data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 #=== _publ_contact_author_name 'Prof. Charles Winter' _publ_contact_author_address ; Department of Chemistry Wayne State University Detroit, Michigan 48202 ; _publ_contact_author_email chw@chem.wayne.edu _publ_section_title ; Synthesis, structure, and properties of volatile lanthanide complexes containing amidinate ligands: Application for Er2O3 thin film growth by atomic layer deposition ; loop_ _publ_author_name _publ_author_address 'Jani Paivasaari' ; Laboratory of Inorganic and Analytical Chemistry Helsinki University of Technology FIN-02015 Espoo, Finland ; 'C.L.Dezelah IV' ; Laboratory of Inorganic and Analytical Chemistry Helsinki University of Technology FIN-02015 Espoo, Finland ; 'Dwayne Back' ; Wayne State University Detroit, Michigan 48202 USA ; H.M.El-Kaderi ; Wayne State University Detroit, Michigan 48202 USA ; 'Mary Jane Heeg' ; Wayne State University Detroit, Michigan 48202 USA ; ; M.Putkonen ; ; Laboratory of Inorganic and Analytical Chemistry Helsinki University of Technology FIN-02015 Espoo, Finland ; 'Lauri Niinisto' ; Laboratory of Inorganic and Analytical Chemistry Helsinki University of Technology FIN-02015 Espoo, Finland ; 'Charles H. Winter' ; Wayne State University Detroit, Michigan 48202 USA ; #=== data_yank _database_code_depnum_ccdc_archive 'CCDC 272568' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H63 N6 Y' _chemical_formula_weight 596.77 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 17.2830(12) _cell_length_b 11.7794(9) _cell_length_c 19.1659(14) _cell_angle_alpha 90.00 _cell_angle_beta 116.1940(10) _cell_angle_gamma 90.00 _cell_volume 3501.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2901 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhomboids _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7285 _exptl_absorpt_correction_T_max 0.7285 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21855 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_sigmaI/netI 0.0992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4058 _reflns_number_gt 2497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-93 _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^)+(0.0543P)^2^+1.4688P] 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 4058 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.5000 0.33334(4) 0.7500 0.03805(18) Uani 1 2 d S . . N1 N 0.46364(19) 0.5125(3) 0.68512(17) 0.0448(8) Uani 1 1 d . . . C1 C 0.4248(3) 0.5571(3) 0.6052(2) 0.0523(10) Uani 1 1 d . . . C2 C 0.3982(3) 0.4527(4) 0.5540(3) 0.0763(14) Uani 1 1 d . . . H2A H 0.4485 0.4089 0.5625 0.092 Uiso 1 1 calc R . . H2B H 0.3695 0.4754 0.5004 0.092 Uiso 1 1 calc R . . H2C H 0.3598 0.4076 0.5665 0.092 Uiso 1 1 calc R . . C3 C 0.4898(3) 0.6223(4) 0.5855(3) 0.0795(15) Uani 1 1 d . . . H3A H 0.5013 0.6951 0.6107 0.095 Uiso 1 1 calc R . . H3B H 0.4662 0.6328 0.5303 0.095 Uiso 1 1 calc R . . H3C H 0.5425 0.5799 0.6033 0.095 Uiso 1 1 calc R . . C4 C 0.3438(3) 0.6294(4) 0.5845(3) 0.0810(15) Uani 1 1 d . . . H4A H 0.3053 0.5904 0.6002 0.097 Uiso 1 1 calc R . . H4B H 0.3156 0.6419 0.5293 0.097 Uiso 1 1 calc R . . H4C H 0.3599 0.7010 0.6109 0.097 Uiso 1 1 calc R . . C5 C 0.5000 0.5735(4) 0.7500 0.0450(13) Uani 1 2 d S . . C6 C 0.5000 0.7034(5) 0.7500 0.0664(18) Uani 1 2 d S . . H6A H 0.5161 0.7305 0.7110 0.080 Uiso 0.50 1 calc PR . . H6B H 0.5405 0.7305 0.8001 0.080 Uiso 0.50 1 calc PR . . H6C H 0.4434 0.7305 0.7388 0.080 Uiso 0.50 1 calc PR . . N2 N 0.5114(2) 0.1977(3) 0.8467(2) 0.0570(9) Uani 1 1 d . . . N3 N 0.3860(2) 0.2890(3) 0.7831(2) 0.0538(9) Uani 1 1 d . . . C7 C 0.5731(3) 0.1119(4) 0.8975(3) 0.0635(12) Uani 1 1 d . . . C8 C 0.6517(4) 0.1257(5) 0.8827(4) 0.109(2) Uani 1 1 d . . . H8A H 0.6356 0.1147 0.8284 0.131 Uiso 1 1 calc R . . H8B H 0.6945 0.0705 0.9125 0.131 Uiso 1 1 calc R . . H8C H 0.6750 0.2006 0.8977 0.131 Uiso 1 1 calc R . . C9 C 0.6023(4) 0.1296(5) 0.9842(3) 0.0973(18) Uani 1 1 d . . . H9A H 0.6244 0.2053 0.9983 0.117 Uiso 1 1 calc R . . H9B H 0.6467 0.0758 1.0130 0.117 Uiso 1 1 calc R . . H9C H 0.5542 0.1190 0.9959 0.117 Uiso 1 1 calc R . . C10 C 0.5422(4) -0.0101(4) 0.8743(4) 0.117(2) Uani 1 1 d . . . H10A H 0.4910 -0.0229 0.8809 0.141 Uiso 1 1 calc R . . H10B H 0.5865 -0.0619 0.9065 0.141 Uiso 1 1 calc R . . H10C H 0.5298 -0.0220 0.8208 0.141 Uiso 1 1 calc R . . C11 C 0.4316(3) 0.2145(3) 0.8391(3) 0.0544(11) Uani 1 1 d . . . C12 C 0.3972(3) 0.1568(4) 0.8911(3) 0.0826(15) Uani 1 1 d . . . H12A H 0.4143 0.0785 0.8981 0.099 Uiso 1 1 calc R . . H12B H 0.3354 0.1617 0.8672 0.099 Uiso 1 1 calc R . . H12C H 0.4203 0.1941 0.9408 0.099 Uiso 1 1 calc R . . C13 C 0.2990(2) 0.3303(4) 0.7653(2) 0.0565(10) Uani 1 1 d . . . C14 C 0.2796(3) 0.4175(5) 0.7021(3) 0.0879(17) Uani 1 1 d . . . H14A H 0.3187 0.4803 0.7224 0.105 Uiso 1 1 calc R . . H14B H 0.2215 0.4440 0.6843 0.105 Uiso 1 1 calc R . . H14C H 0.2864 0.3838 0.6596 0.105 Uiso 1 1 calc R . . C15 C 0.2303(3) 0.2382(5) 0.7330(3) 0.0968(19) Uani 1 1 d . . . H15A H 0.2370 0.1977 0.6925 0.116 Uiso 1 1 calc R . . H15B H 0.1742 0.2724 0.7122 0.116 Uiso 1 1 calc R . . H15C H 0.2365 0.1865 0.7738 0.116 Uiso 1 1 calc R . . C16 C 0.2932(4) 0.3902(5) 0.8333(3) 0.0997(18) Uani 1 1 d . . . H16A H 0.2990 0.3355 0.8724 0.120 Uiso 1 1 calc R . . H16B H 0.2384 0.4276 0.8153 0.120 Uiso 1 1 calc R . . H16C H 0.3386 0.4454 0.8549 0.120 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 Y1 0.0448(3) 0.0342(3) 0.0375(3) 0.000 0.0203(2) 0.000 N1 0.0566(18) 0.0383(18) 0.0400(19) 0.0022(15) 0.0218(15) 0.0029(15) C1 0.064(3) 0.049(2) 0.046(3) 0.014(2) 0.026(2) 0.008(2) C2 0.102(4) 0.076(3) 0.046(3) 0.016(3) 0.029(3) 0.007(3) C3 0.093(4) 0.086(4) 0.067(3) 0.022(3) 0.042(3) 0.001(3) C4 0.081(3) 0.087(4) 0.070(3) 0.022(3) 0.028(3) 0.028(3) C5 0.054(3) 0.035(3) 0.060(4) 0.000 0.037(3) 0.000 C6 0.090(5) 0.043(4) 0.071(5) 0.000 0.039(4) 0.000 N2 0.066(2) 0.051(2) 0.056(2) 0.0086(17) 0.0278(19) 0.0066(16) N3 0.057(2) 0.0451(19) 0.068(2) 0.0040(18) 0.0363(19) 0.0001(16) C7 0.076(3) 0.057(3) 0.055(3) 0.018(2) 0.026(3) 0.014(2) C8 0.104(4) 0.119(5) 0.112(5) 0.050(4) 0.055(4) 0.052(4) C9 0.120(5) 0.091(4) 0.061(3) 0.023(3) 0.021(3) 0.018(3) C10 0.176(6) 0.049(3) 0.104(5) 0.014(3) 0.040(4) 0.023(4) C11 0.065(3) 0.047(2) 0.056(3) -0.004(2) 0.031(2) -0.012(2) C12 0.089(3) 0.089(4) 0.078(3) 0.018(3) 0.045(3) -0.015(3) C13 0.049(2) 0.060(3) 0.066(3) 0.002(3) 0.031(2) -0.002(2) C14 0.073(3) 0.085(4) 0.112(5) 0.018(4) 0.047(3) 0.021(3) C15 0.067(3) 0.090(4) 0.139(6) -0.015(4) 0.051(4) -0.019(3) C16 0.105(4) 0.107(4) 0.103(5) -0.016(4) 0.060(4) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N3 2.379(3) . ? Y1 N3 2.379(3) 6_657 ? Y1 N2 2.388(3) 6_657 ? Y1 N2 2.388(3) . ? Y1 N1 2.389(3) 6_657 ? Y1 N1 2.389(3) . ? N1 C5 1.329(4) . ? N1 C1 1.471(5) . ? C1 C2 1.513(6) . ? C1 C4 1.533(6) . ? C1 C3 1.539(6) . ? C5 N1 1.329(4) 6_657 ? C5 C6 1.530(8) . ? N2 C11 1.336(5) . ? N2 C7 1.480(5) . ? N3 C11 1.341(5) . ? N3 C13 1.469(5) . ? C7 C8 1.515(7) . ? C7 C9 1.522(7) . ? C7 C10 1.529(7) . ? C11 C12 1.527(6) . ? C13 C14 1.508(6) . ? C13 C15 1.523(6) . ? C13 C16 1.523(6) . ? 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 N3 Y1 N3 154.66(16) . 6_657 ? N3 Y1 N2 105.41(12) . 6_657 ? N3 Y1 N2 56.00(12) 6_657 6_657 ? N3 Y1 N2 56.00(11) . . ? N3 Y1 N2 105.41(12) 6_657 . ? N2 Y1 N2 96.00(17) 6_657 . ? N3 Y1 N1 96.52(11) . 6_657 ? N3 Y1 N1 105.91(11) 6_657 6_657 ? N2 Y1 N1 155.20(11) 6_657 6_657 ? N2 Y1 N1 105.95(11) . 6_657 ? N3 Y1 N1 105.91(11) . . ? N3 Y1 N1 96.52(11) 6_657 . ? N2 Y1 N1 105.95(11) 6_657 . ? N2 Y1 N1 155.20(11) . . ? N1 Y1 N1 55.84(15) 6_657 . ? C5 N1 C1 126.2(3) . . ? C5 N1 Y1 94.8(3) . . ? C1 N1 Y1 138.7(3) . . ? N1 C1 C2 104.7(3) . . ? N1 C1 C4 114.4(4) . . ? C2 C1 C4 107.6(4) . . ? N1 C1 C3 112.7(3) . . ? C2 C1 C3 107.0(4) . . ? C4 C1 C3 109.9(4) . . ? N1 C5 N1 114.6(5) . 6_657 ? N1 C5 C6 122.7(2) . . ? N1 C5 C6 122.7(2) 6_657 . ? C11 N2 C7 125.6(4) . . ? C11 N2 Y1 95.1(2) . . ? C7 N2 Y1 139.1(3) . . ? C11 N3 C13 125.6(4) . . ? C11 N3 Y1 95.4(2) . . ? C13 N3 Y1 138.4(3) . . ? N2 C7 C8 104.4(4) . . ? N2 C7 C9 114.8(4) . . ? C8 C7 C9 107.3(4) . . ? N2 C7 C10 113.1(4) . . ? C8 C7 C10 105.9(5) . . ? C9 C7 C10 110.6(4) . . ? N2 C11 N3 113.5(4) . . ? N2 C11 C12 122.9(4) . . ? N3 C11 C12 123.6(4) . . ? N3 C13 C14 104.7(3) . . ? N3 C13 C15 113.1(4) . . ? C14 C13 C15 107.5(4) . . ? N3 C13 C16 113.7(4) . . ? C14 C13 C16 107.2(4) . . ? C15 C13 C16 110.2(4) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.490 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.067 #=== data_xala _database_code_depnum_ccdc_archive 'CCDC 272569' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H63 La N6' _chemical_formula_weight 646.77 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 16.9730(6) _cell_length_b 11.8555(4) _cell_length_c 19.0849(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.0650(10) _cell_angle_gamma 90.00 _cell_volume 3449.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7720 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 31.6 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.264 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6878 _exptl_absorpt_correction_T_max 0.7346 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX2 kappa' _diffrn_measurement_method 'Bruker APEX2' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34170 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 32.83 _reflns_number_total 5190 _reflns_number_gt 4884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.0181P)^2^+29.4086P] 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 5190 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.342 _refine_ls_restrained_S_all 1.342 _refine_ls_shift/su_max 0.004 _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 0.5000 0.66580(3) 0.7500 0.01750(8) Uani 1 2 d S . . N1 N 0.6200(2) 0.7207(3) 0.7119(2) 0.0271(7) Uani 1 1 d . . . N2 N 0.4915(3) 0.8095(3) 0.6473(2) 0.0297(7) Uani 1 1 d . . . C1 C 0.5723(3) 0.7927(3) 0.6545(2) 0.0264(8) Uani 1 1 d . . . C2 C 0.7085(3) 0.6774(4) 0.7321(2) 0.0262(8) Uani 1 1 d . . . C3 C 0.7160(3) 0.6199(5) 0.6623(3) 0.0384(10) Uani 1 1 d . . . H3A H 0.6692 0.5638 0.6390 0.046 Uiso 1 1 calc R . . H3B H 0.7731 0.5826 0.6807 0.046 Uiso 1 1 calc R . . H3C H 0.7104 0.6769 0.6233 0.046 Uiso 1 1 calc R . . C4 C 0.7227(3) 0.5868(4) 0.7921(3) 0.0375(10) Uani 1 1 d . . . H4A H 0.7186 0.6201 0.8374 0.045 Uiso 1 1 calc R . . H4B H 0.7810 0.5533 0.8086 0.045 Uiso 1 1 calc R . . H4C H 0.6778 0.5282 0.7694 0.045 Uiso 1 1 calc R . . C5 C 0.7792(3) 0.7669(5) 0.7686(3) 0.0436(12) Uani 1 1 d . . . H5A H 0.7744 0.8224 0.7289 0.052 Uiso 1 1 calc R . . H5B H 0.8372 0.7311 0.7895 0.052 Uiso 1 1 calc R . . H5C H 0.7717 0.8046 0.8109 0.052 Uiso 1 1 calc R . . C6 C 0.6075(3) 0.8483(4) 0.6020(3) 0.0352(10) Uani 1 1 d . . . H6A H 0.5921 0.8021 0.5552 0.042 Uiso 1 1 calc R . . H6B H 0.6714 0.8551 0.6302 0.042 Uiso 1 1 calc R . . H6C H 0.5815 0.9235 0.5867 0.042 Uiso 1 1 calc R . . C7 C 0.4253(3) 0.8893(4) 0.5953(3) 0.0313(9) Uani 1 1 d . . . C8 C 0.3994(4) 0.8714(5) 0.5087(3) 0.0440(12) Uani 1 1 d . . . H8A H 0.4467 0.8980 0.4967 0.053 Uiso 1 1 calc R . . H8B H 0.3456 0.9138 0.4776 0.053 Uiso 1 1 calc R . . H8C H 0.3891 0.7909 0.4963 0.053 Uiso 1 1 calc R . . C9 C 0.3444(4) 0.8690(5) 0.6080(3) 0.0452(13) Uani 1 1 d . . . H9A H 0.3223 0.7926 0.5909 0.054 Uiso 1 1 calc R . . H9B H 0.2990 0.9240 0.5779 0.054 Uiso 1 1 calc R . . H9C H 0.3595 0.8772 0.6636 0.054 Uiso 1 1 calc R . . C10 C 0.4533(4) 1.0138(4) 0.6189(3) 0.0500(14) Uani 1 1 d . . . H10A H 0.4704 1.0234 0.6747 0.060 Uiso 1 1 calc R . . H10B H 0.4041 1.0640 0.5889 0.060 Uiso 1 1 calc R . . H10C H 0.5032 1.0323 0.6080 0.060 Uiso 1 1 calc R . . N3 N 0.4643(2) 0.4736(3) 0.68522(18) 0.0220(6) Uani 1 1 d . . . C11 C 0.5000 0.4118(4) 0.7500 0.0185(9) Uani 1 2 d S . . C12 C 0.4253(3) 0.4323(3) 0.6040(2) 0.0217(7) Uani 1 1 d . . . C13 C 0.4007(3) 0.5401(4) 0.5547(2) 0.0326(9) Uani 1 1 d . . . H13A H 0.3576 0.5829 0.5651 0.039 Uiso 1 1 calc R . . H13B H 0.3755 0.5202 0.4993 0.039 Uiso 1 1 calc R . . H13C H 0.4533 0.5863 0.5682 0.039 Uiso 1 1 calc R . . C14 C 0.3414(3) 0.3643(4) 0.5815(3) 0.0332(9) Uani 1 1 d . . . H14A H 0.3545 0.2960 0.6136 0.040 Uiso 1 1 calc R . . H14B H 0.3173 0.3433 0.5264 0.040 Uiso 1 1 calc R . . H14C H 0.2984 0.4100 0.5903 0.040 Uiso 1 1 calc R . . C15 C 0.4913(3) 0.3674(4) 0.5840(3) 0.0358(10) Uani 1 1 d . . . H15A H 0.5474 0.4078 0.6052 0.043 Uiso 1 1 calc R . . H15B H 0.4685 0.3613 0.5272 0.043 Uiso 1 1 calc R . . H15C H 0.5001 0.2917 0.6069 0.043 Uiso 1 1 calc R . . C16 C 0.5000 0.2857(5) 0.7500 0.0243(11) Uani 1 2 d S . . H16A H 0.5509 0.2581 0.7961 0.029 Uiso 0.50 1 calc PR . . H16B H 0.5029 0.2581 0.7028 0.029 Uiso 0.50 1 calc PR . . H16C H 0.4461 0.2581 0.7511 0.029 Uiso 0.50 1 calc PR . . 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 0.02250(15) 0.01440(14) 0.01723(13) 0.000 0.01023(10) 0.000 N1 0.0294(18) 0.0266(18) 0.0272(16) 0.0022(13) 0.0143(14) 0.0000(14) N2 0.0360(19) 0.0247(18) 0.0294(17) 0.0074(13) 0.0152(15) 0.0041(14) C1 0.036(2) 0.0202(18) 0.0236(17) -0.0029(14) 0.0141(16) -0.0061(16) C2 0.0234(18) 0.0239(19) 0.0334(19) -0.0051(15) 0.0144(15) -0.0044(15) C3 0.041(3) 0.040(3) 0.038(2) -0.005(2) 0.021(2) 0.001(2) C4 0.033(2) 0.042(3) 0.037(2) 0.0070(19) 0.0144(19) 0.007(2) C5 0.032(2) 0.043(3) 0.054(3) -0.008(2) 0.016(2) -0.009(2) C6 0.043(2) 0.034(2) 0.032(2) 0.0007(17) 0.0194(19) -0.007(2) C7 0.045(3) 0.021(2) 0.0263(19) 0.0093(15) 0.0150(18) 0.0127(18) C8 0.059(3) 0.037(3) 0.030(2) 0.0109(19) 0.015(2) 0.008(2) C9 0.042(3) 0.050(3) 0.045(3) 0.019(2) 0.021(2) 0.018(2) C10 0.081(4) 0.024(2) 0.042(3) 0.006(2) 0.024(3) 0.012(3) N3 0.0314(17) 0.0156(15) 0.0178(14) -0.0017(10) 0.0097(12) -0.0008(12) C11 0.021(2) 0.012(2) 0.025(2) 0.000 0.0121(19) 0.000 C12 0.0248(18) 0.0218(18) 0.0184(16) -0.0043(12) 0.0096(14) -0.0006(14) C13 0.050(3) 0.027(2) 0.0201(17) -0.0016(14) 0.0142(17) -0.0006(19) C14 0.035(2) 0.037(2) 0.028(2) -0.0094(17) 0.0136(17) -0.0119(19) C15 0.036(2) 0.039(3) 0.036(2) -0.0118(19) 0.0187(19) 0.0017(19) C16 0.028(3) 0.022(3) 0.028(3) 0.000 0.016(2) 0.000 _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 N1 2.530(4) . ? La1 N1 2.530(4) 6_657 ? La1 N3 2.536(3) . ? La1 N3 2.536(3) 6_657 ? La1 N2 2.553(3) 6_657 ? La1 N2 2.553(3) . ? La1 C1 3.009(4) 6_657 ? La1 C1 3.009(4) . ? La1 C11 3.011(5) . ? N1 C1 1.343(5) . ? N1 C2 1.470(5) . ? N2 C1 1.332(6) . ? N2 C7 1.471(5) . ? C1 C6 1.523(6) . ? C2 C4 1.510(6) . ? C2 C5 1.523(6) . ? C2 C3 1.550(6) . ? C7 C9 1.516(7) . ? C7 C8 1.525(6) . ? C7 C10 1.555(7) . ? N3 C11 1.332(4) . ? N3 C12 1.476(5) . ? C11 N3 1.332(4) 6_657 ? C11 C16 1.496(7) . ? C12 C14 1.526(6) . ? C12 C13 1.532(6) . ? C12 C15 1.538(6) . ? 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 N1 La1 N1 150.17(17) . 6_657 ? N1 La1 N3 98.14(11) . . ? N1 La1 N3 108.73(11) 6_657 . ? N1 La1 N3 108.73(11) . 6_657 ? N1 La1 N3 98.14(11) 6_657 6_657 ? N3 La1 N3 52.03(14) . 6_657 ? N1 La1 N2 105.53(12) . 6_657 ? N1 La1 N2 52.32(12) 6_657 6_657 ? N3 La1 N2 153.48(11) . 6_657 ? N3 La1 N2 107.73(11) 6_657 6_657 ? N1 La1 N2 52.32(12) . . ? N1 La1 N2 105.53(12) 6_657 . ? N3 La1 N2 107.73(11) . . ? N3 La1 N2 153.48(11) 6_657 . ? N2 La1 N2 96.29(17) 6_657 . ? N1 La1 C1 129.74(12) . 6_657 ? N1 La1 C1 26.27(12) 6_657 6_657 ? N3 La1 C1 132.12(11) . 6_657 ? N3 La1 C1 103.18(11) 6_657 6_657 ? N2 La1 C1 26.10(12) 6_657 6_657 ? N2 La1 C1 103.34(11) . 6_657 ? N1 La1 C1 26.27(12) . . ? N1 La1 C1 129.74(12) 6_657 . ? N3 La1 C1 103.18(11) . . ? N3 La1 C1 132.12(11) 6_657 . ? N2 La1 C1 103.34(12) 6_657 . ? N2 La1 C1 26.10(12) . . ? C1 La1 C1 120.00(16) 6_657 . ? N1 La1 C11 104.92(8) . . ? N1 La1 C11 104.92(8) 6_657 . ? N3 La1 C11 26.02(7) . . ? N3 La1 C11 26.02(7) 6_657 . ? N2 La1 C11 131.86(9) 6_657 . ? N2 La1 C11 131.86(9) . . ? C1 La1 C11 120.00(8) 6_657 . ? C1 La1 C11 120.00(8) . . ? C1 N1 C2 128.0(4) . . ? C1 N1 La1 97.2(3) . . ? C2 N1 La1 133.9(3) . . ? C1 N2 C7 127.7(4) . . ? C1 N2 La1 96.5(2) . . ? C7 N2 La1 135.8(3) . . ? N2 C1 N1 113.8(4) . . ? N2 C1 C6 123.4(4) . . ? N1 C1 C6 122.8(4) . . ? N2 C1 La1 57.4(2) . . ? N1 C1 La1 56.5(2) . . ? C6 C1 La1 175.3(3) . . ? N1 C2 C4 104.6(3) . . ? N1 C2 C5 112.7(4) . . ? C4 C2 C5 108.5(4) . . ? N1 C2 C3 112.9(4) . . ? C4 C2 C3 107.0(4) . . ? C5 C2 C3 110.7(4) . . ? N2 C7 C9 105.4(4) . . ? N2 C7 C8 114.4(4) . . ? C9 C7 C8 107.5(4) . . ? N2 C7 C10 111.7(4) . . ? C9 C7 C10 106.7(4) . . ? C8 C7 C10 110.6(4) . . ? C11 N3 C12 127.2(3) . . ? C11 N3 La1 97.3(2) . . ? C12 N3 La1 135.3(2) . . ? N3 C11 N3 113.3(4) 6_657 . ? N3 C11 C16 123.3(2) 6_657 . ? N3 C11 C16 123.3(2) . . ? N3 C11 La1 56.7(2) 6_657 . ? N3 C11 La1 56.7(2) . . ? C16 C11 La1 180.000(1) . . ? N3 C12 C14 113.7(3) . . ? N3 C12 C13 104.1(3) . . ? C14 C12 C13 107.4(4) . . ? N3 C12 C15 112.8(3) . . ? C14 C12 C15 111.0(4) . . ? C13 C12 C15 107.3(4) . . ? _diffrn_measured_fraction_theta_max 0.809 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.117 _refine_diff_density_min -1.816 _refine_diff_density_rms 0.129 #=== data_tobe _database_code_depnum_ccdc_archive 'CCDC 272570' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H63 Ce N6' _chemical_formula_weight 647.98 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 17.306(6) _cell_length_b 11.928(6) _cell_length_c 19.182(9) _cell_angle_alpha 90.00 _cell_angle_beta 115.953(11) _cell_angle_gamma 90.00 _cell_volume 3560(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.1 _exptl_crystal_description multifaceted _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 1.303 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7450 _exptl_absorpt_correction_T_max 0.7625 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12741 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.35 _reflns_number_total 4202 _reflns_number_gt 3298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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. There is an 80/20 disorder in two of the ligands. The minor component atoms are labelled with prime designations. Two atoms (C10 and C13) are in common with both partial sets. ; _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^)+(0.0168P)^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 4202 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0361 _refine_ls_wR_factor_gt 0.0351 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _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 Ce1 Ce 0.0000 0.163109(11) 0.2500 0.04575(5) Uani 1 2 d S . . N1 N -0.03481(8) -0.02523(11) 0.18561(7) 0.0522(3) Uani 1 1 d . A . C1 C -0.09835(14) 0.03872(17) 0.05626(10) 0.0841(6) Uani 1 1 d . A . H1A H -0.1391 0.0806 0.0672 0.101 Uiso 1 1 calc R . . H1B H -0.1236 0.0189 0.0023 0.101 Uiso 1 1 calc R . . H1C H -0.0481 0.0836 0.0683 0.101 Uiso 1 1 calc R . . C2 C -0.15521(13) -0.13505(18) 0.08414(12) 0.0885(7) Uani 1 1 d . A . H2A H -0.1413 -0.2043 0.1125 0.106 Uiso 1 1 calc R . . H2B H -0.1814 -0.1507 0.0295 0.106 Uiso 1 1 calc R . . H2C H -0.1945 -0.0930 0.0970 0.106 Uiso 1 1 calc R . . C3 C -0.01011(14) -0.13206(18) 0.08458(12) 0.0890(7) Uani 1 1 d . A . H3A H 0.0430 -0.0914 0.1026 0.107 Uiso 1 1 calc R . . H3B H -0.0338 -0.1409 0.0293 0.107 Uiso 1 1 calc R . . H3C H 0.0002 -0.2045 0.1088 0.107 Uiso 1 1 calc R . . C4 C -0.07347(11) -0.06722(14) 0.10526(10) 0.0583(5) Uani 1 1 d . . . C5 C 0.0000 -0.08613(18) 0.2500 0.0502(6) Uani 1 2 d S . . C6 C 0.0000 -0.2129(2) 0.2500 0.0687(7) Uani 1 2 d S A . H6A H 0.0400 -0.2397 0.2315 0.082 Uiso 0.50 1 calc PR . . H6B H -0.0566 -0.2397 0.2167 0.082 Uiso 0.50 1 calc PR . . H6C H 0.0166 -0.2397 0.3018 0.082 Uiso 0.50 1 calc PR . . C10 C -0.20366(11) 0.17490(17) 0.26680(12) 0.0649(5) Uani 1 1 d . . . C13 C 0.07467(17) 0.38778(17) 0.40091(13) 0.0772(6) Uani 1 1 d . . . N2 N -0.11544(13) 0.21650(15) 0.28871(14) 0.0543(5) Uani 0.8164(18) 1 d P A 1 N3 N 0.00869(13) 0.30574(15) 0.35024(11) 0.0598(5) Uani 0.8164(18) 1 d P A 1 C7 C -0.21941(18) 0.0881(2) 0.20671(16) 0.0829(8) Uani 0.8164(18) 1 d P A 1 H7A H -0.2763 0.0584 0.1898 0.099 Uiso 0.8164(18) 1 calc PR A 1 H7B H -0.1782 0.0288 0.2281 0.099 Uiso 0.8164(18) 1 calc PR A 1 H7C H -0.2139 0.1210 0.1634 0.099 Uiso 0.8164(18) 1 calc PR A 1 C8 C -0.2717(3) 0.2671(4) 0.2333(2) 0.0980(13) Uani 0.8164(18) 1 d P A 1 H8A H -0.3280 0.2339 0.2116 0.118 Uiso 0.8164(18) 1 calc PR A 1 H8B H -0.2635 0.3067 0.1935 0.118 Uiso 0.8164(18) 1 calc PR A 1 H8C H -0.2664 0.3183 0.2737 0.118 Uiso 0.8164(18) 1 calc PR A 1 C9 C -0.2108(2) 0.1176(3) 0.33656(17) 0.0972(10) Uani 0.8164(18) 1 d P A 1 H9A H -0.2040 0.1729 0.3752 0.117 Uiso 0.8164(18) 1 calc PR A 1 H9B H -0.1668 0.0618 0.3584 0.117 Uiso 0.8164(18) 1 calc PR A 1 H9C H -0.2662 0.0828 0.3191 0.117 Uiso 0.8164(18) 1 calc PR A 1 C11 C -0.07034(15) 0.29014(17) 0.34318(12) 0.0545(6) Uani 0.8164(18) 1 d P A 1 C12 C -0.10567(17) 0.34792(19) 0.39358(14) 0.0833(8) Uani 0.8164(18) 1 d P A 1 H12A H -0.0899 0.3060 0.4406 0.100 Uiso 0.8164(18) 1 calc PR A 1 H12B H -0.1672 0.3520 0.3662 0.100 Uiso 0.8164(18) 1 calc PR A 1 H12C H -0.0824 0.4223 0.4059 0.100 Uiso 0.8164(18) 1 calc PR A 1 C14 C 0.0995(2) 0.3705(4) 0.4869(2) 0.0988(12) Uani 0.8164(18) 1 d P A 1 H14A H 0.0511 0.3873 0.4970 0.119 Uiso 0.8164(18) 1 calc PR A 1 H14B H 0.1464 0.4193 0.5170 0.119 Uiso 0.8164(18) 1 calc PR A 1 H14C H 0.1165 0.2940 0.5006 0.119 Uiso 0.8164(18) 1 calc PR A 1 C15 C 0.14996(19) 0.3708(3) 0.38642(18) 0.1078(11) Uani 0.8164(18) 1 d P A 1 H15A H 0.1697 0.2949 0.3989 0.129 Uiso 0.8164(18) 1 calc PR A 1 H15B H 0.1948 0.4213 0.4181 0.129 Uiso 0.8164(18) 1 calc PR A 1 H15C H 0.1349 0.3850 0.3327 0.129 Uiso 0.8164(18) 1 calc PR A 1 C16 C 0.0416(3) 0.5089(3) 0.3788(3) 0.1164(13) Uani 0.8164(18) 1 d P A 1 H16A H 0.0190 0.5181 0.3236 0.140 Uiso 0.8164(18) 1 calc PR A 1 H16B H 0.0880 0.5606 0.4042 0.140 Uiso 0.8164(18) 1 calc PR A 1 H16C H -0.0029 0.5233 0.3947 0.140 Uiso 0.8164(18) 1 calc PR A 1 N2' N 0.1457(5) 0.2107(6) 0.2695(6) 0.050(2) Uani 0.1836(18) 1 d P . 2 N3' N 0.0944(6) 0.2959(6) 0.3444(4) 0.059(2) Uani 0.1836(18) 1 d P A 2 C7' C -0.2882(8) 0.1079(12) 0.1928(8) 0.099(5) Uani 0.1836(18) 1 d P A 2 H7D H -0.3162 0.0590 0.2144 0.119 Uiso 0.1836(18) 1 calc PR A 2 H7E H -0.2670 0.0648 0.1626 0.119 Uiso 0.1836(18) 1 calc PR A 2 H7F H -0.3286 0.1626 0.1603 0.119 Uiso 0.1836(18) 1 calc PR A 2 C8' C -0.1598(8) 0.0867(12) 0.3182(7) 0.093(4) Uani 0.1836(18) 1 d P A 2 H8D H -0.1086 0.1155 0.3599 0.112 Uiso 0.1836(18) 1 calc PR A 2 H8E H -0.1446 0.0301 0.2908 0.112 Uiso 0.1836(18) 1 calc PR A 2 H8F H -0.1963 0.0547 0.3388 0.112 Uiso 0.1836(18) 1 calc PR A 2 C9' C -0.2467(13) 0.2567(16) 0.2870(11) 0.112(6) Uani 0.1836(18) 1 d P A 2 H9D H -0.2400 0.2430 0.3387 0.135 Uiso 0.1836(18) 1 calc PR A 2 H9E H -0.3066 0.2550 0.2516 0.135 Uiso 0.1836(18) 1 calc PR A 2 H9F H -0.2233 0.3289 0.2849 0.135 Uiso 0.1836(18) 1 calc PR A 2 C11' C 0.1617(6) 0.2827(8) 0.3276(6) 0.059(3) Uani 0.1836(18) 1 d P A 2 C12' C 0.2463(7) 0.3415(10) 0.3728(8) 0.100(4) Uani 0.1836(18) 1 d P A 2 H12D H 0.2419 0.4180 0.3560 0.120 Uiso 0.1836(18) 1 calc PR A 2 H12E H 0.2906 0.3044 0.3642 0.120 Uiso 0.1836(18) 1 calc PR A 2 H12F H 0.2603 0.3395 0.4271 0.120 Uiso 0.1836(18) 1 calc PR A 2 C14' C 0.1505(10) 0.3562(19) 0.4873(10) 0.102(6) Uani 0.1836(18) 1 d P A 2 H14D H 0.1336 0.3811 0.5263 0.123 Uiso 0.1836(18) 1 calc PR A 2 H14E H 0.2030 0.3926 0.4949 0.123 Uiso 0.1836(18) 1 calc PR A 2 H14F H 0.1590 0.2765 0.4913 0.123 Uiso 0.1836(18) 1 calc PR A 2 C15' C 0.0956(15) 0.5032(15) 0.3727(15) 0.134(8) Uani 0.1836(18) 1 d P A 2 H15D H 0.0786 0.5000 0.3180 0.161 Uiso 0.1836(18) 1 calc PR A 2 H15E H 0.1561 0.5177 0.3996 0.161 Uiso 0.1836(18) 1 calc PR A 2 H15F H 0.0646 0.5622 0.3835 0.161 Uiso 0.1836(18) 1 calc PR A 2 C16' C 0.0029(10) 0.3623(14) 0.3895(9) 0.115(5) Uani 0.1836(18) 1 d P A 2 H16D H -0.0062 0.3821 0.4339 0.139 Uiso 0.1836(18) 1 calc PR A 2 H16E H -0.0048 0.2830 0.3808 0.139 Uiso 0.1836(18) 1 calc PR A 2 H16F H -0.0378 0.4015 0.3448 0.139 Uiso 0.1836(18) 1 calc PR A 2 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 Ce1 0.05684(9) 0.03898(7) 0.04686(8) 0.000 0.02769(6) 0.000 N1 0.0678(9) 0.0459(8) 0.0446(8) -0.0027(7) 0.0261(7) -0.0021(7) C1 0.1172(17) 0.0776(15) 0.0496(12) -0.0069(11) 0.0291(12) -0.0020(12) C2 0.0866(15) 0.0981(17) 0.0741(14) -0.0240(12) 0.0291(12) -0.0269(12) C3 0.1085(17) 0.0954(17) 0.0778(14) -0.0209(12) 0.0544(13) 0.0025(13) C4 0.0716(12) 0.0539(11) 0.0523(11) -0.0108(9) 0.0296(10) -0.0061(9) C5 0.0560(14) 0.0406(13) 0.0659(17) 0.000 0.0377(13) 0.000 C6 0.092(2) 0.0458(14) 0.0772(19) 0.000 0.0447(17) 0.000 C10 0.0603(11) 0.0631(12) 0.0797(13) 0.0035(12) 0.0383(10) 0.0078(10) C13 0.0991(18) 0.0623(13) 0.0661(15) -0.0228(11) 0.0322(14) -0.0204(12) N2 0.0589(12) 0.0541(11) 0.0547(13) -0.0035(11) 0.0294(11) 0.0038(9) N3 0.0764(15) 0.0514(12) 0.0570(12) -0.0133(9) 0.0341(11) -0.0079(9) C7 0.0650(18) 0.087(2) 0.097(2) -0.0180(17) 0.0357(17) -0.0192(15) C8 0.073(2) 0.107(3) 0.116(3) 0.026(3) 0.043(3) 0.0284(19) C9 0.100(2) 0.103(2) 0.107(2) 0.0188(19) 0.062(2) -0.0043(18) C11 0.0729(16) 0.0457(12) 0.0509(14) 0.0054(11) 0.0326(13) 0.0141(11) C12 0.0993(18) 0.0806(18) 0.0788(17) -0.0159(15) 0.0470(15) 0.0182(15) C14 0.109(3) 0.101(3) 0.069(2) -0.0282(18) 0.023(3) -0.015(3) C15 0.108(2) 0.114(3) 0.109(2) -0.056(2) 0.055(2) -0.0538(19) C16 0.174(4) 0.0552(19) 0.119(3) -0.0150(19) 0.064(3) -0.028(3) N2' 0.051(5) 0.046(4) 0.059(6) -0.005(5) 0.029(5) 0.000(4) N3' 0.085(6) 0.043(4) 0.048(5) -0.005(4) 0.029(5) 0.006(4) C7' 0.067(8) 0.105(10) 0.099(10) -0.009(8) 0.012(8) -0.034(8) C8' 0.083(9) 0.128(12) 0.089(9) 0.012(9) 0.055(8) -0.009(8) C9' 0.122(17) 0.067(10) 0.18(2) 0.006(14) 0.092(18) 0.001(10) C11' 0.048(6) 0.053(6) 0.065(7) 0.031(6) 0.015(5) -0.004(4) C12' 0.062(7) 0.108(10) 0.121(10) -0.038(9) 0.031(7) -0.027(7) C14' 0.107(13) 0.113(12) 0.061(8) -0.011(8) 0.012(11) 0.011(12) C15' 0.20(2) 0.060(9) 0.205(19) 0.000(10) 0.147(19) -0.008(12) C16' 0.101(12) 0.118(13) 0.109(12) -0.048(10) 0.030(10) 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 Ce1 N3' 2.422(8) . ? Ce1 N3' 2.422(8) 6_556 ? Ce1 N2' 2.448(8) 6_556 ? Ce1 N2' 2.448(8) . ? Ce1 N2 2.4993(19) . ? Ce1 N2 2.4993(19) 6_556 ? Ce1 N1 2.5068(16) . ? Ce1 N1 2.5068(16) 6_556 ? Ce1 N3 2.522(2) . ? Ce1 N3 2.522(2) 6_556 ? Ce1 C11' 2.904(9) . ? Ce1 C11' 2.904(9) 6_556 ? N1 C5 1.3284(17) . ? N1 C4 1.474(2) . ? C1 C4 1.520(2) . ? C2 C4 1.523(2) . ? C3 C4 1.529(2) . ? C5 N1 1.3284(17) 6_556 ? C5 C6 1.512(3) . ? C10 C9' 1.382(19) . ? C10 C8' 1.414(13) . ? C10 N2 1.481(3) . ? C10 C7 1.483(3) . ? C10 N2' 1.512(8) 6_556 ? C10 C8 1.532(4) . ? C10 C9 1.555(3) . ? C10 C7' 1.725(11) . ? C13 C16' 1.203(15) . ? C13 C15 1.461(4) . ? C13 N3 1.495(3) . ? C13 C14 1.525(5) . ? C13 C16 1.544(5) . ? C13 C15' 1.578(17) . ? C13 C14' 1.645(17) . ? C13 N3' 1.678(8) . ? N2 C11 1.326(3) . ? N3 C11 1.327(3) . ? C11 C12 1.517(3) . ? N2' C11' 1.336(13) . ? N2' C10 1.512(8) 6_556 ? N3' C11' 1.348(12) . ? C11' C12' 1.509(13) . ? 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 N3' Ce1 N3' 98.3(4) . 6_556 ? N3' Ce1 N2' 106.0(3) . 6_556 ? N3' Ce1 N2' 54.7(3) 6_556 6_556 ? N3' Ce1 N2' 54.7(3) . . ? N3' Ce1 N2' 106.0(3) 6_556 . ? N2' Ce1 N2' 153.2(4) 6_556 . ? N3' Ce1 N2 88.6(2) . . ? N3' Ce1 N2 72.0(2) 6_556 . ? N2' Ce1 N2 23.5(2) 6_556 . ? N2' Ce1 N2 143.06(19) . . ? N3' Ce1 N2 72.0(2) . 6_556 ? N3' Ce1 N2 88.6(2) 6_556 6_556 ? N2' Ce1 N2 143.06(19) 6_556 6_556 ? N2' Ce1 N2 23.5(2) . 6_556 ? N2 Ce1 N2 150.48(9) . 6_556 ? N3' Ce1 N1 153.18(19) . . ? N3' Ce1 N1 106.23(18) 6_556 . ? N2' Ce1 N1 97.1(2) 6_556 . ? N2' Ce1 N1 106.99(19) . . ? N2 Ce1 N1 108.89(6) . . ? N2 Ce1 N1 97.64(6) 6_556 . ? N3' Ce1 N1 106.23(18) . 6_556 ? N3' Ce1 N1 153.18(19) 6_556 6_556 ? N2' Ce1 N1 106.99(19) 6_556 6_556 ? N2' Ce1 N1 97.1(2) . 6_556 ? N2 Ce1 N1 97.64(6) . 6_556 ? N2 Ce1 N1 108.89(6) 6_556 6_556 ? N1 Ce1 N1 52.68(7) . 6_556 ? N3' Ce1 N3 36.2(2) . . ? N3' Ce1 N3 85.69(19) 6_556 . ? N2' Ce1 N3 71.0(2) 6_556 . ? N2' Ce1 N3 90.8(2) . . ? N2 Ce1 N3 52.44(7) . . ? N2 Ce1 N3 105.42(7) 6_556 . ? N1 Ce1 N3 154.35(5) . . ? N1 Ce1 N3 107.91(6) 6_556 . ? N3' Ce1 N3 85.69(19) . 6_556 ? N3' Ce1 N3 36.2(2) 6_556 6_556 ? N2' Ce1 N3 90.8(2) 6_556 6_556 ? N2' Ce1 N3 71.0(2) . 6_556 ? N2 Ce1 N3 105.42(7) . 6_556 ? N2 Ce1 N3 52.44(7) 6_556 6_556 ? N1 Ce1 N3 107.91(6) . 6_556 ? N1 Ce1 N3 154.35(5) 6_556 6_556 ? N3 Ce1 N3 95.16(9) . 6_556 ? N3' Ce1 C11' 27.5(3) . . ? N3' Ce1 C11' 104.2(3) 6_556 . ? N2' Ce1 C11' 131.4(3) 6_556 . ? N2' Ce1 C11' 27.2(3) . . ? N2 Ce1 C11' 116.0(2) . . ? N2 Ce1 C11' 46.4(2) 6_556 . ? N1 Ce1 C11' 131.5(2) . . ? N1 Ce1 C11' 102.59(17) 6_556 . ? N3 Ce1 C11' 63.6(2) . . ? N3 Ce1 C11' 77.40(18) 6_556 . ? N3' Ce1 C11' 104.2(3) . 6_556 ? N3' Ce1 C11' 27.5(3) 6_556 6_556 ? N2' Ce1 C11' 27.2(3) 6_556 6_556 ? N2' Ce1 C11' 131.4(3) . 6_556 ? N2 Ce1 C11' 46.4(2) . 6_556 ? N2 Ce1 C11' 116.0(2) 6_556 6_556 ? N1 Ce1 C11' 102.59(17) . 6_556 ? N1 Ce1 C11' 131.5(2) 6_556 6_556 ? N3 Ce1 C11' 77.40(18) . 6_556 ? N3 Ce1 C11' 63.6(2) 6_556 6_556 ? C11' Ce1 C11' 121.2(4) . 6_556 ? C5 N1 C4 126.89(14) . . ? C5 N1 Ce1 96.81(11) . . ? C4 N1 Ce1 136.14(10) . . ? N1 C4 C1 103.91(14) . . ? N1 C4 C2 113.74(15) . . ? C1 C4 C2 107.36(16) . . ? N1 C4 C3 113.22(15) . . ? C1 C4 C3 107.53(16) . . ? C2 C4 C3 110.51(16) . . ? N1 C5 N1 113.7(2) 6_556 . ? N1 C5 C6 123.15(10) 6_556 . ? N1 C5 C6 123.15(10) . . ? N1 C5 Ce1 56.85(10) 6_556 . ? N1 C5 Ce1 56.85(10) . . ? C6 C5 Ce1 180.0 . . ? C9' C10 C8' 121.3(9) . . ? C9' C10 N2 107.4(8) . . ? C8' C10 N2 83.0(5) . . ? C9' C10 C7 140.6(8) . . ? C8' C10 C7 83.3(6) . . ? N2 C10 C7 105.69(17) . . ? C9' C10 N2' 118.6(8) . 6_556 ? C8' C10 N2' 105.6(6) . 6_556 ? N2 C10 N2' 39.3(3) . 6_556 ? C7 C10 N2' 76.8(4) . 6_556 ? C9' C10 C8 37.0(7) . . ? C8' C10 C8 155.0(6) . . ? N2 C10 C8 112.8(2) . . ? C7 C10 C8 109.2(2) . . ? N2' C10 C8 98.5(4) 6_556 . ? C9' C10 C9 79.2(8) . . ? C8' C10 C9 45.1(5) . . ? N2 C10 C9 111.34(19) . . ? C7 C10 C9 107.8(2) . . ? N2' C10 C9 147.1(4) 6_556 . ? C8 C10 C9 109.9(2) . . ? C9' C10 C7' 101.0(10) . . ? C8' C10 C7' 103.4(7) . . ? N2 C10 C7' 141.9(5) . . ? C7 C10 C7' 40.2(5) . . ? N2' C10 C7' 104.3(6) 6_556 . ? C8 C10 C7' 76.5(5) . . ? C9 C10 C7' 98.4(5) . . ? C16' C13 C15 150.2(8) . . ? C16' C13 N3 44.1(7) . . ? C15 C13 N3 106.06(19) . . ? C16' C13 C14 86.7(8) . . ? C15 C13 C14 109.5(2) . . ? N3 C13 C14 112.8(2) . . ? C16' C13 C16 87.5(8) . . ? C15 C13 C16 109.4(2) . . ? N3 C13 C16 110.3(2) . . ? C14 C13 C16 108.6(3) . . ? C16' C13 C15' 122.1(11) . . ? C15 C13 C15' 72.5(7) . . ? N3 C13 C15' 124.9(10) . . ? C14 C13 C15' 119.3(9) . . ? C16 C13 C15' 37.1(6) . . ? C16' C13 C14' 115.5(10) . . ? C15 C13 C14' 77.0(6) . . ? N3 C13 C14' 123.4(8) . . ? C14 C13 C14' 32.5(6) . . ? C16 C13 C14' 121.9(8) . . ? C15' C13 C14' 110.1(13) . . ? C16' C13 N3' 101.8(8) . . ? C15 C13 N3' 48.4(3) . . ? N3 C13 N3' 57.7(3) . . ? C14 C13 N3' 124.7(3) . . ? C16 C13 N3' 126.1(3) . . ? C15' C13 N3' 102.0(7) . . ? C14' C13 N3' 101.7(7) . . ? C11 N2 C10 128.60(19) . . ? C11 N2 Ce1 97.56(13) . . ? C10 N2 Ce1 133.58(14) . . ? C11 N3 C13 128.2(2) . . ? C11 N3 Ce1 96.47(14) . . ? C13 N3 Ce1 135.32(16) . . ? N3 C11 N2 113.46(19) . . ? N3 C11 C12 123.8(2) . . ? N2 C11 C12 122.7(2) . . ? N3 C11 Ce1 57.26(12) . . ? N2 C11 Ce1 56.26(11) . . ? C12 C11 Ce1 176.29(15) . . ? C11' N2' C10 128.9(7) . 6_556 ? C11' N2' Ce1 95.7(6) . . ? C10 N2' Ce1 135.3(5) 6_556 . ? C11' N3' C13 132.3(8) . . ? C11' N3' Ce1 96.6(6) . . ? C13 N3' Ce1 130.5(5) . . ? N2' C11' N3' 112.9(8) . . ? N2' C11' C12' 124.9(10) . . ? N3' C11' C12' 122.1(10) . . ? N2' C11' Ce1 57.0(5) . . ? N3' C11' Ce1 56.0(5) . . ? C12' C11' Ce1 176.2(8) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.372 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.037 #=== data_niod _database_code_depnum_ccdc_archive 'CCDC 272571' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H63 N6 Nd' _chemical_formula_weight 652.10 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 17.2186(11) _cell_length_b 11.8892(7) _cell_length_c 19.2018(12) _cell_angle_alpha 90.00 _cell_angle_beta 116.5880(10) _cell_angle_gamma 90.00 _cell_volume 3515.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6837 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description rods _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 1.502 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5848 _exptl_absorpt_correction_T_max 0.7532 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24924 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4115 _reflns_number_gt 3456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.0280P)^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 4115 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0504 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.004 _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 Nd1 Nd 0.5000 0.665313(13) 0.7500 0.03809(6) Uani 1 2 d S . . N1 N 0.46345(11) 0.47888(14) 0.68548(9) 0.0450(4) Uani 1 1 d . . . C1 C 0.42452(15) 0.43700(19) 0.60455(12) 0.0514(5) Uani 1 1 d . . . C2 C 0.5000 0.4182(2) 0.7500 0.0438(7) Uani 1 2 d S . . C3 C 0.34219(18) 0.3674(2) 0.58253(16) 0.0769(8) Uani 1 1 d . . . H3A H 0.3571 0.2966 0.6093 0.092 Uiso 1 1 calc R . . H3B H 0.3145 0.3545 0.5273 0.092 Uiso 1 1 calc R . . H3C H 0.3032 0.4074 0.5971 0.092 Uiso 1 1 calc R . . C4 C 0.39839(19) 0.5419(2) 0.55491(13) 0.0708(8) Uani 1 1 d . . . H4A H 0.3558 0.5825 0.5643 0.085 Uiso 1 1 calc R . . H4B H 0.3743 0.5213 0.5009 0.085 Uiso 1 1 calc R . . H4C H 0.4485 0.5886 0.5680 0.085 Uiso 1 1 calc R . . C5 C 0.48958(19) 0.3733(3) 0.58512(16) 0.0758(8) Uani 1 1 d . . . H5A H 0.5428 0.4151 0.6037 0.091 Uiso 1 1 calc R . . H5B H 0.4659 0.3639 0.5297 0.091 Uiso 1 1 calc R . . H5C H 0.5009 0.3008 0.6097 0.091 Uiso 1 1 calc R . . C6 C 0.5000 0.2908(3) 0.7500 0.0626(9) Uani 1 2 d S . . H6A H 0.5533 0.2638 0.7913 0.075 Uiso 0.50 1 calc PR . . H6B H 0.4949 0.2638 0.7010 0.075 Uiso 0.50 1 calc PR . . H6C H 0.4518 0.2638 0.7577 0.075 Uiso 0.50 1 calc PR . . N2 N 0.50991(12) 0.80460(15) 0.84993(10) 0.0513(5) Uani 1 1 d . . . N3 N 0.38441(11) 0.71439(15) 0.78713(10) 0.0482(4) Uani 1 1 d . . . C7 C 0.57366(17) 0.8881(2) 0.90058(14) 0.0626(7) Uani 1 1 d . . . C8 C 0.43071(15) 0.78815(18) 0.84267(12) 0.0476(5) Uani 1 1 d . . . C9 C 0.29678(14) 0.6732(2) 0.76783(14) 0.0536(5) Uani 1 1 d . . . C10 C 0.6032(2) 0.8695(3) 0.98712(15) 0.0858(9) Uani 1 1 d . . . H10A H 0.5561 0.8853 0.9994 0.103 Uiso 1 1 calc R . . H10B H 0.6510 0.9187 1.0165 0.103 Uiso 1 1 calc R . . H10C H 0.6213 0.7928 1.0001 0.103 Uiso 1 1 calc R . . C11 C 0.6525(2) 0.8712(3) 0.8862(2) 0.0968(11) Uani 1 1 d . . . H11A H 0.6726 0.7951 0.8985 0.116 Uiso 1 1 calc R . . H11B H 0.6978 0.9219 0.9185 0.116 Uiso 1 1 calc R . . H11C H 0.6372 0.8860 0.8324 0.116 Uiso 1 1 calc R . . C12 C 0.5422(3) 1.0095(2) 0.8785(2) 0.1040(11) Uani 1 1 d . . . H12A H 0.5218 1.0196 0.8235 0.125 Uiso 1 1 calc R . . H12B H 0.5894 1.0603 0.9062 0.125 Uiso 1 1 calc R . . H12C H 0.4959 1.0244 0.8920 0.125 Uiso 1 1 calc R . . C13 C 0.39544(19) 0.8450(2) 0.89314(16) 0.0730(8) Uani 1 1 d . . . H13A H 0.4148 0.8052 0.9415 0.088 Uiso 1 1 calc R . . H13B H 0.3331 0.8448 0.8667 0.088 Uiso 1 1 calc R . . H13C H 0.4160 0.9212 0.9032 0.088 Uiso 1 1 calc R . . C14 C 0.27861(18) 0.5860(3) 0.70447(17) 0.0776(8) Uani 1 1 d . . . H14A H 0.2826 0.6207 0.6610 0.093 Uiso 1 1 calc R . . H14B H 0.2213 0.5560 0.6878 0.093 Uiso 1 1 calc R . . H14C H 0.3204 0.5264 0.7246 0.093 Uiso 1 1 calc R . . C15 C 0.2899(2) 0.6139(3) 0.83537(18) 0.0874(9) Uani 1 1 d . . . H15A H 0.3371 0.5617 0.8592 0.105 Uiso 1 1 calc R . . H15B H 0.2358 0.5741 0.8162 0.105 Uiso 1 1 calc R . . H15C H 0.2926 0.6686 0.8731 0.105 Uiso 1 1 calc R . . C16 C 0.22677(17) 0.7636(3) 0.73324(18) 0.0847(9) Uani 1 1 d . . . H16A H 0.2326 0.8165 0.7731 0.102 Uiso 1 1 calc R . . H16B H 0.1705 0.7291 0.7127 0.102 Uiso 1 1 calc R . . H16C H 0.2333 0.8021 0.6922 0.102 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 Nd1 0.04714(10) 0.03147(8) 0.03938(8) 0.000 0.02266(6) 0.000 N1 0.0556(10) 0.0361(9) 0.0415(9) -0.0031(7) 0.0200(8) -0.0021(8) C1 0.0610(14) 0.0481(12) 0.0459(12) -0.0115(10) 0.0247(10) -0.0066(11) C2 0.0461(16) 0.0350(15) 0.0600(18) 0.000 0.0323(14) 0.000 C3 0.0759(18) 0.085(2) 0.0662(16) -0.0239(14) 0.0285(14) -0.0273(15) C4 0.094(2) 0.0662(17) 0.0430(12) -0.0091(12) 0.0227(13) -0.0034(14) C5 0.0849(19) 0.0834(19) 0.0702(17) -0.0216(15) 0.0444(15) 0.0004(16) C6 0.082(3) 0.0387(17) 0.073(2) 0.000 0.039(2) 0.000 N2 0.0590(12) 0.0465(10) 0.0490(10) -0.0123(8) 0.0247(9) -0.0067(9) N3 0.0498(10) 0.0451(10) 0.0533(10) -0.0040(8) 0.0264(8) 0.0012(8) C7 0.0771(17) 0.0518(14) 0.0569(14) -0.0188(12) 0.0280(13) -0.0156(13) C8 0.0598(14) 0.0395(11) 0.0464(11) 0.0022(9) 0.0264(10) 0.0092(10) C9 0.0478(12) 0.0552(14) 0.0631(13) 0.0030(12) 0.0295(10) 0.0056(12) C10 0.096(2) 0.088(2) 0.0574(15) -0.0247(15) 0.0205(15) -0.0133(17) C11 0.091(2) 0.111(2) 0.094(2) -0.049(2) 0.0461(18) -0.050(2) C12 0.146(3) 0.0522(17) 0.096(2) -0.0113(17) 0.038(2) -0.018(2) C13 0.0810(18) 0.0758(19) 0.0682(15) -0.0185(14) 0.0389(13) 0.0117(15) C14 0.0612(16) 0.079(2) 0.096(2) -0.0228(17) 0.0382(15) -0.0191(15) C15 0.089(2) 0.093(2) 0.097(2) 0.0174(19) 0.0564(18) -0.0072(18) C16 0.0581(17) 0.087(2) 0.108(2) 0.0064(18) 0.0354(16) 0.0177(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N3 2.4658(18) 6_657 ? Nd1 N3 2.4658(18) . ? Nd1 N1 2.4791(16) . ? Nd1 N1 2.4791(16) 6_657 ? Nd1 N2 2.4820(17) . ? Nd1 N2 2.4820(17) 6_657 ? N1 C2 1.324(2) . ? N1 C1 1.476(3) . ? C1 C4 1.511(3) . ? C1 C3 1.529(3) . ? C1 C5 1.531(3) . ? C2 N1 1.324(2) 6_657 ? C2 C6 1.516(4) . ? N2 C8 1.322(3) . ? N2 C7 1.477(3) . ? N3 C8 1.334(3) . ? N3 C9 1.467(3) . ? C7 C11 1.516(4) . ? C7 C10 1.521(4) . ? C7 C12 1.533(4) . ? C8 C13 1.514(3) . ? C9 C14 1.520(3) . ? C9 C15 1.527(4) . ? C9 C16 1.527(3) . ? 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 N3 Nd1 N3 152.62(9) 6_657 . ? N3 Nd1 N1 97.14(6) 6_657 . ? N3 Nd1 N1 107.39(6) . . ? N3 Nd1 N1 107.39(6) 6_657 6_657 ? N3 Nd1 N1 97.14(6) . 6_657 ? N1 Nd1 N1 53.22(7) . 6_657 ? N3 Nd1 N2 106.29(6) 6_657 . ? N3 Nd1 N2 53.39(6) . . ? N1 Nd1 N2 153.78(6) . . ? N1 Nd1 N2 107.22(6) 6_657 . ? N3 Nd1 N2 53.39(6) 6_657 6_657 ? N3 Nd1 N2 106.29(6) . 6_657 ? N1 Nd1 N2 107.22(6) . 6_657 ? N1 Nd1 N2 153.78(6) 6_657 6_657 ? N2 Nd1 N2 96.29(9) . 6_657 ? C2 N1 C1 127.09(18) . . ? C2 N1 Nd1 96.38(13) . . ? C1 N1 Nd1 136.19(13) . . ? N1 C1 C4 104.62(17) . . ? N1 C1 C3 113.7(2) . . ? C4 C1 C3 107.1(2) . . ? N1 C1 C5 112.74(19) . . ? C4 C1 C5 107.4(2) . . ? C3 C1 C5 110.7(2) . . ? N1 C2 N1 114.0(2) 6_657 . ? N1 C2 C6 122.99(12) 6_657 . ? N1 C2 C6 122.99(12) . . ? N1 C2 Nd1 57.01(12) 6_657 . ? N1 C2 Nd1 57.01(12) . . ? C6 C2 Nd1 180.000(1) . . ? C8 N2 C7 126.6(2) . . ? C8 N2 Nd1 96.26(13) . . ? C7 N2 Nd1 137.00(16) . . ? C8 N3 C9 126.88(19) . . ? C8 N3 Nd1 96.64(14) . . ? C9 N3 Nd1 136.04(14) . . ? N2 C7 C11 104.7(2) . . ? N2 C7 C10 114.1(2) . . ? C11 C7 C10 106.9(3) . . ? N2 C7 C12 112.6(2) . . ? C11 C7 C12 108.0(3) . . ? C10 C7 C12 110.1(2) . . ? N2 C8 N3 113.62(19) . . ? N2 C8 C13 123.8(2) . . ? N3 C8 C13 122.5(2) . . ? N2 C8 Nd1 57.16(11) . . ? N3 C8 Nd1 56.52(11) . . ? C13 C8 Nd1 176.56(17) . . ? N3 C9 C14 104.46(19) . . ? N3 C9 C15 113.7(2) . . ? C14 C9 C15 107.4(2) . . ? N3 C9 C16 113.4(2) . . ? C14 C9 C16 107.0(2) . . ? C15 C9 C16 110.4(2) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.734 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.052 #=== data_eurn2 _database_code_depnum_ccdc_archive 'CCDC 272572' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H63 Eu N6' _chemical_formula_weight 659.82 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 17.1087(15) _cell_length_b 11.7908(15) _cell_length_c 19.078(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.9440(10) _cell_angle_gamma 90.00 _cell_volume 3460.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 1002 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.5 _exptl_crystal_description fragments _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.838 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7100 _exptl_absorpt_correction_T_max 0.7575 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9000 _diffrn_reflns_av_R_equivalents 0.109 _diffrn_reflns_av_sigmaI/netI 0.1322 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4040 _reflns_number_gt 2633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.1153P)^2^+8.1083P] 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 4040 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1231 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.2082 _refine_ls_wR_factor_gt 0.1869 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _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 Eu1 Eu 0.5000 0.66691(5) 0.7500 0.0352(2) Uani 1 2 d S . . N1 N 0.4895(6) 0.8060(6) 0.6521(5) 0.051(2) Uani 1 1 d . . . N2 N 0.6158(6) 0.7157(7) 0.7148(6) 0.053(2) Uani 1 1 d . . . C1 C 0.5706(7) 0.7885(9) 0.6594(7) 0.052(3) Uani 1 1 d . . . C2 C 0.4263(8) 0.8902(9) 0.5989(6) 0.056(3) Uani 1 1 d . . . C3 C 0.3457(9) 0.8692(16) 0.6128(10) 0.100(5) Uani 1 1 d . . . H3A H 0.2976 0.8460 0.5643 0.119 Uiso 1 1 calc R . . H3B H 0.3304 0.9385 0.6313 0.119 Uiso 1 1 calc R . . H3C H 0.3581 0.8099 0.6514 0.119 Uiso 1 1 calc R . . C4 C 0.4554(12) 1.0165(9) 0.6227(9) 0.100(5) Uani 1 1 d . . . H4A H 0.4864 1.0220 0.6790 0.119 Uiso 1 1 calc R . . H4B H 0.4045 1.0650 0.6041 0.119 Uiso 1 1 calc R . . H4C H 0.4932 1.0403 0.5996 0.119 Uiso 1 1 calc R . . C5 C 0.3957(10) 0.8696(14) 0.5131(7) 0.090(5) Uani 1 1 d . . . H5A H 0.4293 0.9160 0.4942 0.108 Uiso 1 1 calc R . . H5B H 0.3347 0.8893 0.4854 0.108 Uiso 1 1 calc R . . H5C H 0.4035 0.7902 0.5045 0.108 Uiso 1 1 calc R . . C6 C 0.6046(9) 0.8421(11) 0.6058(7) 0.070(3) Uani 1 1 d . . . H6A H 0.6656 0.8234 0.6240 0.084 Uiso 1 1 calc R . . H6B H 0.5980 0.9238 0.6059 0.084 Uiso 1 1 calc R . . H6C H 0.5720 0.8135 0.5533 0.084 Uiso 1 1 calc R . . C7 C 0.7046(6) 0.6738(9) 0.7344(6) 0.049(2) Uani 1 1 d . . . C8 C 0.7731(8) 0.7626(12) 0.7691(10) 0.092(5) Uani 1 1 d . . . H8A H 0.7650 0.8205 0.7304 0.111 Uiso 1 1 calc R . . H8B H 0.8300 0.7283 0.7860 0.111 Uiso 1 1 calc R . . H8C H 0.7687 0.7968 0.8135 0.111 Uiso 1 1 calc R . . C9 C 0.7202(9) 0.5820(12) 0.7960(8) 0.079(4) Uani 1 1 d . . . H9A H 0.7121 0.6141 0.8391 0.095 Uiso 1 1 calc R . . H9B H 0.7792 0.5535 0.8148 0.095 Uiso 1 1 calc R . . H9C H 0.6794 0.5203 0.7730 0.095 Uiso 1 1 calc R . . C10 C 0.7110(9) 0.6149(12) 0.6660(8) 0.078(4) Uani 1 1 d . . . H10A H 0.6607 0.5665 0.6396 0.094 Uiso 1 1 calc R . . H10B H 0.7635 0.5694 0.6850 0.094 Uiso 1 1 calc R . . H10C H 0.7129 0.6715 0.6298 0.094 Uiso 1 1 calc R . . N3 N 0.4643(5) 0.4804(6) 0.6847(4) 0.0403(17) Uani 1 1 d . . . C11 C 0.5000 0.4225(12) 0.7500 0.048(3) Uani 1 2 d S . . C12 C 0.4250(6) 0.4412(9) 0.6053(6) 0.046(2) Uani 1 1 d . . . C13 C 0.3429(8) 0.3704(11) 0.5832(7) 0.065(3) Uani 1 1 d . . . H13A H 0.3578 0.2989 0.6112 0.078 Uiso 1 1 calc R . . H13B H 0.3162 0.3559 0.5276 0.078 Uiso 1 1 calc R . . H13C H 0.3023 0.4114 0.5969 0.078 Uiso 1 1 calc R . . C14 C 0.3996(8) 0.5450(10) 0.5535(6) 0.059(3) Uani 1 1 d . . . H14A H 0.3545 0.5862 0.5606 0.070 Uiso 1 1 calc R . . H14B H 0.3780 0.5219 0.4995 0.070 Uiso 1 1 calc R . . H14C H 0.4499 0.5936 0.5673 0.070 Uiso 1 1 calc R . . C15 C 0.4894(8) 0.3753(10) 0.5838(7) 0.063(3) Uani 1 1 d . . . H15A H 0.5452 0.4136 0.6056 0.076 Uiso 1 1 calc R . . H15B H 0.4670 0.3718 0.5275 0.076 Uiso 1 1 calc R . . H15C H 0.4965 0.2989 0.6046 0.076 Uiso 1 1 calc R . . C16 C 0.5000 0.2995(13) 0.7500 0.056(4) Uani 1 2 d S . . H16A H 0.5522 0.2720 0.7475 0.068 Uiso 0.50 1 calc PR . . H16B H 0.4492 0.2720 0.7051 0.068 Uiso 0.50 1 calc PR . . H16C H 0.4986 0.2720 0.7974 0.068 Uiso 0.50 1 calc PR . . 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 Eu1 0.0472(4) 0.0211(3) 0.0424(4) 0.000 0.0245(3) 0.000 N1 0.069(6) 0.024(4) 0.060(5) 0.007(3) 0.029(5) 0.004(4) N2 0.057(5) 0.040(5) 0.072(6) 0.008(4) 0.038(5) 0.004(4) C1 0.060(7) 0.036(5) 0.065(7) -0.005(5) 0.032(6) -0.012(5) C2 0.076(7) 0.042(6) 0.054(7) 0.021(5) 0.033(6) 0.027(5) C3 0.075(9) 0.131(14) 0.096(11) 0.054(10) 0.040(8) 0.044(9) C4 0.164(14) 0.017(5) 0.097(10) 0.014(6) 0.038(10) 0.015(7) C5 0.112(12) 0.076(9) 0.060(8) 0.023(7) 0.018(8) 0.011(9) C6 0.078(8) 0.064(8) 0.069(8) 0.021(6) 0.033(7) -0.006(6) C7 0.044(5) 0.043(6) 0.068(6) -0.004(5) 0.031(5) -0.004(5) C8 0.070(9) 0.059(9) 0.148(16) -0.021(9) 0.048(10) -0.021(7) C9 0.068(8) 0.080(10) 0.095(10) 0.023(8) 0.040(8) 0.021(7) C10 0.080(9) 0.070(9) 0.100(10) -0.022(8) 0.053(8) 0.002(7) N3 0.044(4) 0.027(4) 0.049(5) 0.002(3) 0.019(4) -0.002(3) C11 0.043(8) 0.050(9) 0.067(10) 0.000 0.038(8) 0.000 C12 0.051(6) 0.041(5) 0.048(6) -0.001(4) 0.024(5) 0.006(4) C13 0.073(8) 0.057(7) 0.061(7) -0.012(6) 0.026(6) -0.012(6) C14 0.080(8) 0.051(6) 0.048(6) -0.004(5) 0.031(6) -0.002(6) C15 0.074(8) 0.047(6) 0.079(8) -0.019(6) 0.043(7) -0.002(6) C16 0.069(10) 0.049(9) 0.065(10) 0.000 0.042(9) 0.000 _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 Eu1 N2 2.424(8) . ? Eu1 N2 2.424(8) 6_657 ? Eu1 N1 2.432(8) 6_657 ? Eu1 N1 2.432(8) . ? Eu1 N3 2.469(7) . ? Eu1 N3 2.469(7) 6_657 ? Eu1 C11 2.881(15) . ? Eu1 C1 2.886(10) 6_657 ? Eu1 C1 2.886(10) . ? N1 C1 1.348(14) . ? N1 C2 1.492(13) . ? N2 C1 1.318(14) . ? N2 C7 1.481(13) . ? C1 C6 1.519(15) . ? C2 C5 1.504(17) . ? C2 C3 1.533(18) . ? C2 C4 1.572(17) . ? C7 C8 1.493(16) . ? C7 C9 1.532(16) . ? C7 C10 1.524(15) . ? N3 C11 1.313(11) . ? N3 C12 1.439(13) . ? C11 N3 1.313(11) 6_657 ? C11 C16 1.45(2) . ? C12 C14 1.513(15) . ? C12 C13 1.526(15) . ? C12 C15 1.543(14) . ? 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 N2 Eu1 N2 152.6(4) . 6_657 ? N2 Eu1 N1 105.0(3) . 6_657 ? N2 Eu1 N1 54.7(3) 6_657 6_657 ? N2 Eu1 N1 54.7(3) . . ? N2 Eu1 N1 105.0(3) 6_657 . ? N1 Eu1 N1 95.2(4) 6_657 . ? N2 Eu1 N3 97.1(3) . . ? N2 Eu1 N3 107.4(3) 6_657 . ? N1 Eu1 N3 155.1(3) 6_657 . ? N1 Eu1 N3 107.1(3) . . ? N2 Eu1 N3 107.4(3) . 6_657 ? N2 Eu1 N3 97.1(3) 6_657 6_657 ? N1 Eu1 N3 107.1(3) 6_657 6_657 ? N1 Eu1 N3 155.1(3) . 6_657 ? N3 Eu1 N3 54.1(3) . 6_657 ? N2 Eu1 C11 103.7(2) . . ? N2 Eu1 C11 103.7(2) 6_657 . ? N1 Eu1 C11 132.4(2) 6_657 . ? N1 Eu1 C11 132.4(2) . . ? N3 Eu1 C11 27.03(17) . . ? N3 Eu1 C11 27.03(18) 6_657 . ? N2 Eu1 C1 131.0(3) . 6_657 ? N2 Eu1 C1 27.0(3) 6_657 6_657 ? N1 Eu1 C1 27.7(3) 6_657 6_657 ? N1 Eu1 C1 102.4(3) . 6_657 ? N3 Eu1 C1 132.0(3) . 6_657 ? N3 Eu1 C1 102.5(3) 6_657 6_657 ? C11 Eu1 C1 119.8(2) . 6_657 ? N2 Eu1 C1 27.0(3) . . ? N2 Eu1 C1 131.0(3) 6_657 . ? N1 Eu1 C1 102.4(3) 6_657 . ? N1 Eu1 C1 27.7(3) . . ? N3 Eu1 C1 102.5(3) . . ? N3 Eu1 C1 132.0(3) 6_657 . ? C11 Eu1 C1 119.8(2) . . ? C1 Eu1 C1 120.4(4) 6_657 . ? C1 N1 C2 125.4(9) . . ? C1 N1 Eu1 95.2(6) . . ? C2 N1 Eu1 139.4(7) . . ? C1 N2 C7 126.7(9) . . ? C1 N2 Eu1 96.5(6) . . ? C7 N2 Eu1 136.3(6) . . ? N2 C1 N1 113.5(9) . . ? N2 C1 C6 123.2(10) . . ? N1 C1 C6 123.2(10) . . ? N2 C1 Eu1 56.6(5) . . ? N1 C1 Eu1 57.1(5) . . ? C6 C1 Eu1 174.0(8) . . ? C5 C2 N1 115.8(10) . . ? C5 C2 C3 104.5(12) . . ? N1 C2 C3 102.4(9) . . ? C5 C2 C4 112.5(10) . . ? N1 C2 C4 113.0(10) . . ? C3 C2 C4 107.4(12) . . ? N2 C7 C8 113.4(9) . . ? N2 C7 C9 104.2(8) . . ? C8 C7 C9 108.4(11) . . ? N2 C7 C10 112.7(9) . . ? C8 C7 C10 111.3(10) . . ? C9 C7 C10 106.4(10) . . ? C11 N3 C12 129.9(9) . . ? C11 N3 Eu1 94.3(7) . . ? C12 N3 Eu1 135.7(6) . . ? N3 C11 N3 117.4(13) . 6_657 ? N3 C11 C16 121.3(6) . . ? N3 C11 C16 121.3(6) 6_657 . ? N3 C11 Eu1 58.7(6) . . ? N3 C11 Eu1 58.7(6) 6_657 . ? C16 C11 Eu1 180.000(4) . . ? N3 C12 C14 107.2(8) . . ? N3 C12 C13 114.6(8) . . ? C14 C12 C13 107.2(9) . . ? N3 C12 C15 112.5(8) . . ? C14 C12 C15 105.6(9) . . ? C13 C12 C15 109.2(9) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 2.659 _refine_diff_density_min -2.139 _refine_diff_density_rms 0.180 #=== data_earn _database_code_depnum_ccdc_archive 'CCDC 272573' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H63 Er N6' _chemical_formula_weight 675.12 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' 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 C2/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 17.268(3) _cell_length_b 11.7545(18) _cell_length_c 19.135(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.107(2) _cell_angle_gamma 90.00 _cell_volume 3487.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6703 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.5 _exptl_crystal_description multifaceted _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 2.432 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6420 _exptl_absorpt_correction_T_max 0.6420 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'SMART CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24696 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4096 _reflns_number_gt 3491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The atom C2 was held isotropic because twinning produces a false peak nearby at 1/2, 1/2, 3/4. We are unable to apply a rational correction for the twinning, but because this is isostructural with the other 5 complexes in this manuscript we offer this structure as an identification. ; _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^)+(0.0682P)^2^+130.1275P] 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 4096 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2457 _refine_ls_wR_factor_gt 0.2420 _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_restrained_S_all 1.253 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.5000 0.66656(7) 0.7500 0.0401(3) Uani 1 2 d S . . N1 N 0.4626(7) 0.4862(9) 0.6837(7) 0.053(3) Uani 1 1 d . . . C1 C 0.4259(10) 0.4446(13) 0.6067(9) 0.056(3) Uani 1 1 d . . . C2 C 0.5000 0.4291(15) 0.7500 0.041 Uiso 1 2 d S . . C3 C 0.3434(13) 0.3735(18) 0.5845(12) 0.089(6) Uani 1 1 d . . . H3A H 0.3543 0.3144 0.6224 0.107 Uiso 1 1 calc R . . H3B H 0.3266 0.3399 0.5342 0.107 Uiso 1 1 calc R . . H3C H 0.2979 0.4217 0.5832 0.107 Uiso 1 1 calc R . . C4 C 0.3969(13) 0.5504(16) 0.5518(10) 0.080(5) Uani 1 1 d . . . H4A H 0.3533 0.5912 0.5597 0.096 Uiso 1 1 calc R . . H4B H 0.3740 0.5257 0.4986 0.096 Uiso 1 1 calc R . . H4C H 0.4455 0.5993 0.5632 0.096 Uiso 1 1 calc R . . C5 C 0.4909(13) 0.3760(17) 0.5872(11) 0.082(5) Uani 1 1 d . . . H5A H 0.5453 0.4149 0.6077 0.098 Uiso 1 1 calc R . . H5B H 0.4688 0.3689 0.5317 0.098 Uiso 1 1 calc R . . H5C H 0.4986 0.3016 0.6100 0.098 Uiso 1 1 calc R . . C6 C 0.5000 0.3050(15) 0.7500 0.058(5) Uani 1 2 d S . . H6A H 0.5386 0.2777 0.8008 0.070 Uiso 0.50 1 calc PR . . H6B H 0.5187 0.2777 0.7126 0.070 Uiso 0.50 1 calc PR . . H6C H 0.4428 0.2777 0.7366 0.070 Uiso 0.50 1 calc PR . . N2 N 0.5127(9) 0.8028(10) 0.8443(9) 0.070(4) Uani 1 1 d . . . N3 N 0.3865(8) 0.7100(11) 0.7820(8) 0.063(3) Uani 1 1 d . . . C7 C 0.5730(12) 0.8881(13) 0.8984(9) 0.066(4) Uani 1 1 d . . . C8 C 0.4316(11) 0.7848(14) 0.8392(9) 0.062(4) Uani 1 1 d . . . C9 C 0.2982(10) 0.6696(14) 0.7624(11) 0.066(4) Uani 1 1 d . . . C10 C 0.6030(16) 0.869(2) 0.9818(12) 0.111(8) Uani 1 1 d . . . H10A H 0.5578 0.8881 0.9960 0.134 Uiso 1 1 calc R . . H10B H 0.6523 0.9165 1.0103 0.134 Uiso 1 1 calc R . . H10C H 0.6187 0.7908 0.9937 0.134 Uiso 1 1 calc R . . C11 C 0.6534(15) 0.873(2) 0.8855(16) 0.122(9) Uani 1 1 d . . . H11A H 0.6821 0.9444 0.8917 0.146 Uiso 1 1 calc R . . H11B H 0.6371 0.8441 0.8339 0.146 Uiso 1 1 calc R . . H11C H 0.6915 0.8194 0.9229 0.146 Uiso 1 1 calc R . . C12 C 0.540(2) 1.0143(16) 0.871(2) 0.159(13) Uani 1 1 d . . . H12A H 0.5043 1.0384 0.8956 0.191 Uiso 1 1 calc R . . H12B H 0.5065 1.0159 0.8158 0.191 Uiso 1 1 calc R . . H12C H 0.5882 1.0645 0.8861 0.191 Uiso 1 1 calc R . . C13 C 0.3981(15) 0.842(2) 0.8911(13) 0.099(7) Uani 1 1 d . . . H13A H 0.3390 0.8642 0.8607 0.119 Uiso 1 1 calc R . . H13B H 0.4321 0.9088 0.9142 0.119 Uiso 1 1 calc R . . H13C H 0.4018 0.7908 0.9313 0.119 Uiso 1 1 calc R . . C14 C 0.2763(14) 0.5834(19) 0.6966(14) 0.095(7) Uani 1 1 d . . . H14A H 0.2935 0.6131 0.6589 0.114 Uiso 1 1 calc R . . H14B H 0.2153 0.5695 0.6723 0.114 Uiso 1 1 calc R . . H14C H 0.3064 0.5135 0.7175 0.114 Uiso 1 1 calc R . . C15 C 0.2927(16) 0.610(2) 0.8279(18) 0.130(11) Uani 1 1 d . . . H15A H 0.3408 0.5589 0.8517 0.156 Uiso 1 1 calc R . . H15B H 0.2399 0.5671 0.8090 0.156 Uiso 1 1 calc R . . H15C H 0.2937 0.6644 0.8657 0.156 Uiso 1 1 calc R . . C16 C 0.2316(12) 0.7618(18) 0.7306(13) 0.089(6) Uani 1 1 d . . . H16A H 0.2289 0.8029 0.7729 0.107 Uiso 1 1 calc R . . H16B H 0.1764 0.7286 0.6989 0.107 Uiso 1 1 calc R . . H16C H 0.2470 0.8131 0.6997 0.107 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 0.0508(4) 0.0309(4) 0.0381(4) 0.000 0.0191(3) 0.000 N1 0.063(7) 0.029(5) 0.067(7) 0.002(5) 0.027(6) -0.002(5) C1 0.068(9) 0.053(8) 0.048(8) -0.010(6) 0.026(7) -0.009(7) C3 0.098(14) 0.084(13) 0.088(13) -0.031(11) 0.042(11) -0.030(11) C4 0.111(14) 0.075(11) 0.049(9) -0.006(8) 0.029(9) -0.003(10) C5 0.098(13) 0.075(11) 0.083(12) -0.029(10) 0.049(11) -0.005(10) C6 0.091(15) 0.033(9) 0.045(10) 0.000 0.026(10) 0.000 N2 0.081(9) 0.040(7) 0.083(9) -0.010(6) 0.030(8) -0.007(6) N3 0.062(7) 0.044(6) 0.085(9) -0.003(6) 0.035(7) -0.004(6) C7 0.095(12) 0.045(8) 0.053(9) -0.020(7) 0.028(8) -0.013(8) C8 0.070(9) 0.056(8) 0.060(9) -0.001(7) 0.028(7) 0.012(7) C9 0.058(8) 0.058(9) 0.094(11) -0.013(9) 0.044(8) -0.001(7) C10 0.129(19) 0.095(16) 0.086(15) -0.044(13) 0.026(13) -0.017(14) C11 0.101(16) 0.13(2) 0.12(2) -0.063(17) 0.043(15) -0.057(15) C12 0.20(3) 0.029(9) 0.25(4) -0.027(16) 0.10(3) -0.019(13) C13 0.109(15) 0.104(16) 0.097(14) -0.030(13) 0.055(13) 0.018(13) C14 0.096(14) 0.091(15) 0.119(18) -0.022(13) 0.066(14) -0.018(12) C15 0.109(18) 0.100(17) 0.20(3) 0.07(2) 0.09(2) -0.001(14) C16 0.077(12) 0.086(14) 0.108(17) 0.021(12) 0.044(12) 0.021(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 N2 2.350(14) . ? Er1 N2 2.350(14) 2_656 ? Er1 N3 2.351(13) 2_656 ? Er1 N3 2.351(13) . ? Er1 N1 2.408(11) . ? Er1 N1 2.408(11) 2_656 ? N1 C2 1.325(14) . ? N1 C1 1.410(18) . ? C1 C3 1.54(2) . ? C1 C5 1.56(2) . ? C1 C4 1.56(2) . ? C2 N1 1.325(14) 2_656 ? C2 C6 1.46(2) . ? N2 C8 1.38(2) . ? N2 C7 1.488(19) . ? N3 C8 1.35(2) . ? N3 C9 1.480(19) . ? C7 C10 1.46(3) . ? C7 C11 1.52(3) . ? C7 C12 1.59(3) . ? C8 C13 1.51(2) . ? C9 C15 1.48(3) . ? C9 C16 1.50(2) . ? C9 C14 1.53(3) . ? 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 N2 Er1 N2 94.1(7) . 2_656 ? N2 Er1 N3 104.2(5) . 2_656 ? N2 Er1 N3 57.2(5) 2_656 2_656 ? N2 Er1 N3 57.2(5) . . ? N2 Er1 N3 104.2(5) 2_656 . ? N3 Er1 N3 154.9(6) 2_656 . ? N2 Er1 N1 156.5(5) . . ? N2 Er1 N1 106.4(4) 2_656 . ? N3 Er1 N1 96.6(4) 2_656 . ? N3 Er1 N1 105.5(4) . . ? N2 Er1 N1 106.4(4) . 2_656 ? N2 Er1 N1 156.5(5) 2_656 2_656 ? N3 Er1 N1 105.5(4) 2_656 2_656 ? N3 Er1 N1 96.6(4) . 2_656 ? N1 Er1 N1 56.6(6) . 2_656 ? C2 N1 C1 129.0(12) . . ? C2 N1 Er1 92.1(9) . . ? C1 N1 Er1 138.5(9) . . ? N1 C1 C3 114.3(13) . . ? N1 C1 C5 113.0(13) . . ? C3 C1 C5 109.2(14) . . ? N1 C1 C4 106.9(12) . . ? C3 C1 C4 105.2(15) . . ? C5 C1 C4 107.6(14) . . ? N1 C2 N1 119.1(16) . 2_656 ? N1 C2 C6 120.5(8) . . ? N1 C2 C6 120.5(8) 2_656 . ? N1 C2 Er1 59.5(8) . . ? N1 C2 Er1 59.5(8) 2_656 . ? C6 C2 Er1 180.000(5) . . ? C8 N2 C7 122.2(14) . . ? C8 N2 Er1 95.3(9) . . ? C7 N2 Er1 142.5(12) . . ? C8 N3 C9 125.1(14) . . ? C8 N3 Er1 95.9(9) . . ? C9 N3 Er1 138.5(10) . . ? C10 C7 N2 117.4(16) . . ? C10 C7 C11 104.3(19) . . ? N2 C7 C11 102.5(13) . . ? C10 C7 C12 113.6(19) . . ? N2 C7 C12 111.1(17) . . ? C11 C7 C12 106.5(19) . . ? N3 C8 N2 111.3(13) . . ? N3 C8 C13 125.0(17) . . ? N2 C8 C13 123.8(16) . . ? N3 C8 Er1 55.7(8) . . ? N2 C8 Er1 55.7(8) . . ? C13 C8 Er1 176.2(13) . . ? C15 C9 N3 112.5(17) . . ? C15 C9 C16 111.4(16) . . ? N3 C9 C16 113.0(15) . . ? C15 C9 C14 107.4(18) . . ? N3 C9 C14 105.9(13) . . ? C16 C9 C14 106.1(17) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 4.799 _refine_diff_density_min -5.989 _refine_diff_density_rms 0.229 #===end