Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS #Date: October 16, 2000 #"Synthesis, Structure and Characterisation of Ln5O(OPri)13 with #Ln = Nd, Gd and Er" _publ_contact_author 'Dr Gunnar Westin' _publ_contact_author_address ; Dr Gunnar Westin Dept of Inorganic Chemistry, Angstrom Laboratory Uppsala University SE-751 21 Uppsala SWEDEN ; _publ_contact_letter ; Date of submission '9th October, 2000' Please consider this CIF submission as supplementary crystallographic data for the manuscript: "Synthesis, Structure and Characterisation of Ln5O(OPri)13 with Ln = Nd, Gd and Er" ; _publ_requested_journal 'J. C. S. Dalton Trans.' _publ_requested_category ? _publ_section_title ; Synthesis, Structure and Characterisation of Ln5O(OPri)13 with Ln = Nd, Gd and Er ; loop_ _publ_author_name _publ_author_address 'Mikael Kritikos' ; Structural Chemistry Arrhenius Laboratory Stockholm University S-106 91 Stockholm Sweden ; 'Marat Moustiakimov' ; Structural Chemistry Arrhenius Laboratory Stockholm University S-106 91 Stockholm Sweden ; 'Maria Wijk' ; Inorganic Chemistry Angstrom Laboratory Uppsala University S-751 21 Uppsala Sweden ; 'Gunnar Westin' ; Inorganic Chemistry Angstrom Laboratory Uppsala University S-751 21 Uppsala Sweden ; #=========================================================================== data_nd5o _database_code_CSD 158362 _audit_creation_method 'STADI4, SHELXL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H91 Nd5 O14' _chemical_formula_weight 1505.35 _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 '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' '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/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 12.912(5) _cell_length_b 21.611(12) _cell_length_c 21.722(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.54(3) _cell_angle_gamma 90.00 _cell_volume 6059(4) _cell_formula_units_Z 4 _cell_measurement_temperature 220(1) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 11.3 _cell_measurement_theta_max 13.3 _exptl_crystal_description 'irregular' _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method ? _exptl_crystal_F_000 2948 _exptl_absorpt_coefficient_mu 4.255 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2335 _exptl_absorpt_correction_T_max 0.5760 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe 4-circle' _diffrn_measurement_method \w--2\q _diffrn_standards_number 4 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 240 _diffrn_standards_decay_% 28.9 _diffrn_reflns_number 10255 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 22.98 _reflns_number_total 8362 _reflns_number_gt 4490 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _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 0 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+16.0436P] 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 4490 _refine_ls_number_parameters 470 _refine_ls_number_restraints 151 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_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_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 0.09422(7) 0.68063(4) 0.60296(4) 0.0909(3) Uani 1 1 d . B . Nd2 Nd 0.05977(7) 0.81725(5) 0.78269(4) 0.0916(3) Uani 1 1 d . B . Nd3 Nd 0.23122(6) 0.80838(5) 0.66120(4) 0.0878(3) Uani 1 1 d . B . Nd4 Nd -0.07935(7) 0.69096(4) 0.72330(4) 0.0847(3) Uani 1 1 d . B . Nd5 Nd -0.04355(6) 0.82521(4) 0.62553(4) 0.0776(3) Uani 1 1 d . B . O_14 O 0.0673(6) 0.7552(4) 0.6858(4) 0.071(2) Uani 1 1 d . . . O_1 O 0.0866(7) 0.8808(4) 0.6863(4) 0.089(3) Uani 1 1 d D B . C_1 C 0.0996(18) 0.9449(7) 0.6879(9) 0.153(8) Uani 1 1 d D . . H_1 H 0.0406 0.9613 0.7111 0.183 Uiso 1 1 calc R A 1 C1A_1 C 0.193(2) 0.9637(15) 0.7226(14) 0.148(11) Uiso 0.66(3) 1 d PD B 1 H1A1_1 H 0.1896 0.9491 0.7647 0.177 Uiso 0.66(3) 1 calc PR B 1 H1A2_1 H 0.1987 1.0085 0.7224 0.177 Uiso 0.66(3) 1 calc PR B 1 H1A3_1 H 0.2536 0.9460 0.7036 0.177 Uiso 0.66(3) 1 calc PR B 1 C2A_1 C 0.091(3) 0.9733(14) 0.6265(12) 0.151(11) Uiso 0.66(3) 1 d PD B 1 H2A1_1 H 0.1600 0.9787 0.6103 0.181 Uiso 0.66(3) 1 calc PR B 1 H2A2_1 H 0.0575 1.0132 0.6294 0.181 Uiso 0.66(3) 1 calc PR B 1 H2A3_1 H 0.0508 0.9466 0.5991 0.181 Uiso 0.66(3) 1 calc PR B 1 C1B_1 C 0.143(5) 0.968(2) 0.746(2) 0.148(11) Uiso 0.34(3) 1 d PD B 2 H1B1_1 H 0.1515 0.9342 0.7745 0.177 Uiso 0.34(3) 1 calc PR B 2 H1B2_1 H 0.0963 0.9987 0.7625 0.177 Uiso 0.34(3) 1 calc PR B 2 H1B3_1 H 0.2095 0.9872 0.7386 0.177 Uiso 0.34(3) 1 calc PR B 2 C2B_1 C 0.023(5) 0.981(2) 0.653(3) 0.151(11) Uiso 0.34(3) 1 d PD B 2 H2B1_1 H 0.0178 0.9649 0.6111 0.181 Uiso 0.34(3) 1 calc PR B 2 H2B2_1 H 0.0445 1.0238 0.6519 0.181 Uiso 0.34(3) 1 calc PR B 2 H2B3_1 H -0.0435 0.9774 0.6720 0.181 Uiso 0.34(3) 1 calc PR B 2 O_2 O 0.1075(7) 0.7923(5) 0.5703(4) 0.087(3) Uani 1 1 d D B . C_2 C 0.1282(14) 0.8084(11) 0.5096(6) 0.142(8) Uani 1 1 d D . . H_2 H 0.1381 0.8535 0.5154 0.170 Uiso 1 1 calc R C 1 C1A_2 C 0.033(2) 0.810(2) 0.4693(14) 0.135(10) Uiso 0.51(2) 1 d PD D 1 H1A1_2 H -0.0043 0.7715 0.4734 0.163 Uiso 0.51(2) 1 calc PR D 1 H1A2_2 H 0.0528 0.8154 0.4268 0.163 Uiso 0.51(2) 1 calc PR D 1 H1A3_2 H -0.0103 0.8442 0.4815 0.163 Uiso 0.51(2) 1 calc PR D 1 C2A_2 C 0.228(2) 0.7931(18) 0.4886(14) 0.122(9) Uiso 0.51(2) 1 d PD D 1 H2A1_2 H 0.2767 0.7907 0.5235 0.146 Uiso 0.51(2) 1 calc PR D 1 H2A2_2 H 0.2512 0.8247 0.4603 0.146 Uiso 0.51(2) 1 calc PR D 1 H2A3_2 H 0.2257 0.7534 0.4678 0.146 Uiso 0.51(2) 1 calc PR D 1 C1B_2 C 0.060(3) 0.7782(18) 0.4626(14) 0.135(10) Uiso 0.49(2) 1 d PD D 2 H1B1_2 H 0.0794 0.7350 0.4590 0.163 Uiso 0.49(2) 1 calc PR D 2 H1B2_2 H 0.0683 0.7986 0.4232 0.163 Uiso 0.49(2) 1 calc PR D 2 H1B3_2 H -0.0113 0.7812 0.4747 0.163 Uiso 0.49(2) 1 calc PR D 2 C2B_2 C 0.149(3) 0.8738(12) 0.5016(15) 0.122(9) Uiso 0.49(2) 1 d PD D 2 H2B1_2 H 0.0883 0.8975 0.5127 0.146 Uiso 0.49(2) 1 calc PR D 2 H2B2_2 H 0.1644 0.8819 0.4589 0.146 Uiso 0.49(2) 1 calc PR D 2 H2B3_2 H 0.2074 0.8858 0.5278 0.146 Uiso 0.49(2) 1 calc PR D 2 O_3 O -0.0900(7) 0.7176(4) 0.6101(4) 0.083(3) Uani 1 1 d D B . C_3 C -0.1713(14) 0.6978(8) 0.5702(9) 0.130(7) Uani 1 1 d D . . H_3 H -0.1502 0.7086 0.5280 0.156 Uiso 1 1 calc R E 1 C1A_3 C -0.2685(16) 0.7307(11) 0.5800(11) 0.122(8) Uiso 0.76(2) 1 d PD F 1 H1A1_3 H -0.2970 0.7178 0.6188 0.146 Uiso 0.76(2) 1 calc PR F 1 H1A2_3 H -0.3175 0.7211 0.5467 0.146 Uiso 0.76(2) 1 calc PR F 1 H1A3_3 H -0.2556 0.7749 0.5809 0.146 Uiso 0.76(2) 1 calc PR F 1 C2A_3 C -0.183(2) 0.6304(10) 0.5711(14) 0.161(12) Uiso 0.76(2) 1 d PD F 1 H2A1_3 H -0.1156 0.6110 0.5720 0.193 Uiso 0.76(2) 1 calc PR F 1 H2A2_3 H -0.2221 0.6172 0.5345 0.193 Uiso 0.76(2) 1 calc PR F 1 H2A3_3 H -0.2205 0.6183 0.6075 0.193 Uiso 0.76(2) 1 calc PR F 1 C1B_3 C -0.215(5) 0.745(2) 0.530(3) 0.122(8) Uiso 0.24(2) 1 d PD F 2 H1B1_3 H -0.2899 0.7450 0.5321 0.146 Uiso 0.24(2) 1 calc PR F 2 H1B2_3 H -0.1956 0.7371 0.4876 0.146 Uiso 0.24(2) 1 calc PR F 2 H1B3_3 H -0.1887 0.7855 0.5423 0.146 Uiso 0.24(2) 1 calc PR F 2 C2B_3 C -0.150(6) 0.638(2) 0.543(4) 0.161(12) Uiso 0.24(2) 1 d PD F 2 H2B1_3 H -0.1107 0.6433 0.5056 0.193 Uiso 0.24(2) 1 calc PR F 2 H2B2_3 H -0.2145 0.6168 0.5325 0.193 Uiso 0.24(2) 1 calc PR F 2 H2B3_3 H -0.1097 0.6126 0.5718 0.193 Uiso 0.24(2) 1 calc PR F 2 O_4 O -0.1123(7) 0.8047(5) 0.7258(4) 0.087(3) Uani 1 1 d D B . C_4 C -0.2041(13) 0.8313(8) 0.7502(8) 0.118(6) Uani 1 1 d D . . H_4 H -0.2045 0.8259 0.7955 0.141 Uiso 1 1 calc R G 1 C1A_4 C -0.296(2) 0.8017(18) 0.721(2) 0.202(16) Uiso 0.54(2) 1 d PD H 1 H1A1_4 H -0.3090 0.8192 0.6804 0.243 Uiso 0.54(2) 1 calc PR H 1 H1A2_4 H -0.3562 0.8090 0.7462 0.243 Uiso 0.54(2) 1 calc PR H 1 H1A3_4 H -0.2847 0.7575 0.7175 0.243 Uiso 0.54(2) 1 calc PR H 1 C2A_4 C -0.215(3) 0.8980(10) 0.734(2) 0.143(11) Uiso 0.54(2) 1 d PD H 1 H2A1_4 H -0.1546 0.9205 0.7496 0.172 Uiso 0.54(2) 1 calc PR H 1 H2A2_4 H -0.2767 0.9146 0.7518 0.172 Uiso 0.54(2) 1 calc PR H 1 H2A3_4 H -0.2195 0.9023 0.6894 0.172 Uiso 0.54(2) 1 calc PR H 1 C1B_4 C -0.228(4) 0.803(2) 0.8107(16) 0.202(16) Uiso 0.46(2) 1 d PD H 2 H1B1_4 H -0.2289 0.7586 0.8070 0.243 Uiso 0.46(2) 1 calc PR H 2 H1B2_4 H -0.2961 0.8174 0.8232 0.243 Uiso 0.46(2) 1 calc PR H 2 H1B3_4 H -0.1765 0.8157 0.8413 0.243 Uiso 0.46(2) 1 calc PR H 2 C2B_4 C -0.194(4) 0.8991(10) 0.755(2) 0.143(11) Uiso 0.46(2) 1 d PD H 2 H2B1_4 H -0.1242 0.9096 0.7690 0.172 Uiso 0.46(2) 1 calc PR H 2 H2B2_4 H -0.2429 0.9145 0.7849 0.172 Uiso 0.46(2) 1 calc PR H 2 H2B3_4 H -0.2088 0.9179 0.7155 0.172 Uiso 0.46(2) 1 calc PR H 2 O_5 O 0.2368(8) 0.8095(6) 0.7687(4) 0.110(4) Uani 1 1 d D . . CA_5 C 0.320(2) 0.797(2) 0.8098(14) 0.135(10) Uiso 0.54(3) 1 d PD I 1 HA_5 H 0.3392 0.8372 0.8297 0.162 Uiso 0.54(3) 1 calc PR I 1 C1A_5 C 0.298(4) 0.754(3) 0.8589(19) 0.226(19) Uiso 0.54(3) 1 d PD I 1 H1A1_5 H 0.2244 0.7524 0.8652 0.271 Uiso 0.54(3) 1 calc PR I 1 H1A2_5 H 0.3338 0.7670 0.8966 0.271 Uiso 0.54(3) 1 calc PR I 1 H1A3_5 H 0.3228 0.7130 0.8476 0.271 Uiso 0.54(3) 1 calc PR I 1 C2A_5 C 0.413(3) 0.774(3) 0.780(2) 0.25(2) Uiso 0.54(3) 1 d PD I 1 H2A1_5 H 0.3956 0.7366 0.7578 0.302 Uiso 0.54(3) 1 calc PR I 1 H2A2_5 H 0.4659 0.7656 0.8112 0.302 Uiso 0.54(3) 1 calc PR I 1 H2A3_5 H 0.4375 0.8051 0.7518 0.302 Uiso 0.54(3) 1 calc PR I 1 CB_5 C 0.314(2) 0.832(2) 0.8092(15) 0.135(10) Uiso 0.46(3) 1 d PD I 2 HB_5 H 0.3053 0.8773 0.8043 0.162 Uiso 0.46(3) 1 calc PR I 2 C1B_5 C 0.294(4) 0.824(4) 0.8744(15) 0.226(19) Uiso 0.46(3) 1 d PD I 2 H1B1_5 H 0.2223 0.8352 0.8821 0.271 Uiso 0.46(3) 1 calc PR I 2 H1B2_5 H 0.3399 0.8501 0.8987 0.271 Uiso 0.46(3) 1 calc PR I 2 H1B3_5 H 0.3048 0.7809 0.8858 0.271 Uiso 0.46(3) 1 calc PR I 2 C2B_5 C 0.419(3) 0.823(4) 0.790(3) 0.25(2) Uiso 0.46(3) 1 d PD I 2 H2B1_5 H 0.4225 0.7883 0.7628 0.302 Uiso 0.46(3) 1 calc PR I 2 H2B2_5 H 0.4636 0.8160 0.8263 0.302 Uiso 0.46(3) 1 calc PR I 2 H2B3_5 H 0.4424 0.8603 0.7693 0.302 Uiso 0.46(3) 1 calc PR I 2 O_6 O 0.2646(7) 0.7083(6) 0.6312(5) 0.108(4) Uani 1 1 d D . . CA_6 C 0.345(3) 0.665(2) 0.627(2) 0.215(14) Uiso 0.53(4) 1 d PD I 1 HA_6 H 0.3208 0.6306 0.6000 0.257 Uiso 0.53(4) 1 calc PR I 1 C1A_6 C 0.364(4) 0.639(3) 0.690(2) 0.23(2) Uiso 0.53(4) 1 d PD I 1 H1A1_6 H 0.4112 0.6663 0.7126 0.279 Uiso 0.53(4) 1 calc PR I 1 H1A2_6 H 0.3939 0.5984 0.6869 0.279 Uiso 0.53(4) 1 calc PR I 1 H1A3_6 H 0.2988 0.6370 0.7108 0.279 Uiso 0.53(4) 1 calc PR I 1 C2A_6 C 0.435(3) 0.693(3) 0.599(3) 0.25(2) Uiso 0.53(4) 1 d PD I 1 H2A1_6 H 0.4131 0.7150 0.5612 0.299 Uiso 0.53(4) 1 calc PR I 1 H2A2_6 H 0.4852 0.6617 0.5884 0.299 Uiso 0.53(4) 1 calc PR I 1 H2A3_6 H 0.4673 0.7227 0.6271 0.299 Uiso 0.53(4) 1 calc PR I 1 CB_6 C 0.359(3) 0.678(2) 0.624(2) 0.215(14) Uiso 0.47(4) 1 d PD I 2 HB_6 H 0.4108 0.7024 0.6482 0.257 Uiso 0.47(4) 1 calc PR I 2 C1B_6 C 0.360(5) 0.616(2) 0.652(3) 0.23(2) Uiso 0.47(4) 1 d PD I 2 H1B1_6 H 0.3478 0.6193 0.6956 0.279 Uiso 0.47(4) 1 calc PR I 2 H1B2_6 H 0.4276 0.5971 0.6461 0.279 Uiso 0.47(4) 1 calc PR I 2 H1B3_6 H 0.3070 0.5907 0.6324 0.279 Uiso 0.47(4) 1 calc PR I 2 C2B_6 C 0.395(5) 0.678(3) 0.561(3) 0.25(2) Uiso 0.47(4) 1 d PD I 2 H2B1_6 H 0.3399 0.6628 0.5332 0.299 Uiso 0.47(4) 1 calc PR I 2 H2B2_6 H 0.4546 0.6503 0.5579 0.299 Uiso 0.47(4) 1 calc PR I 2 H2B3_6 H 0.4146 0.7191 0.5490 0.299 Uiso 0.47(4) 1 calc PR I 2 O_7 O 0.0274(8) 0.6174(5) 0.6786(5) 0.102(3) Uani 1 1 d D . . C_7 C 0.045(2) 0.5551(9) 0.6900(13) 0.204(13) Uani 1 1 d D I . H_7 H 0.1041 0.5465 0.6635 0.244 Uiso 1 1 calc R J 1 C1A_7 C -0.034(6) 0.514(2) 0.664(4) 0.191(15) Uiso 0.26(2) 1 d PD I 1 H1A1_7 H -0.0883 0.5084 0.6933 0.230 Uiso 0.26(2) 1 calc PR I 1 H1A2_7 H -0.0024 0.4741 0.6553 0.230 Uiso 0.26(2) 1 calc PR I 1 H1A3_7 H -0.0622 0.5316 0.6263 0.230 Uiso 0.26(2) 1 calc PR I 1 C2A_7 C 0.090(8) 0.544(3) 0.752(3) 0.226(17) Uiso 0.26(2) 1 d PD I 1 H2A1_7 H 0.1408 0.5755 0.7615 0.271 Uiso 0.26(2) 1 calc PR I 1 H2A2_7 H 0.1232 0.5035 0.7526 0.271 Uiso 0.26(2) 1 calc PR I 1 H2A3_7 H 0.0357 0.5448 0.7817 0.271 Uiso 0.26(2) 1 calc PR I 1 C1B_7 C -0.040(2) 0.5210(14) 0.7150(17) 0.191(15) Uiso 0.74(2) 1 d PD I 2 H1B1_7 H -0.0267 0.5147 0.7587 0.230 Uiso 0.74(2) 1 calc PR I 2 H1B2_7 H -0.0455 0.4813 0.6945 0.230 Uiso 0.74(2) 1 calc PR I 2 H1B3_7 H -0.1034 0.5441 0.7087 0.230 Uiso 0.74(2) 1 calc PR I 2 C2B_7 C 0.122(3) 0.5228(15) 0.6547(17) 0.226(17) Uiso 0.74(2) 1 d PD I 2 H2B1_7 H 0.1174 0.5365 0.6122 0.271 Uiso 0.74(2) 1 calc PR I 2 H2B2_7 H 0.1090 0.4786 0.6565 0.271 Uiso 0.74(2) 1 calc PR I 2 H2B3_7 H 0.1902 0.5317 0.6719 0.271 Uiso 0.74(2) 1 calc PR I 2 O_8 O -0.0006(9) 0.7219(5) 0.8157(4) 0.105(3) Uani 1 1 d D . . CA_8 C 0.008(4) 0.6903(15) 0.8711(11) 0.167(11) Uiso 0.517(19) 1 d PD I 1 HA_8 H -0.0648 0.6811 0.8817 0.201 Uiso 0.517(19) 1 calc PR I 1 C1A_8 C 0.056(4) 0.6287(16) 0.863(2) 0.208(18) Uiso 0.517(19) 1 d PD I 1 H1A1_8 H 0.0041 0.5967 0.8668 0.249 Uiso 0.517(19) 1 calc PR I 1 H1A2_8 H 0.1104 0.6228 0.8941 0.249 Uiso 0.517(19) 1 calc PR I 1 H1A3_8 H 0.0857 0.6264 0.8224 0.249 Uiso 0.517(19) 1 calc PR I 1 C2A_8 C 0.049(4) 0.724(2) 0.9239(15) 0.178(13) Uiso 0.517(19) 1 d PD I 1 H2A1_8 H 0.1083 0.7489 0.9115 0.214 Uiso 0.517(19) 1 calc PR I 1 H2A2_8 H 0.0713 0.6956 0.9558 0.214 Uiso 0.517(19) 1 calc PR I 1 H2A3_8 H -0.0035 0.7516 0.9395 0.214 Uiso 0.517(19) 1 calc PR I 1 CB_8 C -0.020(4) 0.7000(17) 0.8748(13) 0.167(11) Uiso 0.483(19) 1 d PD I 2 HB_8 H 0.0449 0.7051 0.8993 0.201 Uiso 0.483(19) 1 calc PR I 2 C1B_8 C -0.045(5) 0.6326(16) 0.875(2) 0.208(18) Uiso 0.483(19) 1 d PD I 2 H1B1_8 H -0.1179 0.6268 0.8820 0.249 Uiso 0.483(19) 1 calc PR I 2 H1B2_8 H -0.0045 0.6125 0.9078 0.249 Uiso 0.483(19) 1 calc PR I 2 H1B3_8 H -0.0272 0.6146 0.8358 0.249 Uiso 0.483(19) 1 calc PR I 2 C2B_8 C -0.099(3) 0.736(2) 0.9062(18) 0.178(13) Uiso 0.483(19) 1 d PD I 2 H2B1_8 H -0.0706 0.7762 0.9182 0.214 Uiso 0.483(19) 1 calc PR I 2 H2B2_8 H -0.1209 0.7143 0.9426 0.214 Uiso 0.483(19) 1 calc PR I 2 H2B3_8 H -0.1587 0.7426 0.8786 0.214 Uiso 0.483(19) 1 calc PR I 2 O_9 O -0.1353(10) 0.8838(6) 0.5708(6) 0.144(5) Uani 1 1 d D . . CA_9 C -0.190(4) 0.9278(17) 0.5349(17) 0.223(14) Uiso 0.55(3) 1 d PD K 1 HA_9 H -0.1361 0.9515 0.5132 0.267 Uiso 0.55(3) 1 calc PR K 1 C1A_9 C -0.243(4) 0.973(2) 0.573(2) 0.210(18) Uiso 0.55(3) 1 d PD K 1 H1A1_9 H -0.2696 0.9525 0.6090 0.252 Uiso 0.55(3) 1 calc PR K 1 H1A2_9 H -0.3002 0.9912 0.5493 0.252 Uiso 0.55(3) 1 calc PR K 1 H1A3_9 H -0.1950 1.0053 0.5858 0.252 Uiso 0.55(3) 1 calc PR K 1 C2A_9 C -0.252(4) 0.898(2) 0.487(2) 0.212(19) Uiso 0.55(3) 1 d PD K 1 H2A1_9 H -0.2077 0.8857 0.4534 0.255 Uiso 0.55(3) 1 calc PR K 1 H2A2_9 H -0.3048 0.9259 0.4714 0.255 Uiso 0.55(3) 1 calc PR K 1 H2A3_9 H -0.2844 0.8611 0.5035 0.255 Uiso 0.55(3) 1 calc PR K 1 CB_9 C -0.202(4) 0.9181(19) 0.5311(18) 0.223(14) Uiso 0.45(3) 1 d PD K 2 HB_9 H -0.2738 0.9093 0.5426 0.267 Uiso 0.45(3) 1 calc PR K 2 C1B_9 C -0.184(5) 0.9849(17) 0.539(3) 0.210(18) Uiso 0.45(3) 1 d PD K 2 H1B1_9 H -0.2119 0.9985 0.5774 0.252 Uiso 0.45(3) 1 calc PR K 2 H1B2_9 H -0.2174 1.0071 0.5050 0.252 Uiso 0.45(3) 1 calc PR K 2 H1B3_9 H -0.1098 0.9932 0.5389 0.252 Uiso 0.45(3) 1 calc PR K 2 C2B_9 C -0.190(6) 0.899(3) 0.4662(17) 0.212(19) Uiso 0.45(3) 1 d PD K 2 H2B1_9 H -0.1174 0.8926 0.4582 0.255 Uiso 0.45(3) 1 calc PR K 2 H2B2_9 H -0.2170 0.9317 0.4393 0.255 Uiso 0.45(3) 1 calc PR K 2 H2B3_9 H -0.2283 0.8614 0.4584 0.255 Uiso 0.45(3) 1 calc PR K 2 O_10 O 0.3515(9) 0.8633(7) 0.6297(6) 0.138(5) Uani 1 1 d D . . CA_10 C 0.438(3) 0.896(2) 0.6119(15) 0.230(15) Uiso 0.518(18) 1 d PD I 1 HA_10 H 0.4882 0.8618 0.6067 0.276 Uiso 0.518(18) 1 calc PR I 1 C1A_10 C 0.492(3) 0.933(2) 0.6586(17) 0.200(16) Uiso 0.518(18) 1 d PD I 1 H1A1_10 H 0.4477 0.9664 0.6715 0.241 Uiso 0.518(18) 1 calc PR I 1 H1A2_10 H 0.5549 0.9500 0.6417 0.241 Uiso 0.518(18) 1 calc PR I 1 H1A3_10 H 0.5103 0.9070 0.6938 0.241 Uiso 0.518(18) 1 calc PR I 1 C2A_10 C 0.434(3) 0.9212(18) 0.5498(14) 0.129(10) Uiso 0.518(18) 1 d PD I 1 H2A1_10 H 0.4477 0.8886 0.5204 0.155 Uiso 0.518(18) 1 calc PR I 1 H2A2_10 H 0.4848 0.9537 0.5462 0.155 Uiso 0.518(18) 1 calc PR I 1 H2A3_10 H 0.3651 0.9380 0.5412 0.155 Uiso 0.518(18) 1 calc PR I 1 CB_10 C 0.442(2) 0.8836(17) 0.602(2) 0.230(15) Uiso 0.482(18) 1 d PD I 2 HB_10 H 0.4382 0.8669 0.5591 0.276 Uiso 0.482(18) 1 calc PR I 2 C1B_10 C 0.538(3) 0.859(2) 0.630(2) 0.200(16) Uiso 0.482(18) 1 d PD I 2 H1B1_10 H 0.5645 0.8879 0.6604 0.241 Uiso 0.482(18) 1 calc PR I 2 H1B2_10 H 0.5884 0.8528 0.5983 0.241 Uiso 0.482(18) 1 calc PR I 2 H1B3_10 H 0.5231 0.8196 0.6495 0.241 Uiso 0.482(18) 1 calc PR I 2 C2B_10 C 0.428(3) 0.9506(14) 0.595(2) 0.129(10) Uiso 0.482(18) 1 d PD I 2 H2B1_10 H 0.3843 0.9593 0.5594 0.155 Uiso 0.482(18) 1 calc PR I 2 H2B2_10 H 0.4951 0.9701 0.5907 0.155 Uiso 0.482(18) 1 calc PR I 2 H2B3_10 H 0.3958 0.9667 0.6318 0.155 Uiso 0.482(18) 1 calc PR I 2 O_11 O -0.2202(9) 0.6494(6) 0.7427(6) 0.132(4) Uani 1 1 d D . . CA_11 C -0.307(2) 0.6159(17) 0.7593(18) 0.233(14) Uiso 0.69(2) 1 d PD I 1 HA_11 H -0.2744 0.5876 0.7900 0.280 Uiso 0.69(2) 1 calc PR I 1 C1A_11 C -0.378(2) 0.6482(17) 0.7987(16) 0.181(14) Uiso 0.69(2) 1 d PD I 1 H1A1_11 H -0.3421 0.6607 0.8364 0.217 Uiso 0.69(2) 1 calc PR I 1 H1A2_11 H -0.4352 0.6210 0.8085 0.217 Uiso 0.69(2) 1 calc PR I 1 H1A3_11 H -0.4051 0.6846 0.7775 0.217 Uiso 0.69(2) 1 calc PR I 1 C2A_11 C -0.346(3) 0.5708(16) 0.7149(17) 0.219(17) Uiso 0.69(2) 1 d PD I 1 H2A1_11 H -0.3434 0.5881 0.6737 0.263 Uiso 0.69(2) 1 calc PR I 1 H2A2_11 H -0.4170 0.5603 0.7240 0.263 Uiso 0.69(2) 1 calc PR I 1 H2A3_11 H -0.3035 0.5338 0.7173 0.263 Uiso 0.69(2) 1 calc PR I 1 CB_11 C -0.305(3) 0.611(2) 0.753(3) 0.233(14) Uiso 0.31(2) 1 d PD I 2 HB_11 H -0.3055 0.5800 0.7199 0.280 Uiso 0.31(2) 1 calc PR I 2 C1B_11 C -0.399(3) 0.648(4) 0.744(4) 0.181(14) Uiso 0.31(2) 1 d PD I 2 H1B1_11 H -0.3838 0.6910 0.7528 0.217 Uiso 0.31(2) 1 calc PR I 2 H1B2_11 H -0.4514 0.6334 0.7719 0.217 Uiso 0.31(2) 1 calc PR I 2 H1B3_11 H -0.4242 0.6436 0.7020 0.217 Uiso 0.31(2) 1 calc PR I 2 C2B_11 C -0.290(6) 0.576(3) 0.811(3) 0.219(17) Uiso 0.31(2) 1 d PD I 2 H2B1_11 H -0.2216 0.5852 0.8285 0.263 Uiso 0.31(2) 1 calc PR I 2 H2B2_11 H -0.2960 0.5325 0.8025 0.263 Uiso 0.31(2) 1 calc PR I 2 H2B3_11 H -0.3422 0.5887 0.8397 0.263 Uiso 0.31(2) 1 calc PR I 2 O_12 O 0.0365(10) 0.8822(6) 0.8519(5) 0.133(5) Uani 1 1 d D . . CA_12 C 0.025(3) 0.9222(17) 0.9024(16) 0.223(13) Uiso 0.61(3) 1 d PD I 1 HA_12 H -0.0166 0.9014 0.9339 0.268 Uiso 0.61(3) 1 calc PR I 1 C1A_12 C -0.026(4) 0.9805(19) 0.884(2) 0.28(3) Uiso 0.61(3) 1 d PD I 1 H1A1_12 H -0.0777 0.9722 0.8518 0.334 Uiso 0.61(3) 1 calc PR I 1 H1A2_12 H 0.0258 1.0088 0.8682 0.334 Uiso 0.61(3) 1 calc PR I 1 H1A3_12 H -0.0582 0.9989 0.9191 0.334 Uiso 0.61(3) 1 calc PR I 1 C2A_12 C 0.129(3) 0.937(2) 0.9290(19) 0.199(17) Uiso 0.61(3) 1 d PD I 1 H2A1_12 H 0.1770 0.9043 0.9194 0.239 Uiso 0.61(3) 1 calc PR I 1 H2A2_12 H 0.1246 0.9411 0.9734 0.239 Uiso 0.61(3) 1 calc PR I 1 H2A3_12 H 0.1529 0.9758 0.9118 0.239 Uiso 0.61(3) 1 calc PR I 1 CB_12 C 0.031(4) 0.926(2) 0.8996(18) 0.223(13) Uiso 0.39(3) 1 d PD I 2 HB_12 H 0.0758 0.9613 0.8902 0.268 Uiso 0.39(3) 1 calc PR I 2 C1B_12 C -0.077(5) 0.947(4) 0.904(3) 0.28(3) Uiso 0.39(3) 1 d PD I 2 H1B1_12 H -0.0878 0.9825 0.8774 0.334 Uiso 0.39(3) 1 calc PR I 2 H1B2_12 H -0.0894 0.9591 0.9464 0.334 Uiso 0.39(3) 1 calc PR I 2 H1B3_12 H -0.1237 0.9141 0.8920 0.334 Uiso 0.39(3) 1 calc PR I 2 C2B_12 C 0.068(5) 0.897(3) 0.9576(18) 0.199(17) Uiso 0.39(3) 1 d PD I 2 H2B1_12 H 0.0431 0.8544 0.9594 0.239 Uiso 0.39(3) 1 calc PR I 2 H2B2_12 H 0.0421 0.9198 0.9922 0.239 Uiso 0.39(3) 1 calc PR I 2 H2B3_12 H 0.1431 0.8968 0.9593 0.239 Uiso 0.39(3) 1 calc PR I 2 O_13 O 0.1047(11) 0.6282(6) 0.5207(5) 0.143(5) Uani 1 1 d D . . CA_13 C 0.103(3) 0.5869(14) 0.4700(12) 0.157(11) Uiso 0.59(2) 1 d PD I 1 HA_13 H 0.0297 0.5764 0.4615 0.188 Uiso 0.59(2) 1 calc PR I 1 C1A_13 C 0.154(4) 0.5292(15) 0.4886(19) 0.213(18) Uiso 0.59(2) 1 d PD I 1 H1A1_13 H 0.2264 0.5305 0.4772 0.255 Uiso 0.59(2) 1 calc PR I 1 H1A2_13 H 0.1201 0.4946 0.4682 0.255 Uiso 0.59(2) 1 calc PR I 1 H1A3_13 H 0.1503 0.5242 0.5329 0.255 Uiso 0.59(2) 1 calc PR I 1 C2A_13 C 0.139(3) 0.6195(18) 0.4157(13) 0.176(14) Uiso 0.59(2) 1 d PD I 1 H2A1_13 H 0.1098 0.6609 0.4149 0.211 Uiso 0.59(2) 1 calc PR I 1 H2A2_13 H 0.1161 0.5974 0.3789 0.211 Uiso 0.59(2) 1 calc PR I 1 H2A3_13 H 0.2137 0.6220 0.4173 0.211 Uiso 0.59(2) 1 calc PR I 1 CB_13 C 0.130(3) 0.605(2) 0.4630(14) 0.157(11) Uiso 0.41(2) 1 d PD I 2 HB_13 H 0.1714 0.6376 0.4437 0.188 Uiso 0.41(2) 1 calc PR I 2 C1B_13 C 0.201(5) 0.552(3) 0.469(3) 0.213(18) Uiso 0.41(2) 1 d PD I 2 H1B1_13 H 0.2053 0.5397 0.5122 0.255 Uiso 0.41(2) 1 calc PR I 2 H1B2_13 H 0.2690 0.5646 0.4561 0.255 Uiso 0.41(2) 1 calc PR I 2 H1B3_13 H 0.1754 0.5183 0.4443 0.255 Uiso 0.41(2) 1 calc PR I 2 C2B_13 C 0.038(4) 0.598(3) 0.423(2) 0.176(14) Uiso 0.41(2) 1 d PD I 2 H2B1_13 H -0.0230 0.5982 0.4479 0.211 Uiso 0.41(2) 1 calc PR I 2 H2B2_13 H 0.0417 0.5588 0.4010 0.211 Uiso 0.41(2) 1 calc PR I 2 H2B3_13 H 0.0350 0.6317 0.3939 0.211 Uiso 0.41(2) 1 calc PR I 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 Nd1 0.0961(6) 0.0911(7) 0.0861(5) -0.0115(5) 0.0130(5) 0.0074(5) Nd2 0.0930(6) 0.1164(8) 0.0651(5) -0.0118(5) -0.0012(4) -0.0059(6) Nd3 0.0674(5) 0.1130(8) 0.0828(5) -0.0003(5) -0.0011(4) -0.0032(5) Nd4 0.0877(6) 0.0890(7) 0.0776(5) 0.0091(4) 0.0072(4) -0.0062(5) Nd5 0.0721(5) 0.0835(6) 0.0767(5) 0.0092(4) -0.0067(4) 0.0029(5) O_14 0.064(5) 0.083(6) 0.066(5) 0.000(5) 0.007(4) 0.003(5) O_1 0.089(7) 0.076(7) 0.102(7) -0.007(6) -0.010(5) -0.008(6) C_1 0.20(2) 0.092(15) 0.164(19) -0.006(13) -0.056(16) -0.039(15) O_2 0.092(7) 0.107(8) 0.062(5) 0.009(5) 0.002(5) -0.002(6) C_2 0.133(17) 0.22(3) 0.076(11) 0.007(14) -0.007(11) -0.001(17) O_3 0.076(6) 0.096(7) 0.076(6) -0.007(5) -0.012(5) -0.010(6) C_3 0.153(19) 0.104(16) 0.132(16) -0.001(12) -0.013(14) 0.003(14) O_4 0.069(6) 0.111(8) 0.080(6) -0.007(6) 0.007(5) 0.018(6) C_4 0.141(16) 0.103(14) 0.112(13) -0.013(11) 0.043(12) 0.024(13) O_5 0.086(7) 0.158(11) 0.084(7) -0.004(7) -0.030(5) -0.008(7) O_6 0.068(6) 0.126(9) 0.130(9) 0.003(7) 0.017(6) 0.031(6) O_7 0.101(8) 0.073(7) 0.132(9) 0.013(6) 0.002(7) 0.020(6) C_7 0.18(3) 0.18(3) 0.25(3) 0.04(3) 0.10(3) 0.03(2) O_8 0.126(9) 0.126(9) 0.064(5) 0.022(6) 0.009(6) 0.005(7) O_9 0.131(10) 0.126(10) 0.171(11) 0.072(9) -0.061(9) 0.015(8) O_10 0.098(8) 0.179(13) 0.139(10) 0.004(9) 0.026(7) -0.047(9) O_11 0.115(9) 0.121(10) 0.162(11) 0.007(9) 0.036(8) -0.054(8) O_12 0.146(11) 0.148(12) 0.106(8) -0.054(8) 0.020(8) -0.003(9) O_13 0.176(12) 0.141(12) 0.112(9) -0.057(8) 0.024(8) 0.001(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 Nd1 O_13 2.123(11) . ? Nd1 O_7 2.322(11) . ? Nd1 O_6 2.345(11) . ? Nd1 O_14 2.448(8) . ? Nd1 O_3 2.517(9) . ? Nd1 O_2 2.523(10) . ? Nd2 O_12 2.084(11) . ? Nd2 O_5 2.320(11) . ? Nd2 O_8 2.324(11) . ? Nd2 O_14 2.499(8) . ? Nd2 O_4 2.528(9) . ? Nd2 O_1 2.535(10) . ? Nd3 O_10 2.085(11) . ? Nd3 O_6 2.304(12) . ? Nd3 O_5 2.334(9) . ? Nd3 O_14 2.479(8) . ? Nd3 O_1 2.507(10) . ? Nd3 O_2 2.531(9) . ? Nd4 O_11 2.082(11) . ? Nd4 O_8 2.323(10) . ? Nd4 O_7 2.333(11) . ? Nd4 O_4 2.496(10) . ? Nd4 O_14 2.502(8) . ? Nd4 O_3 2.526(9) . ? Nd5 O_9 2.084(10) . ? Nd5 O_4 2.414(9) . ? Nd5 O_3 2.423(10) . ? Nd5 O_2 2.424(10) . ? Nd5 O_1 2.427(9) . ? Nd5 O_14 2.440(8) . ? O_1 C_1 1.397(14) . ? C_1 C1B_1 1.450(19) . ? C_1 C2B_1 1.452(19) . ? C_1 C1A_1 1.466(18) . ? C_1 C2A_1 1.469(18) . ? O_2 C_2 1.395(14) . ? C_2 C2A_2 1.423(17) . ? C_2 C2B_2 1.450(18) . ? C_2 C1B_2 1.480(18) . ? C_2 C1A_2 1.486(18) . ? O_3 C_3 1.409(14) . ? C_3 C1B_3 1.46(2) . ? C_3 C2B_3 1.46(2) . ? C_3 C1A_3 1.463(17) . ? C_3 C2A_3 1.466(17) . ? O_4 C_4 1.432(14) . ? C_4 C2B_4 1.475(19) . ? C_4 C1A_4 1.481(19) . ? C_4 C1B_4 1.488(19) . ? C_4 C2A_4 1.490(18) . ? O_5 CB_5 1.399(19) . ? O_5 CA_5 1.405(19) . ? CA_5 C1A_5 1.46(2) . ? CA_5 C2A_5 1.46(2) . ? CB_5 C2B_5 1.44(2) . ? CB_5 C1B_5 1.46(2) . ? O_6 CB_6 1.40(2) . ? O_6 CA_6 1.41(2) . ? CA_6 C2A_6 1.47(2) . ? CA_6 C1A_6 1.48(2) . ? CB_6 C1B_6 1.47(2) . ? CB_6 C2B_6 1.47(2) . ? O_7 C_7 1.385(16) . ? C_7 C1B_7 1.431(18) . ? C_7 C1A_7 1.45(2) . ? C_7 C2B_7 1.451(18) . ? C_7 C2A_7 1.47(2) . ? O_8 CA_8 1.384(19) . ? O_8 CB_8 1.40(2) . ? CA_8 C2A_8 1.45(2) . ? CA_8 C1A_8 1.48(2) . ? CB_8 C2B_8 1.47(2) . ? CB_8 C1B_8 1.49(2) . ? O_9 CA_9 1.41(2) . ? O_9 CB_9 1.41(2) . ? CA_9 C2A_9 1.46(2) . ? CA_9 C1A_9 1.46(2) . ? CB_9 C1B_9 1.47(2) . ? CB_9 C2B_9 1.48(2) . ? O_10 CA_10 1.39(2) . ? O_10 CB_10 1.40(2) . ? CA_10 C2A_10 1.46(2) . ? CA_10 C1A_10 1.46(2) . ? CB_10 C2B_10 1.46(2) . ? CB_10 C1B_10 1.47(2) . ? O_11 CA_11 1.389(19) . ? O_11 CB_11 1.39(2) . ? CA_11 C1A_11 1.452(19) . ? CA_11 C2A_11 1.453(19) . ? CB_11 C1B_11 1.46(2) . ? CB_11 C2B_11 1.47(2) . ? O_12 CB_12 1.40(2) . ? O_12 CA_12 1.41(2) . ? CA_12 C1A_12 1.47(2) . ? CA_12 C2A_12 1.48(2) . ? CB_12 C1B_12 1.47(2) . ? CB_12 C2B_12 1.48(2) . ? O_13 CB_13 1.40(2) . ? O_13 CA_13 1.418(19) . ? CA_13 C2A_13 1.46(2) . ? CA_13 C1A_13 1.462(19) . ? CB_13 C1B_13 1.45(2) . ? CB_13 C2B_13 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O_13 Nd1 O_7 108.3(5) . . ? O_13 Nd1 O_6 106.0(5) . . ? O_7 Nd1 O_6 109.2(4) . . ? O_13 Nd1 O_14 169.7(4) . . ? O_7 Nd1 O_14 78.7(3) . . ? O_6 Nd1 O_14 77.9(3) . . ? O_13 Nd1 O_3 107.6(4) . . ? O_7 Nd1 O_3 76.9(3) . . ? O_6 Nd1 O_3 141.7(3) . . ? O_14 Nd1 O_3 66.0(3) . . ? O_13 Nd1 O_2 105.5(4) . . ? O_7 Nd1 O_2 142.4(3) . . ? O_6 Nd1 O_2 76.1(4) . . ? O_14 Nd1 O_2 65.7(3) . . ? O_3 Nd1 O_2 77.6(3) . . ? O_12 Nd2 O_5 107.8(4) . . ? O_12 Nd2 O_8 108.6(4) . . ? O_5 Nd2 O_8 108.4(4) . . ? O_12 Nd2 O_14 168.0(4) . . ? O_5 Nd2 O_14 77.9(3) . . ? O_8 Nd2 O_14 78.8(3) . . ? O_12 Nd2 O_4 106.4(4) . . ? O_5 Nd2 O_4 141.6(3) . . ? O_8 Nd2 O_4 76.0(3) . . ? O_14 Nd2 O_4 65.5(3) . . ? O_12 Nd2 O_1 104.9(4) . . ? O_5 Nd2 O_1 76.9(3) . . ? O_8 Nd2 O_1 142.1(3) . . ? O_14 Nd2 O_1 65.5(3) . . ? O_4 Nd2 O_1 78.0(3) . . ? O_10 Nd3 O_6 107.2(5) . . ? O_10 Nd3 O_5 108.6(4) . . ? O_6 Nd3 O_5 107.0(4) . . ? O_10 Nd3 O_14 169.3(4) . . ? O_6 Nd3 O_14 78.1(3) . . ? O_5 Nd3 O_14 78.0(3) . . ? O_10 Nd3 O_1 106.4(5) . . ? O_6 Nd3 O_1 142.5(3) . . ? O_5 Nd3 O_1 77.2(3) . . ? O_14 Nd3 O_1 66.3(3) . . ? O_10 Nd3 O_2 106.4(4) . . ? O_6 Nd3 O_2 76.6(3) . . ? O_5 Nd3 O_2 141.6(3) . . ? O_14 Nd3 O_2 65.2(3) . . ? O_1 Nd3 O_2 78.3(3) . . ? O_11 Nd4 O_8 108.3(4) . . ? O_11 Nd4 O_7 108.6(5) . . ? O_8 Nd4 O_7 107.8(4) . . ? O_11 Nd4 O_4 105.7(4) . . ? O_8 Nd4 O_4 76.7(3) . . ? O_7 Nd4 O_4 141.6(3) . . ? O_11 Nd4 O_14 168.1(4) . . ? O_8 Nd4 O_14 78.7(3) . . ? O_7 Nd4 O_14 77.4(3) . . ? O_4 Nd4 O_14 65.9(3) . . ? O_11 Nd4 O_3 105.7(4) . . ? O_8 Nd4 O_3 141.9(3) . . ? O_7 Nd4 O_3 76.5(3) . . ? O_4 Nd4 O_3 78.0(3) . . ? O_14 Nd4 O_3 65.1(3) . . ? O_9 Nd5 O_4 114.1(5) . . ? O_9 Nd5 O_3 111.7(4) . . ? O_4 Nd5 O_3 81.6(3) . . ? O_9 Nd5 O_2 110.4(5) . . ? O_4 Nd5 O_2 135.5(3) . . ? O_3 Nd5 O_2 81.3(3) . . ? O_9 Nd5 O_1 112.6(4) . . ? O_4 Nd5 O_1 82.3(3) . . ? O_3 Nd5 O_1 135.7(3) . . ? O_2 Nd5 O_1 81.9(3) . . ? O_9 Nd5 O_14 177.7(5) . . ? O_4 Nd5 O_14 68.1(3) . . ? O_3 Nd5 O_14 67.6(3) . . ? O_2 Nd5 O_14 67.4(3) . . ? O_1 Nd5 O_14 68.1(3) . . ? Nd5 O_14 Nd1 96.1(3) . . ? Nd5 O_14 Nd3 95.1(3) . . ? Nd1 O_14 Nd3 90.4(3) . . ? Nd5 O_14 Nd2 94.8(3) . . ? Nd1 O_14 Nd2 169.1(4) . . ? Nd3 O_14 Nd2 89.2(3) . . ? Nd5 O_14 Nd4 94.6(3) . . ? Nd1 O_14 Nd4 89.8(3) . . ? Nd3 O_14 Nd4 170.2(4) . . ? Nd2 O_14 Nd4 88.7(3) . . ? C_1 O_1 Nd5 125.8(9) . . ? C_1 O_1 Nd3 122.4(12) . . ? Nd5 O_1 Nd3 94.7(3) . . ? C_1 O_1 Nd2 122.4(10) . . ? Nd5 O_1 Nd2 94.2(3) . . ? Nd3 O_1 Nd2 87.8(3) . . ? O_1 C_1 C1B_1 114(2) . . ? O_1 C_1 C2B_1 116(2) . . ? C1B_1 C_1 C2B_1 121(3) . . ? O_1 C_1 C1A_1 112.6(18) . . ? C1B_1 C_1 C1A_1 33(3) . . ? C2B_1 C_1 C1A_1 131(3) . . ? O_1 C_1 C2A_1 112.7(17) . . ? C1B_1 C_1 C2A_1 131(3) . . ? C2B_1 C_1 C2A_1 43(3) . . ? C1A_1 C_1 C2A_1 113(2) . . ? C_2 O_2 Nd5 124.9(10) . . ? C_2 O_2 Nd1 121.4(11) . . ? Nd5 O_2 Nd1 94.5(3) . . ? C_2 O_2 Nd3 124.8(9) . . ? Nd5 O_2 Nd3 94.2(3) . . ? Nd1 O_2 Nd3 87.6(3) . . ? O_2 C_2 C2A_2 116.3(17) . . ? O_2 C_2 C2B_2 113.4(19) . . ? C2A_2 C_2 C2B_2 91(3) . . ? O_2 C_2 C1B_2 114.7(19) . . ? C2A_2 C_2 C1B_2 102(3) . . ? C2B_2 C_2 C1B_2 117(2) . . ? O_2 C_2 C1A_2 112.7(18) . . ? C2A_2 C_2 C1A_2 124(2) . . ? C2B_2 C_2 C1A_2 93(3) . . ? C1B_2 C_2 C1A_2 31(2) . . ? C_3 O_3 Nd5 123.6(9) . . ? C_3 O_3 Nd1 123.7(9) . . ? Nd5 O_3 Nd1 94.7(3) . . ? C_3 O_3 Nd4 123.3(10) . . ? Nd5 O_3 Nd4 94.4(3) . . ? Nd1 O_3 Nd4 87.8(3) . . ? O_3 C_3 C1B_3 115(2) . . ? O_3 C_3 C2B_3 112(3) . . ? C1B_3 C_3 C2B_3 117(3) . . ? O_3 C_3 C1A_3 113.1(15) . . ? C1B_3 C_3 C1A_3 55(3) . . ? C2B_3 C_3 C1A_3 132(4) . . ? O_3 C_3 C2A_3 111.8(16) . . ? C1B_3 C_3 C2A_3 132(3) . . ? C2B_3 C_3 C2A_3 31(4) . . ? C1A_3 C_3 C2A_3 112.8(18) . . ? C_4 O_4 Nd5 126.1(9) . . ? C_4 O_4 Nd4 123.1(9) . . ? Nd5 O_4 Nd4 95.4(3) . . ? C_4 O_4 Nd2 120.0(9) . . ? Nd5 O_4 Nd2 94.7(3) . . ? Nd4 O_4 Nd2 88.1(3) . . ? O_4 C_4 C2B_4 111(2) . . ? O_4 C_4 C1A_4 109.4(19) . . ? C2B_4 C_4 C1A_4 122(3) . . ? O_4 C_4 C1B_4 111(2) . . ? C2B_4 C_4 C1B_4 111(2) . . ? C1A_4 C_4 C1B_4 91(3) . . ? O_4 C_4 C2A_4 112(2) . . ? C2B_4 C_4 C2A_4 21(3) . . ? C1A_4 C_4 C2A_4 104(2) . . ? C1B_4 C_4 C2A_4 126(3) . . ? CB_5 O_5 CA_5 31(2) . . ? CB_5 O_5 Nd2 125.5(18) . . ? CA_5 O_5 Nd2 132.2(15) . . ? CB_5 O_5 Nd3 129.4(17) . . ? CA_5 O_5 Nd3 129.5(16) . . ? Nd2 O_5 Nd3 97.3(3) . . ? O_5 CA_5 C1A_5 115(3) . . ? O_5 CA_5 C2A_5 114(3) . . ? C1A_5 CA_5 C2A_5 106(3) . . ? O_5 CB_5 C2B_5 116(3) . . ? O_5 CB_5 C1B_5 115(3) . . ? C2B_5 CB_5 C1B_5 117(3) . . ? CB_6 O_6 CA_6 14(4) . . ? CB_6 O_6 Nd3 130(3) . . ? CA_6 O_6 Nd3 142(2) . . ? CB_6 O_6 Nd1 132(3) . . ? CA_6 O_6 Nd1 120(2) . . ? Nd3 O_6 Nd1 97.6(4) . . ? O_6 CA_6 C2A_6 110(3) . . ? O_6 CA_6 C1A_6 107(3) . . ? C2A_6 CA_6 C1A_6 116(3) . . ? O_6 CB_6 C1B_6 113(3) . . ? O_6 CB_6 C2B_6 114(3) . . ? C1B_6 CB_6 C2B_6 112(3) . . ? C_7 O_7 Nd1 129.6(12) . . ? C_7 O_7 Nd4 133.0(12) . . ? Nd1 O_7 Nd4 97.4(4) . . ? O_7 C_7 C1B_7 117(2) . . ? O_7 C_7 C1A_7 115(3) . . ? C1B_7 C_7 C1A_7 46(4) . . ? O_7 C_7 C2B_7 119(2) . . ? C1B_7 C_7 C2B_7 119(2) . . ? C1A_7 C_7 C2B_7 89(5) . . ? O_7 C_7 C2A_7 113(3) . . ? C1B_7 C_7 C2A_7 82(4) . . ? C1A_7 C_7 C2A_7 121(3) . . ? C2B_7 C_7 C2A_7 98(5) . . ? CA_8 O_8 CB_8 18(3) . . ? CA_8 O_8 Nd4 129.1(17) . . ? CB_8 O_8 Nd4 128(2) . . ? CA_8 O_8 Nd2 133.3(18) . . ? CB_8 O_8 Nd2 130.8(18) . . ? Nd4 O_8 Nd2 97.5(3) . . ? O_8 CA_8 C2A_8 117(3) . . ? O_8 CA_8 C1A_8 111(3) . . ? C2A_8 CA_8 C1A_8 114(3) . . ? O_8 CB_8 C2B_8 113(3) . . ? O_8 CB_8 C1B_8 112(3) . . ? C2B_8 CB_8 C1B_8 112(3) . . ? CA_9 O_9 CB_9 11(3) . . ? CA_9 O_9 Nd5 174(2) . . ? CB_9 O_9 Nd5 174(2) . . ? O_9 CA_9 C2A_9 111(3) . . ? O_9 CA_9 C1A_9 112(3) . . ? C2A_9 CA_9 C1A_9 116(3) . . ? O_9 CB_9 C1B_9 111(3) . . ? O_9 CB_9 C2B_9 111(3) . . ? C1B_9 CB_9 C2B_9 111(3) . . ? CA_10 O_10 CB_10 14(3) . . ? CA_10 O_10 Nd3 174(2) . . ? CB_10 O_10 Nd3 163(2) . . ? O_10 CA_10 C2A_10 116(3) . . ? O_10 CA_10 C1A_10 117(3) . . ? C2A_10 CA_10 C1A_10 117(3) . . ? O_10 CB_10 C2B_10 105(2) . . ? O_10 CB_10 C1B_10 114(3) . . ? C2B_10 CB_10 C1B_10 120(3) . . ? CA_11 O_11 CB_11 7(3) . . ? CA_11 O_11 Nd4 173(2) . . ? CB_11 O_11 Nd4 169(3) . . ? O_11 CA_11 C1A_11 116(2) . . ? O_11 CA_11 C2A_11 116(2) . . ? C1A_11 CA_11 C2A_11 120(3) . . ? O_11 CB_11 C1B_11 108(3) . . ? O_11 CB_11 C2B_11 111(3) . . ? C1B_11 CB_11 C2B_11 119(4) . . ? CB_12 O_12 CA_12 5(4) . . ? CB_12 O_12 Nd2 175(2) . . ? CA_12 O_12 Nd2 174.7(19) . . ? O_12 CA_12 C1A_12 111(3) . . ? O_12 CA_12 C2A_12 109(3) . . ? C1A_12 CA_12 C2A_12 108(3) . . ? O_12 CB_12 C1B_12 109(3) . . ? O_12 CB_12 C2B_12 109(3) . . ? C1B_12 CB_12 C2B_12 111(3) . . ? CB_13 O_13 CA_13 22(3) . . ? CB_13 O_13 Nd1 166(2) . . ? CA_13 O_13 Nd1 172.0(17) . . ? O_13 CA_13 C2A_13 109(2) . . ? O_13 CA_13 C1A_13 109(2) . . ? C2A_13 CA_13 C1A_13 119(3) . . ? O_13 CB_13 C1B_13 111(3) . . ? O_13 CB_13 C2B_13 111(3) . . ? C1B_13 CB_13 C2B_13 119(3) . . ? _diffrn_measured_fraction_theta_max .534 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full .534 _refine_diff_density_max .858 _refine_diff_density_min -.856 _refine_diff_density_rms .120 _ # ENDdata_Nd5O data_gd5O _database_code_CSD 158363 _audit_creation_date 96-10-16 _audit_creation_method 'X-RED, SHELXL' # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C39 H91 O14 Gd5' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H91 Gd5 O14' _chemical_formula_weight 1570.55 _chemical_melting_point ? _chemical_compound_source ? _computing_data_collection 'DIF4 (STOE, 1990)' _computing_cell_refinement 'DIF4 (STOE, 1990)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 12.7837(16) _cell_length_b 21.248(7) _cell_length_c 21.552(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.085(16) _cell_angle_gamma 90.00 _cell_volume 5853(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 _cell_special_details ; ? ; 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' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3028 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1321 _exptl_absorpt_correction_T_max 0.2672 _exptl_absorpt_coefficient_mu 5.64 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -7.00 -24.00 7.00 0.1617 1.00 -5.00 -1.00 0.1664 21.00 24.00 -17.00 0.1932 -4.00 10.00 -19.00 0.2352 -3.00 23.00 26.00 0.2856 26.00 -30.00 -3.00 0.2865 15.00 -2.00 28.00 0.2911 -13.00 29.00 -13.00 0.2227 -8.00 -26.00 13.00 0.1680 5.00 9.00 -19.00 0.2814 -1.00 25.00 7.00 0.1941 -1.00 16.00 -5.00 0.2033 -29.00 -3.00 21.00 0.2394 10.00 -22.00 -5.00 0.2268 -6.00 16.00 -1.00 0.2437 -7.00 -20.00 -28.00 0.1941 -25.00 2.00 21.00 0.2449 3.00 -12.00 28.00 0.1932 4.00 23.00 -11.00 0.1680 1.00 -24.00 -29.00 0.2017 _diffrn_measurement_device 'STOE-4' _diffrn_measurement_method ; Scan width (omega) = 1.08 - 1.23, scan ratio 2theta:omega = 1.00 ; _diffrn_special_details ? _diffrn_ambient_environment ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_collimation '4.0 mm' _diffrn_radiation_detector '?' _diffrn_radiation_monochromator graphite _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number 4 _diffrn_standards_decay_% 13.5 _diffrn_standards_interval_time 360 _diffrn_reflns_number 6706 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _reflns_number_total 5487 _reflns_number_gt 3372 _reflns_threshold_expression >2sigma(I) # REFINEMENT DATA from SHELXL _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 w=1/[\s^2^(Fo^2^)+(0.1207P)^2^+4.3157P] 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 5487 _refine_ls_number_parameters 328 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1688 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.59252(7) 0.31576(4) 0.10225(7) 0.0651(7) Uani 1 d . . . Gd2 Gd 0.55413(7) 0.18625(4) 0.28115(7) 0.0659(7) Uani 1 d . . . Gd3 Gd 0.72441(6) 0.19107(4) 0.16255(9) 0.0611(8) Uani 1 d . . . Gd4 Gd 0.41970(6) 0.30946(4) 0.21951(7) 0.0620(7) Uani 1 d . . . Gd5 Gd 0.45557(6) 0.17421(4) 0.12763(7) 0.0557(6) Uani 1 d . . . O1 O 0.5790(8) 0.1193(5) 0.1892(7) 0.058(5) Uani 1 d D . . O2 O 0.4089(7) 0.2801(5) 0.1085(7) 0.055(4) Uani 1 d DU . . O3 O 0.3855(7) 0.1968(5) 0.2236(7) 0.055(4) Uani 1 d DU . . O4 O 0.6034(8) 0.2032(5) 0.0714(9) 0.061(6) Uani 1 d D . . O5 O 0.5250(9) 0.3818(5) 0.1748(9) 0.098(7) Uani 1 d D . . O6 O 0.4942(9) 0.2817(7) 0.3103(10) 0.084(6) Uani 1 d D . . O7 O 0.7577(8) 0.2890(6) 0.1309(8) 0.076(6) Uani 1 d D . . O8 O 0.7283(9) 0.1921(6) 0.2702(10) 0.080(8) Uani 1 d D . . O9 O 0.3654(10) 0.1133(6) 0.0760(9) 0.103(7) Uani 1 d D . . O10 O 0.2752(8) 0.3494(6) 0.2384(8) 0.076(6) Uani 1 d D . . O11 O 0.8460(9) 0.1362(7) 0.1323(9) 0.107(7) Uani 1 d D . . O12 O 0.5313(11) 0.1211(7) 0.3538(9) 0.096(7) Uani 1 d D . . O13 O 0.6074(11) 0.3652(7) 0.0194(10) 0.095(7) Uani 1 d D . . O14 O 0.5635(6) 0.2449(4) 0.1864(6) 0.053(5) Uani 1 d . . . C1 C 0.5853(15) 0.0522(9) 0.1949(13) 0.084(6) Uiso 1 d D . . H1 H 0.5200 0.0366 0.2145 0.150 Uiso 1 calc R . . C2 C 0.3266(17) 0.2990(11) 0.0650(14) 0.110(9) Uiso 1 d D . . H2 H 0.3444 0.2835 0.0227 0.150 Uiso 1 calc R . . C3 C 0.2870(16) 0.1683(10) 0.2406(15) 0.091(7) Uiso 1 d D . . H3 H 0.2295 0.1844 0.2128 0.150 Uiso 1 calc R . . C4 C 0.6292(19) 0.1771(13) 0.0119(15) 0.115(10) Uiso 1 d D . . H4 H 0.6296 0.1302 0.0151 0.150 Uiso 1 calc R . . C5 C 0.530(2) 0.4482(12) 0.1769(16) 0.129(10) Uiso 1 d D . . H5 H 0.4892 0.4553 0.1376 0.150 Uiso 1 calc R . . C6 C 0.470(3) 0.3061(15) 0.3699(18) 0.148(13) Uiso 1 d D . . H6 H 0.3948 0.2982 0.3788 0.150 Uiso 1 calc R . . C7 C 0.852(3) 0.3245(17) 0.121(2) 0.190(16) Uiso 1 d D . . H7 H 0.8181 0.3581 0.0947 0.150 Uiso 1 calc R . . C8 C 0.818(2) 0.1779(14) 0.3097(16) 0.129(10) Uiso 1 d D . . H8 H 0.8302 0.1324 0.3191 0.150 Uiso 1 calc R . . C9 C 0.321(3) 0.0701(16) 0.0314(17) 0.177(14) Uiso 1 d D . . H9 H 0.3790 0.0548 0.0049 0.150 Uiso 1 calc R . . C10 C 0.177(2) 0.3755(18) 0.250(2) 0.177(14) Uiso 1 d D . . H10 H 0.1421 0.3486 0.2174 0.150 Uiso 1 calc R . . C11 C 0.940(3) 0.094(2) 0.128(2) 0.28(3) Uiso 1 d D . . H11 H 0.9431 0.0622 0.1616 0.150 Uiso 1 calc R . . C12 C 0.509(3) 0.0827(18) 0.411(2) 0.213(18) Uiso 1 d D . . H12 H 0.4703 0.1090 0.4415 0.150 Uiso 1 calc R . . C13 C 0.626(3) 0.3927(16) -0.0435(18) 0.174(15) Uiso 1 d D . . H13 H 0.6799 0.3682 -0.0660 0.150 Uiso 1 calc R . . C14 C 0.6743(17) 0.0334(12) 0.2329(12) 0.116(8) Uiso 1 d D . . H14A H 0.7385 0.0385 0.2093 0.200 Uiso 1 calc R . . H14B H 0.6665 -0.0108 0.2450 0.200 Uiso 1 calc R . . H14C H 0.6781 0.0598 0.2702 0.200 Uiso 1 calc R . . C15 C 0.5917(19) 0.0252(13) 0.1315(14) 0.136(10) Uiso 1 d D . . H15A H 0.5791 -0.0203 0.1333 0.200 Uiso 1 calc R . . H15B H 0.6614 0.0330 0.1151 0.200 Uiso 1 calc R . . H15C H 0.5388 0.0449 0.1044 0.200 Uiso 1 calc R . . C16 C 0.3204(16) 0.3692(10) 0.0636(13) 0.103(8) Uiso 1 d D . . H16A H 0.2469 0.3823 0.0617 0.200 Uiso 1 calc R . . H16B H 0.3563 0.3850 0.0269 0.200 Uiso 1 calc R . . H16C H 0.3540 0.3864 0.1011 0.200 Uiso 1 calc R . . C17 C 0.2246(14) 0.2682(10) 0.0849(13) 0.093(7) Uiso 1 d D . . H17A H 0.2227 0.2245 0.0704 0.200 Uiso 1 calc R . . H17B H 0.1651 0.2913 0.0669 0.200 Uiso 1 calc R . . H17C H 0.2207 0.2690 0.1303 0.200 Uiso 1 calc R . . C18 C 0.2911(18) 0.0983(11) 0.2372(14) 0.117(9) Uiso 1 d D . . H18A H 0.2200 0.0813 0.2389 0.200 Uiso 1 calc R . . H18B H 0.3329 0.0821 0.2722 0.200 Uiso 1 calc R . . H18C H 0.3232 0.0856 0.1982 0.200 Uiso 1 calc R . . C19 C 0.271(3) 0.1907(14) 0.3058(18) 0.169(14) Uiso 1 d D . . H19A H 0.2522 0.1549 0.3321 0.200 Uiso 1 calc R . . H19B H 0.2140 0.2217 0.3060 0.200 Uiso 1 calc R . . H19C H 0.3353 0.2101 0.3219 0.200 Uiso 1 calc R . . C20 C 0.727(2) 0.1974(14) -0.0121(17) 0.157(13) Uiso 1 d D . . H20A H 0.7422 0.1739 -0.0500 0.200 Uiso 1 calc R . . H20B H 0.7829 0.1898 0.0190 0.200 Uiso 1 calc R . . H20C H 0.7238 0.2425 -0.0215 0.200 Uiso 1 calc R . . C21 C 0.536(2) 0.1977(13) -0.0320(15) 0.143(11) Uiso 1 d D . . H21A H 0.4797 0.2156 -0.0070 0.200 Uiso 1 calc R . . H21B H 0.5090 0.1609 -0.0548 0.200 Uiso 1 calc R . . H21C H 0.5600 0.2293 -0.0615 0.200 Uiso 1 calc R . . C22 C 0.459(2) 0.4814(16) 0.2168(15) 0.176(14) Uiso 1 d D . . H22A H 0.4646 0.4646 0.2591 0.200 Uiso 1 calc R . . H22B H 0.3867 0.4757 0.2011 0.200 Uiso 1 calc R . . H22C H 0.4758 0.5264 0.2172 0.200 Uiso 1 calc R . . C23 C 0.623(2) 0.4758(16) 0.1561(17) 0.197(15) Uiso 1 d D . . H23A H 0.6300 0.5181 0.1737 0.200 Uiso 1 calc R . . H23B H 0.6204 0.4785 0.1107 0.200 Uiso 1 calc R . . H23C H 0.6828 0.4501 0.1693 0.200 Uiso 1 calc R . . C24 C 0.491(3) 0.3771(16) 0.367(2) 0.29(3) Uiso 1 d D . . H24A H 0.5612 0.3861 0.3832 0.200 Uiso 1 calc R . . H24B H 0.4392 0.3992 0.3923 0.200 Uiso 1 calc R . . H24C H 0.4842 0.3915 0.3240 0.200 Uiso 1 calc R . . C25 C 0.537(3) 0.2773(17) 0.419(2) 0.24(2) Uiso 1 d D . . H25A H 0.5065 0.2856 0.4596 0.200 Uiso 1 calc R . . H25B H 0.6071 0.2955 0.4177 0.200 Uiso 1 calc R . . H25C H 0.5408 0.2318 0.4122 0.200 Uiso 1 calc R . . C26 C 0.873(3) 0.3656(18) 0.1767(19) 0.224(18) Uiso 1 d D . . H26A H 0.8404 0.3470 0.2131 0.200 Uiso 1 calc R . . H26B H 0.8444 0.4077 0.1692 0.200 Uiso 1 calc R . . H26C H 0.9489 0.3687 0.1842 0.200 Uiso 1 calc R . . C27 C 0.926(4) 0.3070(19) 0.077(2) 0.27(3) Uiso 1 d D . . H27A H 0.9622 0.2687 0.0909 0.200 Uiso 1 calc R . . H27B H 0.9773 0.3410 0.0723 0.200 Uiso 1 calc R . . H27C H 0.8910 0.2991 0.0369 0.200 Uiso 1 calc R . . C28 C 0.912(3) 0.2136(18) 0.2907(19) 0.209(17) Uiso 1 d D . . H28A H 0.9542 0.1874 0.2636 0.200 Uiso 1 calc R . . H28B H 0.9531 0.2255 0.3276 0.200 Uiso 1 calc R . . H28C H 0.8896 0.2517 0.2684 0.200 Uiso 1 calc R . . C29 C 0.801(3) 0.219(2) 0.364(2) 0.28(2) Uiso 1 d D . . H29A H 0.8246 0.2617 0.3549 0.200 Uiso 1 calc R . . H29B H 0.8405 0.2025 0.4000 0.200 Uiso 1 calc R . . H29C H 0.7262 0.2196 0.3735 0.200 Uiso 1 calc R . . C30 C 0.254(2) 0.1032(15) -0.0052(16) 0.171(14) Uiso 1 d D . . H30A H 0.1825 0.0960 0.0080 0.200 Uiso 1 calc R . . H30B H 0.2616 0.0895 -0.0484 0.200 Uiso 1 calc R . . H30C H 0.2710 0.1481 -0.0020 0.200 Uiso 1 calc R . . C31 C 0.280(3) 0.0165(18) 0.0639(17) 0.216(17) Uiso 1 d D . . H31A H 0.3352 -0.0018 0.0905 0.200 Uiso 1 calc R . . H31B H 0.2556 -0.0151 0.0338 0.200 Uiso 1 calc R . . H31C H 0.2215 0.0298 0.0896 0.200 Uiso 1 calc R . . C32 C 0.152(4) 0.432(2) 0.217(2) 0.32(3) Uiso 1 d D . . H32A H 0.1877 0.4676 0.2368 0.200 Uiso 1 calc R . . H32B H 0.0762 0.4388 0.2172 0.200 Uiso 1 calc R . . H32C H 0.1749 0.4282 0.1739 0.200 Uiso 1 calc R . . C33 C 0.130(4) 0.343(2) 0.297(2) 0.30(3) Uiso 1 d D . . H33A H 0.0565 0.3358 0.2865 0.200 Uiso 1 calc R . . H33B H 0.1352 0.3683 0.3354 0.200 Uiso 1 calc R . . H33C H 0.1658 0.3029 0.3037 0.200 Uiso 1 calc R . . C34 C 0.924(3) 0.0648(16) 0.0673(18) 0.200(16) Uiso 1 d D . . H34A H 0.9654 0.0262 0.0650 0.200 Uiso 1 calc R . . H34B H 0.9450 0.0939 0.0346 0.200 Uiso 1 calc R . . H34C H 0.8494 0.0544 0.0616 0.200 Uiso 1 calc R . . C35 C 1.035(4) 0.137(3) 0.130(2) 0.42(4) Uiso 1 d D . . H35A H 1.0485 0.1506 0.1728 0.200 Uiso 1 calc R . . H35B H 1.0214 0.1742 0.1038 0.200 Uiso 1 calc R . . H35C H 1.0961 0.1146 0.1145 0.200 Uiso 1 calc R . . C36 C 0.617(3) 0.069(2) 0.435(2) 0.27(2) Uiso 1 d D . . H36A H 0.6172 0.0680 0.4806 0.200 Uiso 1 calc R . . H36B H 0.6653 0.1016 0.4211 0.200 Uiso 1 calc R . . H36C H 0.6400 0.0278 0.4195 0.200 Uiso 1 calc R . . C37 C 0.448(4) 0.030(3) 0.394(3) 0.51(6) Uiso 1 d D . . H37A H 0.3829 0.0434 0.3738 0.200 Uiso 1 calc R . . H37B H 0.4317 0.0056 0.4317 0.200 Uiso 1 calc R . . H37C H 0.4875 0.0030 0.3659 0.200 Uiso 1 calc R . . C38 C 0.668(2) 0.4574(14) -0.0236(17) 0.178(14) Uiso 1 d D . . H38A H 0.7239 0.4701 -0.0514 0.200 Uiso 1 calc R . . H38B H 0.6956 0.4550 0.0191 0.200 Uiso 1 calc R . . H38C H 0.6113 0.4884 -0.0257 0.200 Uiso 1 calc R . . C39 C 0.531(3) 0.393(2) -0.077(3) 0.40(4) Uiso 1 d D . . H39A H 0.5424 0.3774 -0.1185 0.200 Uiso 1 calc R . . H39B H 0.5048 0.4366 -0.0788 0.200 Uiso 1 calc R . . H39C H 0.4806 0.3666 -0.0555 0.200 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 Gd1 0.0623(5) 0.0593(6) 0.074(2) 0.0095(6) 0.0104(6) -0.0031(4) Gd2 0.0598(5) 0.0773(7) 0.061(2) 0.0066(7) -0.0001(6) 0.0015(4) Gd3 0.0438(4) 0.0729(6) 0.067(3) 0.0005(6) 0.0002(6) 0.0036(4) Gd4 0.0541(5) 0.0602(5) 0.072(2) -0.0067(6) 0.0070(6) 0.0031(4) Gd5 0.0472(4) 0.0560(5) 0.0638(18) -0.0066(6) -0.0022(5) -0.0031(3) O1 0.080(7) 0.049(6) 0.047(18) -0.003(7) 0.005(8) 0.009(5) O2 0.047(4) 0.075(6) 0.043(10) -0.003(6) -0.015(5) 0.007(4) O3 0.047(5) 0.074(6) 0.045(10) 0.002(6) 0.012(6) 0.000(4) O4 0.061(6) 0.065(7) 0.06(2) 0.005(9) -0.005(8) 0.010(5) O5 0.081(7) 0.031(6) 0.18(2) 0.010(8) -0.009(10) -0.001(5) O6 0.080(8) 0.096(10) 0.08(2) -0.004(11) 0.003(9) 0.012(7) O7 0.045(5) 0.078(8) 0.10(2) -0.005(9) 0.010(7) -0.015(5) O8 0.059(7) 0.103(10) 0.08(3) 0.002(10) -0.008(9) 0.005(6) O9 0.091(9) 0.090(9) 0.13(2) -0.036(11) -0.023(10) -0.033(7) O10 0.060(6) 0.116(10) 0.054(19) -0.011(10) 0.029(8) 0.031(7) O11 0.068(7) 0.144(13) 0.11(2) -0.006(13) 0.024(9) 0.052(8) O12 0.119(10) 0.114(12) 0.05(2) 0.047(12) 0.019(10) -0.018(9) O13 0.121(11) 0.099(11) 0.07(2) 0.030(12) 0.047(11) -0.005(8) O14 0.043(5) 0.050(6) 0.065(18) 0.010(7) 0.001(7) 0.002(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 Gd1 O13 2.084(19) . ? Gd1 O7 2.261(11) . ? Gd1 O5 2.283(16) . ? Gd1 O14 2.391(12) . ? Gd1 O2 2.473(10) . ? Gd1 O4 2.488(12) . ? Gd1 Gd3 3.3865(16) . ? Gd1 Gd4 3.3908(19) . ? Gd1 Gd5 3.5279(15) . ? Gd2 O12 2.114(16) . ? Gd2 O8 2.247(12) . ? Gd2 O6 2.261(15) . ? Gd2 O14 2.398(13) . ? Gd2 O1 2.466(14) . ? Gd2 O3 2.477(11) . ? Gd2 Gd4 3.3891(16) . ? Gd2 Gd3 3.390(2) . ? Gd2 Gd5 3.527(2) . ? Gd3 O11 2.060(12) . ? Gd3 O7 2.234(13) . ? Gd3 O8 2.32(2) . ? Gd3 O14 2.418(9) . ? Gd3 O1 2.481(11) . ? Gd3 O4 2.490(15) . ? Gd3 Gd5 3.5225(12) . ? Gd4 O10 2.080(10) . ? Gd4 O6 2.238(19) . ? Gd4 O5 2.269(13) . ? Gd4 O14 2.412(10) . ? Gd4 O3 2.435(11) . ? Gd4 O2 2.473(15) . ? Gd4 Gd5 3.5248(17) . ? Gd5 O9 2.048(13) . ? Gd5 O3 2.320(15) . ? Gd5 O4 2.346(14) . ? Gd5 O1 2.352(11) . ? Gd5 O2 2.362(11) . ? Gd5 O14 2.387(11) . ? O1 C1 1.43(2) . ? O2 C2 1.45(2) . ? O3 C3 1.45(2) . ? O4 C4 1.44(3) . ? O5 C5 1.41(2) . ? O6 C6 1.43(3) . ? O7 C7 1.44(3) . ? O8 C8 1.45(3) . ? O9 C9 1.44(3) . ? O10 C10 1.40(3) . ? O11 C11 1.51(3) . ? O12 C12 1.51(3) . ? O13 C13 1.50(3) . ? C1 C14 1.45(2) . ? C1 C15 1.49(3) . ? C2 C16 1.49(3) . ? C2 C17 1.53(3) . ? C3 C18 1.49(2) . ? C3 C19 1.50(3) . ? C4 C20 1.43(3) . ? C4 C21 1.57(3) . ? C5 C23 1.40(3) . ? C5 C22 1.45(3) . ? C6 C25 1.48(3) . ? C6 C24 1.53(3) . ? C7 C27 1.40(4) . ? C7 C26 1.51(3) . ? C8 C28 1.48(3) . ? C8 C29 1.48(4) . ? C9 C30 1.35(3) . ? C9 C31 1.44(3) . ? C10 C33 1.38(4) . ? C10 C32 1.43(4) . ? C11 C34 1.45(4) . ? C11 C35 1.52(4) . ? C12 C37 1.41(4) . ? C12 C36 1.50(3) . ? C13 C39 1.39(3) . ? C13 C38 1.54(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 O13 Gd1 O7 105.1(5) . . ? O13 Gd1 O5 108.6(6) . . ? O7 Gd1 O5 109.3(5) . . ? O13 Gd1 O14 170.2(5) . . ? O7 Gd1 O14 78.0(4) . . ? O5 Gd1 O14 78.5(5) . . ? O13 Gd1 O2 107.7(5) . . ? O7 Gd1 O2 142.3(4) . . ? O5 Gd1 O2 77.2(4) . . ? O14 Gd1 O2 66.7(4) . . ? O13 Gd1 O4 104.5(6) . . ? O7 Gd1 O4 77.0(4) . . ? O5 Gd1 O4 142.9(5) . . ? O14 Gd1 O4 66.9(5) . . ? O2 Gd1 O4 77.2(4) . . ? O13 Gd1 Gd3 132.1(4) . . ? O7 Gd1 Gd3 40.8(3) . . ? O5 Gd1 Gd3 114.2(4) . . ? O14 Gd1 Gd3 45.6(2) . . ? O2 Gd1 Gd3 101.9(3) . . ? O4 Gd1 Gd3 47.2(3) . . ? O13 Gd1 Gd4 136.9(4) . . ? O7 Gd1 Gd4 113.9(4) . . ? O5 Gd1 Gd4 41.7(3) . . ? O14 Gd1 Gd4 45.3(2) . . ? O2 Gd1 Gd4 46.7(3) . . ? O4 Gd1 Gd4 101.6(4) . . ? Gd3 Gd1 Gd4 90.56(4) . . ? O13 Gd1 Gd5 128.1(5) . . ? O7 Gd1 Gd5 102.0(3) . . ? O5 Gd1 Gd5 102.9(3) . . ? O14 Gd1 Gd5 42.4(3) . . ? O2 Gd1 Gd5 41.9(3) . . ? O4 Gd1 Gd5 41.6(3) . . ? Gd3 Gd1 Gd5 61.21(3) . . ? Gd4 Gd1 Gd5 61.22(3) . . ? O12 Gd2 O8 105.3(6) . . ? O12 Gd2 O6 109.3(7) . . ? O8 Gd2 O6 108.7(5) . . ? O12 Gd2 O14 168.8(6) . . ? O8 Gd2 O14 79.4(5) . . ? O6 Gd2 O14 78.0(6) . . ? O12 Gd2 O1 103.8(6) . . ? O8 Gd2 O1 78.7(5) . . ? O6 Gd2 O1 142.2(6) . . ? O14 Gd2 O1 66.8(4) . . ? O12 Gd2 O3 107.4(5) . . ? O8 Gd2 O3 142.9(6) . . ? O6 Gd2 O3 76.2(5) . . ? O14 Gd2 O3 65.4(4) . . ? O1 Gd2 O3 76.9(4) . . ? O12 Gd2 Gd4 136.1(4) . . ? O8 Gd2 Gd4 114.4(4) . . ? O6 Gd2 Gd4 40.9(5) . . ? O14 Gd2 Gd4 45.4(2) . . ? O1 Gd2 Gd4 101.7(3) . . ? O3 Gd2 Gd4 45.9(2) . . ? O12 Gd2 Gd3 132.7(4) . . ? O8 Gd2 Gd3 42.9(5) . . ? O6 Gd2 Gd3 114.1(5) . . ? O14 Gd2 Gd3 45.5(2) . . ? O1 Gd2 Gd3 46.9(3) . . ? O3 Gd2 Gd3 100.7(3) . . ? Gd4 Gd2 Gd3 90.52(4) . . ? O12 Gd2 Gd5 126.5(5) . . ? O8 Gd2 Gd5 104.0(6) . . ? O6 Gd2 Gd5 102.0(5) . . ? O14 Gd2 Gd5 42.4(2) . . ? O1 Gd2 Gd5 41.7(3) . . ? O3 Gd2 Gd5 41.0(3) . . ? Gd4 Gd2 Gd5 61.24(4) . . ? Gd3 Gd2 Gd5 61.19(4) . . ? O11 Gd3 O7 106.4(5) . . ? O11 Gd3 O8 108.7(6) . . ? O7 Gd3 O8 107.2(5) . . ? O11 Gd3 O14 170.3(5) . . ? O7 Gd3 O14 78.0(4) . . ? O8 Gd3 O14 77.6(4) . . ? O11 Gd3 O1 107.4(5) . . ? O7 Gd3 O1 142.3(3) . . ? O8 Gd3 O1 77.1(4) . . ? O14 Gd3 O1 66.3(3) . . ? O11 Gd3 O4 105.7(6) . . ? O7 Gd3 O4 77.4(4) . . ? O8 Gd3 O4 142.1(4) . . ? O14 Gd3 O4 66.4(5) . . ? O1 Gd3 O4 77.8(4) . . ? O11 Gd3 Gd1 134.0(5) . . ? O7 Gd3 Gd1 41.4(3) . . ? O8 Gd3 Gd1 112.2(3) . . ? O14 Gd3 Gd1 44.9(3) . . ? O1 Gd3 Gd1 101.5(2) . . ? O4 Gd3 Gd1 47.1(3) . . ? O11 Gd3 Gd2 136.1(5) . . ? O7 Gd3 Gd2 112.8(4) . . ? O8 Gd3 Gd2 41.3(3) . . ? O14 Gd3 Gd2 45.0(3) . . ? O1 Gd3 Gd2 46.6(3) . . ? O4 Gd3 Gd2 101.5(3) . . ? Gd1 Gd3 Gd2 89.48(4) . . ? O11 Gd3 Gd5 127.9(5) . . ? O7 Gd3 Gd5 102.7(3) . . ? O8 Gd3 Gd5 102.5(3) . . ? O14 Gd3 Gd5 42.5(3) . . ? O1 Gd3 Gd5 41.8(3) . . ? O4 Gd3 Gd5 41.7(3) . . ? Gd1 Gd3 Gd5 61.37(3) . . ? Gd2 Gd3 Gd5 61.33(4) . . ? O10 Gd4 O6 107.5(6) . . ? O10 Gd4 O5 110.1(5) . . ? O6 Gd4 O5 107.7(5) . . ? O10 Gd4 O14 167.0(5) . . ? O6 Gd4 O14 78.2(5) . . ? O5 Gd4 O14 78.3(4) . . ? O10 Gd4 O3 103.5(5) . . ? O6 Gd4 O3 77.5(5) . . ? O5 Gd4 O3 142.1(5) . . ? O14 Gd4 O3 65.8(3) . . ? O10 Gd4 O2 105.0(5) . . ? O6 Gd4 O2 142.5(5) . . ? O5 Gd4 O2 77.5(5) . . ? O14 Gd4 O2 66.4(4) . . ? O3 Gd4 O2 77.3(5) . . ? O10 Gd4 Gd2 133.1(4) . . ? O6 Gd4 Gd2 41.4(4) . . ? O5 Gd4 Gd2 112.9(3) . . ? O14 Gd4 Gd2 45.0(3) . . ? O3 Gd4 Gd2 46.9(3) . . ? O2 Gd4 Gd2 101.7(2) . . ? O10 Gd4 Gd1 136.4(4) . . ? O6 Gd4 Gd1 112.9(4) . . ? O5 Gd4 Gd1 42.0(4) . . ? O14 Gd4 Gd1 44.8(3) . . ? O3 Gd4 Gd1 100.7(3) . . ? O2 Gd4 Gd1 46.7(2) . . ? Gd2 Gd4 Gd1 89.42(4) . . ? O10 Gd4 Gd5 124.6(4) . . ? O6 Gd4 Gd5 102.6(4) . . ? O5 Gd4 Gd5 103.2(4) . . ? O14 Gd4 Gd5 42.5(2) . . ? O3 Gd4 Gd5 40.9(3) . . ? O2 Gd4 Gd5 42.0(3) . . ? Gd2 Gd4 Gd5 61.31(4) . . ? Gd1 Gd4 Gd5 61.31(3) . . ? O9 Gd5 O3 113.1(6) . . ? O9 Gd5 O4 109.6(6) . . ? O3 Gd5 O4 137.3(5) . . ? O9 Gd5 O1 110.9(5) . . ? O3 Gd5 O1 82.3(4) . . ? O4 Gd5 O1 83.3(4) . . ? O9 Gd5 O2 111.7(5) . . ? O3 Gd5 O2 81.8(5) . . ? O4 Gd5 O2 82.2(4) . . ? O1 Gd5 O2 137.4(4) . . ? O9 Gd5 O14 178.8(5) . . ? O3 Gd5 O14 68.0(4) . . ? O4 Gd5 O14 69.2(5) . . ? O1 Gd5 O14 68.8(4) . . ? O2 Gd5 O14 68.5(3) . . ? O9 Gd5 Gd3 135.8(4) . . ? O3 Gd5 Gd3 100.4(3) . . ? O4 Gd5 Gd3 44.9(4) . . ? O1 Gd5 Gd3 44.7(3) . . ? O2 Gd5 Gd3 100.5(2) . . ? O14 Gd5 Gd3 43.2(2) . . ? O9 Gd5 Gd4 138.0(4) . . ? O3 Gd5 Gd4 43.4(3) . . ? O4 Gd5 Gd4 101.0(3) . . ? O1 Gd5 Gd4 100.4(3) . . ? O2 Gd5 Gd4 44.4(4) . . ? O14 Gd5 Gd4 43.0(2) . . ? Gd3 Gd5 Gd4 86.21(3) . . ? O9 Gd5 Gd2 138.0(5) . . ? O3 Gd5 Gd2 44.4(3) . . ? O4 Gd5 Gd2 100.9(4) . . ? O1 Gd5 Gd2 44.2(3) . . ? O2 Gd5 Gd2 100.3(3) . . ? O14 Gd5 Gd2 42.6(3) . . ? Gd3 Gd5 Gd2 57.49(4) . . ? Gd4 Gd5 Gd2 57.45(3) . . ? O9 Gd5 Gd1 136.9(5) . . ? O3 Gd5 Gd1 99.4(3) . . ? O4 Gd5 Gd1 44.7(3) . . ? O1 Gd5 Gd1 100.4(3) . . ? O2 Gd5 Gd1 44.4(2) . . ? O14 Gd5 Gd1 42.4(3) . . ? Gd3 Gd5 Gd1 57.41(3) . . ? Gd4 Gd5 Gd1 57.47(3) . . ? Gd2 Gd5 Gd1 85.08(4) . . ? C1 O1 Gd5 125.3(11) . . ? C1 O1 Gd2 120.9(15) . . ? Gd5 O1 Gd2 94.1(4) . . ? C1 O1 Gd3 126.2(11) . . ? Gd5 O1 Gd3 93.6(4) . . ? Gd2 O1 Gd3 86.5(4) . . ? C2 O2 Gd5 123.6(12) . . ? C2 O2 Gd1 123.8(12) . . ? Gd5 O2 Gd1 93.7(3) . . ? C2 O2 Gd4 125.6(14) . . ? Gd5 O2 Gd4 93.6(5) . . ? Gd1 O2 Gd4 86.6(4) . . ? C3 O3 Gd5 119.3(14) . . ? C3 O3 Gd4 125.3(11) . . ? Gd5 O3 Gd4 95.7(5) . . ? C3 O3 Gd2 126.0(14) . . ? Gd5 O3 Gd2 94.6(3) . . ? Gd4 O3 Gd2 87.3(3) . . ? C4 O4 Gd5 124.0(12) . . ? C4 O4 Gd3 120.9(12) . . ? Gd5 O4 Gd3 93.4(6) . . ? C4 O4 Gd1 128.5(15) . . ? Gd5 O4 Gd1 93.7(5) . . ? Gd3 O4 Gd1 85.7(5) . . ? C5 O5 Gd4 133.7(15) . . ? C5 O5 Gd1 128.1(17) . . ? Gd4 O5 Gd1 96.3(4) . . ? C6 O6 Gd4 126.6(17) . . ? C6 O6 Gd2 131.0(19) . . ? Gd4 O6 Gd2 97.8(8) . . ? C7 O7 Gd3 134.3(18) . . ? C7 O7 Gd1 127.3(19) . . ? Gd3 O7 Gd1 97.8(4) . . ? C8 O8 Gd2 134.7(18) . . ? C8 O8 Gd3 126.0(16) . . ? Gd2 O8 Gd3 95.8(6) . . ? C9 O9 Gd5 168(2) . . ? C10 O10 Gd4 179(2) . . ? C11 O11 Gd3 165(2) . . ? C12 O12 Gd2 172(2) . . ? C13 O13 Gd1 172.0(17) . . ? Gd5 O14 Gd1 95.2(5) . . ? Gd5 O14 Gd2 95.0(3) . . ? Gd1 O14 Gd2 169.8(5) . . ? Gd5 O14 Gd4 94.5(3) . . ? Gd1 O14 Gd4 89.8(3) . . ? Gd2 O14 Gd4 89.6(4) . . ? Gd5 O14 Gd3 94.3(4) . . ? Gd1 O14 Gd3 89.5(4) . . ? Gd2 O14 Gd3 89.5(3) . . ? Gd4 O14 Gd3 171.2(5) . . ? O1 C1 C14 111.5(18) . . ? O1 C1 C15 108(2) . . ? C14 C1 C15 111(2) . . ? O2 C2 C16 109.1(19) . . ? O2 C2 C17 108(2) . . ? C16 C2 C17 112.9(19) . . ? O3 C3 C18 111.9(19) . . ? O3 C3 C19 104(2) . . ? C18 C3 C19 112(3) . . ? C20 C4 O4 115(2) . . ? C20 C4 C21 111(3) . . ? O4 C4 C21 104(2) . . ? C23 C5 O5 117(2) . . ? C23 C5 C22 122(3) . . ? O5 C5 C22 118(3) . . ? O6 C6 C25 111(3) . . ? O6 C6 C24 106(3) . . ? C25 C6 C24 110(2) . . ? C27 C7 O7 123(4) . . ? C27 C7 C26 125(3) . . ? O7 C7 C26 109(3) . . ? O8 C8 C28 112(3) . . ? O8 C8 C29 102(3) . . ? C28 C8 C29 93(3) . . ? C30 C9 O9 107(3) . . ? C30 C9 C31 118(3) . . ? O9 C9 C31 109(3) . . ? C33 C10 O10 110(4) . . ? C33 C10 C32 134(4) . . ? O10 C10 C32 116(4) . . ? C34 C11 O11 102(3) . . ? C34 C11 C35 113(3) . . ? O11 C11 C35 106(4) . . ? C37 C12 C36 115(3) . . ? C37 C12 O12 110(4) . . ? C36 C12 O12 101(3) . . ? C39 C13 O13 109(4) . . ? C39 C13 C38 116(3) . . ? O13 C13 C38 99(3) . . ? _diffrn_measured_fraction_theta_max 0.518 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.518 _refine_diff_density_max 1.213 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.177 # ENDdata_Gd5O data_Er5O _database_code_CSD 158364 _audit_creation_date 96-11-28 _audit_creation_method 'X-RED, SHELXL' # CHEMICAL DATA # from shelxl _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C39 H91 O14 Er5' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H91 Er5 O14' _chemical_formula_weight 1620.42 _chemical_melting_point ? _chemical_compound_source ? _computing_data_collection 'DIF4 (STOE, 1990)' _computing_cell_refinement 'DIF4 (STOE, 1990)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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' # from X-RED _cell_length_a 12.769(4) _cell_length_b 21.432(19) _cell_length_c 21.297(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.267(20) _cell_angle_gamma 90.00 _cell_volume 5826.5 _cell_formula_units_Z 4.0 _cell_measurement_temperature 170(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 _cell_special_details ; ? ; #from shelxl 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' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #from X-RED _exptl_crystal_description irregular _exptl_crystal_colour pink _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_meas ? _exptl_crystal_F_000 3108 #from shelxl _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'X-RED (STOE, 1996)' _exptl_absorpt_correction_T_min 0.0219 _exptl_absorpt_correction_T_max 0.1063 _exptl_absorpt_coefficient_mu 7.17 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 5.00 0.00 -6.00 0.3990 -5.00 0.00 6.00 0.3800 0.00 1.00 0.00 0.1425 0.00 -1.00 0.00 0.2565 -2.00 -1.00 -4.00 0.2850 1.00 0.00 2.00 0.3515 _diffrn_measurement_device '' _diffrn_measurement_method ; Scan width (omega) = 1.20 - 1.35, scan ratio 2theta:omega = 1.00 ; _diffrn_special_details ? _diffrn_ambient_environment ? _diffrn_ambient_temperature 170(1) _diffrn_radiation_collimation '4.0 mm' _diffrn_radiation_detector '' _diffrn_radiation_monochromator graphite _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number 4 _diffrn_standards_decay_% 10.8 _diffrn_standards_interval_time 240 _diffrn_reflns_number 6023 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 23.99 _diffrn_reflns_av_sigmaI/netI 0.1321 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 24 # from shelxl _reflns_number_total 3913 _reflns_number_gt 3913 _reflns_observed_criterion >2sigma(I) # REFINEMENT DATA from SHELXL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+( 0.1245P)^2^+250.3243P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3913 _refine_ls_number_parameters 394 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_obs 0.0791 _refine_ls_wR_factor_all 0.2246 _refine_ls_wR_factor_obs 0.2246 _refine_ls_goodness_of_fit_all 1.187 _refine_ls_goodness_of_fit_obs 1.187 _refine_ls_restrained_S_all 1.171 _refine_ls_restrained_S_obs 1.171 _refine_ls_shift/esd_max -0.009 _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 Er1 Er 0.4594(2) 0.18227(12) 0.22006(9) 0.0738(7) Uani 1 d . . Er2 Er 0.28946(14) 0.19071(10) 0.33434(9) 0.0635(6) Uani 1 d . . Er3 Er 0.4152(2) 0.31403(10) 0.39054(9) 0.0678(6) Uani 1 d . . Er4 Er 0.5881(2) 0.30352(10) 0.27794(9) 0.0647(6) Uani 1 d . . Er5 Er 0.55034(14) 0.17663(9) 0.37262(9) 0.0557(5) Uani 1 d . . O1 O 0.4038(20) 0.2075(13) 0.4253(11) 0.064(7) Uani 1 d D . O2 O 0.5912(16) 0.2810(11) 0.3906(10) 0.045(6) Uani 1 d D . O3 O 0.6241(17) 0.1963(13) 0.2778(11) 0.059(7) Uani 1 d D . O4 O 0.4285(19) 0.1221(12) 0.3119(12) 0.059(7) Uani 1 d D . O5 O 0.2857(19) 0.1895(15) 0.2291(14) 0.082(9) Uani 1 d D . O6 O 0.2529(22) 0.2877(14) 0.3598(18) 0.093(11) Uani 1 d D . O7 O 0.5145(23) 0.2708(14) 0.1848(16) 0.082(9) Uani 1 d D . O8 O 0.4853(26) 0.3779(12) 0.3201(15) 0.085(9) Uani 1 d DU . O9 O 0.4850(30) 0.1172(17) 0.1519(14) 0.107(13) Uani 1 d D . O10 O 0.7315(23) 0.3439(15) 0.2629(16) 0.092(10) Uani 1 d D . O11 O 0.4014(29) 0.3693(17) 0.4674(17) 0.116(14) Uani 1 d D . O12 O 0.1676(22) 0.1374(14) 0.3631(15) 0.083(9) Uani 1 d D . O13 O 0.6395(27) 0.1224(17) 0.4281(17) 0.108(13) Uani 1 d D . O14 O 0.4461(17) 0.2396(12) 0.3103(11) 0.052(7) Uani 1 d . . C1 C 0.3694(41) 0.1916(26) 0.4888(17) 0.099(17) Uani 1 d DU . H1 H 0.3047(41) 0.2154(26) 0.4943(17) 0.119 Uiso 1 calc R . C2 C 0.6708(37) 0.2977(23) 0.4387(30) 0.145(25) Uani 1 d DU . H2 H 0.6498(37) 0.2845(23) 0.4807(30) 0.174 Uiso 1 calc R . C3 C 0.7207(39) 0.1673(23) 0.2577(27) 0.118(20) Uani 1 d DU . H3 H 0.7758(39) 0.1837(23) 0.2859(27) 0.141 Uiso 1 calc R . C4 C 0.4240(35) 0.0551(19) 0.3120(22) 0.091(15) Uani 1 d DU . H4 H 0.4874(35) 0.0451(19) 0.2889(22) 0.110 Uiso 1 calc R . C5 C 0.1978(46) 0.1787(34) 0.1852(26) 0.179(31) Uani 1 d DU . H5 H 0.1856(46) 0.1338(34) 0.1805(26) 0.215 Uiso 1 calc R . C6 C 0.1487(41) 0.3138(27) 0.3628(30) 0.142(25) Uani 1 d DU . H6 H 0.1029(41) 0.2891(27) 0.3349(30) 0.171 Uiso 1 calc R . C7 C 0.5401(53) 0.2934(33) 0.1227(23) 0.141(25) Uani 1 d DU . H7 H 0.6131(53) 0.2845(33) 0.1125(23) 0.170 Uiso 1 calc R . C8 C 0.4561(59) 0.4396(26) 0.3065(43) 0.192(33) Uani 1 d DU . H8 H 0.4162(59) 0.4362(26) 0.2669(43) 0.230 Uiso 1 calc R . C9 C 0.5233(62) 0.0789(39) 0.1033(34) 0.210(38) Uani 1 d DU . H9 H 0.5956(62) 0.0904(39) 0.0940(34) 0.253 Uiso 1 calc R . C10 C 0.8254(48) 0.3831(36) 0.2675(39) 0.196(35) Uani 1 d DU . H10 H 0.8457(48) 0.4038(36) 0.3070(39) 0.235 Uiso 1 calc R . C11 C 0.4025(61) 0.4110(37) 0.5225(32) 0.222(42) Uani 1 d DU . H11 H 0.4741(61) 0.4266(37) 0.5285(32) 0.266 Uiso 1 calc R . C12 C 0.0743(39) 0.1045(29) 0.3721(34) 0.139(24) Uani 1 d DU . H12 H 0.0625(39) 0.0824(29) 0.3322(34) 0.167 Uiso 1 calc R . C13 C 0.6984(66) 0.0804(34) 0.4655(35) 0.212(40) Uani 1 d DU . H13 H 0.6389(66) 0.0613(34) 0.4865(35) 0.254 Uiso 1 calc R . C14 C 0.4447(55) 0.2152(37) 0.5409(33) 0.190(34) Uiso 1 d D . H14A H 0.4439(55) 0.1868(37) 0.5758(33) 0.284 Uiso 1 calc R . H14B H 0.4228(55) 0.2558(37) 0.5545(33) 0.284 Uiso 1 calc R . H14C H 0.5143(55) 0.2177(37) 0.5251(33) 0.284 Uiso 1 calc R . C15 C 0.3396(64) 0.1260(30) 0.4990(43) 0.210(39) Uiso 1 d D . H15A H 0.2734(64) 0.1244(30) 0.5195(43) 0.315 Uiso 1 calc R . H15B H 0.3921(64) 0.1058(30) 0.5248(43) 0.315 Uiso 1 calc R . H15C H 0.3338(64) 0.1049(30) 0.4592(43) 0.315 Uiso 1 calc R . C16 C 0.7740(39) 0.2654(27) 0.4192(27) 0.112(19) Uiso 1 d D . H16A H 0.8038(39) 0.2434(27) 0.4545(27) 0.168 Uiso 1 calc R . H16B H 0.8226(39) 0.2963(27) 0.4052(27) 0.168 Uiso 1 calc R . H16C H 0.7592(39) 0.2365(27) 0.3856(27) 0.168 Uiso 1 calc R . C17 C 0.6868(44) 0.3675(24) 0.4355(29) 0.122(21) Uiso 1 d D . H17A H 0.7199(44) 0.3780(24) 0.3969(29) 0.182 Uiso 1 calc R . H17B H 0.7305(44) 0.3807(24) 0.4703(29) 0.182 Uiso 1 calc R . H17C H 0.6202(44) 0.3882(24) 0.4373(29) 0.182 Uiso 1 calc R . C18 C 0.7262(45) 0.0971(24) 0.2643(29) 0.124(21) Uiso 1 d D . H18A H 0.7960(45) 0.0832(24) 0.2559(29) 0.187 Uiso 1 calc R . H18B H 0.6778(45) 0.0781(24) 0.2349(29) 0.187 Uiso 1 calc R . H18C H 0.7083(45) 0.0855(24) 0.3063(29) 0.187 Uiso 1 calc R . C19 C 0.7528(52) 0.1848(32) 0.1930(27) 0.153(26) Uiso 1 d D . H19A H 0.7047(52) 0.1668(32) 0.1628(27) 0.229 Uiso 1 calc R . H19B H 0.8221(52) 0.1694(32) 0.1858(27) 0.229 Uiso 1 calc R . H19C H 0.7522(52) 0.2294(32) 0.1888(27) 0.229 Uiso 1 calc R . C20 C 0.4429(50) 0.0198(30) 0.3696(27) 0.144(24) Uiso 1 d D . H20A H 0.4846(50) -0.0163(30) 0.3607(27) 0.217 Uiso 1 calc R . H20B H 0.3772(50) 0.0068(30) 0.3863(27) 0.217 Uiso 1 calc R . H20C H 0.4793(50) 0.0455(30) 0.3998(27) 0.217 Uiso 1 calc R . C21 C 0.3403(39) 0.0297(26) 0.2673(24) 0.115(19) Uiso 1 d D . H21A H 0.3235(39) -0.0124(26) 0.2789(24) 0.173 Uiso 1 calc R . H21B H 0.3658(39) 0.0302(26) 0.2252(24) 0.173 Uiso 1 calc R . H21C H 0.2786(39) 0.0551(26) 0.2694(24) 0.173 Uiso 1 calc R . C22 C 0.1006(59) 0.2100(40) 0.2133(36) 0.218(42) Uiso 1 d D . H22A H 0.0398(59) 0.2003(40) 0.1878(36) 0.328 Uiso 1 calc R . H22B H 0.1106(59) 0.2544(40) 0.2144(36) 0.328 Uiso 1 calc R . H22C H 0.0910(59) 0.1948(40) 0.2552(36) 0.328 Uiso 1 calc R . C23 C 0.2178(58) 0.2072(38) 0.1223(35) 0.209(39) Uiso 1 d D . H23A H 0.1572(58) 0.2303(38) 0.1084(35) 0.314 Uiso 1 calc R . H23B H 0.2322(58) 0.1748(38) 0.0926(35) 0.314 Uiso 1 calc R . H23C H 0.2769(58) 0.2348(38) 0.1257(35) 0.314 Uiso 1 calc R . C24 C 0.1061(75) 0.3104(40) 0.4261(35) 0.248(49) Uiso 1 d D . H24A H 0.0326(75) 0.3200(40) 0.4243(35) 0.373 Uiso 1 calc R . H24B H 0.1417(75) 0.3399(40) 0.4530(35) 0.373 Uiso 1 calc R . H24C H 0.1160(75) 0.2691(40) 0.4426(35) 0.373 Uiso 1 calc R . C25 C 0.1574(86) 0.3765(39) 0.3356(45) 0.311(66) Uiso 1 d D . H25A H 0.0900(86) 0.3964(39) 0.3353(45) 0.466 Uiso 1 calc R . H25B H 0.1816(86) 0.3732(39) 0.2933(45) 0.466 Uiso 1 calc R . H25C H 0.2062(86) 0.4008(39) 0.3603(45) 0.466 Uiso 1 calc R . C26 C 0.5236(85) 0.3621(41) 0.1375(59) 0.299(63) Uiso 1 d D . H26A H 0.4538(85) 0.3741(41) 0.1249(59) 0.449 Uiso 1 calc R . H26B H 0.5732(85) 0.3868(41) 0.1150(59) 0.449 Uiso 1 calc R . H26C H 0.5335(85) 0.3689(41) 0.1818(59) 0.449 Uiso 1 calc R . C27 C 0.4681(62) 0.2759(43) 0.0718(38) 0.224(43) Uiso 1 d D . H27A H 0.5073(62) 0.2634(43) 0.0359(38) 0.336 Uiso 1 calc R . H27B H 0.4245(62) 0.3108(43) 0.0609(38) 0.336 Uiso 1 calc R . H27C H 0.4252(62) 0.2418(43) 0.0851(38) 0.336 Uiso 1 calc R . C28 C 0.5523(54) 0.4766(37) 0.2892(37) 0.184(33) Uiso 1 d D . H28A H 0.5955(54) 0.4832(37) 0.3261(37) 0.276 Uiso 1 calc R . H28B H 0.5311(54) 0.5161(37) 0.2720(37) 0.276 Uiso 1 calc R . H28C H 0.5911(54) 0.4539(37) 0.2586(37) 0.276 Uiso 1 calc R . C29 C 0.3934(78) 0.4840(48) 0.3444(50) 0.293(61) Uiso 1 d D . H29A H 0.3671(78) 0.5169(48) 0.3178(50) 0.439 Uiso 1 calc R . H29B H 0.4370(78) 0.5015(48) 0.3772(50) 0.439 Uiso 1 calc R . H29C H 0.3357(78) 0.4623(48) 0.3626(50) 0.439 Uiso 1 calc R . C30 C 0.5165(78) 0.0121(44) 0.1179(53) 0.272(56) Uiso 1 d D . H30A H 0.5527(78) -0.0114(44) 0.0868(53) 0.408 Uiso 1 calc R . H30B H 0.4443(78) -0.0004(44) 0.1180(53) 0.408 Uiso 1 calc R . H30C H 0.5480(78) 0.0043(44) 0.1585(53) 0.408 Uiso 1 calc R . C31 C 0.4539(77) 0.0914(52) 0.0485(46) 0.298(63) Uiso 1 d D . H31A H 0.4735(77) 0.0650(52) 0.0142(46) 0.447 Uiso 1 calc R . H31B H 0.4603(77) 0.1343(52) 0.0363(46) 0.447 Uiso 1 calc R . H31C H 0.3827(77) 0.0828(52) 0.0592(46) 0.447 Uiso 1 calc R . C32 C 0.9021(60) 0.3438(35) 0.2327(37) 0.171(31) Uiso 1 d D . H32A H 0.9460(60) 0.3215(35) 0.2622(37) 0.256 Uiso 1 calc R . H32B H 0.9446(60) 0.3701(35) 0.2072(37) 0.256 Uiso 1 calc R . H32C H 0.8647(60) 0.3146(35) 0.2064(37) 0.256 Uiso 1 calc R . C33 C 0.8091(98) 0.4198(56) 0.2079(53) 0.357(79) Uiso 1 d D . H33A H 0.8730(98) 0.4406(56) 0.1977(53) 0.535 Uiso 1 calc R . H33B H 0.7548(98) 0.4501(56) 0.2137(53) 0.535 Uiso 1 calc R . H33C H 0.7891(98) 0.3920(56) 0.1744(53) 0.535 Uiso 1 calc R . C34 C 0.3320(58) 0.4663(35) 0.5087(36) 0.189(34) Uiso 1 d D . H34A H 0.3610(58) 0.5029(35) 0.5284(36) 0.284 Uiso 1 calc R . H34B H 0.2636(58) 0.4584(35) 0.5248(36) 0.284 Uiso 1 calc R . H34C H 0.3266(58) 0.4728(35) 0.4641(36) 0.284 Uiso 1 calc R . C35 C 0.3735(81) 0.3776(44) 0.5805(48) 0.296(64) Uiso 1 d D . H35A H 0.3505(81) 0.4072(44) 0.6111(48) 0.444 Uiso 1 calc R . H35B H 0.4332(81) 0.3553(44) 0.5970(48) 0.444 Uiso 1 calc R . H35C H 0.3179(81) 0.3487(44) 0.5710(48) 0.444 Uiso 1 calc R . C36 C 0.0917(52) 0.0557(32) 0.4166(33) 0.160(28) Uiso 1 d D . H36A H 0.0870(52) 0.0161(32) 0.3958(33) 0.240 Uiso 1 calc R . H36B H 0.0397(52) 0.0579(32) 0.4484(33) 0.240 Uiso 1 calc R . H36C H 0.1601(52) 0.0603(32) 0.4357(33) 0.240 Uiso 1 calc R . C37 C -0.0268(76) 0.1383(61) 0.3820(72) 0.386(89) Uiso 1 d D . H37A H -0.0809(76) 0.1086(61) 0.3908(72) 0.579 Uiso 1 calc R . H37B H -0.0457(76) 0.1614(61) 0.3449(72) 0.579 Uiso 1 calc R . H37C H -0.0186(76) 0.1665(61) 0.4168(72) 0.579 Uiso 1 calc R . C38 C 0.7436(61) 0.1126(38) 0.5218(37) 0.190(34) Uiso 1 d D . H38A H 0.7973(61) 0.0869(38) 0.5407(37) 0.285 Uiso 1 calc R . H38B H 0.6895(61) 0.1198(38) 0.5515(37) 0.285 Uiso 1 calc R . H38C H 0.7733(61) 0.1518(38) 0.5095(37) 0.285 Uiso 1 calc R . C39 C 0.7379(60) 0.0230(36) 0.4371(37) 0.183(33) Uiso 1 d D . H39A H 0.6840(60) -0.0083(36) 0.4371(37) 0.275 Uiso 1 calc R . H39B H 0.7977(60) 0.0084(36) 0.4609(37) 0.275 Uiso 1 calc R . H39C H 0.7577(60) 0.0313(36) 0.3947(37) 0.275 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 Er1 0.0699(13) 0.099(2) 0.0525(11) -0.0112(12) 0.0017(9) -0.0041(13) Er2 0.0486(11) 0.076(2) 0.0658(12) -0.0025(11) 0.0009(9) -0.0013(10) Er3 0.0667(12) 0.0637(14) 0.0734(13) -0.0083(11) 0.0122(10) 0.0023(11) Er4 0.0591(11) 0.0719(15) 0.0634(12) 0.0097(11) 0.0082(9) -0.0003(11) Er5 0.0498(10) 0.0579(12) 0.0592(11) 0.0056(10) -0.0033(8) 0.0050(10) O1 0.063(17) 0.080(20) 0.048(16) -0.006(14) -0.009(13) -0.011(14) O2 0.028(12) 0.065(17) 0.042(13) 0.005(12) -0.011(10) -0.029(11) O3 0.042(13) 0.084(20) 0.052(15) 0.008(14) 0.014(12) 0.013(14) O4 0.055(16) 0.061(18) 0.061(17) -0.027(14) 0.007(13) -0.007(13) O5 0.042(15) 0.112(26) 0.090(21) 0.016(20) -0.026(14) -0.007(17) O6 0.058(18) 0.068(21) 0.154(32) 0.028(21) 0.003(21) 0.001(16) O7 0.076(21) 0.081(23) 0.088(23) 0.017(18) -0.001(18) -0.009(17) O8 0.125(23) 0.035(15) 0.096(20) 0.023(15) 0.009(18) 0.008(16) O9 0.144(32) 0.117(29) 0.059(20) -0.056(19) 0.013(20) -0.024(24) O10 0.066(19) 0.100(26) 0.113(25) 0.010(21) 0.036(19) -0.038(18) O11 0.122(29) 0.110(29) 0.118(29) -0.071(24) 0.052(24) -0.021(23) O12 0.069(19) 0.083(23) 0.097(23) -0.006(19) 0.000(18) -0.018(17) O13 0.102(25) 0.114(29) 0.106(26) 0.039(22) -0.059(21) 0.017(22) O14 0.034(13) 0.083(20) 0.039(13) -0.003(13) -0.006(11) 0.002(13) C1 0.109(34) 0.117(41) 0.071(28) 0.022(29) -0.008(26) -0.063(32) C2 0.114(41) 0.070(38) 0.249(64) 0.015(42) -0.015(47) -0.015(32) C3 0.119(40) 0.104(42) 0.133(43) -0.014(36) 0.039(36) 0.004(35) C4 0.065(28) 0.104(39) 0.105(35) 0.007(32) -0.005(27) -0.017(27) C5 0.186(58) 0.263(68) 0.087(38) -0.063(47) -0.037(40) 0.041(54) C6 0.139(49) 0.129(49) 0.159(49) 0.074(42) 0.021(42) 0.018(41) C7 0.152(49) 0.147(51) 0.122(45) -0.006(41) -0.044(41) -0.062(43) C8 0.204(47) 0.171(46) 0.202(47) 0.021(38) 0.062(37) -0.013(37) C9 0.230(66) 0.224(71) 0.173(60) -0.002(57) -0.085(55) -0.060(58) C10 0.165(58) 0.254(71) 0.170(59) 0.038(57) 0.014(52) 0.019(57) C11 0.244(71) 0.197(69) 0.226(71) -0.011(61) 0.007(62) 0.038(60) C12 0.097(39) 0.137(47) 0.187(54) 0.009(44) 0.079(40) -0.028(36) C13 0.199(64) 0.238(73) 0.196(65) -0.038(60) -0.033(56) 0.022(58) _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 O9 2.04(3) . ? Er1 O7 2.16(3) . ? Er1 O5 2.24(3) . ? Er1 O14 2.29(2) . ? Er1 O4 2.38(3) . ? Er1 O3 2.43(2) . ? Er1 Er4 3.299(4) . ? Er1 Er2 3.301(3) . ? Er1 Er5 3.428(3) . ? Er2 O12 2.04(3) . ? Er2 O6 2.20(3) . ? Er2 O5 2.24(3) . ? Er2 O14 2.33(2) . ? Er2 O4 2.36(2) . ? Er2 O1 2.43(2) . ? Er2 Er3 3.303(4) . ? Er2 Er5 3.425(3) . ? Er3 O11 2.03(3) . ? Er3 O6 2.23(3) . ? Er3 O8 2.23(3) . ? Er3 O2 2.36(2) . ? Er3 O14 2.38(2) . ? Er3 O1 2.40(3) . ? Er3 Er4 3.303(3) . ? Er3 Er5 3.438(4) . ? Er4 O10 2.06(3) . ? Er4 O8 2.26(3) . ? Er4 O7 2.29(3) . ? Er4 O3 2.34(3) . ? Er4 O14 2.39(2) . ? Er4 O2 2.45(2) . ? Er4 Er5 3.426(3) . ? Er5 O13 2.00(3) . ? Er5 O3 2.29(2) . ? Er5 O14 2.30(2) . ? Er5 O1 2.30(3) . ? Er5 O4 2.32(2) . ? Er5 O2 2.33(2) . ? O1 C1 1.47(4) . ? O2 C2 1.47(4) . ? O3 C3 1.45(4) . ? O4 C4 1.44(4) . ? O5 C5 1.46(4) . ? O6 C6 1.45(4) . ? O7 C7 1.45(4) . ? O8 C8 1.40(4) . ? O9 C9 1.42(5) . ? O10 C10 1.47(5) . ? O11 C11 1.47(5) . ? O12 C12 1.40(4) . ? O13 C13 1.41(4) . ? C1 C15 1.48(4) . ? C1 C14 1.54(4) . ? C2 C17 1.51(4) . ? C2 C16 1.55(4) . ? C3 C19 1.49(4) . ? C3 C18 1.51(4) . ? C4 C20 1.46(4) . ? C4 C21 1.52(4) . ? C5 C23 1.50(5) . ? C5 C22 1.54(4) . ? C6 C24 1.47(5) . ? C6 C25 1.47(5) . ? C7 C27 1.45(5) . ? C7 C26 1.52(5) . ? C8 C29 1.49(5) . ? C8 C28 1.51(4) . ? C9 C30 1.47(5) . ? C9 C31 1.47(5) . ? C10 C32 1.50(5) . ? C10 C33 1.50(5) . ? C11 C35 1.48(5) . ? C11 C34 1.52(5) . ? C12 C36 1.43(4) . ? C12 C37 1.50(5) . ? C13 C39 1.46(5) . ? C13 C38 1.49(5) . ? 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 O9 Er1 O7 107.0(14) . . ? O9 Er1 O5 106.4(13) . . ? O7 Er1 O5 107.4(11) . . ? O9 Er1 O14 167.9(13) . . ? O7 Er1 O14 81.5(11) . . ? O5 Er1 O14 78.4(9) . . ? O9 Er1 O4 104.2(12) . . ? O7 Er1 O4 145.1(11) . . ? O5 Er1 O4 77.5(9) . . ? O14 Er1 O4 65.5(8) . . ? O9 Er1 O3 107.1(12) . . ? O7 Er1 O3 77.5(10) . . ? O5 Er1 O3 142.8(9) . . ? O14 Er1 O3 65.7(8) . . ? O4 Er1 O3 79.0(8) . . ? O9 Er1 Er4 135.8(10) . . ? O7 Er1 Er4 43.6(9) . . ? O5 Er1 Er4 113.6(8) . . ? O14 Er1 Er4 46.3(6) . . ? O4 Er1 Er4 102.1(6) . . ? O3 Er1 Er4 45.2(6) . . ? O9 Er1 Er2 132.8(10) . . ? O7 Er1 Er2 115.6(9) . . ? O5 Er1 Er2 42.5(7) . . ? O14 Er1 Er2 44.8(6) . . ? O4 Er1 Er2 45.6(6) . . ? O3 Er1 Er2 101.3(5) . . ? Er4 Er1 Er2 90.66(7) . . ? O9 Er1 Er5 126.4(11) . . ? O7 Er1 Er5 104.7(9) . . ? O5 Er1 Er5 103.7(7) . . ? O14 Er1 Er5 41.7(6) . . ? O4 Er1 Er5 42.4(6) . . ? O3 Er1 Er5 41.7(5) . . ? Er4 Er1 Er5 61.19(6) . . ? Er2 Er1 Er5 61.16(6) . . ? O12 Er2 O6 106.7(12) . . ? O12 Er2 O5 107.2(11) . . ? O6 Er2 O5 104.9(13) . . ? O12 Er2 O14 170.5(11) . . ? O6 Er2 O14 79.4(10) . . ? O5 Er2 O14 77.5(8) . . ? O12 Er2 O4 107.2(11) . . ? O6 Er2 O4 143.3(10) . . ? O5 Er2 O4 77.9(9) . . ? O14 Er2 O4 65.3(9) . . ? O12 Er2 O1 107.1(11) . . ? O6 Er2 O1 77.9(11) . . ? O5 Er2 O1 143.1(9) . . ? O14 Er2 O1 66.6(8) . . ? O4 Er2 O1 79.2(9) . . ? O12 Er2 Er1 135.3(9) . . ? O6 Er2 Er1 112.3(9) . . ? O5 Er2 Er1 42.4(6) . . ? O14 Er2 Er1 43.9(6) . . ? O4 Er2 Er1 46.2(7) . . ? O1 Er2 Er1 101.7(6) . . ? O12 Er2 Er3 135.1(9) . . ? O6 Er2 Er3 42.2(8) . . ? O5 Er2 Er3 111.8(8) . . ? O14 Er2 Er3 46.0(6) . . ? O4 Er2 Er3 102.1(6) . . ? O1 Er2 Er3 46.6(7) . . ? Er1 Er2 Er3 89.35(7) . . ? O12 Er2 Er5 128.7(9) . . ? O6 Er2 Er5 103.6(8) . . ? O5 Er2 Er5 103.7(6) . . ? O14 Er2 Er5 41.9(6) . . ? O4 Er2 Er5 42.4(6) . . ? O1 Er2 Er5 42.1(6) . . ? Er1 Er2 Er5 61.25(6) . . ? Er3 Er2 Er5 61.43(6) . . ? O11 Er3 O6 106.6(14) . . ? O11 Er3 O8 103.1(14) . . ? O6 Er3 O8 109.9(12) . . ? O11 Er3 O2 106.0(12) . . ? O6 Er3 O2 143.5(10) . . ? O8 Er3 O2 77.8(10) . . ? O11 Er3 O14 171.7(13) . . ? O6 Er3 O14 77.7(11) . . ? O8 Er3 O14 81.5(10) . . ? O2 Er3 O14 68.0(7) . . ? O11 Er3 O1 107.4(13) . . ? O6 Er3 O1 77.8(9) . . ? O8 Er3 O1 144.8(10) . . ? O2 Er3 O1 77.2(8) . . ? O14 Er3 O1 66.2(8) . . ? O11 Er3 Er4 134.1(10) . . ? O6 Er3 Er4 113.7(10) . . ? O8 Er3 Er4 43.1(8) . . ? O2 Er3 Er4 47.7(5) . . ? O14 Er3 Er4 46.2(6) . . ? O1 Er3 Er4 101.8(6) . . ? O11 Er3 Er2 135.1(10) . . ? O6 Er3 Er2 41.5(8) . . ? O8 Er3 Er2 116.5(8) . . ? O2 Er3 Er2 102.4(5) . . ? O14 Er3 Er2 44.7(6) . . ? O1 Er3 Er2 47.1(6) . . ? Er4 Er3 Er2 90.56(7) . . ? O11 Er3 Er5 129.9(12) . . ? O6 Er3 Er5 102.5(8) . . ? O8 Er3 Er5 104.0(8) . . ? O2 Er3 Er5 42.4(5) . . ? O14 Er3 Er5 41.8(5) . . ? O1 Er3 Er5 41.9(6) . . ? Er4 Er3 Er5 61.05(6) . . ? Er2 Er3 Er5 61.03(7) . . ? O10 Er4 O8 106.9(12) . . ? O10 Er4 O7 110.2(12) . . ? O8 Er4 O7 109.2(11) . . ? O10 Er4 O3 103.7(11) . . ? O8 Er4 O3 143.8(9) . . ? O7 Er4 O3 77.0(9) . . ? O10 Er4 O14 166.2(11) . . ? O8 Er4 O14 80.7(10) . . ? O7 Er4 O14 76.9(9) . . ? O3 Er4 O14 65.7(8) . . ? O10 Er4 O2 103.9(11) . . ? O8 Er4 O2 75.4(9) . . ? O7 Er4 O2 141.9(9) . . ? O3 Er4 O2 79.0(8) . . ? O14 Er4 O2 66.4(7) . . ? O10 Er4 Er1 135.4(10) . . ? O8 Er4 Er1 114.5(8) . . ? O7 Er4 Er1 40.7(8) . . ? O3 Er4 Er1 47.4(6) . . ? O14 Er4 Er1 44.0(6) . . ? O2 Er4 Er1 102.0(5) . . ? O10 Er4 Er3 134.1(10) . . ? O8 Er4 Er3 42.4(7) . . ? O7 Er4 Er3 112.5(8) . . ? O3 Er4 Er3 101.6(5) . . ? O14 Er4 Er3 46.0(6) . . ? O2 Er4 Er3 45.4(5) . . ? Er1 Er4 Er3 89.39(7) . . ? O10 Er4 Er5 124.3(10) . . ? O8 Er4 Er5 103.6(7) . . ? O7 Er4 Er5 101.9(8) . . ? O3 Er4 Er5 41.6(5) . . ? O14 Er4 Er5 42.0(5) . . ? O2 Er4 Er5 42.7(5) . . ? Er1 Er4 Er5 61.26(7) . . ? Er3 Er4 Er5 61.43(6) . . ? O13 Er5 O3 112.9(13) . . ? O13 Er5 O14 179.0(13) . . ? O3 Er5 O14 68.0(8) . . ? O13 Er5 O1 109.8(13) . . ? O3 Er5 O1 137.1(9) . . ? O14 Er5 O1 69.2(8) . . ? O13 Er5 O4 113.8(13) . . ? O3 Er5 O4 83.4(9) . . ? O14 Er5 O4 66.5(9) . . ? O1 Er5 O4 82.7(8) . . ? O13 Er5 O2 109.9(12) . . ? O3 Er5 O2 82.7(9) . . ? O14 Er5 O2 69.8(8) . . ? O1 Er5 O2 79.9(9) . . ? O4 Er5 O2 136.2(9) . . ? O13 Er5 Er2 137.0(11) . . ? O3 Er5 Er2 101.0(6) . . ? O14 Er5 Er2 42.5(6) . . ? O1 Er5 Er2 45.0(6) . . ? O4 Er5 Er2 43.5(6) . . ? O2 Er5 Er2 99.7(5) . . ? O13 Er5 Er4 136.5(11) . . ? O3 Er5 Er4 42.9(7) . . ? O14 Er5 Er4 44.0(6) . . ? O1 Er5 Er4 100.7(7) . . ? O4 Er5 Er4 100.0(7) . . ? O2 Er5 Er4 45.6(5) . . ? Er2 Er5 Er4 86.50(6) . . ? O13 Er5 Er1 139.3(11) . . ? O3 Er5 Er1 45.1(6) . . ? O14 Er5 Er1 41.6(6) . . ? O1 Er5 Er1 100.9(6) . . ? O4 Er5 Er1 43.9(7) . . ? O2 Er5 Er1 101.1(5) . . ? Er2 Er5 Er1 57.59(6) . . ? Er4 Er5 Er1 57.55(6) . . ? O13 Er5 Er3 135.6(11) . . ? O3 Er5 Er3 99.1(6) . . ? O14 Er5 Er3 43.5(6) . . ? O1 Er5 Er3 44.2(7) . . ? O4 Er5 Er3 99.3(6) . . ? O2 Er5 Er3 43.1(5) . . ? Er2 Er5 Er3 57.54(6) . . ? Er4 Er5 Er3 57.52(7) . . ? Er1 Er5 Er3 85.11(7) . . ? C1 O1 Er5 130.1(29) . . ? C1 O1 Er3 121.6(27) . . ? Er5 O1 Er3 93.9(9) . . ? C1 O1 Er2 120.9(23) . . ? Er5 O1 Er2 92.9(8) . . ? Er3 O1 Er2 86.3(8) . . ? C2 O2 Er5 119.9(24) . . ? C2 O2 Er3 124.8(26) . . ? Er5 O2 Er3 94.5(7) . . ? C2 O2 Er4 129.1(27) . . ? Er5 O2 Er4 91.7(8) . . ? Er3 O2 Er4 86.9(7) . . ? C3 O3 Er5 123.3(25) . . ? C3 O3 Er4 125.9(25) . . ? Er5 O3 Er4 95.4(9) . . ? C3 O3 Er1 121.9(29) . . ? Er5 O3 Er1 93.2(8) . . ? Er4 O3 Er1 87.4(8) . . ? C4 O4 Er5 122.0(23) . . ? C4 O4 Er2 126.3(25) . . ? Er5 O4 Er2 94.1(8) . . ? C4 O4 Er1 123.3(24) . . ? Er5 O4 Er1 93.7(9) . . ? Er2 O4 Er1 88.2(9) . . ? C5 O5 Er1 133.0(32) . . ? C5 O5 Er2 129.8(32) . . ? Er1 O5 Er2 95.0(9) . . ? C6 O6 Er2 125.2(32) . . ? C6 O6 Er3 137.7(35) . . ? Er2 O6 Er3 96.3(11) . . ? C7 O7 Er1 133.7(33) . . ? C7 O7 Er4 126.2(29) . . ? Er1 O7 Er4 95.6(12) . . ? C8 O8 Er3 127.5(37) . . ? C8 O8 Er4 137.4(39) . . ? Er3 O8 Er4 94.5(10) . . ? C9 O9 Er1 167.7(45) . . ? C10 O10 Er4 163.9(39) . . ? C11 O11 Er3 174.2(41) . . ? C12 O12 Er2 168.9(37) . . ? C13 O13 Er5 175.9(44) . . ? Er1 O14 Er5 96.7(9) . . ? Er1 O14 Er2 91.3(9) . . ? Er5 O14 Er2 95.6(9) . . ? Er1 O14 Er3 168.5(11) . . ? Er5 O14 Er3 94.7(8) . . ? Er2 O14 Er3 89.2(8) . . ? Er1 O14 Er4 89.7(8) . . ? Er5 O14 Er4 94.0(8) . . ? Er2 O14 Er4 170.1(11) . . ? Er3 O14 Er4 87.8(8) . . ? O1 C1 C15 116.0(52) . . ? O1 C1 C14 113.2(42) . . ? C15 C1 C14 111.5(55) . . ? O2 C2 C17 107.6(42) . . ? O2 C2 C16 106.3(42) . . ? C17 C2 C16 108.2(47) . . ? O3 C3 C19 114.6(46) . . ? O3 C3 C18 115.8(43) . . ? C19 C3 C18 108.8(49) . . ? O4 C4 C20 121.0(44) . . ? O4 C4 C21 112.7(36) . . ? C20 C4 C21 116.3(44) . . ? O5 C5 C23 111.3(62) . . ? O5 C5 C22 107.2(51) . . ? C23 C5 C22 108.9(35) . . ? O6 C6 C24 112.4(59) . . ? O6 C6 C25 105.0(60) . . ? C24 C6 C25 116.2(40) . . ? O7 C7 C27 116.1(56) . . ? O7 C7 C26 95.8(63) . . ? C27 C7 C26 108.4(76) . . ? O8 C8 C29 129.4(74) . . ? O8 C8 C28 109.3(58) . . ? C29 C8 C28 104.2(67) . . ? O9 C9 C30 112.8(78) . . ? O9 C9 C31 105.2(68) . . ? C30 C9 C31 107.8(80) . . ? O10 C10 C32 100.8(56) . . ? O10 C10 C33 98.4(69) . . ? C32 C10 C33 87.5(67) . . ? O11 C11 C35 111.9(77) . . ? O11 C11 C34 109.0(63) . . ? C35 C11 C34 112.4(38) . . ? O12 C12 C36 109.8(55) . . ? O12 C12 C37 120.9(73) . . ? C36 C12 C37 112.4(73) . . ? O13 C13 C39 119.2(63) . . ? O13 C13 C38 110.6(60) . . ? C39 C13 C38 126.2(64) . . ? _refine_diff_density_max 2.349 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.258 # ENDdata_Er5O