Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Polly Arnold' 'Alexander J. Blake' 'Louise S. Natrajan' 'Julia Weinstein' 'Claire Wilson' _publ_contact_author_name 'Dr Polly Arnold ' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email POLLY.ARNOLD@NOTTINGHAM.AC.UK _publ_section_title ; Group (I) cation templated formation of luminescent heterobimetallic mono- and bis-substituted thionaphthol complexes of Pr, Nd, Eu and Tb ; # Attachment 'Ln_acac_4cifs.CIF' data_PRDITH_compound_1a _database_code_depnum_ccdc_archive 'CCDC 298869' _refine_special_details ; There is disorder in all solvent groups; disordered THF ligated to Pr (C51-C54, O7),modelled by two parts with a common Uiso on O7 and C52. The first with a refined occupancy of 0.6, the second occupancy of 0.4. DFIX and SADI restraints applied. The Et2O solvent ligated to K also shows significant disorder (C61-C64, O8). The disorder was also modelled over 2 sites for C61 and C62, with a common Uiso for O8. The occupancies were refined as 0.6 and 0.4 respectively. Severe disorder was also identified in the Et2O lattice solvent molecule (C1S-C4s, O1S). However, no sensible disorder model could be identified. Squeeze was used to minimise the residual electron density. All partially occupied atom sites were modelled with isotropic adps, and all H- atoms omitted' ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H100 K O8 Pr S. 0.6(C4 H10 O)' _chemical_formula_sum 'C68.40 H106 K O8.60 Pr S' _chemical_formula_weight 1278.00 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 11.0568(14) _cell_length_b 15.356(2) _cell_length_c 21.298(3) _cell_angle_alpha 95.917(2) _cell_angle_beta 104.844(2) _cell_angle_gamma 91.941(2) _cell_volume 3470.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7571 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.3 _exptl_crystal_description column _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1358 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS version 2.01a; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31401 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.069 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 29.07 _reflns_number_total 16042 _reflns_number_gt 11993 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _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^)+(0.050P)^2^+2.518P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Et2O H omitted' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16042 _refine_ls_number_parameters 720 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.116 _refine_ls_wR_factor_gt 0.102 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K K 0.86060(8) 0.71773(6) 0.88856(4) 0.03507(19) Uani 1 1 d . A . S1 S 0.50493(8) 0.75454(5) 0.75993(4) 0.02341(17) Uani 1 1 d . A . Pr Pr 0.714843(18) 0.653578(13) 0.710717(9) 0.02431(6) Uani 1 1 d . A . O1 O 0.7769(2) 0.78751(15) 0.78133(11) 0.0262(5) Uani 1 1 d . . . O2 O 0.6556(2) 0.60647(15) 0.79971(12) 0.0296(5) Uani 1 1 d . . . O3 O 0.9226(2) 0.63189(16) 0.78298(11) 0.0276(5) Uani 1 1 d . . . O4 O 0.7643(2) 0.50333(17) 0.69300(13) 0.0349(6) Uani 1 1 d . . . O5 O 0.6157(2) 0.74078(18) 0.62853(12) 0.0347(6) Uani 1 1 d . . . O6 O 0.8416(2) 0.67190(18) 0.63638(12) 0.0378(6) Uani 1 1 d . . . O7 O 0.5086(2) 0.56765(19) 0.64842(14) 0.0423(7) Uani 1 1 d D . . O8 O 0.9020(3) 0.7496(2) 1.02140(14) 0.0500(8) Uani 1 1 d D . . C11 C 0.5872(3) 0.8581(2) 0.76553(15) 0.0227(7) Uani 1 1 d . . . C12 C 0.7164(3) 0.8594(2) 0.77342(15) 0.0228(7) Uani 1 1 d . . . C13 C 0.7833(3) 0.9421(2) 0.77190(16) 0.0260(7) Uani 1 1 d . . . C14 C 0.7153(3) 1.0140(2) 0.75977(16) 0.0249(7) Uani 1 1 d . . . H14A H 0.7591 1.0679 0.7586 0.030 Uiso 1 1 calc R . . C15 C 0.5193(3) 1.0900(2) 0.73641(16) 0.0273(7) Uani 1 1 d . . . H15A H 0.5661 1.1422 0.7344 0.033 Uiso 1 1 calc R . . C16 C 0.3916(3) 1.0922(2) 0.72708(17) 0.0285(8) Uani 1 1 d . . . C17 C 0.3259(3) 1.0116(2) 0.72815(18) 0.0310(8) Uani 1 1 d . . . H17A H 0.2373 1.0103 0.7207 0.037 Uiso 1 1 calc R . . C18 C 0.3849(3) 0.9359(2) 0.73945(17) 0.0277(7) Uani 1 1 d . . . H18A H 0.3364 0.8835 0.7390 0.033 Uiso 1 1 calc R . . C19 C 0.5168(3) 0.9338(2) 0.75176(15) 0.0226(7) Uani 1 1 d . . . C20 C 0.5834(3) 1.0129(2) 0.74889(16) 0.0239(7) Uani 1 1 d . . . C21 C 0.5408(3) 0.7170(2) 0.83944(16) 0.0231(7) Uani 1 1 d . . . C22 C 0.6037(3) 0.6397(2) 0.84517(16) 0.0242(7) Uani 1 1 d . A . C23 C 0.6157(3) 0.5959(2) 0.90381(17) 0.0259(7) Uani 1 1 d . . . C24 C 0.5702(3) 0.6360(2) 0.95283(17) 0.0266(7) Uani 1 1 d . . . H24A H 0.5811 0.6092 0.9920 0.032 Uiso 1 1 calc R . . C25 C 0.4581(3) 0.7510(2) 0.99975(16) 0.0258(7) Uani 1 1 d . . . H25A H 0.4706 0.7229 1.0384 0.031 Uiso 1 1 calc R . . C26 C 0.3922(3) 0.8253(2) 0.99538(16) 0.0243(7) Uani 1 1 d . . . C27 C 0.3792(3) 0.8669(2) 0.93794(17) 0.0260(7) Uani 1 1 d . . . H27A H 0.3362 0.9194 0.9343 0.031 Uiso 1 1 calc R . . C28 C 0.4261(3) 0.8343(2) 0.88755(16) 0.0250(7) Uani 1 1 d . . . H28A H 0.4151 0.8646 0.8500 0.030 Uiso 1 1 calc R C . C29 C 0.4908(3) 0.7560(2) 0.89026(16) 0.0237(7) Uani 1 1 d . . . C30 C 0.5083(3) 0.7148(2) 0.94848(16) 0.0239(7) Uani 1 1 d . . . C31 C 1.0039(3) 0.5756(2) 0.78010(17) 0.0286(8) Uani 1 1 d . . . C32 C 0.9772(3) 0.4925(2) 0.74562(19) 0.0330(8) Uani 1 1 d . . . H32A H 1.0445 0.4549 0.7490 0.040 Uiso 1 1 calc R . . C33 C 0.8598(3) 0.4592(2) 0.70629(18) 0.0328(8) Uani 1 1 d . . . C41 C 0.6310(3) 0.7677(2) 0.57677(17) 0.0311(8) Uani 1 1 d . . . C42 C 0.7350(4) 0.7512(3) 0.55247(18) 0.0368(9) Uani 1 1 d . . . H42A H 0.7374 0.7726 0.5125 0.044 Uiso 1 1 calc R . . C43 C 0.8356(4) 0.7053(3) 0.58347(19) 0.0361(9) Uani 1 1 d . . . C51 C 0.4347(8) 0.5136(7) 0.6781(4) 0.074(3) Uiso 0.60 1 d PD A 1 H51A H 0.4113 0.5481 0.7146 0.088 Uiso 0.60 1 calc PR A 1 H51B H 0.4816 0.4635 0.6949 0.088 Uiso 0.60 1 calc PR A 1 C51' C 0.3991(8) 0.5538(7) 0.6718(5) 0.047(3) Uiso 0.40 1 d PD A 2 H51C H 0.3534 0.6080 0.6728 0.056 Uiso 0.40 1 calc PR A 2 H51D H 0.4225 0.5354 0.7163 0.056 Uiso 0.40 1 calc PR A 2 C52 C 0.3198(6) 0.4822(4) 0.6237(3) 0.091(2) Uiso 1 1 d D . . H52A H 0.2458 0.5128 0.6303 0.109 Uiso 1 1 calc R A 1 H52B H 0.3023 0.4183 0.6223 0.109 Uiso 1 1 calc R A 1 C53 C 0.3488(7) 0.5033(7) 0.5606(4) 0.066(2) Uiso 0.60 1 d PD A 1 H53A H 0.3351 0.4504 0.5283 0.079 Uiso 0.60 1 calc PR A 1 H53B H 0.2957 0.5494 0.5412 0.079 Uiso 0.60 1 calc PR A 1 C53' C 0.3919(16) 0.4577(9) 0.5735(9) 0.118(7) Uiso 0.40 1 d PD A 2 H53C H 0.3353 0.4494 0.5288 0.142 Uiso 0.40 1 calc PR A 2 H53D H 0.4351 0.4030 0.5822 0.142 Uiso 0.40 1 calc PR A 2 C54 C 0.4864(5) 0.5355(4) 0.5818(3) 0.0705(15) Uiso 1 1 d D A . H54A H 0.5405 0.4868 0.5760 0.085 Uiso 1 1 calc R B 1 H54B H 0.5029 0.5825 0.5560 0.085 Uiso 1 1 calc R B 1 C61 C 0.9227(9) 0.6491(7) 1.1026(6) 0.072(3) Uani 0.60 1 d PD C 1 H61A H 0.9831 0.6199 1.1345 0.109 Uiso 0.60 1 calc PR C 1 H61B H 0.8687 0.6050 1.0701 0.109 Uiso 0.60 1 calc PR C 1 H61C H 0.8712 0.6847 1.1251 0.109 Uiso 0.60 1 calc PR C 1 C62 C 0.9920(7) 0.7072(8) 1.0690(5) 0.059(3) Uani 0.60 1 d PD C 1 H62A H 1.0466 0.7520 1.1016 0.070 Uiso 0.60 1 calc PR C 1 H62B H 1.0454 0.6718 1.0468 0.070 Uiso 0.60 1 calc PR C 1 C61' C 1.0124(13) 0.7030(9) 1.1288(5) 0.059(3) Uani 0.40 1 d PD C 2 H61D H 1.0195 0.6529 1.1543 0.089 Uiso 0.40 1 calc PR C 2 H61E H 0.9811 0.7522 1.1519 0.089 Uiso 0.40 1 calc PR C 2 H61F H 1.0950 0.7203 1.1235 0.089 Uiso 0.40 1 calc PR C 2 C62' C 0.9228(17) 0.6777(8) 1.0626(6) 0.068(4) Uani 0.40 1 d PD C 2 H62C H 0.9557 0.6284 1.0396 0.081 Uiso 0.40 1 calc PR C 2 H62D H 0.8412 0.6567 1.0686 0.081 Uiso 0.40 1 calc PR C 2 C63 C 0.8311(5) 0.8112(3) 1.0482(3) 0.0686(15) Uani 1 1 d D C . H63A H 0.8842 0.8442 1.0889 0.082 Uiso 1 1 calc R . . H63B H 0.7600 0.7806 1.0589 0.082 Uiso 1 1 calc R . . C64 C 0.7839(6) 0.8719(4) 0.9995(3) 0.0790(18) Uani 1 1 d D . . H64A H 0.7344 0.9151 1.0171 0.119 Uiso 1 1 calc R C . H64B H 0.7312 0.8388 0.9595 0.119 Uiso 1 1 calc R . . H64C H 0.8549 0.9022 0.9894 0.119 Uiso 1 1 calc R . . C130 C 0.9261(3) 0.9467(2) 0.78049(19) 0.0310(8) Uani 1 1 d . . . C131 C 0.9936(4) 0.9166(3) 0.8463(2) 0.0545(12) Uani 1 1 d . . . H13A H 1.0843 0.9196 0.8511 0.082 Uiso 1 1 calc R . . H13B H 0.9646 0.8560 0.8479 0.082 Uiso 1 1 calc R . . H13C H 0.9751 0.9548 0.8820 0.082 Uiso 1 1 calc R . . C132 C 0.9766(4) 1.0408(3) 0.7795(3) 0.0487(11) Uani 1 1 d . . . H13D H 1.0674 1.0418 0.7849 0.073 Uiso 1 1 calc R . . H13E H 0.9588 1.0792 0.8153 0.073 Uiso 1 1 calc R . . H13F H 0.9358 1.0616 0.7377 0.073 Uiso 1 1 calc R . . C133 C 0.9573(4) 0.8894(3) 0.7242(2) 0.0436(10) Uani 1 1 d . . . H13G H 1.0483 0.8926 0.7300 0.065 Uiso 1 1 calc R . . H13H H 0.9160 0.9104 0.6826 0.065 Uiso 1 1 calc R . . H13I H 0.9277 0.8285 0.7240 0.065 Uiso 1 1 calc R . . C160 C 0.3219(4) 1.1757(3) 0.7172(2) 0.0358(9) Uani 1 1 d . . . C161 C 0.2139(4) 1.1605(3) 0.6557(2) 0.0547(12) Uani 1 1 d . . . H16A H 0.1579 1.1115 0.6592 0.082 Uiso 1 1 calc R . . H16B H 0.2471 1.1465 0.6176 0.082 Uiso 1 1 calc R . . H16C H 0.1673 1.2136 0.6506 0.082 Uiso 1 1 calc R . . C162 C 0.4072(4) 1.2526(3) 0.7102(3) 0.0523(12) Uani 1 1 d . . . H16D H 0.4416 1.2376 0.6727 0.079 Uiso 1 1 calc R . . H16E H 0.4759 1.2649 0.7500 0.079 Uiso 1 1 calc R . . H16F H 0.3586 1.3046 0.7033 0.079 Uiso 1 1 calc R . . C163 C 0.2699(4) 1.2013(3) 0.7765(2) 0.0467(11) Uani 1 1 d . . . H16G H 0.2144 1.1529 0.7817 0.070 Uiso 1 1 calc R . . H16H H 0.2226 1.2538 0.7696 0.070 Uiso 1 1 calc R . . H16I H 0.3395 1.2133 0.8160 0.070 Uiso 1 1 calc R . . C230 C 0.6733(3) 0.5063(2) 0.90785(18) 0.0293(8) Uani 1 1 d . C . C231 C 0.5935(4) 0.4406(3) 0.8519(2) 0.0449(10) Uani 1 1 d . . . H23A H 0.5065 0.4379 0.8549 0.067 Uiso 1 1 calc R C . H23B H 0.6267 0.3824 0.8554 0.067 Uiso 1 1 calc R . . H23C H 0.5966 0.4597 0.8098 0.067 Uiso 1 1 calc R . . C232 C 0.6734(4) 0.4699(3) 0.9722(2) 0.0380(9) Uani 1 1 d . . . H23D H 0.7239 0.5101 1.0090 0.057 Uiso 1 1 calc R C . H23E H 0.7092 0.4124 0.9726 0.057 Uiso 1 1 calc R . . H23F H 0.5872 0.4638 0.9761 0.057 Uiso 1 1 calc R . . C233 C 0.8094(4) 0.5103(3) 0.9031(2) 0.0410(10) Uani 1 1 d . . . H23G H 0.8603 0.5522 0.9387 0.061 Uiso 1 1 calc R C . H23H H 0.8125 0.5292 0.8610 0.061 Uiso 1 1 calc R . . H23I H 0.8423 0.4521 0.9067 0.061 Uiso 1 1 calc R . . C260 C 0.3352(3) 0.8650(2) 1.04964(17) 0.0277(7) Uani 1 1 d . . . C261 C 0.1959(3) 0.8794(3) 1.02081(19) 0.0365(9) Uani 1 1 d . . . H26A H 0.1877 0.9177 0.9861 0.055 Uiso 1 1 calc R . . H26B H 0.1609 0.9069 1.0553 0.055 Uiso 1 1 calc R . . H26C H 0.1502 0.8228 1.0027 0.055 Uiso 1 1 calc R . . C262 C 0.4063(4) 0.9534(2) 1.08023(19) 0.0379(9) Uani 1 1 d . . . H26D H 0.4019 0.9923 1.0462 0.057 Uiso 1 1 calc R . . H26E H 0.4942 0.9437 1.1004 0.057 Uiso 1 1 calc R . . H26F H 0.3681 0.9804 1.1136 0.057 Uiso 1 1 calc R . . C263 C 0.3423(4) 0.8051(3) 1.10337(18) 0.0358(9) Uani 1 1 d . . . H26G H 0.2972 0.7487 1.0843 0.054 Uiso 1 1 calc R . . H26H H 0.3042 0.8326 1.1366 0.054 Uiso 1 1 calc R . . H26I H 0.4303 0.7957 1.1236 0.054 Uiso 1 1 calc R . . C310 C 1.1402(3) 0.6077(3) 0.81577(18) 0.0337(8) Uani 1 1 d . C . C311 C 1.1815(4) 0.6705(3) 0.7724(2) 0.0489(11) Uani 1 1 d . . . H31A H 1.1783 0.6386 0.7296 0.073 Uiso 1 1 calc R . . H31B H 1.2674 0.6943 0.7933 0.073 Uiso 1 1 calc R . . H31C H 1.1252 0.7187 0.7666 0.073 Uiso 1 1 calc R . . C312 C 1.2311(4) 0.5347(3) 0.8261(3) 0.0578(13) Uani 1 1 d . . . H31D H 1.2052 0.4940 0.8534 0.087 Uiso 1 1 calc R . . H31E H 1.3158 0.5602 0.8478 0.087 Uiso 1 1 calc R . . H31F H 1.2307 0.5030 0.7837 0.087 Uiso 1 1 calc R . . C313 C 1.1450(4) 0.6574(3) 0.8822(2) 0.0452(10) Uani 1 1 d . . . H31G H 1.1189 0.6174 0.9099 0.068 Uiso 1 1 calc R C . H31H H 1.0883 0.7054 0.8763 0.068 Uiso 1 1 calc R . . H31I H 1.2308 0.6815 0.9031 0.068 Uiso 1 1 calc R . . C330 C 0.8400(4) 0.3638(3) 0.6735(2) 0.0484(11) Uani 1 1 d . . . C331 C 0.7938(6) 0.3676(4) 0.5987(3) 0.0817(19) Uani 1 1 d . . . H33A H 0.7173 0.3996 0.5891 0.123 Uiso 1 1 calc R . . H33B H 0.7761 0.3078 0.5761 0.123 Uiso 1 1 calc R . . H33C H 0.8589 0.3977 0.5837 0.123 Uiso 1 1 calc R . . C332 C 0.7395(6) 0.3191(3) 0.6968(4) 0.088(2) Uani 1 1 d . . . H33D H 0.7690 0.3163 0.7440 0.132 Uiso 1 1 calc R . . H33E H 0.7198 0.2596 0.6740 0.132 Uiso 1 1 calc R . . H33F H 0.6641 0.3524 0.6877 0.132 Uiso 1 1 calc R . . C333 C 0.9585(5) 0.3134(3) 0.6858(3) 0.0657(15) Uani 1 1 d . . . H33G H 0.9892 0.3088 0.7327 0.099 Uiso 1 1 calc R . . H33H H 1.0228 0.3445 0.6709 0.099 Uiso 1 1 calc R . . H33I H 0.9397 0.2545 0.6619 0.099 Uiso 1 1 calc R . . C410 C 0.5276(4) 0.8248(3) 0.54293(18) 0.0392(9) Uani 1 1 d . . . C411 C 0.4016(5) 0.7909(5) 0.5517(3) 0.088(2) Uani 1 1 d . . . H41A H 0.3352 0.8269 0.5304 0.131 Uiso 1 1 calc R . . H41B H 0.4060 0.7942 0.5985 0.131 Uiso 1 1 calc R . . H41C H 0.3831 0.7298 0.5319 0.131 Uiso 1 1 calc R . . C412 C 0.5581(6) 0.9168(3) 0.5779(3) 0.0795(19) Uani 1 1 d . . . H41D H 0.6384 0.9396 0.5727 0.119 Uiso 1 1 calc R . . H41E H 0.5637 0.9157 0.6245 0.119 Uiso 1 1 calc R . . H41F H 0.4918 0.9546 0.5592 0.119 Uiso 1 1 calc R . . C413 C 0.5174(5) 0.8261(4) 0.4706(2) 0.0615(14) Uani 1 1 d . . . H41G H 0.5976 0.8482 0.4649 0.092 Uiso 1 1 calc R . . H41H H 0.4515 0.8643 0.4522 0.092 Uiso 1 1 calc R . . H41I H 0.4965 0.7665 0.4480 0.092 Uiso 1 1 calc R . . C430 C 0.9511(4) 0.6940(3) 0.5558(2) 0.0453(10) Uani 1 1 d . . . C431 C 0.9873(5) 0.5994(3) 0.5595(3) 0.0661(15) Uani 1 1 d . . . H43A H 1.0605 0.5906 0.5422 0.099 Uiso 1 1 calc R . . H43B H 0.9170 0.5596 0.5336 0.099 Uiso 1 1 calc R . . H43C H 1.0076 0.5871 0.6052 0.099 Uiso 1 1 calc R . . C432 C 1.0577(4) 0.7558(4) 0.5991(2) 0.0582(13) Uani 1 1 d . . . H43D H 1.0346 0.8166 0.5964 0.087 Uiso 1 1 calc R . . H43E H 1.1339 0.7476 0.5843 0.087 Uiso 1 1 calc R . . H43F H 1.0729 0.7429 0.6445 0.087 Uiso 1 1 calc R . . C433 C 0.9285(5) 0.7160(4) 0.4855(2) 0.0659(15) Uani 1 1 d . . . H43G H 0.9068 0.7772 0.4836 0.099 Uiso 1 1 calc R . . H43H H 0.8596 0.6773 0.4570 0.099 Uiso 1 1 calc R . . H43I H 1.0048 0.7076 0.4707 0.099 Uiso 1 1 calc R . . C1S C 0.8602(15) 0.0747(11) 0.5729(7) 0.125(5) Uiso 0.60 1 d PD . . C2S C 0.8757(12) 0.0404(11) 0.5073(7) 0.135(5) Uiso 0.60 1 d PD . . O1S O 1.0012(11) 0.0214(7) 0.5117(5) 0.121(3) Uiso 0.60 1 d PD . . C3S C 1.0368(16) 0.0038(12) 0.4525(7) 0.151(6) Uiso 0.60 1 d PD . . C4S C 1.1605(18) -0.0274(16) 0.4495(13) 0.199(10) Uiso 0.60 1 d PD . . 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 K 0.0361(4) 0.0406(5) 0.0267(4) 0.0046(3) 0.0050(3) -0.0005(4) S1 0.0235(4) 0.0256(4) 0.0224(4) 0.0048(3) 0.0076(3) 0.0006(3) Pr 0.02144(10) 0.03106(11) 0.02161(10) 0.00357(7) 0.00729(7) 0.00373(7) O1 0.0243(12) 0.0269(13) 0.0285(13) 0.0049(10) 0.0080(10) 0.0027(10) O2 0.0343(14) 0.0286(13) 0.0325(14) 0.0080(11) 0.0182(11) 0.0093(11) O3 0.0215(12) 0.0346(14) 0.0250(12) 0.0014(10) 0.0037(10) 0.0012(10) O4 0.0249(13) 0.0377(15) 0.0387(15) -0.0052(12) 0.0054(11) 0.0056(11) O5 0.0324(14) 0.0473(16) 0.0286(14) 0.0146(12) 0.0109(11) 0.0093(12) O6 0.0332(14) 0.0549(18) 0.0310(14) 0.0145(13) 0.0139(12) 0.0126(13) O7 0.0285(14) 0.0500(17) 0.0449(17) -0.0013(13) 0.0067(12) -0.0038(12) O8 0.0542(19) 0.0538(19) 0.0391(17) 0.0008(14) 0.0072(14) 0.0133(15) C11 0.0274(17) 0.0233(17) 0.0173(16) 0.0032(13) 0.0057(13) -0.0031(13) C12 0.0259(17) 0.0256(18) 0.0163(15) 0.0017(13) 0.0048(13) 0.0004(14) C13 0.0245(17) 0.0329(19) 0.0207(17) 0.0016(14) 0.0072(14) -0.0008(14) C14 0.0286(18) 0.0224(17) 0.0236(17) 0.0004(13) 0.0078(14) -0.0016(14) C15 0.0341(19) 0.0251(18) 0.0254(18) 0.0056(14) 0.0116(15) 0.0009(15) C16 0.0337(19) 0.032(2) 0.0239(18) 0.0091(15) 0.0119(15) 0.0076(15) C17 0.0263(18) 0.037(2) 0.0306(19) 0.0083(16) 0.0073(15) 0.0059(15) C18 0.0287(18) 0.0292(19) 0.0266(18) 0.0032(14) 0.0103(15) -0.0002(15) C19 0.0246(17) 0.0298(18) 0.0147(15) 0.0015(13) 0.0080(13) 0.0017(14) C20 0.0285(18) 0.0265(18) 0.0185(16) 0.0026(13) 0.0093(14) 0.0014(14) C21 0.0223(16) 0.0269(18) 0.0226(17) 0.0061(13) 0.0095(13) -0.0018(13) C22 0.0216(16) 0.0266(18) 0.0251(17) 0.0042(14) 0.0073(14) 0.0000(13) C23 0.0242(17) 0.0254(18) 0.0295(18) 0.0057(14) 0.0084(14) 0.0007(14) C24 0.0254(18) 0.0309(19) 0.0252(18) 0.0093(15) 0.0076(14) 0.0002(14) C25 0.0286(18) 0.0289(19) 0.0214(17) 0.0038(14) 0.0097(14) -0.0034(14) C26 0.0245(17) 0.0277(18) 0.0207(16) 0.0008(14) 0.0073(13) -0.0027(14) C27 0.0276(18) 0.0237(18) 0.0279(18) 0.0036(14) 0.0091(14) 0.0023(14) C28 0.0284(18) 0.0235(17) 0.0221(17) 0.0027(13) 0.0048(14) 0.0006(14) C29 0.0192(16) 0.0279(18) 0.0238(17) 0.0040(14) 0.0058(13) -0.0036(13) C30 0.0233(17) 0.0245(17) 0.0239(17) 0.0027(14) 0.0063(14) -0.0004(13) C31 0.0250(18) 0.038(2) 0.0227(17) 0.0060(15) 0.0057(14) 0.0009(15) C32 0.0214(18) 0.037(2) 0.040(2) 0.0037(17) 0.0054(16) 0.0073(15) C33 0.0292(19) 0.037(2) 0.032(2) -0.0002(16) 0.0097(16) 0.0015(16) C41 0.035(2) 0.033(2) 0.0235(18) 0.0015(15) 0.0040(15) 0.0000(16) C42 0.039(2) 0.051(2) 0.0233(19) 0.0078(17) 0.0110(16) 0.0056(18) C43 0.035(2) 0.045(2) 0.030(2) 0.0020(17) 0.0136(17) 0.0017(17) C61 0.069(7) 0.080(7) 0.074(7) 0.026(6) 0.021(6) 0.016(6) C62 0.045(5) 0.084(8) 0.047(5) 0.013(5) 0.010(4) 0.015(5) C61' 0.075(9) 0.070(9) 0.037(7) 0.019(6) 0.015(6) 0.012(7) C62' 0.089(13) 0.057(10) 0.046(8) 0.008(7) -0.004(9) 0.018(9) C63 0.073(4) 0.059(3) 0.062(3) -0.009(3) -0.001(3) 0.021(3) C64 0.081(4) 0.054(3) 0.086(4) 0.001(3) -0.005(3) 0.010(3) C130 0.0213(17) 0.032(2) 0.040(2) 0.0047(16) 0.0084(16) -0.0021(14) C131 0.028(2) 0.072(3) 0.056(3) 0.012(2) -0.004(2) -0.003(2) C132 0.028(2) 0.040(2) 0.078(3) -0.001(2) 0.018(2) -0.0061(18) C133 0.032(2) 0.046(2) 0.059(3) 0.000(2) 0.026(2) -0.0008(18) C160 0.037(2) 0.032(2) 0.043(2) 0.0141(17) 0.0144(18) 0.0090(17) C161 0.050(3) 0.056(3) 0.056(3) 0.021(2) 0.003(2) 0.020(2) C162 0.051(3) 0.037(2) 0.080(3) 0.026(2) 0.030(3) 0.014(2) C163 0.048(3) 0.042(2) 0.059(3) 0.011(2) 0.025(2) 0.016(2) C230 0.034(2) 0.0246(18) 0.034(2) 0.0072(15) 0.0153(16) 0.0052(15) C231 0.060(3) 0.027(2) 0.047(3) 0.0077(18) 0.010(2) 0.0067(19) C232 0.049(2) 0.030(2) 0.042(2) 0.0130(17) 0.0198(19) 0.0122(18) C233 0.038(2) 0.044(2) 0.051(3) 0.021(2) 0.0217(19) 0.0181(18) C260 0.0339(19) 0.0287(19) 0.0223(17) 0.0007(14) 0.0111(15) 0.0025(15) C261 0.035(2) 0.044(2) 0.033(2) 0.0021(17) 0.0146(17) 0.0054(17) C262 0.054(3) 0.030(2) 0.029(2) -0.0019(16) 0.0121(18) -0.0023(18) C263 0.047(2) 0.036(2) 0.029(2) 0.0009(16) 0.0177(17) 0.0051(18) C310 0.0237(18) 0.042(2) 0.033(2) 0.0013(17) 0.0029(15) 0.0029(16) C311 0.033(2) 0.069(3) 0.043(2) 0.008(2) 0.0084(19) -0.011(2) C312 0.029(2) 0.066(3) 0.066(3) 0.000(3) -0.007(2) 0.009(2) C313 0.029(2) 0.064(3) 0.034(2) -0.004(2) -0.0027(17) -0.0028(19) C330 0.033(2) 0.036(2) 0.068(3) -0.012(2) 0.006(2) 0.0066(18) C331 0.087(4) 0.076(4) 0.060(3) -0.030(3) -0.008(3) 0.025(3) C332 0.080(4) 0.036(3) 0.158(7) -0.015(3) 0.062(4) -0.014(3) C333 0.051(3) 0.047(3) 0.088(4) -0.019(3) 0.006(3) 0.015(2) C410 0.045(2) 0.047(2) 0.0262(19) 0.0085(17) 0.0067(17) 0.0146(19) C411 0.036(3) 0.134(6) 0.101(5) 0.066(4) 0.009(3) 0.022(3) C412 0.128(5) 0.047(3) 0.051(3) 0.002(2) -0.001(3) 0.030(3) C413 0.072(3) 0.085(4) 0.028(2) 0.013(2) 0.008(2) 0.034(3) C430 0.045(2) 0.065(3) 0.032(2) 0.007(2) 0.0202(19) 0.009(2) C431 0.065(3) 0.073(4) 0.075(4) 0.004(3) 0.044(3) 0.019(3) C432 0.040(3) 0.089(4) 0.052(3) 0.007(3) 0.024(2) 0.006(2) C433 0.061(3) 0.108(4) 0.039(3) 0.012(3) 0.030(2) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K O1 2.590(2) . y K O8 2.737(3) . y K O3 2.739(2) . y K O2 2.917(3) . y K C22 2.925(3) . y K C233 3.276(4) . y K C313 3.340(4) . y K C23 3.342(3) . y K C21 3.420(3) . y K C64 3.452(6) . y K Pr 3.7296(10) . y S1 C11 1.783(3) . y S1 C21 1.797(3) . y S1 Pr 3.1693(9) . y Pr O2 2.331(2) . y Pr O5 2.379(2) . y Pr O1 2.388(2) . y Pr O6 2.398(2) . y Pr O4 2.404(3) . y Pr O3 2.470(2) . y Pr O7 2.567(3) . ? O1 C12 1.314(4) . y O2 C22 1.315(4) . y O3 C31 1.276(4) . y O4 C33 1.261(4) . y O5 C41 1.264(4) . ? O6 C43 1.273(4) . ? O7 C54 1.410(5) . ? O7 C51' 1.439(8) . ? O7 C51 1.442(7) . ? O8 C63 1.416(5) . ? O8 C62 1.450(8) . ? O8 C62' 1.469(9) . ? C11 C12 1.395(5) . ? C11 C19 1.433(5) . ? C12 C13 1.454(5) . ? C13 C14 1.366(5) . ? C13 C130 1.541(5) . ? C14 C20 1.416(5) . ? C15 C16 1.377(5) . ? C15 C20 1.415(5) . ? C16 C17 1.419(5) . ? C16 C160 1.524(5) . ? C17 C18 1.365(5) . ? C18 C19 1.416(5) . ? C19 C20 1.414(5) . ? C21 C22 1.397(5) . ? C21 C29 1.425(4) . ? C22 C23 1.457(5) . ? C23 C24 1.371(5) . ? C23 C230 1.537(5) . ? C24 C30 1.410(5) . ? C25 C26 1.374(5) . ? C25 C30 1.420(4) . ? C26 C27 1.415(5) . ? C26 C260 1.536(4) . ? C27 C28 1.365(4) . ? C28 C29 1.418(5) . ? C29 C30 1.422(5) . ? C31 C32 1.388(5) . ? C31 C310 1.542(5) . ? C32 C33 1.399(5) . ? C33 C330 1.540(5) . ? C41 C42 1.398(5) . ? C41 C410 1.539(5) . ? C42 C43 1.393(5) . ? C43 C430 1.546(5) . ? C51 C52 1.509(7) . ? C51' C52 1.506(8) . ? C52 C53' 1.514(8) . ? C52 C53 1.522(7) . ? C53 C54 1.521(7) . ? C53' C54 1.526(8) . ? C61 C62 1.503(10) . ? C61' C62' 1.506(11) . ? C63 C64 1.474(7) . ? C130 C133 1.532(5) . ? C130 C132 1.535(5) . ? C130 C131 1.536(6) . ? C160 C161 1.521(6) . ? C160 C162 1.530(6) . ? C160 C163 1.538(6) . ? C230 C232 1.532(5) . ? C230 C233 1.534(5) . ? C230 C231 1.539(6) . ? C260 C263 1.529(5) . ? C260 C261 1.538(5) . ? C260 C262 1.538(5) . ? C310 C313 1.525(5) . ? C310 C312 1.525(6) . ? C310 C311 1.537(6) . ? C330 C332 1.501(7) . ? C330 C333 1.522(6) . ? C330 C331 1.551(7) . ? C410 C412 1.512(6) . ? C410 C413 1.518(5) . ? C410 C411 1.534(7) . ? C430 C431 1.524(7) . ? C430 C432 1.526(7) . ? C430 C433 1.529(6) . ? C1S C2S 1.496(8) . ? C2S O1S 1.408(8) . ? O1S C3S 1.419(8) . ? C3S C4S 1.479(8) . ? 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 K O8 142.46(9) . . y O1 K O3 66.50(7) . . ? O8 K O3 148.90(8) . . ? O1 K O2 69.48(7) . . y O8 K O2 126.12(9) . . ? O3 K O2 65.88(7) . . y O1 K C22 78.90(9) . . y O8 K C22 103.54(10) . . ? O3 K C22 91.89(9) . . ? O2 K C22 26.01(8) . . ? O1 K C233 123.78(10) . . ? O8 K C233 87.42(10) . . ? O3 K C233 76.56(9) . . ? O2 K C233 57.04(9) . . ? C22 K C233 61.06(10) . . ? O1 K C313 104.26(9) . . ? O8 K C313 98.93(10) . . ? O3 K C313 53.48(8) . . ? O2 K C313 113.83(9) . . ? C22 K C313 136.77(10) . . ? C233 K C313 83.89(10) . . ? O1 K C23 104.62(8) . . ? O8 K C23 81.90(9) . . ? O3 K C23 103.94(8) . . ? O2 K C23 44.23(8) . . ? C22 K C23 25.80(9) . . ? C233 K C23 45.38(9) . . ? C313 K C23 129.27(10) . . ? O1 K C21 66.21(7) . . ? O8 K C21 101.00(9) . . ? O3 K C21 103.66(8) . . ? O2 K C21 42.98(7) . . ? C22 K C21 23.84(9) . . ? C233 K C21 84.28(9) . . ? C313 K C21 156.28(9) . . ? C23 K C21 42.71(8) . . ? O1 K C64 100.36(11) . . ? O8 K C64 42.55(11) . . ? O3 K C64 165.17(12) . . ? O2 K C64 117.33(12) . . ? C22 K C64 92.19(13) . . ? C233 K C64 117.76(13) . . ? C313 K C64 128.21(12) . . ? C23 K C64 85.61(12) . . ? C21 K C64 75.51(12) . . ? O1 K Pr 39.45(5) . . ? O8 K Pr 163.85(7) . . ? O3 K Pr 41.47(5) . . ? O2 K Pr 38.67(5) . . ? C22 K Pr 60.33(7) . . ? C233 K Pr 85.07(8) . . ? C313 K Pr 94.46(7) . . ? C23 K Pr 82.66(6) . . ? C21 K Pr 64.06(6) . . ? C64 K Pr 131.30(9) . . ? C11 S1 C21 108.85(15) . . ? C11 S1 Pr 91.97(11) . . ? C21 S1 Pr 95.91(11) . . ? O2 Pr O5 132.15(8) . . y O2 Pr O1 83.76(8) . . y O5 Pr O1 86.89(9) . . y O2 Pr O6 158.51(8) . . y O5 Pr O6 69.34(8) . . y O1 Pr O6 99.19(9) . . y O2 Pr O4 83.32(9) . . ? O5 Pr O4 126.04(9) . . ? O1 Pr O4 143.76(8) . . y O6 Pr O4 81.91(9) . . ? O2 Pr O3 79.74(8) . . y O5 Pr O3 141.28(8) . . ? O1 Pr O3 74.02(8) . . ? O6 Pr O3 80.65(8) . . ? O4 Pr O3 70.42(8) . . y O2 Pr O7 81.43(9) . . y O5 Pr O7 74.23(9) . . ? O1 Pr O7 137.07(8) . . y O6 Pr O7 109.04(9) . . ? O4 Pr O7 73.60(9) . . ? O3 Pr O7 140.91(9) . . ? O2 Pr S1 62.24(6) . . ? O5 Pr S1 71.95(6) . . ? O1 Pr S1 62.07(6) . . y O6 Pr S1 137.71(6) . . ? O4 Pr S1 136.38(6) . . ? O3 Pr S1 123.25(6) . . ? O7 Pr S1 75.40(6) . . ? O2 Pr K 51.46(7) . . ? O5 Pr K 129.75(7) . . ? O1 Pr K 43.58(6) . . ? O6 Pr K 117.85(7) . . ? O4 Pr K 103.87(6) . . ? O3 Pr K 47.25(6) . . ? O7 Pr K 132.30(6) . . ? S1 Pr K 76.01(2) . . ? C12 O1 Pr 123.5(2) . . ? C12 O1 K 128.0(2) . . ? Pr O1 K 96.97(8) . . ? C22 O2 Pr 137.3(2) . . ? C22 O2 K 77.30(18) . . ? Pr O2 K 89.87(8) . . ? C31 O3 Pr 133.1(2) . . ? C31 O3 K 130.6(2) . . ? Pr O3 K 91.29(7) . . ? C33 O4 Pr 137.5(2) . . ? C41 O5 Pr 139.8(2) . . ? C43 O6 Pr 139.0(2) . . ? C54 O7 C51' 111.4(5) . . ? C54 O7 C51 108.7(5) . . ? C54 O7 Pr 121.2(3) . . ? C51' O7 Pr 127.1(4) . . ? C51 O7 Pr 124.2(3) . . ? C63 O8 C62 115.0(5) . . ? C63 O8 C62' 107.9(8) . . ? C63 O8 K 119.6(3) . . ? C62 O8 K 125.4(5) . . ? C62' O8 K 121.0(6) . . ? C12 C11 C19 122.4(3) . . ? C12 C11 S1 117.9(3) . . ? C19 C11 S1 118.9(2) . . ? O1 C12 C11 121.0(3) . . ? O1 C12 C13 120.4(3) . . ? C11 C12 C13 118.6(3) . . ? C14 C13 C12 118.2(3) . . ? C14 C13 C130 121.2(3) . . ? C12 C13 C130 120.5(3) . . ? C13 C14 C20 123.7(3) . . ? C16 C15 C20 122.4(3) . . ? C15 C16 C17 116.4(3) . . ? C15 C16 C160 123.1(3) . . ? C17 C16 C160 120.5(3) . . ? C18 C17 C16 122.6(3) . . ? C17 C18 C19 121.5(3) . . ? C20 C19 C18 116.7(3) . . ? C20 C19 C11 117.8(3) . . ? C18 C19 C11 125.5(3) . . ? C19 C20 C15 120.4(3) . . ? C19 C20 C14 119.0(3) . . ? C15 C20 C14 120.6(3) . . ? C22 C21 C29 121.8(3) . . ? C22 C21 S1 115.9(2) . . ? C29 C21 S1 121.5(2) . . ? C22 C21 K 57.78(18) . . ? C29 C21 K 111.5(2) . . ? S1 C21 K 105.64(13) . . ? O2 C22 C21 121.6(3) . . ? O2 C22 C23 119.0(3) . . ? C21 C22 C23 119.3(3) . . ? O2 C22 K 76.68(18) . . ? C21 C22 K 98.4(2) . . ? C23 C22 K 93.3(2) . . ? C24 C23 C22 117.7(3) . . ? C24 C23 C230 122.5(3) . . ? C22 C23 C230 119.8(3) . . ? C24 C23 K 109.4(2) . . ? C22 C23 K 60.87(17) . . ? C230 C23 K 99.6(2) . . ? C23 C24 C30 123.8(3) . . ? C26 C25 C30 122.2(3) . . ? C25 C26 C27 117.1(3) . . ? C25 C26 C260 123.3(3) . . ? C27 C26 C260 119.6(3) . . ? C28 C27 C26 122.5(3) . . ? C27 C28 C29 121.2(3) . . ? C28 C29 C30 117.2(3) . . ? C28 C29 C21 124.7(3) . . ? C30 C29 C21 118.1(3) . . ? C24 C30 C25 121.1(3) . . ? C24 C30 C29 119.1(3) . . ? C25 C30 C29 119.7(3) . . ? O3 C31 C32 124.5(3) . . ? O3 C31 C310 115.0(3) . . ? C32 C31 C310 120.4(3) . . ? C31 C32 C33 125.8(3) . . ? O4 C33 C32 124.3(4) . . ? O4 C33 C330 114.7(3) . . ? C32 C33 C330 121.0(3) . . ? O5 C41 C42 123.9(3) . . ? O5 C41 C410 114.7(3) . . ? C42 C41 C410 121.3(3) . . ? C43 C42 C41 123.8(3) . . ? O6 C43 C42 123.7(3) . . ? O6 C43 C430 115.2(3) . . ? C42 C43 C430 121.1(3) . . ? O7 C51 C52 104.7(5) . . ? O7 C51' C52 105.1(6) . . ? C51' C52 C53' 106.2(7) . . ? C51 C52 C53' 94.9(9) . . ? C51' C52 C53 100.7(6) . . ? C51 C52 C53 106.2(6) . . ? C54 C53 C52 104.0(5) . . ? C52 C53' C54 104.1(7) . . ? O7 C54 C53 104.9(5) . . ? O7 C54 C53' 103.3(7) . . ? O8 C62 C61 109.2(7) . . ? O8 C62' C61' 113.7(9) . . ? O8 C63 C64 108.2(5) . . ? C63 C64 K 85.7(3) . . ? C133 C130 C132 107.4(3) . . ? C133 C130 C131 110.2(3) . . ? C132 C130 C131 107.7(3) . . ? C133 C130 C13 109.9(3) . . ? C132 C130 C13 111.2(3) . . ? C131 C130 C13 110.3(3) . . ? C161 C160 C16 109.8(3) . . ? C161 C160 C162 108.1(4) . . ? C16 C160 C162 112.1(3) . . ? C161 C160 C163 109.3(3) . . ? C16 C160 C163 109.3(3) . . ? C162 C160 C163 108.1(4) . . ? C232 C230 C233 106.9(3) . . ? C232 C230 C23 111.9(3) . . ? C233 C230 C23 112.5(3) . . ? C232 C230 C231 107.3(3) . . ? C233 C230 C231 109.3(3) . . ? C23 C230 C231 108.7(3) . . ? C230 C233 K 102.4(2) . . ? C263 C260 C26 112.3(3) . . ? C263 C260 C261 107.2(3) . . ? C26 C260 C261 109.9(3) . . ? C263 C260 C262 108.9(3) . . ? C26 C260 C262 108.9(3) . . ? C261 C260 C262 109.6(3) . . ? C313 C310 C312 108.5(3) . . ? C313 C310 C311 109.4(4) . . ? C312 C310 C311 108.8(4) . . ? C313 C310 C31 110.0(3) . . ? C312 C310 C31 114.3(3) . . ? C311 C310 C31 105.8(3) . . ? C310 C313 K 110.8(2) . . ? C332 C330 C333 111.2(4) . . ? C332 C330 C33 107.5(4) . . ? C333 C330 C33 114.1(4) . . ? C332 C330 C331 109.5(5) . . ? C333 C330 C331 107.5(4) . . ? C33 C330 C331 107.0(4) . . ? C412 C410 C413 109.7(4) . . ? C412 C410 C411 108.3(5) . . ? C413 C410 C411 109.3(4) . . ? C412 C410 C41 107.0(4) . . ? C413 C410 C41 113.5(3) . . ? C411 C410 C41 108.9(3) . . ? C431 C430 C432 109.6(4) . . ? C431 C430 C433 110.0(4) . . ? C432 C430 C433 108.4(4) . . ? C431 C430 C43 108.0(4) . . ? C432 C430 C43 107.5(3) . . ? C433 C430 C43 113.3(4) . . ? _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.00 _refine_diff_density_min -0.74 _refine_diff_density_rms 0.10 #===END of CIF data_prthon_compound_1b _database_code_depnum_ccdc_archive 'CCDC 298870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C66 H102 K O8 Pr S), 0.5 (C4 H10 O)' _chemical_formula_sum 'C68 H107 K1 O8.5 Pr1 S1' _chemical_formula_weight 1278.6 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M ' P 21 21 21' _refine_special_details ; Many atoms showing NPD's due to poor data set, all carbon atoms therefore refined isotropically. DFIX and SADI restraints applied to the coordinated diethyl ether molecules. ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8595(13) _cell_length_b 14.3555(18) _cell_length_c 51.762(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8069.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12880 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 26.7 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.30 (2002)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41456 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.98 _reflns_number_total 15569 _reflns_number_gt 14690 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0806P)^2^+106.8569P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0095(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(3) _refine_ls_number_reflns 15569 _refine_ls_number_parameters 386 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.1271 _refine_ls_R_factor_gt 0.1218 _refine_ls_wR_factor_ref 0.2966 _refine_ls_wR_factor_gt 0.2935 _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_restrained_S_all 1.285 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.27123(6) 0.01687(5) 0.851272(13) 0.0291(2) Uani 1 1 d U . . K1 K 0.2297(3) 0.2672(2) 0.82700(6) 0.0401(7) Uani 1 1 d U . . S1 S 0.5106(3) 0.1360(2) 0.86748(6) 0.0244(6) Uani 1 1 d U . . O1 O 0.2443(6) 0.1684(6) 0.86922(16) 0.0298(16) Uani 1 1 d U . . O2 O 0.3829(8) 0.0909(7) 0.81879(18) 0.0322(17) Uani 1 1 d U . . O3 O 0.2049(7) -0.0820(6) 0.81569(19) 0.0353(19) Uani 1 1 d U . . O4 O 0.1042(8) 0.0971(7) 0.82669(19) 0.0345(19) Uani 1 1 d U . . O5 O 0.3192(8) -0.0275(8) 0.89450(18) 0.041(2) Uani 1 1 d U . . O6 O 0.0950(9) -0.0554(8) 0.8716(2) 0.044(2) Uani 1 1 d U . . O7 O 0.4505(9) -0.1069(7) 0.8452(2) 0.044(2) Uani 1 1 d DU . . O8 O 0.3090(10) 0.4507(7) 0.8210(2) 0.052(3) Uani 1 1 d DU . . O9 O 0.4214(19) 0.6014(16) 0.9166(4) 0.045(5) Uiso 0.50 1 d PDU . . C11 C 0.4291(12) 0.2002(9) 0.8914(2) 0.030(3) Uiso 1 1 d U . . C12 C 0.3015(11) 0.2057(9) 0.8892(2) 0.030(3) Uiso 1 1 d U . . C13 C 0.2310(15) 0.2548(10) 0.9087(3) 0.039(3) Uiso 1 1 d U . . C14 C 0.2914(12) 0.2950(9) 0.9290(2) 0.031(3) Uiso 1 1 d U . . H14A H 0.2453 0.3305 0.9411 0.037 Uiso 1 1 calc R . . C15 C 0.4829(14) 0.3197(11) 0.9549(3) 0.041(3) Uiso 1 1 d U . . H15A H 0.4349 0.3525 0.9672 0.049 Uiso 1 1 calc R . . C16 C 0.6095(14) 0.3085(11) 0.9598(3) 0.041(3) Uiso 1 1 d U . . C17 C 0.6732(15) 0.2603(11) 0.9407(3) 0.040(3) Uiso 1 1 d U . . H17A H 0.7594 0.2523 0.9430 0.048 Uiso 1 1 calc R . . C18 C 0.6227(13) 0.2241(10) 0.9192(3) 0.036(3) Uiso 1 1 d U . . H18A H 0.6736 0.1910 0.9074 0.043 Uiso 1 1 calc R . . C19 C 0.4900(12) 0.2346(9) 0.9133(2) 0.028(3) Uiso 1 1 d U . . C20 C 0.4232(11) 0.2855(9) 0.9328(2) 0.026(3) Uiso 1 1 d U . . C21 C 0.5162(10) 0.2033(8) 0.8378(2) 0.017(2) Uiso 1 1 d U . . C22 C 0.4603(11) 0.1647(9) 0.8168(2) 0.024(2) Uiso 1 1 d U . . C23 C 0.4739(13) 0.2081(10) 0.7916(3) 0.036(3) Uiso 1 1 d U . . C24 C 0.5459(13) 0.2885(10) 0.7895(3) 0.036(3) Uiso 1 1 d U . . H24A H 0.5554 0.3172 0.7731 0.043 Uiso 1 1 calc R . . C25 C 0.6808(13) 0.4084(10) 0.8088(3) 0.034(3) Uiso 1 1 d U . . H25A H 0.6879 0.4374 0.7923 0.041 Uiso 1 1 calc R . . C26 C 0.7437(16) 0.4454(11) 0.8291(3) 0.052(4) Uiso 1 1 d U . . C27 C 0.7242(14) 0.4058(9) 0.8536(3) 0.042(3) Uiso 1 1 d U . . H27A H 0.7625 0.4332 0.8682 0.051 Uiso 1 1 calc R . . C28 C 0.6520(12) 0.3292(9) 0.8569(2) 0.031(3) Uiso 1 1 d U . . H28A H 0.6422 0.3046 0.8738 0.038 Uiso 1 1 calc R . . C29 C 0.5903(11) 0.2844(8) 0.8358(2) 0.022(2) Uiso 1 1 d U . . C30 C 0.6046(11) 0.3279(9) 0.8111(2) 0.023(2) Uiso 1 1 d U . . C31 C 0.1139(12) -0.0869(9) 0.8013(2) 0.028(3) Uiso 1 1 d U . . C32 C 0.0197(12) -0.0209(11) 0.7993(2) 0.037(3) Uiso 1 1 d U . . H32A H -0.0485 -0.0363 0.7886 0.044 Uiso 1 1 calc R . . C33 C 0.0172(12) 0.0651(9) 0.8114(2) 0.031(3) Uiso 1 1 d U . . C41 C 0.2722(16) -0.0642(10) 0.9139(3) 0.041(3) Uiso 1 1 d U . . C42 C 0.1466(14) -0.0990(11) 0.9136(3) 0.043(3) Uiso 1 1 d U . . H42A H 0.1155 -0.1272 0.9288 0.051 Uiso 1 1 calc R . . C43 C 0.0724(17) -0.0934(14) 0.8931(4) 0.055(4) Uiso 1 1 d U . . C51 C 0.613(3) -0.119(3) 0.8137(6) 0.125(11) Uiso 1 1 d DU . . H51A H 0.6313 -0.1378 0.7959 0.187 Uiso 1 1 calc R . . H51B H 0.6605 -0.1583 0.8256 0.187 Uiso 1 1 calc R . . H51C H 0.6361 -0.0538 0.8162 0.187 Uiso 1 1 calc R . . C52 C 0.476(3) -0.131(4) 0.8190(4) 0.21(2) Uiso 1 1 d DU . . H52A H 0.4280 -0.0911 0.8072 0.252 Uiso 1 1 calc R . . H52B H 0.4519 -0.1969 0.8158 0.252 Uiso 1 1 calc R . . C53 C 0.459(3) -0.1932(14) 0.8589(6) 0.114(10) Uiso 1 1 d DU . . H53B H 0.5119 -0.1817 0.8741 0.136 Uiso 1 1 calc R . . H53C H 0.5044 -0.2369 0.8476 0.136 Uiso 1 1 calc R . . C54 C 0.345(3) -0.245(3) 0.8686(8) 0.169(17) Uiso 1 1 d DU . . H54A H 0.3701 -0.3038 0.8767 0.254 Uiso 1 1 calc R . . H54B H 0.2899 -0.2582 0.8540 0.254 Uiso 1 1 calc R . . H54C H 0.3017 -0.2065 0.8813 0.254 Uiso 1 1 calc R . . C61 C 0.244(2) 0.4511(15) 0.7768(4) 0.086(6) Uiso 1 1 d DU . . H61A H 0.2579 0.4811 0.7601 0.129 Uiso 1 1 calc R . . H61B H 0.1576 0.4588 0.7819 0.129 Uiso 1 1 calc R . . H61C H 0.2633 0.3846 0.7755 0.129 Uiso 1 1 calc R . . C62 C 0.3239(19) 0.4944(16) 0.7964(3) 0.073(5) Uiso 1 1 d DU . . H62A H 0.4109 0.4892 0.7909 0.087 Uiso 1 1 calc R . . H62B H 0.3035 0.5614 0.7979 0.087 Uiso 1 1 calc R . . C63 C 0.3754(17) 0.4938(14) 0.8415(3) 0.064(5) Uiso 1 1 d DU . . H63A H 0.3514 0.5602 0.8427 0.077 Uiso 1 1 calc R . . H63B H 0.4647 0.4910 0.8378 0.077 Uiso 1 1 calc R . . C64 C 0.350(2) 0.4471(15) 0.8663(4) 0.071(6) Uiso 1 1 d DU . . H64A H 0.3958 0.4783 0.8802 0.107 Uiso 1 1 calc R . . H64B H 0.3757 0.3818 0.8653 0.107 Uiso 1 1 calc R . . H64C H 0.2616 0.4502 0.8700 0.107 Uiso 1 1 calc R . . C71 C 0.198(4) 0.611(4) 0.9154(10) 0.105(17) Uiso 0.50 1 d PDU . . H71A H 0.1290 0.5897 0.9261 0.157 Uiso 0.50 1 calc PR . . H71B H 0.1915 0.5831 0.8982 0.157 Uiso 0.50 1 calc PR . . H71C H 0.1957 0.6789 0.9139 0.157 Uiso 0.50 1 calc PR . . C72 C 0.319(3) 0.581(4) 0.9279(9) 0.092(15) Uiso 0.50 1 d PDU . . H72A H 0.3218 0.6085 0.9454 0.110 Uiso 0.50 1 calc PR . . H72B H 0.3166 0.5126 0.9300 0.110 Uiso 0.50 1 calc PR . . C73 C 0.521(3) 0.564(4) 0.9250(10) 0.102(17) Uiso 0.50 1 d PDU . . H73A H 0.5155 0.4956 0.9234 0.122 Uiso 0.50 1 calc PR . . H73B H 0.5321 0.5797 0.9435 0.122 Uiso 0.50 1 calc PR . . C74 C 0.632(3) 0.599(3) 0.9097(7) 0.065(10) Uiso 0.50 1 d PDU . . H74A H 0.7065 0.5666 0.9155 0.097 Uiso 0.50 1 calc PR . . H74B H 0.6420 0.6662 0.9124 0.097 Uiso 0.50 1 calc PR . . H74C H 0.6192 0.5867 0.8912 0.097 Uiso 0.50 1 calc PR . . C130 C 0.0871(14) 0.2631(11) 0.9077(3) 0.038(3) Uiso 1 1 d U . . C131 C 0.0362(17) 0.1607(13) 0.9128(3) 0.055(4) Uiso 1 1 d U . . H13A H 0.0664 0.1384 0.9296 0.083 Uiso 1 1 calc R . . H13B H 0.0651 0.1190 0.8991 0.083 Uiso 1 1 calc R . . H13C H -0.0540 0.1618 0.9130 0.083 Uiso 1 1 calc R . . C132 C 0.0398(17) 0.2971(13) 0.8815(3) 0.053(4) Uiso 1 1 d U . . H13D H 0.0722 0.3595 0.8780 0.080 Uiso 1 1 calc R . . H13E H -0.0504 0.2993 0.8818 0.080 Uiso 1 1 calc R . . H13F H 0.0672 0.2542 0.8680 0.080 Uiso 1 1 calc R . . C133 C 0.0362(17) 0.3260(13) 0.9279(3) 0.055(4) Uiso 1 1 d U . . H13G H 0.0670 0.3894 0.9251 0.082 Uiso 1 1 calc R . . H13H H 0.0620 0.3042 0.9450 0.082 Uiso 1 1 calc R . . H13I H -0.0539 0.3260 0.9269 0.082 Uiso 1 1 calc R . . C160 C 0.6660(16) 0.3526(12) 0.9835(3) 0.048(4) Uiso 1 1 d U . . C161 C 0.583(3) 0.392(2) 1.0036(5) 0.100(8) Uiso 1 1 d U . . H16A H 0.5359 0.4433 0.9963 0.150 Uiso 1 1 calc R . . H16B H 0.6324 0.4139 1.0182 0.150 Uiso 1 1 calc R . . H16C H 0.5265 0.3429 1.0096 0.150 Uiso 1 1 calc R . . C162 C 0.724(3) 0.274(2) 0.9981(6) 0.128(10) Uiso 1 1 d U . . H16D H 0.7845 0.2431 0.9871 0.191 Uiso 1 1 calc R . . H16E H 0.6598 0.2294 1.0031 0.191 Uiso 1 1 calc R . . H16F H 0.7643 0.2985 1.0136 0.191 Uiso 1 1 calc R . . C163 C 0.764(2) 0.4184(16) 0.9767(4) 0.081(6) Uiso 1 1 d U . . H16G H 0.7294 0.4707 0.9670 0.122 Uiso 1 1 calc R . . H16H H 0.8260 0.3866 0.9660 0.122 Uiso 1 1 calc R . . H16I H 0.8036 0.4417 0.9925 0.122 Uiso 1 1 calc R . . C230 C 0.4199(13) 0.1617(10) 0.7671(3) 0.038(3) Uiso 1 1 d U . . C231 C 0.4498(17) 0.2160(13) 0.7421(3) 0.053(4) Uiso 1 1 d U . . H23A H 0.5393 0.2206 0.7401 0.079 Uiso 1 1 calc R . . H23B H 0.4143 0.2786 0.7431 0.079 Uiso 1 1 calc R . . H23C H 0.4148 0.1831 0.7272 0.079 Uiso 1 1 calc R . . C232 C 0.4626(17) 0.0619(13) 0.7645(3) 0.056(4) Uiso 1 1 d U . . H23D H 0.5527 0.0602 0.7637 0.084 Uiso 1 1 calc R . . H23E H 0.4283 0.0348 0.7487 0.084 Uiso 1 1 calc R . . H23F H 0.4345 0.0259 0.7795 0.084 Uiso 1 1 calc R . . C233 C 0.2761(14) 0.1589(10) 0.7690(3) 0.039(3) Uiso 1 1 d U . . H23G H 0.2518 0.1254 0.7847 0.058 Uiso 1 1 calc R . . H23H H 0.2425 0.1269 0.7538 0.058 Uiso 1 1 calc R . . H23I H 0.2440 0.2227 0.7696 0.058 Uiso 1 1 calc R . . C260 C 0.8315(16) 0.5286(14) 0.8245(3) 0.056(4) Uiso 1 1 d U . . C261 C 0.880(3) 0.535(3) 0.7973(6) 0.125(11) Uiso 1 1 d U . . H26A H 0.9335 0.4819 0.7938 0.187 Uiso 1 1 calc R . . H26B H 0.9275 0.5931 0.7954 0.187 Uiso 1 1 calc R . . H26C H 0.8111 0.5358 0.7851 0.187 Uiso 1 1 calc R . . C262 C 0.757(4) 0.616(2) 0.8285(6) 0.133(11) Uiso 1 1 d U . . H26D H 0.8101 0.6701 0.8258 0.199 Uiso 1 1 calc R . . H26E H 0.7245 0.6163 0.8461 0.199 Uiso 1 1 calc R . . H26F H 0.6892 0.6170 0.8161 0.199 Uiso 1 1 calc R . . C263 C 0.942(3) 0.529(2) 0.8412(6) 0.118(10) Uiso 1 1 d U . . H26G H 0.9920 0.4738 0.8373 0.177 Uiso 1 1 calc R . . H26H H 0.9159 0.5267 0.8594 0.177 Uiso 1 1 calc R . . H26I H 0.9896 0.5852 0.8381 0.177 Uiso 1 1 calc R . . C310 C 0.1134(13) -0.1740(10) 0.7836(3) 0.037(3) Uiso 1 1 d U . . C311 C 0.153(2) -0.2552(16) 0.7993(4) 0.071(6) Uiso 1 1 d U . . H31A H 0.1536 -0.3111 0.7885 0.106 Uiso 1 1 calc R . . H31B H 0.0949 -0.2640 0.8137 0.106 Uiso 1 1 calc R . . H31C H 0.2354 -0.2439 0.8062 0.106 Uiso 1 1 calc R . . C312 C 0.2021(19) -0.1553(15) 0.7615(4) 0.069(5) Uiso 1 1 d U . . H31D H 0.2035 -0.2093 0.7499 0.104 Uiso 1 1 calc R . . H31E H 0.2849 -0.1446 0.7684 0.104 Uiso 1 1 calc R . . H31F H 0.1750 -0.1001 0.7519 0.104 Uiso 1 1 calc R . . C313 C -0.0142(18) -0.1941(15) 0.7712(4) 0.064(5) Uiso 1 1 d U . . H31G H -0.0083 -0.2493 0.7602 0.096 Uiso 1 1 calc R . . H31H H -0.0398 -0.1404 0.7608 0.096 Uiso 1 1 calc R . . H31I H -0.0750 -0.2053 0.7849 0.096 Uiso 1 1 calc R . . C330 C -0.0970(15) 0.1300(12) 0.8097(3) 0.044(4) Uiso 1 1 d U . . C331 C -0.1707(16) 0.1118(13) 0.8353(3) 0.053(4) Uiso 1 1 d U . . H33A H -0.1926 0.0457 0.8364 0.079 Uiso 1 1 calc R . . H33B H -0.2459 0.1495 0.8353 0.079 Uiso 1 1 calc R . . H33C H -0.1197 0.1288 0.8501 0.079 Uiso 1 1 calc R . . C332 C -0.0586(15) 0.2342(11) 0.8077(3) 0.046(4) Uiso 1 1 d U . . H33D H -0.0110 0.2438 0.7918 0.068 Uiso 1 1 calc R . . H33E H -0.0082 0.2510 0.8227 0.068 Uiso 1 1 calc R . . H33F H -0.1325 0.2733 0.8073 0.068 Uiso 1 1 calc R . . C333 C -0.1794(17) 0.1056(13) 0.7873(3) 0.055(4) Uiso 1 1 d U . . H33G H -0.1350 0.1156 0.7711 0.083 Uiso 1 1 calc R . . H33H H -0.2529 0.1451 0.7877 0.083 Uiso 1 1 calc R . . H33I H -0.2039 0.0400 0.7886 0.083 Uiso 1 1 calc R . . C410 C 0.3466(15) -0.0691(12) 0.9389(3) 0.046(4) Uiso 1 1 d U . . C411 C 0.373(2) 0.0299(16) 0.9465(4) 0.073(5) Uiso 1 1 d U . . H41A H 0.4198 0.0308 0.9627 0.109 Uiso 1 1 calc R . . H41B H 0.2953 0.0635 0.9489 0.109 Uiso 1 1 calc R . . H41C H 0.4213 0.0601 0.9328 0.109 Uiso 1 1 calc R . . C412 C 0.467(2) -0.1106(19) 0.9315(5) 0.092(7) Uiso 1 1 d U . . H41D H 0.5198 -0.1157 0.9468 0.138 Uiso 1 1 calc R . . H41E H 0.5071 -0.0708 0.9186 0.138 Uiso 1 1 calc R . . H41F H 0.4535 -0.1727 0.9241 0.138 Uiso 1 1 calc R . . C413 C 0.283(2) -0.1166(17) 0.9618(4) 0.087(6) Uiso 1 1 d U . . H41G H 0.3373 -0.1153 0.9769 0.131 Uiso 1 1 calc R . . H41H H 0.2640 -0.1814 0.9573 0.131 Uiso 1 1 calc R . . H41I H 0.2062 -0.0836 0.9659 0.131 Uiso 1 1 calc R . . C430 C -0.060(2) -0.1354(16) 0.8934(4) 0.067(5) Uiso 1 1 d U . . C431 C -0.088(3) -0.187(3) 0.9153(6) 0.127(11) Uiso 1 1 d U . . H43A H -0.0391 -0.2449 0.9153 0.190 Uiso 1 1 calc R . . H43B H -0.1757 -0.2029 0.9152 0.190 Uiso 1 1 calc R . . H43C H -0.0685 -0.1509 0.9308 0.190 Uiso 1 1 calc R . . C432 C -0.102(3) -0.170(3) 0.8683(6) 0.128(11) Uiso 1 1 d U . . H43D H -0.0523 -0.2241 0.8634 0.191 Uiso 1 1 calc R . . H43E H -0.0920 -0.1207 0.8553 0.191 Uiso 1 1 calc R . . H43F H -0.1884 -0.1877 0.8695 0.191 Uiso 1 1 calc R . . C433 C -0.147(3) -0.056(2) 0.8975(5) 0.095(8) Uiso 1 1 d U . . H43G H -0.2312 -0.0794 0.8982 0.143 Uiso 1 1 calc R . . H43H H -0.1387 -0.0115 0.8832 0.143 Uiso 1 1 calc R . . H43I H -0.1268 -0.0246 0.9138 0.143 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0206(3) 0.0317(3) 0.0349(3) 0.0017(3) -0.0048(3) -0.0025(3) K1 0.0319(14) 0.0414(15) 0.0470(16) 0.0022(12) -0.0039(14) 0.0005(14) S1 0.0232(14) 0.0214(14) 0.0287(15) 0.0021(12) -0.0009(11) 0.0005(11) O1 0.005(4) 0.047(4) 0.037(4) -0.002(3) -0.004(3) -0.004(3) O2 0.029(4) 0.032(4) 0.036(4) -0.007(3) 0.000(3) -0.008(3) O3 0.019(5) 0.025(4) 0.062(5) -0.001(4) -0.005(4) -0.005(3) O4 0.025(4) 0.034(4) 0.045(5) -0.010(4) -0.010(3) 0.001(3) O5 0.033(4) 0.042(5) 0.047(4) 0.007(4) 0.000(3) -0.002(4) O6 0.031(4) 0.049(6) 0.052(5) 0.008(4) -0.006(4) -0.015(4) O7 0.035(5) 0.042(5) 0.054(6) -0.001(4) -0.010(4) 0.003(4) O8 0.050(7) 0.036(4) 0.068(7) 0.002(5) 0.008(5) -0.003(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 Pr1 O2 2.330(9) . y Pr1 O1 2.383(9) . y Pr1 O5 2.384(10) . y Pr1 O6 2.418(10) . y Pr1 O3 2.434(9) . y Pr1 O4 2.497(9) . y Pr1 O7 2.655(10) . y Pr1 S1 3.223(3) . y Pr1 K1 3.834(3) . y K1 O1 2.610(9) . y K1 O8 2.788(11) . y K1 O4 2.796(10) . y K1 C22 2.952(13) . y K1 O2 3.058(10) . y K1 C21 3.291(11) . y K1 C332 3.321(17) . y K1 C23 3.335(15) . y K1 C233 3.420(14) . y K1 C12 3.428(13) . y K1 C132 3.522(18) . y K1 C64 3.54(2) . y S1 C11 1.780(13) . y S1 C21 1.818(11) . y O1 C12 1.319(15) . ? O2 C22 1.355(15) . ? O3 C31 1.239(15) . ? O4 C33 1.314(16) . ? O5 C41 1.243(16) . ? O6 C43 1.26(2) . ? O7 C52 1.426(10) . ? O7 C53 1.430(10) . ? O8 C63 1.424(17) . ? O8 C62 1.430(17) . ? O9 C73 1.28(4) . ? O9 C72 1.29(4) . ? C11 C12 1.393(18) . ? C11 C19 1.403(18) . ? C12 C13 1.450(19) . ? C13 C14 1.367(19) . ? C13 C130 1.57(2) . ? C14 C20 1.452(18) . ? C15 C20 1.400(19) . ? C15 C16 1.41(2) . ? C16 C17 1.39(2) . ? C16 C160 1.51(2) . ? C17 C18 1.35(2) . ? C18 C19 1.480(19) . ? C19 C20 1.443(17) . ? C21 C22 1.360(16) . ? C21 C29 1.418(16) . ? C22 C23 1.457(18) . ? C23 C24 1.40(2) . ? C23 C230 1.55(2) . ? C24 C30 1.409(18) . ? C25 C26 1.36(2) . ? C25 C30 1.426(18) . ? C26 C27 1.41(2) . ? C26 C260 1.55(2) . ? C27 C28 1.361(19) . ? C28 C29 1.433(17) . ? C29 C30 1.431(16) . ? C31 C32 1.398(19) . ? C31 C310 1.550(19) . ? C32 C33 1.39(2) . ? C33 C330 1.55(2) . ? C41 C42 1.45(2) . ? C41 C410 1.53(2) . ? C42 C43 1.34(2) . ? C43 C430 1.56(3) . ? C51 C52 1.524(10) . ? C53 C54 1.530(10) . ? C61 C62 1.47(2) . ? C63 C64 1.47(2) . ? C71 C72 1.527(9) . ? C73 C74 1.528(9) . ? C130 C133 1.49(2) . ? C130 C132 1.53(2) . ? C130 C131 1.59(2) . ? C160 C163 1.47(3) . ? C160 C161 1.48(3) . ? C160 C162 1.49(3) . ? C230 C232 1.51(2) . ? C230 C231 1.54(2) . ? C230 C233 1.57(2) . ? C260 C263 1.48(3) . ? C260 C262 1.50(4) . ? C260 C261 1.50(3) . ? C310 C311 1.48(3) . ? C310 C312 1.52(2) . ? C310 C313 1.56(2) . ? C330 C333 1.50(2) . ? C330 C332 1.56(2) . ? C330 C331 1.57(2) . ? C410 C412 1.49(3) . ? C410 C411 1.50(3) . ? C410 C413 1.53(3) . ? C430 C431 1.39(4) . ? C430 C432 1.46(4) . ? C430 C433 1.50(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 O2 Pr1 O1 85.9(3) . . y O2 Pr1 O5 133.3(3) . . y O1 Pr1 O5 84.6(3) . . y O2 Pr1 O6 157.2(3) . . y O1 Pr1 O6 97.2(3) . . y O5 Pr1 O6 69.5(3) . . y O2 Pr1 O3 82.8(3) . . y O1 Pr1 O3 142.3(3) . . y O5 Pr1 O3 128.2(4) . . y O6 Pr1 O3 81.1(3) . . y O2 Pr1 O4 78.5(3) . . y O1 Pr1 O4 71.8(3) . . y O5 Pr1 O4 139.5(3) . . y O6 Pr1 O4 81.1(3) . . ? O3 Pr1 O4 70.7(3) . . ? O2 Pr1 O7 80.7(3) . . ? O1 Pr1 O7 138.4(3) . . ? O5 Pr1 O7 76.9(3) . . ? O6 Pr1 O7 110.2(4) . . ? O3 Pr1 O7 74.7(3) . . ? O4 Pr1 O7 141.3(3) . . ? O2 Pr1 S1 61.7(2) . . y O1 Pr1 S1 60.87(18) . . y O5 Pr1 S1 73.8(2) . . y O6 Pr1 S1 138.9(3) . . ? O3 Pr1 S1 138.2(2) . . ? O4 Pr1 S1 118.3(2) . . ? O7 Pr1 S1 78.2(2) . . ? O2 Pr1 K1 52.9(2) . . ? O1 Pr1 K1 42.1(2) . . ? O5 Pr1 K1 125.7(3) . . ? O6 Pr1 K1 116.9(3) . . ? O3 Pr1 K1 105.3(2) . . ? O4 Pr1 K1 46.8(2) . . ? O7 Pr1 K1 132.4(2) . . ? S1 Pr1 K1 71.51(7) . . y O1 K1 O8 126.0(3) . . ? O1 K1 O4 63.9(3) . . ? O8 K1 O4 167.1(3) . . ? O1 K1 C22 80.0(3) . . ? O8 K1 C22 100.9(3) . . ? O4 K1 C22 88.7(3) . . ? O1 K1 O2 68.5(3) . . ? O8 K1 O2 126.7(3) . . ? O4 K1 O2 62.7(3) . . ? C22 K1 O2 26.0(3) . . ? O1 K1 C21 69.5(3) . . ? O8 K1 C21 89.4(3) . . ? O4 K1 C21 102.6(3) . . ? C22 K1 C21 24.4(3) . . ? O2 K1 C21 43.8(3) . . ? O1 K1 C332 103.4(3) . . ? O8 K1 C332 113.1(4) . . ? O4 K1 C332 54.1(3) . . ? C22 K1 C332 132.4(4) . . ? O2 K1 C332 110.7(3) . . ? C21 K1 C332 154.5(4) . . ? O1 K1 C23 105.9(3) . . ? O8 K1 C23 86.2(4) . . ? O4 K1 C23 99.3(3) . . ? C22 K1 C23 25.9(3) . . ? O2 K1 C23 44.0(3) . . ? C21 K1 C23 43.1(3) . . ? C332 K1 C23 123.2(4) . . ? O1 K1 C233 118.6(3) . . ? O8 K1 C233 106.7(3) . . ? O4 K1 C233 70.7(3) . . ? C22 K1 C233 59.5(3) . . ? O2 K1 C233 54.7(3) . . ? C21 K1 C233 83.3(3) . . ? C332 K1 C233 79.0(4) . . ? C23 K1 C233 44.3(4) . . ? O1 K1 C12 19.9(3) . . ? O8 K1 C12 106.1(3) . . ? O4 K1 C12 83.7(3) . . ? C22 K1 C12 81.1(3) . . ? O2 K1 C12 78.1(3) . . ? C21 K1 C12 63.5(3) . . ? C332 K1 C12 117.4(4) . . ? C23 K1 C12 105.7(3) . . ? C233 K1 C12 132.4(3) . . ? O1 K1 C132 55.3(3) . . ? O8 K1 C132 98.9(4) . . ? O4 K1 C132 79.9(4) . . ? C22 K1 C132 134.5(4) . . ? O2 K1 C132 122.1(4) . . ? C21 K1 C132 116.9(4) . . ? C332 K1 C132 72.9(4) . . ? C23 K1 C132 159.7(4) . . ? C233 K1 C132 147.7(4) . . ? C12 K1 C132 54.0(4) . . ? O1 K1 C64 83.8(4) . . ? O8 K1 C64 42.3(4) . . ? O4 K1 C64 145.1(4) . . ? C22 K1 C64 98.8(5) . . ? O2 K1 C64 118.9(4) . . ? C21 K1 C64 75.9(4) . . ? C332 K1 C64 128.7(5) . . ? C23 K1 C64 102.0(4) . . ? C233 K1 C64 141.5(4) . . ? C12 K1 C64 64.1(4) . . ? C132 K1 C64 70.5(5) . . ? C11 S1 C21 109.3(6) . . y C11 S1 Pr1 93.1(4) . . ? C21 S1 Pr1 95.1(4) . . ? C12 O1 Pr1 128.2(8) . . ? C12 O1 K1 117.7(8) . . ? Pr1 O1 K1 100.2(3) . . ? C22 O2 Pr1 137.1(8) . . ? C22 O2 K1 72.6(7) . . ? Pr1 O2 K1 89.7(3) . . ? C31 O3 Pr1 136.3(8) . . ? C33 O4 Pr1 131.8(9) . . ? C33 O4 K1 131.3(8) . . ? Pr1 O4 K1 92.6(3) . . ? C41 O5 Pr1 141.4(9) . . ? C43 O6 Pr1 136.3(11) . . ? C52 O7 C53 104(3) . . ? C52 O7 Pr1 115(2) . . ? C53 O7 Pr1 124.6(14) . . ? C63 O8 C62 114.6(14) . . ? C63 O8 K1 119.0(10) . . ? C62 O8 K1 123.2(11) . . ? C73 O9 C72 119(3) . . ? C12 C11 C19 121.0(12) . . ? C12 C11 S1 117.9(10) . . ? C19 C11 S1 120.7(10) . . ? O1 C12 C11 120.6(11) . . ? O1 C12 C13 119.6(12) . . ? C11 C12 C13 119.7(12) . . ? O1 C12 K1 42.4(6) . . ? C11 C12 K1 108.5(8) . . ? C13 C12 K1 114.0(8) . . ? C14 C13 C12 119.1(14) . . ? C14 C13 C130 118.1(13) . . ? C12 C13 C130 122.8(12) . . ? C13 C14 C20 122.6(12) . . ? C20 C15 C16 124.1(14) . . ? C17 C16 C15 114.3(14) . . ? C17 C16 C160 125.7(14) . . ? C15 C16 C160 119.9(14) . . ? C18 C17 C16 125.3(15) . . ? C17 C18 C19 121.8(13) . . ? C11 C19 C20 120.5(12) . . ? C11 C19 C18 126.1(12) . . ? C20 C19 C18 113.4(11) . . ? C15 C20 C19 121.0(12) . . ? C15 C20 C14 122.3(12) . . ? C19 C20 C14 116.6(11) . . ? C22 C21 C29 122.1(10) . . ? C22 C21 S1 116.2(9) . . ? C29 C21 S1 121.0(8) . . ? C22 C21 K1 63.7(7) . . ? C29 C21 K1 107.2(7) . . ? S1 C21 K1 105.1(4) . . ? O2 C22 C21 122.4(11) . . ? O2 C22 C23 117.7(11) . . ? C21 C22 C23 119.6(11) . . ? O2 C22 K1 81.4(7) . . ? C21 C22 K1 91.9(7) . . ? C23 C22 K1 91.9(8) . . ? C24 C23 C22 118.7(12) . . ? C24 C23 C230 120.3(12) . . ? C22 C23 C230 120.8(12) . . ? C24 C23 K1 106.1(9) . . ? C22 C23 K1 62.2(7) . . ? C230 C23 K1 105.0(9) . . ? C23 C24 C30 121.6(13) . . ? C26 C25 C30 122.7(13) . . ? C25 C26 C27 117.6(15) . . ? C25 C26 C260 119.4(14) . . ? C27 C26 C260 123.0(14) . . ? C28 C27 C26 121.8(14) . . ? C27 C28 C29 122.4(12) . . ? C21 C29 C30 118.9(10) . . ? C21 C29 C28 125.5(11) . . ? C30 C29 C28 115.6(11) . . ? C24 C30 C25 121.3(12) . . ? C24 C30 C29 119.0(12) . . ? C25 C30 C29 119.6(11) . . ? O3 C31 C32 126.2(13) . . ? O3 C31 C310 113.7(11) . . ? C32 C31 C310 120.0(12) . . ? C33 C32 C31 125.7(13) . . ? O4 C33 C32 124.8(12) . . ? O4 C33 C330 113.5(12) . . ? C32 C33 C330 121.5(12) . . ? O5 C41 C42 121.5(13) . . ? O5 C41 C410 119.1(14) . . ? C42 C41 C410 119.3(13) . . ? C43 C42 C41 123.7(16) . . ? O6 C43 C42 127.5(17) . . ? O6 C43 C430 110.8(16) . . ? C42 C43 C430 121.7(17) . . ? O7 C52 C51 109(2) . . ? O7 C53 C54 122(3) . . ? O8 C62 C61 111.2(17) . . ? O8 C63 C64 110.9(16) . . ? C63 C64 K1 84.3(11) . . ? O9 C72 C71 119(4) . . ? O9 C73 C74 111(4) . . ? C133 C130 C132 107.7(14) . . ? C133 C130 C13 113.2(13) . . ? C132 C130 C13 112.7(13) . . ? C133 C130 C131 108.4(14) . . ? C132 C130 C131 109.0(13) . . ? C13 C130 C131 105.7(12) . . ? C130 C132 K1 118.4(11) . . ? C163 C160 C161 111.6(19) . . ? C163 C160 C162 108(2) . . ? C161 C160 C162 101(2) . . ? C163 C160 C16 111.6(15) . . ? C161 C160 C16 118.7(17) . . ? C162 C160 C16 105.3(18) . . ? C232 C230 C231 109.8(13) . . ? C232 C230 C23 111.3(13) . . ? C231 C230 C23 112.9(13) . . ? C232 C230 C233 106.7(13) . . ? C231 C230 C233 106.0(12) . . ? C23 C230 C233 109.8(12) . . ? C230 C233 K1 101.0(8) . . ? C263 C260 C262 111(2) . . ? C263 C260 C261 105(2) . . ? C262 C260 C261 105(2) . . ? C263 C260 C26 114.1(19) . . ? C262 C260 C26 106.9(19) . . ? C261 C260 C26 114.3(19) . . ? C311 C310 C312 111.7(15) . . ? C311 C310 C31 108.0(13) . . ? C312 C310 C31 107.6(13) . . ? C311 C310 C313 109.7(15) . . ? C312 C310 C313 106.6(14) . . ? C31 C310 C313 113.4(13) . . ? C333 C330 C33 112.3(13) . . ? C333 C330 C332 109.3(14) . . ? C33 C330 C332 111.5(13) . . ? C333 C330 C331 107.9(14) . . ? C33 C330 C331 105.0(12) . . ? C332 C330 C331 110.7(13) . . ? C330 C332 K1 111.7(10) . . ? C412 C410 C411 106.2(18) . . ? C412 C410 C41 105.2(15) . . ? C411 C410 C41 106.1(14) . . ? C412 C410 C413 114.8(18) . . ? C411 C410 C413 107.9(16) . . ? C41 C410 C413 115.9(16) . . ? C431 C430 C432 118(3) . . ? C431 C430 C433 99(2) . . ? C432 C430 C433 101(2) . . ? C431 C430 C43 115(2) . . ? C432 C430 C43 114(2) . . ? C433 C430 C43 106.7(19) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 2.691 _refine_diff_density_min -4.039 _refine_diff_density_rms 0.201 #===END of CIF data_NDDITH_compound_2a _database_code_depnum_ccdc_archive 'CCDC 298871' _refine_special_details ; Disorder in the t-butyl group centred on C260 was identified and modelled over two sites with occupancies 0.7:0.3, and C atoms were refined isotropically.Hydrogen atoms have been included. Carbons C62 and C63 (coordinated THF) and C411 and C413 (one methyl fragment from two separate t-butyl groups) show very large thermal motion. However, no sensible disorder model could be identified, so the atoms have been refined isotropically. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H98 K Nd O8 S, 0.5(C6 H14)' _chemical_formula_sum 'C69 H105 K Nd O8 S' _chemical_formula_weight 1277.93 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 10.8384(8) _cell_length_b 15.0949(12) _cell_length_c 21.577(2) _cell_angle_alpha 94.879(1) _cell_angle_beta 103.170(1) _cell_angle_gamma 90.743(1) _cell_volume 3422.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3178 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 23.65 _exptl_crystal_description sphenoid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS version 2.03; Bruker, 2001)' _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29257 _diffrn_reflns_av_R_equivalents 0.139 _diffrn_reflns_av_sigmaI/netI 0.294 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.15 _reflns_number_total 15691 _reflns_number_gt 6203 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _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^)+(0.0899P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0074(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15691 _refine_ls_number_parameters 700 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.201 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.213 _refine_ls_wR_factor_gt 0.168 _refine_ls_goodness_of_fit_ref 0.85 _refine_ls_restrained_S_all 0.85 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 2.00213(4) 1.35056(3) 1.28635(3) 0.03469(18) Uani 1 1 d . . . K1 K 1.98223(18) 1.29349(13) 1.11564(11) 0.0508(6) Uani 1 1 d . . . S1 S 1.74110(18) 1.24580(13) 1.23935(11) 0.0368(5) Uani 1 1 d . . . O1 O 1.8591(5) 1.3986(3) 1.1997(3) 0.0432(16) Uani 1 1 d . . . O2 O 1.9959(5) 1.2188(3) 1.2171(3) 0.0404(15) Uani 1 1 d . . . O3 O 1.9851(5) 1.2609(4) 1.3676(3) 0.0474(16) Uani 1 1 d . . . O4 O 2.2014(5) 1.3391(4) 1.3571(3) 0.0455(16) Uani 1 1 d . . . O5 O 2.1439(5) 1.3780(3) 1.2172(3) 0.0408(15) Uani 1 1 d . . . O6 O 2.0633(5) 1.5048(4) 1.3019(3) 0.0465(16) Uani 1 1 d . . . O7 O 1.8615(5) 1.4300(4) 1.3515(3) 0.0544(18) Uani 1 1 d . . . O8 O 1.8979(7) 1.2257(5) 0.9985(5) 0.084(2) Uani 1 1 d . . . C11 C 1.7016(6) 1.2840(5) 1.1625(4) 0.0307(19) Uani 1 1 d . . . C12 C 1.7622(7) 1.3642(5) 1.1561(4) 0.039(2) Uani 1 1 d . . . C13 C 1.7169(7) 1.4086(5) 1.0988(5) 0.038(2) Uani 1 1 d . . . C14 C 1.6227(7) 1.3687(5) 1.0513(5) 0.043(2) Uani 1 1 d . . . H14A H 1.5953 1.3975 1.0133 0.051 Uiso 1 1 calc R . . C15 C 1.4630(7) 1.2492(5) 1.0057(4) 0.037(2) Uani 1 1 d . . . H15A H 1.4390 1.2793 0.9681 0.045 Uiso 1 1 calc R . . C16 C 1.3991(7) 1.1715(5) 1.0093(5) 0.041(2) Uani 1 1 d . . . C17 C 1.4415(7) 1.1289(5) 1.0652(4) 0.041(2) Uani 1 1 d . . . H17A H 1.4033 1.0729 1.0684 0.050 Uiso 1 1 calc R . . C18 C 1.5360(7) 1.1642(5) 1.1158(5) 0.043(2) Uani 1 1 d . . . H18A H 1.5571 1.1341 1.1535 0.051 Uiso 1 1 calc R . . C19 C 1.6016(7) 1.2439(5) 1.1126(4) 0.035(2) Uani 1 1 d . . . C20 C 1.5643(7) 1.2865(5) 1.0561(5) 0.042(2) Uani 1 1 d . . . C21 C 1.8180(7) 1.1426(5) 1.2340(4) 0.034(2) Uani 1 1 d . . . C22 C 1.9417(7) 1.1436(5) 1.2257(4) 0.039(2) Uani 1 1 d . . . C23 C 2.0094(7) 1.0620(5) 1.2264(4) 0.039(2) Uani 1 1 d . . . C24 C 1.9502(7) 0.9871(5) 1.2381(4) 0.041(2) Uani 1 1 d . . . H24A H 1.9936 0.9328 1.2383 0.050 Uiso 1 1 calc R . . C25 C 1.7745(7) 0.9083(5) 1.2656(4) 0.038(2) Uani 1 1 d . . . H25A H 1.8224 0.8560 1.2674 0.045 Uiso 1 1 calc R . . C26 C 1.6585(7) 0.9040(5) 1.2785(4) 0.038(2) Uani 1 1 d . A . C26A C 1.603(5) 0.743(3) 1.245(3) 0.078(18) Uiso 0.222(15) 1 d P A 2 H26A H 1.5443 0.7523 1.2044 0.117 Uiso 0.222(15) 1 calc PR A 2 H26B H 1.5787 0.6880 1.2608 0.117 Uiso 0.222(15) 1 calc PR A 2 H26C H 1.6894 0.7378 1.2378 0.117 Uiso 0.222(15) 1 calc PR A 2 C26B C 1.470(4) 0.825(3) 1.277(2) 0.059(14) Uiso 0.222(15) 1 d P A 2 H26D H 1.4425 0.8352 1.2313 0.088 Uiso 0.222(15) 1 calc PR A 2 H26E H 1.4454 0.8749 1.3028 0.088 Uiso 0.222(15) 1 calc PR A 2 H26F H 1.4309 0.7697 1.2844 0.088 Uiso 0.222(15) 1 calc PR A 2 C26C C 1.690(6) 0.806(4) 1.355(3) 0.11(2) Uiso 0.222(15) 1 d P A 2 H26G H 1.7714 0.7861 1.3471 0.162 Uiso 0.222(15) 1 calc PR A 2 H26H H 1.6538 0.7601 1.3760 0.162 Uiso 0.222(15) 1 calc PR A 2 H26I H 1.7028 0.8616 1.3823 0.162 Uiso 0.222(15) 1 calc PR A 2 C27 C 1.5913(7) 0.9841(5) 1.2756(5) 0.045(2) Uani 1 1 d . . . H27A H 1.5088 0.9838 1.2838 0.054 Uiso 1 1 calc R . . C28 C 1.6395(7) 1.0606(5) 1.2618(4) 0.039(2) Uani 1 1 d . . . H28A H 1.5913 1.1126 1.2622 0.047 Uiso 1 1 calc R . . C29 C 1.7591(7) 1.0661(5) 1.2466(4) 0.033(2) Uani 1 1 d . . . C30 C 1.8287(7) 0.9865(5) 1.2497(4) 0.038(2) Uani 1 1 d . . . C31 C 2.0516(8) 1.2385(5) 1.4184(5) 0.043(2) Uani 1 1 d . . . C32 C 2.1818(8) 1.2590(5) 1.4413(4) 0.045(2) Uani 1 1 d . . . H32A H 2.2243 1.2385 1.4807 0.054 Uiso 1 1 calc R . . C33 C 2.2499(7) 1.3077(6) 1.4085(5) 0.039(2) Uani 1 1 d . . . C41 C 2.2228(7) 1.4402(6) 1.2157(5) 0.043(2) Uani 1 1 d . . . C42 C 2.2194(8) 1.5248(6) 1.2466(5) 0.050(3) Uani 1 1 d . . . H42A H 2.2797 1.5675 1.2405 0.059 Uiso 1 1 calc R . . C43 C 2.1382(7) 1.5545(6) 1.2854(5) 0.046(2) Uani 1 1 d . . . C51 C 1.9122(9) 1.4650(7) 1.4161(6) 0.069(3) Uani 1 1 d . . . H51A H 1.9782 1.5117 1.4180 0.083 Uiso 1 1 calc R . . H51B H 1.9503 1.4173 1.4423 0.083 Uiso 1 1 calc R . . C52 C 1.8021(11) 1.5036(10) 1.4402(7) 0.100(5) Uani 1 1 d . . . H52A H 1.7613 1.4590 1.4608 0.120 Uiso 1 1 calc R . . H52B H 1.8295 1.5565 1.4709 0.120 Uiso 1 1 calc R . . C53 C 1.7172(13) 1.5274(8) 1.3818(7) 0.095(4) Uani 1 1 d . . . H53A H 1.7321 1.5905 1.3755 0.114 Uiso 1 1 calc R . . H53B H 1.6277 1.5188 1.3841 0.114 Uiso 1 1 calc R . . C54 C 1.7446(11) 1.4687(9) 1.3287(7) 0.101(5) Uani 1 1 d . . . H54A H 1.6770 1.4219 1.3139 0.121 Uiso 1 1 calc R . . H54B H 1.7491 1.5035 1.2923 0.121 Uiso 1 1 calc R . . C61 C 1.8227(13) 1.1472(10) 0.9951(8) 0.118(6) Uani 1 1 d . . . H61A H 1.7889 1.1455 1.0339 0.142 Uiso 1 1 calc R . . H61B H 1.8730 1.0937 0.9907 0.142 Uiso 1 1 calc R . . C62 C 1.7173(14) 1.1514(10) 0.9373(8) 0.110(5) Uiso 1 1 d . . . H62A H 1.7177 1.0993 0.9062 0.132 Uiso 1 1 calc R . . H62B H 1.6344 1.1521 0.9493 0.132 Uiso 1 1 calc R . . C63 C 1.7387(14) 1.2306(10) 0.9107(8) 0.113(5) Uiso 1 1 d . . . H63A H 1.6799 1.2763 0.9208 0.135 Uiso 1 1 calc R . . H63B H 1.7235 1.2196 0.8636 0.135 Uiso 1 1 calc R . . C64 C 1.8756(14) 1.2627(10) 0.9386(8) 0.113(5) Uani 1 1 d . . . H64A H 1.9331 1.2389 0.9121 0.136 Uiso 1 1 calc R . . H64B H 1.8839 1.3285 0.9440 0.136 Uiso 1 1 calc R . . C71 C 1.2332(14) 0.9492(9) 1.4100(7) 0.113(5) Uani 1 1 d . . . H71A H 1.1771 0.9760 1.3747 0.169 Uiso 1 1 calc R . . H71B H 1.1880 0.9415 1.4438 0.169 Uiso 1 1 calc R . . H71C H 1.2590 0.8911 1.3943 0.169 Uiso 1 1 calc R . . C72 C 1.3479(15) 1.0084(9) 1.4360(8) 0.110(5) Uani 1 1 d . . . H72A H 1.3911 1.0171 1.4011 0.132 Uiso 1 1 calc R . . H72B H 1.3204 1.0673 1.4506 0.132 Uiso 1 1 calc R . . C73 C 1.4396(11) 0.9746(8) 1.4896(7) 0.100(5) Uani 1 1 d . . . H73A H 1.3996 0.9738 1.5265 0.120 Uiso 1 1 calc R . . H73B H 1.4576 0.9124 1.4770 0.120 Uiso 1 1 calc R . . C130 C 1.7728(7) 1.5007(5) 1.0927(5) 0.047(3) Uani 1 1 d . . . C131 C 1.7098(9) 1.5364(6) 1.0316(5) 0.063(3) Uani 1 1 d . . . H13A H 1.7224 1.4962 0.9956 0.094 Uiso 1 1 calc R . . H13B H 1.7466 1.5954 1.0295 0.094 Uiso 1 1 calc R . . H13C H 1.6188 1.5411 1.0294 0.094 Uiso 1 1 calc R . . C132 C 1.9155(8) 1.4983(6) 1.0959(5) 0.053(3) Uani 1 1 d . . . H13D H 1.9305 1.4578 1.0606 0.080 Uiso 1 1 calc R . . H13E H 1.9593 1.4773 1.1366 0.080 Uiso 1 1 calc R . . H13F H 1.9479 1.5582 1.0925 0.080 Uiso 1 1 calc R . . C133 C 1.7515(9) 1.5662(5) 1.1495(5) 0.054(3) Uani 1 1 d . . . H13G H 1.6606 1.5692 1.1479 0.081 Uiso 1 1 calc R . . H13H H 1.7856 1.6256 1.1461 0.081 Uiso 1 1 calc R . . H13I H 1.7952 1.5448 1.1902 0.081 Uiso 1 1 calc R . . C160 C 1.2928(7) 1.1291(6) 0.9551(5) 0.046(2) Uani 1 1 d . . . C161 C 1.1772(9) 1.1108(8) 0.9832(5) 0.070(3) Uani 1 1 d . . . H16A H 1.1078 1.0835 0.9493 0.105 Uiso 1 1 calc R . . H16B H 1.1498 1.1669 1.0012 0.105 Uiso 1 1 calc R . . H16C H 1.2005 1.0703 1.0168 0.105 Uiso 1 1 calc R . . C162 C 1.3347(10) 1.0412(6) 0.9284(6) 0.080(4) Uani 1 1 d . . . H16D H 1.4078 1.0518 0.9101 0.121 Uiso 1 1 calc R . . H16E H 1.2649 1.0132 0.8951 0.121 Uiso 1 1 calc R . . H16F H 1.3583 1.0019 0.9628 0.121 Uiso 1 1 calc R . . C163 C 1.2514(9) 1.1885(6) 0.9031(5) 0.068(3) Uani 1 1 d . . . H16G H 1.3228 1.2013 0.8840 0.103 Uiso 1 1 calc R . . H16H H 1.2223 1.2442 0.9208 0.103 Uiso 1 1 calc R . . H16I H 1.1819 1.1590 0.8703 0.103 Uiso 1 1 calc R . . C230 C 2.1454(7) 1.0592(5) 1.2159(5) 0.045(2) Uani 1 1 d . . . C231 C 2.2326(8) 1.1208(6) 1.2687(6) 0.066(3) Uani 1 1 d . . . H23A H 2.2012 1.1814 1.2677 0.099 Uiso 1 1 calc R . . H23B H 2.3188 1.1210 1.2616 0.099 Uiso 1 1 calc R . . H23C H 2.2335 1.0994 1.3104 0.099 Uiso 1 1 calc R . . C232 C 2.1964(8) 0.9657(6) 1.2167(5) 0.054(3) Uani 1 1 d . . . H23D H 2.1419 0.9265 1.1826 0.081 Uiso 1 1 calc R . . H23E H 2.1975 0.9433 1.2581 0.081 Uiso 1 1 calc R . . H23F H 2.2828 0.9672 1.2099 0.081 Uiso 1 1 calc R . . C233 C 2.1475(9) 1.0905(6) 1.1511(5) 0.059(3) Uani 1 1 d . . . H23G H 2.0923 1.0509 1.1175 0.088 Uiso 1 1 calc R . . H23H H 2.2344 1.0893 1.1450 0.088 Uiso 1 1 calc R . . H23I H 2.1172 1.1513 1.1491 0.088 Uiso 1 1 calc R . . C260 C 1.6005(8) 0.8191(6) 1.2923(5) 0.049(3) Uani 1 1 d . . . C261 C 1.4846(11) 0.7908(8) 1.2383(6) 0.050(4) Uiso 0.778(15) 1 d P A 1 H26J H 1.4744 0.8333 1.2057 0.075 Uiso 0.778(15) 1 calc PR A 1 H26K H 1.4085 0.7898 1.2556 0.075 Uiso 0.778(15) 1 calc PR A 1 H26L H 1.4967 0.7314 1.2190 0.075 Uiso 0.778(15) 1 calc PR A 1 C262 C 1.6895(12) 0.7434(8) 1.2977(7) 0.060(4) Uiso 0.778(15) 1 d P A 1 H26M H 1.6767 0.7083 1.2562 0.090 Uiso 0.778(15) 1 calc PR A 1 H26N H 1.6728 0.7055 1.3297 0.090 Uiso 0.778(15) 1 calc PR A 1 H26O H 1.7772 0.7669 1.3106 0.090 Uiso 0.778(15) 1 calc PR A 1 C263 C 1.5624(13) 0.8358(9) 1.3572(7) 0.067(4) Uiso 0.778(15) 1 d P A 1 H26P H 1.4744 0.8546 1.3498 0.100 Uiso 0.778(15) 1 calc PR A 1 H26Q H 1.6182 0.8826 1.3840 0.100 Uiso 0.778(15) 1 calc PR A 1 H26R H 1.5703 0.7809 1.3787 0.100 Uiso 0.778(15) 1 calc PR A 1 C310 C 1.9805(8) 1.1811(6) 1.4567(5) 0.051(3) Uani 1 1 d . . . C311 C 1.9316(11) 1.0983(7) 1.4141(6) 0.084(4) Uani 1 1 d . . . H31A H 2.0032 1.0638 1.4060 0.126 Uiso 1 1 calc R . . H31B H 1.8797 1.1146 1.3736 0.126 Uiso 1 1 calc R . . H31C H 1.8799 1.0623 1.4351 0.126 Uiso 1 1 calc R . . C312 C 1.8724(10) 1.2350(8) 1.4707(7) 0.088(4) Uani 1 1 d . . . H31D H 1.8244 1.2009 1.4946 0.132 Uiso 1 1 calc R . . H31E H 1.8164 1.2488 1.4304 0.132 Uiso 1 1 calc R . . H31F H 1.9060 1.2906 1.4962 0.132 Uiso 1 1 calc R . . C313 C 2.0601(10) 1.1577(7) 1.5185(5) 0.073(3) Uani 1 1 d . . . H31G H 2.1305 1.1218 1.5105 0.110 Uiso 1 1 calc R . . H31H H 2.0085 1.1235 1.5406 0.110 Uiso 1 1 calc R . . H31I H 2.0938 1.2123 1.5453 0.110 Uiso 1 1 calc R . . C330 C 2.3934(8) 1.3243(6) 1.4330(5) 0.048(2) Uani 1 1 d . . . C331 C 2.4228(9) 1.4214(6) 1.4270(6) 0.064(3) Uani 1 1 d . . . H33A H 2.3925 1.4344 1.3825 0.097 Uiso 1 1 calc R . . H33B H 2.5146 1.4332 1.4403 0.097 Uiso 1 1 calc R . . H33C H 2.3804 1.4592 1.4544 0.097 Uiso 1 1 calc R . . C332 C 2.4423(8) 1.3056(7) 1.5018(5) 0.063(3) Uani 1 1 d . . . H33D H 2.4252 1.2429 1.5064 0.094 Uiso 1 1 calc R . . H33E H 2.3995 1.3433 1.5291 0.094 Uiso 1 1 calc R . . H33F H 2.5338 1.3186 1.5145 0.094 Uiso 1 1 calc R . . C333 C 2.4581(8) 1.2654(7) 1.3901(6) 0.073(4) Uani 1 1 d . . . H33G H 2.4266 1.2782 1.3456 0.109 Uiso 1 1 calc R . . H33H H 2.4394 1.2028 1.3943 0.109 Uiso 1 1 calc R . . H33I H 2.5499 1.2773 1.4028 0.109 Uiso 1 1 calc R . . C410 C 2.3269(8) 1.4136(7) 1.1806(5) 0.056(3) Uani 1 1 d . . . C411 C 2.3982(12) 1.4928(9) 1.1658(7) 0.099(4) Uiso 1 1 d . . . H41A H 2.3395 1.5286 1.1373 0.148 Uiso 1 1 calc R . . H41B H 2.4652 1.4721 1.1448 0.148 Uiso 1 1 calc R . . H41C H 2.4362 1.5292 1.2056 0.148 Uiso 1 1 calc R . . C412 C 2.4205(9) 1.3611(9) 1.2243(6) 0.085(4) Uani 1 1 d . . . H41D H 2.3769 1.3091 1.2349 0.127 Uiso 1 1 calc R . . H41E H 2.4583 1.3985 1.2636 0.127 Uiso 1 1 calc R . . H41F H 2.4873 1.3413 1.2030 0.127 Uiso 1 1 calc R . . C413 C 2.2726(9) 1.3561(7) 1.1207(5) 0.066(3) Uani 1 1 d . . . H41G H 2.2295 1.3036 1.1309 0.098 Uiso 1 1 calc R . . H41H H 2.3410 1.3371 1.1002 0.098 Uiso 1 1 calc R . . H41I H 2.2117 1.3896 1.0916 0.098 Uiso 1 1 calc R . . C430 C 2.1409(8) 1.6546(6) 1.3103(5) 0.048(2) Uani 1 1 d . . . C431 C 2.2562(12) 1.6710(9) 1.3616(6) 0.097(4) Uiso 1 1 d . . . H43A H 2.2616 1.7336 1.3786 0.145 Uiso 1 1 calc R . . H43B H 2.3308 1.6573 1.3445 0.145 Uiso 1 1 calc R . . H43C H 2.2531 1.6330 1.3959 0.145 Uiso 1 1 calc R . . C432 C 2.0243(11) 1.6756(7) 1.3333(7) 0.096(5) Uani 1 1 d . . . H43D H 2.0275 1.7387 1.3489 0.144 Uiso 1 1 calc R . . H43E H 2.0190 1.6390 1.3680 0.144 Uiso 1 1 calc R . . H43F H 1.9497 1.6630 1.2980 0.144 Uiso 1 1 calc R . . C433 C 2.1439(13) 1.7135(7) 1.2562(7) 0.094(4) Uani 1 1 d . . . H43G H 2.1461 1.7763 1.2725 0.141 Uiso 1 1 calc R . . H43H H 2.0680 1.7006 1.2217 0.141 Uiso 1 1 calc R . . H43I H 2.2197 1.7014 1.2397 0.141 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0203(2) 0.0272(2) 0.0549(4) -0.0001(2) 0.00652(19) -0.00066(15) K1 0.0408(11) 0.0464(12) 0.0638(16) 0.0023(11) 0.0096(10) 0.0062(9) S1 0.0252(10) 0.0279(10) 0.0551(15) 0.0025(10) 0.0053(10) 0.0036(8) O1 0.028(3) 0.031(3) 0.065(4) 0.000(3) 0.002(3) -0.006(2) O2 0.032(3) 0.027(3) 0.061(4) -0.001(3) 0.011(3) 0.000(2) O3 0.037(3) 0.052(4) 0.049(4) 0.011(3) -0.002(3) 0.002(3) O4 0.024(3) 0.050(4) 0.062(5) 0.017(3) 0.004(3) -0.005(3) O5 0.027(3) 0.038(3) 0.056(4) 0.007(3) 0.007(3) -0.002(2) O6 0.028(3) 0.036(3) 0.075(5) -0.009(3) 0.016(3) -0.006(3) O7 0.035(3) 0.045(4) 0.076(5) -0.016(4) 0.006(3) 0.000(3) O8 0.072(5) 0.065(5) 0.106(7) -0.006(5) 0.010(5) -0.015(4) C11 0.021(4) 0.031(4) 0.038(5) -0.001(4) 0.003(4) 0.005(3) C12 0.026(4) 0.026(4) 0.058(6) 0.006(4) 0.000(4) 0.005(3) C13 0.024(4) 0.027(4) 0.064(7) 0.001(4) 0.011(4) 0.004(3) C14 0.030(4) 0.036(5) 0.067(7) 0.011(5) 0.020(5) 0.006(4) C15 0.026(4) 0.032(4) 0.052(6) -0.002(4) 0.008(4) 0.006(3) C16 0.028(4) 0.030(4) 0.061(7) -0.004(4) 0.006(4) 0.005(3) C17 0.033(4) 0.031(4) 0.055(6) -0.001(4) 0.000(4) 0.002(4) C18 0.034(5) 0.034(5) 0.062(7) -0.001(4) 0.015(4) 0.004(4) C19 0.018(4) 0.031(4) 0.056(6) 0.005(4) 0.006(4) 0.009(3) C20 0.023(4) 0.030(4) 0.074(7) 0.005(4) 0.009(4) 0.005(3) C21 0.025(4) 0.027(4) 0.048(6) -0.003(4) 0.006(4) 0.002(3) C22 0.031(4) 0.033(4) 0.052(6) -0.001(4) 0.005(4) -0.004(4) C23 0.025(4) 0.030(4) 0.056(6) -0.002(4) -0.004(4) 0.000(3) C24 0.034(5) 0.027(4) 0.061(7) 0.005(4) 0.007(4) 0.005(4) C25 0.028(4) 0.025(4) 0.059(6) 0.006(4) 0.007(4) 0.003(3) C26 0.034(4) 0.031(4) 0.047(6) 0.003(4) 0.003(4) -0.006(4) C27 0.023(4) 0.039(5) 0.071(7) 0.004(5) 0.011(4) -0.002(4) C28 0.026(4) 0.032(4) 0.058(6) 0.007(4) 0.006(4) -0.001(3) C29 0.023(4) 0.040(5) 0.037(5) 0.008(4) 0.004(4) -0.002(3) C30 0.029(4) 0.028(4) 0.050(6) -0.004(4) -0.002(4) 0.001(3) C31 0.038(5) 0.036(5) 0.057(7) -0.001(5) 0.015(5) 0.001(4) C32 0.050(5) 0.039(5) 0.038(6) -0.003(4) -0.004(5) 0.002(4) C33 0.029(4) 0.041(5) 0.043(6) 0.002(4) -0.002(4) 0.004(4) C41 0.026(4) 0.044(5) 0.059(7) 0.000(5) 0.009(4) -0.003(4) C42 0.032(5) 0.046(5) 0.070(7) -0.004(5) 0.015(5) -0.018(4) C43 0.024(4) 0.040(5) 0.072(7) -0.001(5) 0.011(5) -0.008(4) C51 0.047(6) 0.054(6) 0.107(10) -0.015(6) 0.028(6) -0.003(5) C52 0.071(8) 0.119(12) 0.113(13) -0.024(10) 0.037(9) 0.011(8) C53 0.107(11) 0.065(8) 0.136(14) 0.026(8) 0.068(10) 0.038(7) C54 0.060(7) 0.119(11) 0.112(11) -0.039(9) 0.010(7) 0.052(7) C61 0.097(11) 0.110(12) 0.149(16) -0.007(11) 0.037(11) -0.027(9) C64 0.107(11) 0.112(12) 0.114(13) 0.034(10) 0.005(10) -0.017(9) C71 0.135(13) 0.082(10) 0.134(14) 0.014(9) 0.059(11) -0.022(9) C72 0.148(14) 0.087(10) 0.125(14) 0.041(10) 0.077(12) 0.046(10) C73 0.103(11) 0.068(9) 0.139(14) 0.015(9) 0.047(11) 0.024(7) C130 0.029(4) 0.035(5) 0.076(7) 0.021(5) 0.005(5) -0.002(4) C131 0.055(6) 0.039(5) 0.081(8) 0.022(5) -0.018(6) -0.012(4) C132 0.038(5) 0.047(5) 0.074(8) 0.019(5) 0.006(5) 0.001(4) C133 0.052(6) 0.032(5) 0.072(8) -0.002(5) 0.006(5) -0.002(4) C160 0.027(4) 0.039(5) 0.067(7) -0.007(5) 0.005(4) -0.003(4) C161 0.053(6) 0.093(8) 0.057(7) 0.005(6) 0.001(5) -0.015(6) C162 0.076(8) 0.048(6) 0.095(10) -0.030(6) -0.014(7) 0.008(5) C163 0.059(6) 0.046(6) 0.080(8) -0.001(6) -0.025(6) -0.006(5) C230 0.031(4) 0.027(4) 0.077(8) 0.000(5) 0.013(5) 0.003(3) C231 0.025(4) 0.051(6) 0.118(10) -0.006(6) 0.013(5) 0.002(4) C232 0.027(4) 0.047(5) 0.090(8) -0.008(5) 0.024(5) 0.011(4) C233 0.047(6) 0.057(6) 0.082(8) 0.020(6) 0.027(6) 0.018(5) C260 0.032(5) 0.037(5) 0.075(8) 0.001(5) 0.009(5) -0.004(4) C310 0.040(5) 0.050(6) 0.064(7) 0.016(5) 0.005(5) 0.003(4) C311 0.101(9) 0.065(7) 0.085(9) 0.015(7) 0.018(8) -0.032(7) C312 0.073(8) 0.090(9) 0.120(12) 0.045(8) 0.051(8) 0.007(7) C313 0.067(7) 0.083(8) 0.073(9) 0.029(7) 0.015(6) -0.008(6) C330 0.033(5) 0.049(5) 0.054(7) -0.001(5) -0.003(4) -0.004(4) C331 0.041(5) 0.055(6) 0.090(9) 0.006(6) 0.003(6) -0.012(5) C332 0.035(5) 0.083(8) 0.062(8) 0.002(6) -0.002(5) 0.004(5) C333 0.033(5) 0.069(7) 0.111(10) -0.014(7) 0.013(6) 0.010(5) C410 0.032(5) 0.074(7) 0.065(7) -0.009(6) 0.018(5) -0.009(5) C412 0.038(6) 0.143(11) 0.074(9) 0.000(8) 0.016(6) 0.041(7) C413 0.046(6) 0.060(6) 0.096(9) -0.012(6) 0.034(6) -0.003(5) C430 0.036(5) 0.043(5) 0.067(7) 0.000(5) 0.016(5) -0.011(4) C432 0.077(8) 0.045(6) 0.168(14) -0.029(8) 0.047(9) 0.005(6) C433 0.135(12) 0.043(6) 0.117(12) 0.015(7) 0.052(10) -0.002(7) _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 O1 2.316(6) . y Nd1 O2 2.374(5) . y Nd1 O3 2.342(6) . y Nd1 O4 2.362(6) . y Nd1 O5 2.427(6) . y Nd1 O6 2.388(5) . y Nd1 O7 2.545(6) . y Nd1 S1 3.136(2) . y Nd1 K1 3.667(2) . y K1 O1 2.873(6) . y K1 O2 2.523(6) . y K1 O5 2.686(6) . y K1 O8 2.600(9) . y K1 C12 2.906(8) . y K1 C132 3.225(9) . y K1 C413 3.250(10) . y K1 C13 3.343(8) . y K1 C61 3.392(15) . y K1 C11 3.422(8) . y K1 C22 3.509(9) . y S1 C11 1.764(8) . y S1 C21 1.783(7) . y O1 C12 1.307(9) . y O2 C22 1.318(9) . y O3 C31 1.243(10) . ? O4 C33 1.249(10) . ? O5 C41 1.269(9) . ? O6 C43 1.229(10) . ? O7 C54 1.404(11) . ? O7 C51 1.427(12) . ? O8 C61 1.416(14) . ? O8 C64 1.422(15) . ? C11 C12 1.402(10) . ? C11 C19 1.429(10) . ? C12 C13 1.446(12) . ? C13 C14 1.364(11) . ? C13 C130 1.538(11) . ? C14 C20 1.408(11) . ? C15 C16 1.370(11) . ? C15 C20 1.429(11) . ? C16 C17 1.403(12) . ? C16 C160 1.531(11) . ? C17 C18 1.379(11) . ? C18 C19 1.404(11) . ? C19 C20 1.405(12) . ? C21 C29 1.389(10) . ? C21 C22 1.393(11) . ? C22 C23 1.441(11) . ? C23 C24 1.363(11) . ? C23 C230 1.543(11) . ? C24 C30 1.395(11) . ? C25 C26 1.350(11) . ? C25 C30 1.413(11) . ? C26 C27 1.419(11) . ? C26 C260 1.501(11) . ? C26A C260 1.48(5) . ? C26B C260 1.38(4) . ? C26C C260 1.50(6) . ? C27 C28 1.344(11) . ? C28 C29 1.411(11) . ? C29 C30 1.425(10) . ? C31 C32 1.405(11) . ? C31 C310 1.557(13) . ? C32 C33 1.378(12) . ? C33 C330 1.535(11) . ? C41 C42 1.394(12) . ? C41 C410 1.535(13) . ? C42 C43 1.400(12) . ? C43 C430 1.558(12) . ? C51 C52 1.511(15) . ? C52 C53 1.456(18) . ? C53 C54 1.475(16) . ? C61 C62 1.493(19) . ? C62 C63 1.407(18) . ? C63 C64 1.525(17) . ? C71 C72 1.493(18) . ? C72 C73 1.475(18) . ? C73 C73 1.47(2) 2_878 ? C130 C131 1.488(13) . ? C130 C132 1.534(11) . ? C130 C133 1.570(13) . ? C160 C163 1.488(13) . ? C160 C162 1.518(12) . ? C160 C161 1.543(13) . ? C230 C233 1.517(14) . ? C230 C232 1.522(11) . ? C230 C231 1.537(12) . ? C260 C262 1.500(15) . ? C260 C261 1.534(14) . ? C260 C263 1.549(17) . ? C310 C313 1.487(13) . ? C310 C311 1.501(13) . ? C310 C312 1.508(14) . ? C330 C332 1.509(13) . ? C330 C331 1.518(12) . ? C330 C333 1.519(13) . ? C410 C413 1.491(13) . ? C410 C412 1.503(14) . ? C410 C411 1.511(15) . ? C430 C431 1.471(15) . ? C430 C432 1.487(14) . ? C430 C433 1.533(15) . ? 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 Nd1 O3 134.2(2) . . y O1 Nd1 O4 156.5(2) . . y O3 Nd1 O4 69.3(2) . . y O1 Nd1 O2 83.34(19) . . y O3 Nd1 O2 88.3(2) . . y O4 Nd1 O2 100.6(2) . . y O1 Nd1 O6 81.45(19) . . y O3 Nd1 O6 125.2(2) . . ? O4 Nd1 O6 82.0(2) . . ? O2 Nd1 O6 143.8(2) . . ? O1 Nd1 O5 79.87(19) . . ? O3 Nd1 O5 139.81(19) . . ? O4 Nd1 O5 79.1(2) . . ? O2 Nd1 O5 73.44(19) . . ? O6 Nd1 O5 71.67(19) . . ? O1 Nd1 O7 84.2(2) . . ? O3 Nd1 O7 72.9(2) . . ? O4 Nd1 O7 106.3(2) . . ? O2 Nd1 O7 138.56(18) . . ? O6 Nd1 O7 71.95(19) . . ? O5 Nd1 O7 141.99(19) . . ? O1 Nd1 S1 62.28(13) . . ? O3 Nd1 S1 73.91(14) . . ? O4 Nd1 S1 140.00(14) . . ? O2 Nd1 S1 62.61(13) . . ? O6 Nd1 S1 133.82(13) . . ? O5 Nd1 S1 123.59(14) . . ? O7 Nd1 S1 76.62(13) . . ? O1 Nd1 K1 51.56(15) . . ? O3 Nd1 K1 130.90(15) . . ? O4 Nd1 K1 117.30(16) . . ? O2 Nd1 K1 43.06(15) . . ? O6 Nd1 K1 103.51(16) . . ? O5 Nd1 K1 47.06(13) . . ? O7 Nd1 K1 135.27(15) . . ? S1 Nd1 K1 76.54(5) . . ? O2 K1 O8 128.0(2) . . y O2 K1 O5 66.81(17) . . y O8 K1 O5 158.1(2) . . y O2 K1 O1 70.28(18) . . y O8 K1 O1 130.8(2) . . y O5 K1 O1 66.36(16) . . y O2 K1 C12 79.3(2) . . ? O8 K1 C12 105.5(3) . . ? O5 K1 C12 92.5(2) . . ? O1 K1 C12 26.14(18) . . ? O2 K1 C132 126.0(2) . . ? O8 K1 C132 98.8(3) . . ? O5 K1 C132 78.8(2) . . ? O1 K1 C132 58.0(2) . . ? C12 K1 C132 61.5(2) . . ? O2 K1 C413 104.5(3) . . ? O8 K1 C413 103.8(3) . . ? O5 K1 C413 54.4(2) . . ? O1 K1 C413 115.2(2) . . ? C12 K1 C413 138.4(2) . . ? C132 K1 C413 85.6(2) . . ? O2 K1 C13 104.7(2) . . ? O8 K1 C13 87.6(2) . . ? O5 K1 C13 104.94(19) . . ? O1 K1 C13 44.2(2) . . ? C12 K1 C13 25.5(2) . . ? C132 K1 C13 45.5(2) . . ? C413 K1 C13 131.1(2) . . ? O2 K1 C61 106.1(3) . . ? O8 K1 C61 22.8(3) . . ? O5 K1 C61 166.8(3) . . ? O1 K1 C61 122.9(3) . . ? C12 K1 C61 97.1(3) . . ? C132 K1 C61 113.8(3) . . ? C413 K1 C61 120.3(3) . . ? C13 K1 C61 87.4(3) . . ? O2 K1 C11 66.18(18) . . ? O8 K1 C11 97.5(2) . . ? O5 K1 C11 103.92(19) . . ? O1 K1 C11 43.11(16) . . ? C12 K1 C11 23.85(19) . . ? C132 K1 C11 84.6(2) . . ? C413 K1 C11 157.7(2) . . ? C13 K1 C11 42.4(2) . . ? C61 K1 C11 82.0(3) . . ? O2 K1 C22 16.89(17) . . ? O8 K1 C22 111.6(2) . . ? O5 K1 C22 83.66(18) . . ? O1 K1 C22 77.37(19) . . ? C12 K1 C22 78.9(2) . . ? C132 K1 C22 135.3(2) . . ? C413 K1 C22 116.2(3) . . ? C13 K1 C22 102.3(2) . . ? C61 K1 C22 89.3(3) . . ? C11 K1 C22 60.35(19) . . ? O2 K1 Nd1 39.98(12) . . ? O8 K1 Nd1 160.4(2) . . ? O5 K1 Nd1 41.42(13) . . ? O1 K1 Nd1 39.16(12) . . ? C12 K1 Nd1 60.77(18) . . ? C132 K1 Nd1 87.0(2) . . ? C413 K1 Nd1 95.3(2) . . ? C13 K1 Nd1 83.08(17) . . ? C61 K1 Nd1 138.9(3) . . ? C11 K1 Nd1 64.25(14) . . ? C22 K1 Nd1 54.36(14) . . ? C11 S1 C21 108.4(4) . . y C11 S1 Nd1 96.8(2) . . ? C21 S1 Nd1 91.5(2) . . ? C12 O1 Nd1 136.8(5) . . ? C12 O1 K1 78.4(5) . . ? Nd1 O1 K1 89.28(17) . . ? C22 O2 Nd1 122.8(5) . . ? C22 O2 K1 129.3(5) . . ? Nd1 O2 K1 96.96(19) . . ? C31 O3 Nd1 138.9(6) . . ? C33 O4 Nd1 140.4(5) . . ? C41 O5 Nd1 134.2(6) . . ? C41 O5 K1 126.0(6) . . ? Nd1 O5 K1 91.52(16) . . ? C43 O6 Nd1 137.8(6) . . ? C54 O7 C51 109.0(8) . . ? C54 O7 Nd1 127.7(7) . . ? C51 O7 Nd1 120.8(5) . . ? C61 O8 C64 111.5(10) . . ? C61 O8 K1 111.9(9) . . ? C64 O8 K1 132.9(8) . . ? C12 C11 C19 121.4(8) . . ? C12 C11 S1 115.4(6) . . ? C19 C11 S1 122.6(6) . . ? C12 C11 K1 57.0(4) . . ? C19 C11 K1 111.7(5) . . ? S1 C11 K1 104.9(3) . . y O1 C12 C11 121.9(8) . . ? O1 C12 C13 119.6(7) . . ? C11 C12 C13 118.5(7) . . ? O1 C12 K1 75.5(4) . . y C11 C12 K1 99.2(5) . . ? C13 C12 K1 94.4(5) . . ? C14 C13 C12 119.3(7) . . ? C14 C13 C130 120.7(8) . . ? C12 C13 C130 120.0(7) . . ? C14 C13 K1 111.1(5) . . ? C12 C13 K1 60.1(4) . . ? C130 C13 K1 98.8(4) . . ? C13 C14 C20 122.7(9) . . ? C16 C15 C20 122.7(9) . . ? C15 C16 C17 115.9(8) . . ? C15 C16 C160 123.5(9) . . ? C17 C16 C160 120.6(7) . . ? C18 C17 C16 123.2(8) . . ? C17 C18 C19 121.2(9) . . ? C18 C19 C20 116.8(8) . . ? C18 C19 C11 124.5(8) . . ? C20 C19 C11 118.6(7) . . ? C19 C20 C14 119.4(8) . . ? C19 C20 C15 120.2(7) . . ? C14 C20 C15 120.4(9) . . ? C29 C21 C22 122.1(7) . . ? C29 C21 S1 118.8(6) . . ? C22 C21 S1 118.6(6) . . ? O2 C22 C21 119.9(7) . . ? O2 C22 C23 120.5(7) . . ? C21 C22 C23 119.5(7) . . ? C21 C22 K1 111.5(5) . . ? C23 C22 K1 118.0(6) . . ? C24 C23 C22 117.8(7) . . ? C24 C23 C230 120.7(7) . . ? C22 C23 C230 121.5(7) . . ? C23 C24 C30 123.0(7) . . ? C26 C25 C30 123.7(7) . . ? C25 C26 C27 115.9(7) . . ? C25 C26 C260 122.7(7) . . ? C27 C26 C260 121.4(7) . . ? C28 C27 C26 122.8(8) . . ? C27 C28 C29 122.2(8) . . ? C21 C29 C28 126.1(7) . . ? C21 C29 C30 117.8(7) . . ? C28 C29 C30 115.9(7) . . ? C24 C30 C25 120.8(7) . . ? C24 C30 C29 119.7(7) . . ? C25 C30 C29 119.5(7) . . ? O3 C31 C32 125.3(9) . . ? O3 C31 C310 114.8(7) . . ? C32 C31 C310 119.9(9) . . ? C33 C32 C31 122.3(9) . . ? O4 C33 C32 123.3(8) . . ? O4 C33 C330 115.8(8) . . ? C32 C33 C330 120.9(8) . . ? O5 C41 C42 122.6(8) . . ? O5 C41 C410 114.9(8) . . ? C42 C41 C410 122.5(8) . . ? C41 C42 C43 128.0(8) . . ? O6 C43 C42 123.1(8) . . ? O6 C43 C430 116.8(8) . . ? C42 C43 C430 120.1(8) . . ? O7 C51 C52 106.2(9) . . ? C53 C52 C51 102.5(12) . . ? C52 C53 C54 106.9(10) . . ? O7 C54 C53 107.5(10) . . ? O8 C61 C62 105.2(13) . . ? O8 C61 K1 45.3(6) . . ? C62 C61 K1 136.3(10) . . ? C63 C62 C61 106.3(13) . . ? C62 C63 C64 108.4(13) . . ? O8 C64 C63 100.2(11) . . ? C73 C72 C71 114.3(12) . . ? C73 C73 C72 115.3(16) 2_878 . ? C131 C130 C132 108.1(8) . . ? C131 C130 C13 111.6(7) . . ? C132 C130 C13 111.8(7) . . ? C131 C130 C133 108.5(7) . . ? C132 C130 C133 108.3(7) . . ? C13 C130 C133 108.4(8) . . ? C130 C132 K1 103.8(5) . . ? C163 C160 C162 110.3(9) . . ? C163 C160 C16 112.7(7) . . ? C162 C160 C16 109.9(7) . . ? C163 C160 C161 107.3(8) . . ? C162 C160 C161 108.5(8) . . ? C16 C160 C161 108.0(8) . . ? C233 C230 C232 106.9(8) . . ? C233 C230 C231 109.5(8) . . ? C232 C230 C231 109.3(7) . . ? C233 C230 C23 109.9(7) . . ? C232 C230 C23 112.3(7) . . ? C231 C230 C23 108.8(7) . . ? C26B C260 C26 108(2) . . ? C26A C260 C26 114(2) . . ? C262 C260 C26 113.3(8) . . ? C26A C260 C26C 110(3) . . ? C26 C260 C26C 99(3) . . ? C262 C260 C261 107.5(9) . . ? C26 C260 C261 109.5(9) . . ? C262 C260 C263 107.4(10) . . ? C26 C260 C263 108.1(8) . . ? C261 C260 C263 111.0(9) . . ? C313 C310 C311 110.3(9) . . ? C313 C310 C312 108.1(10) . . ? C311 C310 C312 110.7(9) . . ? C313 C310 C31 114.1(8) . . ? C311 C310 C31 106.7(9) . . ? C312 C310 C31 106.8(8) . . ? C332 C330 C331 108.4(8) . . ? C332 C330 C333 109.9(8) . . ? C331 C330 C333 109.6(9) . . ? C332 C330 C33 113.8(8) . . ? C331 C330 C33 107.7(7) . . ? C333 C330 C33 107.4(7) . . ? C413 C410 C412 108.6(9) . . ? C413 C410 C411 110.0(10) . . ? C412 C410 C411 107.5(9) . . ? C413 C410 C41 110.6(7) . . ? C412 C410 C41 107.1(9) . . ? C411 C410 C41 112.9(9) . . ? C410 C413 K1 110.8(6) . . ? C431 C430 C432 112.0(10) . . ? C431 C430 C433 110.3(9) . . ? C432 C430 C433 107.1(9) . . ? C431 C430 C43 106.9(9) . . ? C432 C430 C43 110.4(7) . . ? C433 C430 C43 110.3(9) . . ? _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.56 _refine_diff_density_min -2.78 _refine_diff_density_rms 0.15 #===END of CIF data_ndthon_compound_6 _database_code_depnum_ccdc_archive 'CCDC 298872' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H147 Li2 Nd O8 S2' _chemical_formula_weight 1843.54 _refine_special_details ; Disorder in one of the toluene molecules incorporated into the lattice. This was modelled over two sites except C9s which was common to both components. Following competitive refinement of the occupancies of the two components they were fixed to 0.65 and 0.35. Suitable geometry restraints were applied to this and the other toluene molecules. Carbon atoms of the disordered molecule were refined with isotropic adps. ; 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 16.773(3) _cell_length_b 24.082(4) _cell_length_c 25.628(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.527(3) _cell_angle_gamma 90.00 _cell_volume 10304(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8230 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.40 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3924 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.69280 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 15 _diffrn_reflns_number 44443 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.1238 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.66 _reflns_number_total 20802 _reflns_number_gt 13098 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0669P)^2^+0.0096P] 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 20802 _refine_ls_number_parameters 1115 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.099026(16) 0.406996(11) 0.711658(10) 0.01723(8) Uani 1 1 d . . . S1 S 0.24857(7) 0.36458(5) 0.66981(5) 0.0182(3) Uani 1 1 d . . . O1 O 0.0758(2) 0.36049(14) 0.63080(13) 0.0216(8) Uani 1 1 d . . . O1S O 0.0539(2) 0.21766(15) 0.65514(15) 0.0314(9) Uani 1 1 d . . . C1S C 0.1333(3) 0.1987(2) 0.6457(3) 0.0397(15) Uani 1 1 d . . . H1SA H 0.1745 0.2171 0.6701 0.048 Uiso 1 1 calc R . . H1SB H 0.1444 0.2072 0.6093 0.048 Uiso 1 1 calc R . . Li1 Li 0.0450(6) 0.2943(4) 0.6761(4) 0.029(2) Uani 1 1 d . . . S2 S 0.24115(7) 0.43709(5) 0.79104(5) 0.0190(3) Uani 1 1 d . . . O2 O 0.12653(19) 0.31210(14) 0.73037(13) 0.0204(8) Uani 1 1 d . . . O2S O 0.0870(2) 0.59612(16) 0.75772(15) 0.0349(9) Uani 1 1 d . . . C2S C 0.1340(4) 0.1366(2) 0.6548(3) 0.0399(15) Uani 1 1 d . . . H2SA H 0.1476 0.1276 0.6923 0.048 Uiso 1 1 calc R . . H2SB H 0.1722 0.1177 0.6336 0.048 Uiso 1 1 calc R . . Li2 Li 0.0672(5) 0.5234(4) 0.7313(4) 0.029(2) Uani 1 1 d . . . O3 O 0.0657(2) 0.45938(15) 0.78363(13) 0.0218(8) Uani 1 1 d . . . C3S C 0.0475(3) 0.1211(2) 0.6366(3) 0.0382(15) Uani 1 1 d . . . H3SA H 0.0394 0.1175 0.5979 0.046 Uiso 1 1 calc R . . H3SB H 0.0319 0.0860 0.6528 0.046 Uiso 1 1 calc R . . O4 O 0.15702(19) 0.49460(14) 0.69942(13) 0.0203(8) Uani 1 1 d . . . C4S C 0.0009(4) 0.1702(2) 0.6556(3) 0.0369(15) Uani 1 1 d . . . H4SA H -0.0485 0.1766 0.6320 0.044 Uiso 1 1 calc R . . H4SB H -0.0141 0.1633 0.6914 0.044 Uiso 1 1 calc R . . O5 O -0.00639(19) 0.47280(14) 0.68073(13) 0.0225(8) Uani 1 1 d . . . C5S C 0.0365(4) 0.6433(2) 0.7625(3) 0.0432(16) Uani 1 1 d . . . H5SA H -0.0196 0.6316 0.7648 0.052 Uiso 1 1 calc R . . H5SB H 0.0384 0.6684 0.7321 0.052 Uiso 1 1 calc R . . O6 O -0.0266(2) 0.35826(14) 0.70946(13) 0.0238(8) Uani 1 1 d . . . C6S C 0.0695(4) 0.6716(3) 0.8121(3) 0.061(2) Uani 1 1 d . . . H6SA H 0.0451 0.6563 0.8427 0.073 Uiso 1 1 calc R . . H6SB H 0.0594 0.7120 0.8101 0.073 Uiso 1 1 calc R . . C7S C 0.1587(4) 0.6592(3) 0.8158(3) 0.060(2) Uani 1 1 d . . . H7SA H 0.1892 0.6926 0.8070 0.072 Uiso 1 1 calc R . . H7SB H 0.1783 0.6468 0.8515 0.072 Uiso 1 1 calc R . . C8S C 0.1670(4) 0.6142(3) 0.7770(3) 0.0433(16) Uani 1 1 d . . . H8SA H 0.1957 0.6282 0.7476 0.052 Uiso 1 1 calc R . . H8SB H 0.1978 0.5829 0.7937 0.052 Uiso 1 1 calc R . . C11 C 0.2047(3) 0.3286(2) 0.61314(18) 0.0200(11) Uani 1 1 d . . . C12 C 0.1233(3) 0.3364(2) 0.59854(19) 0.0198(11) Uani 1 1 d . . . C13 C 0.0883(3) 0.3185(2) 0.54754(19) 0.0231(11) Uani 1 1 d . . . C14 C 0.1378(3) 0.2926(2) 0.5155(2) 0.0249(12) Uani 1 1 d . . . H14A H 0.1155 0.2808 0.4819 0.030 Uiso 1 1 calc R . . C15 C 0.2693(3) 0.2571(2) 0.4949(2) 0.0283(13) Uani 1 1 d . . . H15A H 0.2463 0.2466 0.4611 0.034 Uiso 1 1 calc R . . C16 C 0.3493(3) 0.2471(2) 0.5083(2) 0.0301(13) Uani 1 1 d . . . C17 C 0.3823(3) 0.2625(2) 0.5592(2) 0.0278(12) Uani 1 1 d . . . H17A H 0.4372 0.2550 0.5697 0.033 Uiso 1 1 calc R . . C18 C 0.3363(3) 0.2880(2) 0.5936(2) 0.0256(12) Uani 1 1 d . . . H18A H 0.3599 0.2978 0.6276 0.031 Uiso 1 1 calc R . . C19 C 0.2546(3) 0.3001(2) 0.57969(19) 0.0218(11) Uani 1 1 d . . . C20 C 0.2202(3) 0.2825(2) 0.5297(2) 0.0249(12) Uani 1 1 d . . . C21 C 0.2669(3) 0.3175(2) 0.72402(18) 0.0186(11) Uani 1 1 d . . . C22 C 0.2015(3) 0.2992(2) 0.74906(19) 0.0199(11) Uani 1 1 d . . . C23 C 0.2147(3) 0.2681(2) 0.7973(2) 0.0241(12) Uani 1 1 d . . . C24 C 0.2919(3) 0.2585(2) 0.8166(2) 0.0269(12) Uani 1 1 d . . . H24A H 0.3010 0.2381 0.8483 0.032 Uiso 1 1 calc R . . C25 C 0.4386(3) 0.2658(2) 0.81492(19) 0.0237(12) Uani 1 1 d . . . H25A H 0.4461 0.2444 0.8461 0.028 Uiso 1 1 calc R . . C26 C 0.5046(3) 0.2850(2) 0.79311(19) 0.0228(11) Uani 1 1 d . . . C27 C 0.4919(3) 0.3181(2) 0.74723(19) 0.0219(11) Uani 1 1 d . . . H27A H 0.5367 0.3324 0.7317 0.026 Uiso 1 1 calc R . . C28 C 0.4162(3) 0.3298(2) 0.72487(18) 0.0198(11) Uani 1 1 d . . . H28A H 0.4100 0.3528 0.6946 0.024 Uiso 1 1 calc R . . C29 C 0.3471(3) 0.3087(2) 0.74548(19) 0.0192(11) Uani 1 1 d . . . C30 C 0.3590(3) 0.2769(2) 0.79262(19) 0.0206(11) Uani 1 1 d . . . C31 C 0.1880(3) 0.4770(2) 0.83601(18) 0.0188(11) Uani 1 1 d . . . C32 C 0.1049(3) 0.4784(2) 0.82753(19) 0.0208(11) Uani 1 1 d . . . C33 C 0.0593(3) 0.5013(2) 0.86816(19) 0.0227(11) Uani 1 1 d . . . C34 C 0.1003(3) 0.5248(3) 0.9104(2) 0.0347(14) Uani 1 1 d . . . H34A H 0.0705 0.5419 0.9357 0.042 Uiso 1 1 calc R . . C35 C 0.2252(3) 0.5474(3) 0.9657(2) 0.0368(15) Uani 1 1 d . . . H35A H 0.1940 0.5650 0.9900 0.044 Uiso 1 1 calc R . . C36 C 0.3066(3) 0.5446(2) 0.9776(2) 0.0280(12) Uani 1 1 d . . . C37 C 0.3515(3) 0.5194(2) 0.9400(2) 0.0257(12) Uani 1 1 d . . . H37A H 0.4081 0.5170 0.9467 0.031 Uiso 1 1 calc R . . C38 C 0.3144(3) 0.4984(2) 0.89386(19) 0.0236(11) Uani 1 1 d . . . H38A H 0.3465 0.4822 0.8694 0.028 Uiso 1 1 calc R . . C39 C 0.2307(3) 0.5002(2) 0.88163(19) 0.0216(11) Uani 1 1 d . . . C40 C 0.1855(3) 0.5256(2) 0.9192(2) 0.0304(13) Uani 1 1 d . . . C41 C 0.2854(3) 0.4834(2) 0.74669(18) 0.0178(11) Uani 1 1 d . . . C42 C 0.2352(3) 0.5036(2) 0.70383(19) 0.0196(11) Uani 1 1 d . . . C43 C 0.2701(3) 0.5338(2) 0.6625(2) 0.0220(11) Uani 1 1 d . . . C44 C 0.3494(3) 0.5477(2) 0.6708(2) 0.0239(11) Uani 1 1 d . . . H44A H 0.3715 0.5709 0.6459 0.029 Uiso 1 1 calc R . . C45 C 0.4828(3) 0.5435(2) 0.7203(2) 0.0276(12) Uani 1 1 d . . . H45A H 0.5018 0.5695 0.6965 0.033 Uiso 1 1 calc R . . C46 C 0.5365(3) 0.5209(2) 0.7589(2) 0.0279(13) Uani 1 1 d . . . C47 C 0.5055(3) 0.4806(2) 0.7920(2) 0.0258(12) Uani 1 1 d . . . H47A H 0.5415 0.4623 0.8173 0.031 Uiso 1 1 calc R . . C48 C 0.4257(3) 0.4667(2) 0.7890(2) 0.0240(12) Uani 1 1 d . . . H48A H 0.4080 0.4396 0.8122 0.029 Uiso 1 1 calc R . . C49 C 0.3695(3) 0.4925(2) 0.75168(19) 0.0204(11) Uani 1 1 d . . . C50 C 0.4003(3) 0.5292(2) 0.7148(2) 0.0212(11) Uani 1 1 d . . . C51 C -0.0804(3) 0.4678(2) 0.6650(2) 0.0231(12) Uani 1 1 d . . . C52 C -0.1268(3) 0.4205(2) 0.6732(2) 0.0270(13) Uani 1 1 d . . . H52A H -0.1821 0.4227 0.6613 0.032 Uiso 1 1 calc R . . C53 C -0.1009(3) 0.3711(2) 0.6967(2) 0.0217(11) Uani 1 1 d . . . C130 C -0.0005(3) 0.3293(2) 0.52970(19) 0.0255(12) Uani 1 1 d . . . C131 C -0.0164(4) 0.3923(2) 0.5283(2) 0.0373(15) Uani 1 1 d . . . H13G H -0.0020 0.4080 0.5632 0.056 Uiso 1 1 calc R . . H13H H -0.0734 0.3991 0.5179 0.056 Uiso 1 1 calc R . . H13I H 0.0159 0.4098 0.5030 0.056 Uiso 1 1 calc R . . C132 C -0.0245(3) 0.3065(3) 0.4739(2) 0.0325(14) Uani 1 1 d . . . H13D H -0.0150 0.2664 0.4734 0.049 Uiso 1 1 calc R . . H13E H 0.0078 0.3247 0.4490 0.049 Uiso 1 1 calc R . . H13F H -0.0813 0.3140 0.4640 0.049 Uiso 1 1 calc R . . C133 C -0.0560(3) 0.3019(3) 0.5662(2) 0.0329(14) Uani 1 1 d . . . H13A H -0.0426 0.3154 0.6021 0.049 Uiso 1 1 calc R . . H13B H -0.0492 0.2615 0.5653 0.049 Uiso 1 1 calc R . . H13C H -0.1117 0.3114 0.5546 0.049 Uiso 1 1 calc R . . C160 C 0.4054(3) 0.2206(3) 0.4711(2) 0.0421(17) Uani 1 1 d . . . C161 C 0.4717(4) 0.2630(4) 0.4613(3) 0.079(3) Uani 1 1 d . . . H16G H 0.5018 0.2727 0.4947 0.119 Uiso 1 1 calc R . . H16H H 0.4472 0.2965 0.4450 0.119 Uiso 1 1 calc R . . H16I H 0.5082 0.2465 0.4379 0.119 Uiso 1 1 calc R . . C162 C 0.4434(5) 0.1685(4) 0.4960(3) 0.079(3) Uani 1 1 d . . . H16D H 0.4014 0.1415 0.5020 0.119 Uiso 1 1 calc R . . H16E H 0.4734 0.1780 0.5295 0.119 Uiso 1 1 calc R . . H16F H 0.4800 0.1523 0.4725 0.119 Uiso 1 1 calc R . . C163 C 0.3605(4) 0.2056(3) 0.4178(2) 0.0505(19) Uani 1 1 d . . . H16A H 0.3183 0.1786 0.4230 0.076 Uiso 1 1 calc R . . H16B H 0.3981 0.1896 0.3950 0.076 Uiso 1 1 calc R . . H16C H 0.3364 0.2392 0.4015 0.076 Uiso 1 1 calc R . . C230 C 0.1426(3) 0.2496(2) 0.8270(2) 0.0323(14) Uani 1 1 d . . . C231 C 0.0931(4) 0.2061(3) 0.7940(3) 0.0462(17) Uani 1 1 d . . . H23G H 0.1272 0.1743 0.7875 0.069 Uiso 1 1 calc R . . H23H H 0.0723 0.2226 0.7605 0.069 Uiso 1 1 calc R . . H23I H 0.0484 0.1937 0.8130 0.069 Uiso 1 1 calc R . . C232 C 0.0898(3) 0.2997(3) 0.8378(2) 0.0373(15) Uani 1 1 d . . . H23D H 0.0446 0.2873 0.8564 0.056 Uiso 1 1 calc R . . H23E H 0.0694 0.3169 0.8045 0.056 Uiso 1 1 calc R . . H23F H 0.1216 0.3269 0.8594 0.056 Uiso 1 1 calc R . . C233 C 0.1713(4) 0.2228(3) 0.8798(2) 0.0491(19) Uani 1 1 d . . . H23A H 0.2049 0.1905 0.8739 0.074 Uiso 1 1 calc R . . H23B H 0.1249 0.2109 0.8974 0.074 Uiso 1 1 calc R . . H23C H 0.2025 0.2499 0.9018 0.074 Uiso 1 1 calc R . . C260 C 0.5914(3) 0.2732(2) 0.8160(2) 0.0258(12) Uani 1 1 d . . . C261 C 0.5933(3) 0.2411(3) 0.8675(2) 0.0385(15) Uani 1 1 d . . . H26G H 0.6491 0.2344 0.8812 0.058 Uiso 1 1 calc R . . H26H H 0.5657 0.2055 0.8613 0.058 Uiso 1 1 calc R . . H26I H 0.5664 0.2628 0.8930 0.058 Uiso 1 1 calc R . . C262 C 0.6350(3) 0.3284(2) 0.8273(2) 0.0348(14) Uani 1 1 d . . . H26D H 0.6902 0.3211 0.8418 0.052 Uiso 1 1 calc R . . H26E H 0.6073 0.3497 0.8526 0.052 Uiso 1 1 calc R . . H26F H 0.6354 0.3496 0.7947 0.052 Uiso 1 1 calc R . . C263 C 0.6345(3) 0.2387(2) 0.7771(2) 0.0298(13) Uani 1 1 d . . . H26A H 0.6897 0.2315 0.7918 0.045 Uiso 1 1 calc R . . H26B H 0.6350 0.2591 0.7441 0.045 Uiso 1 1 calc R . . H26C H 0.6064 0.2033 0.7706 0.045 Uiso 1 1 calc R . . C330 C -0.0328(3) 0.4950(3) 0.8646(2) 0.0301(13) Uani 1 1 d . . . C331 C -0.0681(4) 0.5194(3) 0.9126(2) 0.052(2) Uani 1 1 d . . . H33G H -0.0565 0.5593 0.9149 0.078 Uiso 1 1 calc R . . H33H H -0.0442 0.5009 0.9444 0.078 Uiso 1 1 calc R . . H33I H -0.1262 0.5137 0.9093 0.078 Uiso 1 1 calc R . . C332 C -0.0530(4) 0.4323(3) 0.8628(3) 0.0419(16) Uani 1 1 d . . . H33D H -0.0315 0.4154 0.8323 0.063 Uiso 1 1 calc R . . H33E H -0.1113 0.4275 0.8600 0.063 Uiso 1 1 calc R . . H33F H -0.0291 0.4144 0.8949 0.063 Uiso 1 1 calc R . . C333 C -0.0743(3) 0.5238(3) 0.8159(2) 0.0380(15) Uani 1 1 d . . . H33A H -0.0614 0.5635 0.8171 0.057 Uiso 1 1 calc R . . H33B H -0.1324 0.5189 0.8152 0.057 Uiso 1 1 calc R . . H33C H -0.0556 0.5073 0.7843 0.057 Uiso 1 1 calc R . . C360 C 0.3468(4) 0.5699(3) 1.0287(2) 0.0379(15) Uani 1 1 d . . . C361 C 0.4276(4) 0.5438(3) 1.0444(2) 0.0480(18) Uani 1 1 d . . . H36G H 0.4208 0.5040 1.0506 0.072 Uiso 1 1 calc R . . H36H H 0.4519 0.5614 1.0765 0.072 Uiso 1 1 calc R . . H36I H 0.4625 0.5491 1.0162 0.072 Uiso 1 1 calc R . . C362 C 0.3571(4) 0.6324(3) 1.0189(3) 0.0457(17) Uani 1 1 d . . . H36D H 0.3904 0.6378 0.9900 0.069 Uiso 1 1 calc R . . H36E H 0.3829 0.6499 1.0507 0.069 Uiso 1 1 calc R . . H36F H 0.3044 0.6494 1.0099 0.069 Uiso 1 1 calc R . . C363 C 0.2946(4) 0.5605(3) 1.0740(2) 0.0438(17) Uani 1 1 d . . . H36A H 0.2887 0.5205 1.0798 0.066 Uiso 1 1 calc R . . H36B H 0.2417 0.5771 1.0651 0.066 Uiso 1 1 calc R . . H36C H 0.3202 0.5778 1.1059 0.066 Uiso 1 1 calc R . . C430 C 0.2192(3) 0.5481(2) 0.6115(2) 0.0284(12) Uani 1 1 d . . . C431 C 0.1768(4) 0.4960(3) 0.5868(2) 0.0405(16) Uani 1 1 d . . . H43G H 0.2169 0.4680 0.5801 0.061 Uiso 1 1 calc R . . H43H H 0.1459 0.5062 0.5538 0.061 Uiso 1 1 calc R . . H43I H 0.1406 0.4808 0.6111 0.061 Uiso 1 1 calc R . . C432 C 0.2704(4) 0.5717(3) 0.5703(2) 0.0362(14) Uani 1 1 d . . . H43D H 0.2980 0.6052 0.5840 0.054 Uiso 1 1 calc R . . H43E H 0.2359 0.5810 0.5384 0.054 Uiso 1 1 calc R . . H43F H 0.3100 0.5440 0.5620 0.054 Uiso 1 1 calc R . . C433 C 0.1551(3) 0.5921(3) 0.6215(2) 0.0393(14) Uani 1 1 d . . . H43A H 0.1814 0.6253 0.6372 0.059 Uiso 1 1 calc R . . H43B H 0.1187 0.5768 0.6456 0.059 Uiso 1 1 calc R . . H43C H 0.1246 0.6020 0.5883 0.059 Uiso 1 1 calc R . . C460 C 0.6269(3) 0.5348(3) 0.7651(2) 0.0345(14) Uani 1 1 d . . . C461 C 0.6477(4) 0.5781(3) 0.7254(3) 0.0481(18) Uani 1 1 d . . . H46G H 0.6331 0.5640 0.6898 0.072 Uiso 1 1 calc R . . H46H H 0.7053 0.5857 0.7301 0.072 Uiso 1 1 calc R . . H46I H 0.6180 0.6123 0.7306 0.072 Uiso 1 1 calc R . . C462 C 0.6742(3) 0.4815(3) 0.7568(3) 0.0428(16) Uani 1 1 d . . . H46D H 0.6598 0.4674 0.7212 0.064 Uiso 1 1 calc R . . H46E H 0.6613 0.4535 0.7824 0.064 Uiso 1 1 calc R . . H46F H 0.7317 0.4895 0.7614 0.064 Uiso 1 1 calc R . . C463 C 0.6504(3) 0.5567(3) 0.8208(3) 0.0465(18) Uani 1 1 d . . . H46A H 0.7077 0.5657 0.8248 0.070 Uiso 1 1 calc R . . H46B H 0.6392 0.5283 0.8464 0.070 Uiso 1 1 calc R . . H46C H 0.6193 0.5902 0.8267 0.070 Uiso 1 1 calc R . . C510 C -0.1201(3) 0.5179(2) 0.6351(2) 0.0267(12) Uani 1 1 d . . . C511 C -0.2072(5) 0.5100(4) 0.6168(4) 0.084(3) Uani 1 1 d . . . H51G H -0.2132 0.4782 0.5929 0.125 Uiso 1 1 calc R . . H51H H -0.2278 0.5435 0.5985 0.125 Uiso 1 1 calc R . . H51I H -0.2372 0.5031 0.6471 0.125 Uiso 1 1 calc R . . C512 C -0.1134(6) 0.5680(3) 0.6722(3) 0.078(3) Uani 1 1 d . . . H51D H -0.0570 0.5743 0.6845 0.117 Uiso 1 1 calc R . . H51E H -0.1438 0.5606 0.7022 0.117 Uiso 1 1 calc R . . H51F H -0.1352 0.6010 0.6534 0.117 Uiso 1 1 calc R . . C513 C -0.0731(5) 0.5310(3) 0.5894(3) 0.067(2) Uani 1 1 d . . . H51A H -0.0167 0.5365 0.6020 0.101 Uiso 1 1 calc R . . H51B H -0.0944 0.5648 0.5720 0.101 Uiso 1 1 calc R . . H51C H -0.0778 0.5000 0.5644 0.101 Uiso 1 1 calc R . . C530 C -0.1614(3) 0.3270(2) 0.7119(2) 0.0269(12) Uani 1 1 d . . . C531 C -0.2459(4) 0.3367(3) 0.6852(3) 0.0497(19) Uani 1 1 d . . . H53G H -0.2819 0.3078 0.6962 0.075 Uiso 1 1 calc R . . H53H H -0.2448 0.3353 0.6471 0.075 Uiso 1 1 calc R . . H53I H -0.2652 0.3732 0.6953 0.075 Uiso 1 1 calc R . . C532 C -0.1633(4) 0.3313(3) 0.7712(2) 0.0483(18) Uani 1 1 d . . . H53D H -0.1094 0.3249 0.7885 0.072 Uiso 1 1 calc R . . H53E H -0.2000 0.3033 0.7829 0.072 Uiso 1 1 calc R . . H53F H -0.1817 0.3684 0.7802 0.072 Uiso 1 1 calc R . . C533 C -0.1336(4) 0.2698(2) 0.6986(3) 0.0483(18) Uani 1 1 d . . . H53A H -0.0794 0.2637 0.7155 0.072 Uiso 1 1 calc R . . H53B H -0.1333 0.2665 0.6605 0.072 Uiso 1 1 calc R . . H53C H -0.1701 0.2421 0.7111 0.072 Uiso 1 1 calc R . . C9S C -0.2851(5) 0.2273(3) 0.5682(3) 0.068(2) Uiso 1 1 d D . . H9SA H -0.2407 0.2197 0.5489 0.081 Uiso 0.65 1 calc PR A 1 H9XA H -0.2444 0.2005 0.5646 0.081 Uiso 0.35 1 calc PR A 2 C10S C -0.3078(7) 0.1893(5) 0.6063(4) 0.063(3) Uiso 0.65 1 d PD B 1 H10A H -0.2789 0.1555 0.6119 0.076 Uiso 0.65 1 calc PR B 1 C11S C -0.3720(6) 0.2005(4) 0.6359(4) 0.054(3) Uiso 0.65 1 d PD B 1 H11A H -0.3875 0.1750 0.6614 0.065 Uiso 0.65 1 calc PR B 1 C12S C -0.4122(6) 0.2509(4) 0.6264(4) 0.038(2) Uiso 0.65 1 d PD B 1 H12A H -0.4548 0.2596 0.6469 0.046 Uiso 0.65 1 calc PR B 1 C13S C -0.3933(6) 0.2894(5) 0.5882(4) 0.044(3) Uiso 0.65 1 d PD B 1 H13J H -0.4226 0.3229 0.5820 0.052 Uiso 0.65 1 calc PR B 1 C14S C -0.3290(5) 0.2756(4) 0.5598(4) 0.044(3) Uiso 0.65 1 d PD B 1 C15S C -0.3005(6) 0.3134(4) 0.5205(4) 0.046(3) Uiso 0.65 1 d PD B 1 H15B H -0.2553 0.2963 0.5050 0.070 Uiso 0.65 1 calc PR B 1 H15C H -0.2831 0.3485 0.5374 0.070 Uiso 0.65 1 calc PR B 1 H15D H -0.3440 0.3207 0.4931 0.070 Uiso 0.65 1 calc PR B 1 C14X C -0.3449(10) 0.2253(9) 0.6022(7) 0.063(6) Uiso 0.35 1 d PD B 2 C11X C -0.3476(14) 0.3245(10) 0.5396(10) 0.080(8) Uiso 0.35 1 d PD B 2 H11B H -0.3453 0.3543 0.5155 0.096 Uiso 0.35 1 calc PR B 2 C12X C -0.4010(18) 0.3224(13) 0.5784(11) 0.106(11) Uiso 0.35 1 d PD B 2 H12B H -0.4361 0.3517 0.5860 0.127 Uiso 0.35 1 calc PR B 2 C13X C -0.3954(16) 0.2712(10) 0.6042(13) 0.077(8) Uiso 0.35 1 d PD B 2 H13K H -0.4345 0.2666 0.6283 0.092 Uiso 0.35 1 calc PR B 2 C10X C -0.2977(18) 0.2775(7) 0.5403(11) 0.098(10) Uiso 0.35 1 d PD B 2 H10B H -0.2616 0.2804 0.5141 0.118 Uiso 0.35 1 calc PR B 2 C15X C -0.330(2) 0.1737(10) 0.6328(12) 0.104(10) Uiso 0.35 1 d PD B 2 H15E H -0.2871 0.1526 0.6189 0.156 Uiso 0.35 1 calc PR B 2 H15F H -0.3793 0.1512 0.6302 0.156 Uiso 0.35 1 calc PR B 2 H15G H -0.3151 0.1830 0.6696 0.156 Uiso 0.35 1 calc PR B 2 C16S C 0.7103(5) 0.6028(3) 0.9810(3) 0.064(2) Uani 1 1 d . . . H16J H 0.7356 0.5843 0.9543 0.076 Uiso 1 1 calc R . . C17S C 0.6320(6) 0.6147(4) 0.9723(4) 0.075(3) Uani 1 1 d . . . H17B H 0.6034 0.6047 0.9398 0.090 Uiso 1 1 calc R . . C18S C 0.5929(5) 0.6414(4) 1.0098(5) 0.086(3) Uani 1 1 d . . . H18B H 0.5382 0.6517 1.0027 0.103 Uiso 1 1 calc R . . C19S C 0.6347(5) 0.6533(3) 1.0590(4) 0.074(3) Uani 1 1 d . . . H19A H 0.6083 0.6693 1.0865 0.089 Uiso 1 1 calc R . . C20S C 0.7153(5) 0.6410(3) 1.0655(3) 0.064(2) Uani 1 1 d . . . H20A H 0.7447 0.6500 1.0979 0.077 Uiso 1 1 calc R . . C21S C 0.7552(4) 0.6160(3) 1.0268(3) 0.0473(17) Uani 1 1 d D . . C22S C 0.8433(4) 0.6068(4) 1.0321(4) 0.080(3) Uani 1 1 d D . . H22A H 0.8591 0.5893 1.0002 0.120 Uiso 1 1 calc R . . H22B H 0.8579 0.5825 1.0622 0.120 Uiso 1 1 calc R . . H22C H 0.8709 0.6425 1.0376 0.120 Uiso 1 1 calc R . . C23S C 0.4327(5) 0.4261(3) 0.5924(3) 0.064(2) Uani 1 1 d . . . H23J H 0.3834 0.4214 0.6072 0.076 Uiso 1 1 calc R . . C24S C 0.5013(6) 0.4383(4) 0.6241(3) 0.072(2) Uani 1 1 d . . . H24B H 0.5001 0.4402 0.6610 0.086 Uiso 1 1 calc R . . C25S C 0.5717(6) 0.4477(5) 0.6022(4) 0.097(3) Uani 1 1 d . . . H25B H 0.6184 0.4572 0.6243 0.116 Uiso 1 1 calc R . . C26S C 0.5763(7) 0.4438(5) 0.5500(4) 0.100(4) Uani 1 1 d . . . H26J H 0.6259 0.4497 0.5359 0.120 Uiso 1 1 calc R . . C27S C 0.5071(6) 0.4309(4) 0.5166(4) 0.083(3) Uani 1 1 d . . . H27B H 0.5093 0.4293 0.4798 0.099 Uiso 1 1 calc R . . C28S C 0.4356(5) 0.4207(3) 0.5380(3) 0.066(2) Uani 1 1 d D . . C29S C 0.3632(6) 0.4105(4) 0.5026(4) 0.112(4) Uani 1 1 d D . . H29A H 0.3774 0.4080 0.4665 0.168 Uiso 1 1 calc R . . H29B H 0.3253 0.4410 0.5054 0.168 Uiso 1 1 calc R . . H29C H 0.3386 0.3755 0.5123 0.168 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01884(13) 0.01636(13) 0.01698(12) -0.00033(13) 0.00421(9) -0.00054(13) S1 0.0209(7) 0.0184(6) 0.0155(6) 0.0010(5) 0.0030(5) 0.0001(5) O1 0.0237(19) 0.0193(19) 0.0222(18) -0.0021(15) 0.0036(15) 0.0008(15) O1S 0.032(2) 0.018(2) 0.045(2) -0.0058(17) 0.0100(18) -0.0040(17) C1S 0.030(3) 0.030(4) 0.061(4) -0.009(3) 0.015(3) -0.006(3) Li1 0.031(5) 0.021(5) 0.038(5) -0.001(4) 0.015(4) -0.007(4) S2 0.0209(7) 0.0193(7) 0.0173(6) -0.0005(5) 0.0038(5) 0.0008(5) O2 0.0186(18) 0.021(2) 0.0227(18) 0.0039(15) 0.0089(14) 0.0015(15) O2S 0.033(2) 0.022(2) 0.049(2) -0.003(2) -0.0023(18) 0.0018(19) C2S 0.039(4) 0.025(3) 0.057(4) -0.006(3) 0.010(3) 0.001(3) Li2 0.023(5) 0.021(5) 0.042(6) -0.005(4) 0.002(4) -0.001(4) O3 0.0227(19) 0.027(2) 0.0165(17) -0.0048(15) 0.0076(14) -0.0036(15) C3S 0.039(4) 0.021(3) 0.057(4) 0.000(3) 0.014(3) -0.001(3) O4 0.0200(19) 0.0172(19) 0.0234(18) -0.0004(15) 0.0006(14) -0.0008(15) C4S 0.039(4) 0.025(3) 0.049(4) -0.006(3) 0.016(3) -0.006(3) O5 0.0172(19) 0.023(2) 0.027(2) 0.0044(15) -0.0027(15) -0.0001(15) C5S 0.037(4) 0.020(3) 0.072(5) 0.001(3) 0.001(3) 0.003(3) O6 0.031(2) 0.0159(19) 0.0257(19) -0.0014(15) 0.0087(16) -0.0059(16) C6S 0.044(4) 0.045(5) 0.094(6) -0.029(4) 0.007(4) 0.008(3) C7S 0.039(4) 0.053(5) 0.087(6) -0.033(4) 0.000(4) 0.005(3) C8S 0.035(4) 0.028(3) 0.064(5) -0.009(3) -0.005(3) 0.000(3) C11 0.028(3) 0.017(3) 0.016(2) 0.000(2) 0.004(2) -0.006(2) C12 0.024(3) 0.019(3) 0.018(3) 0.000(2) 0.008(2) 0.001(2) C13 0.026(3) 0.023(3) 0.020(3) 0.002(2) 0.001(2) -0.004(2) C14 0.026(3) 0.030(3) 0.018(3) -0.004(2) 0.002(2) -0.004(2) C15 0.026(3) 0.038(3) 0.022(3) -0.013(2) 0.006(2) -0.008(2) C16 0.025(3) 0.036(4) 0.031(3) -0.010(3) 0.014(2) 0.001(2) C17 0.018(3) 0.037(3) 0.030(3) -0.008(2) 0.005(2) -0.001(2) C18 0.026(3) 0.030(3) 0.021(3) -0.003(2) 0.005(2) -0.005(2) C19 0.020(3) 0.026(3) 0.020(3) 0.000(2) 0.006(2) -0.002(2) C20 0.027(3) 0.028(3) 0.020(3) -0.003(2) 0.005(2) -0.001(2) C21 0.021(3) 0.020(3) 0.015(2) -0.001(2) 0.004(2) 0.000(2) C22 0.024(3) 0.015(3) 0.021(3) 0.001(2) 0.007(2) 0.002(2) C23 0.029(3) 0.019(3) 0.027(3) 0.006(2) 0.015(2) 0.002(2) C24 0.036(3) 0.025(3) 0.020(3) 0.008(2) 0.008(2) 0.008(2) C25 0.023(3) 0.033(3) 0.015(2) 0.004(2) 0.004(2) 0.009(2) C26 0.029(3) 0.023(3) 0.017(3) -0.001(2) 0.004(2) 0.004(2) C27 0.023(3) 0.024(3) 0.020(3) 0.002(2) 0.008(2) 0.001(2) C28 0.026(3) 0.023(3) 0.011(2) 0.001(2) 0.003(2) -0.002(2) C29 0.026(3) 0.014(3) 0.018(2) -0.001(2) 0.005(2) 0.001(2) C30 0.014(3) 0.026(3) 0.024(3) 0.001(2) 0.015(2) 0.003(2) C31 0.023(3) 0.019(3) 0.015(2) -0.004(2) 0.003(2) 0.000(2) C32 0.024(3) 0.016(3) 0.024(3) 0.002(2) 0.005(2) 0.001(2) C33 0.019(3) 0.029(3) 0.020(3) -0.006(2) 0.006(2) -0.001(2) C34 0.027(3) 0.050(4) 0.029(3) -0.013(3) 0.013(2) 0.007(3) C35 0.036(3) 0.041(4) 0.034(3) -0.018(3) 0.006(3) 0.004(3) C36 0.030(3) 0.030(3) 0.024(3) -0.007(2) 0.001(2) -0.001(2) C37 0.024(3) 0.025(3) 0.028(3) 0.003(2) 0.001(2) -0.001(2) C38 0.027(3) 0.026(3) 0.018(3) -0.003(2) 0.006(2) 0.003(2) C39 0.025(3) 0.020(3) 0.021(3) 0.002(2) 0.006(2) -0.002(2) C40 0.030(3) 0.036(3) 0.026(3) -0.013(2) 0.002(2) 0.001(3) C41 0.022(3) 0.015(3) 0.017(2) 0.000(2) 0.005(2) 0.001(2) C42 0.025(3) 0.009(2) 0.026(3) -0.003(2) 0.008(2) 0.000(2) C43 0.025(3) 0.017(3) 0.024(3) 0.002(2) 0.005(2) 0.000(2) C44 0.029(3) 0.017(3) 0.027(3) 0.000(2) 0.010(2) -0.001(2) C45 0.022(3) 0.026(3) 0.036(3) -0.002(2) 0.009(2) -0.001(2) C46 0.018(3) 0.031(3) 0.035(3) -0.008(3) 0.003(2) -0.003(2) C47 0.022(3) 0.033(3) 0.023(3) -0.002(2) 0.000(2) 0.004(2) C48 0.022(3) 0.029(3) 0.021(3) -0.005(2) 0.002(2) 0.000(2) C49 0.023(3) 0.016(3) 0.022(3) -0.006(2) 0.004(2) 0.003(2) C50 0.023(3) 0.015(3) 0.027(3) -0.004(2) 0.008(2) 0.000(2) C51 0.027(3) 0.023(3) 0.021(3) -0.002(2) 0.006(2) 0.005(2) C52 0.023(3) 0.023(3) 0.034(3) 0.003(2) 0.001(2) -0.002(2) C53 0.016(3) 0.027(3) 0.023(3) -0.001(2) 0.008(2) -0.006(2) C130 0.026(3) 0.036(3) 0.015(3) -0.003(2) 0.005(2) -0.001(2) C131 0.038(4) 0.040(4) 0.033(3) -0.003(3) -0.003(3) 0.011(3) C132 0.027(3) 0.045(4) 0.024(3) -0.004(3) -0.002(2) 0.001(3) C133 0.021(3) 0.046(4) 0.031(3) -0.003(3) 0.001(2) -0.004(3) C160 0.029(3) 0.062(5) 0.037(4) -0.025(3) 0.012(3) -0.002(3) C161 0.051(5) 0.130(8) 0.062(5) -0.053(5) 0.037(4) -0.040(5) C162 0.071(6) 0.099(7) 0.065(5) -0.046(5) -0.006(4) 0.036(5) C163 0.041(4) 0.082(6) 0.032(3) -0.030(4) 0.017(3) -0.005(4) C230 0.025(3) 0.036(4) 0.038(3) 0.016(3) 0.017(3) 0.010(3) C231 0.038(4) 0.039(4) 0.063(5) 0.021(3) 0.015(3) -0.008(3) C232 0.032(3) 0.048(4) 0.035(3) 0.012(3) 0.020(3) 0.012(3) C233 0.040(4) 0.064(5) 0.047(4) 0.037(4) 0.026(3) 0.015(3) C260 0.021(3) 0.034(3) 0.022(3) -0.001(2) 0.002(2) 0.001(2) C261 0.026(3) 0.057(4) 0.032(3) 0.014(3) -0.004(3) 0.002(3) C262 0.032(3) 0.035(4) 0.035(3) -0.007(3) -0.011(3) -0.001(3) C263 0.020(3) 0.035(3) 0.035(3) 0.002(3) 0.008(2) 0.001(2) C330 0.017(3) 0.043(4) 0.031(3) -0.006(3) 0.009(2) -0.004(2) C331 0.028(3) 0.093(6) 0.037(4) -0.028(4) 0.011(3) 0.000(4) C332 0.036(4) 0.042(4) 0.049(4) -0.001(3) 0.013(3) -0.010(3) C333 0.030(3) 0.042(4) 0.042(4) -0.002(3) 0.000(3) 0.006(3) C360 0.038(4) 0.046(4) 0.029(3) -0.010(3) -0.003(3) -0.003(3) C361 0.042(4) 0.069(5) 0.030(3) -0.014(3) -0.010(3) 0.003(4) C362 0.062(5) 0.036(4) 0.038(4) -0.011(3) 0.001(3) -0.009(3) C363 0.054(4) 0.054(4) 0.022(3) -0.008(3) -0.004(3) -0.012(3) C430 0.032(3) 0.028(3) 0.026(3) 0.008(2) 0.005(2) -0.003(2) C431 0.052(4) 0.039(4) 0.028(3) 0.008(3) -0.006(3) -0.008(3) C432 0.048(4) 0.034(3) 0.026(3) 0.010(3) 0.006(3) -0.005(3) C433 0.035(3) 0.037(4) 0.045(3) 0.016(3) 0.001(3) 0.004(3) C460 0.022(3) 0.032(3) 0.050(4) -0.006(3) 0.004(3) 0.001(2) C461 0.024(3) 0.043(4) 0.078(5) 0.010(3) 0.009(3) -0.005(3) C462 0.026(3) 0.044(4) 0.059(4) -0.010(3) 0.014(3) 0.004(3) C463 0.024(3) 0.051(4) 0.063(5) -0.019(4) -0.006(3) 0.000(3) C510 0.024(3) 0.027(3) 0.029(3) 0.010(2) 0.003(2) 0.004(2) C511 0.057(5) 0.069(6) 0.118(8) 0.053(6) -0.027(5) -0.004(4) C512 0.117(8) 0.053(5) 0.060(5) 0.002(4) -0.009(5) 0.044(5) C513 0.078(6) 0.064(6) 0.063(5) 0.036(4) 0.024(4) 0.021(4) C530 0.023(3) 0.029(3) 0.030(3) 0.001(2) 0.007(2) -0.005(2) C531 0.032(4) 0.049(4) 0.066(5) 0.016(4) -0.007(3) -0.017(3) C532 0.054(4) 0.056(5) 0.038(4) -0.006(3) 0.020(3) -0.024(4) C533 0.054(4) 0.023(3) 0.074(5) -0.010(3) 0.035(4) -0.012(3) C16S 0.074(6) 0.055(5) 0.061(5) 0.010(4) -0.003(4) -0.015(4) C17S 0.076(7) 0.058(6) 0.088(7) 0.016(5) -0.011(5) 0.000(5) C18S 0.045(5) 0.058(6) 0.150(10) 0.011(6) -0.010(6) -0.001(4) C19S 0.059(6) 0.054(5) 0.110(8) -0.012(5) 0.018(5) -0.001(4) C20S 0.066(6) 0.063(5) 0.065(5) -0.005(4) 0.004(4) -0.012(4) C21S 0.052(4) 0.030(4) 0.059(5) 0.010(3) 0.002(4) 0.000(3) C22S 0.059(5) 0.065(6) 0.119(8) 0.010(5) 0.026(5) -0.001(4) C23S 0.078(6) 0.050(5) 0.068(5) 0.007(4) 0.036(5) -0.003(4) C24S 0.096(7) 0.066(6) 0.056(5) -0.018(4) 0.019(5) -0.021(5) C25S 0.098(8) 0.127(10) 0.068(6) -0.032(6) 0.022(6) -0.044(7) C26S 0.102(8) 0.123(9) 0.083(7) -0.014(7) 0.049(6) -0.052(7) C27S 0.103(8) 0.084(7) 0.067(6) 0.014(5) 0.037(6) 0.006(6) C28S 0.095(7) 0.044(5) 0.059(5) 0.004(4) 0.012(5) -0.004(4) C29S 0.125(9) 0.072(7) 0.136(10) 0.012(7) -0.008(8) -0.015(7) _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 O3 2.346(3) . ? Nd1 O1 2.355(3) . ? Nd1 O4 2.357(3) . ? Nd1 O2 2.371(3) . ? Nd1 O6 2.408(3) . ? Nd1 O5 2.449(3) . ? Nd1 Li2 2.906(9) . ? Nd1 Li1 2.977(9) . ? Nd1 S1 3.0006(13) . ? Nd1 S2 3.0680(13) . ? S1 C11 1.787(5) . ? S1 C21 1.797(5) . ? O1 C12 1.335(6) . ? O1 Li1 2.067(10) . ? O1S C4S 1.449(6) . ? O1S C1S 1.451(7) . ? O1S Li1 1.932(10) . ? C1S C2S 1.513(8) . ? Li1 O2 1.904(10) . ? Li1 O6 2.178(10) . ? Li1 C12 2.685(10) . ? S2 C31 1.801(5) . ? S2 C41 1.802(5) . ? O2 C22 1.339(6) . ? O2S C5S 1.430(7) . ? O2S C8S 1.451(7) . ? O2S Li2 1.896(10) . ? C2S C3S 1.527(8) . ? Li2 O4 1.911(10) . ? Li2 O3 2.045(10) . ? Li2 O5 2.092(10) . ? Li2 C32 2.713(11) . ? O3 C32 1.329(6) . ? C3S C4S 1.523(8) . ? O4 C42 1.324(6) . ? O5 C51 1.274(6) . ? C5S C6S 1.499(9) . ? O6 C53 1.295(6) . ? C6S C7S 1.519(9) . ? C7S C8S 1.486(9) . ? C11 C12 1.392(7) . ? C11 C19 1.431(7) . ? C12 C13 1.446(7) . ? C13 C14 1.372(7) . ? C13 C130 1.539(7) . ? C14 C20 1.415(7) . ? C15 C16 1.374(7) . ? C15 C20 1.410(7) . ? C16 C17 1.417(7) . ? C16 C160 1.539(7) . ? C17 C18 1.372(7) . ? C18 C19 1.412(7) . ? C19 C20 1.419(7) . ? C21 C22 1.394(7) . ? C21 C29 1.419(7) . ? C22 C23 1.446(7) . ? C23 C24 1.360(7) . ? C23 C230 1.553(7) . ? C24 C30 1.405(7) . ? C25 C26 1.367(7) . ? C25 C30 1.427(7) . ? C26 C27 1.419(7) . ? C26 C260 1.543(7) . ? C27 C28 1.371(7) . ? C28 C29 1.412(7) . ? C29 C30 1.429(7) . ? C31 C32 1.391(7) . ? C31 C39 1.425(7) . ? C32 C33 1.458(7) . ? C33 C34 1.350(7) . ? C33 C330 1.546(7) . ? C34 C40 1.425(7) . ? C35 C36 1.373(8) . ? C35 C40 1.409(7) . ? C36 C37 1.414(7) . ? C36 C360 1.540(7) . ? C37 C38 1.379(7) . ? C38 C39 1.409(7) . ? C39 C40 1.422(7) . ? C41 C42 1.404(7) . ? C41 C49 1.422(7) . ? C42 C43 1.453(7) . ? C43 C44 1.368(7) . ? C43 C430 1.532(7) . ? C44 C50 1.419(7) . ? C45 C46 1.384(8) . ? C45 C50 1.418(7) . ? C46 C47 1.421(8) . ? C46 C460 1.546(7) . ? C47 C48 1.374(7) . ? C48 C49 1.419(7) . ? C49 C50 1.428(7) . ? C51 C52 1.407(7) . ? C51 C510 1.544(7) . ? C52 C53 1.384(7) . ? C53 C530 1.544(7) . ? C130 C133 1.530(7) . ? C130 C131 1.540(8) . ? C130 C132 1.548(7) . ? C160 C162 1.520(11) . ? C160 C163 1.538(8) . ? C160 C161 1.548(10) . ? C230 C233 1.535(8) . ? C230 C231 1.537(9) . ? C230 C232 1.538(8) . ? C260 C261 1.528(7) . ? C260 C262 1.531(8) . ? C260 C263 1.531(7) . ? C330 C331 1.534(8) . ? C330 C333 1.536(8) . ? C330 C332 1.546(8) . ? C360 C361 1.513(8) . ? C360 C363 1.538(8) . ? C360 C362 1.539(9) . ? C430 C432 1.533(7) . ? C430 C431 1.547(8) . ? C430 C433 1.548(8) . ? C460 C461 1.520(9) . ? C460 C462 1.534(8) . ? C460 C463 1.538(8) . ? C510 C511 1.503(9) . ? C510 C513 1.506(8) . ? C510 C512 1.532(9) . ? C530 C533 1.503(8) . ? C530 C532 1.527(8) . ? C530 C531 1.531(8) . ? C9S C14S 1.383(7) . ? C9S C14X 1.392(8) . ? C9S C10X 1.410(8) . ? C9S C10S 1.416(7) . ? C10S C11S 1.403(7) . ? C11S C12S 1.396(7) . ? C12S C13S 1.407(8) . ? C13S C14S 1.396(7) . ? C14S C15S 1.473(9) . ? C14X C13X 1.396(8) . ? C14X C15X 1.476(10) . ? C11X C12X 1.402(8) . ? C11X C10X 1.406(8) . ? C12X C13X 1.399(8) . ? C16S C17S 1.342(11) . ? C16S C21S 1.368(10) . ? C17S C18S 1.375(13) . ? C18S C19S 1.413(13) . ? C19S C20S 1.377(11) . ? C20S C21S 1.388(10) . ? C21S C22S 1.487(8) . ? C23S C24S 1.375(11) . ? C23S C28S 1.406(11) . ? C24S C25S 1.373(12) . ? C25S C26S 1.350(12) . ? C26S C27S 1.408(13) . ? C27S C28S 1.387(12) . ? C28S C29S 1.464(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 O3 Nd1 O1 156.33(12) . . ? O3 Nd1 O4 75.87(12) . . ? O1 Nd1 O4 110.12(12) . . ? O3 Nd1 O2 114.56(12) . . ? O1 Nd1 O2 74.46(12) . . ? O4 Nd1 O2 144.58(11) . . ? O3 Nd1 O6 90.35(11) . . ? O1 Nd1 O6 71.19(11) . . ? O4 Nd1 O6 143.58(12) . . ? O2 Nd1 O6 71.81(12) . . ? O3 Nd1 O5 71.77(12) . . ? O1 Nd1 O5 88.28(12) . . ? O4 Nd1 O5 70.85(11) . . ? O2 Nd1 O5 144.05(11) . . ? O6 Nd1 O5 72.83(12) . . ? O3 Nd1 Li2 44.3(2) . . ? O1 Nd1 Li2 126.4(2) . . ? O4 Nd1 Li2 40.9(2) . . ? O2 Nd1 Li2 158.4(2) . . ? O6 Nd1 Li2 107.41(19) . . ? O5 Nd1 Li2 45.00(19) . . ? O3 Nd1 Li1 129.97(19) . . ? O1 Nd1 Li1 43.7(2) . . ? O4 Nd1 Li1 153.25(19) . . ? O2 Nd1 Li1 39.7(2) . . ? O6 Nd1 Li1 46.24(19) . . ? O5 Nd1 Li1 107.6(2) . . ? Li2 Nd1 Li1 151.3(3) . . ? O3 Nd1 S1 137.28(9) . . ? O1 Nd1 S1 66.20(8) . . ? O4 Nd1 S1 83.52(8) . . ? O2 Nd1 S1 65.87(8) . . ? O6 Nd1 S1 125.84(9) . . ? O5 Nd1 S1 134.99(8) . . ? Li2 Nd1 S1 124.33(18) . . ? Li1 Nd1 S1 79.67(18) . . ? O3 Nd1 S2 65.19(8) . . ? O1 Nd1 S2 138.41(8) . . ? O4 Nd1 S2 64.69(8) . . ? O2 Nd1 S2 88.28(9) . . ? O6 Nd1 S2 138.85(9) . . ? O5 Nd1 S2 123.54(8) . . ? Li2 Nd1 S2 78.55(18) . . ? Li1 Nd1 S2 127.79(19) . . ? S1 Nd1 S2 72.21(3) . . ? C11 S1 C21 110.4(2) . . ? C11 S1 Nd1 99.33(17) . . ? C21 S1 Nd1 91.45(16) . . ? C12 O1 Li1 102.1(4) . . ? C12 O1 Nd1 133.9(3) . . ? Li1 O1 Nd1 84.4(3) . . ? C4S O1S C1S 109.1(4) . . ? C4S O1S Li1 133.5(4) . . ? C1S O1S Li1 116.3(4) . . ? O1S C1S C2S 106.1(5) . . ? O2 Li1 O1S 110.4(5) . . ? O2 Li1 O1 92.0(4) . . ? O1S Li1 O1 123.4(5) . . ? O2 Li1 O6 86.5(4) . . ? O1S Li1 O6 147.7(5) . . ? O1 Li1 O6 81.5(4) . . ? O2 Li1 C12 95.0(4) . . ? O1S Li1 C12 95.7(4) . . ? O1 Li1 C12 29.08(18) . . ? O6 Li1 C12 110.6(4) . . ? O2 Li1 Nd1 52.7(2) . . ? O1S Li1 Nd1 157.9(5) . . ? O1 Li1 Nd1 51.9(2) . . ? O6 Li1 Nd1 53.0(2) . . ? C12 Li1 Nd1 74.1(2) . . ? C31 S2 C41 109.4(2) . . ? C31 S2 Nd1 98.61(16) . . ? C41 S2 Nd1 93.94(16) . . ? C22 O2 Li1 142.5(4) . . ? C22 O2 Nd1 116.9(3) . . ? Li1 O2 Nd1 87.5(3) . . ? C5S O2S C8S 105.5(4) . . ? C5S O2S Li2 132.8(4) . . ? C8S O2S Li2 121.6(4) . . ? C1S C2S C3S 101.6(5) . . ? O2S Li2 O4 111.7(5) . . ? O2S Li2 O3 118.3(5) . . ? O4 Li2 O3 93.8(4) . . ? O2S Li2 O5 146.3(5) . . ? O4 Li2 O5 88.1(4) . . ? O3 Li2 O5 85.6(4) . . ? O2S Li2 C32 91.5(4) . . ? O4 Li2 C32 96.9(4) . . ? O3 Li2 C32 28.23(19) . . ? O5 Li2 C32 113.7(4) . . ? O2S Li2 Nd1 157.5(4) . . ? O4 Li2 Nd1 53.9(2) . . ? O3 Li2 Nd1 53.2(2) . . ? O5 Li2 Nd1 55.9(2) . . ? C32 Li2 Nd1 75.0(3) . . ? C32 O3 Li2 105.0(4) . . ? C32 O3 Nd1 135.7(3) . . ? Li2 O3 Nd1 82.6(3) . . ? C4S C3S C2S 102.4(5) . . ? C42 O4 Li2 136.0(4) . . ? C42 O4 Nd1 123.6(3) . . ? Li2 O4 Nd1 85.1(3) . . ? O1S C4S C3S 106.0(4) . . ? C51 O5 Li2 138.6(4) . . ? C51 O5 Nd1 133.9(3) . . ? Li2 O5 Nd1 79.1(3) . . ? O2S C5S C6S 105.1(5) . . ? C53 O6 Li1 128.5(4) . . ? C53 O6 Nd1 135.1(3) . . ? Li1 O6 Nd1 80.8(3) . . ? C5S C6S C7S 104.1(5) . . ? C8S C7S C6S 104.8(5) . . ? O2S C8S C7S 107.7(5) . . ? C12 C11 C19 121.3(4) . . ? C12 C11 S1 118.0(4) . . ? C19 C11 S1 120.0(4) . . ? O1 C12 C11 121.3(4) . . ? O1 C12 C13 118.3(4) . . ? C11 C12 C13 120.3(4) . . ? O1 C12 Li1 48.8(3) . . ? C11 C12 Li1 106.7(4) . . ? C13 C12 Li1 111.8(4) . . ? C14 C13 C12 117.4(5) . . ? C14 C13 C130 121.5(5) . . ? C12 C13 C130 121.1(4) . . ? C13 C14 C20 123.8(5) . . ? C16 C15 C20 122.4(5) . . ? C15 C16 C17 117.9(5) . . ? C15 C16 C160 124.0(5) . . ? C17 C16 C160 118.1(5) . . ? C18 C17 C16 121.0(5) . . ? C17 C18 C19 121.5(5) . . ? C18 C19 C20 117.9(5) . . ? C18 C19 C11 123.9(5) . . ? C20 C19 C11 118.3(4) . . ? C15 C20 C14 121.9(5) . . ? C15 C20 C19 119.2(5) . . ? C14 C20 C19 118.9(5) . . ? C22 C21 C29 122.3(5) . . ? C22 C21 S1 118.1(4) . . ? C29 C21 S1 118.6(4) . . ? O2 C22 C21 121.1(4) . . ? O2 C22 C23 119.1(4) . . ? C21 C22 C23 119.7(5) . . ? C24 C23 C22 117.3(5) . . ? C24 C23 C230 122.2(5) . . ? C22 C23 C230 120.4(5) . . ? C23 C24 C30 124.3(5) . . ? C26 C25 C30 122.5(5) . . ? C25 C26 C27 117.7(5) . . ? C25 C26 C260 123.6(5) . . ? C27 C26 C260 118.6(5) . . ? C28 C27 C26 121.4(5) . . ? C27 C28 C29 122.0(5) . . ? C28 C29 C21 125.7(5) . . ? C28 C29 C30 117.2(4) . . ? C21 C29 C30 117.1(4) . . ? C24 C30 C25 121.7(5) . . ? C24 C30 C29 119.1(4) . . ? C25 C30 C29 119.2(4) . . ? C32 C31 C39 122.4(4) . . ? C32 C31 S2 117.6(4) . . ? C39 C31 S2 119.6(4) . . ? O3 C32 C31 122.1(4) . . ? O3 C32 C33 119.0(4) . . ? C31 C32 C33 119.0(4) . . ? O3 C32 Li2 46.7(3) . . ? C31 C32 Li2 107.1(4) . . ? C33 C32 Li2 114.0(4) . . ? C34 C33 C32 118.1(5) . . ? C34 C33 C330 121.1(5) . . ? C32 C33 C330 120.7(4) . . ? C33 C34 C40 123.9(5) . . ? C36 C35 C40 123.2(5) . . ? C35 C36 C37 117.0(5) . . ? C35 C36 C360 120.9(5) . . ? C37 C36 C360 122.0(5) . . ? C38 C37 C36 121.0(5) . . ? C37 C38 C39 122.5(5) . . ? C38 C39 C40 116.6(5) . . ? C38 C39 C31 125.6(5) . . ? C40 C39 C31 117.8(5) . . ? C35 C40 C39 119.6(5) . . ? C35 C40 C34 121.6(5) . . ? C39 C40 C34 118.7(5) . . ? C42 C41 C49 122.1(4) . . ? C42 C41 S2 117.1(4) . . ? C49 C41 S2 120.2(4) . . ? O4 C42 C41 121.6(4) . . ? O4 C42 C43 119.0(4) . . ? C41 C42 C43 119.3(4) . . ? C44 C43 C42 117.6(5) . . ? C44 C43 C430 122.1(5) . . ? C42 C43 C430 120.3(4) . . ? C43 C44 C50 123.2(5) . . ? C46 C45 C50 122.5(5) . . ? C45 C46 C47 116.4(5) . . ? C45 C46 C460 123.6(5) . . ? C47 C46 C460 119.9(5) . . ? C48 C47 C46 122.9(5) . . ? C47 C48 C49 120.8(5) . . ? C48 C49 C41 125.7(5) . . ? C48 C49 C50 117.2(5) . . ? C41 C49 C50 117.1(4) . . ? C45 C50 C44 120.6(5) . . ? C45 C50 C49 119.7(5) . . ? C44 C50 C49 119.5(5) . . ? O5 C51 C52 124.4(5) . . ? O5 C51 C510 116.3(5) . . ? C52 C51 C510 119.3(5) . . ? C53 C52 C51 127.4(5) . . ? O6 C53 C52 124.7(5) . . ? O6 C53 C530 114.3(5) . . ? C52 C53 C530 121.0(5) . . ? C133 C130 C13 112.0(4) . . ? C133 C130 C131 108.9(5) . . ? C13 C130 C131 109.5(5) . . ? C133 C130 C132 107.1(4) . . ? C13 C130 C132 111.9(4) . . ? C131 C130 C132 107.4(4) . . ? C162 C160 C163 109.2(6) . . ? C162 C160 C16 109.8(6) . . ? C163 C160 C16 111.8(5) . . ? C162 C160 C161 109.5(6) . . ? C163 C160 C161 108.0(6) . . ? C16 C160 C161 108.6(5) . . ? C233 C230 C231 107.8(5) . . ? C233 C230 C232 107.9(5) . . ? C231 C230 C232 110.1(5) . . ? C233 C230 C23 111.0(5) . . ? C231 C230 C23 109.3(5) . . ? C232 C230 C23 110.6(5) . . ? C261 C260 C262 107.8(5) . . ? C261 C260 C263 108.3(5) . . ? C262 C260 C263 110.3(5) . . ? C261 C260 C26 111.2(4) . . ? C262 C260 C26 109.2(5) . . ? C263 C260 C26 109.9(4) . . ? C331 C330 C333 107.4(5) . . ? C331 C330 C332 107.3(5) . . ? C333 C330 C332 109.6(5) . . ? C331 C330 C33 112.1(5) . . ? C333 C330 C33 112.1(5) . . ? C332 C330 C33 108.2(5) . . ? C361 C360 C363 107.4(5) . . ? C361 C360 C362 109.8(6) . . ? C363 C360 C362 110.4(5) . . ? C361 C360 C36 111.7(5) . . ? C363 C360 C36 110.4(5) . . ? C362 C360 C36 107.2(5) . . ? C43 C430 C432 111.6(5) . . ? C43 C430 C431 111.3(4) . . ? C432 C430 C431 106.6(5) . . ? C43 C430 C433 110.5(5) . . ? C432 C430 C433 107.8(5) . . ? C431 C430 C433 108.9(5) . . ? C461 C460 C462 109.0(5) . . ? C461 C460 C463 109.3(5) . . ? C462 C460 C463 109.1(5) . . ? C461 C460 C46 111.4(5) . . ? C462 C460 C46 108.7(5) . . ? C463 C460 C46 109.2(5) . . ? C511 C510 C513 110.5(6) . . ? C511 C510 C512 107.6(6) . . ? C513 C510 C512 107.8(6) . . ? C511 C510 C51 114.5(5) . . ? C513 C510 C51 108.5(5) . . ? C512 C510 C51 107.8(5) . . ? C533 C530 C532 108.9(5) . . ? C533 C530 C531 109.4(5) . . ? C532 C530 C531 109.1(5) . . ? C533 C530 C53 110.3(4) . . ? C532 C530 C53 106.3(4) . . ? C531 C530 C53 112.7(5) . . ? C14S C9S C14X 73.8(10) . . ? C14S C9S C10X 31.6(12) . . ? C14X C9S C10X 105.3(16) . . ? C14S C9S C10S 118.4(8) . . ? C14X C9S C10S 44.6(9) . . ? C10X C9S C10S 149.9(15) . . ? C11S C10S C9S 121.3(10) . . ? C12S C11S C10S 117.1(10) . . ? C11S C12S C13S 123.8(10) . . ? C14S C13S C12S 116.2(10) . . ? C9S C14S C13S 123.1(9) . . ? C9S C14S C15S 115.0(8) . . ? C13S C14S C15S 121.8(8) . . ? C9S C14X C13X 118(2) . . ? C9S C14X C15X 105.6(17) . . ? C13X C14X C15X 136(2) . . ? C12X C11X C10X 112(3) . . ? C13X C12X C11X 110(3) . . ? C14X C13X C12X 134(3) . . ? C11X C10X C9S 139(3) . . ? C17S C16S C21S 122.9(9) . . ? C16S C17S C18S 120.6(9) . . ? C17S C18S C19S 119.3(8) . . ? C20S C19S C18S 117.5(8) . . ? C19S C20S C21S 122.8(8) . . ? C16S C21S C20S 116.7(7) . . ? C16S C21S C22S 120.3(8) . . ? C20S C21S C22S 122.8(7) . . ? C24S C23S C28S 119.9(8) . . ? C25S C24S C23S 119.8(8) . . ? C26S C25S C24S 121.8(9) . . ? C25S C26S C27S 119.7(9) . . ? C28S C27S C26S 119.5(9) . . ? C27S C28S C23S 119.2(8) . . ? C27S C28S C29S 118.9(9) . . ? C23S C28S C29S 121.6(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.500 _refine_diff_density_min -1.554 _refine_diff_density_rms 0.101 #===END of CIF