# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? loop_ _publ_author_address _publ_author_footnote ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; ; ? # Address 2 ; ; ? # Footnote 2 ; _publ_contact_author_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Nowhere, Nowhere, NO1 4T, UK. ; _publ_contact_author_email gqzhang79@gmail.com _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_phone '+44 1865 000000' _publ_contact_author_name 'Guoqi Zhang' # end Validation Reply Form # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_section_title # Title of paper - generally just the systematic or trivial name ; ? ; _publ_author_name 'Guoqi Zhang' data_gq15_203k _database_code_depnum_ccdc_archive 'CCDC 842060' #TrackingRef 'gq15.cif.txt' _audit_creation_date 08-08-25 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'gq15_203k_0m in P2(1)2(1)2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.4805(4) _cell_length_b 20.3239(6) _cell_length_c 24.9820(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6844.5(3) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Sm -0.1638 3.4418 24.0042 2.4727 19.4258 0.1965 13.4396 14.3996 2.8960 128.0070 2.2096 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C108 H112 F18 N8 O48 Pd4 S6 Sm2 # Dc = 1.72 Fooo = 3480.00 Mu = 15.60 M = 1775.43 # Found Formula = C105 H144 F18 N8 O43 Pd4 S6 Sm2 # Dc = 1.68 FOOO = 3480.00 Mu = 15.55 M = 1733.54 _chemical_formula_sum 'C105 H152 F18 N8 O43 Pd4 S6 Sm2' _chemical_formula_moiety ; 2(C48 H66 N4 O9 Pd2 Sm), 6(C F3 O3 S), 3(C H4 O), 4(H2 O) ; _chemical_compound_source ? _chemical_formula_weight 3467.09 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 203 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3480 _exptl_absorpt_coefficient_mu 1.555 # Sheldrick geometric approximatio 0.70 0.94 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.94 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 203 _diffrn_reflns_number 173829 _reflns_number_total 24796 _diffrn_reflns_av_R_equivalents 0.045 # Number of reflections with Friedels Law is 173666 # Number of reflections without Friedels Law is 24796 # Theoretical number of reflections is about 12453 _diffrn_reflns_theta_min 1.988 _diffrn_reflns_theta_max 32.564 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 32.564 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 37 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -4.44 _refine_diff_density_max 8.65 _refine_ls_number_reflns 13722 _refine_ls_number_restraints 1749 _refine_ls_number_parameters 947 #_refine_ls_R_factor_ref 0.0553 _refine_ls_wR_factor_ref 0.0549 _refine_ls_goodness_of_fit_ref 1.0093 #_reflns_number_all 24661 _refine_ls_R_factor_all 0.0973 _refine_ls_wR_factor_all 0.0739 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 13722 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_gt 0.0549 _refine_ls_shift/su_max 0.010417 _refine_ls_abs_structure_Flack 0.001(11) _refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.07 -0.163 1.62 ; # start Validation Reply Form _vrf_PLAT241_gq15_203k ; PROBLEM: Check High Ueq as Compared to Neighbors for F41 RESPONSE: F41 belongs to a disordered triflate anion. The Ueq of F41 (0.154) lies in the same range as that of the other F (F31 - F43) atoms. (Ueq = 0.132 - 0.164) ; _vrf_PLAT432_gq15_203k ; PROBLEM: Short Inter X...Y Contact O43 .. C44 .. 2.59 Ang. RESPONSE: O43 (triflate, occ = 0.5) and C44 (kation, occ = 0.4) are disordered. The sum of their occupancies is less than 1. ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Sm1 Sm 0.47843(3) 0.434613(17) 0.260779(13) 0.0311 1.0000 Uani . . . . . . Pd2 Pd 0.69282(3) 0.43986(3) 0.184892(18) 0.0307 1.0000 Uani . . . . . . Pd3 Pd 0.25948(3) 0.44322(2) 0.333431(17) 0.0282 1.0000 Uani . . . . . . N1 N 0.8231(5) 0.3938(3) 0.1850(2) 0.0370 1.0000 Uani . . . . . . N2 N 0.7326(5) 0.4797(3) 0.1147(2) 0.0382 1.0000 Uani . . . . . . N3 N 0.2111(5) 0.4874(3) 0.4004(2) 0.0358 1.0000 Uani . . . . . . N4 N 0.1274(4) 0.4011(3) 0.3288(2) 0.0296 1.0000 Uani . . . . . . O1 O 0.6425(4) 0.3998(2) 0.2520(2) 0.0405 1.0000 Uani . . . . . . O2 O 0.5627(4) 0.4875(2) 0.1909(2) 0.0387 1.0000 Uani . . . . . . O3 O 0.5705(4) 0.3807(2) 0.34440(18) 0.0397 1.0000 Uani . . . . . . O4 O 0.3932(4) 0.5330(3) 0.2102(2) 0.0446 1.0000 Uani . . . . . . O5 O 0.3942(4) 0.4860(2) 0.3317(2) 0.0370 1.0000 Uani . . . . . . O6 O 0.3146(4) 0.4006(2) 0.26786(18) 0.0337 1.0000 Uani . . . . . . O7 O 0.5669(4) 0.5286(2) 0.3151(2) 0.0380 1.0000 Uani . . . . . . O8 O 0.3855(4) 0.3848(3) 0.17517(19) 0.0409 1.0000 Uani . . . . . . O9 O 0.4769(4) 0.3135(2) 0.2574(2) 0.0447 1.0000 Uani . . . . . . O11 O 0.5364(5) 0.2985(3) 0.0221(3) 0.0731 1.0000 Uani D U . . . . O12 O 0.6686(5) 0.2950(3) 0.0855(2) 0.0692 1.0000 Uani D U . . . . O13 O 0.6346(6) 0.3952(2) 0.0386(3) 0.0646 1.0000 Uani D U . . . . O21 O 0.8238(12) 0.7851(5) 0.0158(5) 0.1657 1.0000 Uani D U . . . . O22 O 0.7667(7) 0.6730(4) 0.0122(3) 0.0986 1.0000 Uani D U . . . . O23 O 0.7565(10) 0.7322(6) 0.0933(3) 0.1490 1.0000 Uani D U . . . . O31 O 1.0532(9) 0.5055(7) 0.2645(6) 0.0919 0.5000 Uani D U . . . . O32 O 0.8809(9) 0.5109(8) 0.2433(6) 0.0945 0.5000 Uani D U . . . . O33 O 0.9496(11) 0.5825(8) 0.3098(5) 0.0893 0.5000 Uani D U . . . . O41 O 1.0957(10) 0.5359(8) 0.2745(6) 0.0928 0.5000 Uani D U . . . . O42 O 0.9512(9) 0.4778(5) 0.2526(4) 0.0617 0.5000 Uani D U . . . . O43 O 1.0414(13) 0.5346(9) 0.1836(4) 0.1003 0.5000 Uani D U . . . . O501 O 0.2986(6) 0.4018(4) 0.4767(3) 0.0759 1.0000 Uani D U . . . . O502 O 0.9164(16) 0.1864(10) 0.1569(8) 0.1074 0.5000 Uani D U . . . . O503 O 0.390(2) 0.2472(9) 0.3093(8) 0.1408 0.5000 Uani . U . . . . O504 O 0.5819(10) 0.2520(5) 0.1842(5) 0.0686 0.6000 Uani . U . . . . O513 O 0.363(2) 0.1985(10) 0.2749(10) 0.1508 0.5000 Uani . U . . . . O514 O 0.6410(16) 0.1930(11) 0.2093(9) 0.0847 0.4000 Uani . U . . . . C1 C 0.6931(5) 0.3569(3) 0.2813(2) 0.0287 1.0000 Uani . . . . . . C2 C 0.6558(5) 0.3451(3) 0.3334(3) 0.0331 1.0000 Uani . . . . . . C3 C 0.7004(6) 0.3012(4) 0.3681(3) 0.0407 1.0000 Uani . . . . . . C4 C 0.7863(6) 0.2685(4) 0.3496(3) 0.0455 1.0000 Uani . . . . . . C5 C 0.8224(5) 0.2786(3) 0.3004(3) 0.0365 1.0000 Uani . . . . . . C6 C 0.7776(5) 0.3232(3) 0.2621(3) 0.0349 1.0000 Uani . . . . . . C7 C 0.8138(6) 0.3256(4) 0.2061(3) 0.0395 1.0000 Uani . . . . . . C8 C 0.8640(5) 0.3982(3) 0.1294(3) 0.0359 1.0000 Uani . . . . . . C9 C 0.9733(7) 0.3830(5) 0.1272(4) 0.0556 1.0000 Uani . . . . . . C10 C 1.0124(7) 0.3919(5) 0.0697(4) 0.0600 1.0000 Uani . . . . . . C11 C 0.9886(9) 0.4600(5) 0.0481(4) 0.0699 1.0000 Uani . . . . . . C12 C 0.8802(7) 0.4766(5) 0.0519(4) 0.0569 1.0000 Uani . . . . . . C13 C 0.8422(5) 0.4667(4) 0.1088(3) 0.0392 1.0000 Uani . . . . . . C14 C 0.7066(6) 0.5514(3) 0.1134(3) 0.0429 1.0000 Uani . . . . . . C15 C 0.5963(5) 0.5665(4) 0.1199(2) 0.0354 1.0000 Uani . . . . . . C16 C 0.5572(7) 0.6164(4) 0.0882(3) 0.0448 1.0000 Uani . . . . . . C17 C 0.4633(6) 0.6397(4) 0.0963(3) 0.0467 1.0000 Uani . . . . . . C18 C 0.4042(6) 0.6140(4) 0.1375(3) 0.0425 1.0000 Uani . . . . . . C19 C 0.4415(5) 0.5632(4) 0.1687(3) 0.0369 1.0000 Uani . . . . . . C20 C 0.5359(5) 0.5383(3) 0.1589(3) 0.0323 1.0000 Uani . . . . . . C21 C 0.4185(5) 0.5380(3) 0.3617(3) 0.0349 1.0000 Uani . . . . . . C22 C 0.5140(5) 0.5620(4) 0.3539(3) 0.0373 1.0000 Uani . . . . . . C23 C 0.5503(6) 0.6157(4) 0.3832(4) 0.0501 1.0000 Uani . . . . . . C24 C 0.4841(8) 0.6458(4) 0.4184(4) 0.0584 1.0000 Uani . . . . . . C25 C 0.3888(7) 0.6242(4) 0.4260(3) 0.0507 1.0000 Uani . . . . . . C26 C 0.3532(5) 0.5699(4) 0.3972(3) 0.0390 1.0000 Uani . . . . . . C27 C 0.2428(6) 0.5560(4) 0.4020(3) 0.0442 1.0000 Uani . . . . . . C28 C 0.1030(5) 0.4787(3) 0.4028(3) 0.0345 1.0000 Uani . . . . . . C29 C 0.0574(7) 0.4895(5) 0.4570(3) 0.0544 1.0000 Uani . . . . . . C30 C -0.0534(7) 0.4764(5) 0.4566(4) 0.0597 1.0000 Uani . . . . . . C31 C -0.0784(7) 0.4088(5) 0.4376(4) 0.0548 1.0000 Uani . . . . . . C32 C -0.0334(6) 0.3975(4) 0.3807(3) 0.0466 1.0000 Uani . . . . . . C33 C 0.0764(6) 0.4099(4) 0.3820(2) 0.0359 1.0000 Uani . . . . . . C34 C 0.1346(6) 0.3322(3) 0.3094(3) 0.0357 1.0000 Uani . . . . . . C35 C 0.1777(5) 0.3271(3) 0.2532(3) 0.0333 1.0000 Uani . . . . . . C36 C 0.1308(6) 0.2838(4) 0.2178(3) 0.0434 1.0000 Uani . . . . . . C37 C 0.1729(7) 0.2705(5) 0.1682(4) 0.0573 1.0000 Uani . . . . . . C38 C 0.2563(6) 0.3035(4) 0.1513(3) 0.0471 1.0000 Uani . . . . . . C39 C 0.3010(5) 0.3492(3) 0.1855(3) 0.0334 1.0000 Uani . . . . . . C40 C 0.2626(5) 0.3594(3) 0.2366(2) 0.0294 1.0000 Uani . . . . . . C41 C 0.5234(8) 0.3750(5) 0.3967(3) 0.0555 1.0000 Uani . . . . . . C42 C 0.5646(13) 0.4169(7) 0.4367(5) 0.0945 1.0000 Uani . . . . . . C43 C 0.2907(6) 0.5555(5) 0.2192(4) 0.0628 1.0000 Uani D U . . . . C44 C 0.2315(16) 0.5186(11) 0.1752(8) 0.0700 0.4000 Uani D U . . . . C45 C 0.6731(6) 0.5454(4) 0.3097(4) 0.0566 1.0000 Uani . . . . . . C46 C 0.7328(8) 0.5187(5) 0.3524(6) 0.0803 1.0000 Uani . . . . . . C47 C 0.4301(8) 0.3786(6) 0.1217(3) 0.0644 1.0000 Uani . . . . . . C48 C 0.3711(12) 0.4172(7) 0.0812(4) 0.1010 1.0000 Uani . . . . . . C54 C 0.2963(13) 0.6213(6) 0.2518(6) 0.0696 0.6000 Uani D U . . . . C100 C 0.7128(7) 0.3003(4) -0.0123(3) 0.0961 1.0000 Uani D U . . . . C200 C 0.9266(6) 0.7052(4) 0.0598(4) 0.1004 1.0000 Uani D U . . . . C300 C 0.9942(12) 0.6034(7) 0.2116(6) 0.1156 0.5000 Uani D U . . . . C400 C 0.9506(10) 0.6056(5) 0.2503(8) 0.1269 0.5000 Uani D U . . . . C501 C 0.3015(10) 0.4101(8) 0.5319(4) 0.0914 1.0000 Uani D U . . . . C502 C 0.9193(18) 0.1977(10) 0.1018(8) 0.0763 0.5000 Uani D U . . . . S1 S 0.62959(18) 0.32546(11) 0.03875(8) 0.0519 1.0000 Uani D U . . . . S2 S 0.8061(3) 0.72616(13) 0.04221(13) 0.0733 1.0000 Uani D U . . . . S3 S 0.9648(4) 0.5454(2) 0.2619(2) 0.0582 0.5000 Uani D U . . . . S4 S 1.0108(5) 0.5306(2) 0.2382(2) 0.0711 0.5000 Uani D U . . . . F11 F 0.7127(7) 0.2357(3) -0.0210(3) 0.1182 1.0000 Uani D U . . . . F12 F 0.6915(7) 0.3282(4) -0.0596(2) 0.1219 1.0000 Uani D U . . . . F13 F 0.8069(6) 0.3162(4) -0.0011(3) 0.1237 1.0000 Uani D U . . . . F21 F 0.9717(6) 0.7415(4) 0.0953(3) 0.1052 1.0000 Uani D U . . . . F22 F 0.9695(10) 0.7169(5) 0.0117(3) 0.1605 1.0000 Uani D U . . . . F23 F 0.9437(8) 0.6423(3) 0.0696(4) 0.1302 1.0000 Uani D U . . . . F31 F 0.9245(14) 0.6497(9) 0.2073(8) 0.1510 0.5000 Uani D U . . . . F32 F 1.0778(14) 0.6348(9) 0.2239(8) 0.1450 0.5000 Uani D U . . . . F33 F 1.0084(14) 0.5793(7) 0.1626(6) 0.1324 0.5000 Uani D U . . . . F41 F 0.9247(15) 0.6141(10) 0.3012(8) 0.1536 0.5000 Uani D U . . . . F42 F 1.0106(11) 0.6549(7) 0.2376(9) 0.1429 0.5000 Uani D U . . . . F43 F 0.8687(12) 0.6111(10) 0.2211(10) 0.1643 0.5000 Uani D U . . . . H1 H 0.8668 0.4177 0.2083 0.0468 1.0000 Uiso R . . . . . H2 H 0.6976 0.4576 0.0865 0.0454 1.0000 Uiso R . . . . . H3 H 0.2401 0.4652 0.4306 0.0427 1.0000 Uiso R . . . . . H4 H 0.0893 0.4256 0.3031 0.0355 1.0000 Uiso R . . . . . H5 H 0.4979 0.3009 0.2868 0.0542 1.0000 Uiso R . . . . . H6 H 0.5088 0.2924 0.2341 0.0548 1.0000 Uiso R . . . . . H9 H 0.2686 0.3663 0.4697 0.0938 1.0000 Uiso R . . . . . H11 H 0.9571 0.1491 0.1650 0.1031 0.5000 Uiso R . . . . . H31 H 0.6746 0.2931 0.4033 0.0485 1.0000 Uiso R . . . . . H41 H 0.8202 0.2386 0.3731 0.0539 1.0000 Uiso R . . . . . H51 H 0.8803 0.2544 0.2898 0.0437 1.0000 Uiso R . . . . . H71 H 0.8776 0.3048 0.2046 0.0472 1.0000 Uiso R . . . . . H72 H 0.7679 0.3019 0.1839 0.0472 1.0000 Uiso R . . . . . H81 H 0.8296 0.3670 0.1073 0.0437 1.0000 Uiso R . . . . . H91 H 1.0078 0.4124 0.1508 0.0641 1.0000 Uiso R . . . . . H92 H 0.9844 0.3384 0.1384 0.0641 1.0000 Uiso R . . . . . H101 H 1.0832 0.3866 0.0701 0.0713 1.0000 Uiso R . . . . . H102 H 0.9833 0.3591 0.0470 0.0713 1.0000 Uiso R . . . . . H111 H 1.0254 0.4922 0.0680 0.0854 1.0000 Uiso R . . . . . H112 H 1.0080 0.4616 0.0112 0.0854 1.0000 Uiso R . . . . . H121 H 0.8704 0.5215 0.0413 0.0682 1.0000 Uiso R . . . . . H122 H 0.8435 0.4481 0.0285 0.0682 1.0000 Uiso R . . . . . H131 H 0.8769 0.4974 0.1313 0.0457 1.0000 Uiso R . . . . . H141 H 0.7417 0.5730 0.1419 0.0506 1.0000 Uiso R . . . . . H142 H 0.7279 0.5688 0.0796 0.0506 1.0000 Uiso R . . . . . H161 H 0.5970 0.6351 0.0603 0.0553 1.0000 Uiso R . . . . . H171 H 0.4376 0.6736 0.0735 0.0557 1.0000 Uiso R . . . . . H181 H 0.3390 0.6313 0.1440 0.0494 1.0000 Uiso R . . . . . H231 H 0.6173 0.6311 0.3794 0.0615 1.0000 Uiso R . . . . . H241 H 0.5064 0.6834 0.4383 0.0703 1.0000 Uiso R . . . . . H251 H 0.3464 0.6466 0.4510 0.0596 1.0000 Uiso R . . . . . H271 H 0.2209 0.5740 0.4355 0.0538 1.0000 Uiso R . . . . . H272 H 0.2103 0.5785 0.3732 0.0538 1.0000 Uiso R . . . . . H281 H 0.0737 0.5099 0.3787 0.0404 1.0000 Uiso R . . . . . H291 H 0.0688 0.5343 0.4675 0.0652 1.0000 Uiso R . . . . . H292 H 0.0887 0.4604 0.4822 0.0652 1.0000 Uiso R . . . . . H301 H -0.0781 0.4814 0.4924 0.0693 1.0000 Uiso R . . . . . H302 H -0.0850 0.5080 0.4336 0.0693 1.0000 Uiso R . . . . . H311 H -0.0522 0.3769 0.4622 0.0663 1.0000 Uiso R . . . . . H312 H -0.1491 0.4042 0.4355 0.0663 1.0000 Uiso R . . . . . H321 H -0.0640 0.4266 0.3553 0.0590 1.0000 Uiso R . . . . . H322 H -0.0451 0.3527 0.3702 0.0590 1.0000 Uiso R . . . . . H331 H 0.1052 0.3788 0.4064 0.0400 1.0000 Uiso R . . . . . H341 H 0.1754 0.3074 0.3336 0.0427 1.0000 Uiso R . . . . . H342 H 0.0689 0.3139 0.3088 0.0427 1.0000 Uiso R . . . . . H361 H 0.0697 0.2629 0.2279 0.0536 1.0000 Uiso R . . . . . H371 H 0.1435 0.2381 0.1452 0.0715 1.0000 Uiso R . . . . . H381 H 0.2834 0.2952 0.1164 0.0568 1.0000 Uiso R . . . . . H411 H 0.5275 0.3300 0.4083 0.0681 1.0000 Uiso R . . . . . H412 H 0.4550 0.3873 0.3930 0.0681 1.0000 Uiso R . . . . . H421 H 0.5307 0.4116 0.4702 0.1218 1.0000 Uiso R . . . . . H422 H 0.6329 0.4047 0.4409 0.1218 1.0000 Uiso R . . . . . H423 H 0.5605 0.4620 0.4255 0.1218 1.0000 Uiso R . . . . . H431 H 0.2855 0.6024 0.2153 0.0763 0.4000 Uiso R . . . . . H432 H 0.2686 0.5431 0.2543 0.0763 0.4000 Uiso R . . . . . H433 H 0.2591 0.5634 0.1854 0.0763 0.6000 Uiso R . . . . . H434 H 0.2547 0.5224 0.2385 0.0763 0.6000 Uiso R . . . . . H441 H 0.1631 0.5310 0.1790 0.0776 0.4000 Uiso R . . . . . H442 H 0.2548 0.5312 0.1403 0.0776 0.4000 Uiso R . . . . . H443 H 0.2378 0.4719 0.1793 0.0776 0.4000 Uiso R . . . . . H451 H 0.6796 0.5924 0.3092 0.0670 1.0000 Uiso R . . . . . H452 H 0.6975 0.5275 0.2767 0.0670 1.0000 Uiso R . . . . . H461 H 0.8011 0.5307 0.3476 0.0930 1.0000 Uiso R . . . . . H462 H 0.7090 0.5366 0.3856 0.0930 1.0000 Uiso R . . . . . H463 H 0.7270 0.4716 0.3532 0.0930 1.0000 Uiso R . . . . . H471 H 0.4969 0.3949 0.1228 0.0757 1.0000 Uiso R . . . . . H472 H 0.4307 0.3331 0.1116 0.0757 1.0000 Uiso R . . . . . H481 H 0.4019 0.4122 0.0468 0.1180 1.0000 Uiso R . . . . . H482 H 0.3704 0.4629 0.0909 0.1180 1.0000 Uiso R . . . . . H483 H 0.3042 0.4011 0.0797 0.1180 1.0000 Uiso R . . . . . H541 H 0.2301 0.6368 0.2582 0.0792 0.6000 Uiso R . . . . . H542 H 0.3328 0.6540 0.2323 0.0792 0.6000 Uiso R . . . . . H543 H 0.3285 0.6130 0.2855 0.0792 0.6000 Uiso R . . . . . H5011 H 0.3355 0.4507 0.5404 0.1110 1.0000 Uiso R . . . . . H5012 H 0.2347 0.4127 0.5457 0.1110 1.0000 Uiso R . . . . . H5013 H 0.3354 0.3742 0.5485 0.1110 1.0000 Uiso R . . . . . H5021 H 0.8781 0.2352 0.0945 0.1180 0.5000 Uiso R . . . . . H5022 H 0.9858 0.2065 0.0900 0.1180 0.5000 Uiso R . . . . . H5023 H 0.8938 0.1600 0.0831 0.1180 0.5000 Uiso 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 Sm1 0.03117(15) 0.03321(15) 0.02895(14) -0.00136(14) 0.00128(12) 0.00450(15) Pd2 0.0303(2) 0.0338(2) 0.0279(2) 0.0003(2) 0.00206(16) 0.0024(2) Pd3 0.0296(2) 0.0322(2) 0.02285(18) -0.00681(18) 0.00065(16) 0.00281(19) N1 0.043(3) 0.035(3) 0.034(3) 0.001(2) 0.000(2) -0.002(2) N2 0.044(3) 0.036(3) 0.035(3) 0.000(2) -0.001(2) -0.003(2) N3 0.048(3) 0.036(3) 0.024(2) -0.007(2) 0.001(2) 0.004(2) N4 0.031(3) 0.036(3) 0.022(2) -0.0040(19) -0.0004(19) 0.006(2) O1 0.039(3) 0.042(2) 0.041(3) 0.007(2) 0.000(2) 0.015(2) O2 0.042(3) 0.037(2) 0.038(2) 0.0133(19) 0.001(2) 0.012(2) O3 0.055(3) 0.041(2) 0.023(2) 0.0038(17) 0.003(2) 0.012(2) O4 0.035(3) 0.045(3) 0.054(3) 0.011(2) -0.002(2) 0.010(2) O5 0.038(2) 0.037(2) 0.037(2) -0.0150(19) -0.001(2) 0.0005(19) O6 0.035(2) 0.035(2) 0.031(2) -0.0104(18) 0.0008(19) -0.0052(18) O7 0.026(2) 0.042(2) 0.046(3) -0.006(2) -0.002(2) -0.0045(19) O8 0.042(3) 0.052(3) 0.028(2) -0.003(2) 0.009(2) -0.001(2) O9 0.051(3) 0.044(2) 0.039(2) -0.001(2) -0.002(2) 0.009(3) O11 0.073(4) 0.079(4) 0.067(4) -0.012(3) 0.001(3) -0.030(3) O12 0.079(4) 0.069(4) 0.060(3) 0.004(3) 0.012(3) -0.003(3) O13 0.086(4) 0.054(3) 0.055(3) -0.013(3) -0.002(3) -0.011(3) O21 0.157(5) 0.129(5) 0.211(7) 0.036(5) -0.027(6) -0.054(6) O22 0.102(5) 0.109(5) 0.085(4) -0.029(4) -0.016(4) -0.030(4) O23 0.125(5) 0.194(6) 0.128(5) -0.073(5) 0.022(5) -0.017(6) O31 0.121(5) 0.075(6) 0.080(6) 0.050(5) 0.007(6) 0.031(5) O32 0.107(5) 0.099(6) 0.078(6) -0.022(6) 0.000(6) -0.046(6) O33 0.103(6) 0.092(7) 0.072(6) -0.018(5) 0.002(6) -0.017(6) O41 0.105(5) 0.081(6) 0.092(6) 0.018(6) -0.022(5) 0.008(6) O42 0.115(5) 0.037(4) 0.033(5) 0.006(3) 0.007(4) 0.013(4) O43 0.121(6) 0.098(6) 0.082(5) 0.009(6) 0.015(6) -0.008(6) O501 0.072(4) 0.086(4) 0.070(4) 0.024(3) -0.010(3) 0.009(4) O502 0.099(6) 0.101(7) 0.123(7) 0.001(7) -0.004(7) 0.021(7) O503 0.243(6) 0.087(6) 0.093(7) -0.026(6) -0.086(7) 0.106(6) O504 0.091(5) 0.047(5) 0.067(5) -0.001(4) 0.006(5) 0.009(5) O513 0.253(6) 0.079(6) 0.121(8) -0.024(6) -0.075(7) 0.085(7) O514 0.089(6) 0.083(7) 0.083(7) -0.001(6) -0.021(7) 0.029(6) C1 0.026(3) 0.033(3) 0.028(3) 0.003(2) -0.004(2) 0.004(2) C2 0.036(3) 0.031(3) 0.032(3) -0.003(2) -0.001(3) -0.004(2) C3 0.039(3) 0.040(3) 0.042(4) 0.007(3) -0.011(3) -0.001(3) C4 0.044(4) 0.036(3) 0.056(4) 0.008(3) -0.013(3) 0.004(3) C5 0.027(3) 0.034(3) 0.048(4) -0.002(3) -0.009(3) 0.005(2) C6 0.033(3) 0.029(3) 0.043(3) 0.000(3) -0.006(3) 0.007(2) C7 0.036(3) 0.042(3) 0.041(3) 0.000(3) 0.010(3) 0.007(3) C8 0.029(3) 0.038(3) 0.040(3) 0.000(3) 0.014(3) -0.007(3) C9 0.043(4) 0.063(4) 0.061(5) -0.005(4) 0.016(4) 0.001(4) C10 0.034(3) 0.075(5) 0.071(5) -0.002(4) 0.021(4) -0.003(4) C11 0.071(5) 0.076(5) 0.063(5) 0.005(4) 0.024(4) -0.019(4) C12 0.065(4) 0.055(4) 0.051(4) 0.003(3) 0.038(4) 0.004(4) C13 0.025(3) 0.048(3) 0.045(4) -0.002(3) 0.010(3) -0.006(3) C14 0.053(4) 0.036(3) 0.040(3) 0.003(3) 0.006(3) -0.005(3) C15 0.034(3) 0.037(3) 0.035(3) 0.004(3) -0.004(2) 0.001(3) C16 0.056(4) 0.034(3) 0.045(4) 0.008(3) -0.013(3) -0.010(3) C17 0.042(4) 0.051(4) 0.047(4) 0.014(3) -0.016(3) 0.010(3) C18 0.042(3) 0.042(4) 0.044(4) 0.007(3) -0.005(3) 0.010(3) C19 0.034(3) 0.037(3) 0.039(3) -0.001(3) -0.004(2) 0.004(3) C20 0.030(3) 0.031(3) 0.036(3) 0.000(2) 0.001(2) -0.002(2) C21 0.035(3) 0.033(3) 0.037(3) -0.007(2) -0.004(3) 0.003(2) C22 0.043(3) 0.028(3) 0.041(3) -0.005(3) -0.011(3) 0.001(3) C23 0.040(4) 0.039(4) 0.072(5) -0.015(3) -0.025(3) -0.001(3) C24 0.078(5) 0.039(3) 0.058(4) -0.020(3) -0.033(4) 0.010(4) C25 0.061(4) 0.045(4) 0.046(4) -0.019(3) -0.008(3) 0.008(3) C26 0.044(3) 0.035(3) 0.038(3) -0.012(3) -0.004(3) 0.008(3) C27 0.044(3) 0.038(3) 0.051(4) -0.021(3) -0.003(3) 0.009(3) C28 0.027(3) 0.042(3) 0.034(3) -0.012(3) 0.006(2) -0.009(3) C29 0.066(4) 0.068(5) 0.029(3) -0.009(3) 0.006(3) 0.017(4) C30 0.045(4) 0.082(5) 0.051(4) -0.017(4) 0.024(4) 0.009(4) C31 0.042(4) 0.077(5) 0.045(4) -0.008(4) 0.014(3) 0.003(4) C32 0.035(3) 0.063(4) 0.041(4) -0.003(3) 0.012(3) 0.005(3) C33 0.043(3) 0.052(3) 0.013(2) -0.011(2) 0.011(2) 0.006(3) C34 0.043(3) 0.036(3) 0.028(3) 0.001(2) 0.007(3) -0.003(3) C35 0.040(3) 0.028(3) 0.031(3) -0.011(2) -0.001(2) 0.000(2) C36 0.034(3) 0.051(4) 0.045(4) -0.014(3) -0.003(3) -0.007(3) C37 0.051(4) 0.077(5) 0.043(4) -0.034(4) -0.005(3) -0.003(4) C38 0.045(4) 0.057(4) 0.040(3) -0.019(3) 0.004(3) -0.003(3) C39 0.033(3) 0.040(3) 0.027(3) -0.006(2) 0.001(2) 0.002(3) C40 0.033(3) 0.033(3) 0.022(2) -0.007(2) -0.003(2) 0.003(2) C41 0.067(4) 0.068(4) 0.032(3) 0.013(3) 0.011(4) 0.026(4) C42 0.134(6) 0.084(6) 0.065(6) -0.003(5) 0.002(6) 0.013(6) C43 0.042(3) 0.070(4) 0.076(5) 0.033(4) 0.012(3) 0.024(4) C44 0.065(6) 0.073(7) 0.072(7) 0.018(6) 0.019(6) 0.030(7) C45 0.040(4) 0.053(4) 0.076(5) -0.007(4) 0.004(4) -0.009(3) C46 0.047(4) 0.062(5) 0.132(7) 0.002(5) -0.032(5) 0.003(4) C47 0.057(4) 0.098(6) 0.039(4) -0.015(4) 0.026(4) -0.023(4) C48 0.151(6) 0.114(7) 0.038(4) 0.020(5) -0.013(5) -0.034(6) C54 0.064(5) 0.070(6) 0.075(7) 0.023(5) -0.001(6) 0.034(5) C100 0.141(5) 0.087(5) 0.061(4) -0.032(4) 0.051(4) -0.056(5) C200 0.089(5) 0.085(5) 0.126(6) -0.052(5) 0.004(5) -0.010(5) C300 0.135(6) 0.075(7) 0.136(7) 0.043(6) -0.013(7) -0.022(6) C400 0.072(6) 0.069(6) 0.240(7) 0.014(7) -0.023(7) 0.017(5) C501 0.069(5) 0.133(7) 0.072(5) 0.016(5) 0.000(5) -0.010(6) C502 0.074(6) 0.049(7) 0.105(7) -0.010(7) -0.008(7) -0.023(6) S1 0.0679(14) 0.0531(11) 0.0346(9) -0.0088(8) 0.0048(9) -0.0145(10) S2 0.0843(19) 0.0560(13) 0.0795(17) -0.0075(12) -0.0120(15) -0.0144(13) S3 0.069(3) 0.047(2) 0.059(2) -0.0059(19) 0.001(2) -0.0102(18) S4 0.099(4) 0.051(2) 0.063(3) 0.002(2) -0.021(3) 0.006(3) F11 0.180(5) 0.084(4) 0.091(4) -0.035(3) 0.066(4) -0.028(4) F12 0.203(5) 0.108(4) 0.054(3) -0.015(3) 0.042(4) -0.060(4) F13 0.133(4) 0.133(5) 0.105(4) -0.039(4) 0.069(4) -0.048(4) F21 0.073(4) 0.122(4) 0.121(5) -0.049(4) -0.005(4) -0.016(4) F22 0.161(5) 0.180(6) 0.141(5) -0.032(5) 0.037(5) -0.013(6) F23 0.130(5) 0.105(4) 0.155(6) -0.032(4) -0.039(5) 0.020(4) F31 0.168(5) 0.106(6) 0.178(7) 0.065(6) -0.003(7) 0.001(6) F32 0.149(5) 0.105(7) 0.181(7) 0.034(6) 0.003(7) -0.051(6) F33 0.153(6) 0.110(6) 0.134(6) 0.055(5) 0.003(6) -0.033(6) F41 0.101(6) 0.093(7) 0.267(6) -0.011(7) 0.001(6) 0.001(6) F42 0.085(5) 0.061(5) 0.283(7) 0.000(6) -0.009(6) 0.009(5) F43 0.076(5) 0.128(7) 0.289(7) 0.016(7) -0.032(6) 0.023(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.17897(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sm1 . Pd2 . 3.4580(6) yes Sm1 . Pd3 . 3.4694(6) yes Sm1 . O1 . 2.332(5) yes Sm1 . O2 . 2.343(5) yes Sm1 . O3 . 2.665(5) yes Sm1 . O4 . 2.630(5) yes Sm1 . O5 . 2.349(5) yes Sm1 . O6 . 2.321(5) yes Sm1 . O7 . 2.629(5) yes Sm1 . O8 . 2.677(5) yes Sm1 . O9 . 2.463(5) yes Pd2 . N1 . 1.990(6) yes Pd2 . N2 . 2.004(6) yes Pd2 . O1 . 1.984(5) yes Pd2 . O2 . 2.009(5) yes Pd3 . N3 . 2.008(5) yes Pd3 . N4 . 1.979(6) yes Pd3 . O5 . 2.014(5) yes Pd3 . O6 . 1.996(5) yes N1 . C7 . 1.488(9) yes N1 . C8 . 1.497(9) yes N1 . H1 . 0.960 no N2 . C13 . 1.508(10) yes N2 . C14 . 1.498(9) yes N2 . H2 . 0.960 no N3 . C27 . 1.459(10) yes N3 . C28 . 1.470(9) yes N3 . H3 . 0.960 no N4 . C33 . 1.508(7) yes N4 . C34 . 1.486(8) yes N4 . H4 . 0.960 no O1 . C1 . 1.327(8) yes O2 . C20 . 1.356(8) yes O3 . C2 . 1.386(9) yes O3 . C41 . 1.456(9) yes O4 . C19 . 1.370(9) yes O4 . C43 . 1.472(9) yes O5 . C21 . 1.336(8) yes O6 . C40 . 1.343(7) yes O7 . C22 . 1.382(9) yes O7 . C45 . 1.476(10) yes O8 . C39 . 1.374(9) yes O8 . C47 . 1.471(9) yes O9 . H5 . 0.830 no O9 . H6 . 0.841 no O11 . S1 . 1.432(5) yes O12 . S1 . 1.423(5) yes O13 . S1 . 1.418(5) yes O21 . S2 . 1.389(7) yes O22 . S2 . 1.418(6) yes O23 . S2 . 1.446(7) yes O31 . S3 . 1.443(7) yes O32 . S3 . 1.408(7) yes O33 . S3 . 1.428(7) yes O41 . S4 . 1.465(8) yes O42 . S4 . 1.387(7) yes O43 . S4 . 1.429(8) yes O501 . C501 . 1.390(8) yes O501 . H9 . 0.845 no O502 . C502 . 1.396(9) yes O502 . H11 . 0.957 no O503 . O513 . 1.36(3) yes O504 . O514 . 1.57(2) yes C1 . C2 . 1.418(10) yes C1 . C6 . 1.412(9) yes C2 . C3 . 1.382(10) yes C3 . C4 . 1.412(12) yes C3 . H31 . 0.960 no C4 . C5 . 1.338(12) yes C4 . H41 . 0.960 no C5 . C6 . 1.451(9) yes C5 . H51 . 0.960 no C6 . C7 . 1.482(11) yes C7 . H71 . 0.960 no C7 . H72 . 0.960 no C8 . C9 . 1.506(12) yes C8 . C13 . 1.512(10) yes C8 . H81 . 0.960 no C9 . C10 . 1.540(13) yes C9 . H91 . 0.960 no C9 . H92 . 0.960 no C10 . C11 . 1.518(15) yes C10 . H101 . 0.960 no C10 . H102 . 0.960 no C11 . C12 . 1.503(15) yes C11 . H111 . 0.960 no C11 . H112 . 0.960 no C12 . C13 . 1.524(11) yes C12 . H121 . 0.960 no C12 . H122 . 0.960 no C13 . H131 . 0.960 no C14 . C15 . 1.527(10) yes C14 . H141 . 0.960 no C14 . H142 . 0.960 no C15 . C16 . 1.390(10) yes C15 . C20 . 1.393(9) yes C16 . C17 . 1.367(12) yes C16 . H161 . 0.960 no C17 . C18 . 1.402(12) yes C17 . H171 . 0.960 no C18 . C19 . 1.388(10) yes C18 . H181 . 0.960 no C19 . C20 . 1.392(9) yes C21 . C22 . 1.391(10) yes C21 . C26 . 1.408(10) yes C22 . C23 . 1.404(9) yes C23 . C24 . 1.394(13) yes C23 . H231 . 0.960 no C24 . C25 . 1.370(14) yes C24 . H241 . 0.960 no C25 . C26 . 1.403(10) yes C25 . H251 . 0.960 no C26 . C27 . 1.519(11) yes C27 . H271 . 0.960 no C27 . H272 . 0.960 no C28 . C29 . 1.503(10) yes C28 . C33 . 1.533(10) yes C28 . H281 . 0.960 no C29 . C30 . 1.516(14) yes C29 . H291 . 0.960 no C29 . H292 . 0.960 no C30 . C31 . 1.493(14) yes C30 . H301 . 0.960 no C30 . H302 . 0.960 no C31 . C32 . 1.561(11) yes C31 . H311 . 0.960 no C31 . H312 . 0.960 no C32 . C33 . 1.501(10) yes C32 . H321 . 0.960 no C32 . H322 . 0.960 no C33 . H331 . 0.960 no C34 . C35 . 1.523(9) yes C34 . H341 . 0.960 no C34 . H342 . 0.960 no C35 . C36 . 1.399(9) yes C35 . C40 . 1.382(10) yes C36 . C37 . 1.389(12) yes C36 . H361 . 0.960 no C37 . C38 . 1.376(13) yes C37 . H371 . 0.960 no C38 . C39 . 1.398(10) yes C38 . H381 . 0.960 no C39 . C40 . 1.394(9) yes C41 . C42 . 1.427(16) yes C41 . H411 . 0.960 no C41 . H412 . 0.960 no C42 . H421 . 0.960 no C42 . H422 . 0.960 no C42 . H423 . 0.960 no C43 . C44 . 1.554(9) yes C43 . C54 . 1.566(9) yes C43 . H431 . 0.960 no C43 . H432 . 0.960 no C43 . H433 . 0.960 no C43 . H434 . 0.960 no C44 . H441 . 0.960 no C44 . H442 . 0.960 no C44 . H443 . 0.960 no C45 . C46 . 1.442(15) yes C45 . H451 . 0.960 no C45 . H452 . 0.960 no C46 . H461 . 0.960 no C46 . H462 . 0.960 no C46 . H463 . 0.960 no C47 . C48 . 1.506(17) yes C47 . H471 . 0.960 no C47 . H472 . 0.960 no C48 . H481 . 0.960 no C48 . H482 . 0.960 no C48 . H483 . 0.960 no C54 . H541 . 0.960 no C54 . H542 . 0.960 no C54 . H543 . 0.960 no C100 . S1 . 1.773(7) yes C100 . F11 . 1.332(7) yes C100 . F12 . 1.342(8) yes C100 . F13 . 1.338(8) yes C200 . S2 . 1.737(8) yes C200 . F21 . 1.304(7) yes C200 . F22 . 1.354(8) yes C200 . F23 . 1.320(8) yes C300 . S3 . 1.769(8) yes C300 . F31 . 1.335(9) yes C300 . F32 . 1.332(9) yes C300 . F33 . 1.333(9) yes C400 . S4 . 1.753(9) yes C400 . F41 . 1.331(9) yes C400 . F42 . 1.327(9) yes C400 . F43 . 1.327(9) yes C501 . H5011 . 0.967 no C501 . H5012 . 0.966 no C501 . H5013 . 0.955 no C502 . H5021 . 0.960 no C502 . H5022 . 0.960 no C502 . H5023 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Pd2 . Sm1 . Pd3 . 175.052(15) yes Pd2 . Sm1 . O1 . 33.43(12) yes Pd3 . Sm1 . O1 . 150.58(12) yes Pd2 . Sm1 . O2 . 34.14(12) yes Pd3 . Sm1 . O2 . 141.17(12) yes O1 . Sm1 . O2 . 67.01(17) yes Pd2 . Sm1 . O3 . 93.06(12) yes Pd3 . Sm1 . O3 . 90.38(12) yes O1 . Sm1 . O3 . 60.48(17) yes O2 . Sm1 . O3 . 123.12(18) yes Pd2 . Sm1 . O4 . 94.50(12) yes Pd3 . Sm1 . O4 . 80.86(12) yes O1 . Sm1 . O4 . 126.87(17) yes O2 . Sm1 . O4 . 60.37(17) yes O3 . Sm1 . O4 . 153.18(17) yes Pd2 . Sm1 . O5 . 143.49(12) yes Pd3 . Sm1 . O5 . 34.08(12) yes O1 . Sm1 . O5 . 131.59(17) yes O2 . Sm1 . O5 . 126.32(17) yes O3 . Sm1 . O5 . 79.42(17) yes Pd2 . Sm1 . O6 . 147.82(11) yes Pd3 . Sm1 . O6 . 33.43(11) yes O1 . Sm1 . O6 . 145.03(17) yes O2 . Sm1 . O6 . 130.90(17) yes O3 . Sm1 . O6 . 105.13(17) yes Pd2 . Sm1 . O7 . 83.17(11) yes Pd3 . Sm1 . O7 . 94.57(11) yes O1 . Sm1 . O7 . 80.69(17) yes O2 . Sm1 . O7 . 80.25(18) yes O3 . Sm1 . O7 . 71.53(16) yes Pd2 . Sm1 . O8 . 87.98(11) yes Pd3 . Sm1 . O8 . 92.23(11) yes O1 . Sm1 . O8 . 104.72(17) yes O2 . Sm1 . O8 . 78.80(18) yes O3 . Sm1 . O8 . 133.50(16) yes Pd2 . Sm1 . O9 . 91.07(13) yes Pd3 . Sm1 . O9 . 93.52(13) yes O1 . Sm1 . O9 . 72.64(19) yes O2 . Sm1 . O9 . 115.89(18) yes O3 . Sm1 . O9 . 67.68(18) yes O4 . Sm1 . O5 . 79.23(18) yes O4 . Sm1 . O6 . 81.20(17) yes O5 . Sm1 . O6 . 67.33(16) yes O4 . Sm1 . O7 . 83.88(17) yes O5 . Sm1 . O7 . 60.49(16) yes O6 . Sm1 . O7 . 127.50(15) yes O4 . Sm1 . O8 . 72.52(18) yes O5 . Sm1 . O8 . 122.98(16) yes O6 . Sm1 . O8 . 60.21(15) yes O7 . Sm1 . O8 . 154.05(16) yes O4 . Sm1 . O9 . 137.71(19) yes O5 . Sm1 . O9 . 117.79(18) yes O6 . Sm1 . O9 . 72.39(18) yes O7 . Sm1 . O9 . 138.40(18) yes O8 . Sm1 . O9 . 65.82(18) yes Sm1 . Pd2 . N1 . 136.26(17) yes Sm1 . Pd2 . N2 . 135.71(19) yes N1 . Pd2 . N2 . 87.4(2) yes Sm1 . Pd2 . O1 . 40.37(14) yes N1 . Pd2 . O1 . 96.2(2) yes N2 . Pd2 . O1 . 175.4(2) yes Sm1 . Pd2 . O2 . 40.88(13) yes N1 . Pd2 . O2 . 175.5(2) yes N2 . Pd2 . O2 . 96.0(2) yes O1 . Pd2 . O2 . 80.53(19) yes Sm1 . Pd3 . N3 . 137.30(18) yes Sm1 . Pd3 . N4 . 135.47(14) yes N3 . Pd3 . N4 . 87.1(2) yes Sm1 . Pd3 . O5 . 40.82(13) yes N3 . Pd3 . O5 . 96.8(2) yes N4 . Pd3 . O5 . 175.4(2) yes Sm1 . Pd3 . O6 . 39.85(13) yes N3 . Pd3 . O6 . 177.1(2) yes N4 . Pd3 . O6 . 95.68(19) yes O5 . Pd3 . O6 . 80.44(18) yes Pd2 . N1 . C7 . 111.4(4) yes Pd2 . N1 . C8 . 107.2(4) yes C7 . N1 . C8 . 114.5(5) yes Pd2 . N1 . H1 . 107.8 no C7 . N1 . H1 . 107.9 no C8 . N1 . H1 . 107.8 no Pd2 . N2 . C13 . 106.1(4) yes Pd2 . N2 . C14 . 110.4(4) yes C13 . N2 . C14 . 113.5(6) yes Pd2 . N2 . H2 . 108.7 no C13 . N2 . H2 . 109.2 no C14 . N2 . H2 . 108.9 no Pd3 . N3 . C27 . 110.8(4) yes Pd3 . N3 . C28 . 107.6(4) yes C27 . N3 . C28 . 113.9(6) yes Pd3 . N3 . H3 . 108.2 no C27 . N3 . H3 . 107.9 no C28 . N3 . H3 . 108.4 no Pd3 . N4 . C33 . 107.9(4) yes Pd3 . N4 . C34 . 111.6(4) yes C33 . N4 . C34 . 115.4(5) yes Pd3 . N4 . H4 . 107.2 no C33 . N4 . H4 . 106.5 no C34 . N4 . H4 . 107.8 no Sm1 . O1 . Pd2 . 106.2(2) yes Sm1 . O1 . C1 . 129.5(4) yes Pd2 . O1 . C1 . 124.0(4) yes Sm1 . O2 . Pd2 . 104.98(19) yes Sm1 . O2 . C20 . 131.3(4) yes Pd2 . O2 . C20 . 123.7(4) yes Sm1 . O3 . C2 . 116.5(4) yes Sm1 . O3 . C41 . 122.2(5) yes C2 . O3 . C41 . 119.8(6) yes Sm1 . O4 . C19 . 119.8(4) yes Sm1 . O4 . C43 . 124.9(5) yes C19 . O4 . C43 . 115.0(6) yes Sm1 . O5 . Pd3 . 105.09(19) yes Sm1 . O5 . C21 . 131.0(4) yes Pd3 . O5 . C21 . 123.4(4) yes Sm1 . O6 . Pd3 . 106.72(19) yes Sm1 . O6 . C40 . 129.7(4) yes Pd3 . O6 . C40 . 123.6(4) yes Sm1 . O7 . C22 . 118.9(4) yes Sm1 . O7 . C45 . 124.1(5) yes C22 . O7 . C45 . 116.8(6) yes Sm1 . O8 . C39 . 115.9(4) yes Sm1 . O8 . C47 . 124.5(5) yes C39 . O8 . C47 . 117.7(6) yes Sm1 . O9 . H5 . 106.0 no Sm1 . O9 . H6 . 122.1 no H5 . O9 . H6 . 106.2 no C501 . O501 . H9 . 108.8 no C502 . O502 . H11 . 108.8 no O1 . C1 . C2 . 115.7(6) yes O1 . C1 . C6 . 123.1(6) yes C2 . C1 . C6 . 121.1(6) yes C1 . C2 . O3 . 112.8(6) yes C1 . C2 . C3 . 122.0(7) yes O3 . C2 . C3 . 125.1(7) yes C2 . C3 . C4 . 117.1(7) yes C2 . C3 . H31 . 121.7 no C4 . C3 . H31 . 121.1 no C3 . C4 . C5 . 121.8(7) yes C3 . C4 . H41 . 119.2 no C5 . C4 . H41 . 119.0 no C4 . C5 . C6 . 123.4(7) yes C4 . C5 . H51 . 118.1 no C6 . C5 . H51 . 118.5 no C5 . C6 . C1 . 114.5(7) yes C5 . C6 . C7 . 120.4(6) yes C1 . C6 . C7 . 124.7(6) yes N1 . C7 . C6 . 113.1(6) yes N1 . C7 . H71 . 108.8 no C6 . C7 . H71 . 108.4 no N1 . C7 . H72 . 108.6 no C6 . C7 . H72 . 108.4 no H71 . C7 . H72 . 109.5 no N1 . C8 . C9 . 112.5(7) yes N1 . C8 . C13 . 107.4(6) yes C9 . C8 . C13 . 111.5(6) yes N1 . C8 . H81 . 108.5 no C9 . C8 . H81 . 108.4 no C13 . C8 . H81 . 108.5 no C8 . C9 . C10 . 110.2(8) yes C8 . C9 . H91 . 108.9 no C10 . C9 . H91 . 109.3 no C8 . C9 . H92 . 109.6 no C10 . C9 . H92 . 109.3 no H91 . C9 . H92 . 109.5 no C9 . C10 . C11 . 111.5(8) yes C9 . C10 . H101 . 108.6 no C11 . C10 . H101 . 108.4 no C9 . C10 . H102 . 109.2 no C11 . C10 . H102 . 109.6 no H101 . C10 . H102 . 109.5 no C10 . C11 . C12 . 112.8(8) yes C10 . C11 . H111 . 109.2 no C12 . C11 . H111 . 108.4 no C10 . C11 . H112 . 108.5 no C12 . C11 . H112 . 108.5 no H111 . C11 . H112 . 109.5 no C11 . C12 . C13 . 110.9(8) yes C11 . C12 . H121 . 109.3 no C13 . C12 . H121 . 109.7 no C11 . C12 . H122 . 109.1 no C13 . C12 . H122 . 108.4 no H121 . C12 . H122 . 109.5 no C12 . C13 . C8 . 111.9(6) yes C12 . C13 . N2 . 113.4(7) yes C8 . C13 . N2 . 108.6(6) yes C12 . C13 . H131 . 107.1 no C8 . C13 . H131 . 107.8 no N2 . C13 . H131 . 107.8 no N2 . C14 . C15 . 115.0(6) yes N2 . C14 . H141 . 108.3 no C15 . C14 . H141 . 108.1 no N2 . C14 . H142 . 107.9 no C15 . C14 . H142 . 108.1 no H141 . C14 . H142 . 109.5 no C14 . C15 . C16 . 117.1(6) yes C14 . C15 . C20 . 124.0(6) yes C16 . C15 . C20 . 118.5(7) yes C15 . C16 . C17 . 121.3(8) yes C15 . C16 . H161 . 119.5 no C17 . C16 . H161 . 119.2 no C16 . C17 . C18 . 120.4(7) yes C16 . C17 . H171 . 119.7 no C18 . C17 . H171 . 120.0 no C17 . C18 . C19 . 118.9(7) yes C17 . C18 . H181 . 120.5 no C19 . C18 . H181 . 120.6 no C18 . C19 . O4 . 125.9(6) yes C18 . C19 . C20 . 120.2(7) yes O4 . C19 . C20 . 113.9(6) yes C15 . C20 . C19 . 120.5(6) yes C15 . C20 . O2 . 124.8(6) yes C19 . C20 . O2 . 114.6(6) yes O5 . C21 . C22 . 115.2(6) yes O5 . C21 . C26 . 124.4(7) yes C22 . C21 . C26 . 120.3(6) yes C21 . C22 . O7 . 113.9(6) yes C21 . C22 . C23 . 121.5(7) yes O7 . C22 . C23 . 124.6(7) yes C22 . C23 . C24 . 116.5(8) yes C22 . C23 . H231 . 121.9 no C24 . C23 . H231 . 121.6 no C23 . C24 . C25 . 123.2(7) yes C23 . C24 . H241 . 118.3 no C25 . C24 . H241 . 118.4 no C24 . C25 . C26 . 120.0(8) yes C24 . C25 . H251 . 119.9 no C26 . C25 . H251 . 120.1 no C21 . C26 . C25 . 118.2(7) yes C21 . C26 . C27 . 125.1(6) yes C25 . C26 . C27 . 116.2(6) yes C26 . C27 . N3 . 117.6(6) yes C26 . C27 . H271 . 107.4 no N3 . C27 . H271 . 107.3 no C26 . C27 . H272 . 107.4 no N3 . C27 . H272 . 107.5 no H271 . C27 . H272 . 109.5 no N3 . C28 . C29 . 115.1(6) yes N3 . C28 . C33 . 109.2(6) yes C29 . C28 . C33 . 110.0(6) yes N3 . C28 . H281 . 107.7 no C29 . C28 . H281 . 107.4 no C33 . C28 . H281 . 107.2 no C28 . C29 . C30 . 111.8(7) yes C28 . C29 . H291 . 108.7 no C30 . C29 . H291 . 109.0 no C28 . C29 . H292 . 108.7 no C30 . C29 . H292 . 109.3 no H291 . C29 . H292 . 109.5 no C29 . C30 . C31 . 112.7(8) yes C29 . C30 . H301 . 108.5 no C31 . C30 . H301 . 108.3 no C29 . C30 . H302 . 108.9 no C31 . C30 . H302 . 109.0 no H301 . C30 . H302 . 109.5 no C30 . C31 . C32 . 109.7(8) yes C30 . C31 . H311 . 109.5 no C32 . C31 . H311 . 110.0 no C30 . C31 . H312 . 109.3 no C32 . C31 . H312 . 108.9 no H311 . C31 . H312 . 109.5 no C31 . C32 . C33 . 109.7(7) yes C31 . C32 . H321 . 110.1 no C33 . C32 . H321 . 109.5 no C31 . C32 . H322 . 108.9 no C33 . C32 . H322 . 109.1 no H321 . C32 . H322 . 109.5 no C28 . C33 . N4 . 107.5(6) yes C28 . C33 . C32 . 113.0(6) yes N4 . C33 . C32 . 114.2(6) yes C28 . C33 . H331 . 106.9 no N4 . C33 . H331 . 107.3 no C32 . C33 . H331 . 107.6 no N4 . C34 . C35 . 112.9(5) yes N4 . C34 . H341 . 109.1 no C35 . C34 . H341 . 109.1 no N4 . C34 . H342 . 108.0 no C35 . C34 . H342 . 108.3 no H341 . C34 . H342 . 109.5 no C34 . C35 . C36 . 116.9(6) yes C34 . C35 . C40 . 124.0(6) yes C36 . C35 . C40 . 119.0(6) yes C35 . C36 . C37 . 120.0(7) yes C35 . C36 . H361 . 120.1 no C37 . C36 . H361 . 119.9 no C36 . C37 . C38 . 120.9(7) yes C36 . C37 . H371 . 120.0 no C38 . C37 . H371 . 119.1 no C37 . C38 . C39 . 119.3(7) yes C37 . C38 . H381 . 120.2 no C39 . C38 . H381 . 120.5 no C38 . C39 . O8 . 126.4(6) yes C38 . C39 . C40 . 119.9(7) yes O8 . C39 . C40 . 113.7(6) yes C39 . C40 . C35 . 120.7(6) yes C39 . C40 . O6 . 115.6(6) yes C35 . C40 . O6 . 123.7(6) yes O3 . C41 . C42 . 114.3(10) yes O3 . C41 . H411 . 108.8 no C42 . C41 . H411 . 109.5 no O3 . C41 . H412 . 108.1 no C42 . C41 . H412 . 106.5 no H411 . C41 . H412 . 109.5 no C41 . C42 . H421 . 111.0 no C41 . C42 . H422 . 107.2 no H421 . C42 . H422 . 109.5 no C41 . C42 . H423 . 110.2 no H421 . C42 . H423 . 109.5 no H422 . C42 . H423 . 109.5 no O4 . C43 . C44 . 102.9(11) yes O4 . C43 . C54 . 107.4(9) yes O4 . C43 . H431 . 111.2 no C44 . C43 . H431 . 111.6 no O4 . C43 . H432 . 110.5 no C44 . C43 . H432 . 111.1 no H431 . C43 . H432 . 109.5 no O4 . C43 . H433 . 109.5 no C54 . C43 . H433 . 109.7 no O4 . C43 . H434 . 109.5 no C44 . C43 . H434 . 75.9 no C54 . C43 . H434 . 111.2 no H433 . C43 . H434 . 109.5 no C43 . C44 . H441 . 107.3 no C43 . C44 . H442 . 110.3 no H441 . C44 . H442 . 109.5 no C43 . C44 . H443 . 110.8 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no O7 . C45 . C46 . 112.8(9) yes O7 . C45 . H451 . 108.7 no C46 . C45 . H451 . 109.6 no O7 . C45 . H452 . 108.8 no C46 . C45 . H452 . 107.5 no H451 . C45 . H452 . 109.5 no C45 . C46 . H461 . 110.3 no C45 . C46 . H462 . 108.0 no H461 . C46 . H462 . 109.5 no C45 . C46 . H463 . 110.1 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no O8 . C47 . C48 . 110.4(9) yes O8 . C47 . H471 . 109.1 no C48 . C47 . H471 . 109.6 no O8 . C47 . H472 . 108.9 no C48 . C47 . H472 . 109.3 no H471 . C47 . H472 . 109.5 no C47 . C48 . H481 . 108.4 no C47 . C48 . H482 . 109.8 no H481 . C48 . H482 . 109.5 no C47 . C48 . H483 . 110.2 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no C43 . C54 . H541 . 108.7 no C43 . C54 . H542 . 110.6 no H541 . C54 . H542 . 109.5 no C43 . C54 . H543 . 109.1 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no S1 . C100 . F11 . 113.7(6) yes S1 . C100 . F12 . 112.1(6) yes F11 . C100 . F12 . 105.7(6) yes S1 . C100 . F13 . 112.4(6) yes F11 . C100 . F13 . 105.8(7) yes F12 . C100 . F13 . 106.5(6) yes S2 . C200 . F21 . 117.9(7) yes S2 . C200 . F22 . 97.6(8) yes F21 . C200 . F22 . 107.8(8) yes S2 . C200 . F23 . 116.6(7) yes F21 . C200 . F23 . 109.9(7) yes F22 . C200 . F23 . 105.1(7) yes S3 . C300 . F31 . 111.7(11) yes S3 . C300 . F32 . 110.2(11) yes F31 . C300 . F32 . 106.0(9) yes S3 . C300 . F33 . 116.1(12) yes F31 . C300 . F33 . 106.7(9) yes F32 . C300 . F33 . 105.5(9) yes S4 . C400 . F41 . 113.5(14) yes S4 . C400 . F42 . 109.5(10) yes F41 . C400 . F42 . 106.8(9) yes S4 . C400 . F43 . 111.4(12) yes F41 . C400 . F43 . 107.2(9) yes F42 . C400 . F43 . 108.2(9) yes O501 . C501 . H5011 . 109.6 no O501 . C501 . H5012 . 109.6 no H5011 . C501 . H5012 . 108.4 no O501 . C501 . H5013 . 110.5 no H5011 . C501 . H5013 . 109.3 no H5012 . C501 . H5013 . 109.4 no O502 . C502 . H5021 . 107.5 no O502 . C502 . H5022 . 111.0 no H5021 . C502 . H5022 . 109.5 no O502 . C502 . H5023 . 109.9 no H5021 . C502 . H5023 . 109.5 no H5022 . C502 . H5023 . 109.5 no C100 . S1 . O11 . 103.6(4) yes C100 . S1 . O12 . 103.4(4) yes O11 . S1 . O12 . 113.4(4) yes C100 . S1 . O13 . 104.8(4) yes O11 . S1 . O13 . 115.0(4) yes O12 . S1 . O13 . 114.8(4) yes C200 . S2 . O23 . 103.3(7) yes C200 . S2 . O22 . 107.3(5) yes O23 . S2 . O22 . 111.0(5) yes C200 . S2 . O21 . 99.9(8) yes O23 . S2 . O21 . 115.2(6) yes O22 . S2 . O21 . 118.1(6) yes C300 . S3 . O31 . 102.8(9) yes C300 . S3 . O33 . 105.9(10) yes O31 . S3 . O33 . 112.2(7) yes C300 . S3 . O32 . 106.0(10) yes O31 . S3 . O32 . 113.5(7) yes O33 . S3 . O32 . 115.1(7) yes C400 . S4 . O41 . 101.0(9) yes C400 . S4 . O43 . 104.3(11) yes O41 . S4 . O43 . 111.2(7) yes C400 . S4 . O42 . 111.2(8) yes O41 . S4 . O42 . 110.5(6) yes O43 . S4 . O42 . 117.3(7) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N1 . H1 . O32 . 140 0.96 2.10 2.897(2) yes N1 . H1 . O42 . 173 0.96 2.00 2.957(2) yes N2 . H2 . O13 . 167 0.96 1.94 2.884(2) yes N3 . H3 . O501 . 164 0.96 1.90 2.837(2) yes N4 . H4 . O31 1_455 153 0.96 1.95 2.842(2) yes O9 . H6 . O504 . 176 0.84 1.79 2.628(2) yes O501 . H9 . O21 3_645 157 0.84 2.10 2.895(2) yes O502 . H11 . O33 3_745 170 0.96 1.95 2.900(2) yes