# ic990533c.cif # 1. SUBMISSION DETAILS _publ_contact_autor ; Peter W. Roesky Universit\"at Karlsruhe Engesserstr. Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author_phone '049 721 608-2855' _publ_contact_author_fax '049 721 661921' _publ_contact_author_email 'roesky@achibm6.chemie.uni-karlsruhe.de' _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ' Bridged Aminotroponiminate Complexes of the Lanthanides - A Structural Contribution ' ; loop_ _publ_author_name _publ_author_address 'Peter W. Roesky, Markus R. Brgstein' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr, Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; #============================================================================== data_2-(tosyloxo)tropone _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H12 O4 S' _chemical_formula_weight 276.30 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc (No. 9) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 7.8987(8) _cell_length_b 14.976(2) _cell_length_c 10.7734(13) _cell_angle_alpha 90.00(2) _cell_angle_beta 96.242(11) _cell_angle_gamma 90.000(13) _cell_volume 1266.9(3) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device STOE STADI IV _diffrn_measurement_method ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1673 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0106 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 29.97 _reflns_number_total 1673 _reflns_number_observed 1631 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.1000P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.17(8) _refine_ls_number_reflns 1672 _refine_ls_number_parameters 173 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_obs 0.0392 _refine_ls_wR_factor_all 0.1160 _refine_ls_wR_factor_obs 0.1109 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.084 _refine_ls_restrained_S_obs 1.050 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S 0.67108(6) 0.18255(3) 0.88963(5) 0.0378(2) Uani 1 d . . C1 C 0.8370(3) 0.29035(14) 0.7548(2) 0.0334(4) Uani 1 d . . C2 C 0.7467(3) 0.2872(2) 0.6413(2) 0.0396(4) Uani 1 d . . H2 H 0.6855(3) 0.2348(2) 0.6236(2) 0.048 Uiso 1 calc R . C3 C 0.7316(4) 0.3526(2) 0.5443(2) 0.0503(6) Uani 1 d . . H3 H 0.6569(4) 0.3386(2) 0.4742(2) 0.060 Uiso 1 calc R . C4 C 0.8123(4) 0.4325(2) 0.5410(3) 0.0535(6) Uani 1 d . . H4 H 0.7879(4) 0.4660(2) 0.4686(3) 0.064 Uiso 1 calc R . C5 C 0.9293(4) 0.4709(2) 0.6352(3) 0.0546(6) Uani 1 d . . H5 H 0.9751(4) 0.5252(2) 0.6138(3) 0.065 Uiso 1 calc R . C6 C 0.9852(4) 0.4414(2) 0.7508(3) 0.0506(6) Uani 1 d . . H6 H 1.0599(4) 0.4801(2) 0.7966(3) 0.061 Uiso 1 calc R . C7 C 0.9494(3) 0.3600(2) 0.8164(2) 0.0429(5) Uani 1 d . . C8 C 0.6158(3) 0.27283(14) 0.9803(2) 0.0349(4) Uani 1 d . . C9 C 0.4784(3) 0.3264(2) 0.9369(2) 0.0425(5) Uani 1 d . . H9 H 0.4184(3) 0.3159(2) 0.8591(2) 0.051 Uiso 1 calc R . C10 C 0.4321(3) 0.3963(2) 1.0119(3) 0.0470(5) Uani 1 d . . H10 H 0.3407(3) 0.4328(2) 0.9836(3) 0.056 Uiso 1 calc R . C11 C 0.5208(3) 0.4119(2) 1.1284(2) 0.0407(4) Uani 1 d . . C12 C 0.6593(3) 0.3573(2) 1.1681(2) 0.0449(5) Uani 1 d . . H12 H 0.7207(3) 0.3683(2) 1.2453(2) 0.054 Uiso 1 calc R . C13 C 0.7076(3) 0.2877(2) 1.0962(2) 0.0416(5) Uani 1 d . . H13 H 0.7993(3) 0.2515(2) 1.1245(2) 0.050 Uiso 1 calc R . C14 C 0.4697(5) 0.4863(2) 1.2100(3) 0.0571(7) Uani 1 d . . H14A H 0.5403(34) 0.4850(17) 1.2884(15) 0.086 Uiso 1 calc R . H14B H 0.3527(15) 0.4789(15) 1.2244(31) 0.086 Uiso 1 calc R . H14C H 0.4835(49) 0.5425(3) 1.1695(17) 0.086 Uiso 1 calc R . O1 O 0.5386(3) 0.1675(2) 0.7917(2) 0.0529(5) Uani 1 d . . O2 O 0.7339(3) 0.11015(14) 0.9674(2) 0.0565(5) Uani 1 d . . O3 O 0.8380(2) 0.21431(12) 0.8309(2) 0.0388(3) Uani 1 d . . O4 O 1.0135(4) 0.3483(2) 0.9245(2) 0.0708(7) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0419(3) 0.0329(2) 0.0390(2) -0.0012(2) 0.0059(2) -0.0055(2) C1 0.0346(8) 0.0313(8) 0.0350(9) -0.0028(7) 0.0069(7) -0.0012(6) C2 0.0413(10) 0.0426(11) 0.0354(9) -0.0051(8) 0.0058(8) -0.0028(8) C3 0.0576(14) 0.059(2) 0.0346(10) 0.0024(10) 0.0046(9) 0.0015(11) C4 0.064(2) 0.0536(15) 0.0445(12) 0.0107(10) 0.0123(11) 0.0107(13) C5 0.0619(15) 0.0416(12) 0.062(2) 0.0066(11) 0.0171(12) -0.0009(11) C6 0.0496(12) 0.0441(12) 0.0583(14) -0.0028(11) 0.0072(11) -0.0117(10) C7 0.0418(10) 0.0413(11) 0.0449(10) -0.0023(9) 0.0022(9) -0.0072(9) C8 0.0343(9) 0.0381(9) 0.0323(8) 0.0013(7) 0.0034(7) -0.0015(7) C9 0.0415(11) 0.0454(11) 0.0387(10) 0.0016(8) -0.0043(8) 0.0045(8) C10 0.0466(12) 0.0446(12) 0.0497(12) 0.0012(10) 0.0042(10) 0.0095(9) C11 0.0423(10) 0.0393(9) 0.0426(10) 0.0009(8) 0.0146(8) -0.0040(8) C12 0.0431(11) 0.0557(14) 0.0353(9) -0.0079(9) 0.0019(8) 0.0008(10) C13 0.0366(9) 0.0491(12) 0.0383(10) -0.0012(8) 0.0000(8) 0.0049(8) C14 0.067(2) 0.0492(14) 0.0596(15) -0.0064(12) 0.0252(13) 0.0047(12) O1 0.0485(10) 0.0592(11) 0.0501(10) -0.0132(9) 0.0013(8) -0.0185(9) O2 0.0751(14) 0.0385(9) 0.0578(11) 0.0096(8) 0.0151(10) 0.0037(9) O3 0.0378(7) 0.0368(8) 0.0425(8) 0.0037(6) 0.0074(6) 0.0034(6) O4 0.073(2) 0.077(2) 0.0572(12) 0.0066(12) -0.0199(11) -0.0279(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O1 1.421(2) . ? S1 O2 1.426(2) . ? S1 O3 1.596(2) . ? S1 C8 1.751(2) . ? C1 C2 1.348(3) . ? C1 O3 1.403(3) . ? C1 C7 1.480(3) . ? C2 C3 1.428(4) . ? C3 C4 1.359(5) . ? C4 C5 1.417(5) . ? C5 C6 1.350(5) . ? C6 C7 1.451(4) . ? C7 O4 1.230(4) . ? C8 C9 1.390(3) . ? C8 C13 1.392(3) . ? C9 C10 1.395(4) . ? C10 C11 1.390(4) . ? C11 C12 1.395(4) . ? C11 C14 1.501(4) . ? C12 C13 1.377(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 O1 S1 O2 119.8(2) . . ? O1 S1 O3 109.04(11) . . ? O2 S1 O3 102.12(13) . . ? O1 S1 C8 109.21(13) . . ? O2 S1 C8 110.56(12) . . ? O3 S1 C8 104.96(10) . . ? C2 C1 O3 118.1(2) . . ? C2 C1 C7 131.6(2) . . ? O3 C1 C7 110.2(2) . . ? C1 C2 C3 129.3(2) . . ? C4 C3 C2 128.4(3) . . ? C3 C4 C5 127.6(3) . . ? C6 C5 C4 130.5(3) . . ? C5 C6 C7 131.5(3) . . ? O4 C7 C6 119.9(3) . . ? O4 C7 C1 119.3(3) . . ? C6 C7 C1 120.8(2) . . ? C9 C8 C13 121.4(2) . . ? C9 C8 S1 119.4(2) . . ? C13 C8 S1 119.2(2) . . ? C8 C9 C10 118.8(2) . . ? C11 C10 C9 120.8(2) . . ? C10 C11 C12 118.7(2) . . ? C10 C11 C14 120.9(3) . . ? C12 C11 C14 120.5(2) . . ? C13 C12 C11 121.8(2) . . ? C12 C13 C8 118.5(2) . . ? C1 O3 S1 121.40(14) . . ? _refine_diff_density_max 0.266 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.061 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_autor ; Peter W. Roesky Universit\"at Karlsruhe Engesserstr. Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author_phone '049 721 608-2855' _publ_contact_author_fax '049 721 661921' _publ_contact_author_email 'roesky@achibm6.chemie.uni-karlsruhe.de' _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ' Bridged Aminotroponiminate Complexes of the Lanthanides - A Structural Contribution ' ; loop_ _publ_author_name _publ_author_address 'Peter W. Roesky, Markus R. Brgstein' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr, Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; #============================================================================== data_2-(N-isopropylamino)tropone _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H13 N O' _chemical_formula_weight 163.21 _chemical_melting_point ? _chemical_compound_source ? 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c (No. 14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.506(2) _cell_length_b 8.202(2) _cell_length_c 13.789(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.14(3) _cell_angle_gamma 90.00 _cell_volume 956.5(3) _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 ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method ? _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device STOE STADI IV _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1869 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.02 _reflns_number_total 1869 _reflns_number_observed 1305 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 22 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.1275P)^2^+0.4540P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1847 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_obs 0.0779 _refine_ls_wR_factor_all 0.2901 _refine_ls_wR_factor_obs 0.2192 _refine_ls_goodness_of_fit_all 1.133 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.214 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O O 0.6758(3) 0.0314(3) 0.5586(2) 0.0790(8) Uani 1 d . . N N 0.4587(3) 0.2366(3) 0.5780(2) 0.0665(8) Uani 1 d . . H0 H 0.4725(3) 0.1753(3) 0.5290(2) 0.080 Uiso 1 calc R . C1 C 0.6956(4) 0.1116(4) 0.6356(2) 0.0576(8) Uani 1 d . . C2 C 0.8353(4) 0.0904(5) 0.6998(3) 0.0730(10) Uani 1 d . . H2 H 0.9077(4) 0.0184(5) 0.6773(3) 0.088 Uiso 1 calc R . C3 C 0.8829(5) 0.1570(6) 0.7891(3) 0.0884(12) Uani 1 d . . H3 H 0.9835(5) 0.1262(6) 0.8157(3) 0.106 Uiso 1 calc R . C4 C 0.8063(6) 0.2619(6) 0.8459(3) 0.0936(14) Uani 1 d . . H4 H 0.8592(6) 0.2900(6) 0.9061(3) 0.112 Uiso 1 calc R . C5 C 0.6612(6) 0.3286(5) 0.8230(3) 0.0876(12) Uani 1 d . . H5 H 0.6258(6) 0.3943(5) 0.8712(3) 0.105 Uiso 1 calc R . C6 C 0.5583(5) 0.3139(4) 0.7394(3) 0.0757(10) Uani 1 d . . H6 H 0.4652(5) 0.3730(4) 0.7402(3) 0.091 Uiso 1 calc R . C7 C 0.5685(4) 0.2269(4) 0.6541(2) 0.0568(8) Uani 1 d . . C8 C 0.3176(4) 0.3391(4) 0.5679(3) 0.0805(11) Uani 1 d . . H8 H 0.3399(4) 0.4381(4) 0.6068(3) 0.097 Uiso 1 calc R . C9 C 0.1803(5) 0.2522(6) 0.6054(4) 0.112(2) Uani 1 d . . H9A H 0.0888(14) 0.3216(21) 0.5982(28) 0.168 Uiso 1 calc R . H9B H 0.2062(19) 0.2260(44) 0.6731(9) 0.168 Uiso 1 calc R . H9C H 0.1582(32) 0.1537(27) 0.5689(20) 0.168 Uiso 1 calc R . C10 C 0.2839(6) 0.3876(6) 0.4619(4) 0.110(2) Uani 1 d . . H10A H 0.1943(29) 0.4595(38) 0.4544(6) 0.165 Uiso 1 calc R . H10B H 0.2614(45) 0.2918(8) 0.4229(5) 0.165 Uiso 1 calc R . H10C H 0.3744(18) 0.4422(42) 0.4413(9) 0.165 Uiso 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 O 0.0748(15) 0.090(2) 0.0701(15) -0.0221(13) -0.0035(11) 0.0188(13) N 0.068(2) 0.066(2) 0.064(2) -0.0080(13) -0.0001(12) 0.0102(13) C1 0.058(2) 0.059(2) 0.055(2) 0.0019(13) 0.0030(12) -0.0016(13) C2 0.062(2) 0.082(2) 0.074(2) 0.003(2) -0.002(2) -0.001(2) C3 0.079(2) 0.099(3) 0.081(2) 0.010(2) -0.019(2) -0.014(2) C4 0.117(3) 0.093(3) 0.065(2) -0.004(2) -0.017(2) -0.031(3) C5 0.118(3) 0.080(2) 0.065(2) -0.021(2) 0.008(2) -0.017(2) C6 0.089(2) 0.070(2) 0.069(2) -0.017(2) 0.010(2) -0.002(2) C7 0.063(2) 0.052(2) 0.055(2) 0.0003(13) 0.0038(13) -0.0054(13) C8 0.069(2) 0.061(2) 0.108(3) -0.008(2) -0.006(2) 0.011(2) C9 0.075(2) 0.100(3) 0.165(5) -0.016(3) 0.028(3) 0.006(2) C10 0.099(3) 0.091(3) 0.128(4) 0.018(3) -0.038(3) 0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O C1 1.245(4) . ? N C7 1.330(4) . ? N C8 1.460(4) . ? C1 C2 1.414(5) . ? C1 C7 1.479(4) . ? C2 C3 1.368(5) . ? C3 C4 1.374(6) . ? C4 C5 1.356(7) . ? C5 C6 1.376(5) . ? C6 C7 1.386(4) . ? C8 C9 1.507(6) . ? C8 C10 1.512(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 C7 N C8 127.6(3) . . ? O C1 C2 119.8(3) . . ? O C1 C7 116.7(3) . . ? C2 C1 C7 123.5(3) . . ? C3 C2 C1 131.4(4) . . ? C2 C3 C4 130.6(4) . . ? C5 C4 C3 126.5(4) . . ? C4 C5 C6 129.9(4) . . ? C5 C6 C7 131.6(4) . . ? N C7 C6 122.4(3) . . ? N C7 C1 111.5(3) . . ? C6 C7 C1 126.0(3) . . ? N C8 C9 110.8(3) . . ? N C8 C10 108.2(3) . . ? C9 C8 C10 112.4(4) . . ? _refine_diff_density_max 0.188 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.049 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_autor ; Peter W. Roesky Universit\"at Karlsruhe Engesserstr. Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author_phone '049 721 608-2855' _publ_contact_author_fax '049 721 661921' _publ_contact_author_email 'roesky@achibm6.chemie.uni-karlsruhe.de' _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ' Bridged Aminotroponiminate Complexes of the Lanthanides - A Structural Contribution ' ; loop_ _publ_author_name _publ_author_address 'Peter W. Roesky, Markus R. Brgstein' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr, Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; #============================================================================== data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C62 H92 Cl2 N8 Nd2 O4' _chemical_formula_weight 1372.82 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'O' 'O' 0.0106 0.0060 '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 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 12.714(3) _cell_length_b 32.835(7) _cell_length_c 16.193(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.62(3) _cell_angle_gamma 90.00 _cell_volume 6326.9(22) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method ? _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 1.758 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device STOE IPDS _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12217 _diffrn_reflns_av_R_equivalents 0.1209 _diffrn_reflns_av_sigmaI/netI 0.3534 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10568 _reflns_number_observed 3393 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2131 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0910P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8437 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2459 _refine_ls_R_factor_obs 0.0887 _refine_ls_wR_factor_all 0.2757 _refine_ls_wR_factor_obs 0.1987 _refine_ls_goodness_of_fit_all 0.861 _refine_ls_goodness_of_fit_obs 1.149 _refine_ls_restrained_S_all 0.892 _refine_ls_restrained_S_obs 1.149 _refine_ls_shift/esd_max -0.020 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 0.74290(9) 0.13957(3) -0.16038(8) 0.0302(3) Uani 1 d . . Nd2 Nd 0.57499(9) 0.13318(3) 0.05432(8) 0.0288(3) Uani 1 d . . Cl1 Cl 0.6694(5) 0.08376(15) -0.0540(4) 0.0356(12) Uani 1 d . . Cl2 Cl 0.6617(6) 0.1885(2) -0.0488(5) 0.0413(13) Uani 1 d . . O1 O 0.9218(13) 0.1465(5) -0.0207(11) 0.047(4) Uani 1 d . . O2 O 0.3997(14) 0.1507(6) -0.0781(11) 0.051(5) Uani 1 d . . O3 O 0.3030(37) 0.0203(14) -0.5251(30) 0.155(14) Uiso 1 d . . O4 O 0.6369(61) 0.2128(22) -0.5070(46) 0.230(25) Uiso 1 d . . N1 N 0.8605(17) 0.0867(6) -0.1995(14) 0.043(5) Uani 1 d . . N2 N 0.8774(18) 0.1650(5) -0.2218(13) 0.040(5) Uani 1 d . . N3 N 0.6480(16) 0.1943(6) -0.2558(14) 0.041(5) Uani 1 d . . N4 N 0.5755(14) 0.1229(6) -0.2797(13) 0.040(5) Uani 1 d . . N5 N 0.7339(16) 0.1053(5) 0.1732(11) 0.031(4) Uani 1 d . . N6 N 0.6936(18) 0.1806(6) 0.1589(14) 0.044(5) Uani 1 d . . N7 N 0.4666(14) 0.1647(5) 0.1356(11) 0.026(3) Uiso 1 d . . N8 N 0.4363(16) 0.0890(6) 0.0918(13) 0.040(5) Uani 1 d . . C1 C 0.9362(19) 0.0981(7) -0.2348(16) 0.035(5) Uiso 1 d . . C2 C 1.0187(22) 0.0706(8) -0.2438(18) 0.048(6) Uiso 1 d . . H2 H 1.0240(22) 0.0462(8) -0.2124(18) 0.057 Uiso 1 calc R . C3 C 1.0909(24) 0.0727(8) -0.2886(19) 0.052(6) Uiso 1 d . . H3 H 1.1388(24) 0.0501(8) -0.2807(19) 0.063 Uiso 1 calc R . C4 C 1.1056(28) 0.1018(10) -0.3425(23) 0.068(8) Uiso 1 d . . H4 H 1.1567(28) 0.0959(10) -0.3709(23) 0.082 Uiso 1 calc R . C5 C 1.0558(26) 0.1377(11) -0.3595(21) 0.072(7) Uiso 1 d . . H5 H 1.0755(26) 0.1541(11) -0.3995(21) 0.086 Uiso 1 calc R . C6 C 0.9746(21) 0.1554(7) -0.3250(17) 0.044(5) Uiso 1 d . . H6 H 0.9460(21) 0.1808(7) -0.3492(17) 0.053 Uiso 1 calc R . C7 C 0.9315(15) 0.1405(6) -0.2606(13) 0.027(4) Uiso 1 d . . C8 C 0.8849(22) 0.2096(7) -0.2340(18) 0.047(6) Uiso 1 d . . H8A H 0.8510(22) 0.2164(7) -0.2969(18) 0.057 Uiso 1 calc R . H8B H 0.9640(22) 0.2179(7) -0.2137(18) 0.057 Uiso 1 calc R . C9 C 0.8252(19) 0.2323(7) -0.1832(16) 0.036(5) Uiso 1 d . . H9A H 0.8605(19) 0.2590(7) -0.1666(16) 0.043 Uiso 1 calc R . H9B H 0.8341(19) 0.2173(7) -0.1288(16) 0.043 Uiso 1 calc R . C10 C 0.6997(19) 0.2382(6) -0.2352(16) 0.038(5) Uiso 1 d . . H10A H 0.6886(19) 0.2531(6) -0.2900(16) 0.045 Uiso 1 calc R . H10B H 0.6642(19) 0.2535(6) -0.2001(16) 0.045 Uiso 1 calc R . C11 C 0.5468(18) 0.1908(6) -0.3143(15) 0.031(4) Uiso 1 d . . C12 C 0.4792(18) 0.2253(6) -0.3622(15) 0.035(4) Uiso 1 d . . H12 H 0.5136(18) 0.2502(6) -0.3396(15) 0.042 Uiso 1 calc R . C13 C 0.3797(21) 0.2313(8) -0.4308(18) 0.048(6) Uiso 1 d . . H13 H 0.3575(21) 0.2584(8) -0.4456(18) 0.058 Uiso 1 calc R . C14 C 0.3127(23) 0.2030(8) -0.4776(18) 0.049(6) Uiso 1 d . . H14 H 0.2506(23) 0.2121(8) -0.5256(18) 0.059 Uiso 1 calc R . C15 C 0.3221(24) 0.1615(8) -0.4649(19) 0.054(6) Uiso 1 d . . H15 H 0.2636(24) 0.1464(8) -0.5052(19) 0.065 Uiso 1 calc R . C16 C 0.4047(20) 0.1376(8) -0.4016(16) 0.049(5) Uiso 1 d . . H16 H 0.3901(20) 0.1095(8) -0.4046(16) 0.058 Uiso 1 calc R . C17 C 0.5053(18) 0.1496(6) -0.3349(15) 0.032(4) Uiso 1 d . . C18 C 0.8465(24) 0.0454(8) -0.1668(19) 0.052(6) Uiso 1 d . . H18 H 0.7755(24) 0.0464(8) -0.1547(19) 0.063 Uiso 1 calc R . C19 C 0.9409(26) 0.0387(10) -0.0759(21) 0.064(7) Uiso 1 d . . H19A H 0.9333(110) 0.0118(23) -0.0539(66) 0.096 Uiso 1 calc R . H19B H 0.9346(109) 0.0591(37) -0.0345(44) 0.096 Uiso 1 calc R . H19C H 1.0136(26) 0.0410(67) -0.0824(34) 0.096 Uiso 1 calc R . C20 C 0.8320(22) 0.0102(8) -0.2339(18) 0.049(6) Uiso 1 d . . H20A H 0.7901(126) 0.0200(16) -0.2929(23) 0.073 Uiso 1 calc R . H20B H 0.7914(130) -0.0120(22) -0.2194(71) 0.073 Uiso 1 calc R . H20C H 0.9053(22) 0.0008(36) -0.2314(82) 0.073 Uiso 1 calc R . C21 C 0.5566(17) 0.0777(6) -0.2968(14) 0.027(4) Uiso 1 d . . H21 H 0.6227(17) 0.0656(6) -0.2506(14) 0.032 Uiso 1 calc R . C22 C 0.4580(24) 0.0594(8) -0.2758(20) 0.056(6) Uiso 1 d . . H22A H 0.4576(107) 0.0301(10) -0.2828(134) 0.084 Uiso 1 calc R . H22B H 0.3880(25) 0.0706(47) -0.3157(87) 0.084 Uiso 1 calc R . H22C H 0.4659(91) 0.0660(53) -0.2154(45) 0.084 Uiso 1 calc R . C23 C 0.5672(25) 0.0613(9) -0.3812(20) 0.057(7) Uiso 1 d . . H23A H 0.4961(52) 0.0646(56) -0.4294(32) 0.086 Uiso 1 calc R . H23B H 0.5869(167) 0.0327(17) -0.3738(48) 0.086 Uiso 1 calc R . H23C H 0.6253(115) 0.0763(41) -0.3943(73) 0.086 Uiso 1 calc R . C24 C 0.8064(19) 0.1276(7) 0.2371(16) 0.039(5) Uiso 1 d . . C25 C 0.8900(24) 0.1107(8) 0.3141(19) 0.054(6) Uiso 1 d . . H25 H 0.8856(24) 0.0825(8) 0.3212(19) 0.064 Uiso 1 calc R . C26 C 0.9767(33) 0.1304(13) 0.3795(26) 0.091(10) Uiso 1 d . . H26 H 1.0182(33) 0.1124(13) 0.4243(26) 0.109 Uiso 1 calc R . C27 C 1.0145(32) 0.1672(11) 0.3943(26) 0.080(9) Uiso 1 d . . H27 H 1.0768(32) 0.1719(11) 0.4459(26) 0.096 Uiso 1 calc R . C28 C 0.9701(25) 0.2002(8) 0.3398(20) 0.054(6) Uiso 1 d . . H28 H 1.0087(25) 0.2250(8) 0.3553(20) 0.065 Uiso 1 calc R . C29 C 0.8725(21) 0.2001(7) 0.2632(17) 0.045(5) Uiso 1 d . . H29 H 0.8609(21) 0.2253(7) 0.2337(17) 0.054 Uiso 1 calc R . C30 C 0.7870(23) 0.1712(8) 0.2194(18) 0.046(5) Uiso 1 d . . C31 C 0.6564(20) 0.2247(7) 0.1441(17) 0.042(5) Uiso 1 d . . H31A H 0.6756(20) 0.2380(7) 0.2017(17) 0.050 Uiso 1 calc R . H31B H 0.6994(20) 0.2382(7) 0.1123(17) 0.050 Uiso 1 calc R . C32 C 0.5355(19) 0.2311(7) 0.0945(16) 0.039(5) Uiso 1 d . . H32A H 0.5153(19) 0.2202(7) 0.0346(16) 0.047 Uiso 1 calc R . H32B H 0.5179(19) 0.2603(7) 0.0905(16) 0.047 Uiso 1 calc R . C33 C 0.4670(18) 0.2081(6) 0.1463(15) 0.032(4) Uiso 1 d . . H33A H 0.5001(18) 0.2147(6) 0.2092(15) 0.038 Uiso 1 calc R . H33B H 0.3892(18) 0.2179(6) 0.1249(15) 0.038 Uiso 1 calc R . C34 C 0.4242(17) 0.1395(7) 0.1832(13) 0.033(4) Uiso 1 d . . C35 C 0.3789(17) 0.1608(6) 0.2460(14) 0.027(4) Uiso 1 d . . H35 H 0.3656(17) 0.1889(6) 0.2375(14) 0.032 Uiso 1 calc R . C36 C 0.3552(21) 0.1435(8) 0.3141(17) 0.051(6) Uiso 1 d . . H36 H 0.3323(21) 0.1624(8) 0.3480(17) 0.062 Uiso 1 calc R . C37 C 0.3580(24) 0.1042(8) 0.3431(20) 0.056(6) Uiso 1 d . . H37 H 0.3362(24) 0.0993(8) 0.3919(20) 0.067 Uiso 1 calc R . C38 C 0.3911(24) 0.0710(8) 0.3045(19) 0.055(6) Uiso 1 d . . H38 H 0.4020(24) 0.0465(8) 0.3367(19) 0.066 Uiso 1 calc R . C39 C 0.4099(22) 0.0689(8) 0.2278(18) 0.049(6) Uiso 1 d . . H39 H 0.4145(22) 0.0416(8) 0.2115(18) 0.059 Uiso 1 calc R . C40 C 0.4244(19) 0.0954(7) 0.1655(16) 0.037(5) Uiso 1 d . . C41 C 0.7351(21) 0.0605(7) 0.1745(17) 0.043(5) Uiso 1 d . . H41 H 0.6726(21) 0.0532(7) 0.1196(17) 0.052 Uiso 1 calc R . C42 C 0.7005(22) 0.0394(7) 0.2489(17) 0.045(5) Uiso 1 d . . H42A H 0.6755(141) 0.0118(19) 0.2312(53) 0.068 Uiso 1 calc R . H42B H 0.6401(101) 0.0548(31) 0.2577(83) 0.068 Uiso 1 calc R . H42C H 0.7648(44) 0.0388(48) 0.3035(34) 0.068 Uiso 1 calc R . C43 C 0.8398(20) 0.0396(7) 0.1621(16) 0.040(5) Uiso 1 d . . H43A H 0.8399(75) 0.0453(42) 0.1033(39) 0.061 Uiso 1 calc R . H43B H 0.8361(75) 0.0104(8) 0.1697(109) 0.061 Uiso 1 calc R . H43C H 0.9082(21) 0.0501(36) 0.2056(68) 0.061 Uiso 1 calc R . C44 C 0.4009(18) 0.0470(6) 0.0533(15) 0.031(4) Uiso 1 d . . H44 H 0.4443(18) 0.0260(6) 0.0956(15) 0.038 Uiso 1 calc R . C45 C 0.2783(25) 0.0415(9) 0.0361(21) 0.063(7) Uiso 1 d . . H45A H 0.2534(48) 0.0157(31) 0.0060(129) 0.094 Uiso 1 calc R . H45B H 0.2365(30) 0.0636(35) -0.0007(118) 0.094 Uiso 1 calc R . H45C H 0.2653(34) 0.0415(67) 0.0916(23) 0.094 Uiso 1 calc R . C46 C 0.4213(27) 0.0425(9) -0.0329(20) 0.062(7) Uiso 1 d . . H46A H 0.5010(32) 0.0451(67) -0.0222(29) 0.093 Uiso 1 calc R . H46B H 0.3805(144) 0.0635(39) -0.0737(52) 0.093 Uiso 1 calc R . H46C H 0.3954(167) 0.0159(25) -0.0582(73) 0.093 Uiso 1 calc R . C47 C 1.0372(23) 0.1501(9) -0.0181(20) 0.056(7) Uiso 1 d . . H47A H 1.0551(23) 0.1273(9) -0.0499(20) 0.067 Uiso 1 calc R . H47B H 1.0465(23) 0.1755(9) -0.0466(20) 0.067 Uiso 1 calc R . C48 C 1.1113(29) 0.1498(10) 0.0723(22) 0.072(9) Uiso 1 d . . H48A H 1.1480(29) 0.1764(10) 0.0880(22) 0.086 Uiso 1 calc R . H48B H 1.1696(29) 0.1291(10) 0.0810(22) 0.086 Uiso 1 calc R . C49 C 1.0465(27) 0.1411(11) 0.1267(22) 0.075(8) Uiso 1 d . . H49A H 1.0661(27) 0.1599(11) 0.1768(22) 0.090 Uiso 1 calc R . H49B H 1.0605(27) 0.1132(11) 0.1493(22) 0.090 Uiso 1 calc R . C50 C 0.9289(20) 0.1461(7) 0.0707(16) 0.041(5) Uiso 1 d . . H50A H 0.8840(20) 0.1236(7) 0.0805(16) 0.050 Uiso 1 calc R . H50B H 0.8995(20) 0.1717(7) 0.0851(16) 0.050 Uiso 1 calc R . C51 C 0.2900(29) 0.1593(11) -0.0733(25) 0.073(9) Uiso 1 d . . H51A H 0.2443(29) 0.1346(11) -0.0812(25) 0.087 Uiso 1 calc R . H51B H 0.2963(29) 0.1723(11) -0.0172(25) 0.087 Uiso 1 calc R . C52 C 0.2475(51) 0.1853(19) -0.1420(40) 0.135(18) Uiso 1 d . . H52A H 0.2423(51) 0.2124(19) -0.1187(40) 0.162 Uiso 1 calc R . H52B H 0.1711(51) 0.1765(19) -0.1770(40) 0.162 Uiso 1 calc R . C53 C 0.3157(48) 0.1884(18) -0.2030(40) 0.132(17) Uiso 1 d . . H53A H 0.2702(48) 0.1834(18) -0.2650(40) 0.158 Uiso 1 calc R . H53B H 0.3554(48) 0.2144(18) -0.1971(40) 0.158 Uiso 1 calc R . C54 C 0.3872(32) 0.1562(11) -0.1649(25) 0.077(9) Uiso 1 d . . H54A H 0.3573(32) 0.1312(11) -0.1978(25) 0.092 Uiso 1 calc R . H54B H 0.4610(32) 0.1615(11) -0.1692(25) 0.092 Uiso 1 calc R . C55 C 0.3031(40) -0.0090(15) -0.4696(35) 0.117(15) Uiso 1 d . . H55A H 0.3159(40) 0.0017(15) -0.4103(35) 0.141 Uiso 1 calc R . H55B H 0.3600(40) -0.0297(15) -0.4664(35) 0.141 Uiso 1 calc R . C56 C 0.1730(56) -0.0275(21) -0.5160(48) 0.159(22) Uiso 1 d . . H56A H 0.1663(56) -0.0455(21) -0.5659(48) 0.191 Uiso 1 calc R . H56B H 0.1480(56) -0.0420(21) -0.4732(48) 0.191 Uiso 1 calc R . C57 C 0.1102(44) 0.0124(16) -0.5456(37) 0.119(15) Uiso 1 d . . H57A H 0.0537(44) 0.0103(16) -0.6050(37) 0.143 Uiso 1 calc R . H57B H 0.0742(44) 0.0216(16) -0.5044(37) 0.143 Uiso 1 calc R . C58 C 0.1969(45) 0.0377(18) -0.5441(42) 0.132(17) Uiso 1 d . . H58A H 0.2032(45) 0.0591(18) -0.5004(42) 0.158 Uiso 1 calc R . H58B H 0.1762(45) 0.0509(18) -0.6018(42) 0.158 Uiso 1 calc R . C59 C 0.6537(53) 0.1656(19) -0.4862(41) 0.136(18) Uiso 1 d . . H59A H 0.7066(53) 0.1611(19) -0.4261(41) 0.163 Uiso 1 calc R . H59B H 0.5820(53) 0.1526(19) -0.4922(41) 0.163 Uiso 1 calc R . C60 C 0.6939(58) 0.1508(20) -0.5446(46) 0.157(23) Uiso 1 d . . H60A H 0.6359(58) 0.1363(20) -0.5918(46) 0.188 Uiso 1 calc R . H60B H 0.7574(58) 0.1325(20) -0.5169(46) 0.188 Uiso 1 calc R . C61 C 0.7315(67) 0.1894(24) -0.5793(53) 0.178(26) Uiso 1 d . . H61A H 0.8097(67) 0.1870(24) -0.5760(53) 0.213 Uiso 1 calc R . H61B H 0.6838(67) 0.1946(24) -0.6407(53) 0.213 Uiso 1 calc R . C62 C 0.7197(63) 0.2232(22) -0.5201(48) 0.159(24) Uiso 1 d . . H62A H 0.7849(63) 0.2245(22) -0.4652(48) 0.191 Uiso 1 calc R . H62B H 0.7094(63) 0.2497(22) -0.5498(48) 0.191 Uiso 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 0.0312(6) 0.0302(5) 0.0307(7) 0.0058(5) 0.0129(6) 0.0020(5) Nd2 0.0321(6) 0.0270(5) 0.0284(7) -0.0004(5) 0.0120(5) 0.0014(5) Cl1 0.041(3) 0.033(2) 0.037(3) 0.006(2) 0.020(3) 0.004(2) Cl2 0.049(3) 0.039(3) 0.043(3) 0.004(3) 0.025(3) 0.004(3) O1 0.031(8) 0.064(12) 0.038(10) 0.003(8) 0.002(8) 0.001(7) O2 0.039(10) 0.085(13) 0.034(11) 0.011(8) 0.021(9) 0.019(8) N1 0.043(12) 0.041(11) 0.052(14) 0.008(9) 0.026(12) 0.018(8) N2 0.068(14) 0.015(8) 0.036(12) -0.014(7) 0.017(11) 0.001(7) N3 0.026(9) 0.055(12) 0.041(12) 0.008(9) 0.013(10) -0.014(8) N4 0.013(8) 0.064(13) 0.036(12) 0.014(9) -0.001(8) 0.006(8) N5 0.046(12) 0.020(8) 0.025(10) -0.004(6) 0.010(9) 0.008(7) N6 0.047(13) 0.045(11) 0.044(13) 0.001(9) 0.023(12) 0.002(9) N8 0.037(11) 0.051(11) 0.045(13) -0.024(9) 0.029(11) -0.008(8) _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 N4 2.38(2) . ? Nd1 N3 2.40(2) . ? Nd1 N2 2.41(2) . ? Nd1 N1 2.51(2) . ? Nd1 O1 2.59(2) . ? Nd1 Cl2 2.868(6) . ? Nd1 Cl1 2.886(5) . ? Nd2 N6 2.40(2) . ? Nd2 N5 2.43(2) . ? Nd2 N7 2.445(14) . ? Nd2 N8 2.52(2) . ? Nd2 O2 2.56(2) . ? Nd2 Cl2 2.934(6) . ? Nd2 Cl1 2.938(5) . ? O1 C50 1.45(3) . ? O1 C47 1.46(3) . ? O2 C54 1.37(4) . ? O2 C51 1.45(3) . ? O3 C55 1.32(6) . ? O3 C58 1.39(6) . ? O4 C62 1.19(7) . ? O4 C59 1.58(8) . ? N1 C1 1.33(2) . ? N1 C18 1.49(3) . ? N2 C7 1.35(2) . ? N2 C8 1.49(3) . ? N3 C11 1.31(3) . ? N3 C10 1.57(3) . ? N4 C17 1.34(3) . ? N4 C21 1.51(3) . ? N5 C24 1.34(3) . ? N5 C41 1.47(3) . ? N6 C30 1.28(3) . ? N6 C31 1.51(3) . ? N7 C34 1.36(2) . ? N7 C33 1.44(2) . ? N8 C40 1.27(3) . ? N8 C44 1.52(3) . ? C1 C2 1.43(3) . ? C1 C7 1.45(3) . ? C2 C3 1.36(3) . ? C3 C4 1.35(4) . ? C4 C5 1.32(5) . ? C5 C6 1.46(3) . ? C6 C7 1.43(3) . ? C8 C9 1.50(3) . ? C9 C10 1.53(3) . ? C11 C17 1.45(3) . ? C11 C12 1.47(3) . ? C12 C13 1.37(3) . ? C13 C14 1.31(4) . ? C14 C15 1.38(3) . ? C15 C16 1.42(4) . ? C16 C17 1.41(3) . ? C18 C20 1.55(4) . ? C18 C19 1.55(4) . ? C21 C23 1.52(3) . ? C21 C22 1.53(3) . ? C24 C25 1.43(4) . ? C24 C30 1.46(3) . ? C25 C26 1.39(5) . ? C26 C27 1.29(5) . ? C27 C28 1.39(4) . ? C28 C29 1.41(4) . ? C29 C30 1.43(4) . ? C31 C32 1.48(3) . ? C32 C33 1.60(3) . ? C34 C40 1.48(3) . ? C34 C35 1.51(2) . ? C35 C36 1.36(3) . ? C36 C37 1.37(4) . ? C37 C38 1.39(4) . ? C38 C39 1.35(3) . ? C39 C40 1.39(3) . ? C41 C43 1.57(3) . ? C41 C42 1.58(3) . ? C44 C45 1.50(3) . ? C44 C46 1.51(3) . ? C47 C48 1.43(4) . ? C48 C49 1.43(4) . ? C49 C50 1.46(4) . ? C51 C52 1.35(6) . ? C52 C53 1.53(6) . ? C53 C54 1.39(6) . ? C55 C56 1.67(8) . ? C56 C57 1.52(8) . ? C57 C58 1.37(6) . ? C59 C60 1.32(7) . ? C60 C61 1.53(9) . ? C61 C62 1.51(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 N4 Nd1 N3 63.1(7) . . ? N4 Nd1 N2 107.8(6) . . ? N3 Nd1 N2 75.2(6) . . ? N4 Nd1 N1 94.4(7) . . ? N3 Nd1 N1 124.3(6) . . ? N2 Nd1 N1 64.1(6) . . ? N4 Nd1 O1 170.9(6) . . ? N3 Nd1 O1 125.7(6) . . ? N2 Nd1 O1 78.3(6) . . ? N1 Nd1 O1 82.2(6) . . ? N4 Nd1 Cl2 102.9(5) . . ? N3 Nd1 Cl2 77.0(5) . . ? N2 Nd1 Cl2 122.1(4) . . ? N1 Nd1 Cl2 157.5(5) . . ? O1 Nd1 Cl2 78.5(4) . . ? N4 Nd1 Cl1 87.3(4) . . ? N3 Nd1 Cl1 131.6(4) . . ? N2 Nd1 Cl1 153.1(5) . . ? N1 Nd1 Cl1 93.3(4) . . ? O1 Nd1 Cl1 84.5(4) . . ? Cl2 Nd1 Cl1 73.51(13) . . ? N6 Nd2 N5 62.9(7) . . ? N6 Nd2 N7 71.3(6) . . ? N5 Nd2 N7 101.7(5) . . ? N6 Nd2 N8 121.5(6) . . ? N5 Nd2 N8 92.8(6) . . ? N7 Nd2 N8 62.5(5) . . ? N6 Nd2 O2 126.2(7) . . ? N5 Nd2 O2 170.8(6) . . ? N7 Nd2 O2 82.3(5) . . ? N8 Nd2 O2 81.6(6) . . ? N6 Nd2 Cl2 74.4(5) . . ? N5 Nd2 Cl2 108.1(4) . . ? N7 Nd2 Cl2 116.1(4) . . ? N8 Nd2 Cl2 158.4(5) . . ? O2 Nd2 Cl2 77.0(4) . . ? N6 Nd2 Cl1 119.5(4) . . ? N5 Nd2 Cl1 82.2(4) . . ? N7 Nd2 Cl1 168.8(4) . . ? N8 Nd2 Cl1 107.1(4) . . ? O2 Nd2 Cl1 92.4(4) . . ? Cl2 Nd2 Cl1 71.81(13) . . ? Nd1 Cl1 Nd2 107.0(2) . . ? Nd1 Cl2 Nd2 107.6(2) . . ? C50 O1 C47 105.7(19) . . ? C50 O1 Nd1 127.6(13) . . ? C47 O1 Nd1 126.7(14) . . ? C54 O2 C51 105.2(24) . . ? C54 O2 Nd2 130.0(18) . . ? C51 O2 Nd2 124.7(16) . . ? C55 O3 C58 102.6(44) . . ? C62 O4 C59 104.8(60) . . ? C1 N1 C18 127.1(17) . . ? C1 N1 Nd1 119.8(14) . . ? C18 N1 Nd1 112.5(12) . . ? C7 N2 C8 117.4(17) . . ? C7 N2 Nd1 122.5(13) . . ? C8 N2 Nd1 118.9(12) . . ? C11 N3 C10 117.8(18) . . ? C11 N3 Nd1 123.0(13) . . ? C10 N3 Nd1 118.2(14) . . ? C17 N4 C21 119.6(19) . . ? C17 N4 Nd1 125.8(16) . . ? C21 N4 Nd1 114.4(12) . . ? C24 N5 C41 122.4(19) . . ? C24 N5 Nd2 124.2(14) . . ? C41 N5 Nd2 112.9(14) . . ? C30 N6 C31 120.3(21) . . ? C30 N6 Nd2 124.3(16) . . ? C31 N6 Nd2 115.1(16) . . ? C34 N7 C33 121.2(15) . . ? C34 N7 Nd2 117.3(12) . . ? C33 N7 Nd2 120.4(10) . . ? C40 N8 C44 114.8(17) . . ? C40 N8 Nd2 117.1(15) . . ? C44 N8 Nd2 123.8(10) . . ? N1 C1 C2 122.2(21) . . ? N1 C1 C7 115.5(17) . . ? C2 C1 C7 122.3(18) . . ? C3 C2 C1 133.0(23) . . ? C2 C3 C4 130.9(27) . . ? C5 C4 C3 127.0(29) . . ? C4 C5 C6 128.9(29) . . ? C7 C6 C5 130.6(25) . . ? N2 C7 C6 121.7(20) . . ? N2 C7 C1 114.6(16) . . ? C6 C7 C1 123.6(17) . . ? N2 C8 C9 110.4(18) . . ? C8 C9 C10 113.1(21) . . ? C9 C10 N3 106.2(17) . . ? N3 C11 C17 115.8(19) . . ? N3 C11 C12 123.9(19) . . ? C17 C11 C12 120.1(21) . . ? C13 C12 C11 137.7(22) . . ? C14 C13 C12 126.5(26) . . ? C13 C14 C15 127.8(29) . . ? C14 C15 C16 131.2(27) . . ? C17 C16 C15 129.9(25) . . ? N4 C17 C16 122.6(20) . . ? N4 C17 C11 110.8(21) . . ? C16 C17 C11 126.6(21) . . ? N1 C18 C20 115.3(21) . . ? N1 C18 C19 108.5(23) . . ? C20 C18 C19 114.9(23) . . ? N4 C21 C23 117.0(17) . . ? N4 C21 C22 115.7(16) . . ? C23 C21 C22 113.5(20) . . ? N5 C24 C25 124.0(21) . . ? N5 C24 C30 111.2(22) . . ? C25 C24 C30 124.8(23) . . ? C26 C25 C24 128.9(29) . . ? C27 C26 C25 136.0(42) . . ? C26 C27 C28 124.8(41) . . ? C27 C28 C29 126.5(29) . . ? C28 C29 C30 135.7(25) . . ? N6 C30 C29 123.7(24) . . ? N6 C30 C24 115.6(23) . . ? C29 C30 C24 120.4(25) . . ? C32 C31 N6 115.5(19) . . ? C31 C32 C33 107.6(20) . . ? N7 C33 C32 112.8(15) . . ? N7 C34 C40 117.1(16) . . ? N7 C34 C35 115.0(18) . . ? C40 C34 C35 127.9(16) . . ? C36 C35 C34 126.7(20) . . ? C35 C36 C37 133.0(23) . . ? C36 C37 C38 124.0(24) . . ? C39 C38 C37 129.3(27) . . ? C38 C39 C40 138.3(25) . . ? N8 C40 C39 131.7(22) . . ? N8 C40 C34 110.7(18) . . ? C39 C40 C34 117.6(19) . . ? N5 C41 C43 116.1(18) . . ? N5 C41 C42 116.3(17) . . ? C43 C41 C42 112.5(21) . . ? C45 C44 C46 108.7(23) . . ? C45 C44 N8 109.0(17) . . ? C46 C44 N8 110.3(17) . . ? C48 C47 O1 108.8(21) . . ? C47 C48 C49 108.4(27) . . ? C48 C49 C50 106.3(27) . . ? O1 C50 C49 108.4(19) . . ? C52 C51 O2 101.1(30) . . ? C51 C52 C53 114.8(45) . . ? C54 C53 C52 95.3(41) . . ? O2 C54 C53 112.2(34) . . ? O3 C55 C56 101.3(45) . . ? C57 C56 C55 98.8(50) . . ? C58 C57 C56 100.7(52) . . ? C57 C58 O3 117.8(58) . . ? C60 C59 O4 105.4(51) . . ? C59 C60 C61 102.1(61) . . ? C62 C61 C60 105.2(58) . . ? O4 C62 C61 101.2(65) . . ? _refine_diff_density_max 1.779 _refine_diff_density_min -1.573 _refine_diff_density_rms 0.198 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_autor ; Peter W. Roesky Universit\"at Karlsruhe Engesserstr. Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author_phone '049 721 608-2855' _publ_contact_author_fax '049 721 661921' _publ_contact_author_email 'roesky@achibm6.chemie.uni-karlsruhe.de' _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ' Bridged Aminotroponiminate Complexes of the Lanthanides - A Structural Contribution ' ; loop_ _publ_author_name _publ_author_address 'Peter W. Roesky, Markus R. Brgstein' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr, Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; #============================================================================== data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25.50 H36 Cl Er N4' _chemical_formula_weight 601.29 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4158(3) _cell_length_b 11.4180(4) _cell_length_c 13.0820(3) _cell_angle_alpha 66.54(2) _cell_angle_beta 73.770(3) _cell_angle_gamma 84.825(4) _cell_volume 1238.41(7) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 30 _cell_measurement_theta_max 45 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method ? _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 3.516 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device STOE-STADI IV _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 2 hours _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 4360 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0110 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4360 _reflns_number_observed 4240 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0322P)^2^+1.5494P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4359 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_obs 0.0177 _refine_ls_wR_factor_all 0.0499 _refine_ls_wR_factor_obs 0.0489 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.019 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.019 _refine_ls_shift/esd_max -0.027 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Er Er 0.874902(12) 0.502761(10) 0.663685(9) 0.01967(5) Uani 1 d . . Cl Cl 0.87572(8) 0.39064(7) 0.51801(6) 0.02807(15) Uani 1 d . . N1 N 0.9107(2) 0.6829(2) 0.7000(2) 0.0219(5) Uani 1 d . . N2 N 0.7171(2) 0.6625(2) 0.5987(2) 0.0217(5) Uani 1 d . . N3 N 0.6486(2) 0.4219(2) 0.7957(2) 0.0238(5) Uani 1 d . . N4 N 0.8983(3) 0.3223(2) 0.8238(2) 0.0242(5) Uani 1 d . . C1 C 0.8504(3) 0.7923(3) 0.6461(2) 0.0217(5) Uani 1 d . . C2 C 0.8668(4) 0.9069(3) 0.6598(3) 0.0342(7) Uani 1 d . . H2 H 0.9115(4) 0.8954(3) 0.7189(3) 0.041 Uiso 1 calc R . C3 C 0.8305(4) 1.0327(3) 0.6041(3) 0.0415(8) Uani 1 d . . H3 H 0.8582(4) 1.0910(3) 0.6298(3) 0.050 Uiso 1 calc R . C4 C 0.7600(4) 1.0859(3) 0.5167(3) 0.0386(8) Uani 1 d . . H4 H 0.7522(4) 1.1752(3) 0.4860(3) 0.046 Uiso 1 calc R . C5 C 0.7010(4) 1.0190(3) 0.4713(3) 0.0343(7) Uani 1 d . . H5 H 0.6573(4) 1.0692(3) 0.4119(3) 0.041 Uiso 1 calc R . C6 C 0.6953(3) 0.8884(3) 0.4993(2) 0.0275(6) Uani 1 d . . H6 H 0.6439(3) 0.8659(3) 0.4574(2) 0.033 Uiso 1 calc R . C7 C 0.7513(3) 0.7822(3) 0.5782(2) 0.0220(5) Uani 1 d . . C8 C 0.5862(3) 0.6419(3) 0.5669(2) 0.0265(6) Uani 1 d . . H8A H 0.6132(3) 0.6569(3) 0.4847(2) 0.032 Uiso 1 calc R . H8B H 0.5101(3) 0.7028(3) 0.5798(2) 0.032 Uiso 1 calc R . C9 C 0.5246(3) 0.5061(3) 0.6388(3) 0.0271(6) Uani 1 d . . H9A H 0.4280(3) 0.4994(3) 0.6267(3) 0.032 Uiso 1 calc R . H9B H 0.5909(3) 0.4472(3) 0.6114(3) 0.032 Uiso 1 calc R . C10 C 0.5069(3) 0.4648(3) 0.7683(2) 0.0275(6) Uani 1 d . . H10A H 0.4721(3) 0.5367(3) 0.7911(2) 0.033 Uiso 1 calc R . H10B H 0.4328(3) 0.3952(3) 0.8121(2) 0.033 Uiso 1 calc R . C11 C 0.6477(3) 0.3576(3) 0.9063(2) 0.0234(6) Uani 1 d . . C12 C 0.5194(3) 0.3488(3) 0.9978(3) 0.0319(7) Uani 1 d . . H12 H 0.4395(3) 0.3950(3) 0.9723(3) 0.038 Uiso 1 calc R . C13 C 0.4882(3) 0.2863(3) 1.1162(3) 0.0356(7) Uani 1 d . . H13 H 0.3932(3) 0.2998(3) 1.1572(3) 0.043 Uiso 1 calc R . C14 C 0.5753(4) 0.2067(3) 1.1842(3) 0.0359(7) Uani 1 d . . H14 H 0.5329(4) 0.1709(3) 1.2645(3) 0.043 Uiso 1 calc R . C15 C 0.7189(4) 0.1758(3) 1.1437(3) 0.0320(7) Uani 1 d . . H15 H 0.7623(4) 0.1195(3) 1.2012(3) 0.038 Uiso 1 calc R . C16 C 0.8101(3) 0.2144(3) 1.0319(3) 0.0279(6) Uani 1 d . . H16 H 0.9043(3) 0.1785(3) 1.0278(3) 0.033 Uiso 1 calc R . C17 C 0.7910(3) 0.2962(2) 0.9229(2) 0.0223(5) Uani 1 d . . C18 C 1.0014(3) 0.6805(3) 0.7772(2) 0.0266(6) Uani 1 d . . H18 H 1.0499(3) 0.7655(3) 0.7472(2) 0.032 Uiso 1 calc R . C19 C 0.9024(4) 0.6525(4) 0.8994(3) 0.0379(7) Uani 1 d . . H19A H 0.9629(5) 0.6477(24) 0.9499(6) 0.057 Uiso 1 calc R . H19B H 0.8496(21) 0.5718(12) 0.9279(9) 0.057 Uiso 1 calc R . H19C H 0.8319(19) 0.7202(13) 0.8977(5) 0.057 Uiso 1 calc R . C20 C 1.1200(3) 0.5815(3) 0.7792(3) 0.0352(7) Uani 1 d . . H20A H 1.1820(17) 0.5848(16) 0.8260(18) 0.053 Uiso 1 calc R . H20B H 1.1801(17) 0.5990(14) 0.7010(4) 0.053 Uiso 1 calc R . H20C H 1.0739(3) 0.4973(4) 0.8118(20) 0.053 Uiso 1 calc R . C21 C 1.0321(3) 0.2429(3) 0.8250(2) 0.0283(6) Uani 1 d . . H21 H 1.0736(3) 0.2408(3) 0.8874(2) 0.034 Uiso 1 calc R . C22 C 0.9947(4) 0.1076(3) 0.8447(3) 0.0418(8) Uani 1 d . . H22A H 1.0819(9) 0.0558(7) 0.8507(23) 0.063 Uiso 1 calc R . H22B H 0.9617(28) 0.1089(4) 0.7803(12) 0.063 Uiso 1 calc R . H22C H 0.9166(21) 0.0715(10) 0.9157(12) 0.063 Uiso 1 calc R . C23 C 1.1471(4) 0.2997(3) 0.7093(3) 0.0388(8) Uani 1 d . . H23A H 1.2351(11) 0.2485(14) 0.7108(8) 0.058 Uiso 1 calc R . H23B H 1.1724(21) 0.3864(9) 0.6949(11) 0.058 Uiso 1 calc R . H23C H 1.1072(11) 0.3003(23) 0.6482(4) 0.058 Uiso 1 calc R . C24 C 0.4966(14) -0.1234(12) 0.2014(11) 0.179(4) Uiso 1 d . . C25A C 0.4138(13) -0.0421(11) 0.1147(10) 0.080(3) Uiso 0.50 d P 1 C25B C 0.5979(19) -0.0838(17) 0.0646(15) 0.125(5) Uiso 0.50 d P 2 C26 C 0.5000 0.0000 0.0000 0.119(3) Uiso 1 d S . 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 Er 0.01692(7) 0.01933(8) 0.01895(8) -0.00635(5) -0.00105(5) 0.00172(5) Cl 0.0254(3) 0.0289(3) 0.0280(3) -0.0150(3) 0.0037(3) -0.0065(3) N1 0.0184(11) 0.0257(12) 0.0210(11) -0.0090(9) -0.0053(9) 0.0026(9) N2 0.0182(11) 0.0246(12) 0.0214(11) -0.0085(10) -0.0053(9) 0.0024(9) N3 0.0171(11) 0.0245(12) 0.0234(12) -0.0053(10) -0.0011(9) -0.0008(9) N4 0.0209(12) 0.0206(11) 0.0247(12) -0.0055(10) -0.0019(9) 0.0027(9) C1 0.0200(13) 0.0231(13) 0.0185(13) -0.0068(11) -0.0014(10) 0.0004(10) C2 0.038(2) 0.028(2) 0.041(2) -0.0136(14) -0.0190(14) 0.0050(13) C3 0.052(2) 0.025(2) 0.054(2) -0.017(2) -0.023(2) 0.0030(14) C4 0.048(2) 0.0199(15) 0.041(2) -0.0053(13) -0.012(2) 0.0066(13) C5 0.037(2) 0.028(2) 0.028(2) -0.0024(13) -0.0096(13) 0.0090(13) C6 0.0278(15) 0.0280(15) 0.0235(14) -0.0067(12) -0.0077(12) 0.0039(12) C7 0.0191(13) 0.0254(14) 0.0191(13) -0.0084(11) -0.0028(10) 0.0031(11) C8 0.0210(14) 0.034(2) 0.0249(14) -0.0112(12) -0.0080(11) 0.0020(12) C9 0.0182(13) 0.035(2) 0.032(2) -0.0161(13) -0.0070(11) 0.0005(11) C10 0.0170(13) 0.032(2) 0.0278(15) -0.0082(12) -0.0033(11) 0.0008(11) C11 0.0216(14) 0.0203(13) 0.0247(14) -0.0075(11) -0.0019(11) -0.0010(11) C12 0.0227(15) 0.038(2) 0.027(2) -0.0089(13) -0.0008(12) 0.0044(12) C13 0.025(2) 0.047(2) 0.027(2) -0.0133(14) 0.0027(12) 0.0022(13) C14 0.036(2) 0.045(2) 0.0203(14) -0.0110(14) 0.0000(13) 0.0002(14) C15 0.034(2) 0.038(2) 0.0210(14) -0.0086(13) -0.0080(12) 0.0013(13) C16 0.0251(14) 0.0306(15) 0.0265(15) -0.0102(12) -0.0068(12) 0.0031(12) C17 0.0230(14) 0.0193(13) 0.0234(14) -0.0086(11) -0.0033(11) -0.0017(10) C18 0.0251(14) 0.0293(15) 0.0277(15) -0.0111(12) -0.0104(12) 0.0000(12) C19 0.035(2) 0.054(2) 0.029(2) -0.019(2) -0.0132(14) 0.0046(15) C20 0.029(2) 0.040(2) 0.040(2) -0.0151(15) -0.0164(14) 0.0086(13) C21 0.0248(15) 0.030(2) 0.0241(14) -0.0074(12) -0.0046(12) 0.0093(12) C22 0.049(2) 0.030(2) 0.039(2) -0.0112(14) -0.008(2) 0.0123(15) C23 0.029(2) 0.040(2) 0.035(2) -0.0106(15) 0.0018(14) 0.0115(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er N2 2.289(2) . ? Er N3 2.324(2) . ? Er N4 2.328(2) . ? Er N1 2.359(2) . ? Er Cl 2.6838(8) . ? Er Cl 2.7816(8) 2_766 ? Cl Er 2.7816(8) 2_766 ? N1 C1 1.333(4) . ? N1 C18 1.485(3) . ? N2 C7 1.335(4) . ? N2 C8 1.471(3) . ? N3 C11 1.335(4) . ? N3 C10 1.469(4) . ? N4 C17 1.344(4) . ? N4 C21 1.484(3) . ? C1 C2 1.418(4) . ? C1 C7 1.495(4) . ? C2 C3 1.388(5) . ? C3 C4 1.384(5) . ? C4 C5 1.366(5) . ? C5 C6 1.389(4) . ? C6 C7 1.417(4) . ? C8 C9 1.524(4) . ? C9 C10 1.530(4) . ? C11 C12 1.421(4) . ? C11 C17 1.494(4) . ? C12 C13 1.378(4) . ? C13 C14 1.385(5) . ? C14 C15 1.377(5) . ? C15 C16 1.387(4) . ? C16 C17 1.410(4) . ? C18 C20 1.513(4) . ? C18 C19 1.530(4) . ? C21 C23 1.521(4) . ? C21 C22 1.519(5) . ? C24 C25A 1.51(2) . ? C24 C25B 1.67(2) . ? C25A C26 1.399(12) . ? C25B C26 1.45(2) . ? C26 C25A 1.399(12) 2_655 ? C26 C25B 1.45(2) 2_655 ? 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 Er N3 77.59(8) . . ? N2 Er N4 143.02(8) . . ? N3 Er N4 67.16(8) . . ? N2 Er N1 68.29(8) . . ? N3 Er N1 101.56(8) . . ? N4 Er N1 107.37(8) . . ? N2 Er Cl 96.67(6) . . ? N3 Er Cl 98.50(6) . . ? N4 Er Cl 99.16(6) . . ? N1 Er Cl 151.35(6) . . ? N2 Er Cl 96.62(6) . 2_766 ? N3 Er Cl 171.95(6) . 2_766 ? N4 Er Cl 119.50(6) . 2_766 ? N1 Er Cl 81.15(6) . 2_766 ? Cl Er Cl 76.43(2) . 2_766 ? Er Cl Er 103.57(2) . 2_766 ? C1 N1 C18 118.8(2) . . ? C1 N1 Er 118.3(2) . . ? C18 N1 Er 122.8(2) . . ? C7 N2 C8 117.7(2) . . ? C7 N2 Er 119.2(2) . . ? C8 N2 Er 122.9(2) . . ? C11 N3 C10 118.3(2) . . ? C11 N3 Er 117.6(2) . . ? C10 N3 Er 122.3(2) . . ? C17 N4 C21 118.5(2) . . ? C17 N4 Er 117.9(2) . . ? C21 N4 Er 123.3(2) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 C7 114.6(2) . . ? C2 C1 C7 122.0(2) . . ? C3 C2 C1 133.3(3) . . ? C4 C3 C2 130.3(3) . . ? C5 C4 C3 125.2(3) . . ? C4 C5 C6 130.1(3) . . ? C5 C6 C7 133.0(3) . . ? N2 C7 C6 121.6(3) . . ? N2 C7 C1 114.3(2) . . ? C6 C7 C1 124.2(3) . . ? N2 C8 C9 110.5(2) . . ? C10 C9 C8 113.4(2) . . ? N3 C10 C9 110.4(2) . . ? N3 C11 C12 121.7(3) . . ? N3 C11 C17 113.8(2) . . ? C12 C11 C17 124.4(3) . . ? C13 C12 C11 133.1(3) . . ? C14 C13 C12 129.9(3) . . ? C15 C14 C13 125.3(3) . . ? C14 C15 C16 130.4(3) . . ? C15 C16 C17 133.5(3) . . ? N4 C17 C16 123.2(3) . . ? N4 C17 C11 113.7(2) . . ? C16 C17 C11 123.1(2) . . ? N1 C18 C20 110.5(2) . . ? N1 C18 C19 110.0(2) . . ? C20 C18 C19 110.4(3) . . ? N4 C21 C23 109.7(2) . . ? N4 C21 C22 110.8(3) . . ? C23 C21 C22 108.1(3) . . ? C26 C25A C24 113.6(9) . . ? C26 C25B C24 102.2(11) . . ? C25A C26 C25A 179.999(1) . 2_655 ? C25B C26 C25B 179.999(2) 2_655 . ? _refine_diff_density_max 0.848 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.080 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_autor ; Peter W. Roesky Universit\"at Karlsruhe Engesserstr. Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author_phone '049 721 608-2855' _publ_contact_author_fax '049 721 661921' _publ_contact_author_email 'roesky@achibm6.chemie.uni-karlsruhe.de' _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ' Bridged Aminotroponiminate Complexes of the Lanthanides - A Structural Contribution ' ; loop_ _publ_author_name _publ_author_address 'Peter W. Roesky, Markus R. Brgstein' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr, Geb.30.45 76128 Karlsruhe Bundesrepublik Deutschland ; #============================================================================== data_pr179a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C51 H72 Cl2 N8 Yb2' _chemical_formula_weight 1214.15 _chemical_melting_point ? _chemical_compound_source ? 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' '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.431(2) _cell_length_b 11.360(3) _cell_length_c 13.083(2) _cell_angle_alpha 66.38(3) _cell_angle_beta 73.44(2) _cell_angle_gamma 84.68(3) _cell_volume 1230.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method ? _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 3.929 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 STOE STADI IV _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4844 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.07 _reflns_number_total 4844 _reflns_number_observed 4570 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.5494P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4842 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_obs 0.0223 _refine_ls_wR_factor_all 0.0591 _refine_ls_wR_factor_obs 0.0562 _refine_ls_goodness_of_fit_all 1.101 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.104 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Yb Yb 0.873019(14) 0.503087(13) 0.662900(11) 0.02146(6) Uani 1 d . . Cl Cl 0.87810(9) 0.39074(8) 0.51795(7) 0.0295(2) Uani 1 d . . N1 N 0.9101(3) 0.6816(3) 0.6990(2) 0.0231(6) Uani 1 d . . N2 N 0.7186(3) 0.6623(3) 0.5969(2) 0.0236(6) Uani 1 d . . N3 N 0.6493(3) 0.4224(3) 0.7945(2) 0.0252(6) Uani 1 d . . N4 N 0.8989(3) 0.3236(3) 0.8214(2) 0.0270(6) Uani 1 d . . C1 C 0.8509(4) 0.7917(3) 0.6449(3) 0.0238(7) Uani 1 d . . C2 C 0.8665(5) 0.9065(4) 0.6592(4) 0.0354(8) Uani 1 d . . H2 H 0.9114(5) 0.8942(4) 0.7190(4) 0.043 Uiso 1 calc R . C3 C 0.8301(5) 1.0329(4) 0.6045(4) 0.0423(10) Uani 1 d . . H3 H 0.8575(5) 1.0916(4) 0.6311(4) 0.051 Uiso 1 calc R . C4 C 0.7601(5) 1.0870(4) 0.5169(4) 0.0411(9) Uani 1 d . . H4 H 0.7521(5) 1.1778(4) 0.4862(4) 0.049 Uiso 1 calc R . C5 C 0.7012(4) 1.0202(4) 0.4710(3) 0.0355(8) Uani 1 d . . H5 H 0.6572(4) 1.0716(4) 0.4110(3) 0.043 Uiso 1 calc R . C6 C 0.6961(4) 0.8892(3) 0.4988(3) 0.0296(7) Uani 1 d . . H6 H 0.6438(4) 0.8664(3) 0.4568(3) 0.036 Uiso 1 calc R . C7 C 0.7527(4) 0.7827(3) 0.5768(3) 0.0236(7) Uani 1 d . . C8 C 0.5878(4) 0.6422(3) 0.5657(3) 0.0277(7) Uani 1 d . . H8A H 0.6150(4) 0.6577(3) 0.4824(3) 0.033 Uiso 1 calc R . H8B H 0.5113(4) 0.7043(3) 0.5789(3) 0.033 Uiso 1 calc R . C9 C 0.5251(4) 0.5053(4) 0.6381(3) 0.0292(7) Uani 1 d . . H9A H 0.4276(4) 0.4989(4) 0.6261(3) 0.035 Uiso 1 calc R . H9B H 0.5918(4) 0.4452(4) 0.6106(3) 0.035 Uiso 1 calc R . C10 C 0.5072(4) 0.4648(4) 0.7668(3) 0.0297(7) Uani 1 d . . H10A H 0.4713(4) 0.5380(4) 0.7893(3) 0.036 Uiso 1 calc R . H10B H 0.4327(4) 0.3938(4) 0.8117(3) 0.036 Uiso 1 calc R . C11 C 0.6488(4) 0.3583(3) 0.9051(3) 0.0251(7) Uani 1 d . . C12 C 0.5197(4) 0.3491(4) 0.9974(3) 0.0334(8) Uani 1 d . . H12 H 0.4387(4) 0.3956(4) 0.9720(3) 0.040 Uiso 1 calc R . C13 C 0.4890(4) 0.2864(4) 1.1161(3) 0.0388(9) Uani 1 d . . H13 H 0.3926(4) 0.2991(4) 1.1580(3) 0.047 Uiso 1 calc R . C14 C 0.5764(4) 0.2079(4) 1.1836(3) 0.0372(9) Uani 1 d . . H14 H 0.5337(4) 0.1716(4) 1.2651(3) 0.045 Uiso 1 calc R . C15 C 0.7207(4) 0.1780(4) 1.1426(3) 0.0339(8) Uani 1 d . . H15 H 0.7651(4) 0.1221(4) 1.2007(3) 0.041 Uiso 1 calc R . C16 C 0.8118(4) 0.2164(4) 1.0299(3) 0.0297(7) Uani 1 d . . H16 H 0.9073(4) 0.1804(4) 1.0255(3) 0.036 Uiso 1 calc R . C17 C 0.7918(4) 0.2975(3) 0.9211(3) 0.0249(7) Uani 1 d . . C18 C 1.0008(4) 0.6790(3) 0.7762(3) 0.0274(7) Uani 1 d . . H18 H 1.0493(4) 0.7656(3) 0.7456(3) 0.033 Uiso 1 calc R . C19 C 0.9023(5) 0.6508(4) 0.8984(3) 0.0400(9) Uani 1 d . . H19A H 0.9636(6) 0.6452(30) 0.9493(7) 0.060 Uiso 1 calc R . H19B H 0.8484(26) 0.5690(15) 0.9275(11) 0.060 Uiso 1 calc R . H19C H 0.8316(23) 0.7199(15) 0.8970(5) 0.060 Uiso 1 calc R . C20 C 1.1203(4) 0.5801(4) 0.7775(4) 0.0371(9) Uani 1 d . . H20A H 1.1835(21) 0.5844(20) 0.8238(22) 0.056 Uiso 1 calc R . H20B H 1.1803(21) 0.5978(17) 0.6980(4) 0.056 Uiso 1 calc R . H20C H 1.0744(4) 0.4941(5) 0.8115(24) 0.056 Uiso 1 calc R . C21 C 1.0322(4) 0.2436(3) 0.8226(3) 0.0306(8) Uani 1 d . . H21 H 1.0738(4) 0.2420(3) 0.8854(3) 0.037 Uiso 1 calc R . C22 C 0.9940(5) 0.1066(4) 0.8446(4) 0.0432(10) Uani 1 d . . H22A H 1.0828(9) 0.0547(9) 0.8477(28) 0.065 Uiso 1 calc R . H22B H 0.9565(34) 0.1073(5) 0.7818(15) 0.065 Uiso 1 calc R . H22C H 0.9180(26) 0.0697(11) 0.9185(14) 0.065 Uiso 1 calc R . C23 C 1.1484(4) 0.2993(4) 0.7070(3) 0.0399(9) Uani 1 d . . H23A H 1.2393(12) 0.2504(19) 0.7113(9) 0.060 Uiso 1 calc R . H23B H 1.1693(25) 0.3894(10) 0.6889(13) 0.060 Uiso 1 calc R . H23C H 1.1116(14) 0.2939(27) 0.6460(6) 0.060 Uiso 1 calc R . C24 C 0.4934(14) -0.1242(13) 0.2061(12) 0.162(5) Uiso 1 d . . C25A C 0.4154(16) -0.0440(14) 0.1176(12) 0.080(4) Uiso 0.50 d P 1 C25B C 0.5895(20) -0.0839(17) 0.0732(16) 0.109(5) Uiso 0.50 d P 2 C26 C 0.5000 0.0000 0.0000 0.114(4) Uiso 1 d S . 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 Yb 0.01932(8) 0.02324(8) 0.01915(8) -0.00752(6) -0.00289(5) 0.00202(5) Cl 0.0277(4) 0.0319(4) 0.0282(4) -0.0158(3) 0.0011(3) -0.0057(3) N1 0.0194(13) 0.0292(14) 0.0202(13) -0.0095(11) -0.0054(11) 0.0028(11) N2 0.0211(14) 0.0287(14) 0.0216(13) -0.0102(11) -0.0070(11) 0.0025(11) N3 0.0166(13) 0.0292(14) 0.0246(14) -0.0064(12) -0.0038(11) 0.0002(11) N4 0.0215(14) 0.0307(15) 0.0238(14) -0.0092(12) -0.0020(11) 0.0031(12) C1 0.022(2) 0.029(2) 0.0186(15) -0.0084(13) -0.0031(12) 0.0003(13) C2 0.043(2) 0.032(2) 0.040(2) -0.017(2) -0.021(2) 0.005(2) C3 0.051(3) 0.031(2) 0.052(3) -0.019(2) -0.022(2) 0.004(2) C4 0.048(2) 0.027(2) 0.044(2) -0.009(2) -0.014(2) 0.004(2) C5 0.038(2) 0.030(2) 0.030(2) -0.003(2) -0.012(2) 0.007(2) C6 0.029(2) 0.033(2) 0.024(2) -0.0079(14) -0.0097(14) 0.0035(14) C7 0.022(2) 0.029(2) 0.0189(15) -0.0100(13) -0.0029(12) 0.0035(13) C8 0.023(2) 0.036(2) 0.024(2) -0.0110(15) -0.0081(13) 0.0025(14) C9 0.020(2) 0.037(2) 0.031(2) -0.014(2) -0.0078(14) -0.0003(14) C10 0.019(2) 0.034(2) 0.030(2) -0.009(2) -0.0041(14) -0.0001(14) C11 0.023(2) 0.026(2) 0.023(2) -0.0084(13) -0.0037(13) -0.0008(13) C12 0.027(2) 0.041(2) 0.026(2) -0.010(2) -0.0041(14) 0.006(2) C13 0.029(2) 0.052(2) 0.028(2) -0.016(2) 0.0035(15) 0.002(2) C14 0.036(2) 0.051(2) 0.021(2) -0.013(2) -0.0036(15) 0.003(2) C15 0.036(2) 0.042(2) 0.024(2) -0.012(2) -0.0103(15) 0.006(2) C16 0.027(2) 0.034(2) 0.027(2) -0.0110(15) -0.0076(14) 0.0044(14) C17 0.025(2) 0.023(2) 0.026(2) -0.0098(13) -0.0055(13) 0.0001(13) C18 0.025(2) 0.033(2) 0.027(2) -0.0119(15) -0.0118(14) 0.0031(14) C19 0.038(2) 0.058(3) 0.028(2) -0.019(2) -0.014(2) 0.006(2) C20 0.033(2) 0.042(2) 0.041(2) -0.016(2) -0.020(2) 0.008(2) C21 0.028(2) 0.032(2) 0.024(2) -0.0072(15) -0.0054(14) 0.0093(15) C22 0.051(3) 0.033(2) 0.040(2) -0.011(2) -0.011(2) 0.011(2) C23 0.032(2) 0.045(2) 0.032(2) -0.012(2) -0.001(2) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb N2 2.262(3) . ? Yb N3 2.298(3) . ? Yb N4 2.308(3) . ? Yb N1 2.334(3) . ? Yb Cl 2.6653(10) . ? Yb Cl 2.7632(13) 2_766 ? Yb C7 3.137(3) . ? Yb C11 3.141(3) . ? Yb C17 3.160(4) . ? Yb C1 3.183(4) . ? Yb Yb 4.2778(9) 2_766 ? Cl Yb 2.7632(13) 2_766 ? N1 C1 1.329(4) . ? N1 C18 1.489(4) . ? N2 C7 1.338(4) . ? N2 C8 1.467(4) . ? N3 C11 1.333(4) . ? N3 C10 1.475(4) . ? N4 C17 1.343(4) . ? N4 C21 1.481(4) . ? C1 C2 1.416(5) . ? C1 C7 1.491(5) . ? C2 C3 1.384(6) . ? C3 C4 1.385(6) . ? C4 C5 1.370(6) . ? C5 C6 1.386(5) . ? C6 C7 1.411(5) . ? C8 C9 1.528(5) . ? C9 C10 1.519(5) . ? C11 C12 1.427(5) . ? C11 C17 1.487(5) . ? C12 C13 1.378(5) . ? C13 C14 1.380(6) . ? C14 C15 1.378(5) . ? C15 C16 1.391(5) . ? C16 C17 1.407(5) . ? C18 C20 1.515(5) . ? C18 C19 1.523(5) . ? C21 C23 1.519(5) . ? C21 C22 1.524(6) . ? C24 C25A 1.49(2) . ? C24 C25B 1.61(2) . ? C25A C26 1.418(14) . ? C25B C26 1.46(2) . ? C26 C25A 1.418(14) 2_655 ? C26 C25B 1.46(2) 2_655 ? 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 Yb N3 78.14(10) . . ? N2 Yb N4 144.14(10) . . ? N3 Yb N4 67.75(10) . . ? N2 Yb N1 69.00(10) . . ? N3 Yb N1 101.80(10) . . ? N4 Yb N1 106.72(10) . . ? N2 Yb Cl 96.82(7) . . ? N3 Yb Cl 99.13(8) . . ? N4 Yb Cl 99.10(8) . . ? N1 Yb Cl 151.42(7) . . ? N2 Yb Cl 96.34(8) . 2_766 ? N3 Yb Cl 172.29(7) . 2_766 ? N4 Yb Cl 118.60(8) . 2_766 ? N1 Yb Cl 80.94(7) . 2_766 ? Cl Yb Cl 76.01(3) . 2_766 ? N2 Yb C7 21.90(9) . . ? N3 Yb C7 92.04(10) . . ? N4 Yb C7 145.87(9) . . ? N1 Yb C7 48.81(9) . . ? Cl Yb C7 111.49(7) . . ? Cl Yb C7 84.35(7) 2_766 . ? N2 Yb C11 95.61(10) . . ? N3 Yb C11 22.15(9) . . ? N4 Yb C11 48.66(9) . . ? N1 Yb C11 95.75(9) . . ? Cl Yb C11 110.65(7) . . ? Cl Yb C11 165.49(7) 2_766 . ? C7 Yb C11 104.19(9) . . ? N2 Yb C17 122.09(10) . . ? N3 Yb C17 48.24(9) . . ? N4 Yb C17 22.14(9) . . ? N1 Yb C17 98.51(9) . . ? Cl Yb C17 109.95(7) . . ? Cl Yb C17 138.88(7) 2_766 . ? C7 Yb C17 126.01(9) . . ? C11 Yb C17 27.30(9) . . ? N2 Yb C1 48.15(9) . . ? N3 Yb C1 99.49(10) . . ? N4 Yb C1 126.15(10) . . ? N1 Yb C1 21.61(9) . . ? Cl Yb C1 134.72(6) . . ? Cl Yb C1 80.35(7) 2_766 . ? C7 Yb C1 27.27(8) . . ? C11 Yb C1 101.76(9) . . ? C17 Yb C1 113.27(9) . . ? N2 Yb Yb 98.36(7) . 2_766 ? N3 Yb Yb 137.64(8) . 2_766 ? N4 Yb Yb 114.07(7) . 2_766 ? N1 Yb Yb 116.45(7) . 2_766 ? Cl Yb Yb 38.81(2) . 2_766 ? Cl Yb Yb 37.20(2) 2_766 2_766 ? C7 Yb Yb 99.48(7) . 2_766 ? C11 Yb Yb 147.68(6) . 2_766 ? C17 Yb Yb 134.36(6) . 2_766 ? C1 Yb Yb 109.28(7) . 2_766 ? Yb Cl Yb 103.99(3) . 2_766 ? C1 N1 C18 118.6(3) . . ? C1 N1 Yb 118.1(2) . . ? C18 N1 Yb 123.3(2) . . ? C7 N2 C8 117.6(3) . . ? C7 N2 Yb 119.0(2) . . ? C8 N2 Yb 123.2(2) . . ? C11 N3 C10 118.7(3) . . ? C11 N3 Yb 117.3(2) . . ? C10 N3 Yb 122.2(2) . . ? C17 N4 C21 118.3(3) . . ? C17 N4 Yb 117.5(2) . . ? C21 N4 Yb 124.0(2) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 C7 114.7(3) . . ? C2 C1 C7 121.7(3) . . ? N1 C1 Yb 40.3(2) . . ? C2 C1 Yb 163.6(2) . . ? C7 C1 Yb 74.6(2) . . ? C3 C2 C1 133.6(4) . . ? C2 C3 C4 130.1(4) . . ? C5 C4 C3 125.3(4) . . ? C4 C5 C6 129.9(4) . . ? C5 C6 C7 133.0(4) . . ? N2 C7 C6 121.2(3) . . ? N2 C7 C1 114.1(3) . . ? C6 C7 C1 124.6(3) . . ? N2 C7 Yb 39.1(2) . . ? C6 C7 Yb 153.8(2) . . ? C1 C7 Yb 78.1(2) . . ? N2 C8 C9 110.7(3) . . ? C10 C9 C8 113.0(3) . . ? N3 C10 C9 110.6(3) . . ? N3 C11 C12 121.5(3) . . ? N3 C11 C17 113.9(3) . . ? C12 C11 C17 124.6(3) . . ? N3 C11 Yb 40.5(2) . . ? C12 C11 Yb 153.8(2) . . ? C17 C11 Yb 77.1(2) . . ? C13 C12 C11 132.9(4) . . ? C12 C13 C14 130.0(4) . . ? C15 C14 C13 125.4(3) . . ? C14 C15 C16 130.5(4) . . ? C15 C16 C17 133.2(3) . . ? N4 C17 C16 123.0(3) . . ? N4 C17 C11 113.7(3) . . ? C16 C17 C11 123.3(3) . . ? N4 C17 Yb 40.4(2) . . ? C16 C17 Yb 158.3(2) . . ? C11 C17 Yb 75.6(2) . . ? N1 C18 C20 110.6(3) . . ? N1 C18 C19 110.1(3) . . ? C20 C18 C19 110.5(3) . . ? N4 C21 C23 110.3(3) . . ? N4 C21 C22 110.8(3) . . ? C23 C21 C22 108.4(3) . . ? C26 C25A C24 116.6(11) . . ? C26 C25B C24 107.7(12) . . ? C25A C26 C25A 179.999(1) . 2_655 ? C25B C26 C25B 179.999(2) 2_655 . ? _refine_diff_density_max 0.819 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.096