# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Shashank Mishra' _publ_contact_author_address ;Universit\'e Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne C\'edex France. ; _publ_contact_author_email mishrashashank74@rediffmail.com _publ_contact_author_phone '(+33) 472445329' _publ_contact_author_fax '(+33) 472445399' loop_ _publ_author_name _publ_author_address _publ_author_footnote S.Mishra ;Universit\'e Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne C\'edex France ; ; ? # Footnote for author 1 ; G.Ledoux ;Universit\'e Claude Bernard Lyon 1 Laboratoire de Physico Chimie des Materiaux Luminescent 10 rue A. M. Ampere 69622 Villeurbanne C\'edex France ; ; ? # Footnote 2 ; E.Jeanneau ;Centre de Diffractom\'etrie Henri Longchambon Universit\'e Claude Bernard Lyon 1 B\^at Raulin RdC 69622 Villeurbanne C\'edex France ; '' S.Daniele ;Universit\'e Claude Bernard Lyon 1 IRCELYON 2 avenue A. Einstein 69626 Villeurbanne C\'edex France ; '' M.F.Joubert ;Universit\'e Claude Bernard Lyon 1 Laboratoire de Physico Chimie des Materiaux Luminescent 10 rue A. M. Ampere 69622 Villeurbanne C\'edex France ; '' _publ_section_title ; Novel heterometal-organic complexes as first single source precursors for up-converting NaY(Ln)F4 (Ln = Yb, Er, Tm) nanomaterials ; #looking for refcif # 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. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' # Attachment '- RevCIF_DT-ART-06-2011-011070.cif' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 796485' #TrackingRef '- RevCIF_DT-ART-06-2011-011070.cif' _audit_creation_date 11-09-06 _audit_creation_method CRYSTALS_ver_14.21 _oxford_structure_analysis_title 'smr147 in P c c a' _chemical_name_systematic ? _chemical_melting_point ? _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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 (Cooper et al, 2010). Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; The compound showed highly disordered trifluoroacetate ligands. In order to get correct geometry for these moieties, restraints on the C-F bond lengths were applied. The displacement parameters of fluorine and carbon atoms were also forced to be similar. ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 29.260(4) _cell_length_b 11.8630(10) _cell_length_c 18.725(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6499.7(13) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c a ' _symmetry_space_group_name_Hall '-P 2a 2ac' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 x,-y,z+1/2 -x,y,-z+1/2 -x+1/2,-y,z x+1/2,y,-z 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' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Y -2.7962 3.5667 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 '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' _cell_formula_units_Z 4 # Given Formula = C20 H25 F16 Na2 O1 Y1 # Dc = 1.47 Fooo = 3000.00 Mu = 19.24 M = 720.27 # Found Formula = C19 H26 F10.50 Na0.50 O12 Y1 # Dc = 1.53 FOOO = 3000.00 Mu = 19.11 M = 746.29 _chemical_formula_sum 'C38 H52 F21 Na O24 Y2' _chemical_formula_moiety 'C22 H16 F21 O16 Y2, C16 H36 Na O8' _chemical_compound_source ? _chemical_formula_weight 1492.61 _cell_measurement_reflns_used 3538 _cell_measurement_theta_min 3.0993 _cell_measurement_theta_max 29.3474 _cell_measurement_temperature 180 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.180 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_max 0.480 _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3000 _exptl_absorpt_coefficient_mu 1.911 # Sheldrick geometric approximatio 0.63 0.71 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.71 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 180 _diffrn_reflns_number 7725 _reflns_number_total 7725 _diffrn_reflns_av_R_equivalents 0.095 # Number of reflections without Friedels Law is 7725 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 9011 _diffrn_reflns_theta_min 3.102 _diffrn_reflns_theta_max 29.445 _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 25.029 _diffrn_measured_fraction_theta_full 0.949 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min 0 _reflns_limit_h_max 39 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _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 difmap _refine_diff_density_min -2.29 _refine_diff_density_max 2.43 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 7725 _refine_ls_number_restraints 141 _refine_ls_number_parameters 457 _oxford_refine_ls_R_factor_ref 0.2072 _refine_ls_wR_factor_ref 0.1857 _refine_ls_goodness_of_fit_ref 1.2329 _refine_ls_shift/su_max 0.0004611 _refine_ls_shift/su_mean 0.0000377 # The values computed from all data _oxford_reflns_number_all 7725 _refine_ls_R_factor_all 0.2072 _refine_ls_wR_factor_all 0.1857 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2334 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_gt 0.0955 # 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 . _refine_ls_structure_factor_coef Fsqd _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: 965. 0.124E+04 378. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Oxford Diffraction, (2010). CrysAlisPro. Oxford Diffraction, (2002). Xcalibur User Manual. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 F1 F 0.6430(9) 0.319(3) 0.8011(17) 0.1100 0.4081 Uani . U . 2 1 . F2 F 0.6432(9) 0.512(3) 0.8035(16) 0.1096 0.4081 Uani . U . 2 1 . F3 F 0.6569(8) 0.432(3) 0.7097(15) 0.1082 0.4081 Uani . U . 2 1 . F4 F 0.6470(6) 0.3277(16) 0.7471(12) 0.1075 0.5919 Uani D U . 2 2 . F5 F 0.6346(6) 0.4087(18) 0.8439(8) 0.1052 0.5919 Uani D U . 2 2 . F6 F 0.6512(6) 0.4963(19) 0.7525(13) 0.1102 0.5919 Uani . U . 2 2 . F7 F 0.5124(7) 0.8047(14) 0.8150(6) 0.0959 0.5000 Uani D U . . . . F8 F 0.5331(6) 0.8176(18) 0.7141(11) 0.0916 0.5000 Uani D U . . . . F9 F 0.5389(5) 0.8196(16) 0.7620(13) 0.0870 0.5000 Uani D U . . . . F10 F 0.4164(5) 0.8135(11) 0.5698(7) 0.1478 1.0000 Uani . U . . . . F11 F 0.3792(4) 0.6827(10) 0.6130(6) 0.1361 1.0000 Uani . U . . . . F12 F 0.3668(4) 0.7368(12) 0.5115(7) 0.1506 1.0000 Uani . U . . . . F13 F 0.3660(7) 0.291(2) 0.4810(14) 0.1452 0.5427 Uani D U . 1 2 . F14 F 0.4047(9) 0.233(3) 0.3942(8) 0.1410 0.5427 Uani D U . 1 2 . F15 F 0.4085(9) 0.1634(18) 0.5003(14) 0.1393 0.5427 Uani D U . 1 2 . F16 F 0.3809(10) 0.235(3) 0.5175(11) 0.1411 0.4573 Uani D U . 1 1 . F17 F 0.3839(11) 0.274(3) 0.4029(11) 0.1415 0.4573 Uani D U . 1 1 . F18 F 0.4335(8) 0.172(2) 0.4536(16) 0.1440 0.4573 Uani D U . 1 1 . Y1 Y 0.50578(4) 0.44338(10) 0.61719(5) 0.0418 1.0000 Uani . . . . . . O8 O 0.5145(3) 0.2401(7) 0.6505(4) 0.0537 1.0000 Uani . . . . . . C9 C 0.4772(5) 0.1604(14) 0.6503(7) 0.0709 1.0000 Uani . . . . . . C10 C 0.4960(8) 0.0656(14) 0.6002(11) 0.1206 1.0000 Uani . . . . . . C11 C 0.5457(7) 0.0682(16) 0.6115(13) 0.1307 1.0000 Uani . . . . . . C12 C 0.5572(5) 0.1777(12) 0.6490(8) 0.0730 1.0000 Uani . . . . . . O1 O 0.5688(3) 0.4261(9) 0.6920(4) 0.0600 1.0000 Uani . . . . . . C1 C 0.5766(4) 0.4144(9) 0.7553(7) 0.0444 1.0000 Uani . U . . . . O2 O 0.5516(3) 0.3987(8) 0.8058(4) 0.0567 1.0000 Uani . . . . . . C2 C 0.6301(6) 0.4143(14) 0.7765(8) 0.0715 1.0000 Uani D U . . . . O7 O 0.4588(4) 0.3399(8) 0.5400(5) 0.0660 1.0000 Uani . . . . . . C7 C 0.4421(5) 0.3514(14) 0.4786(7) 0.0582 1.0000 Uani . U . . . . O6 O 0.4499(3) 0.4179(9) 0.4335(5) 0.0604 1.0000 Uani . . . . . . C8 C 0.4037(7) 0.2486(17) 0.4607(7) 0.0907 1.0000 Uani D U . . . . O4 O 0.4505(3) 0.5649(9) 0.5700(5) 0.0611 1.0000 Uani . . . . . . C5 C 0.4350(6) 0.6347(15) 0.5259(9) 0.0844 1.0000 Uani . U . . . . O5 O 0.4441(4) 0.6426(9) 0.4636(5) 0.0674 1.0000 Uani . . . . . . C6 C 0.3988(9) 0.707(2) 0.5575(13) 0.1257 1.0000 Uani . U . . . . O3 O 0.5026(4) 0.5996(7) 0.6915(4) 0.0712 1.0000 Uani . . . . . . C3 C 0.5000 0.6427(13) 0.7500 0.0534 1.0000 Uani S TU . . . . C4 C 0.5000 0.7788(16) 0.7500 0.0824 1.0000 Uani DS TU . . . . Na1 Na 0.2500 0.0000 0.7584(4) 0.0519 1.0000 Uani S T . . . . O9 O 0.2862(5) 0.1156(12) 0.6601(7) 0.1060 1.0000 Uani . . . . . . C42 C 0.2605(9) 0.1773(19) 0.6074(9) 0.1482 1.0000 Uani . . . . . . C43 C 0.3311(9) 0.085(2) 0.6343(12) 0.1483 1.0000 Uani . . . . . . C44 C 0.3527(7) 0.017(2) 0.6906(12) 0.1288 1.0000 Uani . . . . . . O10 O 0.3276(4) -0.0753(14) 0.7075(6) 0.1010 1.0000 Uani . . . . . . C46 C 0.3495(7) -0.161(2) 0.7541(13) 0.1262 1.0000 Uani . . . . . . C47 C 0.3142(7) -0.2452(16) 0.7746(11) 0.1139 1.0000 Uani . . . . . . O11 O 0.2801(5) -0.1868(10) 0.8139(7) 0.0947 1.0000 Uani . . . . . . C49 C 0.2414(8) -0.2555(14) 0.8258(12) 0.1212 1.0000 Uani . . . . . . C50 C 0.2134(8) -0.1964(17) 0.8779(11) 0.1157 1.0000 Uani . . . . . . O12 O 0.2017(4) -0.0901(11) 0.8573(5) 0.0847 1.0000 Uani . . . . . . C52 C 0.1815(6) -0.0306(18) 0.9138(9) 0.1183 1.0000 Uani . . . . . . H91 H 0.4723 0.1326 0.6971 0.0932 1.0000 Uiso R . . . . . H92 H 0.4490 0.1953 0.6313 0.0928 1.0000 Uiso R . . . . . H101 H 0.4824 -0.0053 0.6157 0.1402 1.0000 Uiso R . . . . . H102 H 0.4882 0.0719 0.5498 0.1402 1.0000 Uiso R . . . . . H112 H 0.5532 0.0067 0.6456 0.1591 1.0000 Uiso R . . . . . H111 H 0.5623 0.0563 0.5687 0.1591 1.0000 Uiso R . . . . . H121 H 0.5682 0.1648 0.6983 0.0859 1.0000 Uiso R . . . . . H122 H 0.5802 0.2195 0.6217 0.0859 1.0000 Uiso R . . . . . H421 H 0.2327 0.2075 0.6281 0.2209 1.0000 Uiso R . . . . . H422 H 0.2529 0.1349 0.5664 0.2210 1.0000 Uiso R . . . . . H423 H 0.2795 0.2378 0.5924 0.2210 1.0000 Uiso R . . . . . H431 H 0.3293 0.0393 0.5917 0.1390 1.0000 Uiso R . . . . . H432 H 0.3485 0.1510 0.6235 0.1392 1.0000 Uiso R . . . . . H441 H 0.3825 -0.0088 0.6735 0.1418 1.0000 Uiso R . . . . . H442 H 0.3561 0.0605 0.7346 0.1419 1.0000 Uiso R . . . . . H461 H 0.3744 -0.2025 0.7286 0.1279 1.0000 Uiso R . . . . . H462 H 0.3622 -0.1236 0.7962 0.1280 1.0000 Uiso R . . . . . H472 H 0.3273 -0.3072 0.8001 0.1262 1.0000 Uiso R . . . . . H471 H 0.3000 -0.2696 0.7291 0.1258 1.0000 Uiso R . . . . . H491 H 0.2500 -0.3284 0.8402 0.1331 1.0000 Uiso R . . . . . H492 H 0.2235 -0.2580 0.7821 0.1330 1.0000 Uiso R . . . . . H501 H 0.2329 -0.1882 0.9214 0.1441 1.0000 Uiso R . . . . . H502 H 0.1863 -0.2386 0.8903 0.1441 1.0000 Uiso R . . . . . H522 H 0.1709 0.0407 0.8966 0.1731 1.0000 Uiso R . . . . . H521 H 0.2032 -0.0208 0.9512 0.1730 1.0000 Uiso R . . . . . H523 H 0.1562 -0.0759 0.9304 0.1730 1.0000 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 F1 0.081(8) 0.137(11) 0.112(11) 0.002(10) -0.002(10) 0.003(9) F2 0.081(7) 0.139(10) 0.109(10) -0.006(9) 0.000(9) -0.003(8) F3 0.081(6) 0.140(10) 0.104(9) -0.007(9) -0.001(8) -0.002(7) F4 0.082(6) 0.142(9) 0.099(9) -0.008(8) -0.011(7) -0.001(7) F5 0.082(6) 0.143(10) 0.091(8) -0.003(8) -0.023(7) -0.011(7) F6 0.088(7) 0.146(10) 0.096(9) 0.001(9) -0.020(8) -0.025(8) F7 0.106(8) 0.063(6) 0.119(10) -0.009(6) -0.010(8) -0.014(5) F8 0.095(8) 0.060(5) 0.119(10) -0.004(6) -0.003(8) -0.019(4) F9 0.089(8) 0.057(5) 0.115(10) -0.003(6) -0.004(8) -0.024(5) F10 0.186(9) 0.097(7) 0.160(8) -0.036(7) 0.038(7) 0.043(7) F11 0.171(8) 0.132(7) 0.106(7) 0.004(7) 0.081(7) 0.074(7) F12 0.146(9) 0.176(9) 0.130(8) -0.005(8) -0.002(7) 0.087(8) F13 0.145(14) 0.165(15) 0.126(10) 0.002(10) -0.001(9) -0.077(11) F14 0.148(14) 0.160(14) 0.114(9) 0.003(9) -0.007(8) -0.081(10) F15 0.151(14) 0.155(14) 0.112(9) 0.011(9) -0.007(8) -0.084(10) F16 0.154(15) 0.159(14) 0.110(9) 0.012(9) -0.009(8) -0.085(10) F17 0.157(15) 0.159(14) 0.109(9) 0.007(9) -0.017(9) -0.083(11) F18 0.160(15) 0.158(15) 0.114(10) 0.005(10) -0.016(9) -0.080(11) Y1 0.0591(7) 0.0452(5) 0.0210(4) 0.0024(5) 0.0055(5) 0.0067(7) O8 0.065(6) 0.051(5) 0.046(4) 0.011(4) 0.006(4) 0.009(5) C9 0.076(11) 0.086(12) 0.051(8) 0.030(9) 0.002(7) -0.025(10) C10 0.149(18) 0.061(10) 0.152(18) 0.002(13) 0.004(19) -0.006(16) C11 0.130(17) 0.071(13) 0.19(2) -0.002(17) 0.055(19) 0.004(14) C12 0.088(12) 0.052(10) 0.078(10) 0.018(8) 0.008(9) 0.029(9) O1 0.062(6) 0.078(7) 0.040(5) 0.012(5) -0.008(4) -0.003(6) C1 0.050(7) 0.041(6) 0.043(6) -0.005(6) -0.019(6) 0.010(5) O2 0.078(7) 0.069(7) 0.023(4) 0.003(4) 0.011(4) -0.011(5) C2 0.083(8) 0.062(8) 0.070(8) -0.012(7) 0.003(7) 0.003(8) O7 0.102(8) 0.058(7) 0.038(5) -0.008(5) -0.022(5) 0.005(6) C7 0.059(8) 0.079(10) 0.037(6) -0.027(7) 0.002(6) 0.010(7) O6 0.079(7) 0.067(7) 0.035(5) 0.010(5) 0.019(4) -0.006(6) C8 0.088(10) 0.119(12) 0.065(8) -0.021(9) 0.011(8) 0.018(9) O4 0.063(6) 0.066(7) 0.054(6) -0.020(6) 0.009(5) 0.009(6) C5 0.115(10) 0.072(9) 0.066(8) 0.000(8) 0.018(8) 0.055(8) O5 0.098(8) 0.064(7) 0.041(5) 0.012(5) 0.013(5) 0.014(6) C6 0.153(8) 0.114(7) 0.109(7) -0.007(7) 0.031(6) 0.067(7) O3 0.124(8) 0.062(6) 0.028(4) -0.010(4) 0.010(6) 0.005(7) C3 0.064(9) 0.029(7) 0.067(9) 0.0000 0.007(9) 0.0000 C4 0.090(8) 0.056(6) 0.101(9) 0.0000 -0.003(8) 0.0000 Na1 0.053(4) 0.062(4) 0.040(4) 0.0000 0.0000 -0.006(4) O9 0.124(11) 0.120(12) 0.074(8) -0.004(8) 0.027(8) -0.047(9) C42 0.25(3) 0.13(2) 0.064(12) 0.039(14) 0.006(17) -0.04(2) C43 0.18(2) 0.17(3) 0.097(16) -0.009(17) 0.081(18) -0.08(2) C44 0.105(17) 0.16(2) 0.123(18) -0.056(18) 0.057(16) -0.059(17) O10 0.076(8) 0.137(12) 0.090(8) -0.035(9) 0.002(7) -0.013(9) C46 0.107(17) 0.16(2) 0.114(16) -0.079(18) -0.040(16) 0.070(17) C47 0.109(17) 0.100(15) 0.13(2) -0.030(15) -0.056(15) 0.017(14) O11 0.097(9) 0.072(8) 0.115(10) -0.037(8) -0.010(8) 0.010(8) C49 0.15(2) 0.049(11) 0.17(2) 0.023(14) -0.023(18) -0.027(13) C50 0.18(2) 0.075(14) 0.093(14) 0.004(14) 0.009(16) -0.006(15) O12 0.111(10) 0.090(10) 0.053(6) 0.018(6) 0.003(6) -0.018(8) C52 0.120(15) 0.16(2) 0.074(11) 0.002(14) 0.039(11) 0.011(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.622(11) 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 F1 . C2 . 1.28(3) yes F2 . C2 . 1.32(3) yes F3 . C2 . 1.49(3) yes F4 . C2 . 1.266(9) yes F5 . C2 . 1.271(9) yes F6 . C2 . 1.24(2) yes F7 . F8 6_656 1.45(2) yes F7 . F9 . 1.27(2) yes F7 . C4 . 1.306(9) yes F8 . F9 . 0.91(2) yes F8 . C4 . 1.266(9) yes F9 . C4 . 1.258(9) yes F10 . C6 . 1.38(3) yes F11 . C6 . 1.22(2) yes F12 . C6 . 1.32(2) yes F13 . C8 . 1.272(10) yes F14 . C8 . 1.259(10) yes F15 . C8 . 1.261(10) yes F16 . C8 . 1.266(10) yes F17 . C8 . 1.261(10) yes F18 . C8 . 1.263(10) yes Y1 . O5 2_666 2.342(10) yes Y1 . O6 2_666 2.301(9) yes Y1 . O2 6_656 2.275(9) yes Y1 . O8 . 2.504(8) yes Y1 . O1 . 2.324(8) yes Y1 . O7 . 2.342(9) yes Y1 . O4 . 2.340(10) yes Y1 . O3 . 2.320(7) yes O8 . C9 . 1.445(14) yes O8 . C12 . 1.453(15) yes C9 . C10 . 1.56(2) yes C9 . H91 . 0.948 no C9 . H92 . 0.989 no C10 . C11 . 1.47(2) yes C10 . H101 . 0.975 no C10 . H102 . 0.974 no C11 . C12 . 1.52(2) yes C11 . H112 . 0.993 no C11 . H111 . 0.949 no C12 . H121 . 0.990 no C12 . H122 . 0.979 no O1 . C1 . 1.216(14) yes C1 . O2 . 1.211(14) yes C1 . C2 . 1.613(19) yes O7 . C7 . 1.258(15) yes C7 . O6 . 1.177(17) yes C7 . C8 . 1.69(2) yes O4 . C5 . 1.253(17) yes C5 . O5 . 1.200(17) yes C5 . C6 . 1.49(2) yes O3 . C3 . 1.211(9) yes C3 . C4 . 1.61(2) yes Na1 . O9 7_555 2.529(13) yes Na1 . O12 7_555 2.562(12) yes Na1 . O11 7_555 2.601(13) yes Na1 . O10 7_555 2.619(12) yes Na1 . O9 . 2.529(13) yes Na1 . O10 . 2.619(12) yes Na1 . O11 . 2.601(13) yes Na1 . O12 . 2.562(12) yes O9 . C42 . 1.44(2) yes O9 . C43 . 1.45(2) yes C42 . H421 . 0.971 no C42 . H422 . 0.945 no C42 . H423 . 0.950 no C43 . C44 . 1.47(3) yes C43 . H431 . 0.965 no C43 . H432 . 0.958 no C44 . O10 . 1.35(2) yes C44 . H441 . 0.978 no C44 . H442 . 0.981 no O10 . C46 . 1.49(2) yes C46 . C47 . 1.49(2) yes C46 . H461 . 0.999 no C46 . H462 . 0.980 no C47 . O11 . 1.42(2) yes C47 . H472 . 0.958 no C47 . H471 . 0.990 no O11 . C49 . 1.41(2) yes C49 . C50 . 1.45(2) yes C49 . H491 . 0.940 no C49 . H492 . 0.971 no C50 . O12 . 1.36(2) yes C50 . H501 . 0.999 no C50 . H502 . 0.966 no O12 . C52 . 1.403(18) yes C52 . H522 . 0.958 no C52 . H521 . 0.953 no C52 . H523 . 0.966 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 F8 6_656 F7 . F9 . 104.7(11) yes F8 6_656 F7 . C4 . 54.5(7) yes F9 . F7 . C4 . 58.4(7) yes F7 6_656 F8 . F9 . 122.9(15) yes F7 6_656 F8 . C4 . 57.1(7) yes F9 . F8 . C4 . 68.3(10) yes F7 . F9 . F8 . 130.4(14) yes F7 . F9 . C4 . 62.2(8) yes F8 . F9 . C4 . 69.2(10) yes O5 2_666 Y1 . O6 2_666 72.0(4) yes O5 2_666 Y1 . O2 6_656 140.4(3) yes O6 2_666 Y1 . O2 6_656 147.6(3) yes O5 2_666 Y1 . O8 . 71.2(3) yes O6 2_666 Y1 . O8 . 137.2(3) yes O2 6_656 Y1 . O8 . 72.1(3) yes O5 2_666 Y1 . O1 . 81.6(3) yes O6 2_666 Y1 . O1 . 82.2(3) yes O2 6_656 Y1 . O1 . 100.5(3) yes O8 . Y1 . O1 . 71.6(3) yes O5 2_666 Y1 . O7 . 75.0(3) yes O6 2_666 Y1 . O7 . 116.8(3) yes O2 6_656 Y1 . O7 . 80.5(3) yes O8 . Y1 . O7 . 73.1(3) yes O1 . Y1 . O7 . 142.3(4) yes O5 2_666 Y1 . O4 . 117.2(3) yes O6 2_666 Y1 . O4 . 78.1(3) yes O2 6_656 Y1 . O4 . 82.7(3) yes O8 . Y1 . O4 . 139.3(3) yes O1 . Y1 . O4 . 146.1(4) yes O5 2_666 Y1 . O3 . 139.5(4) yes O6 2_666 Y1 . O3 . 72.5(3) yes O2 6_656 Y1 . O3 . 77.1(3) yes O8 . Y1 . O3 . 128.6(3) yes O1 . Y1 . O3 . 75.0(4) yes O7 . Y1 . O4 . 71.6(3) yes O7 . Y1 . O3 . 140.0(4) yes O4 . Y1 . O3 . 72.9(3) yes Y1 . O8 . C9 . 123.6(8) yes Y1 . O8 . C12 . 125.0(8) yes C9 . O8 . C12 . 108.5(10) yes O8 . C9 . C10 . 101.9(12) yes O8 . C9 . H91 . 109.8 no C10 . C9 . H91 . 111.0 no O8 . C9 . H92 . 110.9 no C10 . C9 . H92 . 112.3 no H91 . C9 . H92 . 110.7 no C9 . C10 . C11 . 104.3(17) yes C9 . C10 . H101 . 107.4 no C11 . C10 . H101 . 112.2 no C9 . C10 . H102 . 116.4 no C11 . C10 . H102 . 111.7 no H101 . C10 . H102 . 104.9 no C10 . C11 . C12 . 107.7(16) yes C10 . C11 . H112 . 107.3 no C12 . C11 . H112 . 106.4 no C10 . C11 . H111 . 112.5 no C12 . C11 . H111 . 113.9 no H112 . C11 . H111 . 108.6 no C11 . C12 . O8 . 104.7(13) yes C11 . C12 . H121 . 111.8 no O8 . C12 . H121 . 109.9 no C11 . C12 . H122 . 110.3 no O8 . C12 . H122 . 110.1 no H121 . C12 . H122 . 109.9 no Y1 . O1 . C1 . 138.4(9) yes O1 . C1 . O2 . 131.6(12) yes O1 . C1 . C2 . 115.0(12) yes O2 . C1 . C2 . 113.3(11) yes C1 . O2 . Y1 6_656 154.9(9) yes F3 . C2 . C1 . 107.8(14) yes F3 . C2 . F2 . 93(2) yes C1 . C2 . F2 . 112.0(17) yes F3 . C2 . F1 . 106(2) yes C1 . C2 . F1 . 112.0(19) yes F2 . C2 . F1 . 124(2) yes C1 . C2 . F5 . 110.2(15) yes C1 . C2 . F4 . 105.8(15) yes F5 . C2 . F4 . 110.4(18) yes C1 . C2 . F6 . 113.3(15) yes F5 . C2 . F6 . 110.4(19) yes F4 . C2 . F6 . 106.5(19) yes Y1 . O7 . C7 . 137.4(11) yes O7 . C7 . O6 . 130.7(16) yes O7 . C7 . C8 . 111.2(13) yes O6 . C7 . C8 . 118.0(12) yes Y1 2_666 O6 . C7 . 152.2(11) yes C7 . C8 . F16 . 106.1(17) yes C7 . C8 . F18 . 94.4(18) yes F16 . C8 . F18 . 111(3) yes C7 . C8 . F17 . 108(2) yes F16 . C8 . F17 . 121(3) yes F18 . C8 . F17 . 113(2) yes C7 . C8 . F13 . 103.2(18) yes C7 . C8 . F15 . 112.8(17) yes F13 . C8 . F15 . 104(2) yes C7 . C8 . F14 . 106.7(19) yes F13 . C8 . F14 . 112(2) yes F15 . C8 . F14 . 117(2) yes Y1 . O4 . C5 . 154.9(11) yes O4 . C5 . O5 . 127.7(15) yes O4 . C5 . C6 . 112.2(16) yes O5 . C5 . C6 . 119.9(17) yes Y1 2_666 O5 . C5 . 137.1(11) yes C5 . C6 . F10 . 109(2) yes C5 . C6 . F12 . 113.5(20) yes F10 . C6 . F12 . 97.5(18) yes C5 . C6 . F11 . 122(2) yes F10 . C6 . F11 . 105(2) yes F12 . C6 . F11 . 107(2) yes Y1 . O3 . C3 . 151.9(9) yes O3 . C3 . O3 6_656 130.1(15) yes O3 . C3 . C4 . 115.0(8) yes O3 6_656 C3 . C4 . 115.0(8) yes C3 . C4 . F7 6_656 103.6(12) yes C3 . C4 . F7 . 103.6(12) yes F7 6_656 C4 . F7 . 153(2) yes C3 . C4 . F8 6_656 111.3(13) yes F7 6_656 C4 . F8 6_656 101.4(13) yes F7 . C4 . F8 6_656 68.4(11) yes C3 . C4 . F8 . 111.3(13) yes F7 6_656 C4 . F8 . 68.4(11) yes F7 . C4 . F8 . 101.4(13) yes F8 6_656 C4 . F8 . 137(3) yes C3 . C4 . F9 6_656 112.7(13) yes F7 6_656 C4 . F9 6_656 59.4(11) yes F7 . C4 . F9 6_656 109.1(15) yes F8 6_656 C4 . F9 6_656 42.5(11) yes F8 . C4 . F9 6_656 117.2(15) yes C3 . C4 . F9 . 112.7(13) yes F7 6_656 C4 . F9 . 109.1(15) yes F7 . C4 . F9 . 59.4(11) yes F8 6_656 C4 . F9 . 117.2(15) yes F8 . C4 . F9 . 42.5(11) yes F9 6_656 C4 . F9 . 135(3) yes O9 7_555 Na1 . O12 7_555 169.5(5) yes O9 7_555 Na1 . O11 7_555 127.6(5) yes O12 7_555 Na1 . O11 7_555 62.8(4) yes O9 7_555 Na1 . O10 7_555 63.7(5) yes O12 7_555 Na1 . O10 7_555 126.8(5) yes O11 7_555 Na1 . O10 7_555 64.0(5) yes O9 7_555 Na1 . O9 . 86.5(6) yes O12 7_555 Na1 . O9 . 93.9(4) yes O11 7_555 Na1 . O9 . 88.3(4) yes O10 7_555 Na1 . O9 . 85.0(5) yes O9 7_555 Na1 . O10 . 85.0(5) yes O12 7_555 Na1 . O10 . 85.8(4) yes O11 7_555 Na1 . O10 . 136.8(4) yes O10 7_555 Na1 . O10 . 137.3(6) yes O9 . Na1 . O10 . 63.7(5) yes O9 7_555 Na1 . O11 . 88.3(4) yes O12 7_555 Na1 . O11 . 83.1(4) yes O11 7_555 Na1 . O11 . 133.0(6) yes O10 7_555 Na1 . O11 . 136.8(4) yes O9 . Na1 . O11 . 127.6(5) yes O9 7_555 Na1 . O12 . 93.9(4) yes O12 7_555 Na1 . O12 . 87.5(6) yes O11 7_555 Na1 . O12 . 83.1(4) yes O10 7_555 Na1 . O12 . 85.8(4) yes O9 . Na1 . O12 . 169.5(5) yes O10 . Na1 . O11 . 64.0(5) yes O10 . Na1 . O12 . 126.8(5) yes O11 . Na1 . O12 . 62.8(4) yes Na1 . O9 . C42 . 123.8(12) yes Na1 . O9 . C43 . 119.1(14) yes C42 . O9 . C43 . 112.0(16) yes O9 . C42 . H421 . 110.6 no O9 . C42 . H422 . 114.2 no H421 . C42 . H422 . 108.9 no O9 . C42 . H423 . 106.5 no H421 . C42 . H423 . 109.2 no H422 . C42 . H423 . 107.3 no O9 . C43 . C44 . 106.9(16) yes O9 . C43 . H431 . 111.6 no C44 . C43 . H431 . 108.0 no O9 . C43 . H432 . 110.2 no C44 . C43 . H432 . 111.9 no H431 . C43 . H432 . 108.3 no C43 . C44 . O10 . 112.1(19) yes C43 . C44 . H441 . 108.6 no O10 . C44 . H441 . 108.3 no C43 . C44 . H442 . 110.7 no O10 . C44 . H442 . 106.8 no H441 . C44 . H442 . 110.3 no C44 . O10 . Na1 . 106.4(12) yes C44 . O10 . C46 . 117.1(17) yes Na1 . O10 . C46 . 113.2(11) yes O10 . C46 . C47 . 108.2(16) yes O10 . C46 . H461 . 111.7 no C47 . C46 . H461 . 107.5 no O10 . C46 . H462 . 109.0 no C47 . C46 . H462 . 111.2 no H461 . C46 . H462 . 109.3 no C46 . C47 . O11 . 107.1(15) yes C46 . C47 . H472 . 111.5 no O11 . C47 . H472 . 113.4 no C46 . C47 . H471 . 105.4 no O11 . C47 . H471 . 107.1 no H472 . C47 . H471 . 111.9 no C47 . O11 . Na1 . 116.5(12) yes C47 . O11 . C49 . 111.3(15) yes Na1 . O11 . C49 . 106.4(10) yes O11 . C49 . C50 . 106.2(16) yes O11 . C49 . H491 . 111.3 no C50 . C49 . H491 . 113.7 no O11 . C49 . H492 . 108.4 no C50 . C49 . H492 . 106.1 no H491 . C49 . H492 . 110.9 no C49 . C50 . O12 . 113.4(17) yes C49 . C50 . H501 . 105.9 no O12 . C50 . H501 . 106.5 no C49 . C50 . H502 . 111.9 no O12 . C50 . H502 . 109.9 no H501 . C50 . H502 . 108.8 no C50 . O12 . Na1 . 116.9(12) yes C50 . O12 . C52 . 110.9(14) yes Na1 . O12 . C52 . 124.6(11) yes O12 . C52 . H522 . 109.1 no O12 . C52 . H521 . 109.6 no H522 . C52 . H521 . 110.8 no O12 . C52 . H523 . 106.6 no H522 . C52 . H523 . 110.5 no H521 . C52 . H523 . 110.0 no _iucr_refine_instruction_details_constraints ; # # Punched on 06/09/11 at 10:14:41 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) RIDE C ( 11,X'S) H ( 112,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S) RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) RIDE C ( 46,X'S) H ( 461,X'S) H ( 462,X'S) RIDE C ( 47,X'S) H ( 472,X'S) H ( 471,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) RIDE C ( 52,X'S) H ( 522,X'S) H ( 521,X'S) H ( 523,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 06/09/11 at 10:14:41 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) DISTANCE 1.250000 , 0.010000 = F(7) TO C(4) DISTANCE 1.250000 , 0.010000 = F(8) TO C(4) DISTANCE 1.250000 , 0.010000 = F(9) TO C(4) DISTANCE 1.250000 , 0.010000 = F(5) TO C(2) DISTANCE 1.250000 , 0.010000 = F(4) TO C(2) DISTANCE 1.250000 , 0.010000 = F(13) TO C(8) DISTANCE 1.250000 , 0.010000 = F(14) TO C(8) DISTANCE 1.250000 , 0.010000 = F(15) TO C(8) DISTANCE 1.250000 , 0.010000 = F(16) TO C(8) DISTANCE 1.250000 , 0.010000 = F(17) TO C(8) DISTANCE 1.250000 , 0.010000 = F(18) TO C(8) U(IJ)'S 0.0, 0.0050000 = F(7) TO F(8) U(IJ)'S 0.0, 0.0050000 = F(8) TO F(9) U(IJ)'S 0.0, 0.0050000 = F(13) TO F(14) U(IJ)'S 0.0, 0.005000 = F(14) TO F(15) U(IJ)'S 0.0, 0.005000 = F(15) TO F(16) U(IJ)'S 0.0, 0.005000 = F(16) TO F(17) U(IJ)'S 0.0, 0.005000 = F(17) TO F(18) U(IJ)'S 0.0, 0.005000 = F(1) TO F(2) U(IJ)'S 0.0, 0.005000 = F(2) TO F(3) U(IJ)'S 0.0, 0.005000 = F(3) TO F(4) U(IJ)'S 0.0, 0.005000 = F(4) TO F(5) U(IJ)'S 0.0, 0.005000 = F(5) TO F(6) U(IJ)'S 0.0, 0.010000 = C(7) TO C(8) U(IJ)'S 0.0, 0.010000 = C(1) TO C(2) U(IJ)'S 0.0, 0.010000 = F(7) TO C(4) U(IJ)'S 0.0, 0.010000 = F(8) TO C(4) U(IJ)'S 0.0, 0.010000 = F(9) TO C(4) U(IJ)'S 0.0, 0.010000 = C(3) TO C(4) U(IJ)'S 0.0, 0.010000 = C(5) TO C(6) U(IJ)'S 0.0, 0.010000 = F(10) TO C(6) U(IJ)'S 0.0, 0.010000 = F(11) TO C(6) U(IJ)'S 0.0, 0.010000 = F(12) TO C(6) END ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.500 0.535 184 42 ' ' 2 0.250 0.500 1.035 184 43 ' ' 3 0.750 0.500 -0.035 184 44 ' ' 4 0.750 0.500 0.465 184 44 ' ' #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 796486' #TrackingRef '- RevCIF_DT-ART-06-2011-011070.cif' _audit_creation_date 11-09-06 _audit_creation_method CRYSTALS_ver_14.21 _oxford_structure_analysis_title 'import in P 21 c n' _chemical_name_systematic ? _chemical_melting_point ? _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_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _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 Fig. ; ? ; _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 (Cooper et al, 2010). Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; A few atoms showed unusually high displacement parameters. The incriminated atoms were constrained to have thermal parameters similar to a chemically related atom. One C-C distance of the solvent moiety was also too short and was thus constrianed to the expected C-C distance. ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 17.8642(3) _cell_length_b 19.6674(4) _cell_length_c 21.2130(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7453.0(2) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 c n ' _symmetry_space_group_name_Hall 'P -2n 2a' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y,-z x,-y+1/2,z+1/2 x+1/2,y+1/2,-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' 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' 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' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Y -2.7962 3.5667 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C45 H55 F30 Na2.50 O32.50 Y2.50 # Dc = 1.75 Fooo = 3832.00 Mu = 21.03 M = 1965.59 # Found Formula = C44 H54 F30 Na4 O31 Y2 # Dc = 1.71 FOOO = 3832.00 Mu = 17.26 M = 1918.60 _chemical_formula_sum 'C44 H54 F30 Na4 O31 Y2' _chemical_formula_moiety 'C44 H54 F30 Na4 O31 Y2' _chemical_compound_source ? _chemical_formula_weight 1918.60 _cell_measurement_reflns_used 8907 _cell_measurement_theta_min 0.730 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3832 _exptl_absorpt_coefficient_mu 1.726 # Sheldrick geometric approximatio 0.83 0.87 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; J. de Meulenaar and H. Tompa, Acta Crystallogr., Sect A 1965, 19, 1014-1018. ; _exptl_absorpt_correction_T_min 0.8271 _exptl_absorpt_correction_T_max 0.8710 # 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_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _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, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 150 _diffrn_reflns_number 16664 _reflns_number_total 16181 _diffrn_reflns_av_R_equivalents 0.074 # Number of reflections without Friedels Law is 16181 # Number of reflections with Friedels Law is 9088 # Theoretical number of reflections is about 8879 _diffrn_reflns_theta_min 1.412 _diffrn_reflns_theta_max 27.864 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.078 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -23 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 2.13 _oxford_diffrn_Wilson_scale 289.62 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.02 _refine_diff_density_max 1.32 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 16167 _refine_ls_number_restraints 38 _refine_ls_number_parameters 1001 _oxford_refine_ls_R_factor_ref 0.1139 _refine_ls_wR_factor_ref 0.1802 _refine_ls_goodness_of_fit_ref 0.9499 _refine_ls_shift/su_max 0.0013038 _refine_ls_shift/su_mean 0.0000584 # The values computed from all data _oxford_reflns_number_all 16167 _refine_ls_R_factor_all 0.1139 _refine_ls_wR_factor_all 0.1802 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10306 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_gt 0.1535 _refine_ls_abs_structure_Flack 0.472(7) _refine_ls_abs_structure_details 'Flack (1983), 7093 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 Fsqd _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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +13.27P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Nonius (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. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 F1 F 0.8544(3) 0.3797(3) 0.4794(3) 0.0792 1.0000 Uani . . . . . . F2 F 0.8957(3) 0.4482(4) 0.5490(3) 0.1156 1.0000 Uani . . . . . . F3 F 0.8407(4) 0.4886(4) 0.4701(3) 0.1181 1.0000 Uani . . . . . . F4 F 0.6755(4) 0.4846(3) 0.3259(3) 0.0928 1.0000 Uani . . . . . . F5 F 0.6749(6) 0.4831(3) 0.4243(3) 0.1277 1.0000 Uani . . . . . . F6 F 0.5824(5) 0.4422(4) 0.3729(4) 0.1283 1.0000 Uani . . . . . . F7 F 0.8343(7) 0.4109(5) 0.8024(5) 0.1694 1.0000 Uani . . . . . . F8 F 0.8738(6) 0.4156(11) 0.7216(9) 0.2694 1.0000 Uani . . . . . . F9 F 0.8238(6) 0.4976(4) 0.7499(5) 0.1643 1.0000 Uani . . . . . . F10 F 0.5202(3) 0.2078(3) 0.8001(2) 0.0871 1.0000 Uani . . . . . . F11 F 0.4777(3) 0.1735(3) 0.7122(3) 0.0839 1.0000 Uani . . . . . . F12 F 0.4396(3) 0.2668(3) 0.7498(3) 0.0917 1.0000 Uani . . . . . . F13 F 0.5265(3) 0.3086(3) 0.4507(2) 0.0831 1.0000 Uani . . . . . . F14 F 0.4775(4) 0.3400(3) 0.5373(3) 0.0969 1.0000 Uani . . . . . . F15 F 0.4423(3) 0.2498(3) 0.4943(3) 0.0948 1.0000 Uani . . . . . . F16 F 0.9676(5) 0.1957(6) 0.6260(7) 0.1976 1.0000 Uani . . . . . . F17 F 0.9679(6) 0.2807(11) 0.5825(11) 0.2969 1.0000 Uani . . . . . . F18 F 0.9684(6) 0.2798(15) 0.6681(11) 0.3485 1.0000 Uani . . . . . . F19 F 0.8908(3) 0.0615(4) 0.6944(3) 0.0934 1.0000 Uani . . . . . . F20 F 0.8357(4) 0.0171(3) 0.7735(3) 0.0905 1.0000 Uani . . . . . . F21 F 0.8496(3) 0.1241(3) 0.7676(3) 0.0735 1.0000 Uani . . . . . . F22 F 0.6139(5) 0.0755(3) 0.3816(4) 0.1268 1.0000 Uani . . . . . . F23 F 0.5357(4) 0.1403(4) 0.4259(3) 0.1130 1.0000 Uani . . . . . . F24 F 0.5398(4) 0.1342(3) 0.3274(3) 0.0976 1.0000 Uani . . . . . . F25 F 0.8090(5) 0.0027(4) 0.5035(6) 0.1783 1.0000 Uani . . . . . . F26 F 0.8157(9) 0.0829(6) 0.4437(6) 0.2071 1.0000 Uani . . . . . . F27 F 0.8644(5) 0.0950(6) 0.5171(9) 0.2143 1.0000 Uani . . . . . . F28 F 0.9622(5) 0.1725(5) 0.3801(6) 0.1664 1.0000 Uani . . . . . . F29 F 0.9747(4) 0.2596(8) 0.3317(6) 0.2229 1.0000 Uani . . . . . . F30 F 0.9751(4) 0.2551(6) 0.4261(6) 0.1647 1.0000 Uani . . . . . . O1 O 0.7818(4) 0.6347(3) 0.6334(3) 0.0749 1.0000 Uani . U . . . . O2 O 0.6837(4) 0.6293(3) 0.7323(3) 0.0614 1.0000 Uani . . . . . . O3 O 0.5586(3) 0.5521(3) 0.7151(3) 0.0613 1.0000 Uani . . . . . . O4 O 0.5623(3) 0.4712(3) 0.6077(2) 0.0512 1.0000 Uani . . . . . . O5 O 0.6155(4) 0.5995(4) 0.5605(4) 0.1066 1.0000 Uani . U . . . . O6 O 0.7426(4) 0.4869(3) 0.5688(3) 0.0748 1.0000 Uani . . . . . . O7 O 0.7014(3) 0.4471(3) 0.6995(3) 0.0549 1.0000 Uani . . . . . . O8 O 0.7407(4) 0.3434(2) 0.7204(2) 0.0552 1.0000 Uani . . . . . . O9 O 0.5483(3) 0.3182(2) 0.6820(2) 0.0435 1.0000 Uani . . . . . . O10 O 0.7359(3) 0.3760(2) 0.5513(2) 0.0486 1.0000 Uani . . . . . . O11 O 0.7046(3) 0.3535(3) 0.4255(2) 0.0560 1.0000 Uani . . . . . . O12 O 0.6234(3) 0.2793(2) 0.5467(2) 0.0360 1.0000 Uani . . . . . . O13 O 0.5425(3) 0.1956(2) 0.5687(2) 0.0439 1.0000 Uani . . . . . . O14 O 0.6614(3) 0.2116(3) 0.4288(3) 0.0569 1.0000 Uani . . . . . . O15 O 0.8282(3) 0.2462(3) 0.4298(3) 0.0515 1.0000 Uani . . . . . . O16 O 0.7353(4) 0.1618(2) 0.5324(2) 0.0534 1.0000 Uani . . . . . . O17 O 0.6229(3) 0.2300(2) 0.7047(2) 0.0386 1.0000 Uani . . . . . . O18 O 0.7313(3) 0.1327(2) 0.6956(2) 0.0448 1.0000 Uani . . . . . . O19 O 0.7005(3) 0.3509(3) 0.3217(2) 0.0563 1.0000 Uani . . . . . . O20 O 0.8277(3) 0.2471(3) 0.3245(2) 0.0481 1.0000 Uani . . . . . . O21 O 0.6638(3) 0.2074(3) 0.3241(2) 0.0522 1.0000 Uani . . . . . . O22 O 0.8289(4) 0.2405(3) 0.6797(3) 0.0717 1.0000 Uani . . . . . . O23 O 0.8242(4) 0.2654(3) 0.5765(3) 0.0789 1.0000 Uani . . . . . . O24 O 0.6865(3) 0.0603(3) 0.5470(3) 0.0569 1.0000 Uani . . . . . . O25 O 0.7374(5) 0.0218(3) 0.6756(3) 0.0785 1.0000 Uani . . . . . . O26 O 0.6097(4) -0.0797(3) 0.7023(3) 0.0814 1.0000 Uani . . . . . . O27 O 0.5533(3) 0.0396(3) 0.6470(3) 0.0566 1.0000 Uani . . . . . . O28 O 0.5441(3) -0.0431(3) 0.5419(3) 0.0607 1.0000 Uani . . . . . . O29 O 0.6683(4) -0.1223(3) 0.5203(3) 0.0713 1.0000 Uani . . . . . . O30 O 0.7670(4) -0.1311(3) 0.6205(3) 0.0841 1.0000 Uani . . . . . . O31 O 0.2692(8) 0.2374(7) 0.6245(4) 0.1505 1.0000 Uani . . . . . . C1 C 0.8514(7) 0.6156(7) 0.6042(6) 0.1106 1.0000 Uani . U . . . . C2 C 0.7950(6) 0.6738(6) 0.6905(6) 0.1008 1.0000 Uani . U . . . . C3 C 0.7244(6) 0.6907(4) 0.7180(5) 0.0740 1.0000 Uani . U . . . . C4 C 0.6186(6) 0.6405(5) 0.7670(5) 0.0775 1.0000 Uani . . . . . . C5 C 0.5797(6) 0.5746(6) 0.7759(5) 0.0778 1.0000 Uani . . . . . . C6 C 0.5241(5) 0.4851(4) 0.7146(4) 0.0628 1.0000 Uani . . . . . . C7 C 0.4980(4) 0.4737(4) 0.6484(5) 0.0652 1.0000 Uani . . . . . . C8 C 0.5493(6) 0.4932(6) 0.5440(5) 0.0857 1.0000 Uani . U . . . . C9 C 0.5454(7) 0.5733(7) 0.5441(7) 0.1213 1.0000 Uani . U . . . . C10 C 0.6407(8) 0.6416(7) 0.5220(7) 0.1224 1.0000 Uani . U . . . . C11 C 0.7656(4) 0.4332(4) 0.5461(4) 0.0517 1.0000 Uani . . . . . . C12 C 0.8395(6) 0.4375(5) 0.5090(5) 0.0702 1.0000 Uani . . . . . . C13 C 0.7436(5) 0.4073(3) 0.7228(3) 0.0430 1.0000 Uani . . . . . . C14 C 0.8122(7) 0.4365(6) 0.7561(7) 0.0948 1.0000 Uani . . . . . . C15 C 0.6905(4) 0.3758(3) 0.3743(3) 0.0413 1.0000 Uani . . . . . . C16 C 0.6530(8) 0.4471(5) 0.3743(4) 0.0782 1.0000 Uani . . . . . . C17 C 0.5612(4) 0.2475(3) 0.5444(3) 0.0351 1.0000 Uani . . . . . . C18 C 0.5012(4) 0.2861(4) 0.5058(4) 0.0518 1.0000 Uani . . . . . . C19 C 0.5628(4) 0.2645(3) 0.7066(3) 0.0326 1.0000 Uani . . . . . . C20 C 0.5000(4) 0.2284(4) 0.7425(4) 0.0484 1.0000 Uani . . . . . . C21 C 0.8564(4) 0.2444(4) 0.3779(4) 0.0401 1.0000 Uani . . . . . . C22 C 0.9424(5) 0.2382(6) 0.3762(5) 0.0672 1.0000 Uani . . . . . . C23 C 0.6413(4) 0.1918(3) 0.3773(3) 0.0365 1.0000 Uani . . . . . . C24 C 0.5815(5) 0.1358(4) 0.3777(4) 0.0580 1.0000 Uani . . . . . . C25 C 0.8547(4) 0.2524(4) 0.6273(4) 0.0406 1.0000 Uani . . . . . . C26 C 0.9378(6) 0.2528(6) 0.6248(7) 0.0784 1.0000 Uani . . . . . . C27 C 0.7355(6) 0.0992(3) 0.5281(3) 0.0442 1.0000 Uani . . . . . . C28 C 0.8044(8) 0.0669(6) 0.4984(7) 0.0915 1.0000 Uani . . . . . . C29 C 0.7608(4) 0.0749(4) 0.6988(3) 0.0472 1.0000 Uani . . . . . . C30 C 0.8358(5) 0.0709(4) 0.7353(4) 0.0601 1.0000 Uani . . . . . . C31 C 0.6266(8) -0.1437(5) 0.7281(6) 0.0949 1.0000 Uani . . . . . . C32 C 0.5433(7) -0.0508(6) 0.7240(6) 0.0902 1.0000 Uani . . . . . . C33 C 0.5429(7) 0.0231(5) 0.7118(5) 0.0858 1.0000 Uani . . . . . . C34 C 0.4851(5) 0.0347(5) 0.6110(5) 0.0780 1.0000 Uani . . . . . . C35 C 0.5077(5) 0.0215(5) 0.5435(4) 0.0627 1.0000 Uani . . . . . . C36 C 0.5633(5) -0.0649(5) 0.4805(4) 0.0669 1.0000 Uani . . . . . . C37 C 0.5995(6) -0.1322(5) 0.4855(5) 0.0772 1.0000 Uani . . . . . . C38 C 0.7065(8) -0.1836(5) 0.5353(5) 0.0920 1.0000 Uani . . . . . . C39 C 0.7809(8) -0.1676(6) 0.5635(6) 0.0968 1.0000 Uani . . . . . . C40 C 0.8377(8) -0.1131(7) 0.6511(7) 0.1137 1.0000 Uani . . . . . . C41 C 0.2815(13) 0.1147(11) 0.6205(9) 0.1668 1.0000 Uani . U . . . . C42 C 0.3233(10) 0.1780(16) 0.6114(11) 0.1915 1.0000 Uani . U . . . . C43 C 0.3147(13) 0.2970(14) 0.6186(11) 0.2017 1.0000 Uani D U . . . . C44 C 0.2724(14) 0.3562(11) 0.6350(10) 0.1881 1.0000 Uani D U . . . . Y2 Y 0.73740(7) 0.27135(3) 0.49821(2) 0.0329 1.0000 Uani . . . . . . Na3 Na 0.63923(16) 0.37406(13) 0.62406(13) 0.0441 1.0000 Uani . . . . . . Na4 Na 0.67736(17) 0.54902(13) 0.64683(13) 0.0459 1.0000 Uani . . . . . . Y1 Y 0.73744(7) 0.23344(2) 0.75337(2) 0.0325 1.0000 Uani . . . . . . Na2 Na 0.63148(16) 0.13580(13) 0.62536(13) 0.0429 1.0000 Uani . . . . . . Na1 Na 0.66409(19) -0.04072(14) 0.60533(15) 0.0567 1.0000 Uani . . . . . . H11 H 0.8410 0.5917 0.5662 0.1262 1.0000 Uiso R . . . . . H12 H 0.8794 0.6557 0.5948 0.1262 1.0000 Uiso R . . . . . H13 H 0.8797 0.5871 0.6316 0.1262 1.0000 Uiso R . . . . . H21 H 0.8237 0.7135 0.6820 0.1000 1.0000 Uiso R . . . . . H22 H 0.8216 0.6452 0.7190 0.1000 1.0000 Uiso R . . . . . H31 H 0.7324 0.7167 0.7552 0.0884 1.0000 Uiso R . . . . . H32 H 0.6963 0.7170 0.6887 0.0884 1.0000 Uiso R . . . . . H41 H 0.6308 0.6589 0.8071 0.0922 1.0000 Uiso R . . . . . H42 H 0.5866 0.6714 0.7453 0.0922 1.0000 Uiso R . . . . . H51 H 0.6131 0.5424 0.7942 0.0869 1.0000 Uiso R . . . . . H52 H 0.5370 0.5798 0.8022 0.0869 1.0000 Uiso R . . . . . H61 H 0.5598 0.4514 0.7263 0.0752 1.0000 Uiso R . . . . . H62 H 0.4829 0.4838 0.7430 0.0752 1.0000 Uiso R . . . . . H71 H 0.4660 0.5101 0.6359 0.0763 1.0000 Uiso R . . . . . H72 H 0.4714 0.4318 0.6461 0.0763 1.0000 Uiso R . . . . . H81 H 0.5878 0.4771 0.5168 0.1147 1.0000 Uiso R . . . . . H82 H 0.5024 0.4756 0.5305 0.1147 1.0000 Uiso R . . . . . H91 H 0.5088 0.5889 0.5734 0.2064 1.0000 Uiso R . . . . . H92 H 0.5326 0.5886 0.5030 0.2064 1.0000 Uiso R . . . . . H311 H 0.6731 -0.1599 0.7122 0.1171 1.0000 Uiso R . . . . . H312 H 0.6294 -0.1398 0.7727 0.1171 1.0000 Uiso R . . . . . H313 H 0.5879 -0.1749 0.7172 0.1171 1.0000 Uiso R . . . . . H321 H 0.5364 -0.0599 0.7676 0.1021 1.0000 Uiso R . . . . . H322 H 0.5029 -0.0699 0.7008 0.1021 1.0000 Uiso R . . . . . H331 H 0.5836 0.0418 0.7349 0.1074 1.0000 Uiso R . . . . . H332 H 0.4972 0.0425 0.7263 0.1074 1.0000 Uiso R . . . . . H341 H 0.4557 -0.0022 0.6263 0.0954 1.0000 Uiso R . . . . . H342 H 0.4571 0.0759 0.6137 0.0954 1.0000 Uiso R . . . . . H351 H 0.5411 0.0560 0.5293 0.0754 1.0000 Uiso R . . . . . H352 H 0.4644 0.0208 0.5175 0.0754 1.0000 Uiso R . . . . . H361 H 0.5961 -0.0329 0.4611 0.0868 1.0000 Uiso R . . . . . H362 H 0.5190 -0.0690 0.4561 0.0868 1.0000 Uiso R . . . . . H371 H 0.5679 -0.1631 0.5076 0.0915 1.0000 Uiso R . . . . . H372 H 0.6100 -0.1499 0.4448 0.0915 1.0000 Uiso R . . . . . H381 H 0.6773 -0.2093 0.5642 0.1183 1.0000 Uiso R . . . . . H382 H 0.7140 -0.2095 0.4979 0.1183 1.0000 Uiso R . . . . . H391 H 0.8067 -0.2088 0.5733 0.1166 1.0000 Uiso R . . . . . H392 H 0.8101 -0.1413 0.5351 0.1166 1.0000 Uiso R . . . . . H401 H 0.8264 -0.0879 0.6882 0.1383 1.0000 Uiso R . . . . . H402 H 0.8638 -0.1537 0.6622 0.1383 1.0000 Uiso R . . . . . H403 H 0.8682 -0.0862 0.6241 0.1383 1.0000 Uiso R . . . . . H411 H 0.3134 0.0770 0.6119 0.1515 1.0000 Uiso R . . . . . H412 H 0.2638 0.1118 0.6627 0.1515 1.0000 Uiso R . . . . . H413 H 0.2401 0.1140 0.5924 0.1515 1.0000 Uiso R . . . . . H421 H 0.3646 0.1793 0.6395 0.2105 1.0000 Uiso R . . . . . H422 H 0.3410 0.1815 0.5692 0.2105 1.0000 Uiso R . . . . . H441 H 0.2971 0.3990 0.6320 0.3301 1.0000 Uiso R . . . . . H442 H 0.2544 0.3499 0.6768 0.3301 1.0000 Uiso R . . . . . H443 H 0.2314 0.3551 0.6065 0.3301 1.0000 Uiso R . . . . . H431 H 0.3558 0.2974 0.6471 0.2696 1.0000 Uiso R . . . . . H432 H 0.3328 0.3026 0.5768 0.2696 1.0000 Uiso R . . . . . H101 H 0.6882 0.6581 0.5353 0.1702 1.0000 Uiso R . . . . . H102 H 0.6064 0.6786 0.5191 0.1702 1.0000 Uiso R . . . . . H103 H 0.6456 0.6204 0.4819 0.1702 1.0000 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 F1 0.067(3) 0.090(4) 0.080(3) -0.037(3) 0.026(3) -0.003(3) F2 0.058(4) 0.163(7) 0.125(5) -0.058(5) 0.024(4) -0.045(4) F3 0.131(6) 0.102(5) 0.121(6) 0.035(4) 0.074(5) -0.011(4) F4 0.156(6) 0.048(3) 0.075(4) 0.020(3) -0.001(4) 0.007(3) F5 0.239(9) 0.071(4) 0.073(4) -0.020(3) -0.016(5) 0.050(5) F6 0.109(6) 0.105(5) 0.171(8) 0.038(5) 0.035(5) 0.067(5) F7 0.196(10) 0.164(8) 0.148(8) 0.037(7) -0.117(8) -0.074(7) F8 0.080(7) 0.42(3) 0.308(19) -0.107(18) -0.031(9) -0.062(10) F9 0.148(8) 0.080(5) 0.265(12) -0.002(6) -0.101(8) -0.042(5) F10 0.088(4) 0.122(5) 0.051(3) 0.030(3) 0.016(3) -0.029(4) F11 0.088(4) 0.070(3) 0.093(4) -0.012(3) 0.021(3) -0.043(3) F12 0.047(3) 0.085(4) 0.143(6) 0.008(4) 0.038(3) 0.008(3) F13 0.067(3) 0.122(5) 0.060(3) 0.042(3) -0.004(3) 0.018(3) F14 0.111(5) 0.092(4) 0.088(4) -0.012(3) -0.018(4) 0.059(4) F15 0.056(3) 0.100(4) 0.129(6) 0.039(4) -0.049(4) -0.017(3) F16 0.074(5) 0.157(9) 0.362(19) 0.031(10) 0.029(7) 0.043(6) F17 0.073(7) 0.39(2) 0.42(3) 0.26(2) 0.071(11) 0.022(10) F18 0.070(7) 0.58(4) 0.39(3) -0.30(3) -0.023(11) -0.012(13) F19 0.056(3) 0.131(5) 0.094(4) 0.004(4) -0.004(3) 0.034(3) F20 0.094(4) 0.086(4) 0.092(4) 0.022(3) -0.027(3) 0.017(3) F21 0.072(3) 0.069(3) 0.079(3) -0.012(3) -0.032(3) 0.002(3) F22 0.127(6) 0.040(3) 0.213(9) 0.018(4) -0.006(5) -0.016(3) F23 0.114(5) 0.150(6) 0.075(4) -0.014(4) 0.038(4) -0.075(5) F24 0.102(4) 0.120(5) 0.070(4) 0.008(3) -0.030(3) -0.059(4) F25 0.138(7) 0.065(4) 0.332(14) -0.007(6) 0.108(8) 0.037(4) F26 0.291(16) 0.168(10) 0.162(9) 0.005(8) 0.157(11) 0.056(10) F27 0.076(6) 0.158(9) 0.41(2) -0.073(12) 0.055(9) 0.011(6) F28 0.078(5) 0.132(7) 0.289(14) 0.014(7) 0.001(6) 0.052(5) F29 0.041(4) 0.388(18) 0.240(12) 0.221(13) 0.036(6) 0.028(6) F30 0.064(5) 0.256(12) 0.174(10) -0.059(8) -0.047(6) 0.013(6) O1 0.072(4) 0.061(3) 0.092(5) -0.009(3) 0.004(3) -0.027(3) O2 0.083(4) 0.046(3) 0.055(3) -0.006(2) 0.003(3) 0.003(3) O3 0.055(3) 0.062(3) 0.067(4) -0.008(3) 0.004(3) 0.011(3) O4 0.045(3) 0.054(3) 0.055(3) 0.005(2) -0.004(2) -0.004(2) O5 0.080(4) 0.111(5) 0.129(6) 0.073(4) -0.035(4) -0.025(4) O6 0.090(4) 0.063(3) 0.072(4) -0.017(3) 0.031(4) -0.011(4) O7 0.063(3) 0.048(3) 0.054(3) 0.001(2) -0.013(3) 0.011(3) O8 0.067(3) 0.039(2) 0.060(3) 0.0061(19) -0.001(3) 0.004(3) O9 0.050(3) 0.034(2) 0.047(3) 0.003(2) 0.002(2) 0.004(2) O10 0.046(3) 0.052(3) 0.047(3) -0.0097(19) 0.007(3) -0.014(3) O11 0.075(4) 0.052(3) 0.041(3) 0.012(2) -0.002(3) 0.005(2) O12 0.035(2) 0.045(3) 0.028(2) -0.0092(18) 0.0022(19) -0.005(2) O13 0.045(3) 0.044(3) 0.042(3) 0.002(2) -0.003(2) -0.008(2) O14 0.062(3) 0.069(4) 0.040(3) -0.012(3) -0.001(3) -0.013(3) O15 0.053(3) 0.062(3) 0.039(3) -0.003(3) 0.017(3) 0.007(3) O16 0.059(3) 0.044(2) 0.056(3) 0.0069(19) 0.007(3) 0.005(4) O17 0.032(2) 0.043(3) 0.041(3) -0.004(2) 0.002(2) 0.001(2) O18 0.049(3) 0.049(2) 0.037(2) -0.0105(18) -0.011(3) 0.016(3) O19 0.077(4) 0.049(3) 0.043(3) -0.013(2) 0.005(3) 0.011(3) O20 0.058(3) 0.054(3) 0.033(3) -0.001(2) -0.009(3) -0.002(3) O21 0.054(3) 0.065(3) 0.038(3) 0.010(3) 0.003(2) -0.010(3) O22 0.084(5) 0.070(4) 0.061(4) 0.007(3) 0.036(4) 0.007(4) O23 0.097(5) 0.067(4) 0.073(5) 0.003(3) -0.041(4) -0.004(4) O24 0.062(4) 0.049(3) 0.060(3) -0.004(3) 0.000(3) -0.003(3) O25 0.088(4) 0.057(3) 0.090(4) -0.021(3) -0.029(5) 0.010(4) O26 0.089(5) 0.053(3) 0.103(5) 0.024(3) 0.010(4) 0.009(3) O27 0.052(3) 0.050(3) 0.068(4) 0.000(3) 0.002(3) 0.002(2) O28 0.067(4) 0.054(3) 0.061(4) -0.002(3) 0.001(3) -0.014(3) O29 0.089(5) 0.040(3) 0.085(4) -0.013(3) 0.010(4) -0.009(3) O30 0.096(5) 0.064(4) 0.092(5) -0.014(3) -0.012(4) 0.028(3) O31 0.180(14) 0.190(12) 0.082(7) 0.020(6) -0.001(6) -0.067(10) C1 0.101(8) 0.109(8) 0.122(8) 0.009(7) 0.016(7) -0.050(7) C2 0.076(6) 0.097(7) 0.129(9) 0.045(7) -0.027(6) -0.048(6) C3 0.094(7) 0.050(4) 0.078(5) -0.009(4) -0.018(5) -0.010(5) C4 0.095(7) 0.073(6) 0.065(6) -0.024(5) 0.009(5) 0.017(6) C5 0.070(6) 0.098(8) 0.065(6) -0.020(5) 0.005(5) 0.025(6) C6 0.057(5) 0.049(4) 0.082(6) 0.007(4) 0.027(5) 0.008(4) C7 0.041(4) 0.051(5) 0.104(7) -0.018(5) 0.003(4) 0.000(4) C8 0.081(6) 0.093(6) 0.082(6) 0.028(5) -0.033(5) -0.020(5) C9 0.076(6) 0.123(8) 0.165(10) 0.084(7) -0.046(7) -0.042(6) C10 0.124(9) 0.120(8) 0.123(9) 0.027(7) -0.003(8) -0.052(7) C11 0.045(4) 0.054(5) 0.056(5) -0.015(4) 0.005(4) -0.003(3) C12 0.072(6) 0.073(6) 0.066(6) -0.009(5) 0.017(5) -0.026(5) C13 0.043(4) 0.043(3) 0.043(3) -0.003(3) 0.003(4) -0.004(4) C14 0.085(8) 0.070(7) 0.129(11) 0.036(7) -0.050(8) -0.023(6) C15 0.052(4) 0.038(3) 0.034(4) 0.004(3) -0.001(3) 0.008(3) C16 0.121(10) 0.076(6) 0.038(4) -0.008(4) 0.007(5) 0.043(6) C17 0.047(4) 0.034(3) 0.024(3) 0.000(2) -0.010(3) 0.002(3) C18 0.041(4) 0.065(5) 0.049(5) 0.014(4) -0.010(3) 0.002(4) C19 0.036(4) 0.036(3) 0.025(3) -0.005(3) 0.003(3) 0.003(3) C20 0.040(4) 0.051(4) 0.054(5) -0.004(4) 0.008(3) -0.006(3) C21 0.037(4) 0.050(4) 0.033(4) 0.005(3) 0.000(4) 0.008(3) C22 0.037(4) 0.108(8) 0.056(5) -0.016(5) -0.003(5) 0.013(5) C23 0.043(4) 0.030(3) 0.037(4) 0.000(3) 0.001(3) -0.007(3) C24 0.071(5) 0.060(5) 0.043(4) 0.007(4) 0.003(4) -0.019(4) C25 0.041(4) 0.056(4) 0.025(3) 0.000(3) -0.001(4) 0.007(3) C26 0.047(5) 0.095(8) 0.093(8) -0.010(6) 0.016(7) -0.007(5) C27 0.051(4) 0.035(3) 0.046(4) 0.000(2) -0.004(5) 0.011(5) C28 0.091(9) 0.069(7) 0.114(10) -0.002(6) 0.044(8) 0.010(6) C29 0.053(5) 0.051(4) 0.037(4) -0.008(3) -0.009(3) 0.009(3) C30 0.067(6) 0.057(5) 0.057(5) 0.002(4) -0.011(5) 0.014(4) C31 0.117(10) 0.075(7) 0.092(8) 0.008(5) -0.018(7) 0.021(7) C32 0.096(9) 0.083(7) 0.092(8) 0.020(6) 0.015(7) 0.005(6) C33 0.104(9) 0.081(7) 0.072(7) 0.019(5) 0.017(6) 0.018(6) C34 0.053(5) 0.052(5) 0.129(10) -0.020(5) -0.007(5) -0.005(4) C35 0.056(5) 0.068(5) 0.064(5) 0.008(4) -0.015(4) -0.005(4) C36 0.068(6) 0.080(6) 0.053(5) 0.003(4) -0.001(4) -0.011(5) C37 0.083(7) 0.075(6) 0.074(6) -0.032(5) 0.016(5) -0.026(5) C38 0.140(10) 0.051(5) 0.085(8) -0.013(5) 0.032(7) 0.001(6) C39 0.118(10) 0.071(7) 0.101(9) 0.003(6) -0.003(8) 0.034(7) C40 0.120(11) 0.103(9) 0.118(10) 0.009(8) -0.014(9) 0.058(8) C41 0.172(16) 0.179(15) 0.150(14) 0.016(11) 0.029(10) 0.076(13) C42 0.088(11) 0.29(3) 0.197(17) -0.017(16) 0.020(10) 0.054(14) C43 0.105(11) 0.29(3) 0.208(17) -0.008(16) 0.022(10) 0.051(14) C44 0.200(17) 0.191(15) 0.174(14) 0.017(11) 0.050(11) 0.061(13) Y2 0.0336(3) 0.0382(3) 0.0268(3) -0.0006(2) 0.0005(4) 0.0000(4) Na3 0.0452(15) 0.0454(14) 0.0418(14) -0.0104(12) 0.0050(13) -0.0026(12) Na4 0.0528(17) 0.0383(14) 0.0466(15) -0.0017(11) 0.0036(13) 0.0002(12) Y1 0.0349(3) 0.0369(2) 0.0257(3) -0.0001(2) 0.0004(4) 0.0018(4) Na2 0.0450(15) 0.0420(13) 0.0417(14) -0.0072(11) -0.0053(12) 0.0050(11) Na1 0.065(2) 0.0369(14) 0.068(2) -0.0033(13) -0.0071(16) 0.0005(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.14275(7) 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 F1 . C12 . 1.325(11) yes F1 . Y2 . 3.012(6) yes F2 . C12 . 1.331(12) yes F3 . C12 . 1.301(12) yes F4 . C16 . 1.327(11) yes F5 . C16 . 1.334(12) yes F6 . C16 . 1.265(15) yes F7 . C14 . 1.172(12) yes F8 . C14 . 1.38(2) yes F9 . C14 . 1.225(12) yes F10 . C20 . 1.338(9) yes F11 . C20 . 1.318(9) yes F12 . C20 . 1.325(9) yes F13 . C18 . 1.330(9) yes F14 . C18 . 1.322(10) yes F15 . C18 . 1.293(10) yes F16 . C26 . 1.243(15) yes F17 . C26 . 1.181(16) yes F18 . C26 . 1.192(17) yes F19 . C30 . 1.323(11) yes F20 . C30 . 1.333(10) yes F21 . C30 . 1.275(10) yes F21 . Y1 . 2.955(5) yes F22 . C24 . 1.323(12) yes F23 . C24 . 1.314(10) yes F24 . C24 . 1.301(10) yes F25 . C28 . 1.269(13) yes F26 . C28 . 1.220(15) yes F27 . C28 . 1.270(17) yes F28 . C22 . 1.342(14) yes F29 . C22 . 1.183(13) yes F30 . C22 . 1.254(12) yes O1 . C1 . 1.440(14) yes O1 . C2 . 1.455(14) yes O1 . Na4 . 2.530(6) yes O2 . C3 . 1.441(10) yes O2 . C4 . 1.394(12) yes O2 . Na4 . 2.407(6) yes O3 . C5 . 1.415(11) yes O3 . C6 . 1.455(10) yes O3 . Na4 . 2.570(6) yes O4 . C7 . 1.439(10) yes O4 . C8 . 1.437(10) yes O4 . Na3 . 2.379(6) yes O4 . Na4 . 2.694(6) yes O5 . C9 . 1.397(13) yes O5 . C10 . 1.248(13) yes O5 . Na4 . 2.358(7) yes O6 . C11 . 1.230(9) yes O6 . Na4 . 2.365(6) yes O7 . C13 . 1.193(9) yes O7 . Na3 . 2.420(6) yes O7 . Na4 . 2.334(6) yes O8 . C13 . 1.259(8) yes O8 . Y1 . 2.274(4) yes O9 . C19 . 1.208(8) yes O9 . Na3 . 2.315(6) yes O10 . C11 . 1.248(9) yes O10 . Y2 . 2.347(4) yes O10 . Na3 . 2.317(6) yes O11 . C15 . 1.198(8) yes O11 . Y2 . 2.308(5) yes O12 . C17 . 1.277(8) yes O12 . Y2 . 2.287(4) yes O12 . Na3 . 2.499(5) yes O13 . C17 . 1.192(8) yes O13 . Na2 . 2.314(5) yes O14 . C23 . 1.215(8) yes O14 . Y2 . 2.322(5) yes O15 . C21 . 1.212(9) yes O15 . Y2 . 2.231(5) yes O16 . C27 . 1.235(7) yes O16 . Y2 . 2.274(4) yes O16 . Na2 . 2.755(6) yes O17 . C19 . 1.270(8) yes O17 . Y1 . 2.293(5) yes O17 . Na2 . 2.508(5) yes O18 . C29 . 1.255(8) yes O18 . Y1 . 2.332(4) yes O18 . Na2 . 2.325(5) yes O19 . Y1 3_554 2.300(5) yes O19 . C15 . 1.231(8) yes O20 . Y1 3_554 2.241(6) yes O20 . C21 . 1.244(8) yes O21 . Y1 3_554 2.310(5) yes O21 . C23 . 1.236(8) yes O22 . C25 . 1.226(9) yes O22 . Y1 . 2.265(6) yes O23 . C25 . 1.235(9) yes O23 . Y2 . 2.275(7) yes O24 . C27 . 1.230(9) yes O24 . Na2 . 2.437(6) yes O24 . Na1 . 2.374(6) yes O25 . C29 . 1.228(9) yes O25 . Na1 . 2.335(7) yes O26 . C31 . 1.405(11) yes O26 . C32 . 1.394(13) yes O26 . Na1 . 2.401(8) yes O27 . C33 . 1.423(11) yes O27 . C34 . 1.442(11) yes O27 . Na2 . 2.396(6) yes O27 . Na1 . 2.681(6) yes O28 . C35 . 1.427(10) yes O28 . C36 . 1.412(10) yes O28 . Na1 . 2.531(7) yes O29 . C37 . 1.445(12) yes O29 . C38 . 1.421(13) yes O29 . Na1 . 2.416(7) yes O30 . C39 . 1.427(13) yes O30 . C40 . 1.465(16) yes O30 . Na1 . 2.577(7) yes O31 . C42 . 1.54(2) yes O31 . C43 . 1.43(3) yes C1 . H11 . 0.951 no C1 . H12 . 0.953 no C1 . H13 . 0.952 no C2 . C3 . 1.427(16) yes C2 . H21 . 0.953 no C2 . H22 . 0.952 no C3 . H31 . 0.951 no C3 . H32 . 0.952 no C4 . C5 . 1.484(14) yes C4 . H41 . 0.950 no C4 . H42 . 0.953 no C5 . H51 . 0.953 no C5 . H52 . 0.951 no C6 . C7 . 1.496(13) yes C6 . H61 . 0.953 no C6 . H62 . 0.951 no C7 . H71 . 0.953 no C7 . H72 . 0.953 no C8 . C9 . 1.578(17) yes C8 . H81 . 0.951 no C8 . H82 . 0.951 no C9 . H91 . 0.951 no C9 . H92 . 0.950 no C10 . H101 . 0.951 no C10 . H102 . 0.954 no C10 . H103 . 0.951 no C11 . C12 . 1.540(12) yes C13 . C14 . 1.527(13) yes C15 . C16 . 1.555(11) yes C17 . C18 . 1.547(10) yes C19 . C20 . 1.530(9) yes C21 . C22 . 1.542(11) yes C23 . C24 . 1.534(10) yes C25 . C26 . 1.485(13) yes C27 . C28 . 1.520(14) yes C29 . C30 . 1.549(11) yes C31 . H311 . 0.952 no C31 . H312 . 0.950 no C31 . H313 . 0.952 no C32 . C33 . 1.476(14) yes C32 . H321 . 0.950 no C32 . H322 . 0.951 no C33 . H331 . 0.951 no C33 . H332 . 0.952 no C34 . C35 . 1.509(13) yes C34 . H341 . 0.953 no C34 . H342 . 0.954 no C35 . H351 . 0.953 no C35 . H352 . 0.951 no C36 . C37 . 1.478(14) yes C36 . H361 . 0.952 no C36 . H362 . 0.951 no C37 . H371 . 0.952 no C37 . H372 . 0.950 no C38 . C39 . 1.491(17) yes C38 . H381 . 0.952 no C38 . H382 . 0.951 no C39 . H391 . 0.954 no C39 . H392 . 0.952 no C40 . H401 . 0.951 no C40 . H402 . 0.954 no C40 . H403 . 0.952 no C41 . C42 . 1.46(3) yes C41 . H411 . 0.954 no C41 . H412 . 0.950 no C41 . H413 . 0.950 no C42 . H421 . 0.950 no C42 . H422 . 0.950 no C43 . C44 . 1.431(17) yes C43 . H431 . 0.950 no C43 . H432 . 0.950 no C44 . H441 . 0.954 no C44 . H442 . 0.950 no C44 . H443 . 0.950 no Y2 . Na3 . 3.779(3) yes Y1 . Na2 . 3.827(3) yes 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 C12 . F1 . Y2 . 113.9(5) yes C30 . F21 . Y1 . 114.3(5) yes C1 . O1 . C2 . 110.9(8) yes C1 . O1 . Na4 . 120.8(6) yes C2 . O1 . Na4 . 112.2(5) yes C3 . O2 . C4 . 113.6(7) yes C3 . O2 . Na4 . 114.5(5) yes C4 . O2 . Na4 . 117.5(6) yes C5 . O3 . C6 . 113.7(7) yes C5 . O3 . Na4 . 107.5(5) yes C6 . O3 . Na4 . 108.9(4) yes C7 . O4 . C8 . 115.2(7) yes C7 . O4 . Na3 . 113.7(5) yes C8 . O4 . Na3 . 118.2(6) yes C7 . O4 . Na4 . 113.9(4) yes C8 . O4 . Na4 . 104.0(5) yes Na3 . O4 . Na4 . 88.30(19) yes C9 . O5 . C10 . 113.9(10) yes C9 . O5 . Na4 . 117.3(6) yes C10 . O5 . Na4 . 128.2(8) yes C11 . O6 . Na4 . 151.8(6) yes C13 . O7 . Na3 . 100.1(4) yes C13 . O7 . Na4 . 151.3(6) yes Na3 . O7 . Na4 . 96.3(2) yes C13 . O8 . Y1 . 159.7(4) yes C19 . O9 . Na3 . 119.6(4) yes C11 . O10 . Y2 . 138.0(5) yes C11 . O10 . Na3 . 113.0(4) yes Y2 . O10 . Na3 . 108.3(2) yes C15 . O11 . Y2 . 156.2(5) yes C17 . O12 . Y2 . 136.4(4) yes C17 . O12 . Na3 . 119.3(4) yes Y2 . O12 . Na3 . 104.23(18) yes C17 . O13 . Na2 . 117.9(5) yes C23 . O14 . Y2 . 155.0(5) yes C21 . O15 . Y2 . 154.1(5) yes C27 . O16 . Y2 . 157.1(4) yes C27 . O16 . Na2 . 82.6(5) yes Y2 . O16 . Na2 . 114.5(2) yes C19 . O17 . Y1 . 136.4(4) yes C19 . O17 . Na2 . 117.8(4) yes Y1 . O17 . Na2 . 105.64(19) yes C29 . O18 . Y1 . 136.2(4) yes C29 . O18 . Na2 . 112.4(4) yes Y1 . O18 . Na2 . 110.5(2) yes Y1 3_554 O19 . C15 . 154.1(5) yes Y1 3_554 O20 . C21 . 156.5(5) yes Y1 3_554 O21 . C23 . 154.5(5) yes C25 . O22 . Y1 . 155.3(7) yes C25 . O23 . Y2 . 161.6(7) yes C27 . O24 . Na2 . 97.5(4) yes C27 . O24 . Na1 . 144.1(5) yes Na2 . O24 . Na1 . 94.9(2) yes C29 . O25 . Na1 . 153.5(5) yes C31 . O26 . C32 . 114.8(9) yes C31 . O26 . Na1 . 122.2(7) yes C32 . O26 . Na1 . 119.7(6) yes C33 . O27 . C34 . 112.7(8) yes C33 . O27 . Na2 . 116.2(6) yes C34 . O27 . Na2 . 116.3(5) yes C33 . O27 . Na1 . 106.3(5) yes C34 . O27 . Na1 . 114.2(5) yes Na2 . O27 . Na1 . 88.4(2) yes C35 . O28 . C36 . 113.8(7) yes C35 . O28 . Na1 . 110.9(4) yes C36 . O28 . Na1 . 106.9(5) yes C37 . O29 . C38 . 114.1(8) yes C37 . O29 . Na1 . 116.3(5) yes C38 . O29 . Na1 . 114.3(6) yes C39 . O30 . C40 . 110.3(9) yes C39 . O30 . Na1 . 111.5(6) yes C40 . O30 . Na1 . 120.3(6) yes C42 . O31 . C43 . 104.4(17) yes O1 . C1 . H11 . 108.8 no O1 . C1 . H12 . 109.1 no H11 . C1 . H12 . 109.6 no O1 . C1 . H13 . 110.4 no H11 . C1 . H13 . 109.2 no H12 . C1 . H13 . 109.6 no O1 . C2 . C3 . 108.7(8) yes O1 . C2 . H21 . 111.2 no C3 . C2 . H21 . 111.3 no O1 . C2 . H22 . 107.3 no C3 . C2 . H22 . 108.7 no H21 . C2 . H22 . 109.6 no O2 . C3 . C2 . 109.7(8) yes O2 . C3 . H31 . 110.5 no C2 . C3 . H31 . 109.3 no O2 . C3 . H32 . 109.0 no C2 . C3 . H32 . 109.1 no H31 . C3 . H32 . 109.2 no O2 . C4 . C5 . 108.7(7) yes O2 . C4 . H41 . 109.9 no C5 . C4 . H41 . 109.0 no O2 . C4 . H42 . 110.3 no C5 . C4 . H42 . 109.8 no H41 . C4 . H42 . 109.3 no C4 . C5 . O3 . 106.4(8) yes C4 . C5 . H51 . 109.8 no O3 . C5 . H51 . 109.4 no C4 . C5 . H52 . 110.9 no O3 . C5 . H52 . 110.9 no H51 . C5 . H52 . 109.6 no O3 . C6 . C7 . 105.9(7) yes O3 . C6 . H61 . 110.1 no C7 . C6 . H61 . 110.5 no O3 . C6 . H62 . 110.4 no C7 . C6 . H62 . 110.4 no H61 . C6 . H62 . 109.5 no C6 . C7 . O4 . 108.7(7) yes C6 . C7 . H71 . 109.6 no O4 . C7 . H71 . 109.7 no C6 . C7 . H72 . 109.5 no O4 . C7 . H72 . 109.6 no H71 . C7 . H72 . 109.7 no O4 . C8 . C9 . 107.8(9) yes O4 . C8 . H81 . 110.7 no C9 . C8 . H81 . 111.5 no O4 . C8 . H82 . 108.4 no C9 . C8 . H82 . 108.9 no H81 . C8 . H82 . 109.5 no C8 . C9 . O5 . 109.1(10) yes C8 . C9 . H91 . 110.7 no O5 . C9 . H91 . 109.6 no C8 . C9 . H92 . 109.0 no O5 . C9 . H92 . 109.1 no H91 . C9 . H92 . 109.3 no O5 . C10 . H101 . 110.8 no O5 . C10 . H102 . 108.5 no H101 . C10 . H102 . 109.3 no O5 . C10 . H103 . 109.1 no H101 . C10 . H103 . 109.4 no H102 . C10 . H103 . 109.6 no O10 . C11 . O6 . 126.7(7) yes O10 . C11 . C12 . 117.3(7) yes O6 . C11 . C12 . 116.0(7) yes C11 . C12 . F2 . 109.3(7) yes C11 . C12 . F1 . 111.5(7) yes F2 . C12 . F1 . 106.6(9) yes C11 . C12 . F3 . 112.4(9) yes F2 . C12 . F3 . 105.7(8) yes F1 . C12 . F3 . 111.0(8) yes O8 . C13 . O7 . 127.7(8) yes O8 . C13 . C14 . 115.3(8) yes O7 . C13 . C14 . 116.9(7) yes C13 . C14 . F8 . 106.3(11) yes C13 . C14 . F9 . 117.0(9) yes F8 . C14 . F9 . 95.7(13) yes C13 . C14 . F7 . 119.7(10) yes F8 . C14 . F7 . 92.7(13) yes F9 . C14 . F7 . 117.1(12) yes O19 . C15 . O11 . 130.2(7) yes O19 . C15 . C16 . 114.9(6) yes O11 . C15 . C16 . 114.9(6) yes C15 . C16 . F5 . 110.6(8) yes C15 . C16 . F4 . 111.7(7) yes F5 . C16 . F4 . 103.4(10) yes C15 . C16 . F6 . 111.2(10) yes F5 . C16 . F6 . 110.6(9) yes F4 . C16 . F6 . 109.0(9) yes O12 . C17 . O13 . 130.3(6) yes O12 . C17 . C18 . 112.6(6) yes O13 . C17 . C18 . 117.1(7) yes C17 . C18 . F13 . 113.1(6) yes C17 . C18 . F14 . 110.3(6) yes F13 . C18 . F14 . 106.6(7) yes C17 . C18 . F15 . 113.1(7) yes F13 . C18 . F15 . 107.1(7) yes F14 . C18 . F15 . 106.2(7) yes O17 . C19 . O9 . 129.4(6) yes O17 . C19 . C20 . 112.9(6) yes O9 . C19 . C20 . 117.5(6) yes C19 . C20 . F10 . 113.4(6) yes C19 . C20 . F12 . 113.1(6) yes F10 . C20 . F12 . 106.6(7) yes C19 . C20 . F11 . 111.0(6) yes F10 . C20 . F11 . 106.1(6) yes F12 . C20 . F11 . 106.1(7) yes O20 . C21 . O15 . 130.9(7) yes O20 . C21 . C22 . 113.2(7) yes O15 . C21 . C22 . 115.9(7) yes C21 . C22 . F28 . 109.7(9) yes C21 . C22 . F30 . 115.2(9) yes F28 . C22 . F30 . 94.6(10) yes C21 . C22 . F29 . 118.4(9) yes F28 . C22 . F29 . 105.2(11) yes F30 . C22 . F29 . 110.6(13) yes O21 . C23 . O14 . 130.2(6) yes O21 . C23 . C24 . 114.2(6) yes O14 . C23 . C24 . 115.6(6) yes C23 . C24 . F22 . 109.8(8) yes C23 . C24 . F23 . 113.0(7) yes F22 . C24 . F23 . 106.5(8) yes C23 . C24 . F24 . 114.4(6) yes F22 . C24 . F24 . 106.3(8) yes F23 . C24 . F24 . 106.4(8) yes O23 . C25 . O22 . 131.6(9) yes O23 . C25 . C26 . 114.2(9) yes O22 . C25 . C26 . 114.2(9) yes C25 . C26 . F16 . 114.9(10) yes C25 . C26 . F18 . 115.7(12) yes F16 . C26 . F18 . 101.0(18) yes C25 . C26 . F17 . 119.0(13) yes F16 . C26 . F17 . 103.9(14) yes F18 . C26 . F17 . 99.8(19) yes O16 . C27 . O24 . 126.4(8) yes O16 . C27 . C28 . 116.8(9) yes O24 . C27 . C28 . 116.8(7) yes C27 . C28 . F27 . 111.8(11) yes C27 . C28 . F25 . 115.7(10) yes F27 . C28 . F25 . 110.6(13) yes C27 . C28 . F26 . 114.8(12) yes F27 . C28 . F26 . 92.4(13) yes F25 . C28 . F26 . 109.1(12) yes O18 . C29 . O25 . 127.3(7) yes O18 . C29 . C30 . 115.8(6) yes O25 . C29 . C30 . 116.9(7) yes C29 . C30 . F20 . 110.1(7) yes C29 . C30 . F19 . 108.8(7) yes F20 . C30 . F19 . 106.7(7) yes C29 . C30 . F21 . 113.3(7) yes F20 . C30 . F21 . 109.0(7) yes F19 . C30 . F21 . 108.9(8) yes O26 . C31 . H311 . 110.4 no O26 . C31 . H312 . 109.1 no H311 . C31 . H312 . 109.5 no O26 . C31 . H313 . 109.1 no H311 . C31 . H313 . 109.4 no H312 . C31 . H313 . 109.4 no O26 . C32 . C33 . 110.3(9) yes O26 . C32 . H321 . 110.7 no C33 . C32 . H321 . 110.8 no O26 . C32 . H322 . 108.3 no C33 . C32 . H322 . 107.2 no H321 . C32 . H322 . 109.4 no C32 . C33 . O27 . 113.1(9) yes C32 . C33 . H331 . 106.6 no O27 . C33 . H331 . 108.1 no C32 . C33 . H332 . 110.0 no O27 . C33 . H332 . 109.5 no H331 . C33 . H332 . 109.4 no O27 . C34 . C35 . 106.8(7) yes O27 . C34 . H341 . 109.6 no C35 . C34 . H341 . 109.9 no O27 . C34 . H342 . 110.7 no C35 . C34 . H342 . 110.2 no H341 . C34 . H342 . 109.6 no C34 . C35 . O28 . 107.4(7) yes C34 . C35 . H351 . 110.2 no O28 . C35 . H351 . 109.9 no C34 . C35 . H352 . 109.7 no O28 . C35 . H352 . 110.2 no H351 . C35 . H352 . 109.5 no O28 . C36 . C37 . 108.1(8) yes O28 . C36 . H361 . 110.3 no C37 . C36 . H361 . 110.7 no O28 . C36 . H362 . 109.1 no C37 . C36 . H362 . 109.1 no H361 . C36 . H362 . 109.5 no C36 . C37 . O29 . 106.7(7) yes C36 . C37 . H371 . 110.3 no O29 . C37 . H371 . 109.8 no C36 . C37 . H372 . 110.4 no O29 . C37 . H372 . 110.2 no H371 . C37 . H372 . 109.3 no O29 . C38 . C39 . 109.8(9) yes O29 . C38 . H381 . 109.4 no C39 . C38 . H381 . 109.9 no O29 . C38 . H382 . 109.6 no C39 . C38 . H382 . 108.8 no H381 . C38 . H382 . 109.3 no C38 . C39 . O30 . 106.9(10) yes C38 . C39 . H391 . 109.8 no O30 . C39 . H391 . 109.1 no C38 . C39 . H392 . 110.4 no O30 . C39 . H392 . 111.0 no H391 . C39 . H392 . 109.6 no O30 . C40 . H401 . 108.0 no O30 . C40 . H402 . 109.2 no H401 . C40 . H402 . 109.7 no O30 . C40 . H403 . 111.1 no H401 . C40 . H403 . 109.3 no H402 . C40 . H403 . 109.6 no C42 . C41 . H411 . 109.2 no C42 . C41 . H412 . 110.3 no H411 . C41 . H412 . 109.4 no C42 . C41 . H413 . 109.0 no H411 . C41 . H413 . 109.5 no H412 . C41 . H413 . 109.4 no O31 . C42 . C41 . 107.4(15) yes O31 . C42 . H421 . 110.6 no C41 . C42 . H421 . 109.6 no O31 . C42 . H422 . 108.9 no C41 . C42 . H422 . 110.9 no H421 . C42 . H422 . 109.4 no O31 . C43 . C44 . 110.1(20) yes O31 . C43 . H431 . 112.8 no C44 . C43 . H431 . 104.3 no O31 . C43 . H432 . 111.6 no C44 . C43 . H432 . 108.3 no H431 . C43 . H432 . 109.4 no C43 . C44 . H441 . 117.1 no C43 . C44 . H442 . 107.6 no H441 . C44 . H442 . 109.5 no C43 . C44 . H443 . 103.6 no H441 . C44 . H443 . 109.4 no H442 . C44 . H443 . 109.4 no O10 . Y2 . O14 . 137.9(2) yes O10 . Y2 . O11 . 72.79(18) yes O14 . Y2 . O11 . 77.4(2) yes O10 . Y2 . O12 . 73.37(17) yes O14 . Y2 . O12 . 78.43(17) yes O11 . Y2 . O12 . 91.52(18) yes O10 . Y2 . O23 . 72.7(2) yes O14 . Y2 . O23 . 146.7(2) yes O11 . Y2 . O23 . 134.1(2) yes O12 . Y2 . O23 . 106.4(3) yes O10 . Y2 . O16 . 132.67(17) yes O14 . Y2 . O16 . 73.4(2) yes O11 . Y2 . O16 . 150.7(2) yes O12 . Y2 . O16 . 84.67(19) yes O23 . Y2 . O16 . 74.3(2) yes O10 . Y2 . O15 . 121.0(2) yes O14 . Y2 . O15 . 84.3(2) yes O11 . Y2 . O15 . 84.5(2) yes O12 . Y2 . O15 . 162.70(19) yes O23 . Y2 . O15 . 88.2(3) yes O10 . Y2 . F1 . 56.66(16) yes O14 . Y2 . F1 . 132.82(18) yes O11 . Y2 . F1 . 65.94(19) yes O12 . Y2 . F1 . 128.96(14) yes O23 . Y2 . F1 . 70.1(2) yes O10 . Y2 . Na3 . 35.60(14) yes O14 . Y2 . Na3 . 116.56(16) yes O11 . Y2 . Na3 . 88.87(14) yes O12 . Y2 . Na3 . 39.85(11) yes O23 . Y2 . Na3 . 80.1(2) yes O16 . Y2 . O15 . 90.5(2) yes O16 . Y2 . F1 . 136.4(2) yes O15 . Y2 . F1 . 64.32(18) yes O16 . Y2 . Na3 . 105.87(13) yes O15 . Y2 . Na3 . 156.21(16) yes F1 . Y2 . Na3 . 92.13(10) yes O9 . Na3 . O10 . 152.27(19) yes O9 . Na3 . O4 . 93.03(19) yes O10 . Na3 . O4 . 108.7(2) yes O9 . Na3 . O7 . 104.7(2) yes O10 . Na3 . O7 . 95.0(2) yes O4 . Na3 . O7 . 83.4(2) yes O9 . Na3 . O12 . 85.16(18) yes O10 . Na3 . O12 . 70.08(16) yes O4 . Na3 . O12 . 115.9(2) yes O7 . Na3 . O12 . 158.2(2) yes O9 . Na3 . Y2 . 116.57(14) yes O10 . Na3 . Y2 . 36.13(11) yes O4 . Na3 . Y2 . 126.45(16) yes O7 . Na3 . Y2 . 124.82(17) yes O12 . Na3 . Y2 . 35.91(11) yes O7 . Na4 . O5 . 145.0(3) yes O7 . Na4 . O6 . 78.5(2) yes O5 . Na4 . O6 . 84.5(3) yes O7 . Na4 . O2 . 101.2(2) yes O5 . Na4 . O2 . 109.3(3) yes O6 . Na4 . O2 . 147.5(3) yes O7 . Na4 . O1 . 119.3(3) yes O5 . Na4 . O1 . 88.7(3) yes O6 . Na4 . O1 . 84.4(2) yes O2 . Na4 . O1 . 67.2(2) yes O7 . Na4 . O3 . 84.4(2) yes O5 . Na4 . O3 . 92.3(3) yes O6 . Na4 . O3 . 144.5(2) yes O2 . Na4 . O3 . 66.4(2) yes O1 . Na4 . O3 . 131.0(2) yes O7 . Na4 . O4 . 78.47(19) yes O5 . Na4 . O4 . 69.0(2) yes O6 . Na4 . O4 . 82.3(2) yes O2 . Na4 . O4 . 129.9(2) yes O1 . Na4 . O4 . 155.0(2) yes O3 . Na4 . O4 . 63.71(19) yes O18 . Y1 . O21 3_555 137.9(2) yes O18 . Y1 . O19 3_555 72.82(18) yes O21 3_555 Y1 . O19 3_555 77.9(2) yes O18 . Y1 . O17 . 72.34(17) yes O21 3_555 Y1 . O17 . 78.42(17) yes O19 3_555 Y1 . O17 . 90.39(19) yes O18 . Y1 . F21 . 57.81(15) yes O21 3_555 Y1 . F21 . 133.35(18) yes O19 3_555 Y1 . F21 . 66.75(19) yes O17 . Y1 . F21 . 129.04(15) yes O18 . Y1 . O8 . 130.36(17) yes O21 3_555 Y1 . O8 . 74.6(2) yes O19 3_555 Y1 . O8 . 152.6(2) yes O17 . Y1 . O8 . 84.9(2) yes F21 . Y1 . O8 . 134.9(2) yes O18 . Y1 . O22 . 74.0(2) yes O21 3_555 Y1 . O22 . 145.9(2) yes O19 3_555 Y1 . O22 . 133.3(2) yes O17 . Y1 . O22 . 109.6(3) yes F21 . Y1 . O22 . 68.0(2) yes O18 . Y1 . O20 3_555 122.16(19) yes O21 3_555 Y1 . O20 3_555 83.5(2) yes O19 3_555 Y1 . O20 3_555 84.5(2) yes O17 . Y1 . O20 3_555 161.84(19) yes F21 . Y1 . O20 3_555 64.36(17) yes O18 . Y1 . Na2 . 34.68(13) yes O21 3_555 Y1 . Na2 . 115.59(14) yes O19 3_555 Y1 . Na2 . 86.75(14) yes O17 . Y1 . Na2 . 39.13(12) yes F21 . Y1 . Na2 . 92.46(10) yes O8 . Y1 . O22 . 73.2(2) yes O8 . Y1 . O20 3_555 91.6(2) yes O22 . Y1 . O20 3_555 86.3(3) yes O8 . Y1 . Na2 . 105.74(15) yes O22 . Y1 . Na2 . 84.2(2) yes O20 3_555 Y1 . Na2 . 156.81(15) yes O13 . Na2 . O18 . 150.85(19) yes O13 . Na2 . O27 . 95.8(2) yes O18 . Na2 . O27 . 107.6(2) yes O13 . Na2 . O24 . 103.4(2) yes O18 . Na2 . O24 . 96.4(2) yes O27 . Na2 . O24 . 83.4(2) yes O13 . Na2 . O17 . 86.06(18) yes O18 . Na2 . O17 . 68.65(17) yes O27 . Na2 . O17 . 114.8(2) yes O24 . Na2 . O17 . 158.9(2) yes O13 . Na2 . Y1 . 116.97(14) yes O18 . Na2 . Y1 . 34.80(11) yes O27 . Na2 . Y1 . 123.26(17) yes O24 . Na2 . Y1 . 126.21(17) yes O17 . Na2 . Y1 . 35.23(11) yes O13 . Na2 . O16 . 89.79(19) yes O18 . Na2 . O16 . 87.0(2) yes O27 . Na2 . O16 . 132.5(2) yes O24 . Na2 . O16 . 49.70(17) yes O17 . Na2 . O16 . 112.58(17) yes Y1 . Na2 . O16 . 94.68(14) yes O25 . Na1 . O24 . 78.3(2) yes O25 . Na1 . O26 . 81.3(3) yes O24 . Na1 . O26 . 141.5(2) yes O25 . Na1 . O29 . 144.0(3) yes O24 . Na1 . O29 . 99.3(2) yes O26 . Na1 . O29 . 116.1(2) yes O25 . Na1 . O28 . 145.5(2) yes O24 . Na1 . O28 . 83.1(2) yes O26 . Na1 . O28 . 96.2(2) yes O29 . Na1 . O28 . 67.5(2) yes O25 . Na1 . O30 . 83.3(2) yes O24 . Na1 . O30 . 121.4(3) yes O26 . Na1 . O30 . 87.8(3) yes O29 . Na1 . O30 . 67.2(2) yes O28 . Na1 . O30 . 131.1(2) yes O25 . Na1 . O27 . 83.9(2) yes O24 . Na1 . O27 . 78.7(2) yes O26 . Na1 . O27 . 66.9(2) yes O29 . Na1 . O27 . 131.3(2) yes O28 . Na1 . O27 . 64.0(2) yes O30 . Na1 . O27 . 153.0(3) 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 C6 . H61 . O7 . 128.2(2) 0.953 2.595 3.271(16) yes _iucr_refine_instruction_details_constraints ; # # Punched on 06/09/11 at 14:14:52 # #LIST 12 BLOCK SCALE X'S, U'S CONT ENANTIO RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) H ( 103,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) H ( 313,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) RIDE C ( 34,X'S) H ( 341,X'S) H ( 342,X'S) RIDE C ( 35,X'S) H ( 351,X'S) H ( 352,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S) RIDE C ( 37,X'S) H ( 371,X'S) H ( 372,X'S) RIDE C ( 38,X'S) H ( 381,X'S) H ( 382,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S) RIDE C ( 40,X'S) H ( 401,X'S) H ( 402,X'S) H ( 403,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S) RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 06/09/11 at 14:14:52 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = C(1) TO C(10) U(IJ)'S 0.0, 0.010000 = C(2) TO C(9) U(IJ)'S 0.0, 0.010000 = C(3) TO C(8) U(IJ)'S 0.0, 0.010000 = O(1) TO O(5) U(IJ)'S 0.0, 0.010000 = C(41) TO C(44) U(IJ)'S 0.0, 0.010000 = C(42) TO C(43) DISTANCE 1.550000 , 0.020000 = C(43) TO C(44) #===END ;