# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year 2010 #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _publ_contact_author 'Amber L. Thompson' _publ_contact_author_email amber.thompson@chem.ox.ac.uk loop_ _publ_author_name _publ_author_address J.A.Raskatov ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; A.L.Thompson ; Chemical Crystallography Department, Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; J.M.Brown ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA. UK. ; _journal_volume ? _journal_page_first ? _journal_page_last ? _ccdc_journal_depnumber ? _publ_section_title ; Chiral Selection in the Formation of Borates From Racemic Binaphthols and Related Diols ; _publ_section_abstract ; A series of boron-containing chiral anions was investigated. All borates were homochiral in the solid state, although in some cases the heterochiral diastereomers were computed to be thermodynamically preferred (DFT). The crystallographic preference for the homochiral diastereomer was attributed to its lower bulk and the therewith associated better packing ability. ; _publ_contact_author_name 'Amber L. Thompson' #============================================================================== data_3a _database_code_depnum_ccdc_archive 'CCDC 796350' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 07-12-21 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5656 _chemical_name_systematic . _chemical_melting_point 'not measured' _publ_section_exptl_refinement ; The data were collected at 250 K because the compound appeared to undergo a phase transition below this temperature and was unstable to loss of THF above it. Consequently there is a considerable degree of thermal motion. Efforts were made to refine the structure with a multi-part model, but the refinement was unstable. 3D Fourier maps were examined and it was apparent that each atom has a single locus so a single component model was used with prolate thermal ellipsoids and 1,2 and 1,3 vibration/thermal similarity restraints for the THF molecules in order to maintain sensible parameters. The difference map indicated the presence of diffuse electron density believed to be disordered solvent. SQUEEZE was used leaving a void of 352 \%A at X(av) = 0 Y(av) = 0 Z(av) = 0.5 from which 8 e^-^ were removed. ; 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 1 0.000 0.000 0.500 352.5 -7.9 _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _cell_length_a 9.1073(2) _cell_length_b 11.9788(3) _cell_length_c 18.7883(5) _cell_angle_alpha 94.9284(9) _cell_angle_beta 100.7991(9) _cell_angle_gamma 105.1909(12) _cell_volume 1923.24(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' 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 2 # Given Formula = C24 H16 B1 Na1 O4 # Dc = 0.69 Fooo = 656.00 Mu = 0.56 M = 402.19 # Found Formula = C36 H40 B1 Na1 O7 # Dc = 1.07 FOOO = 656.00 Mu = 0.82 M = 618.51 _chemical_formula_sum 'C36 H40 B1 Na1 O7' _chemical_formula_moiety 'C36 H40 B1 Na1 O7' _chemical_compound_source . _chemical_formula_weight 618.51 _cell_measurement_reflns_used 7679 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 250 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.082 # Sheldrick geometric approximatio 0.99 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.99 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 250 _diffrn_reflns_number 8166 _reflns_number_total 8166 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections with Friedels Law is 8166 # Number of reflections without Friedels Law is 14673 # Theoretical number of reflections is about 6041 _diffrn_reflns_theta_min 5.189 _diffrn_reflns_theta_max 27.250 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.615 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 3.31 _oxford_diffrn_Wilson_scale 1.13 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.41 _refine_diff_density_max 0.58 # 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>2.0\s(I) _refine_ls_number_reflns 4106 _refine_ls_number_restraints 156 _refine_ls_number_parameters 406 _oxford_refine_ls_R_factor_ref 0.0854 _refine_ls_wR_factor_ref 0.0934 _refine_ls_goodness_of_fit_ref 1.0857 _refine_ls_shift/su_max 0.000900 # The values computed from all data _oxford_reflns_number_all 5981 _refine_ls_R_factor_all 0.1097 _refine_ls_wR_factor_all 0.1187 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4106 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_gt 0.0934 # 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 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: 1.95 1.80 1.17 ; # 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Na1 Na -0.07991(14) 0.16980(12) 0.22967(8) 0.0781 1.0000 Uani . U . . . . . O2 O 0.1626(2) 0.12967(16) 0.27851(10) 0.0544 1.0000 Uani . . . . . . . C3 C 0.2275(3) 0.0572(2) 0.31815(17) 0.0555 1.0000 Uani . . . . . . . C4 C 0.2646(3) -0.0356(2) 0.28239(17) 0.0585 1.0000 Uani . . . . . . . C5 C 0.2365(3) -0.0554(2) 0.20199(18) 0.0610 1.0000 Uani . . . . . . . C6 C 0.2732(3) 0.0379(2) 0.16286(17) 0.0583 1.0000 Uani . . . . . . . O7 O 0.3468(2) 0.14791(16) 0.19833(11) 0.0585 1.0000 Uani . . . . . . . B8 B 0.2608(3) 0.2073(2) 0.23789(18) 0.0509 1.0000 Uani . . . . . . . O9 O 0.1412(2) 0.24447(15) 0.18879(11) 0.0569 1.0000 Uani . . . . . . . C10 C 0.1883(3) 0.3406(2) 0.15459(17) 0.0593 1.0000 Uani . . . . . . . C11 C 0.2483(4) 0.4512(3) 0.19572(18) 0.0646 1.0000 Uani . . . . . . . C12 C 0.2688(4) 0.4664(2) 0.27648(17) 0.0608 1.0000 Uani . . . . . . . C13 C 0.3310(3) 0.3912(2) 0.31772(16) 0.0556 1.0000 Uani . . . . . . . O14 O 0.3779(2) 0.30492(16) 0.28524(11) 0.0576 1.0000 Uani . . . . . . . C15 C 0.3539(4) 0.4084(3) 0.39382(18) 0.0655 1.0000 Uani . . . . . . . C16 C 0.3134(4) 0.4996(3) 0.4282(2) 0.0782 1.0000 Uani . . . . . . . C17 C 0.2512(5) 0.5723(3) 0.3884(2) 0.0830 1.0000 Uani . . . . . . . C18 C 0.2279(4) 0.5564(3) 0.3130(2) 0.0749 1.0000 Uani . . . . . . . C19 C 0.2859(5) 0.5467(3) 0.1580(2) 0.0802 1.0000 Uani . . . . . . . C20 C 0.2623(6) 0.5330(3) 0.0838(2) 0.0959 1.0000 Uani . . . . . . . C21 C 0.2025(6) 0.4230(3) 0.0440(2) 0.0907 1.0000 Uani . . . . . . . C22 C 0.1660(5) 0.3265(3) 0.07954(19) 0.0766 1.0000 Uani . . . . . . . C23 C 0.2435(4) 0.0181(3) 0.0864(2) 0.0768 1.0000 Uani . . . . . . . C24 C 0.1800(5) -0.0944(4) 0.0496(2) 0.0904 1.0000 Uani . . . . . . . C25 C 0.1443(5) -0.1871(4) 0.0870(2) 0.0916 1.0000 Uani . . . . . . . C26 C 0.1723(4) -0.1680(3) 0.1624(2) 0.0768 1.0000 Uani . . . . . . . C27 C 0.3271(4) -0.1091(3) 0.3249(2) 0.0720 1.0000 Uani . . . . . . . C28 C 0.3509(4) -0.0918(3) 0.4003(2) 0.0826 1.0000 Uani . . . . . . . C29 C 0.3109(4) -0.0024(3) 0.4343(2) 0.0843 1.0000 Uani . . . . . . . C30 C 0.2493(4) 0.0735(3) 0.39351(18) 0.0684 1.0000 Uani . . . . . . . O31 O -0.1668(3) 0.1837(3) 0.33592(16) 0.1076 1.0000 Uani D U . . . . . C32 C -0.3190(4) 0.1656(4) 0.3487(3) 0.1212 1.0000 Uani D U . . . . . C33 C -0.3039(5) 0.2576(6) 0.4099(3) 0.1505 1.0000 Uani D U . . . . . C34 C -0.1432(6) 0.3116(8) 0.4372(4) 0.2019 1.0000 Uani D U . . . . . C35 C -0.0647(4) 0.2512(7) 0.3980(3) 0.1901 1.0000 Uani D U . . . . . O36 O -0.2314(3) -0.0008(3) 0.1609(2) 0.1282 1.0000 Uani D U . . . . . C37 C -0.1731(4) -0.0864(5) 0.1301(4) 0.1397 1.0000 Uani D U . . . . . C38 C -0.3045(7) -0.1882(4) 0.1065(5) 0.1618 1.0000 Uani D U . . . . . C39 C -0.4392(5) -0.1537(6) 0.1118(6) 0.2429 1.0000 Uani D U . . . . . C40 C -0.3917(6) -0.0512(6) 0.1547(6) 0.2173 1.0000 Uani D U . . . . . O41 O -0.2084(4) 0.2977(3) 0.1784(2) 0.1291 1.0000 Uani D U . . . . . C42 C -0.2277(9) 0.3955(6) 0.2202(3) 0.1899 1.0000 Uani D U . . . . . C43 C -0.3121(11) 0.4504(5) 0.1680(4) 0.1967 1.0000 Uani D U . . . . . C44 C -0.3834(9) 0.3673(6) 0.1056(3) 0.1672 1.0000 Uani D U . . . . . C45 C -0.3148(11) 0.2764(6) 0.1123(3) 0.1842 1.0000 Uani D U . . . . . H151 H 0.3965 0.3589 0.4211 0.0741 1.0000 Uiso R . . . . . . H161 H 0.3270 0.5101 0.4793 0.0901 1.0000 Uiso R . . . . . . H171 H 0.2275 0.6351 0.4119 0.0999 1.0000 Uiso R . . . . . . H181 H 0.1832 0.6055 0.2855 0.0895 1.0000 Uiso R . . . . . . H191 H 0.3287 0.6214 0.1841 0.0988 1.0000 Uiso R . . . . . . H201 H 0.2872 0.5997 0.0607 0.1152 1.0000 Uiso R . . . . . . H211 H 0.1842 0.4156 -0.0064 0.1097 1.0000 Uiso R . . . . . . H221 H 0.1286 0.2530 0.0540 0.0894 1.0000 Uiso R . . . . . . H231 H 0.2672 0.0800 0.0603 0.0931 1.0000 Uiso R . . . . . . H241 H 0.1603 -0.1074 -0.0017 0.1082 1.0000 Uiso R . . . . . . H251 H 0.1030 -0.2626 0.0619 0.1051 1.0000 Uiso R . . . . . . H261 H 0.1478 -0.2304 0.1882 0.0890 1.0000 Uiso R . . . . . . H271 H 0.3535 -0.1716 0.3028 0.0847 1.0000 Uiso R . . . . . . H281 H 0.3966 -0.1414 0.4276 0.0968 1.0000 Uiso R . . . . . . H291 H 0.3228 0.0084 0.4846 0.0971 1.0000 Uiso R . . . . . . H301 H 0.2214 0.1342 0.4174 0.0814 1.0000 Uiso R . . . . . . H321 H -0.3568 0.0866 0.3610 0.1474 1.0000 Uiso R . . . . . . H322 H -0.3927 0.1743 0.3052 0.1466 1.0000 Uiso R . . . . . . H331 H -0.3457 0.2219 0.4489 0.1802 1.0000 Uiso R . . . . . . H332 H -0.3598 0.3112 0.3923 0.1803 1.0000 Uiso R . . . . . . H341 H -0.1125 0.3189 0.4903 0.2230 1.0000 Uiso R . . . . . . H342 H -0.1198 0.3898 0.4231 0.2234 1.0000 Uiso R . . . . . . H351 H -0.0384 0.1967 0.4299 0.2012 1.0000 Uiso R . . . . . . H352 H 0.0289 0.2998 0.3869 0.2011 1.0000 Uiso R . . . . . . H371 H -0.0940 -0.1038 0.1676 0.1633 1.0000 Uiso R . . . . . . H372 H -0.1254 -0.0587 0.0892 0.1632 1.0000 Uiso R . . . . . . H422 H -0.2917 0.3692 0.2553 0.2334 1.0000 Uiso R . . . . . . H421 H -0.1289 0.4496 0.2474 0.2332 1.0000 Uiso R . . . . . . H451 H -0.3920 0.2011 0.1088 0.2210 1.0000 Uiso R . . . . . . H452 H -0.2608 0.2718 0.0728 0.2213 1.0000 Uiso R . . . . . . H402 H -0.4230 -0.0442 0.2008 0.2331 1.0000 Uiso R . . . . . . H401 H -0.4434 -0.0094 0.1221 0.2330 1.0000 Uiso R . . . . . . H392 H -0.4823 -0.2023 0.1464 0.2742 1.0000 Uiso R . . . . . . H391 H -0.5198 -0.1666 0.0674 0.2740 1.0000 Uiso R . . . . . . H382 H -0.2894 -0.2512 0.1330 0.1842 1.0000 Uiso R . . . . . . H381 H -0.3200 -0.2118 0.0550 0.1838 1.0000 Uiso R . . . . . . H441 H -0.4934 0.3387 0.1049 0.2152 1.0000 Uiso R . . . . . . H442 H -0.3713 0.4021 0.0613 0.2149 1.0000 Uiso R . . . . . . H432 H -0.3889 0.4798 0.1880 0.2650 1.0000 Uiso R . . . . . . H431 H -0.2361 0.5157 0.1560 0.2649 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 Na1 0.0579(7) 0.0792(8) 0.0998(10) 0.0069(7) 0.0182(6) 0.0254(6) O2 0.0512(10) 0.0501(10) 0.0670(12) 0.0133(9) 0.0146(9) 0.0205(8) C3 0.0479(14) 0.0457(14) 0.073(2) 0.0156(13) 0.0104(13) 0.0126(12) C4 0.0487(15) 0.0441(14) 0.080(2) 0.0140(14) 0.0064(13) 0.0116(12) C5 0.0550(16) 0.0512(16) 0.079(2) 0.0037(14) 0.0080(14) 0.0252(13) C6 0.0539(15) 0.0528(16) 0.0710(19) 0.0024(14) 0.0138(13) 0.0219(12) O7 0.0559(11) 0.0512(11) 0.0720(12) 0.0084(9) 0.0208(9) 0.0170(9) B8 0.0485(16) 0.0409(15) 0.0640(19) 0.0089(14) 0.0100(14) 0.0151(13) O9 0.0552(10) 0.0438(10) 0.0677(12) 0.0086(9) 0.0033(9) 0.0139(8) C10 0.0647(17) 0.0480(16) 0.0662(19) 0.0122(14) 0.0078(14) 0.0213(13) C11 0.0735(19) 0.0472(16) 0.076(2) 0.0110(14) 0.0157(15) 0.0220(14) C12 0.0665(17) 0.0426(15) 0.071(2) 0.0059(13) 0.0152(14) 0.0123(13) C13 0.0502(15) 0.0445(14) 0.0679(19) 0.0036(13) 0.0099(13) 0.0095(12) O14 0.0483(10) 0.0499(10) 0.0711(12) 0.0032(9) 0.0053(9) 0.0152(8) C15 0.0619(17) 0.0571(17) 0.068(2) 0.0022(14) 0.0037(14) 0.0108(14) C16 0.081(2) 0.069(2) 0.076(2) -0.0029(17) 0.0144(17) 0.0128(17) C17 0.101(3) 0.061(2) 0.089(3) -0.0040(18) 0.028(2) 0.0253(19) C18 0.091(2) 0.0535(17) 0.085(2) 0.0097(16) 0.0204(18) 0.0290(16) C19 0.116(3) 0.0512(18) 0.080(2) 0.0155(16) 0.027(2) 0.0288(18) C20 0.147(4) 0.061(2) 0.086(3) 0.028(2) 0.032(2) 0.030(2) C21 0.129(3) 0.079(2) 0.068(2) 0.0216(19) 0.019(2) 0.034(2) C22 0.099(2) 0.0609(19) 0.068(2) 0.0072(16) 0.0070(17) 0.0277(17) C23 0.087(2) 0.077(2) 0.074(2) 0.0056(18) 0.0206(18) 0.0360(18) C24 0.098(3) 0.096(3) 0.078(2) -0.013(2) 0.008(2) 0.044(2) C25 0.099(3) 0.071(2) 0.100(3) -0.018(2) 0.000(2) 0.039(2) C26 0.076(2) 0.0510(18) 0.101(3) 0.0038(17) 0.0058(18) 0.0249(15) C27 0.0650(18) 0.0517(17) 0.098(3) 0.0204(16) 0.0067(17) 0.0199(14) C28 0.083(2) 0.063(2) 0.096(3) 0.0290(19) -0.0014(19) 0.0200(17) C29 0.085(2) 0.081(2) 0.075(2) 0.0278(19) 0.0038(18) 0.0075(19) C30 0.0686(19) 0.0628(18) 0.072(2) 0.0183(15) 0.0123(15) 0.0146(15) O31 0.0695(14) 0.134(2) 0.113(2) -0.0167(17) 0.0255(13) 0.0266(15) C32 0.0684(18) 0.163(4) 0.124(3) 0.015(3) 0.028(2) 0.017(2) C33 0.105(2) 0.264(7) 0.104(3) 0.004(3) 0.036(3) 0.087(4) C34 0.128(3) 0.277(9) 0.167(6) -0.095(6) 0.034(4) 0.037(5) C35 0.072(2) 0.317(10) 0.145(4) -0.086(5) 0.011(3) 0.040(4) O36 0.0617(14) 0.103(2) 0.202(4) -0.035(2) 0.0117(18) 0.0219(13) C37 0.103(3) 0.131(3) 0.183(5) -0.032(4) 0.038(4) 0.040(2) C38 0.159(4) 0.102(3) 0.210(7) -0.025(4) 0.038(5) 0.029(3) C39 0.104(3) 0.158(6) 0.405(14) -0.094(7) 0.038(6) -0.015(3) C40 0.069(2) 0.179(6) 0.362(12) -0.100(7) 0.048(5) 0.007(3) O41 0.100(2) 0.124(2) 0.173(3) 0.016(2) 0.007(2) 0.066(2) C42 0.247(8) 0.152(5) 0.172(5) -0.013(4) -0.032(5) 0.123(6) C43 0.278(10) 0.164(6) 0.183(6) 0.024(4) 0.013(6) 0.150(7) C44 0.194(7) 0.186(6) 0.146(5) 0.050(4) 0.012(4) 0.106(5) C45 0.251(9) 0.181(6) 0.133(4) 0.006(4) -0.011(4) 0.127(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.047(4) 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 Na1 . O2 . 2.413(2) yes Na1 . O9 . 2.280(2) yes Na1 . O31 . 2.290(3) yes Na1 . O36 . 2.269(3) yes Na1 . O41 . 2.328(3) yes O2 . C3 . 1.369(3) yes O2 . B8 . 1.480(4) yes C3 . C4 . 1.398(4) yes C3 . C30 . 1.382(5) yes C4 . C5 . 1.472(5) yes C4 . C27 . 1.397(4) yes C5 . C6 . 1.392(4) yes C5 . C26 . 1.402(5) yes C6 . O7 . 1.359(4) yes C6 . C23 . 1.399(5) yes O7 . B8 . 1.447(4) yes B8 . O9 . 1.477(4) yes B8 . O14 . 1.452(4) yes O9 . C10 . 1.376(3) yes C10 . C11 . 1.392(4) yes C10 . C22 . 1.375(5) yes C11 . C12 . 1.483(5) yes C11 . C19 . 1.399(5) yes C12 . C13 . 1.398(4) yes C12 . C18 . 1.397(5) yes C13 . O14 . 1.358(3) yes C13 . C15 . 1.395(4) yes C15 . C16 . 1.388(5) yes C15 . H151 . 0.929 no C16 . C17 . 1.361(5) yes C16 . H161 . 0.937 no C17 . C18 . 1.381(5) yes C17 . H171 . 0.934 no C18 . H181 . 0.937 no C19 . C20 . 1.358(5) yes C19 . H191 . 0.929 no C20 . C21 . 1.376(6) yes C20 . H201 . 0.937 no C21 . C22 . 1.382(5) yes C21 . H211 . 0.923 no C22 . H221 . 0.911 no C23 . C24 . 1.382(6) yes C23 . H231 . 0.924 no C24 . C25 . 1.364(6) yes C24 . H241 . 0.940 no C25 . C26 . 1.380(6) yes C25 . H251 . 0.929 no C26 . H261 . 0.926 no C27 . C28 . 1.381(5) yes C27 . H271 . 0.932 no C28 . C29 . 1.365(6) yes C28 . H281 . 0.943 no C29 . C30 . 1.397(5) yes C29 . H291 . 0.925 no C30 . H301 . 0.937 no O31 . C32 . 1.415(4) yes O31 . C35 . 1.385(5) yes C32 . C33 . 1.484(5) yes C32 . H321 . 0.982 no C32 . H322 . 0.987 no C33 . C34 . 1.411(6) yes C33 . H331 . 0.968 no C33 . H332 . 0.963 no C34 . C35 . 1.397(6) yes C34 . H341 . 0.974 no C34 . H342 . 0.976 no C35 . H351 . 0.968 no C35 . H352 . 0.968 no O36 . C37 . 1.402(5) yes O36 . C40 . 1.404(5) yes C37 . C38 . 1.435(6) yes C37 . H371 . 0.986 no C37 . H372 . 0.992 no C38 . C39 . 1.411(6) yes C38 . H382 . 0.965 no C38 . H381 . 0.958 no C39 . C40 . 1.329(6) yes C39 . H392 . 0.977 no C39 . H391 . 0.974 no C40 . H402 . 0.964 no C40 . H401 . 0.958 no O41 . C42 . 1.422(6) yes O41 . C45 . 1.382(6) yes C42 . C43 . 1.441(6) yes C42 . H422 . 0.979 no C42 . H421 . 0.978 no C43 . C44 . 1.401(7) yes C43 . H432 . 0.979 no C43 . H431 . 0.973 no C44 . C45 . 1.395(6) yes C44 . H441 . 0.967 no C44 . H442 . 0.975 no C45 . H451 . 0.976 no C45 . H452 . 0.968 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 O2 . Na1 . O9 . 57.98(7) yes O2 . Na1 . O31 . 98.45(10) yes O9 . Na1 . O31 . 138.17(11) yes O2 . Na1 . O36 . 104.39(10) yes O9 . Na1 . O36 . 112.24(12) yes O31 . Na1 . O36 . 106.74(14) yes O2 . Na1 . O41 . 148.72(12) yes O9 . Na1 . O41 . 94.41(12) yes O31 . Na1 . O41 . 93.55(14) yes O36 . Na1 . O41 . 99.55(14) yes Na1 . O2 . C3 . 144.04(16) yes Na1 . O2 . B8 . 97.38(15) yes C3 . O2 . B8 . 117.8(2) yes O2 . C3 . C4 . 120.2(3) yes O2 . C3 . C30 . 119.3(3) yes C4 . C3 . C30 . 120.4(3) yes C3 . C4 . C5 . 120.5(2) yes C3 . C4 . C27 . 118.3(3) yes C5 . C4 . C27 . 121.2(3) yes C4 . C5 . C6 . 120.7(3) yes C4 . C5 . C26 . 121.4(3) yes C6 . C5 . C26 . 118.0(3) yes C5 . C6 . O7 . 120.6(3) yes C5 . C6 . C23 . 120.1(3) yes O7 . C6 . C23 . 119.1(3) yes C6 . O7 . B8 . 118.3(2) yes O2 . B8 . O7 . 112.8(2) yes O2 . B8 . O9 . 100.7(2) yes O7 . B8 . O9 . 112.6(2) yes O2 . B8 . O14 . 113.0(2) yes O7 . B8 . O14 . 105.2(2) yes O9 . B8 . O14 . 112.7(2) yes Na1 . O9 . B8 . 103.29(16) yes Na1 . O9 . C10 . 132.25(17) yes B8 . O9 . C10 . 118.6(2) yes O9 . C10 . C11 . 119.7(3) yes O9 . C10 . C22 . 119.2(3) yes C11 . C10 . C22 . 120.9(3) yes C10 . C11 . C12 . 120.8(3) yes C10 . C11 . C19 . 117.6(3) yes C12 . C11 . C19 . 121.6(3) yes C11 . C12 . C13 . 120.5(3) yes C11 . C12 . C18 . 120.9(3) yes C13 . C12 . C18 . 118.6(3) yes C12 . C13 . O14 . 121.0(3) yes C12 . C13 . C15 . 119.9(3) yes O14 . C13 . C15 . 118.9(3) yes C13 . O14 . B8 . 118.6(2) yes C13 . C15 . C16 . 119.8(3) yes C13 . C15 . H151 . 119.8 no C16 . C15 . H151 . 120.5 no C15 . C16 . C17 . 120.6(3) yes C15 . C16 . H161 . 119.6 no C17 . C16 . H161 . 119.8 no C16 . C17 . C18 . 120.3(3) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 119.4 no C12 . C18 . C17 . 120.8(3) yes C12 . C18 . H181 . 118.9 no C17 . C18 . H181 . 120.3 no C11 . C19 . C20 . 121.5(3) yes C11 . C19 . H191 . 119.4 no C20 . C19 . H191 . 119.1 no C19 . C20 . C21 . 120.1(3) yes C19 . C20 . H201 . 118.6 no C21 . C20 . H201 . 121.2 no C20 . C21 . C22 . 119.9(4) yes C20 . C21 . H211 . 118.9 no C22 . C21 . H211 . 121.2 no C21 . C22 . C10 . 119.9(3) yes C21 . C22 . H221 . 120.9 no C10 . C22 . H221 . 119.1 no C6 . C23 . C24 . 120.0(4) yes C6 . C23 . H231 . 120.2 no C24 . C23 . H231 . 119.9 no C23 . C24 . C25 . 120.8(4) yes C23 . C24 . H241 . 119.7 no C25 . C24 . H241 . 119.5 no C24 . C25 . C26 . 119.5(3) yes C24 . C25 . H251 . 120.3 no C26 . C25 . H251 . 120.2 no C5 . C26 . C25 . 121.7(4) yes C5 . C26 . H261 . 118.4 no C25 . C26 . H261 . 119.9 no C4 . C27 . C28 . 121.3(3) yes C4 . C27 . H271 . 120.5 no C28 . C27 . H271 . 118.3 no C27 . C28 . C29 . 119.7(3) yes C27 . C28 . H281 . 119.3 no C29 . C28 . H281 . 120.9 no C28 . C29 . C30 . 120.5(4) yes C28 . C29 . H291 . 120.5 no C30 . C29 . H291 . 118.9 no C29 . C30 . C3 . 119.7(3) yes C29 . C30 . H301 . 119.8 no C3 . C30 . H301 . 120.4 no Na1 . O31 . C32 . 131.4(2) yes Na1 . O31 . C35 . 118.8(2) yes C32 . O31 . C35 . 106.94(10) yes O31 . C32 . C33 . 105.10(10) yes O31 . C32 . H321 . 109.9 no C33 . C32 . H321 . 112.2 no O31 . C32 . H322 . 111.5 no C33 . C32 . H322 . 109.8 no H321 . C32 . H322 . 108.4 no C32 . C33 . C34 . 107.14(10) yes C32 . C33 . H331 . 109.6 no C34 . C33 . H331 . 107.8 no C32 . C33 . H332 . 109.0 no C34 . C33 . H332 . 113.0 no H331 . C33 . H332 . 110.3 no C33 . C34 . C35 . 106.59(10) yes C33 . C34 . H341 . 113.0 no C35 . C34 . H341 . 115.7 no C33 . C34 . H342 . 107.4 no C35 . C34 . H342 . 105.2 no H341 . C34 . H342 . 108.5 no C34 . C35 . O31 . 109.94(10) yes C34 . C35 . H351 . 103.7 no O31 . C35 . H351 . 106.0 no C34 . C35 . H352 . 114.6 no O31 . C35 . H352 . 112.0 no H351 . C35 . H352 . 109.9 no Na1 . O36 . C37 . 124.18(19) yes Na1 . O36 . C40 . 127.2(2) yes C37 . O36 . C40 . 107.27(10) yes O36 . C37 . C38 . 105.38(10) yes O36 . C37 . H371 . 109.8 no C38 . C37 . H371 . 109.4 no O36 . C37 . H372 . 110.1 no C38 . C37 . H372 . 112.5 no H371 . C37 . H372 . 109.5 no C37 . C38 . C39 . 107.37(10) yes C37 . C38 . H382 . 110.7 no C39 . C38 . H382 . 115.6 no C37 . C38 . H381 . 109.9 no C39 . C38 . H381 . 102.8 no H382 . C38 . H381 . 110.1 no C38 . C39 . C40 . 106.84(10) yes C38 . C39 . H392 . 102.6 no C40 . C39 . H392 . 98.4 no C38 . C39 . H391 . 117.5 no C40 . C39 . H391 . 120.1 no H392 . C39 . H391 . 108.2 no O36 . C40 . C39 . 110.21(10) yes O36 . C40 . H402 . 113.0 no C39 . C40 . H402 . 119.7 no O36 . C40 . H401 . 105.9 no C39 . C40 . H401 . 97.3 no H402 . C40 . H401 . 108.7 no Na1 . O41 . C42 . 123.1(2) yes Na1 . O41 . C45 . 127.2(2) yes C42 . O41 . C45 . 107.03(10) yes O41 . C42 . C43 . 105.19(10) yes O41 . C42 . H422 . 110.1 no C43 . C42 . H422 . 108.4 no O41 . C42 . H421 . 113.2 no C43 . C42 . H421 . 111.9 no H422 . C42 . H421 . 108.0 no C42 . C43 . C44 . 107.29(10) yes C42 . C43 . H432 . 111.9 no C44 . C43 . H432 . 111.3 no C42 . C43 . H431 . 107.2 no C44 . C43 . H431 . 109.9 no H432 . C43 . H431 . 109.0 no C43 . C44 . C45 . 106.72(10) yes C43 . C44 . H441 . 108.6 no C45 . C44 . H441 . 109.8 no C43 . C44 . H442 . 110.8 no C45 . C44 . H442 . 112.2 no H441 . C44 . H442 . 108.8 no C44 . C45 . O41 . 110.09(10) yes C44 . C45 . H451 . 112.0 no O41 . C45 . H451 . 109.3 no C44 . C45 . H452 . 108.6 no O41 . C45 . H452 . 109.0 no H451 . C45 . H452 . 107.9 no _chemical_name_common . #============================================================================== data_3b _database_code_depnum_ccdc_archive 'CCDC 796351' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 08-03-28 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5768 _chemical_name_systematic . _chemical_melting_point . 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 1 0.250 0.250 -0.049 51.4 -0.3 2 0.750 0.750 0.049 51.3 -0.3 3 0.750 0.250 0.072 27.8 0.2 4 0.690 0.542 0.062 8.0 0.0 5 0.810 0.958 0.062 8.0 0.0 6 0.250 0.250 0.451 51.4 -0.3 7 0.250 0.750 0.428 27.9 0.2 8 0.190 0.458 0.437 8.0 0.0 9 0.310 0.042 0.437 8.0 0.0 10 0.750 0.750 0.549 51.3 -0.3 11 0.750 0.250 0.572 27.8 0.2 12 0.690 0.958 0.562 8.0 0.0 13 0.810 0.542 0.562 8.0 0.0 14 0.250 0.750 0.928 27.9 0.2 15 0.190 0.042 0.937 8.0 0.0 16 0.310 0.458 0.937 8.0 0.0 _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _refine_special_details ; Although the electon density modelled with SQUEEZE was small, it made a signifiant improvement to the R-indices. ; _cell_length_a 22.3739(2) _cell_length_b 24.2103(2) _cell_length_c 18.94830(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10263.89(14) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c n ' _symmetry_space_group_name_Hall '-P 2ab 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+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y+1/2,z x+1/2,y+1/2,-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' 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' 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 16 # Given Formula = C48 H32 B0.50 Na2 O8 # Dc = 2.04 Fooo = 4160.00 Mu = 1.66 M = 1576.33 # Found Formula = C28 H28 B1 Na1 O6 # Dc = 1.28 FOOO = 4160.00 Mu = 1.02 M = 988.66 _chemical_formula_sum 'C28 H28 B1 Na1 O6' _chemical_formula_moiety 'C28 H28 B1 Na1 O6' _chemical_compound_source . _chemical_formula_weight 494.33 _cell_measurement_reflns_used 12574 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.38 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4160.000 _exptl_absorpt_coefficient_mu 0.102 # Sheldrick geometric approximatio 0.96 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.96 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 150 _diffrn_reflns_number 131834 _reflns_number_total 11685 _diffrn_reflns_av_R_equivalents 0.062 # Number of reflections with Friedels Law is 11685 # Number of reflections without Friedels Law is 11685 # Theoretical number of reflections is about 11771 _diffrn_reflns_theta_min 5.099 _diffrn_reflns_theta_max 27.484 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.934 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min 0 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 2.71 _oxford_diffrn_Wilson_scale 49.77 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.90 _refine_diff_density_max 1.07 # 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>2.0\s(I) _refine_ls_number_reflns 8042 _refine_ls_number_restraints 78 _refine_ls_number_parameters 648 _oxford_refine_ls_R_factor_ref 0.0644 _refine_ls_wR_factor_ref 0.0679 _refine_ls_goodness_of_fit_ref 1.1706 _refine_ls_shift/su_max 0.000563 # The values computed from all data _oxford_reflns_number_all 11685 _refine_ls_R_factor_all 0.0969 _refine_ls_wR_factor_all 0.0916 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8042 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_gt 0.0679 # 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 F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # 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: 0.933 0.738 0.565 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Na1 Na 0.63966(4) 0.56887(4) 0.29966(5) 0.0326 1.0000 Uani . . . . . . . O2 O 0.56022(7) 0.54680(6) 0.21814(8) 0.0289 1.0000 Uani . . . . . . . C3 C 0.54903(10) 0.50223(9) 0.17585(12) 0.0278 1.0000 Uani . . . . . . . C4 C 0.52619(10) 0.45366(9) 0.20564(13) 0.0291 1.0000 Uani . . . . . . . C5 C 0.50980(10) 0.45119(9) 0.28133(13) 0.0300 1.0000 Uani . . . . . . . C6 C 0.52323(11) 0.40527(10) 0.32277(14) 0.0379 1.0000 Uani . . . . . . . C7 C 0.50647(12) 0.40293(11) 0.39307(15) 0.0437 1.0000 Uani . . . . . . . C8 C 0.47575(12) 0.44628(12) 0.42337(14) 0.0425 1.0000 Uani . . . . . . . C9 C 0.46189(11) 0.49243(11) 0.38329(13) 0.0365 1.0000 Uani . . . . . . . C10 C 0.47846(10) 0.49529(9) 0.31291(13) 0.0297 1.0000 Uani . . . . . . . O11 O 0.46178(6) 0.53987(6) 0.27362(9) 0.0295 1.0000 Uani . . . . . . . B12 B 0.50870(11) 0.57712(10) 0.24718(14) 0.0275 1.0000 Uani . . . . . . . O13 O 0.53695(7) 0.61048(6) 0.30203(8) 0.0303 1.0000 Uani . . . . . . . C14 C 0.50847(10) 0.65539(9) 0.32934(12) 0.0283 1.0000 Uani . . . . . . . C15 C 0.49565(9) 0.70167(9) 0.28718(12) 0.0276 1.0000 Uani . . . . . . . C16 C 0.50953(10) 0.70271(9) 0.21076(12) 0.0282 1.0000 Uani . . . . . . . C17 C 0.50084(9) 0.65612(9) 0.16806(12) 0.0276 1.0000 Uani . . . . . . . O18 O 0.47589(7) 0.60926(6) 0.19502(9) 0.0297 1.0000 Uani . . . . . . . Na19 Na 0.37844(4) 0.56164(4) 0.19442(5) 0.0331 1.0000 Uani . . . . . . . O20 O 0.27870(7) 0.53807(6) 0.14907(9) 0.0323 1.0000 Uani . . . . . . . C21 C 0.23891(10) 0.56472(9) 0.10682(13) 0.0306 1.0000 Uani . . . . . . . C22 C 0.19570(9) 0.60042(9) 0.13540(12) 0.0293 1.0000 Uani . . . . . . . C23 C 0.15975(11) 0.63037(11) 0.08881(14) 0.0372 1.0000 Uani . . . . . . . C24 C 0.16622(12) 0.62565(12) 0.01617(14) 0.0429 1.0000 Uani . . . . . . . C25 C 0.20829(13) 0.58976(12) -0.01085(14) 0.0437 1.0000 Uani . . . . . . . C26 C 0.24424(12) 0.55892(11) 0.03394(14) 0.0388 1.0000 Uani . . . . . . . C27 C 0.18928(9) 0.60730(9) 0.21272(12) 0.0298 1.0000 Uani . . . . . . . C28 C 0.19303(9) 0.56217(9) 0.25860(13) 0.0290 1.0000 Uani . . . . . . . O29 O 0.20108(7) 0.50983(6) 0.23274(9) 0.0305 1.0000 Uani . . . . . . . B30 B 0.25887(11) 0.49666(10) 0.20061(14) 0.0291 1.0000 Uani . . . . . . . O31 O 0.30932(7) 0.49594(6) 0.24976(9) 0.0319 1.0000 Uani . . . . . . . C32 C 0.31380(10) 0.45408(10) 0.29788(13) 0.0316 1.0000 Uani . . . . . . . C33 C 0.31089(11) 0.46683(12) 0.36957(14) 0.0399 1.0000 Uani . . . . . . . C34 C 0.31961(12) 0.42639(13) 0.41979(15) 0.0465 1.0000 Uani . . . . . . . C35 C 0.33134(12) 0.37266(13) 0.39918(15) 0.0470 1.0000 Uani . . . . . . . C36 C 0.33456(11) 0.35968(12) 0.32798(14) 0.0408 1.0000 Uani . . . . . . . C37 C 0.32585(10) 0.39996(10) 0.27596(13) 0.0324 1.0000 Uani . . . . . . . C38 C 0.33174(10) 0.38652(9) 0.20015(13) 0.0312 1.0000 Uani . . . . . . . C39 C 0.29363(10) 0.40971(9) 0.14920(13) 0.0307 1.0000 Uani . . . . . . . O40 O 0.24684(7) 0.44253(6) 0.16881(9) 0.0318 1.0000 Uani . . . . . . . C41 C 0.30156(11) 0.39726(11) 0.07833(14) 0.0384 1.0000 Uani . . . . . . . C42 C 0.34657(13) 0.36108(12) 0.05721(15) 0.0461 1.0000 Uani . . . . . . . C43 C 0.38274(13) 0.33703(12) 0.10695(16) 0.0464 1.0000 Uani . . . . . . . C44 C 0.37566(11) 0.34956(11) 0.17713(14) 0.0384 1.0000 Uani . . . . . . . C45 C 0.18558(10) 0.56922(10) 0.33090(13) 0.0326 1.0000 Uani . . . . . . . C46 C 0.17487(11) 0.62104(12) 0.35842(14) 0.0406 1.0000 Uani . . . . . . . C47 C 0.17119(12) 0.66624(11) 0.31419(15) 0.0413 1.0000 Uani . . . . . . . C48 C 0.17801(11) 0.65943(10) 0.24225(14) 0.0368 1.0000 Uani . . . . . . . O49 O 0.40685(8) 0.49955(8) 0.10623(9) 0.0406 1.0000 Uani . . . . . . . O50 O 0.34426(8) 0.65867(9) 0.18168(11) 0.0496 1.0000 Uani . U . . . . . C51 C 0.33575(12) 0.68689(11) 0.24281(19) 0.0512 1.0000 Uani . U . . . . . C52 C 0.33712(14) 0.64575(15) 0.30680(17) 0.0590 1.0000 Uani . U . . . . . C55 C 0.51361(11) 0.65817(10) 0.09625(13) 0.0364 1.0000 Uani . . . . . . . C56 C 0.53450(12) 0.70645(11) 0.06641(14) 0.0415 1.0000 Uani . . . . . . . C57 C 0.54295(12) 0.75300(11) 0.10709(14) 0.0415 1.0000 Uani . . . . . . . C58 C 0.53051(11) 0.75121(10) 0.17875(13) 0.0363 1.0000 Uani . . . . . . . C59 C 0.46976(11) 0.74758(10) 0.32020(13) 0.0341 1.0000 Uani . . . . . . . C60 C 0.45733(12) 0.74804(11) 0.39176(14) 0.0394 1.0000 Uani . . . . . . . C61 C 0.47060(12) 0.70231(11) 0.43215(14) 0.0390 1.0000 Uani . . . . . . . C62 C 0.49575(11) 0.65595(10) 0.40111(13) 0.0342 1.0000 Uani . . . . . . . C63 C 0.51870(11) 0.40793(10) 0.16119(14) 0.0367 1.0000 Uani . . . . . . . C64 C 0.53260(12) 0.41059(11) 0.08994(14) 0.0411 1.0000 Uani . . . . . . . C65 C 0.55465(12) 0.45889(11) 0.06146(14) 0.0402 1.0000 Uani . . . . . . . C66 C 0.56342(11) 0.50470(10) 0.10457(12) 0.0330 1.0000 Uani . . . . . . . O67 O 0.61222(8) 0.52058(8) 0.40380(10) 0.0440 1.0000 Uani . . . . . . . O68 O 0.66937(10) 0.66252(9) 0.27994(14) 0.0603 1.0000 Uani . U . . . . . C69 C 0.68270(14) 0.68325(13) 0.2189(2) 0.0650 1.0000 Uani . U . . . . . C70 C 0.67593(15) 0.63850(18) 0.1598(2) 0.0730 1.0000 Uani . U . . . . . C71 C 0.6764(2) 0.70097(16) 0.3361(3) 0.0888 1.0000 Uani . U . . . . . C72 C 0.65755(17) 0.68208(16) 0.4085(2) 0.0724 1.0000 Uani . U . . . . . H61 H 0.5442 0.3756 0.3014 0.0447 1.0000 Uiso R . . . . . . H71 H 0.5171 0.3718 0.4203 0.0521 1.0000 Uiso R . . . . . . H81 H 0.4632 0.4445 0.4706 0.0509 1.0000 Uiso R . . . . . . H91 H 0.4412 0.5222 0.4032 0.0439 1.0000 Uiso R . . . . . . H231 H 0.1302 0.6539 0.1077 0.0441 1.0000 Uiso R . . . . . . H241 H 0.1417 0.6463 -0.0142 0.0499 1.0000 Uiso R . . . . . . H251 H 0.2123 0.5862 -0.0586 0.0525 1.0000 Uiso R . . . . . . H261 H 0.2735 0.5342 0.0161 0.0471 1.0000 Uiso R . . . . . . H331 H 0.3028 0.5029 0.3837 0.0483 1.0000 Uiso R . . . . . . H341 H 0.3176 0.4363 0.4673 0.0551 1.0000 Uiso R . . . . . . H351 H 0.3381 0.3454 0.4326 0.0570 1.0000 Uiso R . . . . . . H361 H 0.3424 0.3226 0.3141 0.0482 1.0000 Uiso R . . . . . . H411 H 0.2769 0.4134 0.0455 0.0463 1.0000 Uiso R . . . . . . H421 H 0.3518 0.3528 0.0090 0.0550 1.0000 Uiso R . . . . . . H431 H 0.4127 0.3120 0.0930 0.0558 1.0000 Uiso R . . . . . . H441 H 0.4013 0.3331 0.2100 0.0453 1.0000 Uiso R . . . . . . H451 H 0.1876 0.5380 0.3607 0.0388 1.0000 Uiso R . . . . . . H461 H 0.1706 0.6260 0.4073 0.0487 1.0000 Uiso R . . . . . . H471 H 0.1647 0.7015 0.3321 0.0492 1.0000 Uiso R . . . . . . H481 H 0.1753 0.6902 0.2115 0.0433 1.0000 Uiso R . . . . . . H491 H 0.4396 0.4847 0.1115 0.0607 1.0000 Uiso R . . . . . . H492 H 0.3817 0.4757 0.1032 0.0603 1.0000 Uiso R . . . . . . H511 H 0.2968 0.7053 0.2415 0.0575 1.0000 Uiso R . . . . . . H512 H 0.3683 0.7145 0.2481 0.0575 1.0000 Uiso R . . . . . . H521 H 0.3313 0.6656 0.3495 0.0646 1.0000 Uiso R . . . . . . H522 H 0.3747 0.6274 0.3083 0.0646 1.0000 Uiso R . . . . . . H523 H 0.3061 0.6193 0.3014 0.0646 1.0000 Uiso R . . . . . . H551 H 0.5071 0.6276 0.0681 0.0428 1.0000 Uiso R . . . . . . H561 H 0.5427 0.7085 0.0181 0.0502 1.0000 Uiso R . . . . . . H571 H 0.5572 0.7853 0.0865 0.0504 1.0000 Uiso R . . . . . . H581 H 0.5369 0.7828 0.2052 0.0436 1.0000 Uiso R . . . . . . H591 H 0.4600 0.7784 0.2926 0.0405 1.0000 Uiso R . . . . . . H601 H 0.4404 0.7795 0.4117 0.0464 1.0000 Uiso R . . . . . . H611 H 0.4622 0.7021 0.4805 0.0463 1.0000 Uiso R . . . . . . H621 H 0.5041 0.6248 0.4287 0.0401 1.0000 Uiso R . . . . . . H631 H 0.5037 0.3752 0.1808 0.0432 1.0000 Uiso R . . . . . . H641 H 0.5272 0.3793 0.0608 0.0487 1.0000 Uiso R . . . . . . H651 H 0.5639 0.4613 0.0131 0.0481 1.0000 Uiso R . . . . . . H661 H 0.5789 0.5378 0.0863 0.0392 1.0000 Uiso R . . . . . . H671 H 0.5785 0.5067 0.3989 0.0654 1.0000 Uiso R . . . . . . H672 H 0.6345 0.4936 0.4118 0.0656 1.0000 Uiso R . . . . . . H691 H 0.7238 0.6958 0.2198 0.0785 1.0000 Uiso R . . . . . . H692 H 0.6565 0.7133 0.2082 0.0784 1.0000 Uiso R . . . . . . H701 H 0.6868 0.6569 0.1163 0.1095 1.0000 Uiso R . . . . . . H702 H 0.6352 0.6260 0.1566 0.1090 1.0000 Uiso R . . . . . . H703 H 0.7017 0.6073 0.1682 0.1085 1.0000 Uiso R . . . . . . H711 H 0.6514 0.7327 0.3250 0.1059 1.0000 Uiso R . . . . . . H712 H 0.7187 0.7109 0.3386 0.1052 1.0000 Uiso R . . . . . . H721 H 0.6524 0.7108 0.4387 0.1070 1.0000 Uiso R . . . . . . H722 H 0.6213 0.6641 0.4039 0.1085 1.0000 Uiso R . . . . . . H723 H 0.6851 0.6560 0.4256 0.1079 1.0000 Uiso R . . . . . . C530 C 0.35030(15) 0.69629(13) 0.12519(15) 0.0585 0.778(7) Uani D U P . 1 . . C540 C 0.3558(2) 0.6650(2) 0.05634(18) 0.0652 0.778(7) Uani D U P . 1 . . C531 C 0.35030(15) 0.69629(13) 0.12519(15) 0.0585 0.222(7) Uani D U P . 2 . . C541 C 0.3607(7) 0.7082(7) 0.0476(3) 0.0568 0.222(7) Uani D U P . 2 . . H5301 H 0.38731(15) 0.72002(13) 0.13023(15) 0.0750 0.778(7) Uiso . . P . 1 . . H5302 H 0.31400(15) 0.71900(13) 0.12349(15) 0.0744 0.778(7) Uiso . . P . 1 . . H5401 H 0.3183 0.6456 0.0483 0.0979 0.778(7) Uiso R . P . 1 . . H5402 H 0.3630 0.6959 0.0209 0.0972 0.778(7) Uiso R . P . 1 . . H5403 H 0.3892 0.6393 0.0608 0.0974 0.778(7) Uiso R . P . 1 . . H5311 H 0.38602(15) 0.71718(13) 0.13978(15) 0.0751 0.222(7) Uiso . . P . 2 . . H5312 H 0.31464(15) 0.71861(13) 0.13192(15) 0.0748 0.222(7) Uiso . . P . 2 . . H5411 H 0.3706 0.7442 0.0340 0.0845 0.222(7) Uiso R . P . 2 . . H5412 H 0.3916 0.6832 0.0327 0.0851 0.222(7) Uiso R . P . 2 . . H5413 H 0.3233 0.6983 0.0262 0.0852 0.222(7) Uiso R . P . 2 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0290(4) 0.0300(5) 0.0387(5) -0.0014(4) -0.0033(4) 0.0009(4) O2 0.0257(7) 0.0249(7) 0.0359(8) -0.0018(6) -0.0019(6) 0.0004(6) C3 0.0266(10) 0.0248(10) 0.0320(11) -0.0010(9) -0.0035(9) 0.0033(8) C4 0.0264(10) 0.0248(10) 0.0361(12) -0.0009(9) -0.0051(9) 0.0018(8) C5 0.0288(11) 0.0268(11) 0.0343(12) 0.0017(9) -0.0043(9) -0.0007(9) C6 0.0378(13) 0.0282(12) 0.0476(15) 0.0067(11) -0.0035(11) -0.0002(10) C7 0.0432(14) 0.0412(14) 0.0468(15) 0.0180(12) -0.0035(11) -0.0002(11) C8 0.0389(13) 0.0514(15) 0.0371(14) 0.0115(12) 0.0047(11) -0.0031(12) C9 0.0321(12) 0.0409(13) 0.0365(13) 0.0038(11) 0.0040(10) 0.0002(10) C10 0.0248(10) 0.0260(10) 0.0382(12) 0.0043(9) -0.0024(9) -0.0019(8) O11 0.0257(7) 0.0264(7) 0.0364(8) 0.0032(7) -0.0006(6) 0.0024(6) B12 0.0274(12) 0.0252(12) 0.0301(12) 0.0006(10) -0.0024(10) 0.0010(9) O13 0.0316(8) 0.0253(7) 0.0339(8) -0.0028(6) -0.0093(7) 0.0046(6) C14 0.0270(10) 0.0235(10) 0.0343(12) -0.0013(9) -0.0046(9) -0.0003(8) C15 0.0260(10) 0.0245(10) 0.0322(12) -0.0022(9) -0.0044(9) -0.0018(8) C16 0.0263(10) 0.0262(10) 0.0323(12) 0.0022(9) -0.0045(9) -0.0014(8) C17 0.0255(10) 0.0274(11) 0.0299(11) 0.0027(9) -0.0055(9) 0.0034(8) O18 0.0309(8) 0.0226(7) 0.0355(9) 0.0008(6) -0.0078(7) -0.0010(6) Na19 0.0284(4) 0.0330(5) 0.0377(5) 0.0002(4) -0.0008(4) -0.0023(4) O20 0.0255(7) 0.0308(8) 0.0406(9) 0.0074(7) 0.0031(7) 0.0023(6) C21 0.0280(11) 0.0263(11) 0.0375(12) 0.0012(9) 0.0013(9) -0.0038(8) C22 0.0253(10) 0.0283(10) 0.0344(12) -0.0007(9) 0.0008(9) -0.0007(9) C23 0.0320(11) 0.0387(13) 0.0411(14) 0.0019(11) 0.0008(10) 0.0051(10) C24 0.0375(13) 0.0522(16) 0.0390(14) 0.0089(12) -0.0042(11) 0.0033(12) C25 0.0503(15) 0.0476(15) 0.0330(13) -0.0022(11) 0.0006(11) -0.0035(12) C26 0.0415(13) 0.0363(12) 0.0386(13) -0.0010(11) 0.0075(11) 0.0029(11) C27 0.0239(10) 0.0288(11) 0.0367(12) -0.0013(9) 0.0015(9) 0.0012(8) C28 0.0214(10) 0.0296(11) 0.0361(12) -0.0021(9) 0.0012(9) -0.0020(8) O29 0.0275(7) 0.0243(7) 0.0398(9) -0.0005(7) 0.0024(7) -0.0015(6) B30 0.0238(11) 0.0270(12) 0.0365(13) -0.0007(11) 0.0010(10) 0.0002(9) O31 0.0287(8) 0.0276(8) 0.0395(9) 0.0017(7) -0.0018(7) -0.0029(6) C32 0.0232(10) 0.0365(12) 0.0351(12) 0.0033(10) -0.0018(9) -0.0031(9) C33 0.0340(12) 0.0472(14) 0.0385(14) -0.0067(11) 0.0002(10) -0.0014(11) C34 0.0375(13) 0.0692(19) 0.0328(13) 0.0035(13) -0.0004(11) -0.0008(13) C35 0.0411(14) 0.0591(18) 0.0409(15) 0.0167(13) 0.0013(11) 0.0046(13) C36 0.0365(13) 0.0412(14) 0.0448(15) 0.0079(12) 0.0039(11) 0.0046(11) C37 0.0260(10) 0.0358(12) 0.0355(12) 0.0025(10) 0.0016(9) 0.0022(9) C38 0.0285(10) 0.0279(11) 0.0371(12) 0.0036(9) 0.0035(9) 0.0004(9) C39 0.0276(10) 0.0247(10) 0.0398(13) -0.0001(9) 0.0010(9) -0.0011(8) O40 0.0256(7) 0.0276(8) 0.0421(9) -0.0022(7) -0.0025(7) 0.0008(6) C41 0.0365(12) 0.0420(13) 0.0367(13) -0.0014(11) -0.0036(10) -0.0001(11) C42 0.0472(15) 0.0520(16) 0.0392(14) -0.0117(13) 0.0040(12) 0.0042(13) C43 0.0402(14) 0.0478(15) 0.0513(16) -0.0076(13) 0.0084(12) 0.0116(12) C44 0.0341(12) 0.0371(13) 0.0442(14) 0.0026(11) 0.0023(11) 0.0079(10) C45 0.0281(11) 0.0368(12) 0.0329(12) 0.0022(10) 0.0013(9) -0.0012(9) C46 0.0355(13) 0.0507(15) 0.0355(13) -0.0057(12) 0.0019(10) 0.0018(11) C47 0.0396(13) 0.0358(13) 0.0487(15) -0.0104(12) 0.0014(11) 0.0040(11) C48 0.0371(13) 0.0308(12) 0.0426(14) -0.0005(10) 0.0009(10) 0.0068(10) O49 0.0332(8) 0.0447(10) 0.0440(10) -0.0013(8) 0.0026(7) -0.0016(7) O50 0.0410(10) 0.0517(11) 0.0560(11) 0.0141(8) -0.0071(9) -0.0054(9) C51 0.0288(12) 0.0291(12) 0.0956(18) -0.0098(11) -0.0025(14) 0.0005(10) C52 0.0457(15) 0.082(2) 0.0489(15) -0.0202(14) 0.0066(13) -0.0159(16) C55 0.0404(13) 0.0343(12) 0.0345(13) -0.0003(10) -0.0025(10) 0.0086(10) C56 0.0443(14) 0.0482(15) 0.0321(13) 0.0075(11) 0.0020(11) 0.0104(12) C57 0.0417(13) 0.0403(13) 0.0424(14) 0.0159(12) -0.0008(11) -0.0035(11) C58 0.0387(12) 0.0288(11) 0.0414(14) 0.0035(10) -0.0056(10) -0.0034(10) C59 0.0390(12) 0.0247(10) 0.0384(13) -0.0041(10) -0.0056(10) 0.0012(9) C60 0.0441(13) 0.0339(12) 0.0403(14) -0.0124(11) -0.0010(11) 0.0028(11) C61 0.0433(14) 0.0437(14) 0.0298(13) -0.0065(10) -0.0015(10) -0.0052(11) C62 0.0388(12) 0.0331(12) 0.0306(12) 0.0001(10) -0.0057(10) -0.0012(10) C63 0.0381(12) 0.0261(11) 0.0459(14) -0.0026(10) -0.0077(11) 0.0003(10) C64 0.0485(14) 0.0331(12) 0.0417(14) -0.0101(11) -0.0068(11) 0.0051(11) C65 0.0465(14) 0.0436(14) 0.0307(12) -0.0034(11) -0.0037(11) 0.0095(11) C66 0.0330(11) 0.0317(11) 0.0344(12) 0.0037(10) 0.0001(9) 0.0047(9) O67 0.0368(9) 0.0484(10) 0.0468(11) 0.0019(9) -0.0005(8) 0.0027(8) O68 0.0471(11) 0.0421(10) 0.0917(12) 0.0115(8) -0.0053(10) -0.0035(9) C69 0.0428(14) 0.0469(14) 0.1054(13) 0.0273(10) -0.0009(15) 0.0029(12) C70 0.0425(16) 0.094(2) 0.0825(14) 0.0191(14) -0.0096(16) -0.0078(17) C71 0.103(2) 0.0456(16) 0.1176(16) -0.0065(12) 0.012(2) -0.0154(17) C72 0.064(2) 0.063(2) 0.0902(13) -0.0029(15) -0.0368(16) -0.0089(16) C530 0.0585(7) 0.0585(7) 0.0585(7) 0.0185(7) 0.0185(7) 0.0185(7) C540 0.066(3) 0.073(3) 0.057(2) 0.0046(18) 0.002(2) -0.026(2) C531 0.0585(7) 0.0585(7) 0.0585(7) 0.0185(7) 0.0185(7) 0.0185(7) C541 0.0568 0.0568 0.0568 0.0000 0.0000 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1926(3) 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 Na1 . O29 4_565 2.4281(17) yes Na1 . O40 4_565 2.4866(18) yes Na1 . O2 . 2.4148(17) yes Na1 . O13 . 2.5095(17) yes Na1 . O67 . 2.374(2) yes Na1 . O68 . 2.392(2) yes O2 . C3 . 1.367(3) yes O2 . B12 . 1.473(3) yes C3 . C4 . 1.401(3) yes C3 . C66 . 1.390(3) yes C4 . C5 . 1.482(3) yes C4 . C63 . 1.401(3) yes C5 . C6 . 1.394(3) yes C5 . C10 . 1.410(3) yes C6 . C7 . 1.385(4) yes C6 . H61 . 0.949 no C7 . C8 . 1.380(4) yes C7 . H71 . 0.943 no C8 . C9 . 1.386(4) yes C8 . H81 . 0.939 no C9 . C10 . 1.386(3) yes C9 . H91 . 0.936 no C10 . O11 . 1.363(3) yes O11 . B12 . 1.472(3) yes O11 . Na19 . 2.4508(18) yes B12 . O13 . 1.460(3) yes B12 . O18 . 1.456(3) yes O13 . C14 . 1.362(3) yes C14 . C15 . 1.406(3) yes C14 . C62 . 1.389(3) yes C15 . C16 . 1.481(3) yes C15 . C59 . 1.401(3) yes C16 . C17 . 1.402(3) yes C16 . C58 . 1.403(3) yes C17 . O18 . 1.364(3) yes C17 . C55 . 1.391(3) yes O18 . Na19 . 2.4663(17) yes Na19 . O20 . 2.4584(18) yes Na19 . O31 . 2.4537(18) yes Na19 . O49 . 2.336(2) yes Na19 . O50 . 2.482(2) yes O20 . C21 . 1.360(3) yes O20 . B30 . 1.468(3) yes C21 . C22 . 1.405(3) yes C21 . C26 . 1.393(3) yes C22 . C23 . 1.397(3) yes C22 . C27 . 1.482(3) yes C23 . C24 . 1.389(4) yes C23 . H231 . 0.943 no C24 . C25 . 1.380(4) yes C24 . H241 . 0.939 no C25 . C26 . 1.387(4) yes C25 . H251 . 0.914 no C26 . H261 . 0.948 no C27 . C28 . 1.399(3) yes C27 . C48 . 1.403(3) yes C28 . O29 . 1.370(3) yes C28 . C45 . 1.391(3) yes O29 . B30 . 1.464(3) yes B30 . O31 . 1.463(3) yes B30 . O40 . 1.467(3) yes O31 . C32 . 1.367(3) yes C32 . C33 . 1.395(4) yes C32 . C37 . 1.401(3) yes C33 . C34 . 1.379(4) yes C33 . H331 . 0.932 no C34 . C35 . 1.383(4) yes C34 . H341 . 0.932 no C35 . C36 . 1.387(4) yes C35 . H351 . 0.927 no C36 . C37 . 1.400(4) yes C36 . H361 . 0.953 no C37 . C38 . 1.479(4) yes C38 . C39 . 1.405(3) yes C38 . C44 . 1.399(3) yes C39 . O40 . 1.366(3) yes C39 . C41 . 1.388(4) yes C41 . C42 . 1.393(4) yes C41 . H411 . 0.919 no C42 . C43 . 1.372(4) yes C42 . H421 . 0.943 no C43 . C44 . 1.373(4) yes C43 . H431 . 0.942 no C44 . H441 . 0.936 no C45 . C46 . 1.380(4) yes C45 . H451 . 0.944 no C46 . C47 . 1.381(4) yes C46 . H461 . 0.938 no C47 . C48 . 1.381(4) yes C47 . H471 . 0.931 no C48 . H481 . 0.948 no O49 . H491 . 0.822 no O49 . H492 . 0.808 no O50 . C51 . 1.358(4) yes O50 . C530 . 1.412(4) yes C51 . C52 . 1.569(5) yes C51 . H511 . 0.978 no C51 . H512 . 0.994 no C52 . H521 . 0.950 no C52 . H522 . 0.950 no C52 . H523 . 0.950 no C55 . C56 . 1.380(4) yes C55 . H551 . 0.923 no C56 . C57 . 1.378(4) yes C56 . H561 . 0.934 no C57 . C58 . 1.387(4) yes C57 . H571 . 0.931 no C58 . H581 . 0.926 no C59 . C60 . 1.384(4) yes C59 . H591 . 0.936 no C60 . C61 . 1.378(4) yes C60 . H601 . 0.931 no C61 . C62 . 1.387(4) yes C61 . H611 . 0.936 no C62 . H621 . 0.936 no C63 . C64 . 1.387(4) yes C63 . H631 . 0.937 no C64 . C65 . 1.379(4) yes C64 . H641 . 0.946 no C65 . C66 . 1.391(4) yes C65 . H651 . 0.941 no C66 . H661 . 0.940 no O67 . H671 . 0.831 no O67 . H672 . 0.834 no O68 . C69 . 1.295(4) yes O68 . C71 . 1.423(5) yes C69 . C70 . 1.566(6) yes C69 . H691 . 0.969 no C69 . H692 . 0.955 no C70 . H701 . 0.968 no C70 . H702 . 0.962 no C70 . H703 . 0.964 no C71 . C72 . 1.507(6) yes C71 . H711 . 0.973 no C71 . H712 . 0.977 no C72 . H721 . 0.908 no C72 . H722 . 0.926 no C72 . H723 . 0.939 no C530 . C540 . 1.5136(10) yes C530 . H5301 . 1.012 no C530 . H5302 . 0.981 no C540 . H5401 . 0.974 no C540 . H5402 . 1.018 no C540 . H5403 . 0.976 no C531 . C541 . 1.5154(10) yes C531 . H5311 . 0.985 no C531 . H5312 . 0.972 no C541 . H5411 . 0.936 no C541 . H5412 . 0.962 no C541 . H5413 . 0.959 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 O29 4_565 Na1 . O40 4_565 55.10(5) yes O29 4_565 Na1 . O2 . 94.65(6) yes O40 4_565 Na1 . O2 . 147.03(7) yes O29 4_565 Na1 . O13 . 146.90(6) yes O40 4_565 Na1 . O13 . 157.42(6) yes O2 . Na1 . O13 . 54.99(5) yes O29 4_565 Na1 . O67 . 88.29(7) yes O40 4_565 Na1 . O67 . 89.72(6) yes O2 . Na1 . O67 . 103.43(7) yes O13 . Na1 . O67 . 86.91(6) yes O29 4_565 Na1 . O68 . 123.16(8) yes O40 4_565 Na1 . O68 . 82.81(7) yes O2 . Na1 . O68 . 108.32(8) yes O13 . Na1 . O68 . 82.92(7) yes O67 . Na1 . O68 . 131.95(9) yes Na1 . O2 . C3 . 133.19(13) yes Na1 . O2 . B12 . 103.10(13) yes C3 . O2 . B12 . 117.96(17) yes O2 . C3 . C4 . 119.6(2) yes O2 . C3 . C66 . 119.6(2) yes C4 . C3 . C66 . 120.8(2) yes C3 . C4 . C5 . 120.9(2) yes C3 . C4 . C63 . 117.7(2) yes C5 . C4 . C63 . 121.4(2) yes C4 . C5 . C6 . 121.6(2) yes C4 . C5 . C10 . 120.2(2) yes C6 . C5 . C10 . 118.2(2) yes C5 . C6 . C7 . 121.1(2) yes C5 . C6 . H61 . 118.0 no C7 . C6 . H61 . 120.9 no C6 . C7 . C8 . 120.3(2) yes C6 . C7 . H71 . 119.4 no C8 . C7 . H71 . 120.4 no C7 . C8 . C9 . 119.8(2) yes C7 . C8 . H81 . 120.6 no C9 . C8 . H81 . 119.6 no C8 . C9 . C10 . 120.5(2) yes C8 . C9 . H91 . 120.7 no C10 . C9 . H91 . 118.8 no C5 . C10 . C9 . 120.2(2) yes C5 . C10 . O11 . 120.2(2) yes C9 . C10 . O11 . 119.5(2) yes C10 . O11 . B12 . 118.41(17) yes C10 . O11 . Na19 . 135.48(13) yes B12 . O11 . Na19 . 101.68(13) yes O2 . B12 . O11 . 112.32(18) yes O2 . B12 . O13 . 101.69(17) yes O11 . B12 . O13 . 113.92(19) yes O2 . B12 . O18 . 114.02(19) yes O11 . B12 . O18 . 101.47(17) yes O13 . B12 . O18 . 113.94(18) yes Na1 . O13 . B12 . 99.31(12) yes Na1 . O13 . C14 . 139.07(13) yes B12 . O13 . C14 . 120.61(17) yes O13 . C14 . C15 . 121.0(2) yes O13 . C14 . C62 . 118.4(2) yes C15 . C14 . C62 . 120.4(2) yes C14 . C15 . C16 . 121.8(2) yes C14 . C15 . C59 . 117.6(2) yes C16 . C15 . C59 . 120.6(2) yes C15 . C16 . C17 . 121.43(19) yes C15 . C16 . C58 . 120.5(2) yes C17 . C16 . C58 . 118.1(2) yes C16 . C17 . O18 . 120.7(2) yes C16 . C17 . C55 . 120.5(2) yes O18 . C17 . C55 . 118.7(2) yes C17 . O18 . B12 . 119.49(17) yes C17 . O18 . Na19 . 138.50(13) yes B12 . O18 . Na19 . 101.48(13) yes O11 . Na19 . O18 . 54.91(5) yes O11 . Na19 . O20 . 148.73(6) yes O18 . Na19 . O20 . 155.86(7) yes O11 . Na19 . O31 . 94.50(6) yes O18 . Na19 . O31 . 149.11(7) yes O20 . Na19 . O31 . 55.03(6) yes O11 . Na19 . O49 . 95.31(7) yes O18 . Na19 . O49 . 93.64(6) yes O20 . Na19 . O49 . 81.23(6) yes O31 . Na19 . O49 . 93.44(7) yes O11 . Na19 . O50 . 119.84(7) yes O18 . Na19 . O50 . 80.24(6) yes O20 . Na19 . O50 . 84.61(6) yes O31 . Na19 . O50 . 117.44(7) yes O49 . Na19 . O50 . 128.56(8) yes Na19 . O20 . C21 . 133.62(13) yes Na19 . O20 . B30 . 101.55(13) yes C21 . O20 . B30 . 121.17(17) yes O20 . C21 . C22 . 121.0(2) yes O20 . C21 . C26 . 118.7(2) yes C22 . C21 . C26 . 120.2(2) yes C21 . C22 . C23 . 118.1(2) yes C21 . C22 . C27 . 121.1(2) yes C23 . C22 . C27 . 120.7(2) yes C22 . C23 . C24 . 121.6(2) yes C22 . C23 . H231 . 118.5 no C24 . C23 . H231 . 120.0 no C23 . C24 . C25 . 119.4(2) yes C23 . C24 . H241 . 120.2 no C25 . C24 . H241 . 120.4 no C24 . C25 . C26 . 120.5(2) yes C24 . C25 . H251 . 119.6 no C26 . C25 . H251 . 119.9 no C21 . C26 . C25 . 120.2(2) yes C21 . C26 . H261 . 118.4 no C25 . C26 . H261 . 121.4 no C22 . C27 . C28 . 121.4(2) yes C22 . C27 . C48 . 120.8(2) yes C28 . C27 . C48 . 117.7(2) yes C27 . C28 . O29 . 120.5(2) yes C27 . C28 . C45 . 120.6(2) yes O29 . C28 . C45 . 118.8(2) yes Na1 4_465 O29 . C28 . 137.87(13) yes Na1 4_465 O29 . B30 . 102.93(13) yes C28 . O29 . B30 . 117.77(17) yes O20 . B30 . O29 . 113.25(18) yes O20 . B30 . O31 . 101.44(17) yes O29 . B30 . O31 . 114.8(2) yes O20 . B30 . O40 . 113.1(2) yes O29 . B30 . O40 . 101.72(17) yes O31 . B30 . O40 . 113.10(18) yes Na19 . O31 . B30 . 101.91(13) yes Na19 . O31 . C32 . 136.02(13) yes B30 . O31 . C32 . 119.32(17) yes O31 . C32 . C33 . 118.8(2) yes O31 . C32 . C37 . 120.7(2) yes C33 . C32 . C37 . 120.3(2) yes C32 . C33 . C34 . 120.6(3) yes C32 . C33 . H331 . 119.7 no C34 . C33 . H331 . 119.7 no C33 . C34 . C35 . 120.0(3) yes C33 . C34 . H341 . 118.5 no C35 . C34 . H341 . 121.5 no C34 . C35 . C36 . 119.8(3) yes C34 . C35 . H351 . 120.5 no C36 . C35 . H351 . 119.7 no C35 . C36 . C37 . 121.3(3) yes C35 . C36 . H361 . 119.4 no C37 . C36 . H361 . 119.3 no C32 . C37 . C36 . 118.0(2) yes C32 . C37 . C38 . 120.7(2) yes C36 . C37 . C38 . 121.2(2) yes C37 . C38 . C39 . 121.7(2) yes C37 . C38 . C44 . 120.4(2) yes C39 . C38 . C44 . 117.9(2) yes C38 . C39 . O40 . 120.7(2) yes C38 . C39 . C41 . 120.0(2) yes O40 . C39 . C41 . 119.2(2) yes C39 . O40 . Na1 4_465 137.72(13) yes C39 . O40 . B30 . 119.38(17) yes Na1 4_465 O40 . B30 . 100.22(12) yes C39 . C41 . C42 . 120.5(2) yes C39 . C41 . H411 . 119.0 no C42 . C41 . H411 . 120.5 no C41 . C42 . C43 . 119.7(3) yes C41 . C42 . H421 . 120.2 no C43 . C42 . H421 . 120.1 no C42 . C43 . C44 . 120.2(2) yes C42 . C43 . H431 . 120.1 no C44 . C43 . H431 . 119.7 no C38 . C44 . C43 . 121.6(2) yes C38 . C44 . H441 . 119.7 no C43 . C44 . H441 . 118.7 no C28 . C45 . C46 . 120.3(2) yes C28 . C45 . H451 . 119.1 no C46 . C45 . H451 . 120.6 no C45 . C46 . C47 . 120.1(2) yes C45 . C46 . H461 . 120.4 no C47 . C46 . H461 . 119.5 no C46 . C47 . C48 . 119.8(2) yes C46 . C47 . H471 . 121.0 no C48 . C47 . H471 . 119.1 no C27 . C48 . C47 . 121.4(2) yes C27 . C48 . H481 . 118.2 no C47 . C48 . H481 . 120.4 no Na19 . O49 . H491 . 115.9 no Na19 . O49 . H492 . 108.8 no H491 . O49 . H492 . 108.4 no Na19 . O50 . C51 . 115.86(17) yes Na19 . O50 . C530 . 130.89(17) yes C51 . O50 . C530 . 109.6(2) yes O50 . C51 . C52 . 109.7(2) yes O50 . C51 . H511 . 109.3 no C52 . C51 . H511 . 109.0 no O50 . C51 . H512 . 108.8 no C52 . C51 . H512 . 109.6 no H511 . C51 . H512 . 110.4 no C51 . C52 . H521 . 109.5 no C51 . C52 . H522 . 109.6 no H521 . C52 . H522 . 109.5 no C51 . C52 . H523 . 109.3 no H521 . C52 . H523 . 109.5 no H522 . C52 . H523 . 109.5 no C17 . C55 . C56 . 120.0(2) yes C17 . C55 . H551 . 120.3 no C56 . C55 . H551 . 119.6 no C55 . C56 . C57 . 120.7(2) yes C55 . C56 . H561 . 120.8 no C57 . C56 . H561 . 118.5 no C56 . C57 . C58 . 119.6(2) yes C56 . C57 . H571 . 120.0 no C58 . C57 . H571 . 120.4 no C16 . C58 . C57 . 121.1(2) yes C16 . C58 . H581 . 120.6 no C57 . C58 . H581 . 118.3 no C15 . C59 . C60 . 121.8(2) yes C15 . C59 . H591 . 118.6 no C60 . C59 . H591 . 119.6 no C59 . C60 . C61 . 119.6(2) yes C59 . C60 . H601 . 119.1 no C61 . C60 . H601 . 121.2 no C60 . C61 . C62 . 120.1(2) yes C60 . C61 . H611 . 120.3 no C62 . C61 . H611 . 119.6 no C14 . C62 . C61 . 120.4(2) yes C14 . C62 . H621 . 119.8 no C61 . C62 . H621 . 119.8 no C4 . C63 . C64 . 121.4(2) yes C4 . C63 . H631 . 118.2 no C64 . C63 . H631 . 120.3 no C63 . C64 . C65 . 120.0(2) yes C63 . C64 . H641 . 120.1 no C65 . C64 . H641 . 119.8 no C64 . C65 . C66 . 119.8(2) yes C64 . C65 . H651 . 120.8 no C66 . C65 . H651 . 119.5 no C65 . C66 . C3 . 120.2(2) yes C65 . C66 . H661 . 121.0 no C3 . C66 . H661 . 118.7 no Na1 . O67 . H671 . 110.0 no Na1 . O67 . H672 . 112.4 no H671 . O67 . H672 . 104.2 no Na1 . O68 . C69 . 124.8(2) yes Na1 . O68 . C71 . 122.3(2) yes C69 . O68 . C71 . 112.9(3) yes O68 . C69 . C70 . 110.4(3) yes O68 . C69 . H691 . 108.9 no C70 . C69 . H691 . 108.7 no O68 . C69 . H692 . 110.0 no C70 . C69 . H692 . 108.4 no H691 . C69 . H692 . 110.4 no C69 . C70 . H701 . 105.5 no C69 . C70 . H702 . 110.7 no H701 . C70 . H702 . 109.2 no C69 . C70 . H703 . 111.4 no H701 . C70 . H703 . 110.5 no H702 . C70 . H703 . 109.4 no O68 . C71 . C72 . 116.8(3) yes O68 . C71 . H711 . 106.9 no C72 . C71 . H711 . 106.0 no O68 . C71 . H712 . 107.8 no C72 . C71 . H712 . 107.5 no H711 . C71 . H712 . 111.9 no C71 . C72 . H721 . 112.1 no C71 . C72 . H722 . 107.5 no H721 . C72 . H722 . 108.1 no C71 . C72 . H723 . 109.4 no H721 . C72 . H723 . 112.4 no H722 . C72 . H723 . 107.0 no O50 . C530 . C540 . 109.8(3) yes O50 . C530 . H5301 . 111.90(17) no C540 . C530 . H5301 . 107.4(2) no O50 . C530 . H5302 . 107.88(15) no C540 . C530 . H5302 . 108.6(2) no H5301 . C530 . H5302 . 111.2 no C530 . C540 . H5401 . 107.9 no C530 . C540 . H5402 . 102.3 no H5401 . C540 . H5402 . 112.8 no C530 . C540 . H5403 . 107.9 no H5401 . C540 . H5403 . 111.4 no H5402 . C540 . H5403 . 113.8 no O50 . C531 . C541 . 150.7(7) yes O50 . C531 . H5311 . 101.31(17) no C541 . C531 . H5311 . 92.9(6) no O50 . C531 . H5312 . 100.40(15) no C541 . C531 . H5312 . 98.5(6) no H5311 . C531 . H5312 . 110.1 no C531 . C541 . H5411 . 118.8 no C531 . C541 . H5412 . 106.0 no H5411 . C541 . H5412 . 109.5 no C531 . C541 . H5413 . 103.3 no H5411 . C541 . H5413 . 108.9 no H5412 . C541 . H5413 . 110.1 no 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 C65 . H651 . O49 2_665 161 0.94 2.54 3.442(4) yes _chemical_name_common . #============================================================================== data_3c _database_code_depnum_ccdc_archive 'CCDC 796352' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 08-04-04 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5769 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 11.9831(2) _cell_length_b 21.9931(5) _cell_length_c 13.4659(3) _cell_angle_alpha 90 _cell_angle_beta 106.0392(10) _cell_angle_gamma 90 _cell_volume 3410.73(12) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' 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' _cell_formula_units_Z 4 # Given Formula = C36 H40 B1 Na1 O10 # Dc = 1.30 Fooo = 1448.00 Mu = 1.04 M = 666.51 # Found Formula = C36 H42 B1 Na1 O11 # Dc = 1.33 FOOO = 1448.00 Mu = 1.08 M = 684.52 _chemical_formula_sum 'C36 H42 B1 Na1 O11' _chemical_formula_moiety 'C12 H26 Na1 O7, C24 H16 B O4' _chemical_compound_source . _chemical_formula_weight 684.52 _cell_measurement_reflns_used 68528 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.108 # Sheldrick geometric approximatio 0.98 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.99 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 150 _diffrn_reflns_number 44857 _reflns_number_total 7686 _diffrn_reflns_av_R_equivalents 0.063 # Number of reflections with Friedels Law is 7686 # Number of reflections without Friedels Law is 7686 # Theoretical number of reflections is about 7810 _diffrn_reflns_theta_min 5.105 _diffrn_reflns_theta_max 27.467 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.270 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 2.78 _oxford_diffrn_Wilson_scale 8.40 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.52 _refine_diff_density_max 0.53 # 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>-3.0\s(I) _refine_ls_number_reflns 7685 _refine_ls_number_restraints 0 _refine_ls_number_parameters 442 _oxford_refine_ls_R_factor_ref 0.0979 _refine_ls_wR_factor_ref 0.1313 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.000660 # The values computed from all data _oxford_reflns_number_all 7686 _refine_ls_R_factor_all 0.0980 _refine_ls_wR_factor_all 0.1314 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4972 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_gt 0.1093 # 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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.07P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Na1 Na 0.68957(7) 0.50225(4) 0.47959(6) 0.0395 1.0000 Uani . . . . . . . O2 O 0.74321(12) 0.44952(7) 0.34519(11) 0.0409 1.0000 Uani . . . . . . . O3 O 0.41768(10) 0.62443(6) 0.81832(10) 0.0289 1.0000 Uani . . . . . . . C4 C 0.52679(16) 0.62119(9) 0.88337(14) 0.0276 1.0000 Uani . . . . . . . C5 C 0.61367(16) 0.66199(9) 0.87356(14) 0.0287 1.0000 Uani . . . . . . . C6 C 0.58769(16) 0.70925(9) 0.79245(15) 0.0298 1.0000 Uani . . . . . . . C7 C 0.66465(18) 0.72154(9) 0.73363(16) 0.0355 1.0000 Uani . . . . . . . C8 C 0.6397(2) 0.76414(10) 0.65496(17) 0.0425 1.0000 Uani . . . . . . . C9 C 0.5359(2) 0.79550(10) 0.63314(17) 0.0427 1.0000 Uani . . . . . . . C10 C 0.45775(18) 0.78467(9) 0.69008(16) 0.0361 1.0000 Uani . . . . . . . C11 C 0.48287(16) 0.74176(8) 0.76916(15) 0.0291 1.0000 Uani . . . . . . . O12 O 0.40697(11) 0.73496(6) 0.82735(10) 0.0311 1.0000 Uani . . . . . . . B13 B 0.34501(18) 0.67764(10) 0.82365(17) 0.0281 1.0000 Uani . . . . . . . O14 O 0.24820(11) 0.67034(6) 0.72946(9) 0.0295 1.0000 Uani . . . . . . . C15 C 0.15354(16) 0.70721(8) 0.71676(15) 0.0290 1.0000 Uani . . . . . . . C16 C 0.08139(16) 0.70134(9) 0.78242(15) 0.0290 1.0000 Uani . . . . . . . C17 C 0.10456(16) 0.65432(9) 0.86407(14) 0.0281 1.0000 Uani . . . . . . . C18 C 0.21797(16) 0.64398(9) 0.92667(14) 0.0286 1.0000 Uani . . . . . . . O19 O 0.30719(11) 0.67913(6) 0.91791(10) 0.0304 1.0000 Uani . . . . . . . C20 C 0.23809(18) 0.59979(9) 1.00344(15) 0.0338 1.0000 Uani . . . . . . . C21 C 0.14770(19) 0.56526(10) 1.01855(17) 0.0391 1.0000 Uani . . . . . . . C22 C 0.03605(18) 0.57450(9) 0.95707(16) 0.0375 1.0000 Uani . . . . . . . C23 C 0.01536(17) 0.61864(9) 0.88084(16) 0.0336 1.0000 Uani . . . . . . . C24 C -0.01638(17) 0.73888(9) 0.76385(17) 0.0358 1.0000 Uani . . . . . . . C25 C -0.04434(18) 0.77888(10) 0.68133(18) 0.0415 1.0000 Uani . . . . . . . C26 C 0.02634(18) 0.78273(9) 0.61592(17) 0.0402 1.0000 Uani . . . . . . . C27 C 0.12542(17) 0.74725(9) 0.63414(15) 0.0340 1.0000 Uani . . . . . . . C28 C 0.72584(17) 0.65346(10) 0.93861(16) 0.0352 1.0000 Uani . . . . . . . C29 C 0.75203(18) 0.60591(10) 1.00862(16) 0.0385 1.0000 Uani . . . . . . . C30 C 0.66621(18) 0.56564(10) 1.01538(15) 0.0367 1.0000 Uani . . . . . . . C31 C 0.55380(17) 0.57351(9) 0.95346(15) 0.0324 1.0000 Uani . . . . . . . O32 O 0.53430(12) 0.51794(7) 0.29858(11) 0.0386 1.0000 Uani . . . . . . . C33 C 0.41539(18) 0.50172(11) 0.28150(17) 0.0421 1.0000 Uani . . . . . . . C34 C 0.4089(2) 0.44004(11) 0.32647(16) 0.0438 1.0000 Uani . . . . . . . O35 O 0.44966(13) 0.44293(7) 0.43658(11) 0.0406 1.0000 Uani . . . . . . . C36 C 0.4713(2) 0.38329(10) 0.48138(18) 0.0454 1.0000 Uani . . . . . . . C37 C 0.5878(2) 0.35815(10) 0.48256(19) 0.0461 1.0000 Uani . . . . . . . O38 O 0.67506(13) 0.39451(6) 0.55099(11) 0.0420 1.0000 Uani . . . . . . . C39 C 0.7869(2) 0.36686(11) 0.57516(19) 0.0483 1.0000 Uani . . . . . . . C40 C 0.8694(2) 0.40610(11) 0.65204(19) 0.0523 1.0000 Uani . . . . . . . O41 O 0.87703(13) 0.46316(7) 0.60475(12) 0.0475 1.0000 Uani . . . . . . . C42 C 0.9530(2) 0.50382(13) 0.67365(19) 0.0552 1.0000 Uani . . . . . . . C43 C 0.9598(2) 0.56108(12) 0.6172(2) 0.0519 1.0000 Uani . . . . . . . O44 O 0.84768(13) 0.58839(7) 0.58831(12) 0.0465 1.0000 Uani . . . . . . . C45 C 0.8441(2) 0.64263(11) 0.5290(2) 0.0519 1.0000 Uani . . . . . . . C46 C 0.8200(2) 0.62992(11) 0.4162(2) 0.0517 1.0000 Uani . . . . . . . O47 O 0.71074(13) 0.59955(7) 0.38357(11) 0.0412 1.0000 Uani . . . . . . . C48 C 0.6726(2) 0.59092(11) 0.27488(17) 0.0463 1.0000 Uani . . . . . . . C49 C 0.5468(2) 0.57307(11) 0.24679(17) 0.0456 1.0000 Uani . . . . . . . H71 H 0.7362 0.6987 0.7479 0.0429 1.0000 Uiso R . . . . . . H81 H 0.6936 0.7712 0.6164 0.0528 1.0000 Uiso R . . . . . . H91 H 0.5187 0.8244 0.5797 0.0514 1.0000 Uiso R . . . . . . H101 H 0.3864 0.8061 0.6753 0.0430 1.0000 Uiso R . . . . . . H201 H 0.3155 0.5929 1.0451 0.0405 1.0000 Uiso R . . . . . . H211 H 0.1628 0.5359 1.0717 0.0487 1.0000 Uiso R . . . . . . H221 H -0.0271 0.5517 0.9655 0.0477 1.0000 Uiso R . . . . . . H231 H -0.0603 0.6246 0.8375 0.0403 1.0000 Uiso R . . . . . . H241 H -0.0659 0.7363 0.8092 0.0422 1.0000 Uiso R . . . . . . H251 H -0.1129 0.8036 0.6680 0.0471 1.0000 Uiso R . . . . . . H261 H 0.0066 0.8089 0.5579 0.0450 1.0000 Uiso R . . . . . . H271 H 0.1761 0.7496 0.5896 0.0398 1.0000 Uiso R . . . . . . H281 H 0.7852 0.6815 0.9339 0.0406 1.0000 Uiso R . . . . . . H291 H 0.8286 0.6008 1.0514 0.0445 1.0000 Uiso R . . . . . . H301 H 0.6845 0.5333 1.0614 0.0439 1.0000 Uiso R . . . . . . H311 H 0.4934 0.5467 0.9588 0.0390 1.0000 Uiso R . . . . . . H331 H 0.3775 0.5324 0.3131 0.0494 1.0000 Uiso R . . . . . . H332 H 0.3757 0.5009 0.2055 0.0495 1.0000 Uiso R . . . . . . H341 H 0.4569 0.4109 0.3013 0.0514 1.0000 Uiso R . . . . . . H342 H 0.3283 0.4267 0.3072 0.0524 1.0000 Uiso R . . . . . . H361 H 0.4675 0.3868 0.5528 0.0565 1.0000 Uiso R . . . . . . H362 H 0.4097 0.3558 0.4427 0.0564 1.0000 Uiso R . . . . . . H371 H 0.5977 0.3591 0.4115 0.0562 1.0000 Uiso R . . . . . . H372 H 0.5947 0.3159 0.5099 0.0578 1.0000 Uiso R . . . . . . H391 H 0.8133 0.3618 0.5126 0.0579 1.0000 Uiso R . . . . . . H392 H 0.7844 0.3266 0.6076 0.0589 1.0000 Uiso R . . . . . . H402 H 0.9470 0.3864 0.6735 0.0625 1.0000 Uiso R . . . . . . H401 H 0.8401 0.4123 0.7137 0.0621 1.0000 Uiso R . . . . . . H422 H 1.0311 0.4862 0.6989 0.0640 1.0000 Uiso R . . . . . . H421 H 0.9192 0.5131 0.7312 0.0641 1.0000 Uiso R . . . . . . H431 H 1.0171 0.5885 0.6617 0.0621 1.0000 Uiso R . . . . . . H432 H 0.9827 0.5528 0.5543 0.0613 1.0000 Uiso R . . . . . . H451 H 0.9192 0.6646 0.5557 0.0631 1.0000 Uiso R . . . . . . H452 H 0.7805 0.6681 0.5397 0.0636 1.0000 Uiso R . . . . . . H461 H 0.8179 0.6681 0.3781 0.0651 1.0000 Uiso R . . . . . . H462 H 0.8813 0.6042 0.4033 0.0642 1.0000 Uiso R . . . . . . H482 H 0.6803 0.6291 0.2384 0.0575 1.0000 Uiso R . . . . . . H481 H 0.7226 0.5582 0.2559 0.0573 1.0000 Uiso R . . . . . . H492 H 0.5026 0.6057 0.2665 0.0544 1.0000 Uiso R . . . . . . H491 H 0.5184 0.5664 0.1713 0.0543 1.0000 Uiso R . . . . . . H22 H 0.7609 0.4129 0.3352 0.0601 1.0000 Uiso R . . . . . . H21 H 0.6781 0.4536 0.2989 0.0611 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 Na1 0.0490(5) 0.0331(4) 0.0391(5) -0.0016(4) 0.0166(4) 0.0020(4) O2 0.0390(8) 0.0364(8) 0.0439(8) -0.0090(7) 0.0057(6) 0.0044(7) O3 0.0248(7) 0.0256(7) 0.0356(7) -0.0008(6) 0.0070(6) -0.0003(5) C4 0.0267(10) 0.0265(10) 0.0303(10) -0.0050(8) 0.0088(8) 0.0035(8) C5 0.0280(10) 0.0280(10) 0.0317(10) -0.0058(8) 0.0108(8) 0.0014(8) C6 0.0300(10) 0.0261(10) 0.0349(11) -0.0058(8) 0.0118(8) -0.0059(8) C7 0.0316(11) 0.0332(11) 0.0440(12) -0.0058(9) 0.0143(9) -0.0057(9) C8 0.0450(13) 0.0405(13) 0.0481(13) -0.0016(10) 0.0230(11) -0.0133(10) C9 0.0522(14) 0.0357(12) 0.0411(13) 0.0062(10) 0.0143(10) -0.0073(11) C10 0.0377(11) 0.0266(11) 0.0432(12) 0.0001(9) 0.0098(9) -0.0036(9) C11 0.0312(10) 0.0234(10) 0.0342(11) -0.0036(8) 0.0114(8) -0.0048(8) O12 0.0310(7) 0.0254(7) 0.0402(8) -0.0018(6) 0.0152(6) -0.0007(6) B13 0.0265(11) 0.0280(11) 0.0304(11) 0.0000(9) 0.0087(9) 0.0020(9) O14 0.0279(7) 0.0307(7) 0.0299(7) -0.0016(6) 0.0080(6) 0.0029(6) C15 0.0248(9) 0.0263(10) 0.0334(11) -0.0036(8) 0.0041(8) -0.0006(8) C16 0.0255(10) 0.0266(10) 0.0325(11) -0.0035(8) 0.0042(8) -0.0020(8) C17 0.0271(10) 0.0264(10) 0.0326(10) -0.0048(8) 0.0113(8) 0.0010(8) C18 0.0280(10) 0.0293(10) 0.0308(10) -0.0057(8) 0.0121(8) -0.0007(8) O19 0.0267(7) 0.0351(8) 0.0295(7) -0.0021(6) 0.0083(5) -0.0043(6) C20 0.0356(11) 0.0327(11) 0.0333(11) -0.0005(9) 0.0097(9) 0.0036(9) C21 0.0471(13) 0.0315(11) 0.0428(12) 0.0031(9) 0.0195(10) 0.0012(10) C22 0.0394(12) 0.0320(11) 0.0471(13) -0.002(1) 0.0222(10) -0.0069(9) C23 0.0284(10) 0.0318(11) 0.0426(12) -0.0065(9) 0.0130(9) -0.0007(8) C24 0.0280(10) 0.0316(11) 0.0464(13) -0.0036(9) 0.0083(9) -0.0020(9) C25 0.0308(11) 0.0273(11) 0.0591(15) 0.0001(10) 0.0002(10) 0.0020(9) C26 0.0381(12) 0.0295(11) 0.0444(13) 0.0060(9) -0.0027(10) -0.0026(9) C27 0.0338(11) 0.0315(11) 0.0332(11) 0.0013(9) 0.0032(9) -0.0040(9) C28 0.0280(10) 0.0384(12) 0.0394(12) -0.0086(9) 0.0098(9) -0.0026(9) C29 0.0315(11) 0.0442(13) 0.0362(12) -0.0056(10) 0.0036(9) 0.0088(10) C30 0.0431(12) 0.0345(11) 0.0320(11) 0.0022(9) 0.0094(9) 0.0119(10) C31 0.0343(11) 0.0300(11) 0.0344(11) -0.0019(9) 0.0119(9) 0.0024(9) O32 0.0382(8) 0.0389(8) 0.0383(8) 0.0021(6) 0.0097(6) 0.0038(7) C33 0.0356(12) 0.0499(14) 0.0392(12) -0.0073(10) 0.0074(9) 0.0059(10) C34 0.0414(12) 0.0516(14) 0.0391(12) -0.0175(11) 0.0120(10) -0.0077(11) O35 0.0470(9) 0.0386(8) 0.0390(8) -0.0108(7) 0.0163(7) -0.0035(7) C36 0.0523(14) 0.0407(13) 0.0498(14) -0.0100(11) 0.0253(11) -0.0138(11) C37 0.0588(15) 0.0293(11) 0.0554(14) -0.0058(10) 0.0244(12) -0.0059(11) O38 0.0476(9) 0.0314(8) 0.0490(9) -0.0025(7) 0.0167(7) 0.0018(7) C39 0.0539(15) 0.0361(13) 0.0582(15) 0.0082(11) 0.0212(12) 0.0115(11) C40 0.0533(15) 0.0515(15) 0.0514(14) 0.0110(12) 0.0130(12) 0.0133(12) O41 0.0507(9) 0.0435(9) 0.0427(9) -0.0013(7) 0.0036(7) -0.0011(7) C42 0.0441(14) 0.0651(17) 0.0495(15) -0.0129(13) 0.0015(11) -0.0004(12) C43 0.0388(13) 0.0592(16) 0.0566(15) -0.0176(13) 0.0111(11) -0.0075(12) O44 0.0405(9) 0.0478(10) 0.0529(10) -0.0091(8) 0.0156(7) -0.0059(7) C45 0.0504(14) 0.0384(13) 0.0711(17) -0.0143(12) 0.0237(12) -0.0145(11) C46 0.0536(15) 0.0420(13) 0.0664(17) -0.0007(12) 0.0281(12) -0.0161(11) O47 0.0493(9) 0.0357(8) 0.0429(9) 0.0011(7) 0.0201(7) -0.0070(7) C48 0.0566(14) 0.0442(13) 0.0426(13) 0.0120(10) 0.0214(11) 0.0053(11) C49 0.0551(14) 0.0470(14) 0.0362(12) 0.0095(10) 0.0150(10) 0.0122(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3467(4) 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 Na1 . O35 2_666 2.5598(16) yes Na1 . O2 . 2.3825(16) yes Na1 . O32 . 2.6489(16) yes Na1 . O38 . 2.5809(16) yes Na1 . O41 . 2.5561(17) yes Na1 . O44 . 2.7910(17) yes Na1 . O47 . 2.5489(16) yes O2 . H22 . 0.852 no O2 . H21 . 0.858 no O3 . C4 . 1.360(2) yes O3 . B13 . 1.472(2) yes C4 . C5 . 1.408(3) yes C4 . C31 . 1.388(3) yes C5 . C6 . 1.477(3) yes C5 . C28 . 1.400(3) yes C6 . C7 . 1.398(3) yes C6 . C11 . 1.403(3) yes C7 . C8 . 1.384(3) yes C7 . H71 . 0.966 no C8 . C9 . 1.381(3) yes C8 . H81 . 0.946 no C9 . C10 . 1.385(3) yes C9 . H91 . 0.939 no C10 . C11 . 1.392(3) yes C10 . H101 . 0.949 no C11 . O12 . 1.363(2) yes O12 . B13 . 1.457(3) yes B13 . O14 . 1.472(3) yes B13 . O19 . 1.461(2) yes O14 . C15 . 1.366(2) yes C15 . C16 . 1.403(3) yes C15 . C27 . 1.386(3) yes C16 . C17 . 1.479(3) yes C16 . C24 . 1.398(3) yes C17 . C18 . 1.406(3) yes C17 . C23 . 1.394(3) yes C18 . O19 . 1.351(2) yes C18 . C20 . 1.391(3) yes C20 . C21 . 1.383(3) yes C20 . H201 . 0.954 no C21 . C22 . 1.380(3) yes C21 . H211 . 0.944 no C22 . C23 . 1.385(3) yes C22 . H221 . 0.941 no C23 . H231 . 0.942 no C24 . C25 . 1.384(3) yes C24 . H241 . 0.963 no C25 . C26 . 1.383(3) yes C25 . H251 . 0.960 no C26 . C27 . 1.385(3) yes C26 . H261 . 0.946 no C27 . H271 . 0.965 no C28 . C29 . 1.385(3) yes C28 . H281 . 0.956 no C29 . C30 . 1.379(3) yes C29 . H291 . 0.946 no C30 . C31 . 1.385(3) yes C30 . H301 . 0.928 no C31 . H311 . 0.952 no O32 . C33 . 1.425(3) yes O32 . C49 . 1.427(3) yes C33 . C34 . 1.496(3) yes C33 . H331 . 0.974 no C33 . H332 . 1.003 no C34 . O35 . 1.429(3) yes C34 . H341 . 0.982 no C34 . H342 . 0.973 no O35 . C36 . 1.437(3) yes C36 . C37 . 1.497(3) yes C36 . H361 . 0.978 no C36 . H362 . 0.985 no C37 . O38 . 1.432(3) yes C37 . H371 . 0.997 no C37 . H372 . 0.994 no O38 . C39 . 1.425(3) yes C39 . C40 . 1.493(4) yes C39 . H391 . 0.984 no C39 . H392 . 0.991 no C40 . O41 . 1.422(3) yes C40 . H402 . 0.994 no C40 . H401 . 0.996 no O41 . C42 . 1.422(3) yes C42 . C43 . 1.485(4) yes C42 . H422 . 0.983 no C42 . H421 . 0.990 no C43 . O44 . 1.424(3) yes C43 . H431 . 0.983 no C43 . H432 . 0.977 no O44 . C45 . 1.430(3) yes C45 . C46 . 1.493(3) yes C45 . H451 . 0.997 no C45 . H452 . 0.988 no C46 . O47 . 1.427(3) yes C46 . H461 . 0.981 no C46 . H462 . 0.980 no O47 . C48 . 1.420(3) yes C48 . C49 . 1.502(3) yes C48 . H482 . 0.989 no C48 . H481 . 1.012 no C49 . H492 . 0.972 no C49 . H491 . 0.989 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 O35 2_666 Na1 . O2 . 155.47(6) yes O35 2_666 Na1 . O32 . 88.09(5) yes O2 . Na1 . O32 . 68.45(5) yes O35 2_666 Na1 . O38 . 98.57(5) yes O2 . Na1 . O38 . 84.05(5) yes O32 . Na1 . O38 . 111.10(5) yes O35 2_666 Na1 . O41 . 115.39(6) yes O2 . Na1 . O41 . 87.98(6) yes O32 . Na1 . O41 . 156.42(6) yes O38 . Na1 . O41 . 65.36(5) yes O35 2_666 Na1 . O44 . 83.09(5) yes O2 . Na1 . O44 . 116.25(5) yes O32 . Na1 . O44 . 126.63(5) yes O38 . Na1 . O44 . 122.25(6) yes O41 . Na1 . O44 . 62.41(5) yes O35 2_666 Na1 . O47 . 89.81(5) yes O2 . Na1 . O47 . 86.43(5) yes O32 . Na1 . O47 . 64.33(5) yes O38 . Na1 . O47 . 170.44(6) yes O41 . Na1 . O47 . 115.11(6) yes O44 . Na1 . O47 . 63.12(5) yes Na1 . O2 . H22 . 135.3 no Na1 . O2 . H21 . 96.8 no H22 . O2 . H21 . 101.5 no C4 . O3 . B13 . 119.12(14) yes O3 . C4 . C5 . 120.70(17) yes O3 . C4 . C31 . 118.67(17) yes C5 . C4 . C31 . 120.38(17) yes C4 . C5 . C6 . 120.50(17) yes C4 . C5 . C28 . 117.58(18) yes C6 . C5 . C28 . 121.80(17) yes C5 . C6 . C7 . 121.17(18) yes C5 . C6 . C11 . 121.09(17) yes C7 . C6 . C11 . 117.70(18) yes C6 . C7 . C8 . 121.9(2) yes C6 . C7 . H71 . 118.4 no C8 . C7 . H71 . 119.8 no C7 . C8 . C9 . 119.5(2) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 120.8 no C8 . C9 . C10 . 120.2(2) yes C8 . C9 . H91 . 119.7 no C10 . C9 . H91 . 120.1 no C9 . C10 . C11 . 120.2(2) yes C9 . C10 . H101 . 120.4 no C11 . C10 . H101 . 119.3 no C6 . C11 . C10 . 120.48(18) yes C6 . C11 . O12 . 120.93(17) yes C10 . C11 . O12 . 118.46(17) yes C11 . O12 . B13 . 119.34(14) yes O3 . B13 . O12 . 112.76(15) yes O3 . B13 . O14 . 101.95(15) yes O12 . B13 . O14 . 113.37(16) yes O3 . B13 . O19 . 112.93(16) yes O12 . B13 . O19 . 103.20(15) yes O14 . B13 . O19 . 113.02(15) yes B13 . O14 . C15 . 118.20(14) yes O14 . C15 . C16 . 120.10(17) yes O14 . C15 . C27 . 119.15(17) yes C16 . C15 . C27 . 120.60(18) yes C15 . C16 . C17 . 120.74(16) yes C15 . C16 . C24 . 117.70(18) yes C17 . C16 . C24 . 121.45(17) yes C16 . C17 . C18 . 120.72(17) yes C16 . C17 . C23 . 121.28(17) yes C18 . C17 . C23 . 118.00(18) yes C17 . C18 . O19 . 120.83(17) yes C17 . C18 . C20 . 119.95(18) yes O19 . C18 . C20 . 119.08(17) yes C18 . O19 . B13 . 120.40(15) yes C18 . C20 . C21 . 120.74(19) yes C18 . C20 . H201 . 119.2 no C21 . C20 . H201 . 120.0 no C20 . C21 . C22 . 120.0(2) yes C20 . C21 . H211 . 119.6 no C22 . C21 . H211 . 120.4 no C21 . C22 . C23 . 119.56(19) yes C21 . C22 . H221 . 121.9 no C23 . C22 . H221 . 118.6 no C17 . C23 . C22 . 121.77(19) yes C17 . C23 . H231 . 118.1 no C22 . C23 . H231 . 120.1 no C16 . C24 . C25 . 121.6(2) yes C16 . C24 . H241 . 119.0 no C25 . C24 . H241 . 119.4 no C24 . C25 . C26 . 119.7(2) yes C24 . C25 . H251 . 121.0 no C26 . C25 . H251 . 119.3 no C25 . C26 . C27 . 119.9(2) yes C25 . C26 . H261 . 120.4 no C27 . C26 . H261 . 119.7 no C15 . C27 . C26 . 120.5(2) yes C15 . C27 . H271 . 118.5 no C26 . C27 . H271 . 121.0 no C5 . C28 . C29 . 121.69(19) yes C5 . C28 . H281 . 118.4 no C29 . C28 . H281 . 119.9 no C28 . C29 . C30 . 119.80(19) yes C28 . C29 . H291 . 120.2 no C30 . C29 . H291 . 120.0 no C29 . C30 . C31 . 119.93(19) yes C29 . C30 . H301 . 119.5 no C31 . C30 . H301 . 120.6 no C4 . C31 . C30 . 120.60(19) yes C4 . C31 . H311 . 118.7 no C30 . C31 . H311 . 120.7 no Na1 . O32 . C33 . 122.20(12) yes Na1 . O32 . C49 . 114.74(12) yes C33 . O32 . C49 . 111.66(16) yes O32 . C33 . C34 . 108.86(18) yes O32 . C33 . H331 . 108.8 no C34 . C33 . H331 . 111.6 no O32 . C33 . H332 . 109.9 no C34 . C33 . H332 . 109.5 no H331 . C33 . H332 . 108.2 no C33 . C34 . O35 . 109.79(17) yes C33 . C34 . H341 . 110.5 no O35 . C34 . H341 . 108.8 no C33 . C34 . H342 . 108.9 no O35 . C34 . H342 . 108.7 no H341 . C34 . H342 . 110.2 no C34 . O35 . Na1 2_666 113.64(12) yes C34 . O35 . C36 . 111.42(16) yes Na1 2_666 O35 . C36 . 108.00(12) yes O35 . C36 . C37 . 113.65(18) yes O35 . C36 . H361 . 106.8 no C37 . C36 . H361 . 108.4 no O35 . C36 . H362 . 108.4 no C37 . C36 . H362 . 109.9 no H361 . C36 . H362 . 109.7 no C36 . C37 . O38 . 108.27(17) yes C36 . C37 . H371 . 109.8 no O38 . C37 . H371 . 110.3 no C36 . C37 . H372 . 109.3 no O38 . C37 . H372 . 108.2 no H371 . C37 . H372 . 110.9 no C37 . O38 . Na1 . 112.67(12) yes C37 . O38 . C39 . 112.47(16) yes Na1 . O38 . C39 . 108.72(12) yes O38 . C39 . C40 . 108.20(19) yes O38 . C39 . H391 . 110.9 no C40 . C39 . H391 . 110.5 no O38 . C39 . H392 . 109.9 no C40 . C39 . H392 . 107.8 no H391 . C39 . H392 . 109.4 no C39 . C40 . O41 . 108.18(19) yes C39 . C40 . H402 . 109.7 no O41 . C40 . H402 . 110.1 no C39 . C40 . H401 . 109.8 no O41 . C40 . H401 . 109.6 no H402 . C40 . H401 . 109.5 no C40 . O41 . Na1 . 116.01(14) yes C40 . O41 . C42 . 111.82(18) yes Na1 . O41 . C42 . 120.41(14) yes O41 . C42 . C43 . 108.38(19) yes O41 . C42 . H422 . 110.7 no C43 . C42 . H422 . 109.3 no O41 . C42 . H421 . 108.3 no C43 . C42 . H421 . 108.5 no H422 . C42 . H421 . 111.5 no C42 . C43 . O44 . 108.4(2) yes C42 . C43 . H431 . 109.7 no O44 . C43 . H431 . 110.8 no C42 . C43 . H432 . 110.7 no O44 . C43 . H432 . 108.1 no H431 . C43 . H432 . 109.1 no C43 . O44 . Na1 . 108.03(13) yes C43 . O44 . C45 . 112.63(18) yes Na1 . O44 . C45 . 111.25(13) yes O44 . C45 . C46 . 112.32(19) yes O44 . C45 . H451 . 108.6 no C46 . C45 . H451 . 111.0 no O44 . C45 . H452 . 107.3 no C46 . C45 . H452 . 108.3 no H451 . C45 . H452 . 109.2 no C45 . C46 . O47 . 107.69(18) yes C45 . C46 . H461 . 110.0 no O47 . C46 . H461 . 110.6 no C45 . C46 . H462 . 110.2 no O47 . C46 . H462 . 110.2 no H461 . C46 . H462 . 108.3 no C46 . O47 . Na1 . 116.65(13) yes C46 . O47 . C48 . 112.71(16) yes Na1 . O47 . C48 . 111.21(12) yes O47 . C48 . C49 . 108.01(17) yes O47 . C48 . H482 . 110.5 no C49 . C48 . H482 . 108.7 no O47 . C48 . H481 . 108.1 no C49 . C48 . H481 . 111.9 no H482 . C48 . H481 . 109.6 no C48 . C49 . O32 . 109.42(18) yes C48 . C49 . H492 . 108.9 no O32 . C49 . H492 . 110.8 no C48 . C49 . H491 . 109.5 no O32 . C49 . H491 . 108.9 no H492 . C49 . H491 . 109.3 no 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 C36 . H361 . O47 2_666 128 0.98 2.53 3.225(3) yes C46 . H461 . O12 4_564 154 0.98 2.56 3.469(3) yes O2 . H22 . O14 2_666 160 0.85 2.02 2.833(3) yes O2 . H21 . O3 2_666 125 0.86 2.40 2.977(3) yes O2 . H21 . O32 . 128 0.86 2.23 2.839(3) yes _chemical_name_common . #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 796353' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 08-05-08 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5814 _chemical_name_systematic . _chemical_melting_point 'not measured' _publ_section_exptl_refinement ; The data were particularly bad due to poor quality crystals further hampered further by solvent loss and the apparent presence of a phase transition. In addition, the difference map indicated the presence of diffuse electron density believed to be disordered solvent so SQUEEZE was used leaving voids. Despite the difficulties associated with the data collection, the connectivity and relative stereo chemistry of the BINOL is believed to be correct so the structure is included for completeness. ; 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 -0.176 0.221 0.555 165 11 ' ' 2 0.175 0.779 0.445 164 11 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void regions were treated as contributions to the A and B parts of the calculated structure factors. ; _cell_length_a 9.0212(5) _cell_length_b 16.6116(9) _cell_length_c 18.1651(10) _cell_angle_alpha 71.295(2) _cell_angle_beta 88.316(2) _cell_angle_gamma 79.317(2) _cell_volume 2532.4(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' 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' _cell_formula_units_Z 2 # Given Formula = C33 H22 B60 Na3 O26 # Dc = 2.04 Fooo = 928.00 Mu = 1.57 M = 1552.15 # Found Formula = C56 H56 B1 Na1 O7 # Dc = 1.15 FOOO = 928.00 Mu = 0.81 M = 874.86 _chemical_formula_sum 'C56 H56 B1 Na1 O7' _chemical_formula_moiety 'C56 H56 B1 Na1 O7' _chemical_compound_source . _chemical_formula_weight 874.86 _cell_measurement_reflns_used 7466 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 225 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.081 # Sheldrick geometric approximatio 0.99 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.99 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 'Superflip (Palatinus & Chapuis, 2006)' _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 225 _diffrn_reflns_number 27006 _reflns_number_total 9955 _diffrn_reflns_av_R_equivalents 0.123 # Number of reflections with Friedels Law is 9955 # Number of reflections without Friedels Law is 9955 # Theoretical number of reflections is about 7223 _diffrn_reflns_theta_min 5.008 _diffrn_reflns_theta_max 26.933 _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.048 _diffrn_measured_fraction_theta_full 0.953 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -19 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 3.11 _oxford_diffrn_Wilson_scale 25.11 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.60 _refine_diff_density_max 0.54 # 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>-3.0\s(I) _refine_ls_number_reflns 6983 _refine_ls_number_restraints 44 _refine_ls_number_parameters 583 _oxford_refine_ls_R_factor_ref 0.1732 _refine_ls_wR_factor_ref 0.3397 _refine_ls_goodness_of_fit_ref 0.9985 _refine_ls_shift/su_max 0.001714 # The values computed from all data _oxford_reflns_number_all 6986 _refine_ls_R_factor_all 0.1733 _refine_ls_wR_factor_all 0.3405 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3893 _refine_ls_R_factor_gt 0.1100 _refine_ls_wR_factor_gt 0.2867 # 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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.18P)^2^ + 4.19P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Palatinus, L. & Chapuis, G. (2006). Superflip - a computer program for solution of crystal structures by charge flipping in arbitrary dimensions. EPFL Lausanne, http://superspace.epfl.ch/superflip 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Na1 Na 0.9025(3) 0.18852(17) 0.09218(16) 0.0703 1.0000 Uani . U . . . . . O2 O 0.6814(5) 0.2224(3) 0.0192(2) 0.0561 1.0000 Uani . . . . . . . C3 C 0.6210(7) 0.2133(4) -0.0451(4) 0.0541 1.0000 Uani . . . . . . . C4 C 0.6096(7) 0.2775(4) -0.1149(4) 0.0506 1.0000 Uani . . . . . . . C5 C 0.6649(7) 0.3602(4) -0.1228(4) 0.0507 1.0000 Uani . . . . . . . C6 C 0.6218(7) 0.4006(4) -0.0685(4) 0.0519 1.0000 Uani . . . . . . . O7 O 0.5327(4) 0.3679(3) -0.0079(2) 0.0549 1.0000 Uani . . . . . . . B8 B 0.5914(8) 0.2873(5) 0.0520(5) 0.0558 1.0000 Uani . . . . . . . O9 O 0.7066(4) 0.2941(3) 0.1049(2) 0.0565 1.0000 Uani . . . . . . . C10 C 0.6595(7) 0.3258(4) 0.1649(4) 0.0577 1.0000 Uani . . . . . . . C11 C 0.5790(7) 0.2833(4) 0.2242(4) 0.0528 1.0000 Uani . . . . . . . C12 C 0.5265(7) 0.3208(4) 0.2833(4) 0.0503 1.0000 Uani . . . . . . . C13 C 0.5764(8) 0.3973(4) 0.2841(4) 0.0595 1.0000 Uani . . . . . . . C14 C 0.6722(8) 0.4360(4) 0.2242(4) 0.0605 1.0000 Uani . . . . . . . C15 C 0.7087(7) 0.4027(4) 0.1660(4) 0.0616 1.0000 Uani . . . . . . . C16 C 0.5250(8) 0.4347(4) 0.3429(4) 0.0639 1.0000 Uani . . . . . . . C17 C 0.4213(8) 0.4036(4) 0.3958(4) 0.0606 1.0000 Uani . . . . . . . C18 C 0.3678(8) 0.3313(4) 0.3916(4) 0.0648 1.0000 Uani . . . . . . . C19 C 0.4211(8) 0.2902(4) 0.3381(4) 0.0609 1.0000 Uani . . . . . . . C20 C 0.3624(11) 0.4477(5) 0.4538(5) 0.0904 1.0000 Uani . . . . . . . C21 C 0.5409(7) 0.1992(4) 0.2248(4) 0.0559 1.0000 Uani . . . . . . . C22 C 0.4768(7) 0.1928(4) 0.1580(4) 0.0533 1.0000 Uani . . . . . . . O23 O 0.4577(5) 0.2603(3) 0.0916(2) 0.0563 1.0000 Uani . . . . . . . C24 C 0.4237(7) 0.1176(4) 0.1599(4) 0.0575 1.0000 Uani . . . . . . . C25 C 0.4400(7) 0.0482(4) 0.2257(4) 0.0612 1.0000 Uani . . . . . . . C26 C 0.5152(7) 0.0477(4) 0.2910(4) 0.0551 1.0000 Uani . . . . . . . C27 C 0.5696(7) 0.1231(4) 0.2909(4) 0.0526 1.0000 Uani . . . . . . . C28 C 0.6555(7) 0.1184(4) 0.3577(4) 0.0615 1.0000 Uani . . . . . . . C29 C 0.6835(8) 0.0458(5) 0.4197(4) 0.0696 1.0000 Uani . . . . . . . C30 C 0.6237(8) -0.0303(4) 0.4217(4) 0.0655 1.0000 Uani . . . . . . . C31 C 0.5421(8) -0.0268(4) 0.3584(4) 0.0647 1.0000 Uani . . . . . . . C32 C 0.6578(11) -0.1082(5) 0.4935(5) 0.0893 1.0000 Uani . . . . . . . C33 C 0.6561(7) 0.4839(4) -0.0765(4) 0.0566 1.0000 Uani . . . . . . . C34 C 0.7385(7) 0.5215(4) -0.1373(4) 0.0607 1.0000 Uani . . . . . . . C35 C 0.7969(7) 0.4792(4) -0.1906(4) 0.0544 1.0000 Uani . . . . . . . C36 C 0.7602(7) 0.3971(4) -0.1835(4) 0.0546 1.0000 Uani . . . . . . . C37 C 0.8290(7) 0.3541(4) -0.2357(4) 0.0595 1.0000 Uani . . . . . . . C38 C 0.9192(8) 0.3925(5) -0.2932(4) 0.0709 1.0000 Uani . . . . . . . C39 C 0.9521(8) 0.4747(5) -0.3030(4) 0.0705 1.0000 Uani . . . . . . . C40 C 0.8900(8) 0.5152(5) -0.2511(4) 0.0685 1.0000 Uani . . . . . . . C41 C 1.0489(10) 0.5161(6) -0.3685(5) 0.0923 1.0000 Uani . . . . . . . C42 C 0.5324(7) 0.2675(4) -0.1788(4) 0.0533 1.0000 Uani . . . . . . . C43 C 0.4935(7) 0.3353(4) -0.2491(4) 0.0587 1.0000 Uani . . . . . . . C44 C 0.4095(8) 0.3258(4) -0.3063(4) 0.0630 1.0000 Uani . . . . . . . C45 C 0.3622(7) 0.2485(5) -0.3002(4) 0.0607 1.0000 Uani . . . . . . . C46 C 0.2673(9) 0.2415(5) -0.3641(5) 0.0838 1.0000 Uani . . . . . . . C47 C 0.4011(7) 0.1807(4) -0.2331(4) 0.0618 1.0000 Uani . . . . . . . C48 C 0.4826(7) 0.1884(4) -0.1709(4) 0.0516 1.0000 Uani . . . . . . . C49 C 0.5105(7) 0.1212(4) -0.1004(4) 0.0579 1.0000 Uani . . . . . . . C50 C 0.5748(7) 0.1336(4) -0.0385(4) 0.0616 1.0000 Uani . . . . . . . O51 O 0.9539(5) 0.0423(3) 0.1044(3) 0.0829 1.0000 Uani . . . . . . . C52 C 1.1015(8) -0.0054(5) 0.1032(5) 0.0861 1.0000 Uani . . . . . . . C53 C 1.1033(10) -0.0928(6) 0.1536(7) 0.1286 1.0000 Uani . . . . . . . C54 C 0.9566(10) -0.0965(6) 0.1894(6) 0.1028 1.0000 Uani . . . . . . . C55 C 0.8567(9) -0.0173(6) 0.1410(6) 0.0998 1.0000 Uani . . . . . . . O56 O 1.0163(7) 0.1680(4) 0.2108(4) 0.1045 1.0000 Uani . . . . . . . C57 C 1.0296(11) 0.0923(7) 0.2773(6) 0.1021 1.0000 Uani . . . . . . . C58 C 1.0727(12) 0.1208(9) 0.3455(6) 0.1207 1.0000 Uani . . . . . . . C59 C 1.0370(12) 0.2194(8) 0.3167(6) 0.1127 1.0000 Uani . . . . . . . C60 C 1.0664(11) 0.2371(7) 0.2316(6) 0.1045 1.0000 Uani . . . . . . . O610 O 1.0617(15) 0.2619(7) 0.0104(6) 0.0881(16) 0.531(13) Uiso D U P . 1 . . C620 C 1.1219(19) 0.2641(9) -0.0605(8) 0.0890(16) 0.531(13) Uiso D U P . 1 . . C630 C 1.1866(17) 0.3452(9) -0.0957(7) 0.0886(16) 0.531(13) Uiso D U P . 1 . . C640 C 1.1240(17) 0.3986(6) -0.0448(8) 0.0882(16) 0.531(13) Uiso D U P . 1 . . C650 C 1.0996(16) 0.3353(8) 0.0307(6) 0.0875(15) 0.531(13) Uiso D U P . 1 . . O611 O 1.0837(17) 0.2564(8) 0.0219(7) 0.0886(16) 0.469(13) Uiso D U P . 2 . . C621 C 1.1681(18) 0.2370(7) -0.0367(9) 0.0891(16) 0.469(13) Uiso D U P . 2 . . C631 C 1.1704(19) 0.3162(10) -0.1038(7) 0.0890(17) 0.469(13) Uiso D U P . 2 . . C641 C 1.1499(19) 0.3847(7) -0.0654(9) 0.0889(17) 0.469(13) Uiso D U P . 2 . . C651 C 1.0552(17) 0.3528(8) 0.0040(9) 0.0884(16) 0.469(13) Uiso D U P . 2 . . H141 H 0.7075 0.4842 0.2251 0.0778 1.0000 Uiso R . . . . . . H151 H 0.7682 0.4304 0.1266 0.0768 1.0000 Uiso R . . . . . . H161 H 0.5631 0.4823 0.3456 0.0780 1.0000 Uiso R . . . . . . H181 H 0.2944 0.3104 0.4257 0.0800 1.0000 Uiso R . . . . . . H191 H 0.3852 0.2409 0.3384 0.0750 1.0000 Uiso R . . . . . . H202 H 0.2686 0.4300 0.4732 0.1382 1.0000 Uiso R . . . . . . H203 H 0.3462 0.5096 0.4290 0.1381 1.0000 Uiso R . . . . . . H201 H 0.4364 0.4309 0.4959 0.1383 1.0000 Uiso R . . . . . . H241 H 0.3762 0.1169 0.1156 0.0699 1.0000 Uiso R . . . . . . H251 H 0.3991 0.0002 0.2271 0.0750 1.0000 Uiso R . . . . . . H281 H 0.6947 0.1665 0.3582 0.0788 1.0000 Uiso R . . . . . . H291 H 0.7408 0.0442 0.4629 0.0848 1.0000 Uiso R . . . . . . H311 H 0.5039 -0.0758 0.3592 0.0807 1.0000 Uiso R . . . . . . H322 H 0.5958 -0.1493 0.4921 0.1309 1.0000 Uiso R . . . . . . H323 H 0.6352 -0.0910 0.5391 0.1309 1.0000 Uiso R . . . . . . H321 H 0.7631 -0.1346 0.4959 0.1309 1.0000 Uiso R . . . . . . H331 H 0.6206 0.5117 -0.0410 0.0742 1.0000 Uiso R . . . . . . H341 H 0.7564 0.5765 -0.1439 0.0749 1.0000 Uiso R . . . . . . H371 H 0.8133 0.2988 -0.2309 0.0740 1.0000 Uiso R . . . . . . H381 H 0.9595 0.3631 -0.3276 0.0849 1.0000 Uiso R . . . . . . H401 H 0.9104 0.5702 -0.2564 0.0840 1.0000 Uiso R . . . . . . H412 H 1.0540 0.5736 -0.3693 0.1451 1.0000 Uiso R . . . . . . H413 H 1.0062 0.5198 -0.4173 0.1450 1.0000 Uiso R . . . . . . H411 H 1.1492 0.4825 -0.3625 0.1450 1.0000 Uiso R . . . . . . H431 H 0.5255 0.3877 -0.2572 0.0719 1.0000 Uiso R . . . . . . H441 H 0.3822 0.3729 -0.3510 0.0749 1.0000 Uiso R . . . . . . H462 H 0.2342 0.1864 -0.3477 0.1270 1.0000 Uiso R . . . . . . H461 H 0.1807 0.2872 -0.3768 0.1270 1.0000 Uiso R . . . . . . H463 H 0.3280 0.2454 -0.4095 0.1270 1.0000 Uiso R . . . . . . H471 H 0.3736 0.1281 -0.2283 0.0790 1.0000 Uiso R . . . . . . H491 H 0.4852 0.0680 -0.0950 0.0761 1.0000 Uiso R . . . . . . H501 H 0.5896 0.0885 0.0092 0.0701 1.0000 Uiso R . . . . . . H522 H 1.1753 0.0206 0.1197 0.1043 1.0000 Uiso R . . . . . . H521 H 1.1227 -0.0060 0.0508 0.1042 1.0000 Uiso R . . . . . . H532 H 1.1820 -0.1084 0.1933 0.1462 1.0000 Uiso R . . . . . . H531 H 1.1224 -0.1327 0.1245 0.1462 1.0000 Uiso R . . . . . . H542 H 0.9601 -0.0958 0.2423 0.1213 1.0000 Uiso R . . . . . . H541 H 0.9216 -0.1479 0.1886 0.1210 1.0000 Uiso R . . . . . . H552 H 0.7830 0.0061 0.1727 0.1140 1.0000 Uiso R . . . . . . H551 H 0.8044 -0.0306 0.1013 0.1142 1.0000 Uiso R . . . . . . H572 H 0.9341 0.0722 0.2863 0.1281 1.0000 Uiso R . . . . . . H571 H 1.1076 0.0462 0.2702 0.1280 1.0000 Uiso R . . . . . . H582 H 1.0150 0.0981 0.3911 0.1490 1.0000 Uiso R . . . . . . H581 H 1.1790 0.1012 0.3590 0.1492 1.0000 Uiso R . . . . . . H592 H 1.1030 0.2445 0.3413 0.1439 1.0000 Uiso R . . . . . . H591 H 0.9324 0.2404 0.3257 0.1440 1.0000 Uiso R . . . . . . H602 H 1.0111 0.2936 0.2009 0.1290 1.0000 Uiso R . . . . . . H601 H 1.1745 0.2343 0.2234 0.1290 1.0000 Uiso R . . . . . . H6202 H 1.0431 0.2648 -0.0958 0.1071 0.531(13) Uiso R . P . 1 . . H6201 H 1.1978 0.2125 -0.0536 0.1074 0.531(13) Uiso R . P . 1 . . H6302 H 1.1616 0.3723 -0.1511 0.1069 0.531(13) Uiso R . P . 1 . . H6301 H 1.2954 0.3317 -0.0872 0.1071 0.531(13) Uiso R . P . 1 . . H6402 H 1.1854 0.4390 -0.0410 0.1060 0.531(13) Uiso R . P . 1 . . H6401 H 1.0252 0.4301 -0.0674 0.1060 0.531(13) Uiso R . P . 1 . . H6502 H 1.0191 0.3589 0.0589 0.1051 0.531(13) Uiso R . P . 1 . . H6501 H 1.1933 0.3172 0.0612 0.1050 0.531(13) Uiso R . P . 1 . . H6212 H 1.2728 0.2149 -0.0178 0.1071 0.469(13) Uiso R . P . 2 . . H6211 H 1.1284 0.1940 -0.0526 0.1069 0.469(13) Uiso R . P . 2 . . H6312 H 1.2593 0.3148 -0.1351 0.1071 0.469(13) Uiso R . P . 2 . . H6311 H 1.0819 0.3282 -0.1374 0.1070 0.469(13) Uiso R . P . 2 . . H6412 H 1.1070 0.4422 -0.0989 0.1060 0.469(13) Uiso R . P . 2 . . H6411 H 1.2490 0.3848 -0.0464 0.1062 0.469(13) Uiso R . P . 2 . . H6512 H 1.0813 0.3679 0.0485 0.1062 0.469(13) Uiso R . P . 2 . . H6511 H 0.9500 0.3772 -0.0110 0.1059 0.469(13) Uiso R . P . 2 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0610(15) 0.0698(16) 0.0842(18) -0.0331(14) -0.0118(12) -0.0050(12) O2 0.057(3) 0.055(3) 0.057(3) -0.021(2) -0.009(2) -0.007(2) C3 0.044(3) 0.053(4) 0.064(4) -0.020(3) -0.001(3) -0.007(3) C4 0.052(4) 0.050(4) 0.054(4) -0.023(3) 0.001(3) -0.010(3) C5 0.051(3) 0.047(4) 0.059(4) -0.024(3) 0.000(3) -0.010(3) C6 0.045(3) 0.049(4) 0.059(4) -0.014(3) -0.005(3) -0.006(3) O7 0.055(2) 0.051(2) 0.056(3) -0.015(2) 0.001(2) -0.007(2) B8 0.053(4) 0.048(4) 0.068(5) -0.024(4) -0.002(4) -0.005(4) O9 0.052(2) 0.063(3) 0.056(3) -0.019(2) -0.002(2) -0.014(2) C10 0.056(4) 0.060(4) 0.056(4) -0.018(3) -0.001(3) -0.011(3) C11 0.059(4) 0.048(4) 0.055(4) -0.019(3) -0.003(3) -0.015(3) C12 0.053(4) 0.048(4) 0.052(4) -0.015(3) -0.005(3) -0.017(3) C13 0.067(4) 0.056(4) 0.054(4) -0.018(3) -0.005(3) -0.006(3) C14 0.070(4) 0.053(4) 0.064(4) -0.020(3) 0.000(4) -0.021(3) C15 0.062(4) 0.056(4) 0.067(5) -0.014(4) 0.004(3) -0.022(3) C16 0.074(5) 0.049(4) 0.069(5) -0.017(3) -0.013(4) -0.014(3) C17 0.074(4) 0.048(4) 0.062(4) -0.023(3) -0.003(4) -0.005(3) C18 0.073(4) 0.056(4) 0.063(4) -0.013(4) 0.005(4) -0.018(4) C19 0.073(4) 0.049(4) 0.062(4) -0.019(3) -0.001(4) -0.012(3) C20 0.115(7) 0.077(5) 0.086(6) -0.040(5) 0.000(5) -0.012(5) C21 0.055(4) 0.054(4) 0.058(4) -0.015(3) 0.003(3) -0.015(3) C22 0.052(4) 0.057(4) 0.053(4) -0.018(3) -0.005(3) -0.012(3) O23 0.054(3) 0.059(3) 0.056(3) -0.015(2) -0.007(2) -0.012(2) C24 0.059(4) 0.060(4) 0.062(4) -0.027(4) -0.004(3) -0.019(3) C25 0.064(4) 0.053(4) 0.071(5) -0.024(4) 0.000(4) -0.015(3) C26 0.059(4) 0.049(4) 0.062(4) -0.023(3) 0.003(3) -0.012(3) C27 0.055(4) 0.049(4) 0.054(4) -0.019(3) 0.003(3) -0.006(3) C28 0.063(4) 0.055(4) 0.069(5) -0.020(4) -0.006(4) -0.015(3) C29 0.079(5) 0.067(5) 0.062(5) -0.017(4) -0.009(4) -0.017(4) C30 0.076(5) 0.051(4) 0.065(5) -0.015(4) 0.006(4) -0.011(4) C31 0.078(5) 0.054(4) 0.068(5) -0.023(4) 0.005(4) -0.023(4) C32 0.118(7) 0.067(5) 0.076(5) -0.010(4) -0.010(5) -0.021(5) C33 0.057(4) 0.052(4) 0.068(4) -0.028(3) -0.005(3) -0.010(3) C34 0.067(4) 0.043(4) 0.076(5) -0.018(3) -0.005(4) -0.019(3) C35 0.049(4) 0.049(4) 0.064(4) -0.018(3) -0.005(3) -0.006(3) C36 0.056(4) 0.047(4) 0.059(4) -0.014(3) -0.006(3) -0.008(3) C37 0.064(4) 0.053(4) 0.063(4) -0.021(3) 0.003(4) -0.010(3) C38 0.065(4) 0.074(5) 0.077(5) -0.030(4) 0.007(4) -0.011(4) C39 0.067(4) 0.074(5) 0.073(5) -0.022(4) 0.011(4) -0.025(4) C40 0.061(4) 0.064(4) 0.081(5) -0.020(4) -0.002(4) -0.021(4) C41 0.089(6) 0.101(6) 0.095(6) -0.031(5) 0.027(5) -0.040(5) C42 0.051(4) 0.047(4) 0.063(4) -0.021(3) 0.000(3) -0.006(3) C43 0.069(4) 0.048(4) 0.060(4) -0.015(3) -0.007(4) -0.017(3) C44 0.071(4) 0.056(4) 0.061(4) -0.020(3) -0.007(4) -0.006(3) C45 0.064(4) 0.066(5) 0.061(4) -0.032(4) -0.008(3) -0.012(4) C46 0.094(6) 0.077(5) 0.085(5) -0.033(4) -0.018(5) -0.013(4) C47 0.057(4) 0.059(4) 0.080(5) -0.031(4) 0.000(4) -0.021(3) C48 0.048(3) 0.049(4) 0.058(4) -0.016(3) -0.003(3) -0.010(3) C49 0.063(4) 0.056(4) 0.066(4) -0.030(4) 0.004(3) -0.019(3) C50 0.065(4) 0.050(4) 0.063(4) -0.010(3) 0.007(4) -0.009(3) O51 0.065(3) 0.058(3) 0.124(4) -0.024(3) 0.001(3) -0.015(2) C52 0.062(5) 0.066(5) 0.124(7) -0.024(5) 0.000(5) -0.010(4) C53 0.071(6) 0.085(7) 0.195(11) -0.008(7) 0.033(7) 0.001(5) C54 0.086(6) 0.082(6) 0.123(7) -0.008(5) -0.006(6) -0.015(5) C55 0.063(5) 0.091(6) 0.150(8) -0.036(6) 0.008(5) -0.031(5) O56 0.118(5) 0.109(5) 0.093(4) -0.044(4) -0.035(4) -0.010(4) C57 0.093(6) 0.119(8) 0.103(7) -0.049(7) 0.001(6) -0.016(6) C58 0.093(7) 0.181(12) 0.084(6) -0.041(7) -0.026(5) -0.015(7) C59 0.101(7) 0.134(9) 0.119(9) -0.059(7) -0.001(6) -0.027(7) C60 0.091(6) 0.114(7) 0.112(8) -0.044(6) -0.010(6) -0.014(6) _refine_ls_extinction_coef 896.581 _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.3754(14) 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 Na1 . O2 . 2.305(5) yes Na1 . O9 . 2.310(5) yes Na1 . O51 . 2.325(5) yes Na1 . O56 . 2.311(6) yes Na1 . O610 . 2.262(10) yes O2 . C3 . 1.365(7) yes O2 . B8 . 1.495(8) yes C3 . C4 . 1.362(8) yes C3 . C50 . 1.429(9) yes C4 . C5 . 1.509(8) yes C4 . C42 . 1.440(9) yes C5 . C6 . 1.371(8) yes C5 . C36 . 1.427(9) yes C6 . O7 . 1.372(7) yes C6 . C33 . 1.435(8) yes O7 . B8 . 1.447(8) yes B8 . O9 . 1.479(8) yes B8 . O23 . 1.455(8) yes O9 . C10 . 1.379(7) yes C10 . C11 . 1.357(9) yes C10 . C15 . 1.435(9) yes C11 . C12 . 1.432(8) yes C11 . C21 . 1.496(8) yes C12 . C13 . 1.430(9) yes C12 . C19 . 1.397(9) yes C13 . C14 . 1.430(9) yes C13 . C16 . 1.424(9) yes C14 . C15 . 1.347(9) yes C14 . H141 . 0.920 no C15 . H151 . 0.933 no C16 . C17 . 1.369(9) yes C16 . H161 . 0.935 no C17 . C18 . 1.398(9) yes C17 . C20 . 1.499(9) yes C18 . C19 . 1.386(9) yes C18 . H181 . 0.930 no C19 . H191 . 0.932 no C20 . H202 . 0.967 no C20 . H203 . 0.966 no C20 . H201 . 0.966 no C21 . C22 . 1.401(9) yes C21 . C27 . 1.426(8) yes C22 . O23 . 1.347(7) yes C22 . C24 . 1.409(8) yes C24 . C25 . 1.358(9) yes C24 . H241 . 0.927 no C25 . C26 . 1.380(9) yes C25 . H251 . 0.932 no C26 . C27 . 1.426(9) yes C26 . C31 . 1.422(9) yes C27 . C28 . 1.431(9) yes C28 . C29 . 1.350(9) yes C28 . H281 . 0.935 no C29 . C30 . 1.454(10) yes C29 . H291 . 0.943 no C30 . C31 . 1.363(10) yes C30 . C32 . 1.505(10) yes C31 . H311 . 0.936 no C32 . H322 . 0.967 no C32 . H323 . 0.964 no C32 . H321 . 0.965 no C33 . C34 . 1.359(9) yes C33 . H331 . 0.925 no C34 . C35 . 1.405(9) yes C34 . H341 . 0.927 no C35 . C36 . 1.428(9) yes C35 . C40 . 1.408(9) yes C36 . C37 . 1.424(9) yes C37 . C38 . 1.370(9) yes C37 . H371 . 0.932 no C38 . C39 . 1.406(10) yes C38 . H381 . 0.936 no C39 . C40 . 1.375(10) yes C39 . C41 . 1.513(10) yes C40 . H401 . 0.939 no C41 . H412 . 0.959 no C41 . H413 . 0.956 no C41 . H411 . 0.960 no C42 . C43 . 1.408(9) yes C42 . C48 . 1.429(8) yes C43 . C44 . 1.370(9) yes C43 . H431 . 0.933 no C44 . C45 . 1.397(9) yes C44 . H441 . 0.930 no C45 . C46 . 1.509(9) yes C45 . C47 . 1.369(9) yes C46 . H462 . 0.968 no C46 . H461 . 0.958 no C46 . H463 . 0.967 no C47 . C48 . 1.418(9) yes C47 . H471 . 0.929 no C48 . C49 . 1.396(9) yes C49 . C50 . 1.369(9) yes C49 . H491 . 0.927 no C50 . H501 . 0.940 no O51 . C52 . 1.420(8) yes O51 . C55 . 1.435(9) yes C52 . C53 . 1.444(11) yes C52 . H522 . 0.960 no C52 . H521 . 0.969 no C53 . C54 . 1.461(11) yes C53 . H532 . 0.966 no C53 . H531 . 0.962 no C54 . C55 . 1.477(11) yes C54 . H542 . 0.966 no C54 . H541 . 0.968 no C55 . H552 . 0.975 no C55 . H551 . 0.976 no O56 . C57 . 1.426(11) yes O56 . C60 . 1.465(11) yes C57 . C58 . 1.544(12) yes C57 . H572 . 0.972 no C57 . H571 . 0.978 no C58 . C59 . 1.524(14) yes C58 . H582 . 0.973 no C58 . H581 . 0.966 no C59 . C60 . 1.504(12) yes C59 . H592 . 0.976 no C59 . H591 . 0.972 no C60 . H602 . 0.974 no C60 . H601 . 0.977 no O610 . C620 . 1.375(7) yes O610 . C650 . 1.479(7) yes C620 . C630 . 1.510(7) yes C620 . H6202 . 0.968 no C620 . H6201 . 0.968 no C630 . C640 . 1.507(7) yes C630 . H6302 . 0.974 no C630 . H6301 . 0.971 no C640 . C650 . 1.477(7) yes C640 . H6402 . 0.965 no C640 . H6401 . 0.973 no C650 . H6502 . 0.972 no C650 . H6501 . 0.969 no O611 . C621 . 1.378(7) yes O611 . C651 . 1.503(7) yes C621 . C631 . 1.483(8) yes C621 . H6212 . 0.976 no C621 . H6211 . 0.976 no C631 . C641 . 1.496(7) yes C631 . H6312 . 0.971 no C631 . H6311 . 0.970 no C641 . C651 . 1.508(8) yes C641 . H6412 . 0.969 no C641 . H6411 . 0.969 no C651 . H6512 . 0.968 no C651 . H6511 . 0.970 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 O2 . Na1 . O9 . 59.24(15) yes O2 . Na1 . O51 . 96.43(19) yes O9 . Na1 . O51 . 140.5(2) yes O2 . Na1 . O56 . 147.5(2) yes O9 . Na1 . O56 . 94.1(2) yes O51 . Na1 . O56 . 94.0(2) yes O2 . Na1 . O610 . 104.1(4) yes O9 . Na1 . O610 . 104.8(4) yes O51 . Na1 . O610 . 111.6(4) yes O56 . Na1 . O610 . 100.5(4) yes Na1 . O2 . C3 . 142.3(4) yes Na1 . O2 . B8 . 100.0(4) yes C3 . O2 . B8 . 116.7(5) yes O2 . C3 . C4 . 121.0(6) yes O2 . C3 . C50 . 118.7(6) yes C4 . C3 . C50 . 120.3(6) yes C3 . C4 . C5 . 120.4(6) yes C3 . C4 . C42 . 118.3(6) yes C5 . C4 . C42 . 121.0(6) yes C4 . C5 . C6 . 117.9(5) yes C4 . C5 . C36 . 122.9(5) yes C6 . C5 . C36 . 119.2(6) yes C5 . C6 . O7 . 122.2(5) yes C5 . C6 . C33 . 121.3(6) yes O7 . C6 . C33 . 116.2(6) yes C6 . O7 . B8 . 119.5(5) yes O2 . B8 . O7 . 112.1(6) yes O2 . B8 . O9 . 100.2(5) yes O7 . B8 . O9 . 114.1(5) yes O2 . B8 . O23 . 113.7(5) yes O7 . B8 . O23 . 104.0(5) yes O9 . B8 . O23 . 113.2(6) yes Na1 . O9 . B8 . 100.3(4) yes Na1 . O9 . C10 . 133.9(4) yes B8 . O9 . C10 . 118.7(5) yes O9 . C10 . C11 . 122.1(6) yes O9 . C10 . C15 . 117.5(6) yes C11 . C10 . C15 . 120.2(6) yes C10 . C11 . C12 . 120.1(6) yes C10 . C11 . C21 . 118.9(6) yes C12 . C11 . C21 . 120.9(5) yes C11 . C12 . C13 . 118.9(6) yes C11 . C12 . C19 . 123.9(6) yes C13 . C12 . C19 . 117.1(6) yes C12 . C13 . C14 . 119.0(6) yes C12 . C13 . C16 . 119.1(6) yes C14 . C13 . C16 . 121.8(6) yes C13 . C14 . C15 . 120.2(6) yes C13 . C14 . H141 . 119.7 no C15 . C14 . H141 . 120.1 no C10 . C15 . C14 . 121.1(6) yes C10 . C15 . H151 . 120.4 no C14 . C15 . H151 . 118.5 no C13 . C16 . C17 . 122.5(6) yes C13 . C16 . H161 . 119.1 no C17 . C16 . H161 . 118.4 no C16 . C17 . C18 . 117.5(6) yes C16 . C17 . C20 . 121.2(7) yes C18 . C17 . C20 . 121.2(7) yes C17 . C18 . C19 . 121.7(6) yes C17 . C18 . H181 . 119.0 no C19 . C18 . H181 . 119.3 no C12 . C19 . C18 . 121.8(6) yes C12 . C19 . H191 . 119.0 no C18 . C19 . H191 . 119.2 no C17 . C20 . H202 . 109.0 no C17 . C20 . H203 . 109.4 no H202 . C20 . H203 . 110.2 no C17 . C20 . H201 . 108.5 no H202 . C20 . H201 . 110.2 no H203 . C20 . H201 . 109.6 no C11 . C21 . C22 . 120.0(6) yes C11 . C21 . C27 . 122.6(6) yes C22 . C21 . C27 . 117.4(6) yes C21 . C22 . O23 . 120.5(5) yes C21 . C22 . C24 . 120.9(6) yes O23 . C22 . C24 . 118.5(6) yes C22 . O23 . B8 . 118.3(5) yes C22 . C24 . C25 . 120.5(6) yes C22 . C24 . H241 . 118.7 no C25 . C24 . H241 . 120.9 no C24 . C25 . C26 . 121.1(6) yes C24 . C25 . H251 . 119.5 no C26 . C25 . H251 . 119.4 no C25 . C26 . C27 . 119.6(6) yes C25 . C26 . C31 . 121.6(6) yes C27 . C26 . C31 . 118.8(6) yes C26 . C27 . C21 . 119.9(6) yes C26 . C27 . C28 . 118.0(6) yes C21 . C27 . C28 . 122.1(6) yes C27 . C28 . C29 . 121.8(6) yes C27 . C28 . H281 . 119.4 no C29 . C28 . H281 . 118.9 no C28 . C29 . C30 . 120.7(7) yes C28 . C29 . H291 . 120.2 no C30 . C29 . H291 . 119.1 no C29 . C30 . C31 . 118.1(6) yes C29 . C30 . C32 . 117.4(7) yes C31 . C30 . C32 . 124.5(7) yes C26 . C31 . C30 . 122.5(6) yes C26 . C31 . H311 . 119.0 no C30 . C31 . H311 . 118.5 no C30 . C32 . H322 . 109.1 no C30 . C32 . H323 . 109.8 no H322 . C32 . H323 . 109.0 no C30 . C32 . H321 . 110.1 no H322 . C32 . H321 . 109.7 no H323 . C32 . H321 . 109.2 no C6 . C33 . C34 . 119.0(6) yes C6 . C33 . H331 . 120.0 no C34 . C33 . H331 . 120.9 no C33 . C34 . C35 . 121.7(6) yes C33 . C34 . H341 . 119.0 no C35 . C34 . H341 . 119.2 no C34 . C35 . C36 . 119.1(6) yes C34 . C35 . C40 . 122.2(6) yes C36 . C35 . C40 . 118.7(6) yes C35 . C36 . C5 . 119.2(6) yes C35 . C36 . C37 . 117.2(6) yes C5 . C36 . C37 . 123.5(6) yes C36 . C37 . C38 . 121.2(6) yes C36 . C37 . H371 . 120.0 no C38 . C37 . H371 . 118.8 no C37 . C38 . C39 . 122.4(7) yes C37 . C38 . H381 . 118.8 no C39 . C38 . H381 . 118.9 no C38 . C39 . C40 . 116.7(6) yes C38 . C39 . C41 . 120.9(7) yes C40 . C39 . C41 . 122.4(7) yes C35 . C40 . C39 . 123.7(7) yes C35 . C40 . H401 . 118.0 no C39 . C40 . H401 . 118.2 no C39 . C41 . H412 . 110.3 no C39 . C41 . H413 . 110.0 no H412 . C41 . H413 . 108.2 no C39 . C41 . H411 . 110.5 no H412 . C41 . H411 . 109.1 no H413 . C41 . H411 . 108.6 no C4 . C42 . C43 . 122.6(6) yes C4 . C42 . C48 . 120.5(6) yes C43 . C42 . C48 . 116.8(6) yes C42 . C43 . C44 . 121.1(6) yes C42 . C43 . H431 . 119.8 no C44 . C43 . H431 . 119.1 no C43 . C44 . C45 . 122.8(6) yes C43 . C44 . H441 . 118.6 no C45 . C44 . H441 . 118.6 no C44 . C45 . C46 . 120.9(7) yes C44 . C45 . C47 . 117.4(6) yes C46 . C45 . C47 . 121.6(6) yes C45 . C46 . H462 . 110.0 no C45 . C46 . H461 . 110.4 no H462 . C46 . H461 . 109.2 no C45 . C46 . H463 . 108.6 no H462 . C46 . H463 . 109.0 no H461 . C46 . H463 . 109.5 no C45 . C47 . C48 . 121.9(6) yes C45 . C47 . H471 . 119.0 no C48 . C47 . H471 . 119.1 no C42 . C48 . C47 . 119.9(6) yes C42 . C48 . C49 . 118.9(6) yes C47 . C48 . C49 . 121.2(6) yes C48 . C49 . C50 . 120.0(6) yes C48 . C49 . H491 . 120.3 no C50 . C49 . H491 . 119.6 no C3 . C50 . C49 . 121.5(6) yes C3 . C50 . H501 . 119.4 no C49 . C50 . H501 . 119.1 no Na1 . O51 . C52 . 123.8(4) yes Na1 . O51 . C55 . 124.1(5) yes C52 . O51 . C55 . 108.6(6) yes O51 . C52 . C53 . 107.2(6) yes O51 . C52 . H522 . 110.5 no C53 . C52 . H522 . 111.8 no O51 . C52 . H521 . 109.4 no C53 . C52 . H521 . 109.2 no H522 . C52 . H521 . 108.7 no C52 . C53 . C54 . 108.3(7) yes C52 . C53 . H532 . 109.4 no C54 . C53 . H532 . 110.0 no C52 . C53 . H531 . 110.6 no C54 . C53 . H531 . 109.7 no H532 . C53 . H531 . 108.8 no C53 . C54 . C55 . 104.4(7) yes C53 . C54 . H542 . 111.9 no C55 . C54 . H542 . 109.5 no C53 . C54 . H541 . 110.3 no C55 . C54 . H541 . 111.2 no H542 . C54 . H541 . 109.6 no C54 . C55 . O51 . 105.9(6) yes C54 . C55 . H552 . 110.9 no O51 . C55 . H552 . 111.4 no C54 . C55 . H551 . 109.5 no O51 . C55 . H551 . 109.4 no H552 . C55 . H551 . 109.7 no Na1 . O56 . C57 . 126.3(5) yes Na1 . O56 . C60 . 123.5(6) yes C57 . O56 . C60 . 109.6(7) yes O56 . C57 . C58 . 105.0(8) yes O56 . C57 . H572 . 110.4 no C58 . C57 . H572 . 110.5 no O56 . C57 . H571 . 110.6 no C58 . C57 . H571 . 111.0 no H572 . C57 . H571 . 109.2 no C57 . C58 . C59 . 105.9(8) yes C57 . C58 . H582 . 111.0 no C59 . C58 . H582 . 110.6 no C57 . C58 . H581 . 110.7 no C59 . C58 . H581 . 109.6 no H582 . C58 . H581 . 109.0 no C58 . C59 . C60 . 100.5(8) yes C58 . C59 . H592 . 112.3 no C60 . C59 . H592 . 111.8 no C58 . C59 . H591 . 110.7 no C60 . C59 . H591 . 112.0 no H592 . C59 . H591 . 109.4 no C59 . C60 . O56 . 105.7(8) yes C59 . C60 . H602 . 111.0 no O56 . C60 . H602 . 111.0 no C59 . C60 . H601 . 109.4 no O56 . C60 . H601 . 109.9 no H602 . C60 . H601 . 109.8 no Na1 . O610 . C620 . 136.9(6) yes Na1 . O610 . C650 . 114.7(6) yes C620 . O610 . C650 . 107.90(10) yes O610 . C620 . C630 . 110.72(10) yes O610 . C620 . H6202 . 109.4 no C630 . C620 . H6202 . 107.6 no O610 . C620 . H6201 . 108.9 no C630 . C620 . H6201 . 111.6 no H6202 . C620 . H6201 . 108.7 no C620 . C630 . C640 . 101.96(10) yes C620 . C630 . H6302 . 112.8 no C640 . C630 . H6302 . 115.4 no C620 . C630 . H6301 . 109.5 no C640 . C630 . H6301 . 106.8 no H6302 . C630 . H6301 . 110.0 no C630 . C640 . C650 . 105.20(10) yes C630 . C640 . H6402 . 114.3 no C650 . C640 . H6402 . 113.8 no C630 . C640 . H6401 . 106.1 no C650 . C640 . H6401 . 107.4 no H6402 . C640 . H6401 . 109.5 no O610 . C650 . C640 . 104.44(10) yes O610 . C650 . H6502 . 111.4 no C640 . C650 . H6502 . 112.2 no O610 . C650 . H6501 . 110.3 no C640 . C650 . H6501 . 108.3 no H6502 . C650 . H6501 . 110.1 no Na1 . O611 . C621 . 128.8(9) yes Na1 . O611 . C651 . 115.1(8) yes C621 . O611 . C651 . 107.89(10) yes O611 . C621 . C631 . 110.73(10) yes O611 . C621 . H6212 . 108.7 no C631 . C621 . H6212 . 105.9 no O611 . C621 . H6211 . 110.1 no C631 . C621 . H6211 . 110.8 no H6212 . C621 . H6211 . 110.4 no C621 . C631 . C641 . 101.90(10) yes C621 . C631 . H6312 . 115.3 no C641 . C631 . H6312 . 114.2 no C621 . C631 . H6311 . 109.8 no C641 . C631 . H6311 . 106.7 no H6312 . C631 . H6311 . 108.4 no C631 . C641 . C651 . 105.22(10) yes C631 . C641 . H6412 . 114.8 no C651 . C641 . H6412 . 112.7 no C631 . C641 . H6411 . 106.4 no C651 . C641 . H6411 . 108.0 no H6412 . C641 . H6411 . 109.3 no C641 . C651 . O611 . 104.45(10) yes C641 . C651 . H6512 . 113.3 no O611 . C651 . H6512 . 110.8 no C641 . C651 . H6511 . 108.5 no O611 . C651 . H6511 . 110.4 no H6512 . C651 . H6511 . 109.2 no 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 C33 . H331 . O7 2_665 157 0.92 2.60 3.466(12) yes C43 . H431 . C36 . 122 0.93 2.59 3.182(12) yes C650 . H6501 . O23 1_655 158 0.97 2.41 3.323(12) yes _chemical_name_common . #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 796354' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 07-12-19 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5661 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 14.1036(2) _cell_length_b 22.2147(3) _cell_length_c 16.2473(2) _cell_angle_alpha 90 _cell_angle_beta 104.8169(7) _cell_angle_gamma 90 _cell_volume 4921.13(12) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' 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 = C56 H20 B1 I4 Na1 O8 # Dc = 1.84 Fooo = 2600.00 Mu = 25.98 M = 1362.19 # Found Formula = C52 H46 B1 I4 Na1 O8 # Dc = 1.81 FOOO = 2600.00 Mu = 25.95 M = 1340.35 _chemical_formula_sum 'C52 H46 B1 I4 Na1 O8' _chemical_formula_moiety 'C52 H46 B1 I4 Na1 O8' _chemical_compound_source . _chemical_formula_weight 1340.35 _cell_measurement_reflns_used 11273 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 2.595 # Sheldrick geometric approximatio 0.79 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.86 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 150 _diffrn_reflns_number 70896 _reflns_number_total 11210 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 11210 # Number of reflections without Friedels Law is 21974 # Theoretical number of reflections is about 11319 _diffrn_reflns_theta_min 5.105 _diffrn_reflns_theta_max 27.512 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.687 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _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 -1.77 _refine_diff_density_max 1.46 # 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>-3.0\s(I) _refine_ls_number_reflns 11210 _refine_ls_number_restraints 20 _refine_ls_number_parameters 585 _oxford_refine_ls_R_factor_ref 0.0668 _refine_ls_wR_factor_ref 0.0779 _refine_ls_goodness_of_fit_ref 0.9401 _refine_ls_shift/su_max 0.002780 # The values computed from all data _oxford_reflns_number_all 11210 _refine_ls_R_factor_all 0.0668 _refine_ls_wR_factor_all 0.0779 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7781 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0709 # 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 noref # 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^) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.249073(19) 0.345725(12) 0.863777(15) 0.0293 1.0000 Uani . . . . . . . C2 C 0.3124(3) 0.30888(16) 0.9839(2) 0.0214 1.0000 Uani . . . . . . . C3 C 0.3974(3) 0.33113(16) 1.0337(2) 0.0217 1.0000 Uani . . . . . . . C4 C 0.4430(3) 0.30415(17) 1.1131(2) 0.0229 1.0000 Uani . . . . . . . C5 C 0.4036(3) 0.24964(16) 1.1353(2) 0.0217 1.0000 Uani . . . . . . . C6 C 0.4519(3) 0.22318(17) 1.2155(2) 0.0256 1.0000 Uani . . . . . . . C7 C 0.5332(3) 0.24908(19) 1.2677(2) 0.0305 1.0000 Uani . . . . . . . C8 C 0.5716(3) 0.3029(2) 1.2432(2) 0.0337 1.0000 Uani . . . . . . . C9 C 0.5270(3) 0.32965(18) 1.1678(2) 0.0267 1.0000 Uani . . . . . . . C10 C 0.3160(3) 0.22537(16) 1.0812(2) 0.0204 1.0000 Uani . . . . . . . C11 C 0.2654(3) 0.25792(16) 1.0113(2) 0.0212 1.0000 Uani . . . . . . . O12 O 0.17584(17) 0.24175(11) 0.96561(14) 0.0209 1.0000 Uani . . . . . . . B13 B 0.0947(3) 0.23804(19) 1.0060(2) 0.0207 1.0000 Uani . . . . . . . O14 O 0.02176(17) 0.20550(10) 0.94030(14) 0.0199 1.0000 Uani . . . . . . . C15 C -0.0727(3) 0.20139(16) 0.9459(2) 0.0205 1.0000 Uani . . . . . . . C16 C -0.1290(3) 0.25221(16) 0.9440(2) 0.0201 1.0000 Uani . . . . . . . C17 C -0.2230(3) 0.24606(16) 0.9622(2) 0.0206 1.0000 Uani . . . . . . . C18 C -0.2791(3) 0.29663(18) 0.9760(2) 0.0260 1.0000 Uani . . . . . . . C19 C -0.3659(3) 0.28958(19) 0.9969(2) 0.0320 1.0000 Uani . . . . . . . C20 C -0.4049(3) 0.2314(2) 1.0020(3) 0.0383 1.0000 Uani . . . . . . . C21 C -0.3539(3) 0.18192(19) 0.9884(3) 0.0332 1.0000 Uani . . . . . . . C22 C -0.2610(3) 0.18769(17) 0.9704(2) 0.0250 1.0000 Uani . . . . . . . C23 C -0.2053(3) 0.13680(17) 0.9594(2) 0.0286 1.0000 Uani . . . . . . . C24 C -0.1135(3) 0.14341(17) 0.9488(2) 0.0246 1.0000 Uani . . . . . . . I25 I -0.03281(2) 0.068500(11) 0.929017(17) 0.0313 1.0000 Uani . . . . . . . C26 C -0.0925(3) 0.31130(15) 0.9235(2) 0.0188 1.0000 Uani . . . . . . . C27 C -0.0012(3) 0.33195(15) 0.9688(2) 0.0189 1.0000 Uani . . . . . . . O28 O 0.05851(17) 0.29690(10) 1.02822(14) 0.0195 1.0000 Uani . . . . . . . Na29 Na 0.05130(13) 0.29030(8) 1.16827(9) 0.0398 1.0000 Uani . . . . . . . O30 O 0.0136(2) 0.24452(13) 1.27812(16) 0.0416 1.0000 Uani . . . . . . . O31 O -0.0877(2) 0.35362(13) 1.15110(19) 0.0438 1.0000 Uani . . . . . . . C32 C -0.1625(3) 0.3432(2) 1.1950(3) 0.0387 1.0000 Uani . . . . . . . C33 C -0.2214(4) 0.4004(2) 1.1866(3) 0.0504 1.0000 Uani . . . . . . . C34 C -0.1568(4) 0.4470(2) 1.1629(3) 0.0579 1.0000 Uani . . . . . . . C35 C -0.0944(4) 0.4139(2) 1.1210(4) 0.0611 1.0000 Uani . . . . . . . C41 C 0.0271(3) 0.39168(16) 0.9571(2) 0.0212 1.0000 Uani . . . . . . . I42 I 0.152494(19) 0.427535(11) 1.042074(16) 0.0298 1.0000 Uani . . . . . . . C43 C -0.0278(3) 0.42781(16) 0.8959(2) 0.0259 1.0000 Uani . . . . . . . C44 C -0.1158(3) 0.40555(17) 0.8407(2) 0.0227 1.0000 Uani . . . . . . . C45 C -0.1485(3) 0.34690(16) 0.8539(2) 0.0205 1.0000 Uani . . . . . . . C46 C -0.2337(3) 0.32479(17) 0.7947(2) 0.0280 1.0000 Uani . . . . . . . C47 C -0.2827(3) 0.3591(2) 0.7272(2) 0.0367 1.0000 Uani . . . . . . . C48 C -0.2507(3) 0.4175(2) 0.7165(3) 0.0405 1.0000 Uani . . . . . . . C49 C -0.1699(3) 0.44013(18) 0.7702(3) 0.0353 1.0000 Uani . . . . . . . O50 O 0.11942(18) 0.20910(11) 1.09094(14) 0.0219 1.0000 Uani . . . . . . . C51 C 0.1812(3) 0.16156(16) 1.1082(2) 0.0206 1.0000 Uani . . . . . . . C52 C 0.2770(3) 0.16591(16) 1.1000(2) 0.0215 1.0000 Uani . . . . . . . C53 C 0.3362(3) 0.11294(17) 1.1080(2) 0.0233 1.0000 Uani . . . . . . . C54 C 0.4262(3) 0.11082(18) 1.0848(2) 0.0285 1.0000 Uani . . . . . . . C55 C 0.4784(3) 0.05831(19) 1.0888(3) 0.0331 1.0000 Uani . . . . . . . C56 C 0.4451(3) 0.00508(18) 1.1191(3) 0.0363 1.0000 Uani . . . . . . . C57 C 0.3603(3) 0.00559(18) 1.1431(3) 0.0344 1.0000 Uani . . . . . . . C58 C 0.3015(3) 0.05847(16) 1.1370(2) 0.0240 1.0000 Uani . . . . . . . C59 C 0.2105(3) 0.05877(17) 1.1574(2) 0.0261 1.0000 Uani . . . . . . . C60 C 0.1517(3) 0.10787(17) 1.1420(2) 0.0211 1.0000 Uani . . . . . . . I61 I 0.015650(18) 0.104106(12) 1.172119(15) 0.0279 1.0000 Uani . . . . . . . O62 O 0.5108(3) 1.02769(15) 0.6187(3) 0.0708 1.0000 Uani . . . . . . . C63 C 0.5590(4) 0.9706(2) 0.6222(3) 0.0591 1.0000 Uani . . . . . . . C64 C 0.4924(5) 0.9247(2) 0.6431(4) 0.0671 1.0000 Uani . . . . . . . C65 C 0.3926(5) 0.9530(3) 0.6108(4) 0.0836 1.0000 Uani . . . . . . . C66 C 0.4158(4) 1.0176(3) 0.6308(4) 0.0759 1.0000 Uani . . . . . . . O360 O 0.1808(5) 0.3380(4) 1.2554(5) 0.0418(11) 0.5000 Uiso D . . . 2 . . C370 C 0.2865(7) 0.3294(5) 1.2673(6) 0.0511(17) 0.5000 Uiso D . . . 2 . . C380 C 0.3352(6) 0.3536(5) 1.3513(6) 0.069(2) 0.5000 Uiso D . . . 2 . . C390 C 0.2683(8) 0.4043(5) 1.3630(7) 0.067(2) 0.5000 Uiso D . . . 2 . . C400 C 0.1649(6) 0.3807(5) 1.3185(7) 0.0456(15) 0.5000 Uiso D . . . 2 . . O361 O 0.1776(5) 0.3511(4) 1.2468(5) 0.0418(11) 0.5000 Uiso D . . . 1 . . C371 C 0.2700(8) 0.3263(5) 1.2462(6) 0.0511(17) 0.5000 Uiso D . . . 1 . . C381 C 0.3451(6) 0.3531(5) 1.3222(6) 0.069(2) 0.5000 Uiso D . . . 1 . . C391 C 0.2920(8) 0.4056(4) 1.3472(6) 0.067(2) 0.5000 Uiso D . . . 1 . . C401 C 0.1878(6) 0.3860(5) 1.3238(6) 0.0456(15) 0.5000 Uiso D . . . 1 . . H31 H 0.4256 0.3642 1.0170 0.0270 1.0000 Uiso . . . . . . . H61 H 0.4269 0.1879 1.2312 0.0298 1.0000 Uiso . . . . . . . H71 H 0.5636 0.2311 1.3207 0.0349 1.0000 Uiso . . . . . . . H81 H 0.6280 0.3207 1.2781 0.0384 1.0000 Uiso . . . . . . . H91 H 0.5509 0.3659 1.1514 0.0318 1.0000 Uiso . . . . . . . H181 H -0.2551 0.3359 0.9716 0.0308 1.0000 Uiso . . . . . . . H191 H -0.4006 0.3241 1.0083 0.0389 1.0000 Uiso . . . . . . . H201 H -0.4636 0.2274 1.0155 0.0483 1.0000 Uiso . . . . . . . H211 H -0.3812 0.1442 0.9916 0.0395 1.0000 Uiso . . . . . . . H231 H -0.2299 0.0976 0.9602 0.0341 1.0000 Uiso . . . . . . . H322 H -0.1316 0.3346 1.2536 0.0477 1.0000 Uiso . . . . . . . H321 H -0.2031 0.3096 1.1688 0.0475 1.0000 Uiso . . . . . . . H332 H -0.2378 0.4094 1.2404 0.0623 1.0000 Uiso . . . . . . . H331 H -0.2797 0.3977 1.1403 0.0628 1.0000 Uiso . . . . . . . H341 H -0.1125 0.4608 1.2160 0.0748 1.0000 Uiso . . . . . . . H342 H -0.1933 0.4804 1.1300 0.0741 1.0000 Uiso . . . . . . . H351 H -0.0301 0.4317 1.1296 0.0789 1.0000 Uiso . . . . . . . H352 H -0.1281 0.4144 1.0594 0.0794 1.0000 Uiso . . . . . . . H431 H -0.0078 0.4670 0.8908 0.0325 1.0000 Uiso . . . . . . . H461 H -0.2579 0.2867 0.8015 0.0337 1.0000 Uiso . . . . . . . H471 H -0.3389 0.3431 0.6868 0.0417 1.0000 Uiso . . . . . . . H481 H -0.2851 0.4405 0.6736 0.0467 1.0000 Uiso . . . . . . . H491 H -0.1481 0.4787 0.7639 0.0432 1.0000 Uiso . . . . . . . H541 H 0.4506 0.1459 1.0655 0.0333 1.0000 Uiso . . . . . . . H551 H 0.5386 0.0577 1.0729 0.0391 1.0000 Uiso . . . . . . . H561 H 0.4808 -0.0300 1.1237 0.0427 1.0000 Uiso . . . . . . . H571 H 0.3389 -0.0300 1.1648 0.0404 1.0000 Uiso . . . . . . . H591 H 0.1908 0.0240 1.1797 0.0297 1.0000 Uiso . . . . . . . H632 H 0.6238 0.9705 0.6654 0.0697 1.0000 Uiso . . . . . . . H631 H 0.5688 0.9613 0.5665 0.0695 1.0000 Uiso . . . . . . . H641 H 0.5061 0.9203 0.7048 0.0812 1.0000 Uiso . . . . . . . H642 H 0.4977 0.8859 0.6163 0.0813 1.0000 Uiso . . . . . . . H652 H 0.3436 0.9371 0.6374 0.0993 1.0000 Uiso . . . . . . . H651 H 0.3724 0.9496 0.5476 0.0996 1.0000 Uiso . . . . . . . H662 H 0.4147 1.0246 0.6893 0.0936 1.0000 Uiso . . . . . . . H661 H 0.3682 1.0436 0.5925 0.0939 1.0000 Uiso . . . . . . . H3701 H 0.2994 0.2864 1.2632 0.0620 0.5000 Uiso . . . . 2 . . H3702 H 0.3068 0.3517 1.2240 0.0620 0.5000 Uiso . . . . 2 . . H3801 H 0.3366 0.3232 1.3965 0.0828 0.5000 Uiso . . . . 2 . . H3802 H 0.4009 0.3673 1.3539 0.0830 0.5000 Uiso . . . . 2 . . H3901 H 0.2742 0.4135 1.4214 0.0812 0.5000 Uiso . . . . 2 . . H3902 H 0.2819 0.4413 1.3344 0.0813 0.5000 Uiso . . . . 2 . . H4002 H 0.1330 0.3607 1.3592 0.0553 0.5000 Uiso . . . . 2 . . H4001 H 0.1227 0.4133 1.2914 0.0547 0.5000 Uiso . . . . 2 . . H3712 H 0.2679 0.2830 1.2498 0.0619 0.5000 Uiso . . . . 1 . . H3711 H 0.2858 0.3375 1.1930 0.0619 0.5000 Uiso . . . . 1 . . H3812 H 0.3625 0.3242 1.3692 0.0833 0.5000 Uiso . . . . 1 . . H3811 H 0.4038 0.3657 1.3060 0.0831 0.5000 Uiso . . . . 1 . . H3911 H 0.3147 0.4157 1.4070 0.0811 0.5000 Uiso . . . . 1 . . H3912 H 0.3007 0.4407 1.3129 0.0812 0.5000 Uiso . . . . 1 . . H4012 H 0.1763 0.3611 1.3702 0.0554 0.5000 Uiso . . . . 1 . . H4011 H 0.1423 0.4204 1.3137 0.0549 0.5000 Uiso . . . . 1 . . H301 H 0.0224 0.2622 1.3231 0.0635 1.0000 Uiso . . . . . . . H302 H 0.0417 0.2104 1.2841 0.0637 1.0000 Uiso . . . . . . . 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 I1 0.02880(15) 0.03363(16) 0.02452(13) 0.00848(11) 0.00510(11) -0.00259(12) C2 0.024(2) 0.022(2) 0.0196(17) 0.0015(15) 0.0083(15) 0.0017(16) C3 0.0211(19) 0.021(2) 0.0246(18) 0.0036(16) 0.0087(16) -0.0023(16) C4 0.021(2) 0.025(2) 0.0242(18) 0.0014(16) 0.0091(16) 0.0012(17) C5 0.0184(19) 0.024(2) 0.0237(18) -0.0001(16) 0.0066(15) 0.0032(16) C6 0.026(2) 0.027(2) 0.0234(19) 0.0050(16) 0.0044(17) 0.0010(17) C7 0.025(2) 0.037(2) 0.0247(19) 0.0024(18) -0.0014(17) 0.0000(19) C8 0.023(2) 0.039(3) 0.033(2) -0.0052(19) -0.0021(18) -0.0059(19) C9 0.021(2) 0.027(2) 0.032(2) -0.0047(17) 0.0063(17) -0.0057(17) C10 0.0181(19) 0.0212(19) 0.0231(18) 0.0045(15) 0.0077(15) 0.0024(16) C11 0.022(2) 0.020(2) 0.0239(18) -0.0007(15) 0.0105(16) 0.0002(16) O12 0.0162(13) 0.0267(14) 0.0201(12) -0.0009(11) 0.0053(10) -0.0057(11) B13 0.019(2) 0.020(2) 0.022(2) 0.0012(17) 0.0031(17) -0.0016(18) O14 0.0187(13) 0.0202(13) 0.0216(12) -0.0027(10) 0.0068(10) -0.0032(11) C15 0.0195(19) 0.023(2) 0.0197(17) -0.0025(15) 0.0065(15) -0.0069(16) C16 0.0178(19) 0.024(2) 0.0181(17) -0.0001(15) 0.0046(15) -0.0020(16) C17 0.0186(19) 0.024(2) 0.0180(17) -0.0005(15) 0.0033(15) -0.0027(16) C18 0.025(2) 0.030(2) 0.0224(19) -0.0003(17) 0.0045(16) -0.0017(18) C19 0.027(2) 0.040(3) 0.032(2) -0.0034(19) 0.0140(18) 0.001(2) C20 0.024(2) 0.050(3) 0.046(3) 0.002(2) 0.017(2) -0.004(2) C21 0.024(2) 0.037(3) 0.039(2) 0.0034(19) 0.0104(18) -0.010(2) C22 0.022(2) 0.028(2) 0.0240(19) -0.0011(17) 0.0047(16) -0.0065(18) C23 0.030(2) 0.025(2) 0.030(2) 0.0031(17) 0.0053(18) -0.0115(18) C24 0.026(2) 0.022(2) 0.0260(19) -0.0004(16) 0.0059(16) -0.0022(17) I25 0.03495(16) 0.02067(14) 0.03668(15) -0.00147(11) 0.00637(12) -0.00036(11) C26 0.0217(19) 0.0180(19) 0.0191(17) -0.0016(15) 0.0092(15) -0.0019(16) C27 0.0221(19) 0.0183(19) 0.0187(17) -0.0014(15) 0.0094(15) 0.0011(16) O28 0.0209(13) 0.0182(13) 0.0175(11) 0.0007(10) 0.0012(10) -0.0002(11) Na29 0.0453(10) 0.0484(11) 0.0293(8) 0.0059(8) 0.0162(8) 0.0096(9) O30 0.062(2) 0.0376(17) 0.0284(14) -0.0019(13) 0.0170(15) 0.0065(16) O31 0.046(2) 0.0367(18) 0.0564(19) 0.0113(15) 0.0277(16) 0.0096(15) C32 0.045(3) 0.040(3) 0.035(2) 0.002(2) 0.017(2) -0.007(2) C33 0.035(3) 0.056(3) 0.065(3) -0.010(3) 0.022(2) -0.002(2) C34 0.068(4) 0.046(3) 0.072(3) 0.004(3) 0.040(3) 0.005(3) C35 0.065(4) 0.040(3) 0.095(4) 0.009(3) 0.050(3) 0.002(3) C41 0.0165(18) 0.023(2) 0.0247(18) -0.0007(16) 0.0058(15) -0.0013(16) I42 0.02431(14) 0.02605(15) 0.03733(14) -0.00641(11) 0.00501(11) -0.00569(11) C43 0.030(2) 0.018(2) 0.035(2) 0.0019(17) 0.0167(18) -0.0010(17) C44 0.0192(19) 0.023(2) 0.0239(18) 0.0049(16) 0.0025(16) 0.0034(17) C45 0.0191(19) 0.026(2) 0.0171(17) 0.0013(15) 0.0062(15) 0.0017(16) C46 0.026(2) 0.026(2) 0.032(2) 0.0019(18) 0.0094(18) -0.0037(18) C47 0.026(2) 0.046(3) 0.033(2) 0.005(2) -0.0011(19) -0.003(2) C48 0.033(3) 0.045(3) 0.039(2) 0.019(2) -0.001(2) 0.005(2) C49 0.033(2) 0.029(2) 0.044(2) 0.0107(19) 0.011(2) 0.003(2) O50 0.0219(14) 0.0229(14) 0.0224(12) 0.0070(11) 0.0082(11) 0.0043(11) C51 0.0204(19) 0.024(2) 0.0178(17) 0.0011(15) 0.0052(15) -0.0015(17) C52 0.025(2) 0.0204(19) 0.0190(17) 0.0020(15) 0.0049(15) -0.0017(16) C53 0.021(2) 0.025(2) 0.0223(18) 0.0007(16) 0.0010(16) 0.0002(17) C54 0.026(2) 0.031(2) 0.0279(19) 0.0004(18) 0.0067(17) -0.0003(18) C55 0.025(2) 0.033(2) 0.040(2) -0.0013(19) 0.0073(19) 0.0060(19) C56 0.036(3) 0.026(2) 0.046(2) -0.0023(19) 0.008(2) 0.011(2) C57 0.040(3) 0.021(2) 0.039(2) 0.0012(18) 0.005(2) -0.0028(19) C58 0.023(2) 0.022(2) 0.0248(19) -0.0001(16) 0.0009(16) -0.0006(16) C59 0.031(2) 0.022(2) 0.0225(18) 0.0037(16) 0.0030(17) -0.0082(18) C60 0.0194(19) 0.027(2) 0.0157(16) -0.0013(15) 0.0028(15) -0.0047(17) I61 0.02649(14) 0.03158(15) 0.02737(13) 0.00123(11) 0.01002(11) -0.00548(11) O62 0.049(2) 0.039(2) 0.127(3) -0.005(2) 0.026(2) 0.0050(18) C63 0.055(3) 0.044(3) 0.074(4) -0.003(3) 0.008(3) 0.011(3) C64 0.067(4) 0.048(3) 0.084(4) 0.010(3) 0.015(3) 0.006(3) C65 0.068(4) 0.076(5) 0.101(5) 0.024(4) 0.012(4) -0.021(4) C66 0.055(4) 0.063(4) 0.113(5) 0.021(4) 0.030(4) 0.020(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.099859(16) 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 I1 . C2 . 2.094(3) yes C2 . C3 . 1.356(5) yes C2 . C11 . 1.439(5) yes C3 . C4 . 1.418(5) yes C3 . H31 . 0.908 no C4 . C5 . 1.417(5) yes C4 . C9 . 1.406(5) yes C5 . C6 . 1.434(5) yes C5 . C10 . 1.426(5) yes C6 . C7 . 1.367(5) yes C6 . H61 . 0.921 no C7 . C8 . 1.411(6) yes C7 . H71 . 0.947 no C8 . C9 . 1.362(5) yes C8 . H81 . 0.938 no C9 . H91 . 0.936 no C10 . C11 . 1.381(5) yes C10 . C52 . 1.492(5) yes C11 . O12 . 1.340(4) yes O12 . B13 . 1.460(5) yes B13 . O14 . 1.469(5) yes B13 . O28 . 1.481(5) yes B13 . O50 . 1.481(5) yes O14 . C15 . 1.361(4) yes C15 . C16 . 1.376(5) yes C15 . C24 . 1.417(5) yes C16 . C17 . 1.437(5) yes C16 . C26 . 1.479(5) yes C17 . C18 . 1.425(5) yes C17 . C22 . 1.422(5) yes C18 . C19 . 1.361(5) yes C18 . H181 . 0.946 no C19 . C20 . 1.415(6) yes C19 . H191 . 0.952 no C20 . C21 . 1.362(6) yes C20 . H201 . 0.913 no C21 . C22 . 1.420(5) yes C21 . H211 . 0.928 no C22 . C23 . 1.414(6) yes C23 . C24 . 1.357(5) yes C23 . H231 . 0.938 no C24 . I25 . 2.087(4) yes C26 . C27 . 1.388(5) yes C26 . C45 . 1.440(5) yes C27 . O28 . 1.353(4) yes C27 . C41 . 1.412(5) yes O28 . Na29 . 2.308(3) yes Na29 . O30 . 2.233(3) yes Na29 . O31 . 2.371(3) yes Na29 . O50 . 2.524(3) yes Na29 . O361 . 2.337(7) yes O30 . H301 . 0.811 no O30 . H302 . 0.849 no O31 . C32 . 1.435(5) yes O31 . C35 . 1.421(6) yes C32 . C33 . 1.503(7) yes C32 . H322 . 0.960 no C32 . H321 . 0.970 no C33 . C34 . 1.493(7) yes C33 . H332 . 0.980 no C33 . H331 . 0.964 no C34 . C35 . 1.442(7) yes C34 . H341 . 0.977 no C34 . H342 . 0.980 no C35 . H351 . 0.967 no C35 . H352 . 0.993 no C41 . I42 . 2.103(4) yes C41 . C43 . 1.355(5) yes C43 . C44 . 1.422(5) yes C43 . H431 . 0.926 no C44 . C45 . 1.417(5) yes C44 . C49 . 1.428(5) yes C45 . C46 . 1.420(5) yes C46 . C47 . 1.369(5) yes C46 . H461 . 0.930 no C47 . C48 . 1.399(6) yes C47 . H471 . 0.959 no C48 . C49 . 1.342(6) yes C48 . H481 . 0.900 no C49 . H491 . 0.925 no O50 . C51 . 1.353(4) yes C51 . C52 . 1.395(5) yes C51 . C60 . 1.419(5) yes C52 . C53 . 1.429(5) yes C53 . C54 . 1.414(5) yes C53 . C58 . 1.429(5) yes C54 . C55 . 1.372(6) yes C54 . H541 . 0.938 no C55 . C56 . 1.407(6) yes C55 . H551 . 0.948 no C56 . C57 . 1.350(6) yes C56 . H561 . 0.919 no C57 . C58 . 1.426(5) yes C57 . H571 . 0.946 no C58 . C59 . 1.405(5) yes C59 . C60 . 1.355(5) yes C59 . H591 . 0.926 no C60 . I61 . 2.099(4) yes O62 . C63 . 1.433(6) yes O62 . C66 . 1.422(7) yes C63 . C64 . 1.484(8) yes C63 . H632 . 1.000 no C63 . H631 . 0.972 no C64 . C65 . 1.509(9) yes C64 . H641 . 0.977 no C64 . H642 . 0.977 no C65 . C66 . 1.489(9) yes C65 . H652 . 0.971 no C65 . H651 . 0.996 no C66 . H662 . 0.966 no C66 . H661 . 0.979 no O360 . C370 . 1.466(9) yes O360 . C400 . 1.455(9) yes C370 . C380 . 1.465(10) yes C370 . H3701 . 0.978 no C370 . H3702 . 0.961 no C380 . C390 . 1.513(10) yes C380 . H3801 . 0.994 no C380 . H3802 . 0.966 no C390 . C400 . 1.544(10) yes C390 . H3901 . 0.953 no C390 . H3902 . 0.988 no C400 . H4002 . 0.995 no C400 . H4001 . 0.968 no O361 . C371 . 1.417(9) yes O361 . C401 . 1.447(9) yes C371 . C381 . 1.528(10) yes C371 . H3712 . 0.964 no C371 . H3711 . 0.977 no C381 . C391 . 1.497(10) yes C381 . H3812 . 0.980 no C381 . H3811 . 0.971 no C391 . C401 . 1.486(10) yes C391 . H3911 . 0.968 no C391 . H3912 . 0.984 no C401 . H4012 . 0.982 no C401 . H4011 . 0.985 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 I1 . C2 . C3 . 121.0(3) yes I1 . C2 . C11 . 118.4(3) yes C3 . C2 . C11 . 120.6(3) yes C2 . C3 . C4 . 120.9(3) yes C2 . C3 . H31 . 120.3 no C4 . C3 . H31 . 118.8 no C3 . C4 . C5 . 118.5(3) yes C3 . C4 . C9 . 121.2(3) yes C5 . C4 . C9 . 120.3(3) yes C4 . C5 . C6 . 117.2(3) yes C4 . C5 . C10 . 120.0(3) yes C6 . C5 . C10 . 122.7(3) yes C5 . C6 . C7 . 121.3(3) yes C5 . C6 . H61 . 118.2 no C7 . C6 . H61 . 120.5 no C6 . C7 . C8 . 120.2(3) yes C6 . C7 . H71 . 119.9 no C8 . C7 . H71 . 119.9 no C7 . C8 . C9 . 120.1(4) yes C7 . C8 . H81 . 120.9 no C9 . C8 . H81 . 119.0 no C4 . C9 . C8 . 120.9(4) yes C4 . C9 . H91 . 118.2 no C8 . C9 . H91 . 120.9 no C5 . C10 . C11 . 119.5(3) yes C5 . C10 . C52 . 121.0(3) yes C11 . C10 . C52 . 119.4(3) yes C2 . C11 . C10 . 118.9(3) yes C2 . C11 . O12 . 118.9(3) yes C10 . C11 . O12 . 122.1(3) yes C11 . O12 . B13 . 120.1(3) yes O12 . B13 . O14 . 100.6(3) yes O12 . B13 . O28 . 114.7(3) yes O14 . B13 . O28 . 113.0(3) yes O12 . B13 . O50 . 114.7(3) yes O14 . B13 . O50 . 114.7(3) yes O28 . B13 . O50 . 99.8(3) yes B13 . O14 . C15 . 120.0(3) yes O14 . C15 . C16 . 120.8(3) yes O14 . C15 . C24 . 118.4(3) yes C16 . C15 . C24 . 120.6(3) yes C15 . C16 . C17 . 118.4(3) yes C15 . C16 . C26 . 120.1(3) yes C17 . C16 . C26 . 121.6(3) yes C16 . C17 . C18 . 122.4(3) yes C16 . C17 . C22 . 119.7(3) yes C18 . C17 . C22 . 117.8(3) yes C17 . C18 . C19 . 121.3(4) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 119.1 no C18 . C19 . C20 . 120.5(4) yes C18 . C19 . H191 . 119.7 no C20 . C19 . H191 . 119.8 no C19 . C20 . C21 . 119.9(4) yes C19 . C20 . H201 . 119.6 no C21 . C20 . H201 . 120.5 no C20 . C21 . C22 . 120.9(4) yes C20 . C21 . H211 . 118.4 no C22 . C21 . H211 . 120.7 no C17 . C22 . C21 . 119.4(3) yes C17 . C22 . C23 . 118.9(3) yes C21 . C22 . C23 . 121.7(3) yes C22 . C23 . C24 . 120.5(3) yes C22 . C23 . H231 . 121.4 no C24 . C23 . H231 . 118.1 no C15 . C24 . C23 . 120.8(3) yes C15 . C24 . I25 . 118.5(3) yes C23 . C24 . I25 . 120.6(3) yes C16 . C26 . C27 . 120.2(3) yes C16 . C26 . C45 . 120.8(3) yes C27 . C26 . C45 . 118.9(3) yes C26 . C27 . O28 . 120.8(3) yes C26 . C27 . C41 . 119.6(3) yes O28 . C27 . C41 . 119.4(3) yes C27 . O28 . B13 . 121.6(3) yes C27 . O28 . Na29 . 124.3(2) yes B13 . O28 . Na29 . 106.77(19) yes O28 . Na29 . O30 . 153.67(13) yes O28 . Na29 . O31 . 95.16(11) yes O30 . Na29 . O31 . 90.32(12) yes O28 . Na29 . O50 . 55.70(8) yes O30 . Na29 . O50 . 105.72(11) yes O31 . Na29 . O50 . 140.70(12) yes O28 . Na29 . O361 . 106.4(2) yes O30 . Na29 . O361 . 97.5(2) yes O31 . Na29 . O361 . 102.3(2) yes O50 . Na29 . O361 . 110.5(2) yes Na29 . O30 . H301 . 119.1 no Na29 . O30 . H302 . 107.4 no H301 . O30 . H302 . 111.8 no Na29 . O31 . C32 . 122.5(2) yes Na29 . O31 . C35 . 125.5(3) yes C32 . O31 . C35 . 109.2(3) yes O31 . C32 . C33 . 106.2(3) yes O31 . C32 . H322 . 108.6 no C33 . C32 . H322 . 111.1 no O31 . C32 . H321 . 109.4 no C33 . C32 . H321 . 111.1 no H322 . C32 . H321 . 110.4 no C32 . C33 . C34 . 104.5(4) yes C32 . C33 . H332 . 110.1 no C34 . C33 . H332 . 112.8 no C32 . C33 . H331 . 111.1 no C34 . C33 . H331 . 107.3 no H332 . C33 . H331 . 110.9 no C33 . C34 . C35 . 104.8(4) yes C33 . C34 . H341 . 106.6 no C35 . C34 . H341 . 104.4 no C33 . C34 . H342 . 113.3 no C35 . C34 . H342 . 115.3 no H341 . C34 . H342 . 111.8 no C34 . C35 . O31 . 108.2(4) yes C34 . C35 . H351 . 112.8 no O31 . C35 . H351 . 111.0 no C34 . C35 . H352 . 106.2 no O31 . C35 . H352 . 109.2 no H351 . C35 . H352 . 109.2 no C27 . C41 . I42 . 119.1(3) yes C27 . C41 . C43 . 121.8(3) yes I42 . C41 . C43 . 118.9(3) yes C41 . C43 . C44 . 120.0(3) yes C41 . C43 . H431 . 119.5 no C44 . C43 . H431 . 120.5 no C43 . C44 . C45 . 119.3(3) yes C43 . C44 . C49 . 121.4(3) yes C45 . C44 . C49 . 119.2(3) yes C26 . C45 . C44 . 119.3(3) yes C26 . C45 . C46 . 122.7(3) yes C44 . C45 . C46 . 117.9(3) yes C45 . C46 . C47 . 121.0(4) yes C45 . C46 . H461 . 120.5 no C47 . C46 . H461 . 118.5 no C46 . C47 . C48 . 120.2(4) yes C46 . C47 . H471 . 120.1 no C48 . C47 . H471 . 119.7 no C47 . C48 . C49 . 120.9(4) yes C47 . C48 . H481 . 119.7 no C49 . C48 . H481 . 119.4 no C44 . C49 . C48 . 120.7(4) yes C44 . C49 . H491 . 117.5 no C48 . C49 . H491 . 121.8 no B13 . O50 . Na29 . 97.2(2) yes B13 . O50 . C51 . 121.2(3) yes Na29 . O50 . C51 . 139.6(2) yes O50 . C51 . C52 . 121.0(3) yes O50 . C51 . C60 . 119.9(3) yes C52 . C51 . C60 . 118.9(3) yes C10 . C52 . C51 . 119.8(3) yes C10 . C52 . C53 . 120.7(3) yes C51 . C52 . C53 . 119.4(3) yes C52 . C53 . C54 . 123.1(3) yes C52 . C53 . C58 . 119.1(3) yes C54 . C53 . C58 . 117.7(3) yes C53 . C54 . C55 . 121.6(4) yes C53 . C54 . H541 . 119.5 no C55 . C54 . H541 . 119.0 no C54 . C55 . C56 . 120.5(4) yes C54 . C55 . H551 . 120.3 no C56 . C55 . H551 . 119.1 no C55 . C56 . C57 . 119.6(4) yes C55 . C56 . H561 . 121.0 no C57 . C56 . H561 . 119.4 no C56 . C57 . C58 . 121.9(4) yes C56 . C57 . H571 . 119.4 no C58 . C57 . H571 . 118.7 no C53 . C58 . C57 . 118.6(3) yes C53 . C58 . C59 . 118.9(3) yes C57 . C58 . C59 . 122.5(3) yes C58 . C59 . C60 . 120.9(3) yes C58 . C59 . H591 . 118.1 no C60 . C59 . H591 . 120.9 no C51 . C60 . C59 . 121.4(3) yes C51 . C60 . I61 . 120.0(3) yes C59 . C60 . I61 . 118.6(3) yes C63 . O62 . C66 . 108.0(4) yes O62 . C63 . C64 . 107.2(4) yes O62 . C63 . H632 . 111.7 no C64 . C63 . H632 . 110.8 no O62 . C63 . H631 . 109.3 no C64 . C63 . H631 . 108.3 no H632 . C63 . H631 . 109.4 no C63 . C64 . C65 . 102.9(4) yes C63 . C64 . H641 . 109.5 no C65 . C64 . H641 . 108.7 no C63 . C64 . H642 . 112.3 no C65 . C64 . H642 . 112.6 no H641 . C64 . H642 . 110.5 no C64 . C65 . C66 . 101.1(5) yes C64 . C65 . H652 . 113.7 no C66 . C65 . H652 . 113.2 no C64 . C65 . H651 . 108.8 no C66 . C65 . H651 . 106.7 no H652 . C65 . H651 . 112.6 no C65 . C66 . O62 . 106.5(5) yes C65 . C66 . H662 . 108.2 no O62 . C66 . H662 . 111.3 no C65 . C66 . H661 . 110.6 no O62 . C66 . H661 . 109.6 no H662 . C66 . H661 . 110.5 no Na29 . O360 . C370 . 130.6(4) yes Na29 . O360 . C400 . 120.0(4) yes C370 . O360 . C400 . 109.11(10) yes O360 . C370 . C380 . 107.05(10) yes O360 . C370 . H3701 . 108.6 no C380 . C370 . H3701 . 111.8 no O360 . C370 . H3702 . 108.6 no C380 . C370 . H3702 . 109.7 no H3701 . C370 . H3702 . 111.0 no C370 . C380 . C390 . 103.38(10) yes C370 . C380 . H3801 . 110.8 no C390 . C380 . H3801 . 108.0 no C370 . C380 . H3802 . 111.8 no C390 . C380 . H3802 . 112.4 no H3801 . C380 . H3802 . 110.2 no C380 . C390 . C400 . 103.49(10) yes C380 . C390 . H3901 . 112.8 no C400 . C390 . H3901 . 111.8 no C380 . C390 . H3902 . 111.0 no C400 . C390 . H3902 . 109.6 no H3901 . C390 . H3902 . 108.1 no C390 . C400 . O360 . 104.70(10) yes C390 . C400 . H4002 . 111.9 no O360 . C400 . H4002 . 110.8 no C390 . C400 . H4001 . 110.9 no O360 . C400 . H4001 . 110.8 no H4002 . C400 . H4001 . 107.8 no Na29 . O361 . C371 . 110.2(5) yes Na29 . O361 . C401 . 132.5(5) yes C371 . O361 . C401 . 109.01(10) yes O361 . C371 . C381 . 106.98(10) yes O361 . C371 . H3712 . 110.1 no C381 . C371 . H3712 . 111.4 no O361 . C371 . H3711 . 109.1 no C381 . C371 . H3711 . 110.4 no H3712 . C371 . H3711 . 108.9 no C371 . C381 . C391 . 103.37(10) yes C371 . C381 . H3812 . 111.0 no C391 . C381 . H3812 . 110.0 no C371 . C381 . H3811 . 110.8 no C391 . C381 . H3811 . 111.7 no H3812 . C381 . H3811 . 109.8 no C381 . C391 . C401 . 103.42(10) yes C381 . C391 . H3911 . 113.1 no C401 . C391 . H3911 . 112.2 no C381 . C391 . H3912 . 108.7 no C401 . C391 . H3912 . 110.2 no H3911 . C391 . H3912 . 109.2 no C391 . C401 . O361 . 104.61(10) yes C391 . C401 . H4012 . 108.3 no O361 . C401 . H4012 . 111.3 no C391 . C401 . H4011 . 112.0 no O361 . C401 . H4011 . 110.8 no H4012 . C401 . H4011 . 109.7 no 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 C9 . H91 . O62 4_565 144 0.94 2.46 3.262(7) yes O30 . H301 . O14 4_555 168 0.81 2.04 2.835(7) yes _chemical_name_common . #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 796355' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 07-12-14 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5657 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 25.5708(2) _cell_length_b 9.8286(1) _cell_length_c 23.5937(2) _cell_angle_alpha 90 _cell_angle_beta 111.3071(4) _cell_angle_gamma 90 _cell_volume 5524.37(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' 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 = C56 H32 B1 Na1 O4 # Dc = 0.97 Fooo = 2304.00 Mu = 0.66 M = 401.33 # Found Formula = C72 H64 B1 Na1 O8 # Dc = 1.31 FOOO = 2304.00 Mu = 0.91 M = 545.55 _chemical_formula_sum 'C72 H64 B1 Na1 O8' _chemical_formula_moiety 'C72 H64 B1 Na1 O8' _chemical_compound_source . _chemical_formula_weight 1091.10 _cell_measurement_reflns_used 6653 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.26 _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 0.091 # Sheldrick geometric approximatio 0.98 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.99 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 150 _diffrn_reflns_number 73285 _reflns_number_total 6298 _diffrn_reflns_av_R_equivalents 0.047 # Number of reflections with Friedels Law is 6298 # Number of reflections without Friedels Law is 12582 # Theoretical number of reflections is about 6335 _diffrn_reflns_theta_min 5.127 _diffrn_reflns_theta_max 27.483 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.934 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -33 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _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 -0.51 _refine_diff_density_max 1.15 # 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>-3.0\s(I) _refine_ls_number_reflns 6298 _refine_ls_number_restraints 0 _refine_ls_number_parameters 371 _oxford_refine_ls_R_factor_ref 0.0703 _refine_ls_wR_factor_ref 0.1352 _refine_ls_goodness_of_fit_ref 0.9241 _refine_ls_shift/su_max 0.000474 # The values computed from all data _oxford_reflns_number_all 6298 _refine_ls_R_factor_all 0.0703 _refine_ls_wR_factor_all 0.1352 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4517 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_gt 0.1277 # 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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 2.38P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Na1 Na 0.5000 -0.17400(8) 0.2500 0.0271 1.0000 Uani S T . . . . . O2 O 0.54111(4) 0.04956(10) 0.24175(4) 0.0221 1.0000 Uani . . . . . . . C3 C 0.58737(6) 0.10684(14) 0.23520(6) 0.0207 1.0000 Uani . . . . . . . C4 C 0.62705(6) 0.17087(14) 0.28283(6) 0.0207 1.0000 Uani . . . . . . . C5 C 0.67214(6) 0.24290(14) 0.27172(6) 0.0219 1.0000 Uani . . . . . . . C6 C 0.67830(6) 0.23372(15) 0.21431(6) 0.0240 1.0000 Uani . . . . . . . C7 C 0.63816(6) 0.15383(15) 0.16607(6) 0.0238 1.0000 Uani . . . . . . . C8 C 0.59275(6) 0.09169(14) 0.17669(6) 0.0221 1.0000 Uani . . . . . . . C9 C 0.55348(6) 0.01320(15) 0.13067(6) 0.0269 1.0000 Uani . . . . . . . C10 C 0.55889(7) -0.00333(16) 0.07535(7) 0.0311 1.0000 Uani . . . . . . . C11 C 0.60307(7) 0.06004(17) 0.06393(7) 0.0334 1.0000 Uani . . . . . . . C12 C 0.64155(7) 0.13752(16) 0.10788(7) 0.0300 1.0000 Uani . . . . . . . C13 C 0.72168(6) 0.30948(16) 0.20520(7) 0.0302 1.0000 Uani . . . . . . . C14 C 0.75626(7) 0.39344(17) 0.24934(8) 0.0339 1.0000 Uani . . . . . . . C15 C 0.74918(7) 0.40492(17) 0.30516(7) 0.0327 1.0000 Uani . . . . . . . C16 C 0.70836(6) 0.33110(16) 0.31607(7) 0.0272 1.0000 Uani . . . . . . . C17 C 0.62191(6) 0.17589(14) 0.34376(6) 0.0200 1.0000 Uani . . . . . . . C18 C 0.57242(6) 0.21454(14) 0.34905(6) 0.0205 1.0000 Uani . . . . . . . O19 O 0.52505(4) 0.23992(10) 0.30073(4) 0.0232 1.0000 Uani . . . . . . . B20 B 0.5000 0.1458(2) 0.2500 0.0210 1.0000 Uani S T . . . . . C21 C 0.56956(6) 0.24649(14) 0.40777(6) 0.0214 1.0000 Uani . . . . . . . C22 C 0.52039(6) 0.30425(15) 0.41133(7) 0.0252 1.0000 Uani . . . . . . . C23 C 0.51879(7) 0.34634(16) 0.46619(7) 0.0297 1.0000 Uani . . . . . . . C24 C 0.56674(7) 0.33228(16) 0.51887(7) 0.0320 1.0000 Uani . . . . . . . C25 C 0.61454(7) 0.27312(16) 0.51688(7) 0.0287 1.0000 Uani . . . . . . . C26 C 0.61717(6) 0.22678(15) 0.46120(6) 0.0229 1.0000 Uani . . . . . . . C27 C 0.66597(6) 0.15862(15) 0.45681(6) 0.0234 1.0000 Uani . . . . . . . C28 C 0.66845(6) 0.13527(14) 0.39845(6) 0.0217 1.0000 Uani . . . . . . . C29 C 0.71544(6) 0.06527(15) 0.39516(7) 0.0272 1.0000 Uani . . . . . . . C30 C 0.75793(6) 0.02055(17) 0.44653(7) 0.0317 1.0000 Uani . . . . . . . C31 C 0.75524(6) 0.04313(17) 0.50398(7) 0.0330 1.0000 Uani . . . . . . . C32 C 0.71033(6) 0.11115(16) 0.50864(7) 0.0291 1.0000 Uani . . . . . . . O33 O 0.45521(4) -0.21420(12) 0.14058(5) 0.0356 1.0000 Uani . . . . . . . C34 C 0.45343(8) -0.3418(2) 0.11111(10) 0.0578 1.0000 Uani . . . . . . . C35 C 0.39972(9) -0.3489(2) 0.05794(11) 0.0676 1.0000 Uani . . . . . . . C36 C 0.36240(8) -0.2541(2) 0.07491(10) 0.0589 1.0000 Uani . . . . . . . C37 C 0.40199(7) -0.14868(18) 0.11315(8) 0.0410 1.0000 Uani . . . . . . . O38 O 0.42698(5) -0.32262(12) 0.24859(6) 0.0421 1.0000 Uani . . . . . . . C39 C 0.37642(7) -0.26727(19) 0.25156(8) 0.0425 1.0000 Uani . . . . . . . C40 C 0.36904(9) -0.3346(2) 0.30573(9) 0.0503 1.0000 Uani . . . . . . . C41 C 0.40169(7) -0.46768(18) 0.31325(8) 0.0376 1.0000 Uani . . . . . . . C42 C 0.42609(8) -0.46395(18) 0.26354(9) 0.0412 1.0000 Uani . . . . . . . H91 H 0.5245 -0.0252 0.1407 0.0339 1.0000 Uiso R . . . . . . H101 H 0.5326 -0.0578 0.0452 0.0380 1.0000 Uiso R . . . . . . H111 H 0.6061 0.0426 0.0230 0.0408 1.0000 Uiso R . . . . . . H121 H 0.6714 0.1789 0.0986 0.0395 1.0000 Uiso R . . . . . . H131 H 0.7268 0.3015 0.1660 0.0404 1.0000 Uiso R . . . . . . H141 H 0.7884 0.4410 0.2423 0.0418 1.0000 Uiso R . . . . . . H151 H 0.7735 0.4650 0.3367 0.0420 1.0000 Uiso R . . . . . . H161 H 0.7023 0.3410 0.3536 0.0318 1.0000 Uiso R . . . . . . H221 H 0.4881 0.3145 0.3762 0.0302 1.0000 Uiso R . . . . . . H231 H 0.4830 0.3844 0.4676 0.0387 1.0000 Uiso R . . . . . . H241 H 0.5666 0.3608 0.5569 0.0387 1.0000 Uiso R . . . . . . H251 H 0.6487 0.2678 0.5561 0.0350 1.0000 Uiso R . . . . . . H291 H 0.7178 0.0462 0.3532 0.0326 1.0000 Uiso R . . . . . . H301 H 0.7899 -0.0274 0.4450 0.0362 1.0000 Uiso R . . . . . . H311 H 0.7870 0.0107 0.5420 0.0372 1.0000 Uiso R . . . . . . H321 H 0.7083 0.1248 0.5474 0.0330 1.0000 Uiso R . . . . . . H342 H 0.4865 -0.3494 0.1004 0.0657 1.0000 Uiso R . . . . . . H341 H 0.4548 -0.4179 0.1414 0.0664 1.0000 Uiso R . . . . . . H352 H 0.3991 -0.3061 0.0151 0.0795 1.0000 Uiso R . . . . . . H351 H 0.3856 -0.4441 0.0501 0.0776 1.0000 Uiso R . . . . . . H362 H 0.3465 -0.3106 0.1025 0.0650 1.0000 Uiso R . . . . . . H361 H 0.3327 -0.2242 0.0392 0.0634 1.0000 Uiso R . . . . . . H372 H 0.4064 -0.0793 0.0866 0.0496 1.0000 Uiso R . . . . . . H371 H 0.3906 -0.1124 0.1471 0.0485 1.0000 Uiso R . . . . . . H392 H 0.3779 -0.1666 0.2546 0.0518 1.0000 Uiso R . . . . . . H391 H 0.3436 -0.2857 0.2143 0.0511 1.0000 Uiso R . . . . . . H402 H 0.3845 -0.2706 0.3435 0.0664 1.0000 Uiso R . . . . . . H401 H 0.3312 -0.3506 0.3025 0.0646 1.0000 Uiso R . . . . . . H412 H 0.4324 -0.4697 0.3558 0.0466 1.0000 Uiso R . . . . . . H411 H 0.3759 -0.5482 0.3051 0.0476 1.0000 Uiso R . . . . . . H422 H 0.4667 -0.4975 0.2789 0.0578 1.0000 Uiso R . . . . . . H421 H 0.4006 -0.5183 0.2253 0.0549 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 Na1 0.0252(4) 0.0260(4) 0.0288(4) 0.0000 0.0082(3) 0.0000 O2 0.0178(5) 0.0236(5) 0.0243(5) -0.0030(4) 0.0067(4) -0.0017(4) C3 0.0186(6) 0.0209(7) 0.0217(7) 0.0007(6) 0.0062(5) 0.0015(5) C4 0.0201(7) 0.0205(7) 0.0207(7) 0.0023(5) 0.0064(5) 0.0034(5) C5 0.0203(7) 0.0225(7) 0.0220(7) 0.0025(6) 0.0067(5) 0.0032(5) C6 0.0227(7) 0.0242(7) 0.0254(7) 0.0034(6) 0.0091(6) 0.0048(6) C7 0.0248(7) 0.0240(7) 0.0224(7) 0.0036(6) 0.0084(6) 0.0068(6) C8 0.0235(7) 0.0225(7) 0.0191(7) 0.0001(6) 0.0062(5) 0.0063(6) C9 0.0280(7) 0.0265(8) 0.0240(7) -0.0010(6) 0.0066(6) 0.0036(6) C10 0.0354(8) 0.0311(8) 0.0218(7) -0.0042(6) 0.0045(6) 0.0066(7) C11 0.0431(9) 0.0358(9) 0.0218(7) -0.0005(7) 0.0124(7) 0.0098(7) C12 0.0338(8) 0.0335(9) 0.0261(7) 0.0032(6) 0.0148(6) 0.0072(7) C13 0.0290(8) 0.0335(9) 0.0317(8) 0.0049(7) 0.0156(7) 0.0024(7) C14 0.0272(8) 0.0366(9) 0.0406(9) 0.0051(8) 0.0155(7) -0.0039(7) C15 0.0291(8) 0.0337(9) 0.0335(8) -0.0014(7) 0.0091(7) -0.0082(7) C16 0.0246(7) 0.0308(8) 0.0246(7) 0.0007(6) 0.0069(6) -0.0021(6) C17 0.0203(6) 0.0208(7) 0.0169(6) -0.0002(5) 0.0043(5) -0.0018(5) C18 0.0202(7) 0.0187(7) 0.0188(6) 0.0007(5) 0.0027(5) -0.0007(5) O19 0.0195(5) 0.0254(5) 0.0197(5) -0.0015(4) 0.0011(4) 0.0032(4) B20 0.0196(10) 0.0240(11) 0.0179(10) 0.0000 0.0050(8) 0.0000 C21 0.0234(7) 0.0194(7) 0.0208(7) -0.0006(5) 0.0073(6) -0.0026(5) C22 0.0249(7) 0.0234(7) 0.0260(7) -0.0005(6) 0.0079(6) -0.0010(6) C23 0.0341(8) 0.0279(8) 0.0312(8) -0.0006(7) 0.0167(7) 0.0009(7) C24 0.0444(9) 0.0318(8) 0.0228(7) -0.0024(6) 0.0159(7) 0.0006(7) C25 0.0346(8) 0.0291(8) 0.0210(7) 0.0003(6) 0.0083(6) -0.0017(7) C26 0.0256(7) 0.0226(7) 0.0195(7) 0.0006(6) 0.0070(6) -0.0037(6) C27 0.0230(7) 0.0237(7) 0.0206(7) 0.0013(6) 0.0045(6) -0.0029(6) C28 0.0200(7) 0.0218(7) 0.0206(7) 0.0013(6) 0.0043(5) -0.0031(5) C29 0.0239(7) 0.0292(8) 0.0264(7) 0.0005(6) 0.0067(6) 0.0005(6) C30 0.0235(7) 0.0347(9) 0.0330(8) 0.0020(7) 0.0055(6) 0.0052(6) C31 0.0267(8) 0.0366(9) 0.0266(8) 0.0048(7) -0.0012(6) 0.0029(7) C32 0.0287(8) 0.0331(8) 0.0207(7) 0.0023(6) 0.0033(6) -0.0009(6) O33 0.0325(6) 0.0346(6) 0.0341(6) -0.0045(5) 0.0055(5) -0.0019(5) C34 0.0428(11) 0.0582(13) 0.0617(13) -0.0270(11) 0.0062(9) 0.0132(9) C35 0.0520(12) 0.0560(13) 0.0765(16) -0.0302(12) 0.0016(11) 0.0045(10) C36 0.0332(10) 0.0590(13) 0.0687(14) -0.0207(11) -0.0005(9) 0.0058(9) C37 0.0465(10) 0.0323(9) 0.0369(9) -0.0013(7) 0.0065(8) 0.0087(8) O38 0.0380(6) 0.0396(7) 0.0547(8) -0.0003(6) 0.0239(6) -0.0087(5) C39 0.0389(10) 0.0418(10) 0.0477(10) 0.0045(8) 0.0169(8) -0.0005(8) C40 0.0542(12) 0.0564(12) 0.0464(11) 0.0107(10) 0.0257(9) 0.0155(10) C41 0.0406(9) 0.0342(9) 0.0394(9) -0.0035(8) 0.0162(8) -0.0083(7) C42 0.0455(10) 0.0356(9) 0.0479(10) -0.0044(8) 0.0233(8) -0.0050(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.20792(17) 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 Na1 . O38 5_655 2.3615(12) yes Na1 . O33 5_655 2.4463(11) yes Na1 . O2 5_655 2.4737(12) yes Na1 . O2 . 2.4737(12) yes Na1 . O33 . 2.4463(11) yes Na1 . O38 . 2.3615(12) yes O2 . C3 . 1.3687(16) yes O2 . B20 . 1.4783(17) yes C3 . C4 . 1.3637(19) yes C3 . C8 . 1.4440(19) yes C4 . C5 . 1.4556(19) yes C4 . C17 . 1.4913(18) yes C5 . C6 . 1.4222(19) yes C5 . C16 . 1.414(2) yes C6 . C7 . 1.455(2) yes C6 . C13 . 1.416(2) yes C7 . C8 . 1.413(2) yes C7 . C12 . 1.416(2) yes C8 . C9 . 1.411(2) yes C9 . C10 . 1.371(2) yes C9 . H91 . 0.935 no C10 . C11 . 1.399(2) yes C10 . H101 . 0.947 no C11 . C12 . 1.372(2) yes C11 . H111 . 1.010 no C12 . H121 . 0.959 no C13 . C14 . 1.370(2) yes C13 . H131 . 0.983 no C14 . C15 . 1.398(2) yes C14 . H141 . 1.009 no C15 . C16 . 1.370(2) yes C15 . H151 . 0.976 no C16 . H161 . 0.958 no C17 . C18 . 1.3697(19) yes C17 . C28 . 1.4576(18) yes C18 . O19 . 1.3511(15) yes C18 . C21 . 1.4481(19) yes O19 . B20 . 1.4636(17) yes C21 . C22 . 1.409(2) yes C21 . C26 . 1.4120(19) yes C22 . C23 . 1.374(2) yes C22 . H221 . 0.939 no C23 . C24 . 1.400(2) yes C23 . H231 . 1.001 no C24 . C25 . 1.370(2) yes C24 . H241 . 0.942 no C25 . C26 . 1.415(2) yes C25 . H251 . 1.017 no C26 . C27 . 1.453(2) yes C27 . C28 . 1.4198(19) yes C27 . C32 . 1.4113(19) yes C28 . C29 . 1.411(2) yes C29 . C30 . 1.373(2) yes C29 . H291 . 1.030 no C30 . C31 . 1.400(2) yes C30 . H301 . 0.956 no C31 . C32 . 1.367(2) yes C31 . H311 . 1.018 no C32 . H321 . 0.943 no O33 . C34 . 1.427(2) yes O33 . C37 . 1.430(2) yes C34 . C35 . 1.488(3) yes C34 . H342 . 0.970 no C34 . H341 . 1.025 no C35 . C36 . 1.489(3) yes C35 . H352 . 1.090 no C35 . H351 . 0.996 no C36 . C37 . 1.500(3) yes C36 . H362 . 1.044 no C36 . H361 . 0.953 no C37 . H372 . 0.959 no C37 . H371 . 1.012 no O38 . C39 . 1.428(2) yes O38 . C42 . 1.435(2) yes C39 . C40 . 1.511(3) yes C39 . H392 . 0.992 no C39 . H391 . 0.987 no C40 . C41 . 1.527(3) yes C40 . H402 . 1.044 no C40 . H401 . 0.955 no C41 . C42 . 1.516(2) yes C41 . H412 . 1.025 no C41 . H411 . 1.004 no C42 . H422 . 1.023 no C42 . H421 . 1.048 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 O38 5_655 Na1 . O33 5_655 79.67(4) yes O38 5_655 Na1 . O2 5_655 154.79(4) yes O33 5_655 Na1 . O2 5_655 96.30(4) yes O38 5_655 Na1 . O2 . 101.19(4) yes O33 5_655 Na1 . O2 . 100.20(4) yes O2 5_655 Na1 . O2 . 54.69(5) yes O38 5_655 Na1 . O33 . 88.83(4) yes O33 5_655 Na1 . O33 . 161.41(7) yes O2 5_655 Na1 . O33 . 100.20(4) yes O2 . Na1 . O33 . 96.30(4) yes O38 5_655 Na1 . O38 . 103.58(7) yes O33 5_655 Na1 . O38 . 88.83(4) yes O2 5_655 Na1 . O38 . 101.19(4) yes O2 . Na1 . O38 . 154.79(4) yes O33 . Na1 . O38 . 79.67(4) yes Na1 . O2 . C3 . 141.60(8) yes Na1 . O2 . B20 . 102.42(8) yes C3 . O2 . B20 . 115.90(11) yes O2 . C3 . C4 . 120.77(12) yes O2 . C3 . C8 . 116.88(12) yes C4 . C3 . C8 . 122.31(12) yes C3 . C4 . C5 . 118.49(12) yes C3 . C4 . C17 . 120.65(12) yes C5 . C4 . C17 . 120.69(12) yes C4 . C5 . C6 . 120.64(12) yes C4 . C5 . C16 . 120.90(12) yes C6 . C5 . C16 . 118.31(13) yes C5 . C6 . C7 . 119.25(12) yes C5 . C6 . C13 . 118.38(13) yes C7 . C6 . C13 . 122.28(13) yes C6 . C7 . C8 . 119.10(12) yes C6 . C7 . C12 . 123.05(13) yes C8 . C7 . C12 . 117.82(13) yes C3 . C8 . C7 . 119.66(13) yes C3 . C8 . C9 . 120.25(13) yes C7 . C8 . C9 . 120.08(13) yes C8 . C9 . C10 . 120.49(14) yes C8 . C9 . H91 . 115.7 no C10 . C9 . H91 . 123.8 no C9 . C10 . C11 . 119.89(14) yes C9 . C10 . H101 . 119.4 no C11 . C10 . H101 . 120.7 no C10 . C11 . C12 . 120.59(14) yes C10 . C11 . H111 . 117.1 no C12 . C11 . H111 . 122.2 no C7 . C12 . C11 . 121.08(15) yes C7 . C12 . H121 . 120.6 no C11 . C12 . H121 . 118.3 no C6 . C13 . C14 . 121.75(14) yes C6 . C13 . H131 . 118.7 no C14 . C13 . H131 . 119.6 no C13 . C14 . C15 . 119.72(14) yes C13 . C14 . H141 . 119.5 no C15 . C14 . H141 . 120.6 no C14 . C15 . C16 . 120.18(14) yes C14 . C15 . H151 . 120.1 no C16 . C15 . H151 . 119.7 no C5 . C16 . C15 . 121.62(14) yes C5 . C16 . H161 . 117.7 no C15 . C16 . H161 . 120.7 no C4 . C17 . C18 . 120.33(12) yes C4 . C17 . C28 . 120.98(12) yes C18 . C17 . C28 . 118.65(12) yes C17 . C18 . O19 . 123.31(12) yes C17 . C18 . C21 . 121.12(12) yes O19 . C18 . C21 . 115.19(11) yes C18 . O19 . B20 . 124.41(11) yes O2 . B20 . O2 5_655 100.47(15) yes O2 . B20 . O19 . 113.03(5) yes O2 5_655 B20 . O19 . 114.69(5) yes O2 . B20 . O19 5_655 114.69(5) yes O2 5_655 B20 . O19 5_655 113.03(5) yes O19 . B20 . O19 5_655 101.56(16) yes C18 . C21 . C22 . 120.04(12) yes C18 . C21 . C26 . 119.83(12) yes C22 . C21 . C26 . 120.03(12) yes C21 . C22 . C23 . 120.67(13) yes C21 . C22 . H221 . 120.6 no C23 . C22 . H221 . 118.7 no C22 . C23 . C24 . 119.37(14) yes C22 . C23 . H231 . 119.0 no C24 . C23 . H231 . 121.6 no C23 . C24 . C25 . 121.06(14) yes C23 . C24 . H241 . 120.7 no C25 . C24 . H241 . 118.2 no C24 . C25 . C26 . 120.85(14) yes C24 . C25 . H251 . 118.2 no C26 . C25 . H251 . 120.9 no C25 . C26 . C21 . 117.92(13) yes C25 . C26 . C27 . 123.13(13) yes C21 . C26 . C27 . 118.94(12) yes C26 . C27 . C28 . 119.07(12) yes C26 . C27 . C32 . 122.09(13) yes C28 . C27 . C32 . 118.81(13) yes C17 . C28 . C27 . 120.29(12) yes C17 . C28 . C29 . 121.50(12) yes C27 . C28 . C29 . 118.11(12) yes C28 . C29 . C30 . 121.59(14) yes C28 . C29 . H291 . 119.3 no C30 . C29 . H291 . 119.1 no C29 . C30 . C31 . 120.17(14) yes C29 . C30 . H301 . 122.6 no C31 . C30 . H301 . 117.2 no C30 . C31 . C32 . 119.58(14) yes C30 . C31 . H311 . 120.0 no C32 . C31 . H311 . 120.4 no C27 . C32 . C31 . 121.73(14) yes C27 . C32 . H321 . 118.9 no C31 . C32 . H321 . 119.3 no Na1 . O33 . C34 . 125.17(11) yes Na1 . O33 . C37 . 114.10(9) yes C34 . O33 . C37 . 108.59(12) yes O33 . C34 . C35 . 107.95(16) yes O33 . C34 . H342 . 108.6 no C35 . C34 . H342 . 113.7 no O33 . C34 . H341 . 108.4 no C35 . C34 . H341 . 109.9 no H342 . C34 . H341 . 108.2 no C34 . C35 . C36 . 103.27(17) yes C34 . C35 . H352 . 117.5 no C36 . C35 . H352 . 102.3 no C34 . C35 . H351 . 111.3 no C36 . C35 . H351 . 114.4 no H352 . C35 . H351 . 107.9 no C35 . C36 . C37 . 103.64(16) yes C35 . C36 . H362 . 105.5 no C37 . C36 . H362 . 108.8 no C35 . C36 . H361 . 109.8 no C37 . C36 . H361 . 117.8 no H362 . C36 . H361 . 110.4 no C36 . C37 . O33 . 106.52(14) yes C36 . C37 . H372 . 108.2 no O33 . C37 . H372 . 107.2 no C36 . C37 . H371 . 113.2 no O33 . C37 . H371 . 107.5 no H372 . C37 . H371 . 113.7 no Na1 . O38 . C39 . 119.28(10) yes Na1 . O38 . C42 . 132.70(11) yes C39 . O38 . C42 . 105.14(13) yes O38 . C39 . C40 . 105.57(15) yes O38 . C39 . H392 . 111.8 no C40 . C39 . H392 . 112.9 no O38 . C39 . H391 . 112.2 no C40 . C39 . H391 . 110.3 no H392 . C39 . H391 . 104.3 no C39 . C40 . C41 . 104.03(15) yes C39 . C40 . H402 . 109.5 no C41 . C40 . H402 . 113.3 no C39 . C40 . H401 . 116.0 no C41 . C40 . H401 . 111.3 no H402 . C40 . H401 . 103.1 no C40 . C41 . C42 . 104.52(14) yes C40 . C41 . H412 . 108.8 no C42 . C41 . H412 . 112.0 no C40 . C41 . H411 . 111.1 no C42 . C41 . H411 . 107.3 no H412 . C41 . H411 . 112.8 no C41 . C42 . O38 . 105.14(14) yes C41 . C42 . H422 . 111.6 no O38 . C42 . H422 . 107.1 no C41 . C42 . H421 . 110.6 no O38 . C42 . H421 . 110.0 no H422 . C42 . H421 . 112.1 no 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 C9 . H91 . O33 . 154 0.94 2.57 3.434(2) yes C41 . H411 . C6 5_645 173 1.00 2.50 3.500(2) yes _chemical_name_common . #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 796356' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 08-03-26 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5771 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 14.7887(2) _cell_length_b 14.5866(2) _cell_length_c 18.4806(3) _cell_angle_alpha 90 _cell_angle_beta 92.9658(5) _cell_angle_gamma 90 _cell_volume 3981.24(10) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' 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 = C36 H36 B1 I4 Na1 O10 # Dc = 1.95 Fooo = 2240.00 Mu = 31.95 M = 1170.09 # Found Formula = C36 H36 B1 I4 Na1 O10 # Dc = 1.95 FOOO = 2240.00 Mu = 31.95 M = 1170.09 _chemical_formula_sum 'C36 H36 B1 I4 Na1 O10' _chemical_formula_moiety 'C24 H12 B1 I4 O4, C12 H24 Na O6' _chemical_compound_source . _chemical_formula_weight 1170.09 _cell_measurement_reflns_used 9723 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.16 _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 3.195 # Sheldrick geometric approximatio 0.62 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.91 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 150 _diffrn_reflns_number 67704 _reflns_number_total 9426 _diffrn_reflns_av_R_equivalents 0.088 # Number of reflections with Friedels Law is 9426 # Number of reflections without Friedels Law is 18714 # Theoretical number of reflections is about 9490 _diffrn_reflns_theta_min 5.110 _diffrn_reflns_theta_max 27.870 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.870 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 2.48 _oxford_diffrn_Wilson_scale 312.22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.45 _refine_diff_density_max 2.14 # 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>-3.0\s(I) _refine_ls_number_reflns 9424 _refine_ls_number_restraints 0 _refine_ls_number_parameters 469 _oxford_refine_ls_R_factor_ref 0.0825 _refine_ls_wR_factor_ref 0.0845 _refine_ls_goodness_of_fit_ref 0.9318 _refine_ls_shift/su_max 0.000951 # The values computed from all data _oxford_reflns_number_all 9424 _refine_ls_R_factor_all 0.0825 _refine_ls_wR_factor_all 0.0845 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6020 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_gt 0.0728 # 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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.43P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.548501(19) 0.551007(19) 0.202743(16) 0.0271 1.0000 Uani . . . . . . . C2 C 0.4538(3) 0.4657(3) 0.1495(2) 0.0225 1.0000 Uani . . . . . . . C3 C 0.4177(3) 0.3912(3) 0.1863(2) 0.0178 1.0000 Uani . . . . . . . O4 O 0.44679(17) 0.37523(18) 0.25579(14) 0.0182 1.0000 Uani . . . . . . . B5 B 0.4915(3) 0.2873(3) 0.2720(3) 0.0198 1.0000 Uani . . . . . . . O6 O 0.52104(18) 0.29536(18) 0.34826(14) 0.0206 1.0000 Uani . . . . . . . C7 C 0.5578(3) 0.2204(3) 0.3818(2) 0.0184 1.0000 Uani . . . . . . . C8 C 0.6407(3) 0.1846(3) 0.3602(2) 0.0225 1.0000 Uani . . . . . . . C9 C 0.6742(3) 0.1052(3) 0.3949(2) 0.0285 1.0000 Uani . . . . . . . C10 C 0.6323(3) 0.0664(3) 0.4525(2) 0.0283 1.0000 Uani . . . . . . . C11 C 0.5555(3) 0.1075(3) 0.4779(2) 0.0290 1.0000 Uani . . . . . . . C12 C 0.5188(3) 0.1833(3) 0.4424(2) 0.0253 1.0000 Uani . . . . . . . I13 I 0.40175(2) 0.24365(2) 0.480105(17) 0.0359 1.0000 Uani . . . . . . . C14 C 0.6936(3) 0.2319(3) 0.3060(2) 0.0213 1.0000 Uani . . . . . . . C15 C 0.7876(3) 0.2349(3) 0.3178(2) 0.0238 1.0000 Uani . . . . . . . C16 C 0.8438(3) 0.2725(3) 0.2692(2) 0.0242 1.0000 Uani . . . . . . . C17 C 0.8073(3) 0.3071(3) 0.2039(2) 0.0282 1.0000 Uani . . . . . . . C18 C 0.7142(3) 0.3058(3) 0.1916(2) 0.0231 1.0000 Uani . . . . . . . C19 C 0.6547(3) 0.2712(3) 0.2411(2) 0.0190 1.0000 Uani . . . . . . . O20 O 0.56649(17) 0.2709(2) 0.22348(15) 0.0223 1.0000 Uani . . . . . . . I21 I 0.66304(2) 0.35000(2) 0.089536(16) 0.0325 1.0000 Uani . . . . . . . O22 O 0.43187(18) 0.20771(18) 0.25875(15) 0.0210 1.0000 Uani . . . . . . . C23 C 0.3424(3) 0.2074(3) 0.2410(2) 0.0222 1.0000 Uani . . . . . . . C24 C 0.2908(3) 0.1364(3) 0.2697(2) 0.0244 1.0000 Uani . . . . . . . I25 I 0.35410(2) 0.03461(2) 0.334351(18) 0.0368 1.0000 Uani . . . . . . . C26 C 0.1981(3) 0.1290(3) 0.2541(3) 0.0293 1.0000 Uani . . . . . . . C27 C 0.1555(3) 0.1920(3) 0.2070(3) 0.0322 1.0000 Uani . . . . . . . C28 C 0.2059(3) 0.2592(3) 0.1765(2) 0.0264 1.0000 Uani . . . . . . . C29 C 0.2996(3) 0.2679(3) 0.1918(2) 0.0205 1.0000 Uani . . . . . . . C30 C 0.3482(3) 0.3392(3) 0.1522(2) 0.0187 1.0000 Uani . . . . . . . C31 C 0.3221(3) 0.3588(3) 0.0794(2) 0.0247 1.0000 Uani . . . . . . . C32 C 0.3617(3) 0.4304(3) 0.0429(3) 0.0312 1.0000 Uani . . . . . . . C33 C 0.4255(3) 0.4852(3) 0.0776(2) 0.0261 1.0000 Uani . . . . . . . Na34 Na 0.13746(11) 0.44952(11) 0.50981(9) 0.0271 1.0000 Uani . . . . . . . O35 O 0.0787(2) 0.4364(2) 0.63070(15) 0.0283 1.0000 Uani . . . . . . . C36 C -0.0166(3) 0.4456(3) 0.6431(2) 0.0276 1.0000 Uani . . . . . . . C37 C -0.0688(3) 0.3806(3) 0.5933(2) 0.0288 1.0000 Uani . . . . . . . O38 O -0.06156(19) 0.41114(19) 0.51979(15) 0.0241 1.0000 Uani . . . . . . . C39 C -0.0891(3) 0.3419(3) 0.4689(2) 0.0272 1.0000 Uani . . . . . . . C40 C -0.0140(3) 0.2752(3) 0.4564(3) 0.0269 1.0000 Uani . . . . . . . O41 O 0.05963(19) 0.32618(19) 0.43190(16) 0.0273 1.0000 Uani . . . . . . . C42 C 0.1248(3) 0.2709(3) 0.3985(3) 0.0286 1.0000 Uani . . . . . . . C43 C 0.1869(3) 0.3340(3) 0.3597(2) 0.0310 1.0000 Uani . . . . . . . O44 O 0.2281(2) 0.39589(19) 0.41107(16) 0.0274 1.0000 Uani . . . . . . . C45 C 0.2900(3) 0.4559(3) 0.3752(3) 0.0318 1.0000 Uani . . . . . . . C46 C 0.3463(3) 0.5056(3) 0.4316(3) 0.0339 1.0000 Uani . . . . . . . O47 O 0.2886(2) 0.5615(2) 0.47200(17) 0.0323 1.0000 Uani . . . . . . . C48 C 0.3340(3) 0.5979(3) 0.5359(3) 0.0398 1.0000 Uani . . . . . . . C49 C 0.3340(3) 0.5327(3) 0.5974(3) 0.0401 1.0000 Uani . . . . . . . O50 O 0.2426(2) 0.5107(2) 0.60881(18) 0.0372 1.0000 Uani . . . . . . . C51 C 0.2286(3) 0.4635(4) 0.6750(3) 0.0383 1.0000 Uani . . . . . . . C52 C 0.1314(3) 0.4707(3) 0.6901(3) 0.0377 1.0000 Uani . . . . . . . H91 H 0.7259 0.0776 0.3775 0.0340 1.0000 Uiso R . . . . . . H101 H 0.6555 0.0137 0.4750 0.0341 1.0000 Uiso R . . . . . . H111 H 0.5279 0.0838 0.5179 0.0360 1.0000 Uiso R . . . . . . H151 H 0.8125 0.2099 0.3607 0.0301 1.0000 Uiso R . . . . . . H161 H 0.9060 0.2748 0.2800 0.0311 1.0000 Uiso R . . . . . . H171 H 0.8445 0.3301 0.1690 0.0322 1.0000 Uiso R . . . . . . H261 H 0.1653 0.0817 0.2742 0.0330 1.0000 Uiso R . . . . . . H271 H 0.0924 0.1895 0.1979 0.0391 1.0000 Uiso R . . . . . . H281 H 0.1770 0.3003 0.1437 0.0341 1.0000 Uiso R . . . . . . H311 H 0.2770 0.3233 0.0558 0.0300 1.0000 Uiso R . . . . . . H321 H 0.3437 0.4411 -0.0058 0.0379 1.0000 Uiso R . . . . . . H331 H 0.4512 0.5342 0.0537 0.0310 1.0000 Uiso R . . . . . . H361 H -0.0277 0.4309 0.6933 0.0352 1.0000 Uiso R . . . . . . H362 H -0.0357 0.5085 0.6327 0.0352 1.0000 Uiso R . . . . . . H371 H -0.1319 0.3785 0.6056 0.0372 1.0000 Uiso R . . . . . . H372 H -0.0425 0.3197 0.5987 0.0369 1.0000 Uiso R . . . . . . H391 H -0.1408 0.3088 0.4869 0.0322 1.0000 Uiso R . . . . . . H392 H -0.1063 0.3711 0.4229 0.0319 1.0000 Uiso R . . . . . . H401 H 0.0037 0.2446 0.5019 0.0348 1.0000 Uiso R . . . . . . H402 H -0.0337 0.2292 0.4206 0.0352 1.0000 Uiso R . . . . . . H421 H 0.1602 0.2362 0.4350 0.0368 1.0000 Uiso R . . . . . . H422 H 0.0946 0.2290 0.3641 0.0371 1.0000 Uiso R . . . . . . H431 H 0.1514 0.3681 0.3228 0.0390 1.0000 Uiso R . . . . . . H432 H 0.2335 0.2984 0.3373 0.0391 1.0000 Uiso R . . . . . . H451 H 0.2558 0.4998 0.3450 0.0441 1.0000 Uiso R . . . . . . H452 H 0.3288 0.4191 0.3457 0.0442 1.0000 Uiso R . . . . . . H461 H 0.3900 0.5443 0.4085 0.0470 1.0000 Uiso R . . . . . . H462 H 0.3773 0.4611 0.4633 0.0469 1.0000 Uiso R . . . . . . H481 H 0.3020 0.6530 0.5495 0.0481 1.0000 Uiso R . . . . . . H482 H 0.3960 0.6140 0.5262 0.0480 1.0000 Uiso R . . . . . . H491 H 0.3623 0.5604 0.6409 0.0492 1.0000 Uiso R . . . . . . H492 H 0.3668 0.4775 0.5856 0.0490 1.0000 Uiso R . . . . . . H511 H 0.2651 0.4912 0.7141 0.0491 1.0000 Uiso R . . . . . . H512 H 0.2455 0.3995 0.6702 0.0490 1.0000 Uiso R . . . . . . H521 H 0.1171 0.5353 0.6971 0.0431 1.0000 Uiso R . . . . . . H522 H 0.1190 0.4355 0.7331 0.0428 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 I1 0.02232(15) 0.02366(15) 0.03512(18) 0.00422(13) -0.00186(12) -0.00367(13) C2 0.023(2) 0.017(2) 0.027(2) 0.0082(18) -0.0022(18) 0.0053(19) C3 0.019(2) 0.018(2) 0.017(2) -0.0006(17) 0.0028(17) 0.0078(18) O4 0.0217(15) 0.0163(14) 0.0165(15) 0.0021(12) 0.0009(12) 0.0013(12) B5 0.020(2) 0.019(2) 0.021(3) 0.000(2) -0.003(2) -0.003(2) O6 0.0253(16) 0.0207(15) 0.0158(15) 0.0030(12) 0.0030(12) 0.0035(13) C7 0.024(2) 0.0145(19) 0.016(2) -0.0003(16) -0.0065(17) -0.0048(18) C8 0.023(2) 0.022(2) 0.023(2) -0.0038(18) -0.0033(18) -0.002(2) C9 0.022(2) 0.030(3) 0.033(3) 0.000(2) 0.000(2) 0.002(2) C10 0.036(3) 0.019(2) 0.029(3) 0.0047(19) -0.006(2) 0.001(2) C11 0.034(3) 0.030(2) 0.022(2) -0.002(2) -0.003(2) -0.010(2) C12 0.026(2) 0.025(2) 0.025(2) 0.0061(19) 0.0018(19) -0.001(2) I13 0.03499(18) 0.03939(19) 0.03456(19) 0.00407(15) 0.01386(14) 0.00483(15) C14 0.018(2) 0.022(2) 0.024(2) -0.0029(18) 0.0004(17) 0.0003(19) C15 0.021(2) 0.026(2) 0.023(2) -0.0012(19) -0.0095(18) 0.000(2) C16 0.015(2) 0.031(2) 0.025(2) -0.001(2) -0.0060(18) 0.001(2) C17 0.024(2) 0.031(2) 0.030(3) -0.001(2) 0.010(2) 0.000(2) C18 0.022(2) 0.023(2) 0.024(2) 0.0016(19) 0.0046(18) 0.0023(19) C19 0.018(2) 0.021(2) 0.018(2) 0.0006(17) 0.0017(17) 0.0014(19) O20 0.0156(14) 0.0322(16) 0.0194(15) -0.0004(13) 0.0020(12) 0.0017(13) I21 0.02925(17) 0.0455(2) 0.02321(16) 0.00600(14) 0.00501(12) 0.00227(15) O22 0.0164(15) 0.0171(14) 0.0295(17) 0.0022(13) 0.0020(12) -0.0028(13) C23 0.022(2) 0.022(2) 0.024(2) -0.0036(19) 0.0092(18) -0.007(2) C24 0.025(2) 0.025(2) 0.023(2) -0.0012(19) 0.0033(18) 0.001(2) I25 0.0502(2) 0.02588(16) 0.03457(19) 0.00697(14) 0.00436(15) -0.00910(15) C26 0.031(3) 0.022(2) 0.036(3) -0.003(2) 0.012(2) -0.010(2) C27 0.017(2) 0.033(3) 0.048(3) -0.014(2) 0.004(2) -0.003(2) C28 0.020(2) 0.029(2) 0.031(3) -0.007(2) -0.0009(19) -0.001(2) C29 0.014(2) 0.019(2) 0.028(2) -0.0010(18) -0.0018(17) -0.0015(18) C30 0.013(2) 0.018(2) 0.026(2) -0.0011(17) 0.0054(16) 0.0060(18) C31 0.018(2) 0.028(2) 0.028(3) -0.004(2) -0.0034(18) 0.004(2) C32 0.030(3) 0.036(3) 0.029(3) 0.001(2) 0.008(2) 0.005(2) C33 0.026(2) 0.026(2) 0.027(2) 0.009(2) 0.0031(19) -0.002(2) Na34 0.0313(10) 0.0245(9) 0.0258(9) -0.0010(7) 0.0029(7) 0.0028(8) O35 0.0362(18) 0.0322(17) 0.0166(16) 0.0005(13) 0.0029(13) -0.0005(15) C36 0.033(3) 0.030(2) 0.020(2) -0.0009(19) 0.0079(19) 0.001(2) C37 0.034(3) 0.033(3) 0.021(2) 0.002(2) 0.0092(19) -0.007(2) O38 0.0284(17) 0.0189(15) 0.0252(17) 0.0000(13) 0.0030(13) -0.0027(14) C39 0.025(2) 0.027(2) 0.029(3) 0.002(2) 0.0061(19) -0.003(2) C40 0.028(2) 0.019(2) 0.035(3) -0.0012(19) 0.004(2) -0.001(2) O41 0.0282(17) 0.0168(14) 0.0376(19) -0.0043(13) 0.0098(14) -0.0014(14) C42 0.035(3) 0.022(2) 0.030(3) -0.003(2) 0.007(2) 0.004(2) C43 0.035(3) 0.031(3) 0.027(3) -0.009(2) 0.001(2) -0.001(2) O44 0.0313(17) 0.0266(16) 0.0248(17) 0.0003(13) 0.0080(13) -0.0026(14) C45 0.034(3) 0.028(2) 0.036(3) 0.001(2) 0.020(2) -0.005(2) C46 0.029(3) 0.029(2) 0.045(3) -0.002(2) 0.016(2) -0.004(2) O47 0.0282(17) 0.0291(17) 0.040(2) -0.0029(15) 0.0025(14) -0.0014(15) C48 0.027(3) 0.038(3) 0.053(3) -0.005(3) -0.008(2) -0.008(2) C49 0.030(3) 0.039(3) 0.051(3) -0.007(3) -0.005(2) -0.003(2) O50 0.0318(18) 0.0392(19) 0.040(2) 0.0076(16) -0.0085(15) -0.0062(16) C51 0.038(3) 0.043(3) 0.033(3) 0.010(2) -0.015(2) -0.003(3) C52 0.050(3) 0.035(3) 0.027(3) 0.000(2) -0.008(2) 0.000(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.057184(6) 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 I1 . C2 . 2.082(4) yes C2 . C3 . 1.403(6) yes C2 . C33 . 1.401(6) yes C3 . O4 . 1.353(5) yes C3 . C30 . 1.401(6) yes O4 . B5 . 1.467(5) yes B5 . O6 . 1.459(5) yes B5 . O20 . 1.481(6) yes B5 . O22 . 1.470(5) yes O6 . C7 . 1.356(5) yes C7 . C8 . 1.409(6) yes C7 . C12 . 1.396(6) yes C8 . C9 . 1.402(6) yes C8 . C14 . 1.474(6) yes C9 . C10 . 1.381(6) yes C9 . H91 . 0.936 no C10 . C11 . 1.387(6) yes C10 . H101 . 0.931 no C11 . C12 . 1.382(6) yes C11 . H111 . 0.930 no C12 . I13 . 2.094(4) yes C14 . C15 . 1.395(5) yes C14 . C19 . 1.424(6) yes C15 . C16 . 1.370(6) yes C15 . H151 . 0.932 no C16 . C17 . 1.390(6) yes C16 . H161 . 0.933 no C17 . C18 . 1.383(6) yes C17 . H171 . 0.932 no C18 . C19 . 1.397(6) yes C18 . I21 . 2.097(4) yes C19 . O20 . 1.328(4) yes O22 . C23 . 1.346(5) yes C23 . C24 . 1.407(6) yes C23 . C29 . 1.396(6) yes C24 . I25 . 2.096(4) yes C24 . C26 . 1.389(6) yes C26 . C27 . 1.394(6) yes C26 . H261 . 0.931 no C27 . C28 . 1.371(6) yes C27 . H271 . 0.941 no C28 . C29 . 1.405(5) yes C28 . H281 . 0.939 no C29 . C30 . 1.479(6) yes C30 . C31 . 1.409(6) yes C31 . C32 . 1.389(6) yes C31 . H311 . 0.935 no C32 . C33 . 1.370(6) yes C32 . H321 . 0.938 no C33 . H331 . 0.931 no Na34 . O38 2_566 2.372(3) yes Na34 . O35 . 2.446(3) yes Na34 . O41 . 2.542(3) yes Na34 . O44 . 2.448(3) yes Na34 . O50 . 2.503(3) yes O35 . C36 . 1.446(5) yes O35 . C52 . 1.405(5) yes C36 . C37 . 1.507(6) yes C36 . H361 . 0.975 no C36 . H362 . 0.975 no C37 . O38 . 1.439(5) yes C37 . H371 . 0.972 no C37 . H372 . 0.971 no O38 . C39 . 1.425(5) yes C39 . C40 . 1.503(6) yes C39 . H391 . 0.977 no C39 . H392 . 0.974 no C40 . O41 . 1.412(5) yes C40 . H401 . 0.976 no C40 . H402 . 0.977 no O41 . C42 . 1.422(5) yes C42 . C43 . 1.508(6) yes C42 . H421 . 0.974 no C42 . H422 . 0.973 no C43 . O44 . 1.424(5) yes C43 . H431 . 0.974 no C43 . H432 . 0.973 no O44 . C45 . 1.452(5) yes C45 . C46 . 1.488(6) yes C45 . H451 . 0.974 no C45 . H452 . 0.973 no C46 . O47 . 1.420(5) yes C46 . H461 . 0.972 no C46 . H462 . 0.974 no O47 . C48 . 1.431(5) yes C48 . C49 . 1.482(7) yes C48 . H481 . 0.972 no C48 . H482 . 0.972 no C49 . O50 . 1.416(6) yes C49 . H491 . 0.974 no C49 . H492 . 0.972 no O50 . C51 . 1.427(6) yes C51 . C52 . 1.482(7) yes C51 . H511 . 0.969 no C51 . H512 . 0.972 no C52 . H521 . 0.975 no C52 . H522 . 0.972 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 I1 . C2 . C3 . 119.8(3) yes I1 . C2 . C33 . 119.2(3) yes C3 . C2 . C33 . 121.0(4) yes C2 . C3 . O4 . 118.9(4) yes C2 . C3 . C30 . 119.3(4) yes O4 . C3 . C30 . 121.6(4) yes C3 . O4 . B5 . 117.5(3) yes O4 . B5 . O6 . 103.6(3) yes O4 . B5 . O20 . 111.1(3) yes O6 . B5 . O20 . 113.7(3) yes O4 . B5 . O22 . 113.4(3) yes O6 . B5 . O22 . 111.8(3) yes O20 . B5 . O22 . 103.5(3) yes B5 . O6 . C7 . 118.0(3) yes O6 . C7 . C8 . 120.3(4) yes O6 . C7 . C12 . 120.4(4) yes C8 . C7 . C12 . 119.0(4) yes C7 . C8 . C9 . 118.0(4) yes C7 . C8 . C14 . 121.3(4) yes C9 . C8 . C14 . 120.6(4) yes C8 . C9 . C10 . 122.0(4) yes C8 . C9 . H91 . 118.4 no C10 . C9 . H91 . 119.6 no C9 . C10 . C11 . 119.4(4) yes C9 . C10 . H101 . 120.9 no C11 . C10 . H101 . 119.7 no C10 . C11 . C12 . 119.5(4) yes C10 . C11 . H111 . 120.6 no C12 . C11 . H111 . 119.8 no C7 . C12 . C11 . 121.6(4) yes C7 . C12 . I13 . 119.1(3) yes C11 . C12 . I13 . 119.3(3) yes C8 . C14 . C15 . 117.9(4) yes C8 . C14 . C19 . 123.7(4) yes C15 . C14 . C19 . 118.3(4) yes C14 . C15 . C16 . 122.9(4) yes C14 . C15 . H151 . 117.9 no C16 . C15 . H151 . 119.2 no C15 . C16 . C17 . 119.5(4) yes C15 . C16 . H161 . 120.0 no C17 . C16 . H161 . 120.5 no C16 . C17 . C18 . 118.4(4) yes C16 . C17 . H171 . 121.0 no C18 . C17 . H171 . 120.6 no C17 . C18 . C19 . 123.6(4) yes C17 . C18 . I21 . 117.0(3) yes C19 . C18 . I21 . 119.3(3) yes C14 . C19 . C18 . 117.1(4) yes C14 . C19 . O20 . 123.7(4) yes C18 . C19 . O20 . 119.0(4) yes B5 . O20 . C19 . 127.4(3) yes B5 . O22 . C23 . 128.1(3) yes O22 . C23 . C24 . 117.2(4) yes O22 . C23 . C29 . 124.3(3) yes C24 . C23 . C29 . 118.3(4) yes C23 . C24 . I25 . 120.0(3) yes C23 . C24 . C26 . 121.9(4) yes I25 . C24 . C26 . 118.0(3) yes C24 . C26 . C27 . 119.1(4) yes C24 . C26 . H261 . 120.3 no C27 . C26 . H261 . 120.6 no C26 . C27 . C28 . 119.4(4) yes C26 . C27 . H271 . 119.9 no C28 . C27 . H271 . 120.7 no C27 . C28 . C29 . 122.2(4) yes C27 . C28 . H281 . 118.9 no C29 . C28 . H281 . 118.9 no C28 . C29 . C23 . 118.9(4) yes C28 . C29 . C30 . 117.6(4) yes C23 . C29 . C30 . 123.5(3) yes C29 . C30 . C3 . 121.4(4) yes C29 . C30 . C31 . 119.9(4) yes C3 . C30 . C31 . 118.6(4) yes C30 . C31 . C32 . 121.0(4) yes C30 . C31 . H311 . 119.1 no C32 . C31 . H311 . 119.9 no C31 . C32 . C33 . 120.5(4) yes C31 . C32 . H321 . 119.0 no C33 . C32 . H321 . 120.5 no C2 . C33 . C32 . 119.4(4) yes C2 . C33 . H331 . 119.7 no C32 . C33 . H331 . 120.9 no O38 2_566 Na34 . O35 . 95.27(11) yes O38 2_566 Na34 . O41 . 106.31(11) yes O35 . Na34 . O41 . 106.86(11) yes O38 2_566 Na34 . O44 . 111.89(12) yes O35 . Na34 . O44 . 152.85(12) yes O41 . Na34 . O44 . 66.49(10) yes O38 2_566 Na34 . O50 . 97.58(12) yes O35 . Na34 . O50 . 66.22(11) yes O41 . Na34 . O50 . 155.78(12) yes O44 . Na34 . O50 . 108.38(12) yes Na34 . O35 . C36 . 122.2(2) yes Na34 . O35 . C52 . 118.4(3) yes C36 . O35 . C52 . 110.4(3) yes O35 . C36 . C37 . 108.5(3) yes O35 . C36 . H361 . 110.2 no C37 . C36 . H361 . 109.6 no O35 . C36 . H362 . 109.4 no C37 . C36 . H362 . 109.7 no H361 . C36 . H362 . 109.4 no C36 . C37 . O38 . 108.7(3) yes C36 . C37 . H371 . 110.1 no O38 . C37 . H371 . 110.4 no C36 . C37 . H372 . 108.9 no O38 . C37 . H372 . 109.3 no H371 . C37 . H372 . 109.4 no Na34 2_566 O38 . C37 . 115.2(3) yes Na34 2_566 O38 . C39 . 109.8(2) yes C37 . O38 . C39 . 111.8(3) yes O38 . C39 . C40 . 111.8(3) yes O38 . C39 . H391 . 109.1 no C40 . C39 . H391 . 109.2 no O38 . C39 . H392 . 108.6 no C40 . C39 . H392 . 108.2 no H391 . C39 . H392 . 109.9 no C39 . C40 . O41 . 107.3(3) yes C39 . C40 . H401 . 109.4 no O41 . C40 . H401 . 109.9 no C39 . C40 . H402 . 110.6 no O41 . C40 . H402 . 110.6 no H401 . C40 . H402 . 109.1 no C40 . O41 . Na34 . 121.6(2) yes C40 . O41 . C42 . 113.1(3) yes Na34 . O41 . C42 . 110.5(2) yes O41 . C42 . C43 . 107.6(3) yes O41 . C42 . H421 . 110.3 no C43 . C42 . H421 . 109.1 no O41 . C42 . H422 . 109.9 no C43 . C42 . H422 . 110.0 no H421 . C42 . H422 . 109.8 no C42 . C43 . O44 . 108.7(4) yes C42 . C43 . H431 . 109.0 no O44 . C43 . H431 . 109.9 no C42 . C43 . H432 . 109.8 no O44 . C43 . H432 . 109.4 no H431 . C43 . H432 . 110.1 no C43 . O44 . Na34 . 117.9(2) yes C43 . O44 . C45 . 109.6(3) yes Na34 . O44 . C45 . 122.0(2) yes O44 . C45 . C46 . 108.5(4) yes O44 . C45 . H451 . 109.7 no C46 . C45 . H451 . 109.6 no O44 . C45 . H452 . 109.1 no C46 . C45 . H452 . 109.7 no H451 . C45 . H452 . 110.2 no C45 . C46 . O47 . 108.5(4) yes C45 . C46 . H461 . 109.6 no O47 . C46 . H461 . 109.2 no C45 . C46 . H462 . 109.0 no O47 . C46 . H462 . 110.0 no H461 . C46 . H462 . 110.4 no C46 . O47 . C48 . 112.2(4) yes O47 . C48 . C49 . 112.1(4) yes O47 . C48 . H481 . 107.8 no C49 . C48 . H481 . 108.3 no O47 . C48 . H482 . 110.1 no C49 . C48 . H482 . 109.6 no H481 . C48 . H482 . 109.0 no C48 . C49 . O50 . 107.3(4) yes C48 . C49 . H491 . 110.4 no O50 . C49 . H491 . 110.2 no C48 . C49 . H492 . 109.8 no O50 . C49 . H492 . 109.7 no H491 . C49 . H492 . 109.4 no C49 . O50 . Na34 . 122.3(3) yes C49 . O50 . C51 . 114.7(4) yes Na34 . O50 . C51 . 110.0(3) yes O50 . C51 . C52 . 108.2(4) yes O50 . C51 . H511 . 109.8 no C52 . C51 . H511 . 109.8 no O50 . C51 . H512 . 109.6 no C52 . C51 . H512 . 110.0 no H511 . C51 . H512 . 109.4 no C51 . C52 . O35 . 109.4(4) yes C51 . C52 . H521 . 108.3 no O35 . C52 . H521 . 109.5 no C51 . C52 . H522 . 110.0 no O35 . C52 . H522 . 109.2 no H521 . C52 . H522 . 110.5 no 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 C36 . H361 . O22 4_455 135 0.98 2.45 3.213(6) yes C45 . H452 . O4 . 161 0.97 2.55 3.487(6) yes _chemical_name_common . #============================================================================== data_8 _database_code_depnum_ccdc_archive 'CCDC 796357' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _audit_creation_date 08-02-19 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5714 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 11.3796(2) _cell_length_b 21.7120(4) _cell_length_c 12.3028(2) _cell_angle_alpha 90 _cell_angle_beta 116.3450(8) _cell_angle_gamma 90 _cell_volume 2723.99(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' 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 = C24 H14 B1 I2 Na1 O4 # Dc = 1.59 Fooo = 1408.00 Mu = 23.49 M = 1307.97 # Found Formula = C28 H22 B1 I2 Na1 O5 # Dc = 1.77 FOOO = 1408.00 Mu = 23.61 M = 1452.18 _chemical_formula_sum 'C28 H22 B1 I2 Na1 O5' _chemical_formula_moiety 'C28 H22 B1 I2 Na1 O5' _chemical_compound_source . _chemical_formula_weight 726.09 _cell_measurement_reflns_used 6241 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.44 _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.361 # Sheldrick geometric approximatio 0.91 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.93 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # 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 150 _diffrn_reflns_number 36816 _reflns_number_total 11234 _diffrn_reflns_av_R_equivalents 0.064 # Number of reflections with Friedels Law is 6334 # Number of reflections without Friedels Law is 11234 # Theoretical number of reflections is about 6219 _diffrn_reflns_theta_min 5.096 _diffrn_reflns_theta_max 27.438 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.438 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min -28 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 3.76 _oxford_diffrn_Wilson_scale 38.73 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.13 _refine_diff_density_max 1.84 # 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>-3.0\s(I) _refine_ls_number_reflns 11224 _refine_ls_number_restraints 11 _refine_ls_number_parameters 659 _oxford_refine_ls_R_factor_ref 0.0695 _refine_ls_wR_factor_ref 0.1098 _refine_ls_goodness_of_fit_ref 0.9593 _refine_ls_shift/su_max 0.000526 # The values computed from all data _oxford_reflns_number_all 11224 _refine_ls_R_factor_all 0.0695 _refine_ls_wR_factor_all 0.1098 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8712 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_gt 0.0977 _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_abs_structure_details 'Flack (1983), 4900 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 noref # 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^) + ( 0.04P)^2^ + 8.57P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 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. 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. 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.41639(5) 0.68230(5) 0.11639(5) 0.0502 1.0000 Uani . . . . . . . C2 C 0.2815(7) 0.6565(3) 0.1784(6) 0.0376 1.0000 Uani . . . . . . . C3 C 0.1471(7) 0.6676(3) 0.1102(5) 0.0315 1.0000 Uani . . . . . . . O4 O 0.1035(4) 0.6929(2) -0.0042(4) 0.0331 1.0000 Uani . . . . . . . Na5 Na 0.1051(3) 0.78894(14) -0.0858(2) 0.0390 1.0000 Uani . . . . . . . O6 O -0.0268(5) 0.7085(2) -0.2028(4) 0.0314 1.0000 Uani . . . . . . . B7 B 0.0070(8) 0.6597(4) -0.1101(7) 0.0342 1.0000 Uani . . . . . . . O8 O -0.1066(5) 0.6382(2) -0.0938(4) 0.0367 1.0000 Uani . . . . . . . Na9 Na -0.1171(3) 0.53466(15) -0.1395(2) 0.0498 1.0000 Uani . . . . . . . O10 O 0.0500(5) 0.6030(2) -0.1423(5) 0.0406 1.0000 Uani . . . . . . . C11 C 0.1394(7) 0.6039(4) -0.1902(7) 0.0408 1.0000 Uani . . . . . . . C12 C 0.1085(8) 0.6302(4) -0.3017(8) 0.0505 1.0000 Uani . . . . . . . C13 C -0.0201(7) 0.6596(4) -0.3739(7) 0.0381 1.0000 Uani . . . . . . . C14 C -0.0825(7) 0.6964(3) -0.3235(5) 0.0327 1.0000 Uani . . . . . . . C15 C -0.2007(8) 0.7253(4) -0.4011(7) 0.0444 1.0000 Uani . . . . . . . I16 I -0.28233(6) 0.78931(5) -0.32795(5) 0.0578 1.0000 Uani . . . . . . . C17 C -0.2577(8) 0.7143(4) -0.5254(6) 0.0465 1.0000 Uani . . . . . . . C18 C -0.2017(9) 0.6761(4) -0.5766(7) 0.0518 1.0000 Uani . . . . . . . C19 C -0.0826(9) 0.6488(4) -0.5018(7) 0.0505 1.0000 Uani . . . . . . . C20 C 0.1986(10) 0.6263(6) -0.3492(9) 0.0687 1.0000 Uani . . . . . . . C21 C 0.3158(10) 0.5947(6) -0.2864(10) 0.0790 1.0000 Uani . . . . . . . C22 C 0.3433(9) 0.5662(6) -0.1793(11) 0.0766 1.0000 Uani . . . . . . . C23 C 0.2544(9) 0.5700(5) -0.1293(8) 0.0647 1.0000 Uani . . . . . . . O24 O -0.1100(4) 0.4749(2) 0.0269(4) 0.0330 1.0000 Uani . . . . . . . C25 C -0.0569(7) 0.4787(3) 0.1503(6) 0.0316 1.0000 Uani . . . . . . . C26 C 0.0758(7) 0.4626(3) 0.2224(6) 0.0373 1.0000 Uani . . . . . . . C27 C 0.1566(6) 0.4401(4) 0.1655(6) 0.0354 1.0000 Uani . . . . . . . C28 C 0.1131(7) 0.3960(3) 0.0762(6) 0.0351 1.0000 Uani . . . . . . . O29 O -0.0129(4) 0.3724(2) 0.0352(4) 0.0340 1.0000 Uani . . . . . . . B30 B -0.1257(7) 0.4116(4) -0.0279(6) 0.0293 1.0000 Uani . . . . . . . O31 O -0.1513(5) 0.4279(2) -0.1519(4) 0.0352 1.0000 Uani . . . . . . . C32 C -0.1673(8) 0.3801(3) -0.2299(6) 0.0409 1.0000 Uani . . . . . . . C33 C -0.2725(9) 0.3398(4) -0.2627(7) 0.0477 1.0000 Uani . . . . . . . C34 C -0.2810(10) 0.2905(4) -0.3378(7) 0.0584 1.0000 Uani . . . . . . . C35 C -0.1916(12) 0.2829(4) -0.3840(8) 0.0683 1.0000 Uani . . . . . . . C36 C -0.0936(11) 0.3242(5) -0.3597(7) 0.0646 1.0000 Uani . . . . . . . C37 C -0.0798(9) 0.3753(4) -0.2841(7) 0.0462 1.0000 Uani . . . . . . . I38 I 0.05134(6) 0.44618(5) -0.26081(5) 0.0546 1.0000 Uani . . . . . . . C39 C -0.3785(8) 0.3529(4) -0.2283(7) 0.0450 1.0000 Uani . . . . . . . C40 C -0.3558(8) 0.3741(3) -0.1139(7) 0.0415 1.0000 Uani . . . . . . . O41 O -0.2314(5) 0.3762(2) -0.0210(4) 0.0372 1.0000 Uani . . . . . . . C42 C -0.4595(8) 0.3880(4) -0.0870(8) 0.0514 1.0000 Uani . . . . . . . C43 C -0.5882(9) 0.3840(5) -0.1770(10) 0.0639 1.0000 Uani . . . . . . . C44 C -0.6137(9) 0.3636(5) -0.2919(10) 0.0724 1.0000 Uani . . . . . . . C45 C -0.5123(10) 0.3483(4) -0.3174(8) 0.0600 1.0000 Uani . . . . . . . C46 C 0.1949(8) 0.3681(4) 0.0335(7) 0.0479 1.0000 Uani . . . . . . . C47 C 0.3226(8) 0.3887(5) 0.0759(8) 0.0548 1.0000 Uani . . . . . . . C48 C 0.3695(8) 0.4356(5) 0.1612(8) 0.0575 1.0000 Uani . . . . . . . C49 C 0.2876(8) 0.4614(4) 0.2056(8) 0.0514 1.0000 Uani . . . . . . . C50 C 0.1274(8) 0.4674(4) 0.3480(7) 0.0427 1.0000 Uani . . . . . . . C51 C 0.0534(9) 0.4902(4) 0.4032(7) 0.0487 1.0000 Uani . . . . . . . C52 C -0.0745(9) 0.5079(4) 0.3323(8) 0.0511 1.0000 Uani . . . . . . . C53 C -0.1292(8) 0.5032(4) 0.2064(7) 0.0444 1.0000 Uani . . . . . . . I54 I -0.31712(5) 0.53835(5) 0.10400(5) 0.0533 1.0000 Uani . . . . . . . C60 C -0.1551(7) 0.6698(3) -0.0253(6) 0.0341 1.0000 Uani . . . . . . . C61 C -0.2872(7) 0.6877(4) -0.0805(7) 0.0468 1.0000 Uani . . . . . . . C62 C -0.3390(8) 0.7163(4) -0.0131(8) 0.0521 1.0000 Uani . . . . . . . C63 C -0.2628(9) 0.7288(4) 0.1078(9) 0.0540 1.0000 Uani . . . . . . . C64 C -0.1358(8) 0.7092(4) 0.1627(7) 0.0438 1.0000 Uani . . . . . . . C65 C -0.0775(7) 0.6793(3) 0.0977(6) 0.0357 1.0000 Uani . . . . . . . C66 C 0.0595(7) 0.6585(3) 0.1600(6) 0.0330 1.0000 Uani . . . . . . . C67 C 0.1081(8) 0.6317(4) 0.2770(6) 0.0427 1.0000 Uani . . . . . . . C68 C 0.2407(9) 0.6184(4) 0.3420(7) 0.0488 1.0000 Uani . . . . . . . C69 C 0.3266(8) 0.6313(4) 0.2943(7) 0.0461 1.0000 Uani . . . . . . . O70 O 0.1849(6) 0.7953(3) -0.2257(5) 0.0512 1.0000 Uani . . . . . . . C71 C 0.1409(10) 0.8422(5) -0.3155(9) 0.0650 1.0000 Uani . . . . . . . C72 C 0.2609(11) 0.8665(5) -0.3226(9) 0.0644 1.0000 Uani . . . . . . . C73 C 0.3519(10) 0.8104(5) -0.2857(9) 0.0661 1.0000 Uani . . . . . . . C74 C 0.3199(10) 0.7791(5) -0.1929(9) 0.0701 1.0000 Uani . . . . . . . O550 O -0.3394(12) 0.5446(5) -0.3177(9) 0.050(3) 0.5000 Uiso D . . . 1 . . C560 C -0.4385(19) 0.4979(10) -0.3891(18) 0.069(4) 0.5000 Uiso D . . . 1 . . C570 C -0.407(2) 0.4680(9) -0.4845(18) 0.062(4) 0.5000 Uiso D . . . 1 . . C580 C -0.343(3) 0.5216(10) -0.509(2) 0.083(4) 0.5000 Uiso D . . . 1 . . C590 C -0.330(2) 0.5731(9) -0.4224(14) 0.069(4) 0.5000 Uiso D . . . 1 . . O551 O -0.2892(11) 0.5374(6) -0.3285(9) 0.047(3) 0.5000 Uiso D . . . 2 . . C561 C -0.4158(17) 0.5069(11) -0.3509(18) 0.069(4) 0.5000 Uiso D . . . 2 . . C571 C -0.433(2) 0.4758(10) -0.4673(17) 0.062(4) 0.5000 Uiso D . . . 2 . . C581 C -0.372(3) 0.5082(12) -0.535(2) 0.083(4) 0.5000 Uiso D . . . 2 . . C591 C -0.287(2) 0.5541(9) -0.4421(13) 0.069(4) 0.5000 Uiso D . . . 2 . . H171 H -0.3371 0.7333 -0.5746 0.0518 1.0000 Uiso . . . . . . . H181 H -0.2406 0.6686 -0.6598 0.0628 1.0000 Uiso . . . . . . . H191 H -0.0429 0.6220 -0.5348 0.0628 1.0000 Uiso . . . . . . . H201 H 0.1795 0.6451 -0.4234 0.0891 1.0000 Uiso . . . . . . . H211 H 0.3768 0.5933 -0.3178 0.0929 1.0000 Uiso . . . . . . . H221 H 0.4220 0.5445 -0.1394 0.0870 1.0000 Uiso . . . . . . . H231 H 0.2765 0.5487 -0.0520 0.0734 1.0000 Uiso . . . . . . . H341 H -0.3490 0.2621 -0.3581 0.0639 1.0000 Uiso . . . . . . . H351 H -0.1978 0.2488 -0.4317 0.0769 1.0000 Uiso . . . . . . . H361 H -0.0349 0.3191 -0.3929 0.0780 1.0000 Uiso . . . . . . . H421 H -0.4435 0.4008 -0.0091 0.0591 1.0000 Uiso . . . . . . . H431 H -0.6573 0.3948 -0.1601 0.0750 1.0000 Uiso . . . . . . . H441 H -0.6993 0.3607 -0.3514 0.0752 1.0000 Uiso . . . . . . . H451 H -0.5300 0.3347 -0.3941 0.0620 1.0000 Uiso . . . . . . . H461 H 0.1666 0.3356 -0.0210 0.0578 1.0000 Uiso . . . . . . . H471 H 0.3767 0.3710 0.0455 0.0678 1.0000 Uiso . . . . . . . H481 H 0.4555 0.4502 0.1890 0.0691 1.0000 Uiso . . . . . . . H491 H 0.3180 0.4931 0.2627 0.0580 1.0000 Uiso . . . . . . . H501 H 0.2134 0.4556 0.3954 0.0510 1.0000 Uiso . . . . . . . H511 H 0.0905 0.4937 0.4879 0.0579 1.0000 Uiso . . . . . . . H521 H -0.1246 0.5232 0.3694 0.0669 1.0000 Uiso . . . . . . . H611 H -0.3389 0.6800 -0.1631 0.0581 1.0000 Uiso . . . . . . . H621 H -0.4269 0.7272 -0.0494 0.0641 1.0000 Uiso . . . . . . . H631 H -0.2996 0.7509 0.1518 0.0742 1.0000 Uiso . . . . . . . H641 H -0.0858 0.7164 0.2460 0.0569 1.0000 Uiso . . . . . . . H671 H 0.0497 0.6230 0.3101 0.0541 1.0000 Uiso . . . . . . . H681 H 0.2697 0.6010 0.4185 0.0561 1.0000 Uiso . . . . . . . H691 H 0.4163 0.6234 0.3399 0.0541 1.0000 Uiso . . . . . . . H711 H 0.0968 0.8747 -0.2927 0.0800 1.0000 Uiso . . . . . . . H712 H 0.0797 0.8249 -0.3924 0.0800 1.0000 Uiso . . . . . . . H721 H 0.2989 0.9007 -0.2667 0.0808 1.0000 Uiso . . . . . . . H722 H 0.2404 0.8798 -0.4048 0.0809 1.0000 Uiso . . . . . . . H731 H 0.4441 0.8222 -0.2513 0.0810 1.0000 Uiso . . . . . . . H732 H 0.3317 0.7839 -0.3551 0.0814 1.0000 Uiso . . . . . . . H741 H 0.3770 0.7941 -0.1116 0.0870 1.0000 Uiso . . . . . . . H742 H 0.3294 0.7346 -0.1959 0.0869 1.0000 Uiso . . . . . . . H5601 H -0.5222 0.5189 -0.4307 0.0818 0.5000 Uiso . . . . 1 . . H5602 H -0.4440 0.4670 -0.3352 0.0820 0.5000 Uiso . . . . 1 . . H5701 H -0.4850 0.4550 -0.5551 0.0750 0.5000 Uiso . . . . 1 . . H5702 H -0.3489 0.4329 -0.4526 0.0752 0.5000 Uiso . . . . 1 . . H5801 H -0.3937 0.5358 -0.5921 0.1000 0.5000 Uiso . . . . 1 . . H5802 H -0.2558 0.5092 -0.4973 0.1000 0.5000 Uiso . . . . 1 . . H5901 H -0.4011 0.6024 -0.4618 0.0820 0.5000 Uiso . . . . 1 . . H5902 H -0.2464 0.5944 -0.3959 0.0820 0.5000 Uiso . . . . 1 . . H5611 H -0.4849 0.5356 -0.3628 0.0820 0.5000 Uiso . . . . 2 . . H5612 H -0.4067 0.4779 -0.2872 0.0820 0.5000 Uiso . . . . 2 . . H5711 H -0.5268 0.4722 -0.5195 0.0751 0.5000 Uiso . . . . 2 . . H5712 H -0.3952 0.4346 -0.4474 0.0751 0.5000 Uiso . . . . 2 . . H5811 H -0.4367 0.5286 -0.6065 0.1001 0.5000 Uiso . . . . 2 . . H5812 H -0.3190 0.4803 -0.5570 0.1001 0.5000 Uiso . . . . 2 . . H5911 H -0.3200 0.5957 -0.4667 0.0820 0.5000 Uiso . . . . 2 . . H5912 H -0.1970 0.5516 -0.4323 0.0821 0.5000 Uiso . . . . 2 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0396(3) 0.0667(4) 0.0451(3) -0.0015(3) 0.0194(2) -0.0016(3) C2 0.043(4) 0.038(4) 0.029(3) 0.001(3) 0.013(3) 0.005(3) C3 0.045(4) 0.030(4) 0.021(3) -0.005(3) 0.016(3) -0.005(3) O4 0.038(2) 0.033(3) 0.029(2) 0.000(2) 0.016(2) 0.000(2) Na5 0.0541(16) 0.0285(14) 0.0371(13) -0.0017(13) 0.0228(13) -0.0027(13) O6 0.039(3) 0.029(2) 0.027(2) -0.0072(19) 0.015(2) -0.004(2) B7 0.044(4) 0.031(4) 0.026(4) 0.002(3) 0.014(3) 0.002(3) O8 0.040(3) 0.036(3) 0.036(3) -0.003(2) 0.019(2) -0.007(2) Na9 0.079(2) 0.0320(15) 0.0351(14) 0.0019(13) 0.0220(14) -0.0081(16) O10 0.055(3) 0.028(3) 0.042(3) 0.001(2) 0.024(2) 0.006(2) C11 0.033(4) 0.041(4) 0.043(4) -0.012(3) 0.012(3) 0.009(3) C12 0.049(5) 0.056(5) 0.052(5) -0.013(4) 0.027(4) 0.001(4) C13 0.041(4) 0.041(4) 0.038(4) -0.005(3) 0.023(3) 0.003(3) C14 0.041(4) 0.031(4) 0.024(3) -0.003(3) 0.012(3) -0.004(3) C15 0.061(5) 0.035(4) 0.037(4) 0.000(3) 0.022(4) 0.007(4) I16 0.0742(4) 0.0529(3) 0.0391(3) 0.0004(3) 0.0186(3) 0.0242(3) C17 0.058(5) 0.041(4) 0.029(3) 0.006(3) 0.009(3) 0.004(4) C18 0.070(5) 0.055(5) 0.033(4) 0.001(4) 0.024(4) 0.006(4) C19 0.060(5) 0.056(5) 0.043(4) -0.015(4) 0.030(4) -0.016(4) C20 0.063(6) 0.100(8) 0.059(5) -0.019(5) 0.041(5) 0.000(5) C21 0.044(5) 0.121(10) 0.067(7) -0.018(7) 0.020(5) 0.016(6) C22 0.038(5) 0.097(8) 0.082(7) -0.022(6) 0.015(5) 0.021(5) C23 0.054(5) 0.072(7) 0.056(5) -0.016(5) 0.014(5) 0.012(5) O24 0.038(3) 0.032(3) 0.028(2) 0.000(2) 0.014(2) -0.002(2) C25 0.042(4) 0.030(4) 0.025(3) -0.003(3) 0.016(3) -0.005(3) C26 0.041(4) 0.041(4) 0.026(3) 0.003(3) 0.012(3) 0.001(3) C27 0.032(3) 0.039(4) 0.036(3) 0.009(3) 0.016(3) 0.007(3) C28 0.038(4) 0.038(4) 0.032(3) 0.007(3) 0.018(3) 0.006(3) O29 0.038(3) 0.028(3) 0.033(2) -0.003(2) 0.014(2) 0.002(2) B30 0.036(4) 0.031(4) 0.018(3) 0.003(3) 0.009(3) 0.003(3) O31 0.045(3) 0.033(3) 0.026(2) 0.001(2) 0.015(2) -0.002(2) C32 0.068(5) 0.029(4) 0.024(3) 0.000(3) 0.019(3) 0.006(4) C33 0.063(5) 0.037(4) 0.029(4) -0.004(3) 0.007(4) -0.003(4) C34 0.094(7) 0.030(4) 0.037(4) -0.012(4) 0.016(4) -0.008(4) C35 0.113(8) 0.037(5) 0.042(4) -0.011(4) 0.022(5) 0.002(5) C36 0.106(8) 0.053(6) 0.034(4) 0.005(4) 0.031(5) 0.025(6) C37 0.065(5) 0.042(5) 0.030(4) 0.004(3) 0.020(4) 0.013(4) I38 0.0654(4) 0.0622(4) 0.0468(3) 0.0079(3) 0.0344(3) 0.0072(3) C39 0.052(5) 0.032(4) 0.034(4) -0.001(3) 0.004(3) -0.006(4) C40 0.042(4) 0.032(4) 0.042(4) 0.001(3) 0.011(3) -0.005(3) O41 0.041(3) 0.031(3) 0.029(2) 0.001(2) 0.006(2) -0.004(2) C42 0.044(5) 0.042(5) 0.062(5) 0.001(4) 0.017(4) -0.006(4) C43 0.045(5) 0.066(6) 0.076(7) 0.002(5) 0.022(5) -0.010(4) C44 0.040(5) 0.071(7) 0.077(7) 0.014(6) 0.000(5) -0.016(5) C45 0.063(6) 0.046(5) 0.046(5) -0.001(4) 0.002(4) -0.019(4) C46 0.050(5) 0.052(5) 0.042(4) 0.003(4) 0.020(4) 0.007(4) C47 0.051(5) 0.069(6) 0.050(5) 0.012(5) 0.028(4) 0.021(4) C48 0.039(4) 0.069(6) 0.064(5) 0.002(5) 0.023(4) 0.002(4) C49 0.039(4) 0.053(5) 0.051(5) -0.001(4) 0.010(4) -0.002(4) C50 0.046(4) 0.047(5) 0.034(4) -0.003(3) 0.016(3) 0.000(3) C51 0.064(5) 0.052(5) 0.030(4) -0.008(4) 0.021(4) -0.014(4) C52 0.072(6) 0.044(5) 0.051(5) -0.013(4) 0.039(5) -0.006(4) C53 0.049(5) 0.043(4) 0.047(4) -0.001(4) 0.026(4) -0.005(3) I54 0.0483(3) 0.0473(3) 0.0696(4) -0.0016(3) 0.0308(3) 0.0064(3) C60 0.040(4) 0.027(4) 0.040(4) 0.005(3) 0.022(3) -0.002(3) C61 0.045(4) 0.052(5) 0.048(4) 0.007(4) 0.025(4) 0.000(4) C62 0.038(4) 0.056(5) 0.066(6) 0.024(4) 0.026(4) 0.007(4) C63 0.056(5) 0.045(5) 0.083(7) 0.015(4) 0.051(5) 0.009(4) C64 0.055(5) 0.035(4) 0.052(4) 0.006(3) 0.034(4) -0.001(3) C65 0.044(4) 0.029(4) 0.040(4) -0.002(3) 0.025(3) 0.001(3) C66 0.037(4) 0.030(4) 0.032(3) -0.001(3) 0.015(3) 0.003(3) C67 0.061(5) 0.040(4) 0.035(4) 0.004(3) 0.028(4) 0.004(4) C68 0.060(5) 0.051(5) 0.030(4) 0.009(3) 0.014(4) 0.004(4) C69 0.053(5) 0.042(4) 0.041(4) 0.006(4) 0.019(4) 0.013(4) O70 0.060(3) 0.049(3) 0.052(3) 0.005(3) 0.033(3) -0.001(3) C71 0.070(6) 0.074(7) 0.055(5) 0.019(5) 0.031(5) 0.005(5) C72 0.088(7) 0.054(6) 0.060(6) 0.002(5) 0.041(5) -0.020(5) C73 0.067(6) 0.076(7) 0.059(5) -0.019(5) 0.030(5) -0.019(5) C74 0.068(6) 0.073(7) 0.075(6) 0.003(6) 0.037(5) 0.013(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.16839(6) 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 I1 . C2 . 2.072(7) yes C2 . C3 . 1.401(10) yes C2 . C69 . 1.395(10) yes C3 . O4 . 1.382(8) yes C3 . C66 . 1.396(9) yes O4 . Na5 . 2.318(5) yes O4 . B7 . 1.468(9) yes Na5 . O29 2_555 2.313(5) yes Na5 . O41 2_555 2.388(6) yes Na5 . B30 2_555 2.968(8) yes Na5 . O6 . 2.336(5) yes Na5 . O70 . 2.279(6) yes O6 . B7 . 1.476(9) yes O6 . C14 . 1.357(7) yes B7 . O8 . 1.470(10) yes B7 . O10 . 1.444(10) yes O8 . Na9 . 2.307(6) yes O8 . C60 . 1.378(8) yes Na9 . O10 . 2.424(6) yes Na9 . O24 . 2.395(5) yes Na9 . O31 . 2.345(6) yes Na9 . I38 . 3.483(3) yes Na9 . O550 . 2.516(11) yes O10 . C11 . 1.384(9) yes C11 . C12 . 1.381(12) yes C11 . C23 . 1.394(11) yes C12 . C13 . 1.478(11) yes C12 . C20 . 1.389(11) yes C13 . C14 . 1.385(10) yes C13 . C19 . 1.429(11) yes C14 . C15 . 1.406(11) yes C15 . I16 . 2.085(8) yes C15 . C17 . 1.391(11) yes C17 . C18 . 1.359(12) yes C17 . H171 . 0.931 no C18 . C19 . 1.388(12) yes C18 . H181 . 0.932 no C19 . H191 . 0.933 no C20 . C21 . 1.391(15) yes C20 . H201 . 0.934 no C21 . C22 . 1.360(17) yes C21 . H211 . 0.933 no C22 . C23 . 1.401(14) yes C22 . H221 . 0.934 no C23 . H231 . 0.984 no O24 . C25 . 1.364(8) yes O24 . B30 . 1.506(9) yes C25 . C26 . 1.414(10) yes C25 . C53 . 1.394(10) yes C26 . C27 . 1.464(10) yes C26 . C50 . 1.393(10) yes C27 . C28 . 1.374(10) yes C27 . C49 . 1.424(11) yes C28 . O29 . 1.390(8) yes C28 . C46 . 1.395(10) yes O29 . B30 . 1.446(9) yes B30 . O31 . 1.465(8) yes B30 . O41 . 1.462(9) yes O31 . C32 . 1.369(8) yes C32 . C33 . 1.391(11) yes C32 . C37 . 1.427(11) yes C33 . C34 . 1.388(12) yes C33 . C39 . 1.473(12) yes C34 . C35 . 1.378(15) yes C34 . H341 . 0.934 no C35 . C36 . 1.357(15) yes C35 . H351 . 0.926 no C36 . C37 . 1.411(12) yes C36 . H361 . 0.931 no C37 . I38 . 2.073(9) yes C39 . C40 . 1.392(11) yes C39 . C45 . 1.431(12) yes C40 . O41 . 1.370(9) yes C40 . C42 . 1.392(12) yes C42 . C43 . 1.393(12) yes C42 . H421 . 0.935 no C43 . C44 . 1.383(15) yes C43 . H431 . 0.929 no C44 . C45 . 1.366(15) yes C44 . H441 . 0.925 no C45 . H451 . 0.922 no C46 . C47 . 1.382(12) yes C46 . H461 . 0.927 no C47 . C48 . 1.388(13) yes C47 . H471 . 0.933 no C48 . C49 . 1.391(12) yes C48 . H481 . 0.937 no C49 . H491 . 0.932 no C50 . C51 . 1.387(11) yes C50 . H501 . 0.926 no C51 . C52 . 1.377(13) yes C51 . H511 . 0.938 no C52 . C53 . 1.393(11) yes C52 . H521 . 0.935 no C53 . I54 . 2.086(8) yes C60 . C61 . 1.402(10) yes C60 . C65 . 1.389(10) yes C61 . C62 . 1.361(12) yes C61 . H611 . 0.936 no C62 . C63 . 1.376(13) yes C62 . H621 . 0.928 no C63 . C64 . 1.363(12) yes C63 . H631 . 0.948 no C64 . C65 . 1.405(10) yes C64 . H641 . 0.938 no C65 . C66 . 1.470(10) yes C66 . C67 . 1.418(10) yes C67 . C68 . 1.389(12) yes C67 . H671 . 0.939 no C68 . C69 . 1.375(12) yes C68 . H681 . 0.928 no C69 . H691 . 0.937 no O70 . C71 . 1.420(11) yes O70 . C74 . 1.448(11) yes C71 . C72 . 1.502(13) yes C71 . H711 . 0.976 no C71 . H712 . 0.967 no C72 . C73 . 1.531(15) yes C72 . H721 . 0.973 no C72 . H722 . 0.975 no C73 . C74 . 1.505(14) yes C73 . H731 . 0.975 no C73 . H732 . 0.969 no C74 . H741 . 0.976 no C74 . H742 . 0.974 no O550 . C560 . 1.480(9) yes O550 . C590 . 1.476(9) yes C560 . C570 . 1.513(9) yes C560 . H5601 . 0.972 no C560 . H5602 . 0.965 no C570 . C580 . 1.478(10) yes C570 . H5701 . 0.966 no C570 . H5702 . 0.973 no C580 . C590 . 1.507(10) yes C580 . H5801 . 0.970 no C580 . H5802 . 0.975 no C590 . H5901 . 0.976 no C590 . H5902 . 0.973 no O551 . C561 . 1.497(9) yes O551 . C591 . 1.457(9) yes C561 . C571 . 1.514(10) yes C561 . H5611 . 0.963 no C561 . H5612 . 0.974 no C571 . C581 . 1.481(10) yes C571 . H5711 . 0.970 no C571 . H5712 . 0.977 no C581 . C591 . 1.499(10) yes C581 . H5811 . 0.970 no C581 . H5812 . 0.975 no C591 . H5911 . 0.975 no C591 . H5912 . 0.974 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 I1 . C2 . C3 . 121.5(5) yes I1 . C2 . C69 . 119.1(6) yes C3 . C2 . C69 . 119.2(7) yes C2 . C3 . O4 . 118.8(6) yes C2 . C3 . C66 . 121.0(6) yes O4 . C3 . C66 . 119.9(6) yes C3 . O4 . Na5 . 137.0(4) yes C3 . O4 . B7 . 119.9(5) yes Na5 . O4 . B7 . 101.8(4) yes O29 2_555 Na5 . O4 . 119.76(19) yes O29 2_555 Na5 . O41 2_555 57.65(17) yes O4 . Na5 . O41 2_555 126.41(19) yes O29 2_555 Na5 . B30 2_555 28.47(19) yes O4 . Na5 . B30 2_555 128.1(2) yes O41 2_555 Na5 . B30 2_555 29.18(19) yes O29 2_555 Na5 . O6 . 120.5(2) yes O4 . Na5 . O6 . 57.85(17) yes O41 2_555 Na5 . O6 . 175.7(2) yes B30 2_555 Na5 . O6 . 148.9(2) yes O29 2_555 Na5 . O70 . 122.4(2) yes O4 . Na5 . O70 . 117.7(2) yes O41 2_555 Na5 . O70 . 91.3(2) yes B30 2_555 Na5 . O70 . 109.1(2) yes O6 . Na5 . O70 . 86.7(2) yes Na5 . O6 . B7 . 100.7(4) yes Na5 . O6 . C14 . 132.8(4) yes B7 . O6 . C14 . 122.7(5) yes O6 . B7 . O4 . 99.7(6) yes O6 . B7 . O8 . 112.9(6) yes O4 . B7 . O8 . 113.0(6) yes O6 . B7 . O10 . 113.9(6) yes O4 . B7 . O10 . 116.9(6) yes O8 . B7 . O10 . 101.0(6) yes B7 . O8 . Na9 . 103.3(4) yes B7 . O8 . C60 . 122.7(5) yes Na9 . O8 . C60 . 130.0(4) yes O8 . Na9 . O10 . 56.71(18) yes O8 . Na9 . O24 . 110.0(2) yes O10 . Na9 . O24 . 127.9(2) yes O8 . Na9 . O31 . 165.6(2) yes O10 . Na9 . O31 . 135.5(2) yes O24 . Na9 . O31 . 57.42(17) yes O8 . Na9 . I38 . 131.52(16) yes O10 . Na9 . I38 . 75.34(14) yes O24 . Na9 . I38 . 104.54(15) yes O31 . Na9 . I38 . 62.20(14) yes O8 . Na9 . O550 . 93.0(3) yes O10 . Na9 . O550 . 115.3(3) yes O24 . Na9 . O550 . 115.5(3) yes O31 . Na9 . O550 . 87.4(3) yes I38 . Na9 . O550 . 101.8(3) yes Na9 . O10 . B7 . 98.9(4) yes Na9 . O10 . C11 . 138.1(4) yes B7 . O10 . C11 . 120.5(6) yes O10 . C11 . C12 . 121.2(6) yes O10 . C11 . C23 . 117.1(8) yes C12 . C11 . C23 . 121.1(8) yes C11 . C12 . C13 . 121.6(7) yes C11 . C12 . C20 . 118.9(8) yes C13 . C12 . C20 . 119.5(8) yes C12 . C13 . C14 . 123.2(7) yes C12 . C13 . C19 . 117.9(7) yes C14 . C13 . C19 . 118.9(7) yes C13 . C14 . O6 . 121.2(6) yes C13 . C14 . C15 . 118.7(6) yes O6 . C14 . C15 . 119.9(6) yes C14 . C15 . I16 . 118.7(5) yes C14 . C15 . C17 . 120.5(7) yes I16 . C15 . C17 . 120.6(6) yes C15 . C17 . C18 . 121.9(7) yes C15 . C17 . H171 . 118.8 no C18 . C17 . H171 . 119.2 no C17 . C18 . C19 . 118.2(7) yes C17 . C18 . H181 . 121.7 no C19 . C18 . H181 . 120.1 no C13 . C19 . C18 . 121.5(7) yes C13 . C19 . H191 . 118.7 no C18 . C19 . H191 . 119.8 no C12 . C20 . C21 . 120.1(10) yes C12 . C20 . H201 . 119.3 no C21 . C20 . H201 . 120.6 no C20 . C21 . C22 . 121.0(9) yes C20 . C21 . H211 . 119.5 no C22 . C21 . H211 . 119.5 no C21 . C22 . C23 . 119.9(9) yes C21 . C22 . H221 . 119.5 no C23 . C22 . H221 . 120.6 no C22 . C23 . C11 . 118.9(9) yes C22 . C23 . H231 . 118.1 no C11 . C23 . H231 . 122.9 no Na9 . O24 . C25 . 138.4(4) yes Na9 . O24 . B30 . 99.2(3) yes C25 . O24 . B30 . 117.4(5) yes O24 . C25 . C26 . 120.3(6) yes O24 . C25 . C53 . 120.5(6) yes C26 . C25 . C53 . 119.0(6) yes C25 . C26 . C27 . 120.3(6) yes C25 . C26 . C50 . 119.0(6) yes C27 . C26 . C50 . 120.7(6) yes C26 . C27 . C28 . 122.3(6) yes C26 . C27 . C49 . 120.6(7) yes C28 . C27 . C49 . 117.0(7) yes C27 . C28 . O29 . 119.6(6) yes C27 . C28 . C46 . 122.7(7) yes O29 . C28 . C46 . 117.2(7) yes Na5 2_545 O29 . C28 . 135.2(4) yes Na5 2_545 O29 . B30 . 101.8(4) yes C28 . O29 . B30 . 120.4(5) yes O24 . B30 . O29 . 113.3(5) yes O24 . B30 . Na5 2_545 129.7(4) yes O29 . B30 . Na5 2_545 49.7(3) yes O24 . B30 . O31 . 100.1(5) yes O29 . B30 . O31 . 114.8(6) yes Na5 2_545 B30 . O31 . 130.2(5) yes O24 . B30 . O41 . 113.1(5) yes O29 . B30 . O41 . 102.5(5) yes Na5 2_545 B30 . O41 . 52.8(3) yes O31 . B30 . O41 . 113.5(5) yes Na9 . O31 . B30 . 102.7(4) yes Na9 . O31 . C32 . 139.6(4) yes B30 . O31 . C32 . 116.8(5) yes O31 . C32 . C33 . 120.7(7) yes O31 . C32 . C37 . 118.7(7) yes C33 . C32 . C37 . 120.5(7) yes C32 . C33 . C34 . 118.4(8) yes C32 . C33 . C39 . 120.3(7) yes C34 . C33 . C39 . 121.1(8) yes C33 . C34 . C35 . 121.4(9) yes C33 . C34 . H341 . 119.5 no C35 . C34 . H341 . 119.1 no C34 . C35 . C36 . 121.0(8) yes C34 . C35 . H351 . 119.6 no C36 . C35 . H351 . 119.4 no C35 . C36 . C37 . 120.3(9) yes C35 . C36 . H361 . 120.4 no C37 . C36 . H361 . 119.3 no C32 . C37 . C36 . 118.0(8) yes C32 . C37 . I38 . 119.3(6) yes C36 . C37 . I38 . 122.5(7) yes C37 . I38 . Na9 . 88.3(2) yes C33 . C39 . C40 . 123.1(7) yes C33 . C39 . C45 . 119.7(7) yes C40 . C39 . C45 . 117.1(8) yes C39 . C40 . O41 . 121.0(7) yes C39 . C40 . C42 . 121.0(7) yes O41 . C40 . C42 . 117.7(7) yes Na5 2_545 O41 . C40 . 125.5(4) yes Na5 2_545 O41 . B30 . 98.0(4) yes C40 . O41 . B30 . 122.7(5) yes C40 . C42 . C43 . 120.0(8) yes C40 . C42 . H421 . 120.5 no C43 . C42 . H421 . 119.4 no C42 . C43 . C44 . 120.2(9) yes C42 . C43 . H431 . 120.2 no C44 . C43 . H431 . 119.7 no C43 . C44 . C45 . 119.8(8) yes C43 . C44 . H441 . 120.1 no C45 . C44 . H441 . 120.1 no C39 . C45 . C44 . 121.8(9) yes C39 . C45 . H451 . 118.8 no C44 . C45 . H451 . 119.4 no C28 . C46 . C47 . 118.8(8) yes C28 . C46 . H461 . 121.8 no C47 . C46 . H461 . 119.4 no C46 . C47 . C48 . 120.7(7) yes C46 . C47 . H471 . 119.0 no C48 . C47 . H471 . 120.3 no C47 . C48 . C49 . 119.5(8) yes C47 . C48 . H481 . 120.8 no C49 . C48 . H481 . 119.7 no C27 . C49 . C48 . 121.0(8) yes C27 . C49 . H491 . 118.9 no C48 . C49 . H491 . 120.2 no C26 . C50 . C51 . 121.4(7) yes C26 . C50 . H501 . 119.0 no C51 . C50 . H501 . 119.5 no C50 . C51 . C52 . 119.3(7) yes C50 . C51 . H511 . 120.0 no C52 . C51 . H511 . 120.7 no C51 . C52 . C53 . 120.6(7) yes C51 . C52 . H521 . 119.4 no C53 . C52 . H521 . 119.9 no C25 . C53 . C52 . 120.5(7) yes C25 . C53 . I54 . 120.8(6) yes C52 . C53 . I54 . 118.6(6) yes O8 . C60 . C61 . 118.5(6) yes O8 . C60 . C65 . 120.5(6) yes C61 . C60 . C65 . 120.9(6) yes C60 . C61 . C62 . 119.5(7) yes C60 . C61 . H611 . 119.9 no C62 . C61 . H611 . 120.6 no C61 . C62 . C63 . 120.9(7) yes C61 . C62 . H621 . 119.3 no C63 . C62 . H621 . 119.8 no C62 . C63 . C64 . 119.6(8) yes C62 . C63 . H631 . 119.4 no C64 . C63 . H631 . 121.0 no C63 . C64 . C65 . 121.8(8) yes C63 . C64 . H641 . 119.0 no C65 . C64 . H641 . 119.2 no C64 . C65 . C60 . 117.2(7) yes C64 . C65 . C66 . 120.4(6) yes C60 . C65 . C66 . 122.5(6) yes C65 . C66 . C3 . 121.8(6) yes C65 . C66 . C67 . 120.0(6) yes C3 . C66 . C67 . 118.1(6) yes C66 . C67 . C68 . 120.3(7) yes C66 . C67 . H671 . 119.4 no C68 . C67 . H671 . 120.3 no C67 . C68 . C69 . 120.6(7) yes C67 . C68 . H681 . 118.4 no C69 . C68 . H681 . 121.1 no C2 . C69 . C68 . 120.5(7) yes C2 . C69 . H691 . 119.5 no C68 . C69 . H691 . 120.0 no Na5 . O70 . C71 . 120.6(5) yes Na5 . O70 . C74 . 120.3(5) yes C71 . O70 . C74 . 110.8(7) yes O70 . C71 . C72 . 106.3(8) yes O70 . C71 . H711 . 110.1 no C72 . C71 . H711 . 111.1 no O70 . C71 . H712 . 109.5 no C72 . C71 . H712 . 111.0 no H711 . C71 . H712 . 108.7 no C71 . C72 . C73 . 102.5(8) yes C71 . C72 . H721 . 110.9 no C73 . C72 . H721 . 111.5 no C71 . C72 . H722 . 111.1 no C73 . C72 . H722 . 111.3 no H721 . C72 . H722 . 109.4 no C72 . C73 . C74 . 103.0(8) yes C72 . C73 . H731 . 112.0 no C74 . C73 . H731 . 111.4 no C72 . C73 . H732 . 110.2 no C74 . C73 . H732 . 111.0 no H731 . C73 . H732 . 109.1 no C73 . C74 . O70 . 105.2(8) yes C73 . C74 . H741 . 110.5 no O70 . C74 . H741 . 110.3 no C73 . C74 . H742 . 110.6 no O70 . C74 . H742 . 110.6 no H741 . C74 . H742 . 109.6 no Na9 . O550 . C560 . 131.7(12) yes Na9 . O550 . C590 . 111.2(10) yes C560 . O550 . C590 . 95.8(13) yes O550 . C560 . C570 . 112.0(14) yes O550 . C560 . H5601 . 107.6 no C570 . C560 . H5601 . 107.7 no O550 . C560 . H5602 . 109.5 no C570 . C560 . H5602 . 110.1 no H5601 . C560 . H5602 . 109.8 no C560 . C570 . C580 . 97.5(16) yes C560 . C570 . H5701 . 112.8 no C580 . C570 . H5701 . 112.5 no C560 . C570 . H5702 . 112.1 no C580 . C570 . H5702 . 112.8 no H5701 . C570 . H5702 . 108.8 no C570 . C580 . C590 . 109.8(17) yes C570 . C580 . H5801 . 110.4 no C590 . C580 . H5801 . 109.5 no C570 . C580 . H5802 . 108.4 no C590 . C580 . H5802 . 108.9 no H5801 . C580 . H5802 . 109.8 no C580 . C590 . O550 . 106.6(15) yes C580 . C590 . H5901 . 109.5 no O550 . C590 . H5901 . 109.8 no C580 . C590 . H5902 . 111.5 no O550 . C590 . H5902 . 110.2 no H5901 . C590 . H5902 . 109.2 no Na9 . O551 . C561 . 119.8(10) yes Na9 . O551 . C591 . 127.7(10) yes C561 . O551 . C591 . 111.1(13) yes O551 . C561 . C571 . 94.9(13) yes O551 . C561 . H5611 . 113.2 no C571 . C561 . H5611 . 112.9 no O551 . C561 . H5612 . 112.8 no C571 . C561 . H5612 . 113.4 no H5611 . C561 . H5612 . 109.2 no C561 . C571 . C581 . 114.9(17) yes C561 . C571 . H5711 . 107.9 no C581 . C571 . H5711 . 108.6 no C561 . C571 . H5712 . 108.2 no C581 . C571 . H5712 . 107.9 no H5711 . C571 . H5712 . 109.2 no C571 . C581 . C591 . 101.4(16) yes C571 . C581 . H5811 . 111.6 no C591 . C581 . H5811 . 111.3 no C571 . C581 . H5812 . 111.5 no C591 . C581 . H5812 . 110.8 no H5811 . C581 . H5812 . 110.0 no C581 . C591 . O551 . 106.4(14) yes C581 . C591 . H5911 . 110.4 no O551 . C591 . H5911 . 110.9 no C581 . C591 . H5912 . 110.2 no O551 . C591 . H5912 . 109.5 no H5911 . C591 . H5912 . 109.4 no _chemical_name_common . #============================================================================== data_9 #Structure reported previously by Straub et al. included for reference #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 796358' #TrackingRef 'MW Aldebat EuJOC 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H112 Al Li O8' _chemical_formula_weight 1139.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.954(2) _cell_length_b 28.502(6) _cell_length_c 20.998(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.49(3) _cell_angle_gamma 90.00 _cell_volume 7056(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 136 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.384 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.203 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25812 _diffrn_reflns_av_R_equivalents 0.1128 _diffrn_reflns_av_sigmaI/netI 0.1166 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 19.64 _reflns_number_total 6223 _reflns_number_gt 3423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS' _computing_cell_refinement 'STOE IPDS' _computing_data_reduction 'STOE IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6223 _refine_ls_number_parameters 823 _refine_ls_number_restraints 1257 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 0.818 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 1.6513(10) 0.8564(4) 0.2723(5) 0.068(3) Uani 1 1 d . . . O5 O 1.5460(4) 0.90435(15) 0.2347(2) 0.0806(15) Uani 1 1 d . . . O6 O 1.5854(4) 0.79512(15) 0.2557(2) 0.0753(15) Uani 1 1 d . . . O7 O 1.7851(4) 0.86084(18) 0.2336(2) 0.0888(16) Uani 1 1 d . . . O8 O 1.6986(4) 0.86930(18) 0.3634(2) 0.0852(16) Uani 1 1 d . . . C51 C 1.5435(7) 0.9522(2) 0.2548(4) 0.088(3) Uani 1 1 d U . . H51A H 1.6132 0.9601 0.2834 0.106 Uiso 1 1 calc R . . H51B H 1.4804 0.9573 0.2778 0.106 Uiso 1 1 calc R . . C52 C 1.5307(9) 0.9811(3) 0.1969(4) 0.112(3) Uani 1 1 d U . . H52A H 1.4722 1.0045 0.1980 0.134 Uiso 1 1 calc R . . H52B H 1.6014 0.9970 0.1939 0.134 Uiso 1 1 calc R . . C53 C 1.4998(9) 0.9502(3) 0.1428(4) 0.111(3) Uani 1 1 d U . . H53A H 1.5549 0.9524 0.1137 0.133 Uiso 1 1 calc R . . H53B H 1.4259 0.9587 0.1191 0.133 Uiso 1 1 calc R . . C54 C 1.4972(8) 0.9031(3) 0.1681(4) 0.113(3) Uani 1 1 d U . . H54A H 1.4197 0.8919 0.1631 0.135 Uiso 1 1 calc R . . H54B H 1.5401 0.8821 0.1449 0.135 Uiso 1 1 calc R . . C61 C 1.4691(7) 0.7849(3) 0.2496(6) 0.120(3) Uani 1 1 d U . . H61A H 1.4292 0.7962 0.2084 0.144 Uiso 1 1 calc R . . H61B H 1.4371 0.8000 0.2838 0.144 Uiso 1 1 calc R . . C62 C 1.4579(8) 0.7349(4) 0.2536(7) 0.162(5) Uani 1 1 d U . . H62A H 1.4234 0.7270 0.2909 0.195 Uiso 1 1 calc R . . H62B H 1.4090 0.7234 0.2153 0.195 Uiso 1 1 calc R . . C63 C 1.5597(8) 0.7146(3) 0.2588(5) 0.117(3) Uani 1 1 d U . . H63A H 1.5629 0.6948 0.2215 0.140 Uiso 1 1 calc R . . H63B H 1.5736 0.6952 0.2972 0.140 Uiso 1 1 calc R . . C64 C 1.6448(7) 0.7517(3) 0.2626(5) 0.118(4) Uani 1 1 d U . . H64A H 1.6951 0.7506 0.3038 0.141 Uiso 1 1 calc R . . H64B H 1.6898 0.7481 0.2285 0.141 Uiso 1 1 calc R . . C71 C 1.8448(9) 0.9042(4) 0.2391(6) 0.133(4) Uani 1 1 d U . . H71A H 1.9099 0.9022 0.2733 0.159 Uiso 1 1 calc R . . H71B H 1.7957 0.9291 0.2496 0.159 Uiso 1 1 calc R . . C72 C 1.8810(11) 0.9138(5) 0.1792(6) 0.160(5) Uani 1 1 d U . . H72A H 1.9497 0.9325 0.1853 0.192 Uiso 1 1 calc R . . H72B H 1.8225 0.9300 0.1498 0.192 Uiso 1 1 calc R . . C73 C 1.9015(12) 0.8670(5) 0.1552(7) 0.185(6) Uani 1 1 d U . . H73A H 1.9797 0.8577 0.1693 0.222 Uiso 1 1 calc R . . H73B H 1.8856 0.8663 0.1084 0.222 Uiso 1 1 calc R . . C74 C 1.8215(9) 0.8349(4) 0.1835(5) 0.126(3) Uani 1 1 d U . . H74A H 1.7574 0.8264 0.1509 0.151 Uiso 1 1 calc R . . H74B H 1.8603 0.8066 0.2003 0.151 Uiso 1 1 calc R . . C81 C 1.6490(8) 0.8925(4) 0.4101(4) 0.112(3) Uani 1 1 d U . . H81A H 1.5875 0.8738 0.4215 0.134 Uiso 1 1 calc R . . H81B H 1.6184 0.9224 0.3933 0.134 Uiso 1 1 calc R . . C82 C 1.7353(8) 0.9001(4) 0.4670(4) 0.111(3) Uani 1 1 d U . . H82A H 1.7541 0.9331 0.4720 0.134 Uiso 1 1 calc R . . H82B H 1.7086 0.8892 0.5056 0.134 Uiso 1 1 calc R . . C83 C 1.8302(9) 0.8740(4) 0.4562(4) 0.129(4) Uani 1 1 d U . . H83A H 1.8503 0.8513 0.4905 0.155 Uiso 1 1 calc R . . H83B H 1.8944 0.8947 0.4558 0.155 Uiso 1 1 calc R . . C84 C 1.8032(7) 0.8505(3) 0.3956(4) 0.118(4) Uani 1 1 d U . . H84A H 1.8627 0.8556 0.3700 0.141 Uiso 1 1 calc R . . H84B H 1.7960 0.8171 0.4023 0.141 Uiso 1 1 calc R . . Al1 Al 0.79845(15) 0.60275(6) 0.25158(8) 0.0425(5) Uani 1 1 d . . . O1 O 0.7247(3) 0.59877(12) 0.17377(16) 0.0444(10) Uani 1 1 d . . . O2 O 0.8221(3) 0.66256(12) 0.26440(18) 0.0432(10) Uani 1 1 d . . . O3 O 0.9221(3) 0.56964(12) 0.25986(16) 0.0416(10) Uani 1 1 d . . . O4 O 0.7194(3) 0.58000(12) 0.30520(17) 0.0459(10) Uani 1 1 d . . . C11 C 0.6707(5) 0.63269(19) 0.1355(3) 0.0407(15) Uani 1 1 d U . . C12 C 0.5617(5) 0.62343(19) 0.1023(3) 0.0446(15) Uani 1 1 d U . . C13 C 0.5102(5) 0.6582(2) 0.0610(3) 0.0496(16) Uani 1 1 d U . . H13 H 0.4378 0.6524 0.0385 0.060 Uiso 1 1 calc R . . C14 C 0.5600(5) 0.70087(19) 0.0514(3) 0.0462(16) Uani 1 1 d U . . C15 C 0.6675(5) 0.70850(19) 0.0865(3) 0.0435(15) Uani 1 1 d U . . H15 H 0.7029 0.7371 0.0818 0.052 Uiso 1 1 calc R . . C16 C 0.7245(5) 0.67527(19) 0.1282(3) 0.0389(14) Uani 1 1 d U . . C18 C 0.5046(5) 0.73910(19) 0.0070(3) 0.0533(17) Uani 1 1 d DU . . C21 C 0.8840(5) 0.68375(19) 0.2244(3) 0.0406(15) Uani 1 1 d U . . C22 C 0.9924(5) 0.70270(19) 0.2496(3) 0.0479(16) Uani 1 1 d U . . C23 C 1.0550(6) 0.7211(2) 0.2066(3) 0.0575(17) Uani 1 1 d U . . H23 H 1.1258 0.7335 0.2230 0.069 Uiso 1 1 calc R . . C24 C 1.0207(6) 0.7225(2) 0.1400(3) 0.0566(17) Uani 1 1 d U A . C25 C 0.9124(5) 0.70650(19) 0.1181(3) 0.0480(16) Uani 1 1 d U . . H25 H 0.8846 0.7083 0.0741 0.058 Uiso 1 1 calc R . . C26 C 0.8435(5) 0.68795(18) 0.1581(3) 0.0406(15) Uani 1 1 d U . . C27 C 1.0335(5) 0.7047(2) 0.3224(3) 0.0612(19) Uani 1 1 d DU . . C28 C 1.0968(7) 0.7390(3) 0.0958(4) 0.090(2) Uani 1 1 d DU . . C31 C 0.9032(5) 0.5244(2) 0.2397(3) 0.0401(14) Uani 1 1 d U . . C32 C 0.9492(5) 0.50788(19) 0.1872(3) 0.0459(15) Uani 1 1 d U . . C33 C 0.9137(5) 0.4640(2) 0.1630(3) 0.0476(16) Uani 1 1 d U . . H33 H 0.9413 0.4528 0.1270 0.057 Uiso 1 1 calc R . . C34 C 0.8392(5) 0.43601(19) 0.1901(3) 0.0451(15) Uani 1 1 d U B . C35 C 0.8065(5) 0.45172(19) 0.2456(3) 0.0438(15) Uani 1 1 d U . . H35 H 0.7614 0.4323 0.2665 0.053 Uiso 1 1 calc R . . C36 C 0.8375(5) 0.49544(19) 0.2725(3) 0.0396(14) Uani 1 1 d U . . C37 C 1.0360(5) 0.5359(2) 0.1568(3) 0.0574(17) Uani 1 1 d DU . . C38 C 0.7911(5) 0.3907(2) 0.1570(3) 0.0569(17) Uani 1 1 d DU . . C41 C 0.7494(5) 0.54692(19) 0.3514(3) 0.0429(15) Uani 1 1 d U . . C42 C 0.7198(5) 0.5529(2) 0.4119(3) 0.0471(16) Uani 1 1 d U . . C43 C 0.7487(5) 0.5173(2) 0.4571(3) 0.0542(17) Uani 1 1 d U . . H43 H 0.7278 0.5208 0.4976 0.065 Uiso 1 1 calc R . . C44 C 0.8067(5) 0.4773(2) 0.4450(3) 0.0486(16) Uani 1 1 d U C . C45 C 0.8333(5) 0.4729(2) 0.3845(3) 0.0476(16) Uani 1 1 d U . . H45 H 0.8709 0.4459 0.3751 0.057 Uiso 1 1 calc R . . C46 C 0.8075(5) 0.50660(18) 0.3361(3) 0.0398(15) Uani 1 1 d U . . C47 C 0.6599(6) 0.5972(2) 0.4299(3) 0.0621(18) Uani 1 1 d DU . . C48 C 0.8371(6) 0.4395(2) 0.4971(3) 0.0606(17) Uani 1 1 d DU . . C17 C 0.5005(5) 0.5771(2) 0.1107(3) 0.0535(17) Uani 1 1 d DU . . C171 C 0.4784(6) 0.5741(2) 0.1797(3) 0.073(2) Uani 1 1 d DU . . H17A H 0.4410 0.5450 0.1857 0.109 Uiso 1 1 calc R . . H17B H 0.4312 0.5998 0.1881 0.109 Uiso 1 1 calc R . . H17C H 0.5492 0.5755 0.2088 0.109 Uiso 1 1 calc R . . C172 C 0.5699(6) 0.5351(2) 0.0949(4) 0.081(2) Uani 1 1 d DU . . H17D H 0.5300 0.5067 0.1010 0.122 Uiso 1 1 calc R . . H17E H 0.6421 0.5351 0.1228 0.122 Uiso 1 1 calc R . . H17F H 0.5814 0.5371 0.0508 0.122 Uiso 1 1 calc R . . C173 C 0.3859(5) 0.5744(2) 0.0664(3) 0.081(2) Uani 1 1 d DU . . H17G H 0.3502 0.5450 0.0729 0.121 Uiso 1 1 calc R . . H17H H 0.3969 0.5768 0.0223 0.121 Uiso 1 1 calc R . . H17I H 0.3386 0.5997 0.0763 0.121 Uiso 1 1 calc R . . C181 C 0.3908(6) 0.7240(2) -0.0301(4) 0.086(3) Uani 1 1 d DU . . H18A H 0.3586 0.7491 -0.0575 0.129 Uiso 1 1 calc R . . H18B H 0.3409 0.7161 -0.0002 0.129 Uiso 1 1 calc R . . H18C H 0.4009 0.6970 -0.0559 0.129 Uiso 1 1 calc R . . C182 C 0.5806(6) 0.7508(3) -0.0412(3) 0.087(2) Uani 1 1 d DU . . H18D H 0.5464 0.7752 -0.0694 0.131 Uiso 1 1 calc R . . H18E H 0.5911 0.7234 -0.0661 0.131 Uiso 1 1 calc R . . H18F H 0.6528 0.7613 -0.0188 0.131 Uiso 1 1 calc R . . C183 C 0.4864(7) 0.7831(2) 0.0461(4) 0.094(3) Uani 1 1 d DU . . H18G H 0.4516 0.8072 0.0174 0.141 Uiso 1 1 calc R . . H18H H 0.5581 0.7941 0.0684 0.141 Uiso 1 1 calc R . . H18I H 0.4379 0.7757 0.0769 0.141 Uiso 1 1 calc R . . C271 C 1.1515(6) 0.7272(3) 0.3388(4) 0.099(3) Uani 1 1 d DU . . H27A H 1.1743 0.7279 0.3848 0.148 Uiso 1 1 calc R . . H27B H 1.1488 0.7586 0.3221 0.148 Uiso 1 1 calc R . . H27C H 1.2051 0.7091 0.3197 0.148 Uiso 1 1 calc R . . C272 C 1.0431(6) 0.6552(2) 0.3523(3) 0.082(2) Uani 1 1 d DU . . H27D H 1.0683 0.6576 0.3980 0.124 Uiso 1 1 calc R . . H27E H 1.0965 0.6370 0.3332 0.124 Uiso 1 1 calc R . . H27F H 0.9702 0.6401 0.3443 0.124 Uiso 1 1 calc R . . C273 C 0.9513(6) 0.7333(2) 0.3540(3) 0.085(2) Uani 1 1 d DU . . H27G H 0.9770 0.7344 0.3998 0.127 Uiso 1 1 calc R . . H27H H 0.8775 0.7192 0.3455 0.127 Uiso 1 1 calc R . . H27I H 0.9473 0.7646 0.3369 0.127 Uiso 1 1 calc R . . C281 C 1.201(2) 0.7685(11) 0.1143(18) 0.108(13) Uani 0.425(15) 1 d PDU A 1 H28A H 1.2361 0.7740 0.0769 0.162 Uiso 0.425(15) 1 calc PR A 1 H28B H 1.2538 0.7525 0.1466 0.162 Uiso 0.425(15) 1 calc PR A 1 H28C H 1.1808 0.7980 0.1313 0.162 Uiso 0.425(15) 1 calc PR A 1 C282 C 1.0197(16) 0.7800(7) 0.0484(9) 0.093(7) Uani 0.425(15) 1 d PDU A 1 H28D H 1.0638 0.7921 0.0177 0.140 Uiso 0.425(15) 1 calc PR A 1 H28E H 1.0002 0.8052 0.0749 0.140 Uiso 0.425(15) 1 calc PR A 1 H28F H 0.9517 0.7659 0.0258 0.140 Uiso 0.425(15) 1 calc PR A 1 C283 C 1.105(3) 0.7070(7) 0.0406(9) 0.103(8) Uani 0.425(15) 1 d PDU A 1 H28G H 1.1551 0.7202 0.0143 0.154 Uiso 0.425(15) 1 calc PR A 1 H28H H 1.0306 0.7032 0.0151 0.154 Uiso 0.425(15) 1 calc PR A 1 H28I H 1.1328 0.6770 0.0567 0.154 Uiso 0.425(15) 1 calc PR A 1 C371 C 1.0860(7) 0.5078(2) 0.1063(4) 0.088(2) Uani 1 1 d DU . . H37A H 1.1399 0.5269 0.0888 0.132 Uiso 1 1 calc R . . H37B H 1.0263 0.4986 0.0722 0.132 Uiso 1 1 calc R . . H37C H 1.1232 0.4804 0.1260 0.132 Uiso 1 1 calc R . . C372 C 0.9828(7) 0.5800(2) 0.1239(4) 0.085(2) Uani 1 1 d DU . . H37D H 1.0388 0.5970 0.1053 0.127 Uiso 1 1 calc R . . H37E H 0.9548 0.5995 0.1552 0.127 Uiso 1 1 calc R . . H37F H 0.9212 0.5715 0.0906 0.127 Uiso 1 1 calc R . . C373 C 1.1353(6) 0.5498(3) 0.2086(4) 0.085(2) Uani 1 1 d DU . . H37G H 1.1895 0.5673 0.1892 0.128 Uiso 1 1 calc R . . H37H H 1.1708 0.5221 0.2286 0.128 Uiso 1 1 calc R . . H37I H 1.1082 0.5688 0.2406 0.128 Uiso 1 1 calc R . . C381 C 0.800(2) 0.3516(6) 0.2075(8) 0.083(6) Uani 0.59(3) 1 d PDU B 1 H38A H 0.7660 0.3619 0.2436 0.125 Uiso 0.59(3) 1 calc PR B 1 H38B H 0.8778 0.3439 0.2220 0.125 Uiso 0.59(3) 1 calc PR B 1 H38C H 0.7600 0.3243 0.1887 0.125 Uiso 0.59(3) 1 calc PR B 1 C382 C 0.6603(10) 0.3978(7) 0.1361(12) 0.083(7) Uani 0.59(3) 1 d PDU B 1 H38D H 0.6280 0.4090 0.1722 0.125 Uiso 0.59(3) 1 calc PR B 1 H38E H 0.6259 0.3684 0.1216 0.125 Uiso 0.59(3) 1 calc PR B 1 H38F H 0.6468 0.4203 0.1016 0.125 Uiso 0.59(3) 1 calc PR B 1 C383 C 0.8406(19) 0.3751(8) 0.1000(10) 0.090(6) Uani 0.59(3) 1 d PDU B 1 H38G H 0.8041 0.3466 0.0831 0.135 Uiso 0.59(3) 1 calc PR B 1 H38H H 0.9204 0.3694 0.1128 0.135 Uiso 0.59(3) 1 calc PR B 1 H38I H 0.8295 0.3990 0.0674 0.135 Uiso 0.59(3) 1 calc PR B 1 C471 C 0.5461(5) 0.6034(2) 0.3861(3) 0.074(2) Uani 1 1 d DU . . H47A H 0.5100 0.6314 0.3981 0.110 Uiso 1 1 calc R . . H47B H 0.4986 0.5768 0.3904 0.110 Uiso 1 1 calc R . . H47C H 0.5578 0.6059 0.3421 0.110 Uiso 1 1 calc R . . C472 C 0.7378(6) 0.6393(2) 0.4244(3) 0.079(2) Uani 1 1 d DU . . H47D H 0.7015 0.6675 0.4354 0.118 Uiso 1 1 calc R . . H47E H 0.7525 0.6415 0.3809 0.118 Uiso 1 1 calc R . . H47F H 0.8080 0.6351 0.4534 0.118 Uiso 1 1 calc R . . C473 C 0.6359(8) 0.5952(3) 0.4985(3) 0.100(3) Uani 1 1 d DU . . H47G H 0.5983 0.6235 0.5080 0.150 Uiso 1 1 calc R . . H47H H 0.7060 0.5921 0.5280 0.150 Uiso 1 1 calc R . . H47I H 0.5881 0.5688 0.5031 0.150 Uiso 1 1 calc R . . C481 C 0.762(2) 0.3978(7) 0.4773(13) 0.098(8) Uani 0.59(3) 1 d PDU C 1 H48A H 0.7718 0.3878 0.4349 0.147 Uiso 0.59(3) 1 calc PR C 1 H48B H 0.6843 0.4064 0.4770 0.147 Uiso 0.59(3) 1 calc PR C 1 H48C H 0.7823 0.3727 0.5074 0.147 Uiso 0.59(3) 1 calc PR C 1 C482 C 0.9597(11) 0.4250(10) 0.5004(13) 0.098(7) Uani 0.59(3) 1 d PDU C 1 H48D H 1.0078 0.4518 0.5105 0.147 Uiso 0.59(3) 1 calc PR C 1 H48E H 0.9705 0.4123 0.4595 0.147 Uiso 0.59(3) 1 calc PR C 1 H48F H 0.9785 0.4016 0.5334 0.147 Uiso 0.59(3) 1 calc PR C 1 C483 C 0.821(4) 0.4550(8) 0.5643(8) 0.139(11) Uani 0.59(3) 1 d PDU C 1 H48G H 0.8690 0.4816 0.5772 0.209 Uiso 0.59(3) 1 calc PR C 1 H48H H 0.8418 0.4297 0.5942 0.209 Uiso 0.59(3) 1 calc PR C 1 H48I H 0.7435 0.4634 0.5640 0.209 Uiso 0.59(3) 1 calc PR C 1 C284 C 1.061(2) 0.7398(10) 0.0278(7) 0.181(15) Uani 0.575(15) 1 d PDU A 2 H28J H 1.1212 0.7515 0.0072 0.272 Uiso 0.575(15) 1 calc PR A 2 H28K H 0.9958 0.7598 0.0175 0.272 Uiso 0.575(15) 1 calc PR A 2 H28L H 1.0415 0.7085 0.0128 0.272 Uiso 0.575(15) 1 calc PR A 2 C285 C 1.1966(13) 0.6981(4) 0.1052(8) 0.110(7) Uani 0.575(15) 1 d PDU A 2 H28M H 1.2517 0.7051 0.0782 0.165 Uiso 0.575(15) 1 calc PR A 2 H28N H 1.1629 0.6681 0.0935 0.165 Uiso 0.575(15) 1 calc PR A 2 H28O H 1.2329 0.6973 0.1496 0.165 Uiso 0.575(15) 1 calc PR A 2 C286 C 1.1668(14) 0.7798(5) 0.1265(10) 0.066(6) Uani 0.575(15) 1 d PDU A 2 H28P H 1.2165 0.7904 0.0980 0.098 Uiso 0.575(15) 1 calc PR A 2 H28Q H 1.2109 0.7699 0.1667 0.098 Uiso 0.575(15) 1 calc PR A 2 H28R H 1.1174 0.8049 0.1344 0.098 Uiso 0.575(15) 1 calc PR A 2 C384 C 0.713(3) 0.4067(7) 0.0959(15) 0.104(14) Uani 0.41(3) 1 d PDU B 2 H38J H 0.7544 0.4273 0.0718 0.156 Uiso 0.41(3) 1 calc PR B 2 H38K H 0.6493 0.4230 0.1073 0.156 Uiso 0.41(3) 1 calc PR B 2 H38L H 0.6877 0.3798 0.0700 0.156 Uiso 0.41(3) 1 calc PR B 2 C385 C 0.890(2) 0.3637(8) 0.1344(19) 0.083(8) Uani 0.41(3) 1 d PDU B 2 H38M H 0.9290 0.3841 0.1091 0.125 Uiso 0.41(3) 1 calc PR B 2 H38N H 0.8604 0.3372 0.1088 0.125 Uiso 0.41(3) 1 calc PR B 2 H38O H 0.9418 0.3530 0.1714 0.125 Uiso 0.41(3) 1 calc PR B 2 C386 C 0.735(3) 0.3593(9) 0.1977(13) 0.067(7) Uani 0.41(3) 1 d PDU B 2 H38P H 0.7072 0.3319 0.1733 0.101 Uiso 0.41(3) 1 calc PR B 2 H38Q H 0.6720 0.3754 0.2112 0.101 Uiso 0.41(3) 1 calc PR B 2 H38R H 0.7878 0.3501 0.2349 0.101 Uiso 0.41(3) 1 calc PR B 2 C484 C 0.895(3) 0.4637(9) 0.5578(12) 0.099(11) Uani 0.41(3) 1 d PDU C 2 H48J H 0.9628 0.4787 0.5496 0.149 Uiso 0.41(3) 1 calc PR C 2 H48K H 0.9133 0.4409 0.5916 0.149 Uiso 0.41(3) 1 calc PR C 2 H48L H 0.8445 0.4868 0.5708 0.149 Uiso 0.41(3) 1 calc PR C 2 C485 C 0.734(2) 0.4137(15) 0.5102(18) 0.103(11) Uani 0.41(3) 1 d PDU C 2 H48M H 0.6957 0.3999 0.4709 0.155 Uiso 0.41(3) 1 calc PR C 2 H48N H 0.6839 0.4351 0.5266 0.155 Uiso 0.41(3) 1 calc PR C 2 H48O H 0.7565 0.3894 0.5414 0.155 Uiso 0.41(3) 1 calc PR C 2 C486 C 0.919(4) 0.4040(15) 0.4755(17) 0.135(16) Uani 0.41(3) 1 d PDU C 2 H48P H 0.9856 0.4199 0.4670 0.202 Uiso 0.41(3) 1 calc PR C 2 H48Q H 0.8828 0.3884 0.4370 0.202 Uiso 0.41(3) 1 calc PR C 2 H48R H 0.9399 0.3812 0.5091 0.202 Uiso 0.41(3) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.077(8) 0.054(7) 0.068(7) -0.015(6) -0.001(6) 0.001(6) O5 0.104(4) 0.059(3) 0.071(3) -0.013(2) -0.011(3) 0.015(3) O6 0.058(3) 0.056(3) 0.105(4) -0.015(3) -0.004(3) 0.008(3) O7 0.079(4) 0.092(4) 0.096(4) -0.028(3) 0.017(3) -0.026(3) O8 0.079(4) 0.104(4) 0.066(3) -0.025(3) -0.008(3) 0.029(3) C51 0.119(7) 0.061(5) 0.079(5) -0.014(4) 0.000(5) 0.013(5) C52 0.157(9) 0.087(6) 0.081(6) 0.001(5) -0.010(6) 0.013(6) C53 0.154(9) 0.101(6) 0.071(5) -0.003(5) -0.001(6) 0.026(6) C54 0.153(9) 0.092(6) 0.074(6) -0.025(5) -0.038(6) 0.018(6) C61 0.064(7) 0.104(6) 0.189(10) -0.005(7) 0.011(6) 0.007(5) C62 0.072(6) 0.107(7) 0.288(16) 0.050(9) -0.028(8) -0.017(6) C63 0.095(7) 0.067(5) 0.193(10) -0.011(6) 0.040(7) -0.006(5) C64 0.075(6) 0.066(6) 0.201(11) -0.034(6) -0.007(6) 0.010(4) C71 0.115(8) 0.126(9) 0.160(9) 0.000(7) 0.028(7) -0.054(7) C72 0.113(10) 0.203(11) 0.158(10) 0.047(10) 0.005(8) -0.037(9) C73 0.168(12) 0.241(15) 0.170(11) 0.076(11) 0.098(10) 0.077(11) C74 0.121(9) 0.155(9) 0.107(7) -0.046(7) 0.034(6) 0.008(7) C81 0.104(7) 0.151(8) 0.080(6) 0.002(6) 0.015(5) 0.036(6) C82 0.108(7) 0.161(9) 0.067(5) -0.015(6) 0.019(5) 0.003(6) C83 0.126(8) 0.166(10) 0.082(6) -0.014(6) -0.018(6) 0.041(7) C84 0.092(7) 0.137(8) 0.112(7) -0.040(6) -0.021(6) 0.050(6) Al1 0.0519(12) 0.0315(10) 0.0411(10) 0.0029(8) -0.0010(9) 0.0010(9) O1 0.056(3) 0.033(2) 0.040(2) 0.0036(19) -0.005(2) -0.001(2) O2 0.054(3) 0.031(2) 0.041(2) 0.0017(19) -0.005(2) -0.002(2) O3 0.048(2) 0.030(2) 0.044(2) 0.0001(18) -0.0009(19) -0.0002(18) O4 0.054(3) 0.038(2) 0.046(2) 0.010(2) 0.006(2) 0.008(2) C11 0.051(4) 0.034(3) 0.036(3) 0.006(3) 0.002(3) 0.000(3) C12 0.048(4) 0.040(3) 0.043(4) 0.005(3) -0.001(3) -0.006(3) C13 0.049(4) 0.042(4) 0.053(4) 0.002(3) -0.007(3) -0.007(3) C14 0.049(4) 0.038(3) 0.046(4) 0.001(3) -0.007(3) -0.008(3) C15 0.050(4) 0.035(3) 0.046(4) 0.007(3) 0.007(3) -0.009(3) C16 0.047(4) 0.035(3) 0.032(3) 0.001(3) 0.000(3) -0.005(3) C18 0.050(4) 0.043(4) 0.061(4) 0.018(3) -0.010(3) -0.004(3) C21 0.048(4) 0.027(3) 0.046(4) 0.005(3) 0.004(3) 0.005(3) C22 0.051(4) 0.035(3) 0.053(4) 0.001(3) -0.004(3) -0.002(3) C23 0.048(4) 0.052(4) 0.067(4) -0.008(3) -0.007(4) -0.015(3) C24 0.052(4) 0.057(4) 0.060(4) -0.004(3) 0.006(4) -0.016(3) C25 0.054(4) 0.048(4) 0.040(4) 0.002(3) -0.001(3) -0.011(3) C26 0.051(4) 0.028(3) 0.041(4) 0.005(3) 0.001(3) -0.002(3) C27 0.072(5) 0.045(4) 0.055(4) 0.001(3) -0.020(4) -0.009(3) C28 0.088(6) 0.099(6) 0.091(5) -0.020(4) 0.037(5) -0.041(4) C31 0.043(4) 0.032(4) 0.042(4) 0.002(3) -0.005(3) 0.003(3) C32 0.046(4) 0.038(4) 0.051(4) 0.002(3) 0.002(3) 0.004(3) C33 0.056(4) 0.044(4) 0.042(4) 0.000(3) 0.005(3) 0.005(3) C34 0.049(4) 0.039(3) 0.046(4) -0.008(3) 0.003(3) 0.005(3) C35 0.045(4) 0.037(3) 0.048(4) 0.004(3) 0.003(3) 0.000(3) C36 0.044(4) 0.032(3) 0.040(3) 0.005(3) 0.001(3) 0.009(3) C37 0.061(4) 0.043(4) 0.070(4) 0.002(3) 0.016(3) -0.002(3) C38 0.060(4) 0.042(4) 0.065(4) -0.013(3) 0.000(3) 0.000(3) C41 0.050(4) 0.034(4) 0.042(4) 0.004(3) -0.002(3) 0.001(3) C42 0.057(4) 0.045(4) 0.038(4) 0.000(3) 0.004(3) 0.006(3) C43 0.076(5) 0.051(4) 0.037(3) 0.003(3) 0.013(3) 0.004(3) C44 0.062(4) 0.044(4) 0.039(4) 0.002(3) 0.007(3) 0.005(3) C45 0.058(4) 0.036(3) 0.047(4) 0.001(3) 0.004(3) 0.006(3) C46 0.046(4) 0.031(3) 0.040(3) 0.003(3) 0.000(3) 0.003(3) C47 0.084(5) 0.052(4) 0.052(4) -0.001(3) 0.018(4) 0.020(4) C48 0.086(5) 0.050(4) 0.046(4) 0.015(3) 0.010(4) 0.007(3) C17 0.052(4) 0.043(4) 0.062(4) 0.011(3) -0.001(3) -0.017(3) C171 0.071(5) 0.071(5) 0.076(5) 0.025(4) 0.009(4) -0.022(4) C172 0.088(5) 0.039(4) 0.110(6) -0.008(4) -0.003(5) -0.017(4) C173 0.065(5) 0.065(5) 0.102(5) 0.019(4) -0.015(4) -0.031(4) C181 0.065(5) 0.073(5) 0.102(6) 0.034(4) -0.035(4) -0.006(4) C182 0.088(6) 0.089(6) 0.078(5) 0.051(4) -0.006(4) -0.007(4) C183 0.110(7) 0.052(4) 0.105(6) 0.005(4) -0.027(5) 0.019(4) C271 0.090(6) 0.098(6) 0.090(6) 0.005(5) -0.038(5) -0.035(5) C272 0.102(6) 0.058(4) 0.069(5) 0.010(4) -0.037(4) -0.001(4) C273 0.115(6) 0.074(5) 0.055(4) -0.019(4) -0.017(4) 0.017(5) C281 0.062(16) 0.16(3) 0.100(19) -0.016(16) 0.017(14) -0.048(18) C282 0.084(13) 0.144(17) 0.058(12) 0.012(10) 0.032(10) -0.056(11) C283 0.12(2) 0.143(19) 0.059(16) -0.007(12) 0.041(14) -0.051(14) C371 0.106(7) 0.073(5) 0.098(6) -0.007(4) 0.057(5) -0.008(4) C372 0.108(6) 0.061(4) 0.090(5) 0.030(4) 0.030(5) 0.006(4) C373 0.057(5) 0.089(6) 0.109(6) -0.003(4) 0.010(4) -0.018(4) C381 0.104(16) 0.037(8) 0.111(11) -0.025(6) 0.022(12) -0.019(10) C382 0.063(7) 0.075(10) 0.106(15) -0.031(11) -0.007(8) -0.015(7) C383 0.090(13) 0.092(14) 0.088(11) -0.055(10) 0.013(10) -0.020(10) C471 0.072(5) 0.066(4) 0.083(5) 0.002(4) 0.016(4) 0.022(4) C472 0.099(6) 0.048(4) 0.087(5) -0.020(4) 0.006(4) 0.011(4) C473 0.161(8) 0.075(5) 0.070(5) -0.002(4) 0.038(5) 0.047(5) C481 0.115(13) 0.086(11) 0.083(15) 0.055(9) -0.018(11) -0.028(11) C482 0.076(8) 0.127(18) 0.082(16) 0.058(11) -0.014(8) 0.010(8) C483 0.30(3) 0.071(13) 0.058(8) 0.031(7) 0.067(15) 0.038(18) C284 0.17(3) 0.31(4) 0.063(8) 0.033(19) -0.009(13) -0.11(3) C285 0.132(13) 0.086(9) 0.133(16) -0.024(9) 0.085(12) -0.012(8) C286 0.046(10) 0.062(8) 0.092(12) 0.031(8) 0.022(9) -0.013(7) C384 0.14(3) 0.058(12) 0.089(18) 0.009(11) -0.06(2) -0.034(13) C385 0.117(18) 0.042(12) 0.10(2) -0.039(14) 0.040(15) -0.013(11) C386 0.079(18) 0.043(13) 0.077(13) -0.008(9) 0.005(14) -0.014(12) C484 0.15(3) 0.084(15) 0.052(12) 0.046(10) -0.030(14) -0.023(15) C485 0.110(16) 0.13(3) 0.06(2) 0.058(16) -0.015(12) -0.029(15) C486 0.20(3) 0.13(3) 0.09(2) 0.077(15) 0.05(2) 0.11(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O7 1.914(14) . ? Li1 O6 1.926(11) . ? Li1 O5 1.935(12) . ? Li1 O8 1.937(11) . ? O5 C54 1.424(8) . ? O5 C51 1.430(7) . ? O6 C61 1.405(9) . ? O6 C64 1.421(8) . ? O7 C74 1.411(10) . ? O7 C71 1.421(10) . ? O8 C81 1.394(9) . ? O8 C84 1.425(8) . ? C51 C52 1.455(10) . ? C52 C53 1.436(10) . ? C53 C54 1.447(11) . ? C61 C62 1.434(11) . ? C62 C63 1.336(11) . ? C63 C64 1.462(11) . ? C71 C72 1.424(14) . ? C72 C73 1.460(16) . ? C73 C74 1.514(15) . ? C81 C82 1.460(10) . ? C82 C83 1.406(11) . ? C83 C84 1.426(11) . ? Al1 O4 1.712(4) . ? Al1 O1 1.727(4) . ? Al1 O3 1.738(4) . ? Al1 O2 1.742(4) . ? O1 C11 1.352(6) . ? O2 C21 1.350(7) . ? O3 C31 1.363(6) . ? O4 C41 1.358(6) . ? C11 C16 1.393(7) . ? C11 C12 1.397(7) . ? C12 C13 1.391(7) . ? C12 C17 1.534(8) . ? C13 C14 1.384(8) . ? C14 C15 1.389(7) . ? C14 C18 1.513(8) . ? C15 C16 1.390(7) . ? C16 C26 1.501(8) . ? C18 C182 1.505(8) . ? C18 C181 1.515(7) . ? C18 C183 1.534(8) . ? C21 C26 1.400(8) . ? C21 C22 1.424(8) . ? C22 C23 1.369(9) . ? C22 C27 1.526(8) . ? C23 C24 1.390(9) . ? C24 C25 1.378(8) . ? C24 C28 1.480(10) . ? C25 C26 1.376(8) . ? C27 C273 1.514(9) . ? C27 C271 1.536(8) . ? C27 C272 1.541(8) . ? C28 C284 1.422(14) . ? C28 C283 1.492(15) . ? C28 C281 1.503(16) . ? C28 C286 1.512(13) . ? C28 C285 1.657(13) . ? C28 C282 1.705(14) . ? C31 C32 1.394(8) . ? C31 C36 1.398(8) . ? C32 C33 1.390(8) . ? C32 C37 1.529(9) . ? C33 C34 1.384(8) . ? C34 C35 1.366(8) . ? C34 C38 1.531(8) . ? C35 C36 1.393(7) . ? C36 C46 1.473(8) . ? C37 C372 1.524(8) . ? C37 C373 1.524(8) . ? C37 C371 1.527(8) . ? C38 C386 1.476(14) . ? C38 C383 1.489(12) . ? C38 C384 1.524(13) . ? C38 C381 1.532(12) . ? C38 C385 1.550(14) . ? C38 C382 1.565(11) . ? C41 C42 1.384(8) . ? C41 C46 1.407(8) . ? C42 C43 1.394(8) . ? C42 C47 1.528(8) . ? C43 C44 1.381(8) . ? C44 C45 1.364(8) . ? C44 C48 1.535(8) . ? C45 C46 1.396(7) . ? C47 C473 1.516(8) . ? C47 C471 1.522(8) . ? C47 C472 1.535(8) . ? C48 C485 1.499(15) . ? C48 C481 1.504(13) . ? C48 C484 1.512(15) . ? C48 C482 1.513(14) . ? C48 C483 1.521(13) . ? C48 C486 1.528(16) . ? C17 C171 1.516(8) . ? C17 C172 1.524(8) . ? C17 C173 1.525(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Li1 O6 109.1(6) . . ? O7 Li1 O5 108.2(6) . . ? O6 Li1 O5 110.3(6) . . ? O7 Li1 O8 106.2(6) . . ? O6 Li1 O8 113.3(6) . . ? O5 Li1 O8 109.5(6) . . ? C54 O5 C51 106.8(5) . . ? C54 O5 Li1 121.1(6) . . ? C51 O5 Li1 126.6(5) . . ? C61 O6 C64 107.4(6) . . ? C61 O6 Li1 125.0(6) . . ? C64 O6 Li1 126.0(6) . . ? C74 O7 C71 107.7(8) . . ? C74 O7 Li1 131.6(6) . . ? C71 O7 Li1 117.7(7) . . ? C81 O8 C84 106.6(6) . . ? C81 O8 Li1 134.1(6) . . ? C84 O8 Li1 119.3(6) . . ? O5 C51 C52 107.2(6) . . ? C53 C52 C51 107.1(7) . . ? C52 C53 C54 107.2(7) . . ? O5 C54 C53 107.9(6) . . ? O6 C61 C62 107.5(7) . . ? C63 C62 C61 110.1(8) . . ? C62 C63 C64 107.8(8) . . ? O6 C64 C63 107.0(7) . . ? O7 C71 C72 108.4(10) . . ? C71 C72 C73 102.9(12) . . ? C72 C73 C74 105.2(11) . . ? O7 C74 C73 105.6(9) . . ? O8 C81 C82 108.8(7) . . ? C83 C82 C81 105.6(7) . . ? C82 C83 C84 108.8(8) . . ? O8 C84 C83 107.4(7) . . ? O4 Al1 O1 110.3(2) . . ? O4 Al1 O3 106.32(19) . . ? O1 Al1 O3 110.6(2) . . ? O4 Al1 O2 111.2(2) . . ? O1 Al1 O2 104.77(18) . . ? O3 Al1 O2 113.73(19) . . ? C11 O1 Al1 129.4(3) . . ? C21 O2 Al1 115.7(3) . . ? C31 O3 Al1 112.9(3) . . ? C41 O4 Al1 128.5(4) . . ? O1 C11 C16 120.2(5) . . ? O1 C11 C12 118.5(5) . . ? C16 C11 C12 121.3(5) . . ? C13 C12 C11 117.2(5) . . ? C13 C12 C17 120.9(5) . . ? C11 C12 C17 121.9(5) . . ? C14 C13 C12 124.0(5) . . ? C13 C14 C15 116.3(5) . . ? C13 C14 C18 124.6(5) . . ? C15 C14 C18 119.1(5) . . ? C14 C15 C16 122.8(5) . . ? C15 C16 C11 118.4(5) . . ? C15 C16 C26 115.6(5) . . ? C11 C16 C26 125.9(5) . . ? C182 C18 C14 108.9(5) . . ? C182 C18 C181 107.9(6) . . ? C14 C18 C181 112.1(5) . . ? C182 C18 C183 109.5(6) . . ? C14 C18 C183 110.2(5) . . ? C181 C18 C183 108.2(5) . . ? O2 C21 C26 121.4(5) . . ? O2 C21 C22 119.8(5) . . ? C26 C21 C22 118.8(6) . . ? C23 C22 C21 117.5(6) . . ? C23 C22 C27 121.8(6) . . ? C21 C22 C27 120.6(6) . . ? C22 C23 C24 124.9(6) . . ? C25 C24 C23 115.6(6) . . ? C25 C24 C28 122.5(6) . . ? C23 C24 C28 121.9(6) . . ? C26 C25 C24 123.2(6) . . ? C25 C26 C21 119.7(6) . . ? C25 C26 C16 117.3(5) . . ? C21 C26 C16 122.9(6) . . ? C273 C27 C22 109.6(5) . . ? C273 C27 C271 108.3(6) . . ? C22 C27 C271 111.8(6) . . ? C273 C27 C272 109.0(6) . . ? C22 C27 C272 111.4(5) . . ? C271 C27 C272 106.7(5) . . ? C284 C28 C24 121.3(12) . . ? C284 C28 C283 43.5(12) . . ? C24 C28 C283 114.6(12) . . ? C284 C28 C281 111(2) . . ? C24 C28 C281 126.0(16) . . ? C283 C28 C281 112.8(17) . . ? C284 C28 C286 118.1(14) . . ? C24 C28 C286 109.4(10) . . ? C283 C28 C286 134.5(16) . . ? C281 C28 C286 23.4(18) . . ? C284 C28 C285 102.8(14) . . ? C24 C28 C285 101.9(8) . . ? C283 C28 C285 61.7(11) . . ? C281 C28 C285 79.2(14) . . ? C286 C28 C285 98.8(10) . . ? C284 C28 C282 50.1(12) . . ? C24 C28 C282 104.8(9) . . ? C283 C28 C282 93.5(11) . . ? C281 C28 C282 96.5(15) . . ? C286 C28 C282 86.0(11) . . ? C285 C28 C282 149.5(10) . . ? O3 C31 C32 120.0(5) . . ? O3 C31 C36 118.9(5) . . ? C32 C31 C36 121.1(5) . . ? C33 C32 C31 117.2(6) . . ? C33 C32 C37 120.4(6) . . ? C31 C32 C37 122.4(5) . . ? C34 C33 C32 123.2(6) . . ? C35 C34 C33 117.1(5) . . ? C35 C34 C38 121.6(6) . . ? C33 C34 C38 121.2(6) . . ? C34 C35 C36 123.0(6) . . ? C35 C36 C31 117.6(5) . . ? C35 C36 C46 118.2(5) . . ? C31 C36 C46 124.0(5) . . ? C372 C37 C373 109.0(5) . . ? C372 C37 C371 107.4(6) . . ? C373 C37 C371 106.5(6) . . ? C372 C37 C32 111.0(5) . . ? C373 C37 C32 110.0(5) . . ? C371 C37 C32 112.7(5) . . ? C386 C38 C383 124.3(15) . . ? C386 C38 C384 113.3(13) . . ? C383 C38 C384 71.3(13) . . ? C386 C38 C34 115.1(13) . . ? C383 C38 C34 116.6(9) . . ? C384 C38 C34 105.2(8) . . ? C386 C38 C381 30.8(8) . . ? C383 C38 C381 110.4(11) . . ? C384 C38 C381 139.6(11) . . ? C34 C38 C381 108.9(9) . . ? C386 C38 C385 108.6(13) . . ? C383 C38 C385 34.9(9) . . ? C384 C38 C385 106.2(13) . . ? C34 C38 C385 108.0(11) . . ? C381 C38 C385 83.3(11) . . ? C386 C38 C382 73.1(10) . . ? C383 C38 C382 108.9(9) . . ? C384 C38 C382 44.3(12) . . ? C34 C38 C382 107.6(7) . . ? C381 C38 C382 103.7(9) . . ? C385 C38 C382 139.0(13) . . ? O4 C41 C42 119.5(5) . . ? O4 C41 C46 119.1(5) . . ? C42 C41 C46 121.4(5) . . ? C41 C42 C43 117.6(5) . . ? C41 C42 C47 122.1(5) . . ? C43 C42 C47 120.3(5) . . ? C44 C43 C42 123.5(6) . . ? C45 C44 C43 116.6(5) . . ? C45 C44 C48 122.3(5) . . ? C43 C44 C48 121.0(6) . . ? C44 C45 C46 123.9(5) . . ? C45 C46 C41 117.0(5) . . ? C45 C46 C36 117.1(5) . . ? C41 C46 C36 125.9(5) . . ? C473 C47 C471 106.8(6) . . ? C473 C47 C42 112.0(5) . . ? C471 C47 C42 110.8(5) . . ? C473 C47 C472 108.2(6) . . ? C471 C47 C472 110.8(5) . . ? C42 C47 C472 108.1(5) . . ? C485 C48 C481 36.2(13) . . ? C485 C48 C484 110.0(13) . . ? C481 C48 C484 139.5(12) . . ? C485 C48 C482 132.5(19) . . ? C481 C48 C482 109.0(11) . . ? C484 C48 C482 77.4(14) . . ? C485 C48 C483 75.0(12) . . ? C481 C48 C483 109.0(11) . . ? C484 C48 C483 36.2(12) . . ? C482 C48 C483 107.6(13) . . ? C485 C48 C486 108.4(16) . . ? C481 C48 C486 77.1(18) . . ? C484 C48 C486 109.1(16) . . ? C482 C48 C486 33.9(17) . . ? C483 C48 C486 130.6(16) . . ? C485 C48 C44 111.7(13) . . ? C481 C48 C44 107.3(9) . . ? C484 C48 C44 107.6(11) . . ? C482 C48 C44 109.8(11) . . ? C483 C48 C44 114.0(9) . . ? C486 C48 C44 110.0(13) . . ? C171 C17 C172 110.5(5) . . ? C171 C17 C173 107.4(5) . . ? C172 C17 C173 107.1(5) . . ? C171 C17 C12 108.7(5) . . ? C172 C17 C12 111.3(5) . . ? C173 C17 C12 111.7(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 19.64 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.196 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.038 #============================================================================== data_DFT-RR #This is a sythesised structure included only to aid the reader _database_code_depnum_ccdc_archive 'CCDC 803750' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _cell_length_a 100.0000 _cell_length_b 100.0000 _cell_length_c 100.0000 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1000000 _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_space_group_name_Hall 'P 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens O1 O -0.0084 -0.0082 -0.0091 0.0500 1.0000 Uiso . . . . . . . C2 C -0.0197 -0.0146 -0.0044 0.0500 1.0000 Uiso . . . . . . . C3 C -0.0308 -0.0075 0.0004 0.0500 1.0000 Uiso . . . . . . . C4 C -0.0417 -0.0150 0.0062 0.0500 1.0000 Uiso . . . . . . . C5 C -0.0417 -0.0294 0.0056 0.0500 1.0000 Uiso . . . . . . . C6 C -0.0306 -0.0361 -0.0005 0.0500 1.0000 Uiso . . . . . . . C7 C -0.0198 -0.0289 -0.0052 0.0500 1.0000 Uiso . . . . . . . H71 H -0.0110 -0.0336 -0.0095 0.0500 1.0000 Uiso . . . . . . . H61 H -0.0307 -0.0470 -0.0012 0.0500 1.0000 Uiso . . . . . . . C8 C -0.0525 -0.0368 0.0113 0.0500 1.0000 Uiso . . . . . . . C9 C -0.0630 -0.0304 0.0178 0.0500 1.0000 Uiso . . . . . . . C10 C -0.0628 -0.0162 0.0189 0.0500 1.0000 Uiso . . . . . . . C11 C -0.0525 -0.0087 0.0133 0.0500 1.0000 Uiso . . . . . . . H111 H -0.0525 0.0020 0.0143 0.0500 1.0000 Uiso . . . . . . . H101 H -0.0708 -0.0111 0.0242 0.0500 1.0000 Uiso . . . . . . . H91 H -0.0711 -0.0361 0.0221 0.0500 1.0000 Uiso . . . . . . . H81 H -0.0523 -0.0477 0.0106 0.0500 1.0000 Uiso . . . . . . . C12 C -0.0308 0.0075 -0.0004 0.0500 1.0000 Uiso . . . . . . . C13 C -0.0197 0.0146 0.0044 0.0500 1.0000 Uiso . . . . . . . O14 O -0.0084 0.0082 0.0091 0.0500 1.0000 Uiso . . . . . . . B15 B 0.0000 0.0000 0.0000 0.0500 1.0000 Uiso . . . . . . . O16 O 0.0084 0.0082 -0.0091 0.0500 1.0000 Uiso . . . . . . . C17 C 0.0197 0.0146 -0.0044 0.0500 1.0000 Uiso . . . . . . . C18 C 0.0308 0.0075 0.0004 0.0500 1.0000 Uiso . . . . . . . C19 C 0.0417 0.0150 0.0062 0.0500 1.0000 Uiso . . . . . . . C20 C 0.0417 0.0294 0.0056 0.0500 1.0000 Uiso . . . . . . . C21 C 0.0525 0.0368 0.0113 0.0500 1.0000 Uiso . . . . . . . C22 C 0.0630 0.0304 0.0178 0.0500 1.0000 Uiso . . . . . . . C23 C 0.0628 0.0162 0.0189 0.0500 1.0000 Uiso . . . . . . . C24 C 0.0525 0.0087 0.0133 0.0500 1.0000 Uiso . . . . . . . H241 H 0.0525 -0.0020 0.0144 0.0500 1.0000 Uiso . . . . . . . H231 H 0.0708 0.0111 0.0242 0.0500 1.0000 Uiso . . . . . . . H221 H 0.0711 0.0361 0.0221 0.0500 1.0000 Uiso . . . . . . . H211 H 0.0523 0.0477 0.0106 0.0500 1.0000 Uiso . . . . . . . C25 C 0.0306 0.0361 -0.0005 0.0500 1.0000 Uiso . . . . . . . C26 C 0.0198 0.0289 -0.0052 0.0500 1.0000 Uiso . . . . . . . H261 H 0.0110 0.0336 -0.0095 0.0500 1.0000 Uiso . . . . . . . H251 H 0.0307 0.0470 -0.0012 0.0500 1.0000 Uiso . . . . . . . C27 C 0.0308 -0.0075 -0.0004 0.0500 1.0000 Uiso . . . . . . . C28 C 0.0417 -0.0150 -0.0062 0.0500 1.0000 Uiso . . . . . . . C29 C 0.0417 -0.0294 -0.0056 0.0500 1.0000 Uiso . . . . . . . C30 C 0.0306 -0.0361 0.0005 0.0500 1.0000 Uiso . . . . . . . C31 C 0.0198 -0.0289 0.0051 0.0500 1.0000 Uiso . . . . . . . C32 C 0.0197 -0.0146 0.0044 0.0500 1.0000 Uiso . . . . . . . O33 O 0.0084 -0.0082 0.0091 0.0500 1.0000 Uiso . . . . . . . H311 H 0.0110 -0.0336 0.0095 0.0500 1.0000 Uiso . . . . . . . H301 H 0.0307 -0.0470 0.0011 0.0500 1.0000 Uiso . . . . . . . C34 C 0.0525 -0.0368 -0.0113 0.0500 1.0000 Uiso . . . . . . . C35 C 0.0630 -0.0304 -0.0178 0.0500 1.0000 Uiso . . . . . . . C36 C 0.0628 -0.0162 -0.0189 0.0500 1.0000 Uiso . . . . . . . C37 C 0.0525 -0.0087 -0.0133 0.0500 1.0000 Uiso . . . . . . . H371 H 0.0525 0.0021 -0.0143 0.0500 1.0000 Uiso . . . . . . . H361 H 0.0709 -0.0111 -0.0242 0.0500 1.0000 Uiso . . . . . . . H351 H 0.0712 -0.0361 -0.0221 0.0500 1.0000 Uiso . . . . . . . H341 H 0.0523 -0.0477 -0.0106 0.0500 1.0000 Uiso . . . . . . . C38 C -0.0198 0.0289 0.0051 0.0500 1.0000 Uiso . . . . . . . C39 C -0.0306 0.0361 0.0005 0.0500 1.0000 Uiso . . . . . . . C40 C -0.0417 0.0294 -0.0056 0.0500 1.0000 Uiso . . . . . . . C41 C -0.0417 0.0150 -0.0062 0.0500 1.0000 Uiso . . . . . . . C42 C -0.0525 0.0087 -0.0133 0.0500 1.0000 Uiso . . . . . . . C43 C -0.0628 0.0162 -0.0189 0.0500 1.0000 Uiso . . . . . . . C44 C -0.0630 0.0304 -0.0178 0.0500 1.0000 Uiso . . . . . . . C45 C -0.0525 0.0368 -0.0113 0.0500 1.0000 Uiso . . . . . . . H451 H -0.0523 0.0477 -0.0106 0.0500 1.0000 Uiso . . . . . . . H441 H -0.0712 0.0361 -0.0221 0.0500 1.0000 Uiso . . . . . . . H431 H -0.0709 0.0111 -0.0242 0.0500 1.0000 Uiso . . . . . . . H421 H -0.0525 -0.0021 -0.0143 0.0500 1.0000 Uiso . . . . . . . H391 H -0.0307 0.0470 0.0011 0.0500 1.0000 Uiso . . . . . . . H381 H -0.0110 0.0336 0.0095 0.0500 1.0000 Uiso . . . . . . . #============================================================================== data_DFT-RS #This is a sythesised structure included only to aid the reader _database_code_depnum_ccdc_archive 'CCDC 803751' #TrackingRef '- CEC-000709-CrystallographicData.cif' #============================================================================== _cell_length_a 100.0000 _cell_length_b 100.0000 _cell_length_c 100.0000 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1000000 _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_space_group_name_Hall 'P 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens O1 O -0.0085 0.0122 -0.0003 0.0500 1.0000 Uiso . . . . . . . C2 C -0.0196 0.0131 0.0077 0.0500 1.0000 Uiso . . . . . . . C3 C -0.0308 0.0048 0.0058 0.0500 1.0000 Uiso . . . . . . . C4 C -0.0416 0.0056 0.0153 0.0500 1.0000 Uiso . . . . . . . C5 C -0.0415 0.0157 0.0256 0.0500 1.0000 Uiso . . . . . . . C6 C -0.0522 0.0165 0.0349 0.0500 1.0000 Uiso . . . . . . . C7 C -0.0628 0.0075 0.0346 0.0500 1.0000 Uiso . . . . . . . C8 C -0.0628 -0.0029 0.0248 0.0500 1.0000 Uiso . . . . . . . C9 C -0.0525 -0.0038 0.0155 0.0500 1.0000 Uiso . . . . . . . H91 H -0.0526 -0.0118 0.0082 0.0500 1.0000 Uiso . . . . . . . H81 H -0.0708 -0.0102 0.0247 0.0500 1.0000 Uiso . . . . . . . H71 H -0.0709 0.0081 0.0418 0.0500 1.0000 Uiso . . . . . . . H61 H -0.0519 0.0243 0.0425 0.0500 1.0000 Uiso . . . . . . . C10 C -0.0303 0.0246 0.0264 0.0500 1.0000 Uiso . . . . . . . C11 C -0.0195 0.0232 0.0179 0.0500 1.0000 Uiso . . . . . . . H111 H -0.0107 0.0294 0.0185 0.0500 1.0000 Uiso . . . . . . . H101 H -0.0302 0.0323 0.0341 0.0500 1.0000 Uiso . . . . . . . C12 C -0.0308 -0.0048 -0.0057 0.0500 1.0000 Uiso . . . . . . . C13 C -0.0416 -0.0056 -0.0153 0.0500 1.0000 Uiso . . . . . . . C14 C -0.0415 -0.0157 -0.0256 0.0500 1.0000 Uiso . . . . . . . C15 C -0.0303 -0.0246 -0.0264 0.0500 1.0000 Uiso . . . . . . . C16 C -0.0196 -0.0232 -0.0178 0.0500 1.0000 Uiso . . . . . . . C17 C -0.0196 -0.0131 -0.0077 0.0500 1.0000 Uiso . . . . . . . O18 O -0.0085 -0.0122 0.0003 0.0500 1.0000 Uiso . . . . . . . B19 B 0.0000 0.0000 0.0000 0.0500 1.0000 Uiso . . . . . . . O20 O 0.0085 -0.0003 -0.0122 0.0500 1.0000 Uiso . . . . . . . C21 C 0.0196 0.0077 -0.0131 0.0500 1.0000 Uiso . . . . . . . C22 C 0.0308 0.0057 -0.0048 0.0500 1.0000 Uiso . . . . . . . C23 C 0.0308 -0.0058 0.0048 0.0500 1.0000 Uiso . . . . . . . C24 C 0.0196 -0.0078 0.0131 0.0500 1.0000 Uiso . . . . . . . O25 O 0.0085 0.0003 0.0122 0.0500 1.0000 Uiso . . . . . . . C26 C 0.0196 -0.0179 0.0232 0.0500 1.0000 Uiso . . . . . . . C27 C 0.0304 -0.0264 0.0246 0.0500 1.0000 Uiso . . . . . . . C28 C 0.0415 -0.0256 0.0157 0.0500 1.0000 Uiso . . . . . . . C29 C 0.0416 -0.0153 0.0055 0.0500 1.0000 Uiso . . . . . . . C30 C 0.0525 -0.0154 -0.0038 0.0500 1.0000 Uiso . . . . . . . C31 C 0.0628 -0.0248 -0.0029 0.0500 1.0000 Uiso . . . . . . . C32 C 0.0628 -0.0345 0.0075 0.0500 1.0000 Uiso . . . . . . . C33 C 0.0523 -0.0349 0.0165 0.0500 1.0000 Uiso . . . . . . . H331 H 0.0520 -0.0425 0.0243 0.0500 1.0000 Uiso . . . . . . . H321 H 0.0710 -0.0418 0.0081 0.0500 1.0000 Uiso . . . . . . . H311 H 0.0708 -0.0246 -0.0102 0.0500 1.0000 Uiso . . . . . . . H301 H 0.0526 -0.0082 -0.0119 0.0500 1.0000 Uiso . . . . . . . H271 H 0.0303 -0.0341 0.0324 0.0500 1.0000 Uiso . . . . . . . H261 H 0.0107 -0.0186 0.0294 0.0500 1.0000 Uiso . . . . . . . C34 C 0.0416 0.0153 -0.0056 0.0500 1.0000 Uiso . . . . . . . C35 C 0.0525 0.0155 0.0038 0.0500 1.0000 Uiso . . . . . . . C36 C 0.0627 0.0248 0.0029 0.0500 1.0000 Uiso . . . . . . . C37 C 0.0627 0.0346 -0.0075 0.0500 1.0000 Uiso . . . . . . . C38 C 0.0522 0.0350 -0.0165 0.0500 1.0000 Uiso . . . . . . . C39 C 0.0414 0.0256 -0.0157 0.0500 1.0000 Uiso . . . . . . . C40 C 0.0303 0.0264 -0.0246 0.0500 1.0000 Uiso . . . . . . . C41 C 0.0195 0.0178 -0.0232 0.0500 1.0000 Uiso . . . . . . . H411 H 0.0107 0.0185 -0.0294 0.0500 1.0000 Uiso . . . . . . . H401 H 0.0302 0.0341 -0.0324 0.0500 1.0000 Uiso . . . . . . . H381 H 0.0519 0.0425 -0.0243 0.0500 1.0000 Uiso . . . . . . . H371 H 0.0708 0.0419 -0.0081 0.0500 1.0000 Uiso . . . . . . . H361 H 0.0708 0.0247 0.0102 0.0500 1.0000 Uiso . . . . . . . H351 H 0.0526 0.0082 0.0118 0.0500 1.0000 Uiso . . . . . . . H161 H -0.0107 -0.0295 -0.0185 0.0500 1.0000 Uiso . . . . . . . H151 H -0.0303 -0.0324 -0.0341 0.0500 1.0000 Uiso . . . . . . . C42 C -0.0523 -0.0165 -0.0349 0.0500 1.0000 Uiso . . . . . . . C43 C -0.0628 -0.0075 -0.0346 0.0500 1.0000 Uiso . . . . . . . C44 C -0.0627 0.0029 -0.0248 0.0500 1.0000 Uiso . . . . . . . C45 C -0.0525 0.0038 -0.0155 0.0500 1.0000 Uiso . . . . . . . H451 H -0.0526 0.0119 -0.0082 0.0500 1.0000 Uiso . . . . . . . H441 H -0.0708 0.0102 -0.0247 0.0500 1.0000 Uiso . . . . . . . H431 H -0.0709 -0.0081 -0.0418 0.0500 1.0000 Uiso . . . . . . . H421 H -0.0520 -0.0243 -0.0425 0.0500 1.0000 Uiso . . . . . . . #============================================================================== # Start Validation Reply Form #============================================================================== _vrf_PLAT241_3a ; PROBLEM: Check High Ueq as Compared to Neighbors for C39 RESPONSE: The data were collected at 250 K because the compound appeared to undergo a phase transition below this temperature and was unstable to loss of THF above it. Consequently there is a considerable degree of thermal motion. Efforts were made to refine the structure with a multi-part model, but the refinement was unstable. 3D Fourier maps were examined and it was apparent that each atom has a single locus so a single component model was used with prolate thermal ellipsoids and 1,2 and 1,3 vibration/thermal similarity restraints for the THF molecules in order to maintain sensible parameters. ; _vrf_PLAT420_3b ; PROBLEM: D-H Without Acceptor RESPONSE: The nature of the compound means there isn't space for a conventional acceptor, however, there are phenyl rings aligned providing a O-H...pi interactions. ; _vrf_EXPT005_9 ; PROBLEM: _exptl_crystal_description is missing RESPONSE: Structure reported previously by Straub et al. included for reference and the benefit for readers only. ; _vrf_THETM01_9 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Structure reported previously by Straub et al. included for reference and the benefit for readers only. ; _vrf_PLAT023_9 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 19.64 Deg. RESPONSE: Structure reported previously by Straub et al. included for reference and the benefit for readers only. ; _vrf_PLAT761_9 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Structure reported previously by Straub et al. included for reference and the benefit for readers only. ; _vrf_PLAT762_9 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: Structure reported previously by Straub et al. included for reference and the benefit for readers only. ; #============================================================================== # End Validation Reply Form #==============================================================================