C2 121.1(8) . . ? C1 C2 C3 121.1(7) . . ? C2 C3 C4 116.3(8) . . ? C2 C3 C6 122.7(8) . . ? C4 C3 C6 121.1(9) . . ? C5 C4 C3 121.2(8) . . ? N1 C5 C4 119.7(7) . . ? C3 C6 C7 109.5(7) . . ? C6 C7 C10 111.1(8) . . ? N2 C8 C9 121.3(8) . . ? C8 C9 C10 120.7(8) . . ? C9 C10 C11 116.0(8) . . ? C9 C10 C7 122.6(9) . . ? C11 C10 C7 121.4(8) . . ? C12 C11 C10 122.2(8) . . ? C11 C12 N2 119.9(8) . . ? N3 C13 C14 120.1(8) . . ? C13 C14 C15 120.2(8) . . ? C14 C15 C16 117.4(7) . . ? C14 C15 C18 119.7(7) . . ? C16 C15 C18 122.9(8) . . ? C17 C16 C15 121.2(8) . . ? N3 C17 C16 119.5(7) . . ? C15 C18 C18 110.6(8) . 3_676 ? O5 N4 O6 123.0(10) . . ? O5 N4 O4 116.1(8) . . ? O6 N4 O4 120.9(10) . . ? O5 N4 Yb1 58.8(4) . . ? O6 N4 Yb1 175.3(8) . . ? O4 N4 Yb1 57.6(4) . . ? N4 O4 Yb1 95.8(5) . . ? N4 O5 Yb1 96.1(5) . . ? O9 N5 O8 122.8(9) . . ? O9 N5 O7 121.3(9) . . ? O8 N5 O7 115.8(7) . . ? O9 N5 Yb1 170.2(6) . . ? O8 N5 Yb1 57.5(4) . . ? O7 N5 Yb1 58.7(4) . . ? N5 O7 Yb1 95.1(5) . . ? N5 O8 Yb1 96.9(5) . . ? O12 N6 O11 122.5(9) . . ? O12 N6 O10 120.6(9) . . ? O11 N6 O10 116.9(7) . . ? O12 N6 Yb1 177.4(7) . . ? O11 N6 Yb1 58.8(4) . . ? O10 N6 Yb1 58.1(4) . . ? N6 O10 Yb1 95.2(5) . . ? N6 O11 Yb1 95.2(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.010 _refine_diff_density_min -1.764 _refine_diff_density_rms 0.190 #=========================================END data_compound_5 _database_code_CSD 170493 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H22 Cl2 La N5 O13' _chemical_formula_weight 690.19 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' 'La' 'La' -0.2871 2.4523 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.609(2) _cell_length_b 10.801(3) _cell_length_c 13.566(3) _cell_angle_alpha 78.380(5) _cell_angle_beta 82.011(5) _cell_angle_gamma 89.895(5) _cell_volume 1365.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9333 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.1156 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.06 _reflns_number_total 6474 _reflns_number_gt 4154 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^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 6474 _refine_ls_number_parameters 352 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.982 _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 La1 La 0.55170(5) 0.49046(4) 0.33634(4) 0.03439(17) Uani 1 1 d . . . O1 O 0.4201(5) 0.3972(4) 0.5130(4) 0.0350(12) Uani 1 1 d . . . O2 O 0.3830(6) 0.3488(5) 0.2914(5) 0.0504(15) Uani 1 1 d . . . O3 O 0.5786(8) 0.5667(6) 0.1378(5) 0.0612(17) Uani 1 1 d . . . O4 O 0.6993(7) 0.4042(6) 0.1909(5) 0.0589(17) Uani 1 1 d . . . O5 O 0.7217(11) 0.4877(10) 0.0307(6) 0.110(3) Uani 1 1 d . . . O6 O 0.4693(7) 0.7275(6) 0.2840(6) 0.0641(19) Uani 1 1 d . . . O7 O 0.3027(7) 0.5848(6) 0.3268(6) 0.0635(18) Uani 1 1 d . . . O8 O 0.2537(9) 0.7780(8) 0.2605(8) 0.100(3) Uani 1 1 d . . . O9 O 0.6164(7) 0.2496(6) 0.3942(5) 0.0535(15) Uani 1 1 d . . . O10 O 0.7538(6) 0.3841(6) 0.4343(6) 0.0615(18) Uani 1 1 d . . . O11 O 0.7437(9) 0.1871(7) 0.5122(8) 0.096(3) Uani 1 1 d . . . N1 N 0.3205(6) 0.3041(5) 0.5234(5) 0.0331(14) Uani 1 1 d . . . N2 N 0.4049(7) 0.2607(7) 0.2340(6) 0.0456(17) Uani 1 1 d . . . N3 N 0.6678(10) 0.4865(9) 0.1176(6) 0.061(2) Uani 1 1 d . . . N4 N 0.3396(9) 0.7005(7) 0.2896(6) 0.058(2) Uani 1 1 d . . . N5 N 0.7084(8) 0.2715(8) 0.4482(7) 0.057(2) Uani 1 1 d . . . C1 C 0.1910(8) 0.3351(7) 0.5042(7) 0.0423(19) Uani 1 1 d . . . H1A H 0.1701 0.4197 0.4838 0.051 Uiso 1 1 calc R . . C2 C 0.0876(9) 0.2425(8) 0.5145(7) 0.049(2) Uani 1 1 d . . . H2A H -0.0029 0.2649 0.5025 0.059 Uiso 1 1 calc R . . C3 C 0.1198(9) 0.1161(7) 0.5428(6) 0.0410(19) Uani 1 1 d . . . C4 C 0.2537(9) 0.0886(7) 0.5630(6) 0.0402(19) Uani 1 1 d . . . H4A H 0.2772 0.0050 0.5846 0.048 Uiso 1 1 calc R . . C5 C 0.3546(8) 0.1842(7) 0.5514(6) 0.0394(18) Uani 1 1 d . . . H5A H 0.4458 0.1644 0.5633 0.047 Uiso 1 1 calc R . . C6 C 0.0098(9) 0.0124(8) 0.5512(3) 0.050(2) Uani 1 1 d D . . H6A H 0.0380 -0.0647 0.5930 0.059 Uiso 1 1 calc R . . H6B H -0.0791 0.0368 0.5844 0.059 Uiso 1 1 calc R . . C7 C 0.4138(11) 0.1396(9) 0.2770(8) 0.061(3) Uani 1 1 d . . . H7A H 0.4045 0.1153 0.3474 0.073 Uiso 1 1 calc R . . C8 C 0.4361(13) 0.0514(9) 0.2190(8) 0.066(3) Uani 1 1 d . . . H8A H 0.4410 -0.0331 0.2502 0.080 Uiso 1 1 calc R . . C9 C 0.4519(11) 0.0843(8) 0.1140(8) 0.059(3) Uani 1 1 d . . . C10 C 0.4410(12) 0.2088(9) 0.0716(7) 0.062(3) Uani 1 1 d . . . H10A H 0.4503 0.2341 0.0012 0.074 Uiso 1 1 calc R . . C11 C 0.4163(10) 0.2981(9) 0.1313(7) 0.053(2) Uani 1 1 d . . . H11A H 0.4076 0.3827 0.1016 0.064 Uiso 1 1 calc R . . C12 C 0.4878(16) -0.0209(9) 0.0564(2) 0.092(4) Uani 1 1 d D . . H12A H 0.5717 -0.0614 0.0782 0.110 Uiso 1 1 calc R . . H12B H 0.4118 -0.0838 0.0746 0.110 Uiso 1 1 calc R . . C13 C 0.8017(15) 0.7445(12) 0.2125(10) 0.102(5) Uani 1 1 d . . . H13A H 0.8981 0.7701 0.2096 0.153 Uiso 1 1 calc R . . H13B H 0.7414 0.8073 0.2350 0.153 Uiso 1 1 calc R . . H13C H 0.7847 0.7356 0.1462 0.153 Uiso 1 1 calc R . . O12 O 0.7741(7) 0.6282(6) 0.2810(5) 0.0624(18) Uani 1 1 d . . . H12O H 0.8445 0.5831 0.2920 0.080 Uiso 1 1 d . . . C14 C 1.0530(18) 0.440(2) 0.2396(15) 0.164(9) Uani 1 1 d . . . H14A H 1.1010 0.4812 0.1743 0.197 Uiso 1 1 calc R . . H14B H 0.9661 0.4027 0.2313 0.197 Uiso 1 1 calc R . . H14C H 1.1110 0.3759 0.2710 0.197 Uiso 1 1 calc R . . O13 O 1.0252(9) 0.5302(11) 0.3016(10) 0.126(4) Uani 1 1 d . . . H13O H 1.0878 0.5297 0.3371 0.200 Uiso 1 1 calc R . . C15 C 0.1012(11) 0.7960(14) -0.0818(8) 0.135(7) Uani 1 1 d D . . Cl1 Cl 0.1685(9) 0.9105(6) -0.1838(5) 0.217(3) Uani 1 1 d D . . Cl2 Cl 0.1676(11) 0.8113(18) 0.0262(7) 0.065(4) Uani 0.25 1 d PDU . . Cl3 Cl -0.0831(10) 0.7981(16) -0.0719(11) 0.088(5) Uani 0.25 1 d PDU . . Cl4 Cl 0.1219(12) 0.832(2) 0.0315(8) 0.084(6) Uani 0.25 1 d PDU . . Cl5 Cl -0.0658(14) 0.750(2) -0.0804(15) 0.143(9) Uani 0.25 1 d PDU . . 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 La1 0.0380(3) 0.0300(3) 0.0379(3) -0.01517(17) -0.00292(18) -0.00915(17) O1 0.036(3) 0.026(3) 0.043(3) -0.013(2) 0.000(2) -0.016(2) O2 0.052(4) 0.050(4) 0.060(4) -0.038(3) -0.006(3) -0.010(3) O3 0.073(5) 0.053(4) 0.058(4) -0.009(3) -0.011(4) 0.005(4) O4 0.067(4) 0.062(4) 0.051(4) -0.022(3) -0.006(3) 0.000(3) O5 0.128(8) 0.154(9) 0.041(5) -0.017(5) 0.007(5) 0.005(7) O6 0.058(4) 0.034(4) 0.100(6) -0.007(3) -0.021(4) -0.008(3) O7 0.056(4) 0.043(4) 0.090(5) -0.011(3) -0.012(4) -0.006(3) O8 0.092(6) 0.065(5) 0.147(9) -0.004(5) -0.057(6) 0.014(5) O9 0.059(4) 0.045(4) 0.061(4) -0.023(3) -0.005(3) -0.003(3) O10 0.047(4) 0.044(4) 0.102(6) -0.027(4) -0.019(4) -0.007(3) O11 0.100(6) 0.053(5) 0.147(8) -0.015(5) -0.068(6) 0.025(4) N1 0.032(3) 0.025(3) 0.046(4) -0.017(3) -0.005(3) -0.011(3) N2 0.050(4) 0.043(4) 0.053(5) -0.028(3) -0.013(3) -0.009(3) N3 0.071(6) 0.068(6) 0.042(5) -0.008(4) -0.002(4) -0.014(5) N4 0.070(6) 0.042(5) 0.070(6) -0.015(4) -0.028(5) 0.006(4) N5 0.048(5) 0.050(5) 0.082(6) -0.028(4) -0.020(4) 0.008(4) C1 0.041(5) 0.028(4) 0.057(5) -0.008(4) -0.006(4) -0.008(3) C2 0.039(5) 0.047(5) 0.066(6) -0.017(4) -0.014(4) -0.018(4) C3 0.048(5) 0.034(4) 0.044(5) -0.016(3) -0.002(4) -0.016(4) C4 0.047(5) 0.028(4) 0.045(5) -0.006(3) -0.008(4) -0.014(3) C5 0.037(4) 0.035(5) 0.048(5) -0.013(4) -0.008(4) -0.009(3) C6 0.045(5) 0.039(5) 0.065(6) -0.010(4) -0.009(4) -0.023(4) C7 0.088(8) 0.046(6) 0.050(6) -0.018(4) -0.003(5) -0.017(5) C8 0.109(9) 0.039(5) 0.050(6) -0.013(4) -0.005(6) -0.010(5) C9 0.089(8) 0.035(5) 0.060(6) -0.026(4) -0.007(5) -0.009(5) C10 0.097(8) 0.047(6) 0.046(5) -0.022(4) -0.012(5) -0.009(5) C11 0.064(6) 0.047(5) 0.055(6) -0.016(4) -0.024(5) -0.003(4) C12 0.154(13) 0.058(7) 0.063(7) -0.035(6) 0.018(8) -0.021(7) C13 0.113(11) 0.101(10) 0.079(9) -0.007(7) 0.015(8) -0.058(9) O12 0.059(4) 0.065(4) 0.061(4) -0.021(3) 0.012(3) -0.025(3) C14 0.090(12) 0.27(3) 0.158(19) -0.103(18) -0.023(12) 0.044(14) O13 0.055(5) 0.171(11) 0.165(11) -0.069(8) -0.013(6) -0.014(6) C15 0.097(11) 0.099(12) 0.180(19) -0.013(11) 0.056(11) -0.019(9) Cl1 0.293(9) 0.167(6) 0.162(6) 0.016(4) -0.009(6) -0.039(6) Cl2 0.009(6) 0.140(11) 0.057(7) -0.052(7) 0.007(4) -0.005(7) Cl3 0.039(6) 0.158(14) 0.102(9) -0.115(10) 0.000(6) -0.005(7) Cl4 0.008(6) 0.187(17) 0.065(8) -0.062(8) 0.020(5) -0.009(8) Cl5 0.066(9) 0.25(2) 0.156(13) -0.189(14) 0.048(8) -0.065(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 La1 O2 2.449(5) . ? La1 O12 2.541(6) . ? La1 O1 2.559(5) . ? La1 O4 2.595(7) . ? La1 O7 2.608(7) . ? La1 O1 2.623(5) 2_666 ? La1 O3 2.629(7) . ? La1 O10 2.637(6) . ? La1 O9 2.661(6) . ? La1 O6 2.665(6) . ? La1 N3 3.030(9) . ? La1 N5 3.056(9) . ? O1 N1 1.362(7) . ? O1 La1 2.623(5) 2_666 ? O2 N2 1.344(8) . ? O3 N3 1.260(11) . ? O4 N3 1.264(10) . ? O5 N3 1.218(11) . ? O6 N4 1.270(10) . ? O7 N4 1.280(9) . ? O8 N4 1.222(10) . ? O9 N5 1.274(9) . ? O10 N5 1.261(9) . ? O11 N5 1.210(10) . ? N1 C5 1.327(10) . ? N1 C1 1.335(10) . ? N2 C7 1.329(11) . ? N2 C11 1.360(11) . ? C1 C2 1.384(10) . ? C2 C3 1.389(12) . ? C3 C4 1.372(12) . ? C3 C6 1.518(10) . ? C4 C5 1.388(10) . ? C6 C6 1.502(5) 2_556 ? C7 C8 1.352(13) . ? C8 C9 1.383(13) . ? C9 C10 1.362(13) . ? C9 C12 1.518(13) . ? C10 C11 1.379(13) . ? C12 C12 1.491(5) 2_655 ? C13 O12 1.406(13) . ? C14 O13 1.409(19) . ? C15 Cl5 1.678(13) . ? C15 Cl4 1.698(14) . ? C15 Cl1 1.711(10) . ? C15 Cl2 1.714(13) . ? C15 Cl3 1.758(13) . ? Cl3 Cl5 0.58(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O12 147.6(2) . . ? O2 La1 O1 79.99(18) . . ? O12 La1 O1 131.31(19) . . ? O2 La1 O4 77.5(2) . . ? O12 La1 O4 72.9(2) . . ? O1 La1 O4 136.48(19) . . ? O2 La1 O7 66.5(2) . . ? O12 La1 O7 121.7(2) . . ? O1 La1 O7 77.6(2) . . ? O4 La1 O7 124.5(2) . . ? O2 La1 O1 138.48(17) . 2_666 ? O12 La1 O1 73.75(18) . 2_666 ? O1 La1 O1 61.22(17) . 2_666 ? O4 La1 O1 141.34(18) . 2_666 ? O7 La1 O1 89.8(2) . 2_666 ? O2 La1 O3 78.6(2) . . ? O12 La1 O3 72.2(2) . . ? O1 La1 O3 155.26(19) . . ? O4 La1 O3 48.8(2) . . ? O7 La1 O3 82.6(2) . . ? O1 La1 O3 133.90(18) 2_666 . ? O2 La1 O10 117.0(2) . . ? O12 La1 O10 70.8(2) . . ? O1 La1 O10 77.4(2) . . ? O4 La1 O10 80.5(2) . . ? O7 La1 O10 153.5(2) . . ? O1 La1 O10 70.52(19) 2_666 . ? O3 La1 O10 123.8(2) . . ? O2 La1 O9 68.9(2) . . ? O12 La1 O9 110.3(2) . . ? O1 La1 O9 69.57(18) . . ? O4 La1 O9 67.7(2) . . ? O7 La1 O9 127.99(19) . . ? O1 La1 O9 107.14(18) 2_666 . ? O3 La1 O9 113.2(2) . . ? O10 La1 O9 48.17(19) . . ? O2 La1 O6 108.5(2) . . ? O12 La1 O6 73.4(2) . . ? O1 La1 O6 107.4(2) . . ? O4 La1 O6 114.9(2) . . ? O7 La1 O6 48.35(19) . . ? O1 La1 O6 72.8(2) 2_666 . ? O3 La1 O6 68.4(2) . . ? O10 La1 O6 134.2(2) . . ? O9 La1 O6 176.2(2) . . ? O2 La1 N3 77.9(2) . . ? O12 La1 N3 69.7(2) . . ? O1 La1 N3 154.6(2) . . ? O4 La1 N3 24.4(2) . . ? O7 La1 N3 104.4(2) . . ? O1 La1 N3 143.02(18) 2_666 . ? O3 La1 N3 24.4(2) . . ? O10 La1 N3 101.9(2) . . ? O9 La1 N3 90.8(2) . . ? O6 La1 N3 91.3(2) . . ? O2 La1 N5 93.0(2) . . ? O12 La1 N5 92.5(2) . . ? O1 La1 N5 68.2(2) . . ? O4 La1 N5 76.3(2) . . ? O7 La1 N5 142.9(2) . . ? O1 La1 N5 86.25(19) 2_666 . ? O3 La1 N5 125.1(2) . . ? O10 La1 N5 24.19(18) . . ? O9 La1 N5 24.53(19) . . ? O6 La1 N5 157.2(2) . . ? N3 La1 N5 100.7(2) . . ? N1 O1 La1 119.3(4) . . ? N1 O1 La1 121.0(4) . 2_666 ? La1 O1 La1 118.78(17) . 2_666 ? N2 O2 La1 129.8(5) . . ? N3 O3 La1 95.9(5) . . ? N3 O4 La1 97.5(6) . . ? N4 O6 La1 96.4(5) . . ? N4 O7 La1 98.8(5) . . ? N5 O9 La1 95.4(5) . . ? N5 O10 La1 96.9(5) . . ? C5 N1 C1 121.3(6) . . ? C5 N1 O1 119.3(6) . . ? C1 N1 O1 119.3(6) . . ? C7 N2 O2 120.6(8) . . ? C7 N2 C11 120.8(8) . . ? O2 N2 C11 118.6(7) . . ? O5 N3 O3 121.4(9) . . ? O5 N3 O4 121.0(10) . . ? O3 N3 O4 117.6(8) . . ? O5 N3 La1 176.3(8) . . ? O3 N3 La1 59.7(5) . . ? O4 N3 La1 58.1(5) . . ? O8 N4 O6 123.2(8) . . ? O8 N4 O7 121.0(9) . . ? O6 N4 O7 115.8(7) . . ? O11 N5 O10 123.1(8) . . ? O11 N5 O9 119.8(8) . . ? O10 N5 O9 117.0(8) . . ? O11 N5 La1 163.4(7) . . ? O10 N5 La1 59.0(4) . . ? O9 N5 La1 60.1(4) . . ? N1 C1 C2 120.6(8) . . ? C1 C2 C3 119.7(8) . . ? C4 C3 C2 117.7(7) . . ? C4 C3 C6 121.5(7) . . ? C2 C3 C6 120.8(8) . . ? C3 C4 C5 120.8(8) . . ? N1 C5 C4 119.8(8) . . ? C6 C6 C3 111.9(7) 2_556 . ? N2 C7 C8 120.4(9) . . ? C7 C8 C9 121.4(9) . . ? C10 C9 C8 117.3(8) . . ? C10 C9 C12 125.8(8) . . ? C8 C9 C12 116.8(8) . . ? C9 C10 C11 121.1(9) . . ? N2 C11 C10 119.1(9) . . ? C12 C12 C9 114.6(11) 2_655 . ? C13 O12 La1 131.5(7) . . ? Cl5 C15 Cl4 110.2(9) . . ? Cl5 C15 Cl1 115.5(11) . . ? Cl4 C15 Cl1 113.1(10) . . ? Cl5 C15 Cl2 122.6(9) . . ? Cl4 C15 Cl2 16.7(6) . . ? Cl1 C15 Cl2 111.6(9) . . ? Cl5 C15 Cl3 19.2(8) . . ? Cl4 C15 Cl3 99.5(9) . . ? Cl1 C15 Cl3 108.0(9) . . ? Cl2 C15 Cl3 114.9(9) . . ? Cl5 Cl3 C15 72.6(16) . . ? Cl3 Cl5 C15 88.2(15) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.366 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.171 #===========================================END data_compound_6 _database_code_CSD 175817 _journal_coden_Cambridge 440 loop_ _publ_author_name 'Wen-Jie Lu' 'Lin-Ping Zhang' 'Hai-Bin Song' 'Quan-Ming Wang' 'Thomas C. W. Mak' _publ_contact_author_name 'Prof Thomas C W Mak' _publ_contact_author_address ; The Chinese University of Hong Kong Department of Chemistry Shatin New Territories Hong Kong SAR, P R CHINA ; _publ_contact_author_email 'TCWMAK@CUHK.EDU.HK' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Novel lanthanide (III) coordination networks ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H37 Cl Er N3 O21' _chemical_formula_weight 882.26 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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1013(16) _cell_length_b 11.2822(17) _cell_length_c 16.313(3) _cell_angle_alpha 79.512(3) _cell_angle_beta 88.198(3) _cell_angle_gamma 66.963(3) _cell_volume 1680.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block-like _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 2.665 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11459 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.99 _reflns_number_total 7914 _reflns_number_gt 6160 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^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 7914 _refine_ls_number_parameters 469 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 1.016 _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 0.61121(3) 0.21902(2) 0.465522(14) 0.02441(8) Uani 1 1 d . . . O1 O 0.7382(4) 0.2131(3) 0.34390(19) 0.0302(8) Uani 1 1 d . . . N1 N 0.6837(5) 0.2865(4) 0.2693(2) 0.0308(10) Uani 1 1 d . . . C1 C 0.5862(7) 0.2639(6) 0.2280(3) 0.0415(14) Uani 1 1 d . . . H1A H 0.5525 0.2005 0.2523 0.050 Uiso 1 1 calc R . . C2 C 0.5359(7) 0.3351(6) 0.1492(4) 0.0497(17) Uani 1 1 d . . . H2A H 0.4683 0.3191 0.1205 0.060 Uiso 1 1 calc R . . C3 C 0.5850(7) 0.4299(6) 0.1124(3) 0.0472(16) Uani 1 1 d . . . C4 C 0.6825(8) 0.4507(7) 0.1565(4) 0.059(2) Uani 1 1 d . . . H4A H 0.7177 0.5136 0.1334 0.071 Uiso 1 1 calc R . . C5 C 0.7297(7) 0.3796(6) 0.2349(4) 0.0475(16) Uani 1 1 d . . . H5A H 0.7952 0.3965 0.2648 0.057 Uiso 1 1 calc R . . C6 C 0.5413(8) 0.5056(7) 0.0254(4) 0.0580(18) Uani 1 1 d . . . H6A H 0.5800 0.5678 0.0071 0.070 Uiso 1 1 calc R . . O2 O 0.9675(5) -0.1046(4) 0.3697(2) 0.0501(11) Uani 1 1 d . . . N2 N 0.9485(6) -0.0487(5) 0.2896(3) 0.0430(12) Uani 1 1 d . . . C7 C 0.8381(7) -0.0476(6) 0.2445(4) 0.0503(16) Uani 1 1 d . . . H7A H 0.7788 -0.0883 0.2693 0.060 Uiso 1 1 calc R . . C8 C 0.8128(8) 0.0126(7) 0.1629(4) 0.0574(19) Uani 1 1 d . . . H8A H 0.7360 0.0134 0.1326 0.069 Uiso 1 1 calc R . . C9 C 0.9008(8) 0.0731(6) 0.1246(4) 0.0490(16) Uani 1 1 d . . . C10 C 1.0150(8) 0.0654(7) 0.1725(4) 0.0569(18) Uani 1 1 d . . . H10A H 1.0781 0.1023 0.1486 0.068 Uiso 1 1 calc R . . C11 C 1.0373(7) 0.0052(7) 0.2541(4) 0.0537(17) Uani 1 1 d . . . H11A H 1.1148 0.0017 0.2851 0.064 Uiso 1 1 calc R . . C12 C 0.8801(8) 0.1425(7) 0.0361(4) 0.0594(19) Uani 1 1 d . . . H12A H 0.9497 0.1738 0.0159 0.071 Uiso 1 1 calc R . . C13 C 0.7748(8) 0.1637(7) -0.0158(4) 0.0569(18) Uani 1 1 d . . . H13A H 0.7040 0.1335 0.0037 0.068 Uiso 1 1 calc R . . C14 C 0.8341(8) 0.3505(7) -0.2180(4) 0.063(2) Uani 1 1 d . . . H14A H 0.8970 0.3891 -0.2399 0.076 Uiso 1 1 calc R . . C15 C 0.8526(9) 0.2882(8) -0.1365(4) 0.068(2) Uani 1 1 d . . . H15A H 0.9285 0.2839 -0.1037 0.082 Uiso 1 1 calc R . . C16 C 0.7595(8) 0.2313(7) -0.1023(4) 0.0507(16) Uani 1 1 d . . . C17 C 0.6501(8) 0.2423(7) -0.1535(4) 0.062(2) Uani 1 1 d . . . H17A H 0.5842 0.2067 -0.1327 0.074 Uiso 1 1 calc R . . C18 C 0.6347(8) 0.3046(7) -0.2352(4) 0.0579(18) Uani 1 1 d . . . H18A H 0.5591 0.3106 -0.2690 0.070 Uiso 1 1 calc R . . N3 N 0.7270(6) 0.3565(5) -0.2663(3) 0.0414(12) Uani 1 1 d . . . O3 O 0.7145(5) 0.4135(4) -0.3468(2) 0.0517(12) Uani 1 1 d . . . C19 C 0.4552(6) 0.4824(5) 0.5356(3) 0.0288(11) Uani 1 1 d . . . O4 O 0.4615(4) 0.3668(3) 0.5476(2) 0.0309(8) Uani 1 1 d . . . O5 O 0.3859(4) 0.5696(3) 0.5759(2) 0.0317(8) Uani 1 1 d . . . C20 C 0.4927(6) 0.0085(5) 0.5462(3) 0.0279(11) Uani 1 1 d . . . O6 O 0.5241(4) 0.0974(3) 0.5647(2) 0.0359(9) Uani 1 1 d . . . O7 O 0.4526(4) -0.0683(3) 0.5944(2) 0.0347(9) Uani 1 1 d . . . O8 O 1.0009(7) 0.3924(5) 0.4709(4) 0.0844(18) Uani 1 1 d . . . C21 C 1.1005(9) 0.3789(7) 0.5327(5) 0.077(2) Uani 1 1 d . . . H21A H 1.1936 0.3609 0.5082 0.093 Uiso 1 1 calc R . . H21B H 1.1096 0.3034 0.5751 0.093 Uiso 1 1 calc R . . C22 C 1.0665(14) 0.4891(10) 0.5718(7) 0.147(6) Uani 1 1 d . . . H22A H 1.0087 0.4781 0.6190 0.176 Uiso 1 1 calc R . . H22B H 1.1561 0.4853 0.5944 0.176 Uiso 1 1 calc R . . O1W O 0.4067(4) 0.3298(4) 0.3800(2) 0.0421(10) Uani 1 1 d . . . H1WA H 0.3586 0.2985 0.3552 0.051 Uiso 1 1 d R . . H1WB H 0.3435 0.4072 0.3771 0.051 Uiso 1 1 d R . . O2W O 0.8183(4) 0.0248(4) 0.4839(2) 0.0449(10) Uani 1 1 d . . . H2WA H 0.8663 0.0025 0.4416 0.054 Uiso 1 1 d R . . H2WB H 0.8554 -0.0348 0.5264 0.054 Uiso 1 1 d R . . O3W O 0.7607(4) 0.2231(4) 0.5687(2) 0.0449(10) Uani 1 1 d . . . H3WA H 0.8486 0.1799 0.5845 0.054 Uiso 1 1 d R . . H3WB H 0.7354 0.2780 0.6015 0.054 Uiso 1 1 d R . . O4W O 1.0233(5) 0.1906(4) 0.3950(2) 0.0507(11) Uani 1 1 d . . . H4WA H 0.9437 0.1857 0.3849 0.076 Uiso 1 1 d R . . H4WB H 1.0031 0.2412 0.4304 0.076 Uiso 1 1 d R . . O5W O 1.2445(6) 0.2333(5) 0.2971(3) 0.0766(16) Uani 1 1 d . . . H5WA H 1.1573 0.2457 0.3066 0.115 Uiso 1 1 d R . . H5WB H 1.2331 0.2782 0.2481 0.115 Uiso 1 1 d R . . O6W O 0.4627(9) 1.0074(7) 0.2295(5) 0.145(3) Uani 1 1 d . . . H6WA H 0.3971 0.9795 0.2445 0.217 Uiso 1 1 d R . . H6WB H 0.4294 1.0712 0.1888 0.217 Uiso 1 1 d R . . O7W O 0.6387(7) 0.7511(7) 0.2997(3) 0.102(2) Uani 1 1 d . . . H7WA H 0.6103 0.7166 0.3437 0.152 Uiso 1 1 d R . . H7WB H 0.5849 0.8294 0.2781 0.152 Uiso 1 1 d R . . O8W O 0.8538(8) 0.6340(7) 0.2038(4) 0.113(2) Uani 1 1 d . . . H8WA H 0.7857 0.6702 0.2344 0.170 Uiso 1 1 d R . . H8WB H 0.8406 0.6874 0.1578 0.170 Uiso 1 1 d R . . O9W O 1.0625(9) 0.4047(8) 0.1656(5) 0.156(3) Uani 1 1 d . . . H9WA H 0.9995 0.4841 0.1552 0.234 Uiso 1 1 d R . . H9WB H 1.1427 0.4127 0.1430 0.234 Uiso 1 1 d R . . Cl1 Cl 0.7140(4) 0.8005(4) -0.00778(18) 0.1290(13) Uani 1 1 d D . . O11 O 0.7967(18) 0.8261(18) 0.0473(9) 0.177(7) Uani 0.50 1 d PDU . . O12 O 0.5808(13) 0.805(2) 0.0225(13) 0.256(9) Uani 0.50 1 d PDU . . O13 O 0.690(2) 0.888(2) -0.0847(8) 0.282(10) Uani 0.50 1 d PDU . . O14 O 0.791(2) 0.6720(12) -0.0249(16) 0.432(13) Uani 0.50 1 d PDU . . O11' O 0.749(2) 0.9050(16) -0.0475(11) 0.206(9) Uani 0.50 1 d PDU . . O12' O 0.658(2) 0.827(2) 0.0708(7) 0.229(9) Uani 0.50 1 d PDU . . O13' O 0.609(2) 0.789(3) -0.0558(11) 0.385(9) Uani 0.50 1 d PDU . . O14' O 0.8386(18) 0.6830(15) 0.0058(15) 0.430(18) Uani 0.50 1 d PDU . . 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 0.03499(14) 0.01828(11) 0.02171(11) -0.00206(8) -0.00020(8) -0.01292(9) O1 0.038(2) 0.0279(19) 0.0187(17) 0.0014(14) -0.0029(15) -0.0093(17) N1 0.039(3) 0.028(2) 0.024(2) -0.0021(18) 0.0004(19) -0.012(2) C1 0.055(4) 0.040(3) 0.035(3) -0.003(3) -0.004(3) -0.026(3) C2 0.060(5) 0.063(4) 0.034(3) -0.011(3) -0.008(3) -0.031(4) C3 0.061(5) 0.041(4) 0.029(3) 0.004(3) -0.002(3) -0.013(3) C4 0.086(6) 0.061(5) 0.037(3) 0.014(3) -0.010(3) -0.046(4) C5 0.060(5) 0.053(4) 0.037(3) 0.007(3) -0.011(3) -0.036(4) C6 0.072(5) 0.055(4) 0.044(4) 0.003(3) -0.016(3) -0.026(4) O2 0.049(3) 0.049(3) 0.036(2) 0.000(2) -0.004(2) -0.005(2) N2 0.042(3) 0.041(3) 0.038(3) -0.011(2) 0.003(2) -0.006(2) C7 0.053(4) 0.052(4) 0.046(4) -0.004(3) 0.001(3) -0.023(3) C8 0.066(5) 0.060(5) 0.048(4) -0.010(3) -0.016(3) -0.026(4) C9 0.061(5) 0.047(4) 0.038(3) -0.012(3) 0.005(3) -0.019(3) C10 0.058(5) 0.070(5) 0.046(4) -0.001(3) 0.003(3) -0.033(4) C11 0.050(4) 0.069(5) 0.050(4) -0.016(3) -0.002(3) -0.028(4) C12 0.066(5) 0.070(5) 0.044(4) -0.011(4) 0.004(4) -0.030(4) C13 0.062(5) 0.061(5) 0.047(4) -0.009(3) 0.005(4) -0.025(4) C14 0.075(6) 0.080(5) 0.050(4) 0.003(4) -0.016(4) -0.051(5) C15 0.086(6) 0.088(6) 0.047(4) -0.010(4) -0.015(4) -0.051(5) C16 0.057(5) 0.055(4) 0.036(3) -0.004(3) -0.001(3) -0.019(4) C17 0.059(5) 0.079(5) 0.057(4) -0.016(4) 0.005(4) -0.035(4) C18 0.051(5) 0.071(5) 0.056(4) -0.016(4) -0.011(3) -0.026(4) N3 0.044(3) 0.035(3) 0.041(3) -0.011(2) -0.007(2) -0.010(2) O3 0.078(3) 0.032(2) 0.039(2) -0.0034(19) -0.018(2) -0.014(2) C19 0.033(3) 0.029(3) 0.026(3) 0.001(2) -0.005(2) -0.016(2) O4 0.041(2) 0.0180(18) 0.036(2) -0.0023(15) 0.0084(17) -0.0155(17) O5 0.044(2) 0.0201(18) 0.0332(19) -0.0064(15) 0.0091(17) -0.0144(17) C20 0.037(3) 0.020(3) 0.026(3) -0.003(2) 0.000(2) -0.011(2) O6 0.064(3) 0.032(2) 0.0255(18) -0.0098(16) 0.0059(18) -0.032(2) O7 0.059(3) 0.030(2) 0.0252(18) -0.0019(15) 0.0041(17) -0.029(2) O8 0.098(5) 0.047(3) 0.106(4) -0.017(3) -0.040(4) -0.022(3) C21 0.080(6) 0.048(5) 0.096(6) -0.012(4) -0.031(5) -0.016(4) C22 0.191(13) 0.085(8) 0.140(10) -0.017(7) -0.114(10) -0.022(8) O1W 0.045(3) 0.030(2) 0.049(2) -0.0079(18) -0.0160(19) -0.0105(19) O2W 0.055(3) 0.028(2) 0.029(2) -0.0031(17) -0.0051(18) 0.0071(19) O3W 0.043(3) 0.038(2) 0.051(2) -0.0159(19) -0.0169(19) -0.007(2) O4W 0.057(3) 0.046(3) 0.047(2) -0.006(2) -0.009(2) -0.019(2) O5W 0.063(4) 0.098(4) 0.084(4) -0.020(3) 0.000(3) -0.047(3) O6W 0.190(9) 0.125(7) 0.126(6) -0.040(5) 0.007(6) -0.061(6) O7W 0.105(5) 0.151(6) 0.071(4) -0.023(4) 0.028(4) -0.074(5) O8W 0.124(6) 0.126(6) 0.106(5) -0.032(4) 0.020(4) -0.063(5) O9W 0.140(8) 0.115(6) 0.183(8) -0.005(6) -0.045(6) -0.024(6) Cl1 0.187(3) 0.188(3) 0.0796(18) -0.014(2) 0.0079(19) -0.150(3) O11 0.203(16) 0.244(18) 0.177(15) -0.053(14) -0.038(13) -0.179(15) O12 0.277(18) 0.48(2) 0.20(2) -0.090(19) 0.088(16) -0.346(17) O13 0.38(2) 0.47(2) 0.125(15) 0.083(17) -0.033(16) -0.365(18) O14 0.90(3) 0.448(18) 0.24(3) -0.06(2) -0.09(3) -0.571 O11' 0.27(2) 0.254(17) 0.21(2) -0.033(15) 0.048(16) -0.238(16) O12' 0.188(19) 0.42(2) 0.140(16) -0.045(17) 0.043(14) -0.193(18) O13' 0.588(17) 0.669(18) 0.21(2) -0.06(2) -0.04(2) -0.582 O14' 0.89(5) 0.38(3) 0.14(2) 0.04(2) -0.09(3) -0.40(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 O1W 2.303(4) . ? Er1 O6 2.307(3) . ? Er1 O3W 2.315(4) . ? Er1 O1 2.326(3) . ? Er1 O2W 2.341(4) . ? Er1 O4 2.361(3) . ? Er1 O5 2.369(3) 2_666 ? Er1 O7 2.401(3) 2_656 ? O1 N1 1.337(5) . ? N1 C5 1.337(6) . ? N1 C1 1.337(7) . ? C1 C2 1.378(8) . ? C2 C3 1.384(8) . ? C3 C4 1.353(9) . ? C3 C6 1.497(8) . ? C4 C5 1.367(8) . ? C6 C6 1.249(12) 2_665 ? O2 N2 1.328(6) . ? N2 C11 1.333(8) . ? N2 C7 1.351(8) . ? C7 C8 1.361(8) . ? C8 C9 1.389(9) . ? C9 C10 1.380(9) . ? C9 C12 1.490(9) . ? C10 C11 1.361(9) . ? C12 C13 1.299(9) . ? C13 C16 1.457(9) . ? C14 N3 1.332(8) . ? C14 C15 1.367(9) . ? C15 C16 1.384(9) . ? C16 C17 1.360(9) . ? C17 C18 1.370(9) . ? C18 N3 1.325(8) . ? N3 O3 1.341(6) . ? C19 O5 1.248(6) . ? C19 O4 1.259(6) . ? C19 C19 1.541(10) 2_666 ? O5 Er1 2.369(3) 2_666 ? C20 O7 1.241(5) . ? C20 O6 1.250(5) . ? C20 C20 1.548(9) 2_656 ? O7 Er1 2.401(3) 2_656 ? O8 C22 1.310(10) 2_766 ? O8 C21 1.393(8) . ? C21 C22 1.419(11) . ? C22 O8 1.310(10) 2_766 ? Cl1 O11 1.386(4) . ? Cl1 O13' 1.400(5) . ? Cl1 O11' 1.402(5) . ? Cl1 O12 1.403(5) . ? Cl1 O14' 1.412(5) . ? Cl1 O13 1.412(5) . ? Cl1 O12' 1.419(5) . ? Cl1 O14 1.427(5) . ? O11 O12' 1.439(17) . ? O11 O11' 1.621(16) . ? O11 O14' 1.76(2) . ? O12 O12' 1.244(17) . ? O12 O13' 1.330(19) . ? O13 O11' 0.949(18) . ? O13 O13' 1.635(18) . ? O14 O14' 0.76(3) . ? O14 O13' 1.81(2) . ? 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 O1W Er1 O6 98.95(14) . . ? O1W Er1 O3W 147.86(14) . . ? O6 Er1 O3W 88.63(13) . . ? O1W Er1 O1 86.21(13) . . ? O6 Er1 O1 143.59(12) . . ? O3W Er1 O1 106.00(14) . . ? O1W Er1 O2W 140.70(13) . . ? O6 Er1 O2W 82.97(14) . . ? O3W Er1 O2W 71.02(13) . . ? O1 Er1 O2W 71.26(13) . . ? O1W Er1 O4 78.20(13) . . ? O6 Er1 O4 74.13(12) . . ? O3W Er1 O4 73.94(14) . . ? O1 Er1 O4 141.59(11) . . ? O2W Er1 O4 138.23(12) . . ? O1W Er1 O5 76.92(13) . 2_666 ? O6 Er1 O5 142.53(12) . 2_666 ? O3W Er1 O5 78.22(13) . 2_666 ? O1 Er1 O5 73.82(12) . 2_666 ? O2W Er1 O5 123.80(14) . 2_666 ? O4 Er1 O5 68.55(11) . 2_666 ? O1W Er1 O7 69.57(13) . 2_656 ? O6 Er1 O7 68.97(11) . 2_656 ? O3W Er1 O7 141.06(13) . 2_656 ? O1 Er1 O7 79.53(12) . 2_656 ? O2W Er1 O7 74.83(14) . 2_656 ? O4 Er1 O7 125.32(12) . 2_656 ? O5 Er1 O7 138.14(12) 2_666 2_656 ? N1 O1 Er1 125.0(3) . . ? O1 N1 C5 120.1(4) . . ? O1 N1 C1 119.9(4) . . ? C5 N1 C1 120.0(5) . . ? N1 C1 C2 119.7(5) . . ? C1 C2 C3 120.7(5) . . ? C4 C3 C2 117.7(5) . . ? C4 C3 C6 118.6(6) . . ? C2 C3 C6 123.6(6) . . ? C3 C4 C5 120.4(6) . . ? N1 C5 C4 121.4(5) . . ? C6 C6 C3 127.2(9) 2_665 . ? O2 N2 C11 120.6(5) . . ? O2 N2 C7 119.1(5) . . ? C11 N2 C7 120.4(5) . . ? N2 C7 C8 120.5(6) . . ? C7 C8 C9 120.6(6) . . ? C10 C9 C8 116.7(6) . . ? C10 C9 C12 119.1(6) . . ? C8 C9 C12 124.2(6) . . ? C11 C10 C9 121.5(6) . . ? N2 C11 C10 120.3(6) . . ? C13 C12 C9 126.7(7) . . ? C12 C13 C16 124.8(7) . . ? N3 C14 C15 120.6(6) . . ? C14 C15 C16 120.8(6) . . ? C17 C16 C15 116.5(6) . . ? C17 C16 C13 120.8(6) . . ? C15 C16 C13 122.8(6) . . ? C16 C17 C18 121.5(7) . . ? N3 C18 C17 120.4(6) . . ? C18 N3 C14 120.2(6) . . ? C18 N3 O3 120.3(5) . . ? C14 N3 O3 119.5(5) . . ? O5 C19 O4 126.8(5) . . ? O5 C19 C19 117.3(5) . 2_666 ? O4 C19 C19 115.9(6) . 2_666 ? C19 O4 Er1 119.4(3) . . ? C19 O5 Er1 118.7(3) . 2_666 ? O7 C20 O6 126.6(4) . . ? O7 C20 C20 116.8(5) . 2_656 ? O6 C20 C20 116.5(5) . 2_656 ? C20 O6 Er1 120.3(3) . . ? C20 O7 Er1 117.1(3) . 2_656 ? C22 O8 C21 116.1(6) 2_766 . ? O8 C21 C22 115.1(7) . . ? O8 C22 C21 120.1(8) 2_766 . ? O11 Cl1 O13' 169.4(11) . . ? O11 Cl1 O11' 71.1(8) . . ? O13' Cl1 O11' 109.9(7) . . ? O11 Cl1 O12 114.0(7) . . ? O13' Cl1 O12 56.6(9) . . ? O11' Cl1 O12 128.0(15) . . ? O11 Cl1 O14' 77.8(11) . . ? O13' Cl1 O14' 110.9(7) . . ? O11' Cl1 O14' 110.3(7) . . ? O12 Cl1 O14' 121.6(16) . . ? O11 Cl1 O13 110.5(6) . . ? O13' Cl1 O13 71.1(9) . . ? O11' Cl1 O13 39.4(8) . . ? O12 Cl1 O13 109.1(7) . . ? O14' Cl1 O13 119.7(16) . . ? O11 Cl1 O12' 61.7(8) . . ? O13' Cl1 O12' 108.8(7) . . ? O11' Cl1 O12' 108.5(7) . . ? O12 Cl1 O12' 52.3(8) . . ? O14' Cl1 O12' 108.5(7) . . ? O13 Cl1 O12' 128.5(16) . . ? O11 Cl1 O14 109.1(7) . . ? O13' Cl1 O14 79.8(12) . . ? O11' Cl1 O14 120.2(16) . . ? O12 Cl1 O14 107.0(6) . . ? O14' Cl1 O14 31.3(12) . . ? O13 Cl1 O14 106.9(7) . . ? O12' Cl1 O14 124.2(16) . . ? Cl1 O11 O12' 60.3(5) . . ? Cl1 O11 O11' 54.9(4) . . ? O12' O11 O11' 96.7(9) . . ? Cl1 O11 O14' 51.7(6) . . ? O12' O11 O14' 91.4(8) . . ? O11' O11 O14' 86.1(7) . . ? O12' O12 O13' 125.8(6) . . ? O12' O12 Cl1 64.5(5) . . ? O13' O12 Cl1 61.6(5) . . ? O11' O13 Cl1 69.7(6) . . ? O11' O13 O13' 123.0(8) . . ? Cl1 O13 O13' 54.1(5) . . ? O14' O14 Cl1 73.3(7) . . ? O14' O14 O13' 122.5(8) . . ? Cl1 O14 O13' 49.5(6) . . ? O13 O11' Cl1 70.9(6) . . ? O13 O11' O11 124.9(6) . . ? Cl1 O11' O11 54.0(4) . . ? O12 O12' Cl1 63.2(5) . . ? O12 O12' O11 121.2(6) . . ? Cl1 O12' O11 58.0(5) . . ? O12 O13' Cl1 61.8(5) . . ? O12 O13' O13 100.9(10) . . ? Cl1 O13' O13 54.8(5) . . ? O12 O13' O14 91.5(10) . . ? Cl1 O13' O14 50.8(6) . . ? O13 O13' O14 82.6(8) . . ? O14 O14' Cl1 75.4(8) . . ? O14 O14' O11 125.8(7) . . ? Cl1 O14' O11 50.4(6) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.974 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.139 #===============================================END