# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Annie Powell' _publ_contact_author_email ANNIE.POWELL@KIT.EDU _publ_section_title ; [Ln2(PhCO2)6(MeOH)4] (Ln = Pr, Nd, Gd): The effect of lanthanide radius on network dimensionality ; loop_ _publ_author_name 'Annie Powell' 'Christopher E. Anson' 'George E. Kostakis' 'Sanjit Nayak' # Attachment 'sms989.cif' data_sms989 _database_code_depnum_ccdc_archive 'CCDC 763979' #TrackingRef 'sms989.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 O16 Pr2' _chemical_formula_weight 1136.65 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2557(12) _cell_length_b 14.7071(19) _cell_length_c 14.8141(18) _cell_angle_alpha 90.327(10) _cell_angle_beta 90.161(10) _cell_angle_gamma 97.787(10) _cell_volume 2213.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20689 _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 27.28 _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 2.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.304 _exptl_absorpt_correction_T_max 0.624 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14362 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7974 _reflns_number_gt 5163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Geometrical restraints were applied to coordinates of O-H H atoms. ; _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^)+(0.1077P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7974 _refine_ls_number_parameters 593 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1646 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.89374(5) 0.49864(4) 0.17740(4) 0.03569(18) Uani 1 1 d . . . Pr2 Pr 0.39521(5) 0.50387(4) 0.32280(4) 0.03573(18) Uani 1 1 d . . . O1 O 0.7741(7) 0.6263(5) 0.2031(5) 0.0430(17) Uani 1 1 d . . . O2 O 0.5875(7) 0.6025(5) 0.2802(5) 0.0427(17) Uani 1 1 d . . . C1 C 0.6723(10) 0.6530(8) 0.2353(7) 0.039(2) Uani 1 1 d . . . C2 C 0.6546(10) 0.7497(8) 0.2204(7) 0.041(2) Uani 1 1 d . . . C3 C 0.7505(12) 0.8113(8) 0.1792(8) 0.047(3) Uani 1 1 d . . . H3A H 0.8306 0.7909 0.1610 0.057 Uiso 1 1 calc R . . C4 C 0.7326(14) 0.9006(9) 0.1640(9) 0.059(3) Uani 1 1 d . . . H4A H 0.8006 0.9416 0.1367 0.071 Uiso 1 1 calc R . . C5 C 0.6148(16) 0.9318(10) 0.1884(10) 0.066(4) Uani 1 1 d . . . H5A H 0.6020 0.9936 0.1776 0.080 Uiso 1 1 calc R . . C6 C 0.5166(15) 0.8712(10) 0.2286(9) 0.062(4) Uani 1 1 d . . . H6A H 0.4354 0.8911 0.2446 0.074 Uiso 1 1 calc R . . C7 C 0.5373(12) 0.7819(9) 0.2452(8) 0.050(3) Uani 1 1 d . . . H7A H 0.4704 0.7415 0.2742 0.060 Uiso 1 1 calc R . . O3 O 0.6870(7) 0.4054(5) 0.1619(5) 0.0451(18) Uani 1 1 d . . . O4 O 0.4822(7) 0.4118(6) 0.2113(5) 0.0460(19) Uani 1 1 d . . . C8 C 0.5661(12) 0.3726(8) 0.1716(7) 0.044(3) Uani 1 1 d . . . C9 C 0.5237(10) 0.2798(8) 0.1297(7) 0.039(2) Uani 1 1 d . . . C10 C 0.3944(11) 0.2388(8) 0.1394(7) 0.042(2) Uani 1 1 d . . . H10A H 0.3338 0.2690 0.1728 0.051 Uiso 1 1 calc R . . C11 C 0.3540(13) 0.1542(9) 0.1006(9) 0.057(3) Uani 1 1 d . . . H11A H 0.2651 0.1269 0.1071 0.068 Uiso 1 1 calc R . . C12 C 0.4403(14) 0.1087(9) 0.0526(10) 0.062(3) Uani 1 1 d . . . H12A H 0.4115 0.0506 0.0257 0.074 Uiso 1 1 calc R . . C13 C 0.5720(14) 0.1496(9) 0.0440(9) 0.058(3) Uani 1 1 d . . . H13A H 0.6328 0.1186 0.0117 0.070 Uiso 1 1 calc R . . C14 C 0.6133(13) 0.2346(9) 0.0823(8) 0.051(3) Uani 1 1 d . . . H14A H 0.7022 0.2620 0.0764 0.061 Uiso 1 1 calc R . . O5 O 0.2241(7) 0.5974(5) 0.3348(5) 0.0450(18) Uani 1 1 d . . . O6 O 0.0151(7) 0.5926(5) 0.2905(5) 0.0433(18) Uani 1 1 d . . . C15 C 0.1168(10) 0.6305(8) 0.3292(7) 0.040(2) Uani 1 1 d . . . C16 C 0.1115(10) 0.7214(7) 0.3753(7) 0.037(2) Uani 1 1 d . . . C17 C 0.2212(12) 0.7662(8) 0.4213(8) 0.047(3) Uani 1 1 d . . . H17A H 0.3013 0.7404 0.4212 0.057 Uiso 1 1 calc R . . C18 C 0.2142(14) 0.8478(9) 0.4670(9) 0.058(3) Uani 1 1 d . . . H18A H 0.2881 0.8769 0.5000 0.070 Uiso 1 1 calc R . . C19 C 0.0988(15) 0.8864(9) 0.4641(9) 0.062(3) Uani 1 1 d . . . H19A H 0.0941 0.9428 0.4948 0.074 Uiso 1 1 calc R . . C20 C -0.0094(12) 0.8444(9) 0.4175(9) 0.053(3) Uani 1 1 d . . . H20A H -0.0887 0.8711 0.4169 0.063 Uiso 1 1 calc R . . C21 C -0.0019(11) 0.7633(8) 0.3714(7) 0.042(2) Uani 1 1 d . . . H21A H -0.0751 0.7359 0.3368 0.051 Uiso 1 1 calc R . . O7 O 0.2272(7) 0.3762(5) 0.2972(5) 0.0415(17) Uani 1 1 d . . . O8 O 0.0458(7) 0.4001(5) 0.2236(5) 0.0409(17) Uani 1 1 d . . . C22 C 0.1134(10) 0.3480(8) 0.2647(7) 0.038(2) Uani 1 1 d . . . C23 C 0.0616(11) 0.2492(8) 0.2752(7) 0.041(2) Uani 1 1 d . . . C24 C 0.1382(12) 0.1881(8) 0.3091(8) 0.047(3) Uani 1 1 d . . . H24A H 0.2257 0.2091 0.3282 0.056 Uiso 1 1 calc R . . C25 C 0.0885(13) 0.0951(9) 0.3157(9) 0.058(3) Uani 1 1 d . . . H25A H 0.1430 0.0530 0.3384 0.069 Uiso 1 1 calc R . . C26 C -0.0378(14) 0.0642(10) 0.2899(9) 0.063(4) Uani 1 1 d . . . H26A H -0.0707 0.0008 0.2932 0.075 Uiso 1 1 calc R . . C27 C -0.1168(13) 0.1259(9) 0.2590(10) 0.059(3) Uani 1 1 d . . . H27A H -0.2055 0.1049 0.2428 0.071 Uiso 1 1 calc R . . C28 C -0.0693(12) 0.2179(9) 0.2512(8) 0.052(3) Uani 1 1 d . . . H28A H -0.1249 0.2598 0.2297 0.062 Uiso 1 1 calc R . . O9 O 0.9156(7) 0.3846(5) 0.0523(4) 0.0390(16) Uani 1 1 d . . . O10 O 0.9080(7) 0.4242(5) -0.0920(4) 0.0369(16) Uani 1 1 d D . . C29 C 0.9107(10) 0.3649(8) -0.0297(7) 0.041(2) Uani 1 1 d . . . C30 C 0.9045(10) 0.2659(7) -0.0561(7) 0.037(2) Uani 1 1 d . . . C31 C 0.9401(11) 0.2036(8) 0.0070(8) 0.045(3) Uani 1 1 d . . . H31A H 0.9676 0.2243 0.0658 0.054 Uiso 1 1 calc R . . C32 C 0.9356(14) 0.1112(9) -0.0157(9) 0.058(3) Uani 1 1 d . . . H32A H 0.9607 0.0690 0.0272 0.069 Uiso 1 1 calc R . . C33 C 0.8939(13) 0.0809(9) -0.1021(9) 0.057(3) Uani 1 1 d . . . H33A H 0.8892 0.0179 -0.1180 0.068 Uiso 1 1 calc R . . C34 C 0.8597(12) 0.1430(9) -0.1638(8) 0.051(3) Uani 1 1 d . . . H34A H 0.8323 0.1224 -0.2226 0.062 Uiso 1 1 calc R . . C35 C 0.8643(12) 0.2348(8) -0.1421(7) 0.048(3) Uani 1 1 d . . . H35A H 0.8402 0.2766 -0.1857 0.057 Uiso 1 1 calc R . . O11 O 0.5589(7) 0.4211(5) 0.4074(5) 0.0378(16) Uani 1 1 d D . . O12 O 0.5371(7) 0.3829(5) 0.5527(5) 0.0391(16) Uani 1 1 d . . . C36 C 0.5342(9) 0.3639(8) 0.4715(7) 0.039(2) Uani 1 1 d . . . C37 C 0.5003(11) 0.2636(7) 0.4456(7) 0.040(2) Uani 1 1 d . . . C38 C 0.4366(12) 0.2025(8) 0.5086(8) 0.048(3) Uani 1 1 d . . . H38A H 0.4146 0.2236 0.5666 0.058 Uiso 1 1 calc R . . C39 C 0.4057(13) 0.1100(9) 0.4850(9) 0.057(3) Uani 1 1 d . . . H39A H 0.3621 0.0679 0.5270 0.068 Uiso 1 1 calc R . . C40 C 0.4382(14) 0.0797(9) 0.4007(9) 0.059(3) Uani 1 1 d . . . H40A H 0.4170 0.0166 0.3853 0.070 Uiso 1 1 calc R . . C41 C 0.5003(14) 0.1390(9) 0.3395(9) 0.058(3) Uani 1 1 d . . . H41A H 0.5230 0.1171 0.2819 0.070 Uiso 1 1 calc R . . C42 C 0.5304(12) 0.2312(9) 0.3608(8) 0.050(3) Uani 1 1 d . . . H42A H 0.5719 0.2726 0.3173 0.060 Uiso 1 1 calc R . . O13 O 0.8128(8) 0.4408(7) 0.3311(5) 0.059(2) Uani 1 1 d D . . H13 H 0.729(5) 0.446(9) 0.344(8) 0.071 Uiso 1 1 d D . . C43 C 0.8864(12) 0.4117(9) 0.4074(7) 0.052(3) Uani 1 1 d . . . H43A H 0.8631 0.4433 0.4622 0.077 Uiso 1 1 calc R . . H43B H 0.9809 0.4269 0.3961 0.077 Uiso 1 1 calc R . . H43C H 0.8648 0.3452 0.4152 0.077 Uiso 1 1 calc R . . O14 O 0.8174(7) 0.5545(5) 0.0246(5) 0.0420(17) Uani 1 1 d D . . H14 H 0.866(9) 0.523(6) -0.010(7) 0.050 Uiso 1 1 d D . . C44 C 0.7588(12) 0.6267(8) -0.0137(8) 0.047(3) Uani 1 1 d . . . H44A H 0.6864 0.6013 -0.0537 0.071 Uiso 1 1 calc R . . H44B H 0.8247 0.6663 -0.0486 0.071 Uiso 1 1 calc R . . H44C H 0.7246 0.6627 0.0344 0.071 Uiso 1 1 calc R . . O15 O 0.2961(7) 0.4499(5) 0.4742(5) 0.0418(17) Uani 1 1 d D . . H15 H 0.354(9) 0.484(6) 0.510(7) 0.050 Uiso 1 1 d D . . C45 C 0.2082(11) 0.3765(8) 0.5119(7) 0.045(3) Uani 1 1 d . . . H45A H 0.1383 0.4016 0.5449 0.067 Uiso 1 1 calc R . . H45B H 0.2566 0.3415 0.5534 0.067 Uiso 1 1 calc R . . H45C H 0.1692 0.3360 0.4634 0.067 Uiso 1 1 calc R . . O16 O 0.3364(9) 0.5566(8) 0.1678(5) 0.062(3) Uani 1 1 d D . . H16 H 0.254(6) 0.559(10) 0.150(9) 0.074 Uiso 1 1 d D . . C46 C 0.4213(12) 0.5866(9) 0.0906(7) 0.049(3) Uani 1 1 d . . . H46A H 0.3758 0.5663 0.0343 0.074 Uiso 1 1 calc R . . H46B H 0.5035 0.5598 0.0950 0.074 Uiso 1 1 calc R . . H46C H 0.4410 0.6537 0.0912 0.074 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 0.0317(3) 0.0395(4) 0.0362(3) -0.0007(2) -0.0021(2) 0.0061(3) Pr2 0.0318(3) 0.0389(4) 0.0366(3) -0.0018(2) -0.0020(2) 0.0056(3) O1 0.038(4) 0.044(4) 0.048(4) -0.004(3) 0.001(3) 0.010(3) O2 0.038(4) 0.040(4) 0.047(4) -0.002(3) 0.006(3) -0.006(3) C1 0.033(5) 0.044(6) 0.040(5) -0.005(5) -0.006(4) 0.003(5) C2 0.033(5) 0.044(6) 0.049(6) -0.002(5) -0.003(5) 0.011(5) C3 0.044(6) 0.041(7) 0.057(7) 0.001(5) 0.005(5) 0.008(5) C4 0.061(8) 0.050(8) 0.064(8) 0.005(6) 0.001(6) 0.002(6) C5 0.088(11) 0.048(8) 0.065(8) -0.010(6) -0.011(8) 0.020(8) C6 0.067(9) 0.057(8) 0.067(8) -0.014(7) 0.001(7) 0.029(7) C7 0.045(7) 0.047(7) 0.059(7) -0.005(5) -0.006(5) 0.007(5) O3 0.027(4) 0.043(4) 0.064(5) -0.014(4) -0.005(3) -0.003(3) O4 0.039(4) 0.056(5) 0.044(4) -0.021(4) 0.003(3) 0.012(4) C8 0.052(7) 0.044(6) 0.036(6) 0.005(5) -0.009(5) 0.004(5) C9 0.037(6) 0.043(6) 0.038(5) -0.001(4) -0.004(4) 0.004(5) C10 0.043(6) 0.039(6) 0.045(6) -0.003(5) -0.005(5) 0.002(5) C11 0.048(7) 0.042(7) 0.079(9) 0.004(6) -0.009(6) 0.004(6) C12 0.063(8) 0.046(7) 0.076(9) -0.015(6) -0.012(7) 0.008(6) C13 0.068(9) 0.056(8) 0.052(7) -0.010(6) 0.010(6) 0.014(7) C14 0.051(7) 0.049(7) 0.053(7) -0.006(5) 0.006(5) 0.010(6) O5 0.036(4) 0.043(4) 0.058(5) -0.011(4) -0.008(3) 0.018(3) O6 0.039(4) 0.049(5) 0.041(4) -0.012(3) -0.010(3) 0.002(3) C15 0.037(6) 0.046(6) 0.039(6) 0.005(5) 0.008(4) 0.010(5) C16 0.036(5) 0.037(6) 0.037(5) 0.003(4) 0.000(4) 0.003(4) C17 0.048(7) 0.040(6) 0.053(7) -0.008(5) -0.005(5) 0.002(5) C18 0.066(9) 0.049(8) 0.059(8) -0.003(6) -0.008(6) 0.005(6) C19 0.081(10) 0.044(7) 0.063(8) -0.010(6) 0.003(7) 0.017(7) C20 0.046(7) 0.046(7) 0.067(8) 0.000(6) 0.007(6) 0.010(6) C21 0.038(6) 0.040(6) 0.048(6) -0.001(5) 0.001(5) 0.001(5) O7 0.036(4) 0.035(4) 0.053(4) -0.001(3) -0.003(3) 0.003(3) O8 0.038(4) 0.047(4) 0.040(4) -0.001(3) -0.008(3) 0.015(3) C22 0.035(5) 0.050(6) 0.031(5) -0.009(4) -0.005(4) 0.008(5) C23 0.038(6) 0.043(6) 0.041(6) -0.001(5) 0.003(4) 0.004(5) C24 0.046(6) 0.048(7) 0.047(6) 0.001(5) -0.010(5) 0.009(5) C25 0.061(8) 0.044(7) 0.068(8) 0.007(6) -0.005(6) 0.005(6) C26 0.066(8) 0.049(8) 0.068(8) -0.001(6) -0.011(7) -0.009(7) C27 0.052(7) 0.044(7) 0.077(9) -0.002(6) -0.008(6) -0.003(6) C28 0.048(7) 0.050(7) 0.058(7) -0.005(6) -0.009(6) 0.007(6) O9 0.041(4) 0.045(4) 0.032(4) -0.004(3) -0.004(3) 0.009(3) O10 0.031(4) 0.043(4) 0.036(4) 0.002(3) -0.004(3) 0.001(3) C29 0.029(5) 0.045(6) 0.048(6) -0.001(5) -0.004(4) 0.006(5) C30 0.026(5) 0.042(6) 0.044(6) 0.003(4) 0.008(4) 0.005(4) C31 0.046(6) 0.035(6) 0.055(7) 0.001(5) 0.002(5) 0.009(5) C32 0.070(9) 0.046(7) 0.059(8) 0.001(6) -0.004(6) 0.017(6) C33 0.058(8) 0.046(7) 0.065(8) -0.004(6) 0.011(6) 0.002(6) C34 0.052(7) 0.053(8) 0.047(6) -0.008(5) -0.001(5) -0.002(6) C35 0.051(7) 0.049(7) 0.040(6) -0.004(5) -0.002(5) -0.004(5) O11 0.035(4) 0.043(4) 0.037(4) 0.003(3) 0.001(3) 0.011(3) O12 0.042(4) 0.039(4) 0.036(4) -0.004(3) -0.003(3) 0.004(3) C36 0.023(5) 0.053(7) 0.043(6) 0.004(5) 0.001(4) 0.014(5) C37 0.038(6) 0.036(6) 0.046(6) 0.004(4) -0.002(5) 0.007(5) C38 0.051(7) 0.045(7) 0.048(6) -0.005(5) -0.006(5) 0.005(5) C39 0.055(7) 0.040(7) 0.072(9) 0.002(6) -0.006(6) -0.001(6) C40 0.069(9) 0.041(7) 0.066(8) -0.013(6) -0.021(7) 0.009(6) C41 0.064(8) 0.054(8) 0.061(8) -0.013(6) -0.016(6) 0.021(7) C42 0.051(7) 0.054(7) 0.046(6) -0.004(5) -0.007(5) 0.013(6) O13 0.045(5) 0.091(7) 0.038(4) 0.016(4) 0.011(4) 0.000(5) C43 0.059(8) 0.064(8) 0.036(6) 0.010(5) 0.009(5) 0.024(6) O14 0.041(4) 0.039(4) 0.048(4) -0.003(3) -0.003(3) 0.014(3) C44 0.053(7) 0.050(7) 0.042(6) 0.001(5) 0.000(5) 0.015(6) O15 0.040(4) 0.037(4) 0.047(4) -0.001(3) 0.001(3) 0.002(3) C45 0.041(6) 0.052(7) 0.039(6) 0.002(5) -0.002(5) -0.002(5) O16 0.055(5) 0.105(8) 0.033(4) 0.010(4) -0.002(4) 0.042(5) C46 0.048(7) 0.062(8) 0.036(6) 0.005(5) -0.007(5) -0.001(6) _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 O8 2.370(7) 1_655 ? Pr1 O3 2.373(7) . ? Pr1 O6 2.401(7) 1_655 ? Pr1 O1 2.407(7) . ? Pr1 O9 2.523(7) . ? Pr1 O10 2.535(7) 2_765 ? Pr1 O13 2.538(8) . ? Pr1 O14 2.569(7) . ? Pr2 O2 2.374(7) . ? Pr2 O5 2.379(7) . ? Pr2 O4 2.381(7) . ? Pr2 O7 2.398(7) . ? Pr2 O12 2.511(7) 2_666 ? Pr2 O16 2.525(8) . ? Pr2 O11 2.536(7) . ? Pr2 O15 2.551(8) . ? O1 C1 1.258(13) . ? O2 C1 1.259(13) . ? C1 C2 1.475(16) . ? C2 C3 1.390(16) . ? C2 C7 1.400(16) . ? C3 C4 1.372(18) . ? C3 H3A 0.9500 . ? C4 C5 1.40(2) . ? C4 H4A 0.9500 . ? C5 C6 1.39(2) . ? C5 H5A 0.9500 . ? C6 C7 1.381(18) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? O3 C8 1.278(14) . ? O4 C8 1.245(14) . ? C8 C9 1.506(15) . ? C9 C10 1.388(15) . ? C9 C14 1.394(16) . ? C10 C11 1.379(16) . ? C10 H10A 0.9500 . ? C11 C12 1.377(19) . ? C11 H11A 0.9500 . ? C12 C13 1.409(19) . ? C12 H12A 0.9500 . ? C13 C14 1.382(17) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? O5 C15 1.265(13) . ? O6 C15 1.249(13) . ? O6 Pr1 2.401(7) 1_455 ? C15 C16 1.505(15) . ? C16 C21 1.389(15) . ? C16 C17 1.399(15) . ? C17 C18 1.384(17) . ? C17 H17A 0.9500 . ? C18 C19 1.381(19) . ? C18 H18A 0.9500 . ? C19 C20 1.377(18) . ? C19 H19A 0.9500 . ? C20 C21 1.382(17) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? O7 C22 1.276(12) . ? O8 C22 1.259(13) . ? O8 Pr1 2.370(7) 1_455 ? C22 C23 1.488(16) . ? C23 C24 1.367(16) . ? C23 C28 1.403(16) . ? C24 C25 1.399(17) . ? C24 H24A 0.9500 . ? C25 C26 1.366(18) . ? C25 H25A 0.9500 . ? C26 C27 1.376(19) . ? C26 H26A 0.9500 . ? C27 C28 1.379(18) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? O9 C29 1.247(13) . ? O10 C29 1.276(13) . ? O10 Pr1 2.535(7) 2_765 ? C29 C30 1.499(15) . ? C30 C35 1.393(15) . ? C30 C31 1.395(15) . ? C31 C32 1.392(17) . ? C31 H31A 0.9500 . ? C32 C33 1.400(18) . ? C32 H32A 0.9500 . ? C33 C34 1.374(18) . ? C33 H33A 0.9500 . ? C34 C35 1.380(17) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? O11 C36 1.274(13) . ? O12 C36 1.232(12) . ? O12 Pr2 2.511(7) 2_666 ? C36 C37 1.516(16) . ? C37 C42 1.392(16) . ? C37 C38 1.399(16) . ? C38 C39 1.396(17) . ? C38 H38A 0.9500 . ? C39 C40 1.380(19) . ? C39 H39A 0.9500 . ? C40 C41 1.36(2) . ? C40 H40A 0.9500 . ? C41 C42 1.384(18) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? O13 C43 1.455(13) . ? O13 H13 0.89(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O14 C44 1.410(13) . ? O14 H14 0.89(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O15 C45 1.427(13) . ? O15 H15 0.90(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O16 C46 1.472(14) . ? O16 H16 0.89(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? 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 O8 Pr1 O3 106.5(3) 1_655 . ? O8 Pr1 O6 79.5(3) 1_655 1_655 ? O3 Pr1 O6 138.5(3) . 1_655 ? O8 Pr1 O1 151.5(2) 1_655 . ? O3 Pr1 O1 87.4(3) . . ? O6 Pr1 O1 73.9(3) 1_655 . ? O8 Pr1 O9 71.4(2) 1_655 . ? O3 Pr1 O9 72.7(3) . . ? O6 Pr1 O9 143.5(2) 1_655 . ? O1 Pr1 O9 137.1(2) . . ? O8 Pr1 O10 82.3(2) 1_655 2_765 ? O3 Pr1 O10 144.3(2) . 2_765 ? O6 Pr1 O10 76.7(2) 1_655 2_765 ? O1 Pr1 O10 101.0(2) . 2_765 ? O9 Pr1 O10 78.0(2) . 2_765 ? O8 Pr1 O13 75.3(3) 1_655 . ? O3 Pr1 O13 70.3(3) . . ? O6 Pr1 O13 71.9(3) 1_655 . ? O1 Pr1 O13 86.8(3) . . ? O9 Pr1 O13 119.3(3) . . ? O10 Pr1 O13 144.0(2) 2_765 . ? O8 Pr1 O14 134.9(2) 1_655 . ? O3 Pr1 O14 79.5(3) . . ? O6 Pr1 O14 125.7(3) 1_655 . ? O1 Pr1 O14 71.2(2) . . ? O9 Pr1 O14 68.0(2) . . ? O10 Pr1 O14 70.9(2) 2_765 . ? O13 Pr1 O14 143.3(3) . . ? O2 Pr2 O5 106.5(3) . . ? O2 Pr2 O4 79.4(3) . . ? O5 Pr2 O4 138.0(3) . . ? O2 Pr2 O7 152.5(3) . . ? O5 Pr2 O7 87.5(3) . . ? O4 Pr2 O7 74.6(3) . . ? O2 Pr2 O12 70.2(2) . 2_666 ? O5 Pr2 O12 73.9(2) . 2_666 ? O4 Pr2 O12 142.3(2) . 2_666 ? O7 Pr2 O12 137.3(3) . 2_666 ? O2 Pr2 O16 77.2(3) . . ? O5 Pr2 O16 70.4(3) . . ? O4 Pr2 O16 70.6(3) . . ? O7 Pr2 O16 85.8(3) . . ? O12 Pr2 O16 121.2(3) 2_666 . ? O2 Pr2 O11 83.0(3) . . ? O5 Pr2 O11 146.1(2) . . ? O4 Pr2 O11 75.3(2) . . ? O7 Pr2 O11 98.7(2) . . ? O12 Pr2 O11 79.4(2) 2_666 . ? O16 Pr2 O11 143.1(3) . . ? O2 Pr2 O15 133.8(2) . . ? O5 Pr2 O15 79.7(3) . . ? O4 Pr2 O15 126.7(3) . . ? O7 Pr2 O15 71.1(2) . . ? O12 Pr2 O15 68.0(2) 2_666 . ? O16 Pr2 O15 142.9(3) . . ? O11 Pr2 O15 71.1(2) . . ? C1 O1 Pr1 146.6(7) . . ? C1 O2 Pr2 162.9(7) . . ? O1 C1 O2 123.7(11) . . ? O1 C1 C2 117.3(10) . . ? O2 C1 C2 119.0(10) . . ? C3 C2 C7 117.5(11) . . ? C3 C2 C1 121.9(10) . . ? C7 C2 C1 120.6(11) . . ? C4 C3 C2 121.6(12) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 120.3(13) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 119.1(13) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C7 C6 C5 119.9(13) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C2 121.5(13) . . ? C6 C7 H7A 119.2 . . ? C2 C7 H7A 119.2 . . ? C8 O3 Pr1 162.4(7) . . ? C8 O4 Pr2 157.6(7) . . ? O4 C8 O3 125.2(11) . . ? O4 C8 C9 118.6(10) . . ? O3 C8 C9 116.2(11) . . ? C10 C9 C14 120.0(11) . . ? C10 C9 C8 119.4(10) . . ? C14 C9 C8 120.6(10) . . ? C11 C10 C9 120.0(12) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C11 C10 121.0(12) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 119.0(12) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 120.4(12) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C9 119.6(12) . . ? C13 C14 H14A 120.2 . . ? C9 C14 H14A 120.2 . . ? C15 O5 Pr2 165.1(7) . . ? C15 O6 Pr1 155.1(7) . 1_455 ? O6 C15 O5 125.1(11) . . ? O6 C15 C16 118.1(9) . . ? O5 C15 C16 116.8(10) . . ? C21 C16 C17 118.7(10) . . ? C21 C16 C15 120.6(9) . . ? C17 C16 C15 120.8(10) . . ? C18 C17 C16 120.6(12) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 119.3(12) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C20 C19 C18 120.9(12) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C19 C20 C21 119.6(12) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C20 C21 C16 120.7(11) . . ? C20 C21 H21A 119.6 . . ? C16 C21 H21A 119.6 . . ? C22 O7 Pr2 147.0(7) . . ? C22 O8 Pr1 167.2(7) . 1_455 ? O8 C22 O7 122.6(10) . . ? O8 C22 C23 119.6(9) . . ? O7 C22 C23 117.7(9) . . ? C24 C23 C28 119.1(11) . . ? C24 C23 C22 121.5(10) . . ? C28 C23 C22 119.5(10) . . ? C23 C24 C25 120.4(11) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 120.5(12) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C27 119.4(12) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? C26 C27 C28 121.0(12) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? C27 C28 C23 119.6(12) . . ? C27 C28 H28A 120.2 . . ? C23 C28 H28A 120.2 . . ? C29 O9 Pr1 149.5(7) . . ? C29 O10 Pr1 125.6(6) . 2_765 ? O9 C29 O10 123.5(10) . . ? O9 C29 C30 118.0(10) . . ? O10 C29 C30 118.4(9) . . ? C35 C30 C31 119.4(11) . . ? C35 C30 C29 121.5(10) . . ? C31 C30 C29 119.1(10) . . ? C32 C31 C30 120.3(11) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 119.7(12) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C34 C33 C32 119.5(12) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C33 C34 C35 121.4(11) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C34 C35 C30 119.8(11) . . ? C34 C35 H35A 120.1 . . ? C30 C35 H35A 120.1 . . ? C36 O11 Pr2 127.0(6) . . ? C36 O12 Pr2 149.0(7) . 2_666 ? O12 C36 O11 125.8(11) . . ? O12 C36 C37 117.1(10) . . ? O11 C36 C37 117.1(9) . . ? C42 C37 C38 119.4(11) . . ? C42 C37 C36 121.5(10) . . ? C38 C37 C36 119.0(10) . . ? C39 C38 C37 119.1(11) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? C40 C39 C38 120.2(13) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C41 C40 C39 120.8(12) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C40 C41 C42 120.1(13) . . ? C40 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? C41 C42 C37 120.4(12) . . ? C41 C42 H42A 119.8 . . ? C37 C42 H42A 119.8 . . ? C43 O13 Pr1 129.7(7) . . ? C43 O13 H13 114(7) . . ? Pr1 O13 H13 116(7) . . ? O13 C43 H43A 109.5 . . ? O13 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O13 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C44 O14 Pr1 141.1(7) . . ? C44 O14 H14 119(8) . . ? Pr1 O14 H14 97(8) . . ? O14 C44 H44A 109.5 . . ? O14 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O14 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C45 O15 Pr2 140.4(6) . . ? C45 O15 H15 119(8) . . ? Pr2 O15 H15 98(8) . . ? O15 C45 H45A 109.5 . . ? O15 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O15 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 O16 Pr2 130.3(6) . . ? C46 O16 H16 107(9) . . ? Pr2 O16 H16 123(9) . . ? O16 C46 H46A 109.5 . . ? O16 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O16 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 O11 0.89(4) 1.98(4) 2.821(11) 157(10) . O14 H14 O10 0.89(3) 1.98(3) 2.824(10) 158(9) . O15 H15 O11 0.90(3) 1.97(3) 2.842(10) 165(10) 2_666 O16 H16 O10 0.89(3) 1.92(3) 2.794(10) 169(13) 2_665 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.627 _refine_diff_density_min -2.502 _refine_diff_density_rms 0.225