#------------------------------------------------------------------------------ #$Date: 2020-07-06 05:00:07 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253809 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126454.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7126454 loop_ _publ_author_name 'Iniesta, Ester' 'Vidal-Ferran, Anton' _publ_section_title ; Supramolecularly regulated copper-bisoxazoline catalysts for the efficient insertion of carbenoid species into hydroxyl bonds. ; _journal_issue 47 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 6364 _journal_page_last 6367 _journal_paper_doi 10.1039/d0cc00224k _journal_volume 56 _journal_year 2020 _chemical_formula_sum 'C52 H48 B F24 N2 Na O7' _chemical_formula_weight 1302.72 _chemical_name_common NaBArF.L1 _chemical_name_systematic EI33 _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-03-04 deposited with the CCDC. 2020-04-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.5057(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.7633(4) _cell_length_b 18.5020(6) _cell_length_c 24.5224(8) _cell_measurement_reflns_used 9900 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.69 _cell_measurement_theta_min 2.35 _cell_volume 5753.6(3) _computing_cell_refinement 'Bruker APEX3 v2015.9-0' _computing_data_collection 'Bruker APEX3 v2015.9-0' _computing_data_reduction 'Bruker SAINT V8.35A' _computing_molecular_graphics ; SHELXle: C.B. Huebschle, G.M. Sheldrick & B. Dittrich J.Appl.Cryst. (2011) 44, 1281-1284. ; _computing_publication_material 'XCIF, SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT V2014/4 (Sheldrick 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 512 _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_unetI/netI 0.0542 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 68048 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.154 _diffrn_reflns_theta_min 1.672 _diffrn_source 'Microfocus source E025 IuS' _diffrn_source_current 0.6 _diffrn_source_power 50 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_source_type 'Bruker APEX DUO' _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_correction_T_min 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.504 _exptl_crystal_description block _exptl_crystal_F_000 2648 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.801 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1169 _refine_ls_number_reflns 14080 _refine_ls_number_restraints 1502 _refine_ls_restrained_S_all 5.780 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0680 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+5.9577P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1701 _refine_ls_wR_factor_ref 0.2003 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8629 _reflns_number_total 14080 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc00224k2.cif _cod_data_source_block mo_EI33_0m _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. data item '_symmetry_cell_setting' value 'Monoclinic' was changed to 'monoclinic' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 7126454--7126456.cif. ; _cod_original_sg_symbol_H-M P2(1)/c _cod_database_code 7126454 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.985 _shelx_estimated_absorpt_t_max 0.991 _shelx_res_file ; mo_EI33_0m.res created by SHELXL-2014/7 TITL mo_EI33_0m in P2(1)/c CELL 0.71073 12.76330 18.50200 24.52240 90.0000 96.5057 90.0000 ZERR 4.00 0.00040 0.00060 0.00080 0.0000 0.0010 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H B N O F NA UNIT 208 192 4 8 28 96 4 LIST 4 TEMP -173.140 SIZE 0.06 0.10 0.10 L.S. 16 BOND FMAP 2 PLAN 5 EADP F21A F19' ACTA CONF ISOR 0.005 F13' WGHT 0.089200 5.957700 FVAR 0.05448 MOLE 1 ISOR 0.005 $F NA1 7 0.410132 0.258447 0.506944 11.00000 0.02834 0.04117 = 0.03332 -0.00524 0.00861 -0.00074 N1 4 0.290191 0.213529 0.572633 11.00000 0.04322 0.02926 = 0.03273 0.00049 0.01256 -0.00100 N2 4 0.554835 0.348041 0.488883 11.00000 0.05468 0.04761 = 0.03965 0.00482 0.01920 -0.00557 O1 5 0.182461 0.247306 0.635305 11.00000 0.05605 0.03784 = 0.03712 0.00015 0.02282 -0.00077 O2 5 0.296553 0.358253 0.538539 11.00000 0.04734 0.03365 = 0.03616 0.00099 0.01070 -0.00260 O6 5 0.532972 0.285557 0.590215 11.00000 0.05102 0.08130 = 0.04146 0.00995 0.00784 -0.03016 O7 5 0.654087 0.437937 0.530660 11.00000 0.07583 0.04794 = 0.06938 -0.00400 0.02781 -0.02064 C1 1 0.239574 0.145319 0.588133 11.00000 0.04537 0.03133 = 0.03902 -0.00010 0.01086 -0.00527 C2 1 0.182984 0.169095 0.637589 11.00000 0.05465 0.03860 = 0.04080 0.00459 0.01555 -0.00525 AFIX 23 H2A 2 0.110138 0.149911 0.634427 11.00000 -1.20000 H2B 2 0.221598 0.151853 0.672452 11.00000 -1.20000 AFIX 0 C3 1 0.162110 0.122933 0.540064 11.00000 0.06221 0.04109 = 0.05388 -0.01364 0.01004 -0.00680 AFIX 137 H3A 2 0.126584 0.078282 0.549135 11.00000 -1.50000 H3B 2 0.199745 0.114722 0.507934 11.00000 -1.50000 H3C 2 0.109662 0.161247 0.531890 11.00000 -1.50000 AFIX 0 C4 1 0.320860 0.086807 0.602949 11.00000 0.05653 0.03668 = 0.07836 0.01078 0.02067 0.00170 AFIX 137 H4A 2 0.285789 0.043446 0.614946 11.00000 -1.50000 H4B 2 0.372630 0.103925 0.632715 11.00000 -1.50000 H4C 2 0.356745 0.075200 0.570772 11.00000 -1.50000 AFIX 0 C5 1 0.251425 0.263618 0.598765 11.00000 0.04358 0.03267 = 0.03124 -0.00133 0.01494 -0.00012 C6 1 0.272268 0.342799 0.592419 11.00000 0.06024 0.02959 = 0.04444 -0.00555 0.02244 0.00046 AFIX 23 H6A 2 0.209309 0.370761 0.599877 11.00000 -1.20000 H6B 2 0.331946 0.357666 0.619425 11.00000 -1.20000 AFIX 0 SIMU 0.01 O3 > C14' DELU 0.01 O3 > C14' PART 1 10.75 O3 5 0.264094 0.280061 0.439840 10.75000 0.04449 0.04427 = 0.02779 -0.00320 0.01265 0.00171 O4 5 0.426813 0.194117 0.421807 10.75000 0.05456 0.04224 = 0.04819 -0.00987 0.02049 0.00250 O5 5 0.526424 0.154987 0.525340 10.75000 0.06880 0.07822 = 0.05331 -0.00447 -0.00124 0.03188 C7 1 0.198779 0.359292 0.502540 10.75000 0.04797 0.04129 = 0.02886 0.00182 0.00970 0.01435 AFIX 23 H7A 2 0.161579 0.405589 0.506641 10.75000 -1.20000 H7B 2 0.152544 0.319445 0.512236 10.75000 -1.20000 AFIX 0 C8 1 0.222941 0.350606 0.443986 10.75000 0.05575 0.04458 = 0.02799 -0.00031 0.00793 0.01020 AFIX 23 H8A 2 0.158040 0.356664 0.418191 10.75000 -1.20000 H8B 2 0.275205 0.387116 0.435212 10.75000 -1.20000 AFIX 0 C9 1 0.278548 0.260369 0.383764 10.75000 0.05827 0.05393 = 0.02969 -0.00805 0.01140 0.00079 AFIX 23 H9A 2 0.323478 0.296215 0.367479 10.75000 -1.20000 H9B 2 0.209810 0.257390 0.360703 10.75000 -1.20000 AFIX 0 C10 1 0.330963 0.188277 0.388425 10.75000 0.06029 0.05681 = 0.04406 -0.01078 0.01725 -0.00493 AFIX 23 H10A 2 0.284846 0.152980 0.404464 10.75000 -1.20000 H10B 2 0.343514 0.170860 0.351549 10.75000 -1.20000 AFIX 0 C11 1 0.481712 0.128263 0.430255 10.75000 0.06429 0.04339 = 0.05986 -0.00979 0.02245 0.01569 AFIX 23 H11A 2 0.509847 0.113039 0.396050 10.75000 -1.20000 H11B 2 0.433676 0.090074 0.440935 10.75000 -1.20000 AFIX 0 C12 1 0.570001 0.139393 0.474830 10.75000 0.05758 0.06279 = 0.07858 -0.01410 0.02110 0.02237 AFIX 23 H12A 2 0.614210 0.095358 0.479265 10.75000 -1.20000 H12B 2 0.614862 0.180090 0.465276 10.75000 -1.20000 AFIX 0 C13 1 0.584006 0.158381 0.578102 10.75000 0.05120 0.08687 = 0.06195 0.01426 0.00494 0.01688 AFIX 23 H13A 2 0.645069 0.125128 0.579902 10.75000 -1.20000 H13B 2 0.538521 0.143136 0.606149 10.75000 -1.20000 AFIX 0 C14 1 0.619932 0.230388 0.588997 10.75000 0.05934 0.09071 = 0.06164 0.03114 -0.00100 -0.00179 AFIX 23 H14A 2 0.665050 0.244763 0.560547 10.75000 -1.20000 H14B 2 0.664256 0.231175 0.624839 10.75000 -1.20000 AFIX 0 PART 2 10.25 DFIX 1.49 0.01 O2 C7' O3' C8' O3' C9' O4' C10' O4' C11' O5' C12' O5' C13' DFIX 1.49 0.01 O6 C14' DFIX 1.52 0.01 C7' C8' C9' C10' C11' C12' C13' C14' O3' 5 0.279768 0.280561 0.434861 10.25000 0.04932 0.04896 = 0.03461 -0.00131 0.01014 0.00847 O4' 5 0.377342 0.146746 0.445350 10.25000 0.06672 0.05429 = 0.05935 -0.00500 0.01865 0.00538 O5' 5 0.536917 0.169843 0.511075 10.25000 0.06190 0.06113 = 0.04904 0.01806 0.02634 0.00750 C7' 1 0.237345 0.381416 0.487072 10.25000 0.06050 0.05142 = 0.03977 0.00065 0.00502 0.01348 AFIX 23 H7'A 2 0.284869 0.406889 0.464253 10.25000 -1.20000 H7'B 2 0.180814 0.415300 0.494769 10.25000 -1.20000 AFIX 0 C8' 1 0.189526 0.316163 0.456473 10.25000 0.05072 0.05034 = 0.03935 0.00189 0.00573 0.01246 AFIX 23 H8'A 2 0.156288 0.283514 0.481487 10.25000 -1.20000 H8'B 2 0.135822 0.330985 0.426223 10.25000 -1.20000 AFIX 0 C9' 1 0.234711 0.216237 0.404396 10.25000 0.05816 0.05425 = 0.04083 -0.01020 0.00709 -0.00341 AFIX 23 H9'A 2 0.190832 0.231106 0.370358 10.25000 -1.20000 H9'B 2 0.190467 0.187962 0.427306 10.25000 -1.20000 AFIX 0 C10' 1 0.328595 0.171657 0.390873 10.25000 0.06222 0.05359 = 0.04417 -0.01537 0.01510 -0.00406 AFIX 23 H10D 2 0.305454 0.130199 0.366965 10.25000 -1.20000 H10E 2 0.378446 0.201536 0.372435 10.25000 -1.20000 AFIX 0 C11' 1 0.477869 0.108228 0.440451 10.25000 0.06646 0.05531 = 0.06553 -0.01112 0.02279 0.01560 AFIX 23 H11D 2 0.525838 0.138987 0.421464 10.25000 -1.20000 H11E 2 0.464415 0.062980 0.419263 10.25000 -1.20000 AFIX 0 C12' 1 0.526556 0.091559 0.498495 10.25000 0.06902 0.06335 = 0.07089 -0.00168 0.02000 0.02061 AFIX 23 H12D 2 0.478128 0.065972 0.520739 10.25000 -1.20000 H12E 2 0.595061 0.066107 0.500064 10.25000 -1.20000 AFIX 0 C13' 1 0.620152 0.190191 0.554934 10.25000 0.03595 0.05975 = 0.03497 0.02612 0.01796 0.00872 AFIX 23 H13D 2 0.663916 0.229065 0.541471 10.25000 -1.20000 H13E 2 0.666313 0.147963 0.564360 10.25000 -1.20000 AFIX 0 C14' 1 0.574458 0.216123 0.606160 10.25000 0.02749 0.08160 = 0.03612 0.02736 0.02033 -0.00277 AFIX 23 H14D 2 0.518193 0.183293 0.615870 10.25000 -1.20000 H14E 2 0.629832 0.219848 0.637744 10.25000 -1.20000 AFIX 0 PART 0 C15 1 0.578153 0.353552 0.590083 11.00000 0.07285 0.06889 = 0.04155 -0.00865 0.01036 -0.02677 AFIX 23 H15A 2 0.647274 0.352680 0.612914 11.00000 -1.20000 H15B 2 0.532421 0.388571 0.606685 11.00000 -1.20000 AFIX 0 C16 1 0.593556 0.378251 0.533014 11.00000 0.05633 0.04742 = 0.04971 -0.00231 0.01909 -0.00934 C17 1 0.663579 0.447724 0.473369 11.00000 0.09102 0.05176 = 0.07351 0.00572 0.03930 -0.01112 AFIX 23 H17A 2 0.737565 0.440609 0.466019 11.00000 -1.20000 H17B 2 0.641111 0.497038 0.461533 11.00000 -1.20000 AFIX 0 C18 1 0.591517 0.390854 0.442609 11.00000 0.05813 0.04150 = 0.04999 0.01266 0.02723 0.00213 C19 1 0.650622 0.340950 0.407470 11.00000 0.06528 0.05582 = 0.05199 0.00671 0.02941 0.00936 AFIX 137 H19A 2 0.669569 0.367506 0.375427 11.00000 -1.50000 H19B 2 0.605567 0.299830 0.395237 11.00000 -1.50000 H19C 2 0.714829 0.323347 0.429095 11.00000 -1.50000 AFIX 0 C20 1 0.496677 0.423343 0.408941 11.00000 0.08293 0.07734 = 0.07338 0.03380 0.03751 0.03058 AFIX 137 H20A 2 0.520036 0.452668 0.379308 11.00000 -1.50000 H20B 2 0.458011 0.453879 0.432477 11.00000 -1.50000 H20C 2 0.450455 0.384561 0.393194 11.00000 -1.50000 AFIX 0 MOLE 2 B1A 3 0.870626 0.331669 0.243073 11.00000 0.02196 0.01557 = 0.01573 0.00062 0.00548 0.00255 C1A 1 0.746112 0.348713 0.247939 11.00000 0.02331 0.01890 = 0.01562 0.00350 0.00219 -0.00099 C2A 1 0.709075 0.419902 0.252229 11.00000 0.01850 0.02091 = 0.02761 0.00506 0.00807 -0.00010 AFIX 43 H2AA 2 0.758563 0.458450 0.255165 11.00000 -1.20000 AFIX 0 C3A 1 0.602685 0.435813 0.252323 11.00000 0.02289 0.02476 = 0.03610 0.00763 0.00976 0.00085 C4A 1 0.528168 0.381216 0.249230 11.00000 0.01710 0.03435 = 0.04284 0.00938 0.00499 -0.00254 AFIX 43 H4AA 2 0.455558 0.391826 0.250131 11.00000 -1.20000 AFIX 0 C5A 1 0.562462 0.310602 0.244781 11.00000 0.02450 0.03151 = 0.03813 0.00791 0.00018 -0.01068 C6A 1 0.668407 0.294917 0.243744 11.00000 0.02735 0.02218 = 0.02764 0.00328 0.00005 -0.00239 AFIX 43 H6AA 2 0.689031 0.245985 0.240061 11.00000 -1.20000 AFIX 0 C7A 1 0.571202 0.513813 0.256089 11.00000 0.02625 0.03136 = 0.06460 0.01371 0.01797 0.00847 C8A 1 0.484036 0.250250 0.243101 11.00000 0.03169 0.04436 = 0.06724 0.00659 0.00439 -0.01432 PART 1 10.70 SIMU 0.01 C9A > F12" DELU 0.01 C9A > F12" C9A 1 0.908488 0.255591 0.272527 10.70000 0.02475 0.01653 = 0.01528 -0.00437 0.00285 0.00251 C10A 1 0.856395 0.222677 0.313262 10.70000 0.02963 0.01917 = 0.01961 0.00398 0.00311 0.00525 AFIX 43 H10C 2 0.794747 0.244748 0.324019 10.70000 -1.20000 AFIX 0 C11A 1 0.892487 0.158462 0.338443 10.70000 0.03152 0.02590 = 0.02465 0.00687 0.00752 0.00805 C12A 1 0.981544 0.124483 0.324136 10.70000 0.03028 0.02132 = 0.02947 0.00677 0.00097 0.00611 AFIX 43 H12C 2 1.004931 0.080071 0.340737 10.70000 -1.20000 AFIX 0 C13A 1 1.036163 0.156938 0.284790 10.70000 0.02038 0.01637 = 0.02835 -0.00113 0.00060 0.00334 C14A 1 1.000515 0.221641 0.260446 10.70000 0.02594 0.01548 = 0.02012 0.00035 0.00351 -0.00106 AFIX 43 H14C 2 1.040534 0.243561 0.234540 10.70000 -1.20000 AFIX 0 C15A 1 0.830781 0.125425 0.380480 10.70000 0.04794 0.03593 = 0.03436 0.01813 0.01585 0.01405 C16A 1 1.132059 0.122629 0.267155 10.70000 0.02739 0.01729 = 0.03703 0.00026 0.00193 -0.00072 REM PART 1 10.70 DFIX 1.34 0.01 C15A F7A C15A F8A C15A F9A C15" F7A" C15" F8A" C15" F9A" DFIX 1.34 0.01 C16" F10" C16" F11" C16" F12" DFIX 2.15 0.01 F10" F11" F11" F12" F12" F10" DFIX 2.15 0.01 F7A F8A F8A F9A F9A F7A F7A" F8A" F8A" F9A" F9A" F7A" F7A 6 0.829265 0.171443 0.423580 10.70000 0.09330 0.06116 = 0.01972 0.00161 0.01895 -0.01444 F8A 6 0.731230 0.113882 0.362072 10.70000 0.03905 0.05023 = 0.04152 0.01506 0.01901 -0.00333 F9A 6 0.870664 0.063807 0.401845 10.70000 0.07082 0.05694 = 0.06689 0.04597 0.02414 0.01804 F10A 6 1.176298 0.073007 0.303399 10.70000 0.03615 0.03151 = 0.05764 0.01675 0.00426 0.01397 F11A 6 1.113102 0.087162 0.219041 10.70000 0.03505 0.04349 = 0.05032 -0.01880 0.00273 0.00788 F12A 6 1.207938 0.170273 0.260466 10.70000 0.02303 0.02636 = 0.05939 0.00145 0.00939 0.00169 PART 2 10.30 SAME 0.005 c9A > c16A C9" 1 0.916377 0.253262 0.269593 10.30000 0.02577 0.01739 = 0.01745 0.00329 0.00308 -0.00295 C10" 1 0.873814 0.221023 0.313816 10.30000 0.02539 0.02632 = 0.02214 0.00022 0.00724 0.00832 AFIX 43 H10" 2 0.815881 0.243547 0.328134 10.30000 -1.20000 AFIX 0 C11" 1 0.914056 0.156803 0.337429 10.30000 0.03521 0.02552 = 0.02762 0.01270 0.01015 0.00467 C12" 1 1.001579 0.124562 0.319798 10.30000 0.02537 0.02172 = 0.03101 0.00289 0.00835 0.00900 AFIX 43 H12" 2 1.029010 0.080822 0.335924 10.30000 -1.20000 AFIX 0 C13" 1 1.048712 0.157500 0.277926 10.30000 0.02496 0.01616 = 0.02365 0.00411 0.00491 0.00079 C14" 1 1.006422 0.220634 0.253696 10.30000 0.02195 0.01498 = 0.01927 0.00149 0.00179 0.00111 AFIX 43 H14" 2 1.040260 0.242292 0.225235 10.30000 -1.20000 AFIX 0 C15" 1 0.871100 0.129764 0.388001 10.30000 0.05213 0.04663 = 0.04540 0.02253 0.01796 0.00767 C16" 1 1.140607 0.123965 0.255550 10.30000 0.02374 0.02044 = 0.03102 0.00182 0.00635 0.00834 F7A" 6 0.773558 0.151878 0.392418 10.30000 0.08539 0.10494 = 0.10271 0.04998 0.05623 0.02630 F8A" 6 0.867605 0.057243 0.386919 10.30000 0.06745 0.04395 = 0.03345 0.01984 0.01082 -0.01691 F9A" 6 0.929686 0.147963 0.434993 10.30000 0.11996 0.09180 = 0.04213 -0.00321 0.03265 -0.01937 F10" 6 1.177075 0.068004 0.286394 10.30000 0.04845 0.02413 = 0.03548 0.00976 0.01645 0.01962 F11" 6 1.115552 0.099062 0.204522 10.30000 0.03879 0.03954 = 0.02560 -0.00676 0.00819 0.00456 F12" 6 1.220563 0.170185 0.253049 10.30000 0.02222 0.02853 = 0.04843 0.00448 0.00707 -0.00040 PART 0 C17A 1 0.880517 0.331577 0.176927 11.00000 0.01930 0.01728 = 0.01829 -0.00263 0.00363 0.00096 C18A 1 0.891632 0.269147 0.145760 11.00000 0.03043 0.01769 = 0.02182 -0.00344 0.00250 0.00361 AFIX 43 H18A 2 0.896729 0.223601 0.163752 11.00000 -1.20000 AFIX 0 C19A 1 0.895437 0.271689 0.089443 11.00000 0.03812 0.02390 = 0.02621 -0.00906 0.00381 0.00642 C20A 1 0.884455 0.335860 0.060976 11.00000 0.03938 0.03216 = 0.01711 -0.00518 0.00565 0.00528 AFIX 43 H20D 2 0.886843 0.337270 0.022411 11.00000 -1.20000 AFIX 0 C21A 1 0.869732 0.398648 0.090476 11.00000 0.02906 0.02295 = 0.01750 -0.00157 0.00331 0.00333 C22A 1 0.868872 0.396633 0.147078 11.00000 0.02479 0.01823 = 0.01554 -0.00210 0.00329 0.00179 AFIX 43 H22A 2 0.860162 0.440485 0.166207 11.00000 -1.20000 AFIX 0 C23A 1 0.911571 0.202800 0.059120 11.00000 0.05685 0.03364 = 0.03214 -0.01215 0.00279 0.00594 C24A 1 0.853877 0.468569 0.060300 11.00000 0.04236 0.02743 = 0.01554 -0.00070 0.00393 0.00453 C25A 1 0.947349 0.391991 0.276104 11.00000 0.02097 0.01436 = 0.01761 0.00260 0.00656 0.00464 C26A 1 1.037845 0.421326 0.257449 11.00000 0.02092 0.02141 = 0.01732 -0.00083 0.00576 0.00473 AFIX 43 H26A 2 1.053027 0.410131 0.221361 11.00000 -1.20000 AFIX 0 C27A 1 1.106117 0.466182 0.289851 11.00000 0.01818 0.02524 = 0.02461 0.00299 0.00629 0.00029 C28A 1 1.087433 0.484461 0.342640 11.00000 0.02227 0.01933 = 0.02315 0.00097 0.00042 -0.00100 AFIX 43 H28A 2 1.133946 0.515459 0.364755 11.00000 -1.20000 AFIX 0 C29A 1 0.998442 0.455887 0.362008 11.00000 0.02764 0.01649 = 0.01465 0.00116 0.00509 0.00167 C30A 1 0.930740 0.410926 0.329601 11.00000 0.02139 0.01610 = 0.01968 0.00139 0.00901 0.00000 AFIX 43 H30A 2 0.870586 0.392192 0.344312 11.00000 -1.20000 AFIX 0 C31A 1 1.206339 0.491820 0.269953 11.00000 0.02965 0.04692 = 0.03808 -0.00523 0.01344 -0.01142 C32A 1 0.973838 0.472736 0.418840 11.00000 0.04092 0.02106 = 0.01945 -0.00121 0.00802 -0.00406 SIMU 0.01 F1A > F24A DELU 0.01 F1A > F24A PART 1 DFIX 1.34 0.01 C7A F1A C7A F21A C7A F3A C7A F1' C7A F2' C7A F3' DFIX 2.15 0.01 F1A F2A F2A F3A F3A F1A F1' F2' F2' F3' F3' F1' F1A 6 0.571409 0.545516 0.207616 10.60000 0.08036 0.03486 = 0.09162 0.03362 0.01505 0.00763 F2A 6 0.637415 0.551647 0.291171 10.60000 0.03591 0.03136 = 0.11587 -0.02695 0.01093 0.00782 F3A 6 0.477761 0.522911 0.273751 10.60000 0.03888 0.03413 = 0.10695 0.00053 0.04402 0.00607 DFIX 1.34 0.01 C8A F4A C8A F5A C8A F6A C8A F4' C8A F5' C8A F6' DFIX 2.15 0.01 F4A F5A F5A F6A F6A F4A F4' F5' F5' F6' F6' F4' F4A 6 0.396886 0.264201 0.207178 10.60000 0.03221 0.05983 = 0.08317 0.00651 -0.02330 -0.02286 F5A 6 0.457183 0.233076 0.289380 10.60000 0.07763 0.08619 = 0.05905 -0.00514 0.03168 -0.05722 F6A 6 0.521353 0.187861 0.221471 10.60000 0.03982 0.03262 = 0.08620 -0.00161 -0.00991 -0.01779 PART 2 F1' 6 0.465030 0.519236 0.244464 10.40000 0.02273 0.05020 = 0.13975 0.00376 0.01793 0.01510 F2' 6 0.607647 0.557023 0.220455 10.40000 0.04783 0.02697 = 0.11687 0.01663 0.05112 0.00415 F3' 6 0.597733 0.541012 0.305152 10.40000 0.12129 0.05400 = 0.08669 -0.01791 0.00771 0.02722 F4' 6 0.386252 0.273148 0.250666 10.40000 0.03260 0.05941 = 0.15351 0.01504 0.00623 -0.02107 F5' 6 0.505818 0.209943 0.291415 10.40000 0.06075 0.06739 = 0.09626 0.02529 0.01670 -0.03630 F6' 6 0.485500 0.204127 0.204986 10.40000 0.09179 0.10374 = 0.05334 -0.02656 0.01941 -0.06771 PART 1 10.40 DFIX 1.34 0.01 C23A F13A C23A F14A C23A F15A C23A F13' C23A F14' C23A F15' DFIX 2.15 0.01 F13' F14' F14' F15' F15' F13' F13A F14A F14A F15A F15A F13A F13A 6 0.825134 0.169392 0.043088 10.40000 0.04135 0.06200 = 0.06314 -0.03782 -0.01209 0.00900 F14A 6 0.977005 0.157033 0.088892 10.40000 0.07769 0.03463 = 0.04946 -0.01570 0.00190 0.02693 F15A 6 0.962848 0.216061 0.013604 10.40000 0.05663 0.04098 = 0.04367 -0.01866 0.02547 0.00759 PART 2 10.35 F13' 6 0.832980 0.154060 0.067712 10.35000 0.03539 0.03583 = 0.05481 -0.03267 -0.03166 0.01680 F14' 6 0.907839 0.210323 0.005834 10.35000 0.09416 0.05401 = 0.03290 -0.02497 -0.00449 0.02076 F15' 6 0.999641 0.167534 0.077671 10.35000 0.03201 0.03393 = 0.05361 -0.01450 0.01287 0.01160 PART 3 10.25 F13" 6 0.832470 0.199905 0.010082 10.25000 0.05587 0.03128 = 0.02913 -0.01821 -0.01225 0.00676 F14" 6 0.869567 0.144045 0.084921 10.25000 0.08960 0.02832 = 0.04537 -0.00750 0.00603 0.00897 F15" 6 0.997044 0.190036 0.046871 10.25000 0.07014 0.06004 = 0.07049 -0.03440 0.00474 0.02495 PART 1 10.55 DFIX 1.34 0.01 C24A F16A C24A F17A C24A F18A C24A F16' C24A F17' C24A F18' DFIX 2.15 0.01 F16A F17A F17A F18A F18A F16A F16' F17' F17' F18' F18' F16' F16A 6 0.770160 0.505180 0.078489 10.55000 0.06448 0.03493 = 0.04882 0.02265 0.02858 0.02499 F17A 6 0.822921 0.458042 0.007591 10.55000 0.08880 0.03103 = 0.01744 0.00219 -0.00845 0.00005 F18A 6 0.932384 0.509943 0.067269 10.55000 0.05291 0.03152 = 0.05398 0.01189 -0.01128 -0.02188 PART 2 10.45 F16' 6 0.848589 0.527659 0.091258 10.45000 0.10151 0.02390 = 0.02285 0.00221 0.00511 0.01136 F17' 6 0.776468 0.469797 0.021105 10.45000 0.05453 0.03803 = 0.05833 0.02001 -0.02802 -0.01031 F18' 6 0.941811 0.486794 0.032920 10.45000 0.04790 0.04679 = 0.07063 0.02746 0.02132 0.00459 PART 1 10.50 ISOR 0.001 F19' F21A DFIX 1.34 0.01 C31A F19A C31A F20A C31A F21A C31A F19' C31A F20' C31A F21' DFIX 2.15 0.01 F19A F20A F20A F21A F21A F19A F19' F20' F20' F21' F21' F19' F19A 6 1.212892 0.484586 0.216899 10.50000 0.04459 0.06021 = 0.04666 -0.01920 0.03473 -0.02107 F20A 6 1.290713 0.462762 0.297725 10.50000 0.02518 0.10660 = 0.08206 0.01969 0.00722 -0.00652 F21A 6 1.216731 0.566399 0.279007 10.50000 0.03373 0.04329 = 0.04390 -0.00213 0.00689 -0.01295 PART 2 10.50 F19' 6 1.247628 0.550163 0.292519 10.50000 0.03373 0.04329 = 0.04390 -0.00213 0.00689 -0.01295 F20' 6 1.281451 0.439450 0.278486 10.50000 0.01833 0.06945 = 0.08398 0.00565 0.02097 0.00448 F21' 6 1.193018 0.500305 0.215208 10.50000 0.04084 0.05007 = 0.04769 0.00198 0.02862 -0.00326 PART 0 F22A 6 1.051558 0.507662 0.448953 11.00000 0.06399 0.04208 = 0.01982 -0.00814 0.00801 -0.02250 F23A 6 0.887934 0.513950 0.418715 11.00000 0.05939 0.05237 = 0.03270 -0.00704 0.01965 0.02068 F24A 6 0.954362 0.413049 0.446906 11.00000 0.06814 0.02943 = 0.01968 0.00003 0.01570 -0.01380 HKLF 4 REM mo_EI33_0m in P2(1)/c REM R1 = 0.0680 for 8629 Fo > 4sig(Fo) and 0.1199 for all 14080 data REM 1169 parameters refined using 1502 restraints END WGHT 0.0892 5.9579 REM Highest difference peak 0.801, deepest hole -0.535, 1-sigma level 0.068 Q1 1 0.3959 0.3605 0.5779 11.00000 0.05 0.80 Q2 1 1.2780 0.5198 0.3114 11.00000 0.05 0.63 Q3 1 0.5553 0.2542 0.5625 11.00000 0.05 0.60 Q4 1 0.4964 0.5256 0.2098 11.00000 0.05 0.57 Q5 1 0.4951 0.1526 0.4787 11.00000 0.05 0.49 ; _shelx_res_checksum 3443 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.41013(9) 0.25845(7) 0.50694(5) 0.0339(3) Uani 1 1 d . . . . . N1 N 0.2902(2) 0.21353(13) 0.57263(10) 0.0344(6) Uani 1 1 d . . . . . N2 N 0.5548(2) 0.34804(16) 0.48888(12) 0.0463(7) Uani 1 1 d . . . . . O1 O 0.18246(19) 0.24731(12) 0.63530(9) 0.0423(6) Uani 1 1 d . . . . . O2 O 0.29655(18) 0.35825(11) 0.53854(9) 0.0386(5) Uani 1 1 d D . . . . O6 O 0.5330(2) 0.28556(16) 0.59021(10) 0.0577(7) Uani 1 1 d D . . . . O7 O 0.6541(2) 0.43794(14) 0.53066(12) 0.0629(8) Uani 1 1 d . . . . . C1 C 0.2396(3) 0.14532(17) 0.58813(13) 0.0381(7) Uani 1 1 d . . . . . C2 C 0.1830(3) 0.16909(18) 0.63759(14) 0.0439(8) Uani 1 1 d . . . . . H2A H 0.1101 0.1499 0.6344 0.053 Uiso 1 1 calc R U . . . H2B H 0.2216 0.1519 0.6725 0.053 Uiso 1 1 calc R U . . . C3 C 0.1621(3) 0.1229(2) 0.54006(16) 0.0521(9) Uani 1 1 d . . . . . H3A H 0.1266 0.0783 0.5491 0.078 Uiso 1 1 calc R U . . . H3B H 0.1997 0.1147 0.5079 0.078 Uiso 1 1 calc R U . . . H3C H 0.1097 0.1612 0.5319 0.078 Uiso 1 1 calc R U . . . C4 C 0.3209(3) 0.0868(2) 0.60295(18) 0.0562(10) Uani 1 1 d . . . . . H4A H 0.2858 0.0434 0.6149 0.084 Uiso 1 1 calc R U . . . H4B H 0.3726 0.1039 0.6327 0.084 Uiso 1 1 calc R U . . . H4C H 0.3567 0.0752 0.5708 0.084 Uiso 1 1 calc R U . . . C5 C 0.2514(3) 0.26362(16) 0.59876(12) 0.0350(7) Uani 1 1 d . . . . . C6 C 0.2723(3) 0.34280(17) 0.59242(14) 0.0435(8) Uani 1 1 d . . . . . H6A H 0.2093 0.3708 0.5999 0.052 Uiso 1 1 calc R U . . . H6B H 0.3319 0.3577 0.6194 0.052 Uiso 1 1 calc R U . . . O3 O 0.2641(5) 0.2801(4) 0.4398(4) 0.0382(10) Uani 0.75 1 d . U P A 1 O4 O 0.4268(3) 0.19412(17) 0.42181(13) 0.0472(7) Uani 0.75 1 d . U P A 1 O5 O 0.5264(5) 0.1550(3) 0.52534(19) 0.0674(15) Uani 0.75 1 d . U P A 1 C7 C 0.1988(4) 0.3593(3) 0.50254(18) 0.0390(10) Uani 0.75 1 d . U P A 1 H7A H 0.1616 0.4056 0.5066 0.047 Uiso 0.75 1 calc R U P A 1 H7B H 0.1525 0.3194 0.5122 0.047 Uiso 0.75 1 calc R U P A 1 C8 C 0.2229(4) 0.3506(3) 0.44399(18) 0.0425(10) Uani 0.75 1 d . U P A 1 H8A H 0.1580 0.3567 0.4182 0.051 Uiso 0.75 1 calc R U P A 1 H8B H 0.2752 0.3871 0.4352 0.051 Uiso 0.75 1 calc R U P A 1 C9 C 0.2785(4) 0.2604(3) 0.38376(18) 0.0468(10) Uani 0.75 1 d . U P A 1 H9A H 0.3235 0.2962 0.3675 0.056 Uiso 0.75 1 calc R U P A 1 H9B H 0.2098 0.2574 0.3607 0.056 Uiso 0.75 1 calc R U P A 1 C10 C 0.3310(6) 0.1883(4) 0.3884(3) 0.0529(16) Uani 0.75 1 d . U P A 1 H10A H 0.2848 0.1530 0.4045 0.063 Uiso 0.75 1 calc R U P A 1 H10B H 0.3435 0.1709 0.3515 0.063 Uiso 0.75 1 calc R U P A 1 C11 C 0.4817(5) 0.1283(3) 0.4303(3) 0.0547(14) Uani 0.75 1 d . U P A 1 H11A H 0.5098 0.1130 0.3961 0.066 Uiso 0.75 1 calc R U P A 1 H11B H 0.4337 0.0901 0.4409 0.066 Uiso 0.75 1 calc R U P A 1 C12 C 0.5700(5) 0.1394(3) 0.4748(3) 0.0653(13) Uani 0.75 1 d . U P A 1 H12A H 0.6142 0.0954 0.4793 0.078 Uiso 0.75 1 calc R U P A 1 H12B H 0.6149 0.1801 0.4653 0.078 Uiso 0.75 1 calc R U P A 1 C13 C 0.5840(5) 0.1584(4) 0.5781(3) 0.0668(13) Uani 0.75 1 d . U P A 1 H13A H 0.6451 0.1251 0.5799 0.080 Uiso 0.75 1 calc R U P A 1 H13B H 0.5385 0.1431 0.6061 0.080 Uiso 0.75 1 calc R U P A 1 C14 C 0.6199(5) 0.2304(4) 0.5890(3) 0.0712(15) Uani 0.75 1 d . U P A 1 H14A H 0.6650 0.2448 0.5605 0.085 Uiso 0.75 1 calc R U P A 1 H14B H 0.6643 0.2312 0.6248 0.085 Uiso 0.75 1 calc R U P A 1 O3' O 0.2798(15) 0.2806(14) 0.4349(14) 0.044(2) Uani 0.25 1 d D U P A 2 O4' O 0.3773(9) 0.1467(6) 0.4454(4) 0.0592(19) Uani 0.25 1 d D U P A 2 O5' O 0.5369(14) 0.1698(8) 0.5111(6) 0.056(2) Uani 0.25 1 d D U P A 2 C7' C 0.2373(13) 0.3814(7) 0.4871(5) 0.051(3) Uani 0.25 1 d D U P A 2 H7'A H 0.2849 0.4069 0.4643 0.061 Uiso 0.25 1 calc R U P A 2 H7'B H 0.1808 0.4153 0.4948 0.061 Uiso 0.25 1 calc R U P A 2 C8' C 0.1895(12) 0.3162(8) 0.4565(6) 0.047(2) Uani 0.25 1 d D U P A 2 H8'A H 0.1563 0.2835 0.4815 0.056 Uiso 0.25 1 calc R U P A 2 H8'B H 0.1358 0.3310 0.4262 0.056 Uiso 0.25 1 calc R U P A 2 C9' C 0.2347(12) 0.2162(8) 0.4044(6) 0.051(2) Uani 0.25 1 d D U P A 2 H9'A H 0.1908 0.2311 0.3704 0.061 Uiso 0.25 1 calc R U P A 2 H9'B H 0.1905 0.1880 0.4273 0.061 Uiso 0.25 1 calc R U P A 2 C10' C 0.3286(19) 0.1717(14) 0.3909(7) 0.053(2) Uani 0.25 1 d D U P A 2 H10D H 0.3055 0.1302 0.3670 0.063 Uiso 0.25 1 calc R U P A 2 H10E H 0.3784 0.2015 0.3724 0.063 Uiso 0.25 1 calc R U P A 2 C11' C 0.4779(14) 0.1082(13) 0.4405(8) 0.061(2) Uani 0.25 1 d D U P A 2 H11D H 0.5258 0.1390 0.4215 0.074 Uiso 0.25 1 calc R U P A 2 H11E H 0.4644 0.0630 0.4193 0.074 Uiso 0.25 1 calc R U P A 2 C12' C 0.5266(15) 0.0916(8) 0.4985(7) 0.067(2) Uani 0.25 1 d D U P A 2 H12D H 0.4781 0.0660 0.5207 0.080 Uiso 0.25 1 calc R U P A 2 H12E H 0.5951 0.0661 0.5001 0.080 Uiso 0.25 1 calc R U P A 2 C13' C 0.6202(10) 0.1902(8) 0.5549(5) 0.042(2) Uani 0.25 1 d D U P A 2 H13D H 0.6639 0.2291 0.5415 0.051 Uiso 0.25 1 calc R U P A 2 H13E H 0.6663 0.1480 0.5644 0.051 Uiso 0.25 1 calc R U P A 2 C14' C 0.5745(11) 0.2161(6) 0.6062(5) 0.047(2) Uani 0.25 1 d D U P A 2 H14D H 0.5182 0.1833 0.6159 0.057 Uiso 0.25 1 calc R U P A 2 H14E H 0.6298 0.2198 0.6377 0.057 Uiso 0.25 1 calc R U P A 2 C15 C 0.5782(4) 0.3536(2) 0.59008(16) 0.0608(11) Uani 1 1 d . . . . . H15A H 0.6473 0.3527 0.6129 0.073 Uiso 1 1 calc R U . . . H15B H 0.5324 0.3886 0.6067 0.073 Uiso 1 1 calc R U . . . C16 C 0.5936(3) 0.3783(2) 0.53301(16) 0.0502(9) Uani 1 1 d . . . . . C17 C 0.6636(4) 0.4477(2) 0.47337(19) 0.0698(13) Uani 1 1 d . . . . . H17A H 0.7376 0.4406 0.4660 0.084 Uiso 1 1 calc R U . . . H17B H 0.6411 0.4970 0.4615 0.084 Uiso 1 1 calc R U . . . C18 C 0.5915(3) 0.39085(19) 0.44261(15) 0.0483(9) Uani 1 1 d . . . . . C19 C 0.6506(3) 0.3410(2) 0.40747(16) 0.0560(10) Uani 1 1 d . . . . . H19A H 0.6696 0.3675 0.3754 0.084 Uiso 1 1 calc R U . . . H19B H 0.6056 0.2998 0.3952 0.084 Uiso 1 1 calc R U . . . H19C H 0.7148 0.3233 0.4291 0.084 Uiso 1 1 calc R U . . . C20 C 0.4967(4) 0.4233(3) 0.40894(19) 0.0757(15) Uani 1 1 d . . . . . H20A H 0.5200 0.4527 0.3793 0.114 Uiso 1 1 calc R U . . . H20B H 0.4580 0.4539 0.4325 0.114 Uiso 1 1 calc R U . . . H20C H 0.4505 0.3846 0.3932 0.114 Uiso 1 1 calc R U . . . B1A B 0.8706(2) 0.33167(14) 0.24307(11) 0.0175(5) Uani 1 1 d . . . . . C1A C 0.7461(2) 0.34871(13) 0.24794(10) 0.0193(5) Uani 1 1 d . . . . . C2A C 0.7091(2) 0.41990(14) 0.25223(11) 0.0219(5) Uani 1 1 d . . . . . H2AA H 0.7586 0.4585 0.2552 0.026 Uiso 1 1 calc R U . . . C3A C 0.6027(2) 0.43581(15) 0.25232(12) 0.0274(6) Uani 1 1 d . . . . . C4A C 0.5282(2) 0.38122(16) 0.24923(13) 0.0313(6) Uani 1 1 d . . . . . H4AA H 0.4556 0.3918 0.2501 0.038 Uiso 1 1 calc R U . . . C5A C 0.5625(2) 0.31060(16) 0.24478(13) 0.0316(7) Uani 1 1 d . . . . . C6A C 0.6684(2) 0.29492(15) 0.24374(11) 0.0260(6) Uani 1 1 d . . . . . H6AA H 0.6890 0.2460 0.2401 0.031 Uiso 1 1 calc R U . . . C7A C 0.5712(2) 0.51381(17) 0.25609(14) 0.0398(8) Uani 1 1 d D . . . . C8A C 0.4840(3) 0.25025(18) 0.24310(15) 0.0479(9) Uani 1 1 d D . . . . C9A C 0.9085(12) 0.2556(7) 0.2725(6) 0.0188(11) Uani 0.7 1 d D U P B 1 C10A C 0.8564(8) 0.2227(5) 0.3133(5) 0.0228(13) Uani 0.7 1 d D U P B 1 H10C H 0.7947 0.2447 0.3240 0.027 Uiso 0.7 1 calc R U P B 1 C11A C 0.8925(6) 0.1585(4) 0.3384(3) 0.0270(12) Uani 0.7 1 d D U P B 1 C12A C 0.9815(7) 0.1245(5) 0.3241(4) 0.0272(12) Uani 0.7 1 d D U P B 1 H12C H 1.0049 0.0801 0.3407 0.033 Uiso 0.7 1 calc R U P B 1 C13A C 1.0362(7) 0.1569(5) 0.2848(4) 0.0219(10) Uani 0.7 1 d D U P B 1 C14A C 1.0005(10) 0.2216(6) 0.2604(5) 0.0204(13) Uani 0.7 1 d D U P B 1 H14C H 1.0405 0.2436 0.2345 0.025 Uiso 0.7 1 calc R U P B 1 C15A C 0.8308(4) 0.1254(3) 0.3805(2) 0.0386(11) Uani 0.7 1 d D U P B 1 C16A C 1.1321(5) 0.1226(4) 0.2672(3) 0.0274(12) Uani 0.7 1 d D U P B 1 F7A F 0.8293(3) 0.17144(17) 0.42358(11) 0.0571(9) Uani 0.7 1 d D U P B 1 F8A F 0.7312(2) 0.11388(16) 0.36207(11) 0.0425(7) Uani 0.7 1 d D U P B 1 F9A F 0.8707(6) 0.0638(3) 0.4018(3) 0.0636(17) Uani 0.7 1 d D U P B 1 F10A F 1.1763(6) 0.0730(4) 0.3034(2) 0.0418(13) Uani 0.7 1 d . U P B 1 F11A F 1.1131(7) 0.0872(4) 0.2190(2) 0.0431(14) Uani 0.7 1 d . U P B 1 F12A F 1.2079(8) 0.1703(5) 0.2605(5) 0.0359(16) Uani 0.7 1 d . U P B 1 C9" C 0.916(3) 0.2533(18) 0.2696(16) 0.020(2) Uani 0.3 1 d D U P B 2 C10" C 0.874(2) 0.2210(13) 0.3138(12) 0.024(2) Uani 0.3 1 d D U P B 2 H10" H 0.8159 0.2435 0.3281 0.029 Uiso 0.3 1 calc R U P B 2 C11" C 0.9141(15) 0.1568(11) 0.3374(8) 0.0289(19) Uani 0.3 1 d D U P B 2 C12" C 1.0016(17) 0.1246(11) 0.3198(10) 0.026(2) Uani 0.3 1 d D U P B 2 H12" H 1.0290 0.0808 0.3359 0.031 Uiso 0.3 1 calc R U P B 2 C13" C 1.0487(18) 0.1575(12) 0.2779(10) 0.0214(18) Uani 0.3 1 d D U P B 2 C14" C 1.006(2) 0.2206(14) 0.2537(13) 0.019(2) Uani 0.3 1 d D U P B 2 H14" H 1.0403 0.2423 0.2252 0.023 Uiso 0.3 1 calc R U P B 2 C15" C 0.8711(8) 0.1298(6) 0.3880(4) 0.047(2) Uani 0.3 1 d D U P B 2 C16" C 1.1406(11) 0.1240(9) 0.2555(6) 0.025(2) Uani 0.3 1 d D U P B 2 F7A" F 0.7736(7) 0.1519(6) 0.3924(5) 0.094(3) Uani 0.3 1 d D U P B 2 F8A" F 0.8676(12) 0.0572(5) 0.3869(6) 0.048(3) Uani 0.3 1 d D U P B 2 F9A" F 0.9297(8) 0.1480(5) 0.4350(3) 0.083(2) Uani 0.3 1 d D U P B 2 F10" F 1.1771(16) 0.0680(9) 0.2864(4) 0.035(2) Uani 0.3 1 d D U P B 2 F11" F 1.1156(16) 0.0991(10) 0.2045(5) 0.034(3) Uani 0.3 1 d D U P B 2 F12" F 1.2206(19) 0.1702(12) 0.2530(10) 0.033(3) Uani 0.3 1 d D U P B 2 C17A C 0.88052(19) 0.33158(13) 0.17693(10) 0.0182(5) Uani 1 1 d . . . . . C18A C 0.8916(2) 0.26915(14) 0.14576(11) 0.0233(5) Uani 1 1 d . . . . . H18A H 0.8967 0.2236 0.1638 0.028 Uiso 1 1 calc R U . . . C19A C 0.8954(2) 0.27169(15) 0.08944(11) 0.0294(6) Uani 1 1 d . . . . . C20A C 0.8845(2) 0.33586(15) 0.06098(11) 0.0294(6) Uani 1 1 d . . . . . H20D H 0.8868 0.3373 0.0224 0.035 Uiso 1 1 calc R U . . . C21A C 0.8697(2) 0.39865(14) 0.09048(10) 0.0231(5) Uani 1 1 d . . . . . C22A C 0.8689(2) 0.39663(13) 0.14708(10) 0.0194(5) Uani 1 1 d . . . . . H22A H 0.8602 0.4405 0.1662 0.023 Uiso 1 1 calc R U . . . C23A C 0.9116(3) 0.20280(17) 0.05912(12) 0.0410(8) Uani 1 1 d D . . . . C24A C 0.8539(2) 0.46857(15) 0.06030(10) 0.0284(6) Uani 1 1 d D . . . . C25A C 0.9473(2) 0.39199(12) 0.27610(10) 0.0173(5) Uani 1 1 d . . . . . C26A C 1.0378(2) 0.42133(13) 0.25745(10) 0.0196(5) Uani 1 1 d . . . . . H26A H 1.0530 0.4101 0.2214 0.024 Uiso 1 1 calc R U . . . C27A C 1.1061(2) 0.46618(14) 0.28985(11) 0.0224(5) Uani 1 1 d . . . . . C28A C 1.0874(2) 0.48446(13) 0.34264(11) 0.0217(5) Uani 1 1 d . . . . . H28A H 1.1339 0.5155 0.3648 0.026 Uiso 1 1 calc R U . . . C29A C 0.9984(2) 0.45589(13) 0.36201(10) 0.0194(5) Uani 1 1 d . . . . . C30A C 0.9307(2) 0.41093(13) 0.32960(10) 0.0185(5) Uani 1 1 d . . . . . H30A H 0.8706 0.3922 0.3443 0.022 Uiso 1 1 calc R U . . . C31A C 1.2063(2) 0.49182(17) 0.26995(12) 0.0375(7) Uani 1 1 d D . . . . C32A C 0.9738(2) 0.47274(14) 0.41884(11) 0.0268(6) Uani 1 1 d . . . . . F1A F 0.5714(5) 0.5455(4) 0.2076(2) 0.0685(19) Uani 0.6 1 d D U P C 1 F2A F 0.6374(3) 0.5516(3) 0.2912(2) 0.0609(15) Uani 0.6 1 d D U P C 1 F3A F 0.4778(4) 0.5229(3) 0.2738(2) 0.0572(14) Uani 0.6 1 d D U P C 1 F4A F 0.3969(3) 0.2642(2) 0.20718(19) 0.0607(11) Uani 0.6 1 d D U P D 1 F5A F 0.4572(5) 0.2331(3) 0.28938(18) 0.0725(18) Uani 0.6 1 d D U P D 1 F6A F 0.5214(4) 0.1879(2) 0.2215(2) 0.0542(14) Uani 0.6 1 d D U P D 1 F1' F 0.4650(5) 0.5192(6) 0.2445(4) 0.070(3) Uani 0.4 1 d D U P C 2 F2' F 0.6076(6) 0.5570(5) 0.2205(3) 0.061(3) Uani 0.4 1 d D U P C 2 F3' F 0.5977(7) 0.5410(6) 0.3052(3) 0.088(3) Uani 0.4 1 d D U P C 2 F4' F 0.3863(4) 0.2731(3) 0.2507(4) 0.082(2) Uani 0.4 1 d D U P D 2 F5' F 0.5058(6) 0.2099(5) 0.2914(3) 0.074(3) Uani 0.4 1 d D U P D 2 F6' F 0.4855(7) 0.2041(5) 0.2050(3) 0.082(3) Uani 0.4 1 d D U P D 2 F13A F 0.8251(5) 0.1694(5) 0.0431(4) 0.057(2) Uani 0.4 1 d D U P E 1 F14A F 0.9770(7) 0.1570(6) 0.0889(4) 0.054(3) Uani 0.4 1 d D U P E 1 F15A F 0.9628(6) 0.2161(4) 0.0136(3) 0.0456(17) Uani 0.4 1 d D U P E 1 F13' F 0.8330(5) 0.1541(4) 0.0677(4) 0.045(2) Uani 0.35 1 d D U P E 2 F14' F 0.9078(9) 0.2103(5) 0.0058(2) 0.061(2) Uani 0.35 1 d D U P E 2 F15' F 0.9996(5) 0.1675(6) 0.0777(5) 0.039(2) Uani 0.35 1 d D U P E 2 F13" F 0.8325(9) 0.1999(5) 0.0101(4) 0.0401(19) Uani 0.25 1 d . U P E 3 F14" F 0.8696(12) 0.1440(6) 0.0849(5) 0.055(3) Uani 0.25 1 d . U P E 3 F15" F 0.9970(10) 0.1900(7) 0.0469(7) 0.067(3) Uani 0.25 1 d . U P E 3 F16A F 0.7702(3) 0.50518(19) 0.07849(15) 0.0477(10) Uani 0.55 1 d D U P F 1 F17A F 0.8229(4) 0.4580(3) 0.00759(15) 0.0469(13) Uani 0.55 1 d D U P F 1 F18A F 0.9324(3) 0.50994(19) 0.06727(18) 0.0475(10) Uani 0.55 1 d D U P F 1 F16' F 0.8486(5) 0.5277(2) 0.09126(15) 0.0496(12) Uani 0.45 1 d D U P F 2 F17' F 0.7765(4) 0.4698(3) 0.0211(2) 0.0529(17) Uani 0.45 1 d D U P F 2 F18' F 0.9418(3) 0.4868(3) 0.0329(2) 0.0540(13) Uani 0.45 1 d D U P F 2 F19A F 1.2129(10) 0.4846(5) 0.2169(2) 0.048(2) Uani 0.5 1 d D U P G 1 F20A F 1.2907(6) 0.4628(4) 0.2977(3) 0.071(2) Uani 0.5 1 d D U P G 1 F21A F 1.2167(3) 0.5664(2) 0.27901(18) 0.0401(8) Uani 0.5 1 d D U P G 1 F19' F 1.2476(3) 0.5502(2) 0.29252(18) 0.0401(8) Uani 0.5 1 d D U P G 2 F20' F 1.2815(5) 0.4394(3) 0.2785(3) 0.0561(18) Uani 0.5 1 d D U P G 2 F21' F 1.1930(10) 0.5003(6) 0.2152(2) 0.044(2) Uani 0.5 1 d D U P G 2 F22A F 1.05156(16) 0.50766(10) 0.44895(7) 0.0417(5) Uani 1 1 d . U . . . F23A F 0.88793(16) 0.51395(11) 0.41872(7) 0.0470(5) Uani 1 1 d . U . . . F24A F 0.95436(16) 0.41305(9) 0.44691(6) 0.0383(4) Uani 1 1 d . U . . . 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 0.0283(6) 0.0412(7) 0.0333(6) -0.0052(5) 0.0086(5) -0.0007(5) N1 0.0432(16) 0.0293(13) 0.0327(13) 0.0005(10) 0.0126(11) -0.0010(11) N2 0.0547(19) 0.0476(17) 0.0397(16) 0.0048(13) 0.0192(14) -0.0056(14) O1 0.0560(15) 0.0378(12) 0.0371(12) 0.0002(10) 0.0228(11) -0.0008(11) O2 0.0473(14) 0.0336(11) 0.0362(12) 0.0010(9) 0.0107(10) -0.0026(10) O6 0.0510(16) 0.081(2) 0.0415(14) 0.0100(13) 0.0078(12) -0.0302(15) O7 0.076(2) 0.0479(15) 0.0694(19) -0.0040(13) 0.0278(15) -0.0206(14) C1 0.0454(19) 0.0313(15) 0.0390(17) -0.0001(13) 0.0109(15) -0.0053(14) C2 0.055(2) 0.0386(18) 0.0408(18) 0.0046(14) 0.0155(16) -0.0053(16) C3 0.062(3) 0.0411(19) 0.054(2) -0.0136(17) 0.0100(19) -0.0068(18) C4 0.057(2) 0.0367(19) 0.078(3) 0.0108(18) 0.021(2) 0.0017(17) C5 0.0436(19) 0.0327(15) 0.0312(16) -0.0013(13) 0.0149(14) -0.0001(14) C6 0.060(2) 0.0296(16) 0.0444(19) -0.0055(14) 0.0224(17) 0.0005(15) O3 0.044(2) 0.0443(18) 0.028(2) -0.0032(15) 0.0126(17) 0.0017(18) O4 0.0546(19) 0.0422(16) 0.0482(18) -0.0099(14) 0.0205(14) 0.0025(15) O5 0.069(3) 0.078(3) 0.053(3) -0.004(2) -0.001(2) 0.032(2) C7 0.048(3) 0.041(2) 0.029(2) 0.0018(18) 0.0097(19) 0.014(2) C8 0.056(3) 0.045(2) 0.028(2) -0.0003(18) 0.0079(19) 0.010(2) C9 0.058(3) 0.054(2) 0.030(2) -0.0081(19) 0.0114(19) 0.001(2) C10 0.060(3) 0.057(4) 0.044(2) -0.011(2) 0.017(2) -0.005(3) C11 0.064(3) 0.043(3) 0.060(3) -0.010(2) 0.022(2) 0.016(2) C12 0.058(3) 0.063(3) 0.079(3) -0.014(3) 0.021(2) 0.022(2) C13 0.051(3) 0.087(3) 0.062(3) 0.014(3) 0.005(2) 0.017(3) C14 0.059(3) 0.091(4) 0.062(3) 0.031(3) -0.001(3) -0.002(3) O3' 0.049(4) 0.049(4) 0.035(5) -0.001(4) 0.010(4) 0.008(4) O4' 0.067(4) 0.054(4) 0.059(4) -0.005(4) 0.019(3) 0.005(3) O5' 0.062(4) 0.061(4) 0.049(4) 0.018(4) 0.026(4) 0.007(4) C7' 0.061(6) 0.051(5) 0.040(5) 0.001(4) 0.005(5) 0.013(5) C8' 0.051(4) 0.050(4) 0.039(4) 0.002(4) 0.006(4) 0.012(4) C9' 0.058(4) 0.054(4) 0.041(4) -0.010(4) 0.007(4) -0.003(4) C10' 0.062(4) 0.054(5) 0.044(4) -0.015(4) 0.015(4) -0.004(4) C11' 0.066(4) 0.055(5) 0.066(4) -0.011(4) 0.023(4) 0.016(4) C12' 0.069(4) 0.063(4) 0.071(4) -0.002(4) 0.020(4) 0.021(4) C13' 0.036(4) 0.060(4) 0.035(4) 0.026(4) 0.018(3) 0.009(4) C14' 0.027(5) 0.082(6) 0.036(5) 0.027(4) 0.020(4) -0.003(5) C15 0.073(3) 0.069(3) 0.042(2) -0.0087(19) 0.0104(19) -0.027(2) C16 0.056(2) 0.047(2) 0.050(2) -0.0023(17) 0.0191(18) -0.0093(18) C17 0.091(3) 0.052(2) 0.074(3) 0.006(2) 0.039(3) -0.011(2) C18 0.058(2) 0.0415(19) 0.050(2) 0.0127(16) 0.0272(18) 0.0021(17) C19 0.065(3) 0.056(2) 0.052(2) 0.0067(18) 0.029(2) 0.009(2) C20 0.083(3) 0.077(3) 0.073(3) 0.034(2) 0.038(3) 0.031(3) B1A 0.0220(14) 0.0156(12) 0.0157(13) 0.0006(10) 0.0055(11) 0.0026(11) C1A 0.0233(13) 0.0189(11) 0.0156(11) 0.0035(9) 0.0022(10) -0.0010(10) C2A 0.0185(13) 0.0209(12) 0.0276(13) 0.0051(10) 0.0081(10) -0.0001(10) C3A 0.0229(14) 0.0248(13) 0.0361(16) 0.0076(11) 0.0098(12) 0.0008(11) C4A 0.0171(14) 0.0344(15) 0.0428(17) 0.0094(13) 0.0050(12) -0.0025(12) C5A 0.0245(15) 0.0315(15) 0.0381(16) 0.0079(13) 0.0002(12) -0.0107(12) C6A 0.0274(15) 0.0222(13) 0.0276(14) 0.0033(11) 0.0000(11) -0.0024(11) C7A 0.0262(16) 0.0314(16) 0.065(2) 0.0137(16) 0.0180(15) 0.0085(13) C8A 0.0317(19) 0.044(2) 0.067(3) 0.0066(18) 0.0044(17) -0.0143(15) C9A 0.025(3) 0.017(2) 0.015(2) -0.0044(19) 0.0029(18) 0.0025(19) C10A 0.030(4) 0.0192(19) 0.020(2) 0.0040(17) 0.003(2) 0.005(2) C11A 0.032(3) 0.0259(19) 0.0247(19) 0.0069(16) 0.008(2) 0.008(2) C12A 0.030(4) 0.021(2) 0.029(2) 0.0068(18) 0.001(2) 0.006(2) C13A 0.020(3) 0.0164(18) 0.028(3) -0.0011(18) 0.0006(16) 0.0033(18) C14A 0.026(2) 0.0155(19) 0.020(3) 0.000(2) 0.0035(19) -0.0011(18) C15A 0.048(3) 0.036(2) 0.034(2) 0.0181(18) 0.016(2) 0.014(2) C16A 0.027(2) 0.0173(19) 0.037(3) 0.000(2) 0.002(2) -0.0007(17) F7A 0.093(3) 0.0612(19) 0.0197(14) 0.0016(13) 0.0189(15) -0.0144(18) F8A 0.0391(15) 0.0502(16) 0.0415(15) 0.0151(13) 0.0190(12) -0.0033(13) F9A 0.071(3) 0.057(2) 0.067(4) 0.046(2) 0.024(3) 0.018(2) F10A 0.0362(19) 0.032(2) 0.058(3) 0.017(3) 0.004(3) 0.0140(15) F11A 0.035(2) 0.043(3) 0.050(3) -0.019(3) 0.003(3) 0.0079(19) F12A 0.023(3) 0.026(2) 0.059(4) 0.001(2) 0.009(2) 0.0017(17) C9" 0.026(4) 0.017(4) 0.017(4) 0.003(4) 0.003(4) -0.003(4) C10" 0.025(5) 0.026(4) 0.022(4) 0.000(3) 0.007(4) 0.008(4) C11" 0.035(4) 0.026(3) 0.028(3) 0.013(3) 0.010(3) 0.005(3) C12" 0.025(5) 0.022(4) 0.031(4) 0.003(3) 0.008(3) 0.009(4) C13" 0.025(4) 0.016(3) 0.024(4) 0.004(3) 0.005(3) 0.001(3) C14" 0.022(4) 0.015(4) 0.019(5) 0.001(4) 0.002(3) 0.001(3) C15" 0.052(5) 0.047(4) 0.045(4) 0.023(4) 0.018(4) 0.008(4) C16" 0.024(4) 0.020(4) 0.031(5) 0.002(4) 0.006(3) 0.008(3) F7A" 0.085(5) 0.105(6) 0.103(6) 0.050(5) 0.056(4) 0.026(5) F8A" 0.067(5) 0.044(4) 0.033(5) 0.020(3) 0.011(4) -0.017(4) F9A" 0.120(5) 0.092(5) 0.042(3) -0.003(4) 0.033(4) -0.019(5) F10" 0.048(4) 0.024(3) 0.035(5) 0.010(4) 0.016(4) 0.020(3) F11" 0.039(4) 0.040(5) 0.026(4) -0.007(4) 0.008(4) 0.005(4) F12" 0.022(5) 0.029(5) 0.048(6) 0.004(4) 0.007(4) 0.000(4) C17A 0.0193(12) 0.0173(11) 0.0183(12) -0.0026(9) 0.0036(9) 0.0010(10) C18A 0.0304(15) 0.0177(12) 0.0218(13) -0.0034(10) 0.0025(11) 0.0036(11) C19A 0.0381(17) 0.0239(13) 0.0262(14) -0.0091(11) 0.0038(12) 0.0064(12) C20A 0.0394(17) 0.0322(15) 0.0171(12) -0.0052(11) 0.0057(11) 0.0053(13) C21A 0.0291(15) 0.0229(13) 0.0175(12) -0.0016(10) 0.0033(10) 0.0033(11) C22A 0.0248(14) 0.0182(11) 0.0155(12) -0.0021(9) 0.0033(10) 0.0018(10) C23A 0.057(2) 0.0336(17) 0.0321(17) -0.0122(14) 0.0028(16) 0.0059(16) C24A 0.0424(18) 0.0274(14) 0.0155(13) -0.0007(11) 0.0039(12) 0.0045(13) C25A 0.0210(13) 0.0144(11) 0.0176(12) 0.0026(9) 0.0066(9) 0.0046(9) C26A 0.0209(13) 0.0214(12) 0.0173(12) -0.0008(10) 0.0058(10) 0.0047(10) C27A 0.0182(13) 0.0252(13) 0.0246(13) 0.0030(11) 0.0063(10) 0.0003(10) C28A 0.0223(13) 0.0193(12) 0.0231(13) 0.0010(10) 0.0004(10) -0.0010(10) C29A 0.0276(14) 0.0165(11) 0.0147(12) 0.0012(9) 0.0051(10) 0.0017(10) C30A 0.0214(13) 0.0161(11) 0.0197(12) 0.0014(9) 0.0090(10) 0.0000(10) C31A 0.0296(17) 0.0469(19) 0.0381(17) -0.0052(14) 0.0134(14) -0.0114(14) C32A 0.0409(17) 0.0211(13) 0.0195(13) -0.0012(10) 0.0080(12) -0.0041(12) F1A 0.080(4) 0.035(3) 0.092(3) 0.034(2) 0.015(3) 0.008(3) F2A 0.036(2) 0.031(2) 0.116(4) -0.027(2) 0.011(2) 0.0078(17) F3A 0.039(2) 0.0341(19) 0.107(4) 0.001(3) 0.044(3) 0.0061(18) F4A 0.032(2) 0.060(2) 0.083(3) 0.007(2) -0.023(2) -0.0229(17) F5A 0.078(4) 0.086(4) 0.059(3) -0.005(2) 0.032(3) -0.057(3) F6A 0.040(2) 0.0326(18) 0.086(4) -0.002(2) -0.010(2) -0.0178(16) F1' 0.023(3) 0.050(4) 0.140(7) 0.004(5) 0.018(4) 0.015(2) F2' 0.048(4) 0.027(3) 0.117(6) 0.017(4) 0.051(4) 0.004(3) F3' 0.121(7) 0.054(4) 0.087(5) -0.018(4) 0.008(5) 0.027(5) F4' 0.033(3) 0.059(4) 0.154(6) 0.015(4) 0.006(4) -0.021(3) F5' 0.061(5) 0.067(5) 0.096(5) 0.025(4) 0.017(4) -0.036(4) F6' 0.092(6) 0.104(6) 0.053(4) -0.027(4) 0.019(4) -0.068(5) F13A 0.041(3) 0.062(5) 0.063(5) -0.038(4) -0.012(4) 0.009(3) F14A 0.078(5) 0.035(4) 0.049(4) -0.016(3) 0.002(4) 0.027(4) F15A 0.057(4) 0.041(3) 0.044(4) -0.019(3) 0.025(3) 0.008(3) F13' 0.035(3) 0.036(4) 0.055(5) -0.033(4) -0.032(3) 0.017(3) F14' 0.094(6) 0.054(4) 0.033(3) -0.025(3) -0.004(5) 0.021(5) F15' 0.032(3) 0.034(4) 0.054(5) -0.015(4) 0.013(4) 0.012(3) F13" 0.056(5) 0.031(4) 0.029(4) -0.018(3) -0.012(4) 0.007(4) F14" 0.090(6) 0.028(4) 0.045(5) -0.007(4) 0.006(5) 0.009(5) F15" 0.070(5) 0.060(5) 0.070(6) -0.034(5) 0.005(5) 0.025(5) F16A 0.064(3) 0.0349(19) 0.049(2) 0.0226(17) 0.029(2) 0.0250(18) F17A 0.089(4) 0.031(2) 0.0174(17) 0.0022(14) -0.008(2) 0.000(3) F18A 0.053(2) 0.0315(19) 0.054(2) 0.0119(18) -0.011(2) -0.0219(18) F16' 0.102(4) 0.024(2) 0.023(2) 0.0022(16) 0.005(2) 0.011(2) F17' 0.055(3) 0.038(3) 0.058(4) 0.020(3) -0.028(3) -0.010(3) F18' 0.048(3) 0.047(3) 0.071(3) 0.027(3) 0.021(3) 0.005(2) F19A 0.045(5) 0.060(5) 0.047(3) -0.019(3) 0.035(2) -0.021(4) F20A 0.025(3) 0.107(5) 0.082(5) 0.020(4) 0.007(3) -0.007(3) F21A 0.0337(14) 0.0433(13) 0.0439(13) -0.0021(10) 0.0069(11) -0.0129(10) F19' 0.0337(14) 0.0433(13) 0.0439(13) -0.0021(10) 0.0069(11) -0.0129(10) F20' 0.018(3) 0.069(3) 0.084(4) 0.006(3) 0.021(3) 0.004(3) F21' 0.041(4) 0.050(4) 0.048(3) 0.002(2) 0.029(2) -0.003(3) F22A 0.0640(13) 0.0421(10) 0.0198(8) -0.0081(7) 0.0080(8) -0.0225(9) F23A 0.0594(13) 0.0524(11) 0.0327(10) -0.0070(8) 0.0197(9) 0.0207(10) F24A 0.0681(13) 0.0294(9) 0.0197(8) 0.0000(7) 0.0157(8) -0.0138(8) 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O5' Na1 O3' 126.8(5) . . ? O3 Na1 O5 132.5(2) . . ? O3 Na1 O4 68.05(15) . . ? O5 Na1 O4 70.33(14) . . ? O5' Na1 O6 74.4(4) . . ? O3' Na1 O6 157.3(5) . . ? O3 Na1 O6 155.36(16) . . ? O5 Na1 O6 72.00(14) . . ? O4 Na1 O6 134.15(12) . . ? O5' Na1 N1 102.4(4) . . ? O3' Na1 N1 96.4(7) . . ? O3 Na1 N1 90.7(2) . . ? O5 Na1 N1 91.39(15) . . ? O4 Na1 N1 120.81(11) . . ? O6 Na1 N1 84.98(9) . . ? O5' Na1 O2 159.2(4) . . ? O3' Na1 O2 73.6(4) . . ? O3 Na1 O2 69.92(14) . . ? O5 Na1 O2 151.47(13) . . ? O4 Na1 O2 136.94(11) . . ? O6 Na1 O2 86.03(10) . . ? N1 Na1 O2 68.19(8) . . ? O5' Na1 N2 87.2(4) . . ? O3' Na1 N2 102.9(7) . . ? O3 Na1 N2 107.2(2) . . ? O5 Na1 N2 96.01(16) . . ? O4 Na1 N2 91.91(11) . . ? O6 Na1 N2 67.05(9) . . ? N1 Na1 N2 146.95(10) . . ? O2 Na1 N2 91.73(9) . . ? O5' Na1 O4' 61.2(4) . . ? O3' Na1 O4' 68.8(5) . . ? O6 Na1 O4' 133.9(3) . . ? N1 Na1 O4' 92.3(3) . . ? O2 Na1 O4' 135.2(3) . . ? N2 Na1 O4' 119.5(3) . . ? O5' Na1 C13' 27.2(3) . . ? O3' Na1 C13' 151.9(4) . . ? O6 Na1 C13' 47.6(3) . . ? N1 Na1 C13' 100.9(2) . . ? O2 Na1 C13' 133.6(3) . . ? N2 Na1 C13' 73.6(3) . . ? O4' Na1 C13' 88.4(4) . . ? O5' Na1 C14' 51.7(4) . . ? O3' Na1 C14' 174.9(7) . . ? O6 Na1 C14' 26.4(2) . . ? N1 Na1 C14' 79.6(2) . . ? O2 Na1 C14' 107.6(2) . . ? N2 Na1 C14' 82.1(3) . . ? O4' Na1 C14' 107.9(3) . . ? C13' Na1 C14' 28.39(18) . . ? C5 N1 C1 106.7(2) . . ? C5 N1 Na1 112.9(2) . . ? C1 N1 Na1 140.02(19) . . ? C16 N2 C18 106.7(3) . . ? C16 N2 Na1 110.9(2) . . ? C18 N2 Na1 140.0(2) . . ? C5 O1 C2 104.3(2) . . ? C6 O2 C7 107.9(3) . . ? C6 O2 C7' 135.8(8) . . ? C6 O2 Na1 109.39(18) . . ? C7 O2 Na1 108.0(2) . . ? C7' O2 Na1 102.0(6) . . ? C15 O6 C14' 132.6(7) . . ? C15 O6 C14 107.9(4) . . ? C15 O6 Na1 114.0(2) . . ? C14' O6 Na1 102.9(6) . . ? C14 O6 Na1 104.1(3) . . ? C16 O7 C17 104.9(3) . . ? N1 C1 C3 107.4(3) . . ? N1 C1 C4 111.2(3) . . ? C3 C1 C4 111.2(3) . . ? N1 C1 C2 102.4(2) . . ? C3 C1 C2 111.6(3) . . ? C4 C1 C2 112.6(3) . . ? O1 C2 C1 104.8(2) . . ? N1 C5 O1 119.5(3) . . ? N1 C5 C6 125.5(3) . . ? O1 C5 C6 114.9(3) . . ? O2 C6 C5 110.7(2) . . ? C8 O3 C9 112.8(8) . . ? C8 O3 Na1 112.0(4) . . ? C9 O3 Na1 116.0(4) . . ? C10 O4 C11 114.0(5) . . ? C10 O4 Na1 112.6(3) . . ? C11 O4 Na1 112.8(3) . . ? C13 O5 C12 125.6(6) . . ? C13 O5 Na1 112.2(4) . . ? C12 O5 Na1 106.5(4) . . ? O2 C7 C8 108.9(4) . . ? O3 C8 C7 106.5(5) . . ? O3 C9 C10 104.8(6) . . ? O4 C10 C9 109.3(6) . . ? O4 C11 C12 108.1(5) . . ? O5 C12 C11 108.9(5) . . ? O5 C13 C14 109.6(5) . . ? C13 C14 O6 114.5(5) . . ? C8' O3' C9' 105.3(13) . . ? C8' O3' Na1 109.0(17) . . ? C9' O3' Na1 116.4(19) . . ? C10' O4' C11' 110.8(11) . . ? C10' O4' Na1 107.7(12) . . ? C11' O4' Na1 110.5(12) . . ? C13' O5' C12' 116.2(15) . . ? C13' O5' Na1 107.2(10) . . ? C12' O5' Na1 129.9(12) . . ? O2 C7' C8' 109.6(10) . . ? O3' C8' C7' 104.3(13) . . ? O3' C9' C10' 105.9(16) . . ? O4' C10' C9' 103.5(13) . . ? O4' C11' C12' 106.7(14) . . ? O5' C12' C11' 90.8(15) . . ? O5' C13' C14' 111.8(12) . . ? O5' C13' Na1 45.6(8) . . ? C14' C13' Na1 77.7(7) . . ? O6 C14' C13' 102.9(9) . . ? O6 C14' Na1 50.7(5) . . ? C13' C14' Na1 73.9(7) . . ? O6 C15 C16 112.1(3) . . ? N2 C16 O7 119.5(3) . . ? N2 C16 C15 125.5(3) . . ? O7 C16 C15 115.0(3) . . ? O7 C17 C18 106.4(3) . . ? N2 C18 C20 108.9(3) . . ? N2 C18 C19 109.0(3) . . ? C20 C18 C19 110.5(3) . . ? N2 C18 C17 102.2(3) . . ? C20 C18 C17 113.2(4) . . ? C19 C18 C17 112.7(3) . . ? C9A B1A C25A 103.8(8) . . ? C9A B1A C1A 112.0(5) . . ? C25A B1A C1A 111.32(19) . . ? C9A B1A C17A 112.6(5) . . ? C25A B1A C17A 112.4(2) . . ? C1A B1A C17A 104.8(2) . . ? C25A B1A C9" 103.7(19) . . ? C1A B1A C9" 116.0(10) . . ? C17A B1A C9" 108.8(13) . . ? C6A C1A C2A 115.4(2) . . ? C6A C1A B1A 122.9(2) . . ? C2A C1A B1A 121.5(2) . . ? C3A C2A C1A 122.3(2) . . ? C4A C3A C2A 120.7(3) . . ? C4A C3A C7A 121.1(3) . . ? C2A C3A C7A 118.1(2) . . ? C3A C4A C5A 118.1(3) . . ? C6A C5A C4A 121.1(3) . . ? C6A C5A C8A 119.6(3) . . ? C4A C5A C8A 119.3(3) . . ? C5A C6A C1A 122.3(3) . . ? F2' C7A F3' 107.7(6) . . ? F3A C7A F1A 109.3(4) . . ? F3A C7A F2A 104.5(4) . . ? F1A C7A F2A 106.3(4) . . ? F2' C7A F1' 103.7(5) . . ? F3' C7A F1' 108.2(5) . . ? F2' C7A C3A 115.3(5) . . ? F3' C7A C3A 112.4(5) . . ? F3A C7A C3A 113.5(3) . . ? F1A C7A C3A 110.0(4) . . ? F2A C7A C3A 112.9(3) . . ? F1' C7A C3A 109.0(5) . . ? F6' C8A F4' 113.8(5) . . ? F5A C8A F4A 110.1(4) . . ? F5A C8A F6A 106.0(4) . . ? F4A C8A F6A 101.7(4) . . ? F6' C8A F5' 104.3(6) . . ? F4' C8A F5' 98.6(5) . . ? F5A C8A C5A 114.3(4) . . ? F6' C8A C5A 117.2(5) . . ? F4' C8A C5A 112.8(4) . . ? F4A C8A C5A 111.8(3) . . ? F6A C8A C5A 112.1(3) . . ? F5' C8A C5A 107.8(4) . . ? C14A C9A C10A 115.8(3) . . ? C14A C9A B1A 120.7(5) . . ? C10A C9A B1A 123.4(4) . . ? C11A C10A C9A 121.8(4) . . ? C12A C11A C10A 121.1(3) . . ? C12A C11A C15A 120.2(4) . . ? C10A C11A C15A 118.7(4) . . ? C11A C12A C13A 118.2(3) . . ? C12A C13A C14A 120.3(4) . . ? C12A C13A C16A 120.8(3) . . ? C14A C13A C16A 118.9(4) . . ? C13A C14A C9A 122.6(4) . . ? F8A C15A F9A 107.9(5) . . ? F8A C15A F7A 105.7(4) . . ? F9A C15A F7A 105.6(4) . . ? F8A C15A C11A 113.1(5) . . ? F9A C15A C11A 114.4(5) . . ? F7A C15A C11A 109.6(5) . . ? F12A C16A F11A 106.0(5) . . ? F12A C16A F10A 105.9(5) . . ? F11A C16A F10A 105.3(5) . . ? F12A C16A C13A 112.8(7) . . ? F11A C16A C13A 113.0(7) . . ? F10A C16A C13A 113.2(5) . . ? C14" C9" C10" 115.9(5) . . ? C14" C9" B1A 122.1(9) . . ? C10" C9" B1A 121.5(9) . . ? C11" C10" C9" 121.9(6) . . ? C12" C11" C10" 120.8(5) . . ? C12" C11" C15" 120.1(6) . . ? C10" C11" C15" 118.5(6) . . ? C11" C12" C13" 118.5(5) . . ? C12" C13" C14" 120.3(5) . . ? C12" C13" C16" 121.1(6) . . ? C14" C13" C16" 118.5(6) . . ? C13" C14" C9" 122.5(5) . . ? F7A" C15" F8A" 106.3(9) . . ? F7A" C15" F9A" 106.8(8) . . ? F8A" C15" F9A" 106.3(8) . . ? F7A" C15" C11" 113.6(9) . . ? F8A" C15" C11" 109.4(12) . . ? F9A" C15" C11" 114.0(13) . . ? F10" C16" F11" 107.1(9) . . ? F10" C16" F12" 107.6(10) . . ? F11" C16" F12" 106.3(9) . . ? F10" C16" C13" 110.7(10) . . ? F11" C16" C13" 112.0(16) . . ? F12" C16" C13" 112.8(17) . . ? C18A C17A C22A 115.6(2) . . ? C18A C17A B1A 124.3(2) . . ? C22A C17A B1A 119.8(2) . . ? C19A C18A C17A 122.1(2) . . ? C20A C19A C18A 121.4(2) . . ? C20A C19A C23A 119.5(3) . . ? C18A C19A C23A 119.1(3) . . ? C19A C20A C21A 117.9(2) . . ? C22A C21A C20A 120.9(2) . . ? C22A C21A C24A 120.2(2) . . ? C20A C21A C24A 119.0(2) . . ? C21A C22A C17A 122.0(2) . . ? F14' C23A F15' 109.0(6) . . ? F13A C23A F14A 108.8(6) . . ? F13A C23A F15A 107.9(5) . . ? F14A C23A F15A 103.2(5) . . ? F14' C23A F13' 106.0(5) . . ? F15' C23A F13' 103.1(5) . . ? F15" C23A F14" 111.8(9) . . ? F15" C23A F13" 110.4(8) . . ? F14" C23A F13" 94.5(7) . . ? F15" C23A C19A 118.4(6) . . ? F13A C23A C19A 113.5(4) . . ? F14' C23A C19A 114.4(4) . . ? F15' C23A C19A 113.8(6) . . ? F14A C23A C19A 112.2(5) . . ? F15A C23A C19A 110.7(4) . . ? F13' C23A C19A 109.6(4) . . ? F14" C23A C19A 110.8(5) . . ? F13" C23A C19A 108.3(4) . . ? F18A C24A F17A 111.6(3) . . ? F17' C24A F16' 108.8(4) . . ? F18A C24A F16A 106.9(3) . . ? F17A C24A F16A 103.4(3) . . ? F17' C24A F18' 102.9(4) . . ? F16' C24A F18' 99.7(4) . . ? F18A C24A C21A 113.5(3) . . ? F17' C24A C21A 115.5(4) . . ? F17A C24A C21A 111.4(3) . . ? F16' C24A C21A 116.1(3) . . ? F16A C24A C21A 109.3(2) . . ? F18' C24A C21A 111.8(3) . . ? C30A C25A C26A 115.4(2) . . ? C30A C25A B1A 119.3(2) . . ? C26A C25A B1A 124.9(2) . . ? C27A C26A C25A 122.2(2) . . ? C28A C27A C26A 121.2(2) . . ? C28A C27A C31A 118.1(2) . . ? C26A C27A C31A 120.5(2) . . ? C27A C28A C29A 117.5(2) . . ? C30A C29A C28A 121.0(2) . . ? C30A C29A C32A 118.5(2) . . ? C28A C29A C32A 120.5(2) . . ? C29A C30A C25A 122.6(2) . . ? F19A C31A F20A 109.1(6) . . ? F19' C31A F21' 109.2(6) . . ? F19' C31A F20' 106.3(4) . . ? F21' C31A F20' 104.1(5) . . ? F19A C31A F21A 103.9(5) . . ? F20A C31A F21A 105.2(4) . . ? F19' C31A C27A 116.5(3) . . ? F19A C31A C27A 116.2(6) . . ? F20A C31A C27A 112.3(5) . . ? F21' C31A C27A 110.3(6) . . ? F20' C31A C27A 109.7(4) . . ? F21A C31A C27A 109.2(3) . . ? F22A C32A F23A 106.5(2) . . ? F22A C32A F24A 106.5(2) . . ? F23A C32A F24A 105.8(2) . . ? F22A C32A C29A 113.3(2) . . ? F23A C32A C29A 112.1(2) . . ? F24A C32A C29A 112.2(2) . . ? 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 Na1 O5' 2.298(19) . ? Na1 O3' 2.32(3) . ? Na1 O3 2.376(10) . ? Na1 O5 2.433(6) . ? Na1 O4 2.433(3) . ? Na1 O6 2.481(3) . ? Na1 N1 2.488(3) . ? Na1 O2 2.523(2) . ? Na1 N2 2.557(3) . ? Na1 O4' 2.566(11) . ? Na1 C13' 3.074(13) . ? Na1 C14' 3.127(13) . ? N1 C5 1.259(4) . ? N1 C1 1.487(4) . ? N2 C16 1.268(5) . ? N2 C18 1.502(4) . ? O1 C5 1.359(4) . ? O1 C2 1.448(4) . ? O2 C6 1.420(4) . ? O2 C7 1.445(5) . ? O2 C7' 1.460(9) . ? O6 C15 1.384(5) . ? O6 C14' 1.427(9) . ? O6 C14 1.511(8) . ? O7 C16 1.353(4) . ? O7 C17 1.435(5) . ? C1 C3 1.508(5) . ? C1 C4 1.515(5) . ? C1 C2 1.544(5) . ? C5 C6 1.500(4) . ? O3 C8 1.415(9) . ? O3 C9 1.454(9) . ? O4 C10 1.397(9) . ? O4 C11 1.409(6) . ? O5 C13 1.415(7) . ? O5 C12 1.443(7) . ? C7 C8 1.511(6) . ? C9 C10 1.491(8) . ? C11 C12 1.493(9) . ? C13 C14 1.424(9) . ? O3' C8' 1.476(10) . ? O3' C9' 1.486(10) . ? O4' C10' 1.482(10) . ? O4' C11' 1.484(10) . ? O5' C13' 1.472(10) . ? O5' C12' 1.484(10) . ? C7' C8' 1.513(10) . ? C9' C10' 1.522(10) . ? C11' C12' 1.519(10) . ? C13' C14' 1.521(9) . ? C15 C16 1.506(5) . ? C17 C18 1.538(6) . ? C18 C20 1.511(6) . ? C18 C19 1.520(5) . ? B1A C9A 1.630(6) . ? B1A C25A 1.637(4) . ? B1A C1A 1.638(4) . ? B1A C17A 1.641(3) . ? B1A C9" 1.668(13) . ? C1A C6A 1.401(4) . ? C1A C2A 1.407(3) . ? C2A C3A 1.390(4) . ? C3A C4A 1.384(4) . ? C3A C7A 1.504(4) . ? C4A C5A 1.386(4) . ? C5A C6A 1.386(4) . ? C5A C8A 1.497(4) . ? C7A F2' 1.308(7) . ? C7A F3' 1.313(7) . ? C7A F3A 1.325(5) . ? C7A F1A 1.326(5) . ? C7A F2A 1.334(6) . ? C7A F1' 1.357(6) . ? C8A F5A 1.263(5) . ? C8A F6' 1.267(6) . ? C8A F4' 1.351(6) . ? C8A F4A 1.363(4) . ? C8A F6A 1.378(5) . ? C8A F5' 1.401(7) . ? C9A C14A 1.393(5) . ? C9A C10A 1.400(5) . ? C10A C11A 1.393(4) . ? C11A C12A 1.379(5) . ? C11A C15A 1.497(5) . ? C12A C13A 1.389(5) . ? C13A C14A 1.391(4) . ? C13A C16A 1.486(5) . ? C15A F8A 1.317(6) . ? C15A F9A 1.331(6) . ? C15A F7A 1.359(5) . ? C16A F12A 1.333(6) . ? C16A F11A 1.348(7) . ? C16A F10A 1.356(7) . ? C9" C14" 1.392(6) . ? C9" C10" 1.400(6) . ? C10" C11" 1.394(5) . ? C11" C12" 1.378(6) . ? C11" C15" 1.498(6) . ? C12" C13" 1.388(6) . ? C13" C14" 1.391(5) . ? C13" C16" 1.486(6) . ? C15" F7A" 1.327(8) . ? C15" F8A" 1.343(9) . ? C15" F9A" 1.344(9) . ? C16" F10" 1.335(10) . ? C16" F11" 1.338(9) . ? C16" F12" 1.338(9) . ? C17A C18A 1.401(3) . ? C17A C22A 1.408(3) . ? C18A C19A 1.388(4) . ? C19A C20A 1.376(4) . ? C19A C23A 1.502(4) . ? C20A C21A 1.392(4) . ? C21A C22A 1.390(3) . ? C21A C24A 1.493(4) . ? C23A F15" 1.188(12) . ? C23A F13A 1.287(6) . ? C23A F14' 1.310(6) . ? C23A F15' 1.334(7) . ? C23A F14A 1.345(7) . ? C23A F15A 1.378(6) . ? C23A F13' 1.383(7) . ? C23A F14" 1.395(12) . ? C23A F13" 1.481(9) . ? C24A F18A 1.257(4) . ? C24A F17' 1.298(5) . ? C24A F17A 1.322(4) . ? C24A F16' 1.337(4) . ? C24A F16A 1.381(4) . ? C24A F18' 1.412(5) . ? C25A C30A 1.397(3) . ? C25A C26A 1.399(3) . ? C26A C27A 1.387(4) . ? C27A C28A 1.385(4) . ? C27A C31A 1.497(4) . ? C28A C29A 1.385(4) . ? C29A C30A 1.384(4) . ? C29A C32A 1.496(3) . ? C31A F19' 1.297(5) . ? C31A F19A 1.320(7) . ? C31A F20A 1.321(6) . ? C31A F21' 1.343(7) . ? C31A F20' 1.362(6) . ? C31A F21A 1.402(5) . ? C32A F22A 1.334(3) . ? C32A F23A 1.335(3) . ? C32A F24A 1.339(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C3 106.1(3) . . . . ? Na1 N1 C1 C3 -66.3(4) . . . . ? C5 N1 C1 C4 -132.0(3) . . . . ? Na1 N1 C1 C4 55.6(4) . . . . ? C5 N1 C1 C2 -11.6(4) . . . . ? Na1 N1 C1 C2 176.0(3) . . . . ? C5 O1 C2 C1 -13.0(3) . . . . ? N1 C1 C2 O1 14.9(3) . . . . ? C3 C1 C2 O1 -99.6(3) . . . . ? C4 C1 C2 O1 134.5(3) . . . . ? C1 N1 C5 O1 3.8(4) . . . . ? Na1 N1 C5 O1 178.5(2) . . . . ? C1 N1 C5 C6 -174.5(3) . . . . ? Na1 N1 C5 C6 0.2(4) . . . . ? C2 O1 C5 N1 6.4(4) . . . . ? C2 O1 C5 C6 -175.1(3) . . . . ? C7 O2 C6 C5 78.1(4) . . . . ? C7' O2 C6 C5 93.7(8) . . . . ? Na1 O2 C6 C5 -39.1(3) . . . . ? N1 C5 C6 O2 28.3(5) . . . . ? O1 C5 C6 O2 -150.1(3) . . . . ? C6 O2 C7 C8 -161.3(3) . . . . ? Na1 O2 C7 C8 -43.2(4) . . . . ? C9 O3 C8 C7 172.6(5) . . . . ? Na1 O3 C8 C7 -54.4(6) . . . . ? O2 C7 C8 O3 66.5(6) . . . . ? C8 O3 C9 C10 174.9(6) . . . . ? Na1 O3 C9 C10 43.9(7) . . . . ? C11 O4 C10 C9 178.3(5) . . . . ? Na1 O4 C10 C9 48.1(6) . . . . ? O3 C9 C10 O4 -59.6(6) . . . . ? C10 O4 C11 C12 -168.8(5) . . . . ? Na1 O4 C11 C12 -38.8(6) . . . . ? C13 O5 C12 C11 170.3(6) . . . . ? Na1 O5 C12 C11 -55.5(5) . . . . ? O4 C11 C12 O5 65.0(7) . . . . ? C12 O5 C13 C14 90.4(8) . . . . ? Na1 O5 C13 C14 -41.7(7) . . . . ? O5 C13 C14 O6 62.4(8) . . . . ? C15 O6 C14 C13 -168.2(5) . . . . ? Na1 O6 C14 C13 -46.8(6) . . . . ? C6 O2 C7' C8' -85.0(14) . . . . ? Na1 O2 C7' C8' 50.0(13) . . . . ? C9' O3' C8' C7' -179.8(19) . . . . ? Na1 O3' C8' C7' 54.6(18) . . . . ? O2 C7' C8' O3' -74(2) . . . . ? C8' O3' C9' C10' -170(2) . . . . ? Na1 O3' C9' C10' -49.0(19) . . . . ? C11' O4' C10' C9' -174.1(17) . . . . ? Na1 O4' C10' C9' -53(2) . . . . ? O3' C9' C10' O4' 67(3) . . . . ? C10' O4' C11' C12' 174.6(18) . . . . ? Na1 O4' C11' C12' 55.3(18) . . . . ? C13' O5' C12' C11' -154.7(14) . . . . ? Na1 O5' C12' C11' 58.0(16) . . . . ? O4' C11' C12' O5' -63.2(19) . . . . ? C12' O5' C13' C14' -109.8(16) . . . . ? Na1 O5' C13' C14' 44.5(12) . . . . ? C12' O5' C13' Na1 -154.3(18) . . . . ? C15 O6 C14' C13' -84.8(11) . . . . ? Na1 O6 C14' C13' 56.3(10) . . . . ? C15 O6 C14' Na1 -141.1(6) . . . . ? O5' C13' C14' O6 -72.8(14) . . . . ? Na1 C13' C14' O6 -42.0(8) . . . . ? O5' C13' C14' Na1 -30.8(10) . . . . ? C14' O6 C15 C16 106.1(7) . . . . ? C14 O6 C15 C16 83.3(5) . . . . ? Na1 O6 C15 C16 -31.8(4) . . . . ? C18 N2 C16 O7 0.5(5) . . . . ? Na1 N2 C16 O7 -165.7(3) . . . . ? C18 N2 C16 C15 -179.7(4) . . . . ? Na1 N2 C16 C15 14.1(5) . . . . ? C17 O7 C16 N2 -4.2(5) . . . . ? C17 O7 C16 C15 176.0(4) . . . . ? O6 C15 C16 N2 11.5(6) . . . . ? O6 C15 C16 O7 -168.6(4) . . . . ? C16 O7 C17 C18 5.7(4) . . . . ? C16 N2 C18 C20 -116.8(4) . . . . ? Na1 N2 C18 C20 43.0(5) . . . . ? C16 N2 C18 C19 122.6(4) . . . . ? Na1 N2 C18 C19 -77.6(4) . . . . ? C16 N2 C18 C17 3.1(4) . . . . ? Na1 N2 C18 C17 162.9(3) . . . . ? O7 C17 C18 N2 -5.4(4) . . . . ? O7 C17 C18 C20 111.5(4) . . . . ? O7 C17 C18 C19 -122.2(4) . . . . ? C9A B1A C1A C6A -38.1(8) . . . . ? C25A B1A C1A C6A -153.8(2) . . . . ? C17A B1A C1A C6A 84.4(3) . . . . ? C9" B1A C1A C6A -36(2) . . . . ? C9A B1A C1A C2A 147.2(8) . . . . ? C25A B1A C1A C2A 31.4(3) . . . . ? C17A B1A C1A C2A -90.4(3) . . . . ? C9" B1A C1A C2A 150(2) . . . . ? C6A C1A C2A C3A 0.0(4) . . . . ? B1A C1A C2A C3A 175.1(2) . . . . ? C1A C2A C3A C4A 1.3(4) . . . . ? C1A C2A C3A C7A -178.9(3) . . . . ? C2A C3A C4A C5A -1.5(4) . . . . ? C7A C3A C4A C5A 178.8(3) . . . . ? C3A C4A C5A C6A 0.3(4) . . . . ? C3A C4A C5A C8A 178.1(3) . . . . ? C4A C5A C6A C1A 1.0(4) . . . . ? C8A C5A C6A C1A -176.8(3) . . . . ? C2A C1A C6A C5A -1.2(4) . . . . ? B1A C1A C6A C5A -176.2(2) . . . . ? C4A C3A C7A F2' -128.6(5) . . . . ? C2A C3A C7A F2' 51.6(6) . . . . ? C4A C3A C7A F3' 107.5(6) . . . . ? C2A C3A C7A F3' -72.3(6) . . . . ? C4A C3A C7A F3A 20.7(5) . . . . ? C2A C3A C7A F3A -159.1(4) . . . . ? C4A C3A C7A F1A -102.1(4) . . . . ? C2A C3A C7A F1A 78.2(4) . . . . ? C4A C3A C7A F2A 139.4(4) . . . . ? C2A C3A C7A F2A -40.4(4) . . . . ? C4A C3A C7A F1' -12.5(5) . . . . ? C2A C3A C7A F1' 167.7(5) . . . . ? C6A C5A C8A F5A 99.1(5) . . . . ? C4A C5A C8A F5A -78.7(5) . . . . ? C6A C5A C8A F6' -52.0(6) . . . . ? C4A C5A C8A F6' 130.2(6) . . . . ? C6A C5A C8A F4' 172.9(5) . . . . ? C4A C5A C8A F4' -4.9(6) . . . . ? C6A C5A C8A F4A -135.0(4) . . . . ? C4A C5A C8A F4A 47.2(5) . . . . ? C6A C5A C8A F6A -21.6(5) . . . . ? C4A C5A C8A F6A 160.6(3) . . . . ? C6A C5A C8A F5' 65.2(5) . . . . ? C4A C5A C8A F5' -112.7(5) . . . . ? C25A B1A C9A C14A -77.5(16) . . . . ? C1A B1A C9A C14A 162.3(13) . . . . ? C17A B1A C9A C14A 44.3(18) . . . . ? C25A B1A C9A C10A 98.4(17) . . . . ? C1A B1A C9A C10A -22(2) . . . . ? C17A B1A C9A C10A -139.8(14) . . . . ? C14A C9A C10A C11A -2(2) . . . . ? B1A C9A C10A C11A -178.5(13) . . . . ? C9A C10A C11A C12A 0.0(19) . . . . ? C9A C10A C11A C15A -178.2(14) . . . . ? C10A C11A C12A C13A 1.6(15) . . . . ? C15A C11A C12A C13A 179.8(10) . . . . ? C11A C12A C13A C14A -0.6(17) . . . . ? C11A C12A C13A C16A -179.3(10) . . . . ? C12A C13A C14A C9A -2(2) . . . . ? C16A C13A C14A C9A 176.7(14) . . . . ? C10A C9A C14A C13A 3(2) . . . . ? B1A C9A C14A C13A 179.6(15) . . . . ? C12A C11A C15A F8A -123.0(8) . . . . ? C10A C11A C15A F8A 55.2(10) . . . . ? C12A C11A C15A F9A 1.1(11) . . . . ? C10A C11A C15A F9A 179.3(9) . . . . ? C12A C11A C15A F7A 119.4(9) . . . . ? C10A C11A C15A F7A -62.4(10) . . . . ? C12A C13A C16A F12A -139.4(10) . . . . ? C14A C13A C16A F12A 41.8(13) . . . . ? C12A C13A C16A F11A 100.4(11) . . . . ? C14A C13A C16A F11A -78.3(12) . . . . ? C12A C13A C16A F10A -19.2(13) . . . . ? C14A C13A C16A F10A 162.0(11) . . . . ? C25A B1A C9" C14" -79(4) . . . . ? C1A B1A C9" C14" 159(3) . . . . ? C17A B1A C9" C14" 41(4) . . . . ? C25A B1A C9" C10" 93(4) . . . . ? C1A B1A C9" C10" -29(5) . . . . ? C17A B1A C9" C10" -147(4) . . . . ? C14" C9" C10" C11" -5(6) . . . . ? B1A C9" C10" C11" -178(3) . . . . ? C9" C10" C11" C12" 4(5) . . . . ? C9" C10" C11" C15" 174(3) . . . . ? C10" C11" C12" C13" 0(4) . . . . ? C15" C11" C12" C13" -170(2) . . . . ? C11" C12" C13" C14" -2(4) . . . . ? C11" C12" C13" C16" -178(3) . . . . ? C12" C13" C14" C9" 0(5) . . . . ? C16" C13" C14" C9" 176(4) . . . . ? C10" C9" C14" C13" 4(6) . . . . ? B1A C9" C14" C13" 176(4) . . . . ? C12" C11" C15" F7A" -163(2) . . . . ? C10" C11" C15" F7A" 26(3) . . . . ? C12" C11" C15" F8A" -45(3) . . . . ? C10" C11" C15" F8A" 145(2) . . . . ? C12" C11" C15" F9A" 74(2) . . . . ? C10" C11" C15" F9A" -97(2) . . . . ? C12" C13" C16" F10" -10(3) . . . . ? C14" C13" C16" F10" 174(3) . . . . ? C12" C13" C16" F11" 110(3) . . . . ? C14" C13" C16" F11" -66(3) . . . . ? C12" C13" C16" F12" -130(3) . . . . ? C14" C13" C16" F12" 54(3) . . . . ? C9A B1A C17A C18A 16.6(8) . . . . ? C25A B1A C17A C18A 133.5(3) . . . . ? C1A B1A C17A C18A -105.5(3) . . . . ? C9" B1A C17A C18A 19.2(17) . . . . ? C9A B1A C17A C22A -168.9(8) . . . . ? C25A B1A C17A C22A -52.1(3) . . . . ? C1A B1A C17A C22A 69.0(3) . . . . ? C9" B1A C17A C22A -166.3(17) . . . . ? C22A C17A C18A C19A 2.6(4) . . . . ? B1A C17A C18A C19A 177.4(3) . . . . ? C17A C18A C19A C20A -2.5(5) . . . . ? C17A C18A C19A C23A 177.7(3) . . . . ? C18A C19A C20A C21A 0.3(5) . . . . ? C23A C19A C20A C21A -179.9(3) . . . . ? C19A C20A C21A C22A 1.6(4) . . . . ? C19A C20A C21A C24A -177.9(3) . . . . ? C20A C21A C22A C17A -1.3(4) . . . . ? C24A C21A C22A C17A 178.2(2) . . . . ? C18A C17A C22A C21A -0.8(4) . . . . ? B1A C17A C22A C21A -175.7(2) . . . . ? C20A C19A C23A F15" 78.9(11) . . . . ? C18A C19A C23A F15" -101.3(11) . . . . ? C20A C19A C23A F13A -92.1(6) . . . . ? C18A C19A C23A F13A 87.8(6) . . . . ? C20A C19A C23A F14' -3.6(7) . . . . ? C18A C19A C23A F14' 176.2(6) . . . . ? C20A C19A C23A F15' 122.6(6) . . . . ? C18A C19A C23A F15' -57.6(6) . . . . ? C20A C19A C23A F14A 144.2(5) . . . . ? C18A C19A C23A F14A -36.0(6) . . . . ? C20A C19A C23A F15A 29.5(5) . . . . ? C18A C19A C23A F15A -150.7(5) . . . . ? C20A C19A C23A F13' -122.5(5) . . . . ? C18A C19A C23A F13' 57.3(5) . . . . ? C20A C19A C23A F14" -150.0(7) . . . . ? C18A C19A C23A F14" 29.8(8) . . . . ? C20A C19A C23A F13" -47.7(6) . . . . ? C18A C19A C23A F13" 132.1(6) . . . . ? C22A C21A C24A F18A 73.6(4) . . . . ? C20A C21A C24A F18A -106.9(4) . . . . ? C22A C21A C24A F17' -123.6(4) . . . . ? C20A C21A C24A F17' 55.9(5) . . . . ? C22A C21A C24A F17A -159.4(3) . . . . ? C20A C21A C24A F17A 20.1(4) . . . . ? C22A C21A C24A F16' 5.6(5) . . . . ? C20A C21A C24A F16' -174.9(4) . . . . ? C22A C21A C24A F16A -45.7(4) . . . . ? C20A C21A C24A F16A 133.8(3) . . . . ? C22A C21A C24A F18' 119.1(4) . . . . ? C20A C21A C24A F18' -61.4(4) . . . . ? C9A B1A C25A C30A -73.0(4) . . . . ? C1A B1A C25A C30A 47.7(3) . . . . ? C17A B1A C25A C30A 165.0(2) . . . . ? C9" B1A C25A C30A -77.7(7) . . . . ? C9A B1A C25A C26A 99.3(4) . . . . ? C1A B1A C25A C26A -140.0(2) . . . . ? C17A B1A C25A C26A -22.7(3) . . . . ? C9" B1A C25A C26A 94.6(7) . . . . ? C30A C25A C26A C27A -0.1(4) . . . . ? B1A C25A C26A C27A -172.7(2) . . . . ? C25A C26A C27A C28A -0.3(4) . . . . ? C25A C26A C27A C31A 175.3(2) . . . . ? C26A C27A C28A C29A 0.4(4) . . . . ? C31A C27A C28A C29A -175.2(2) . . . . ? C27A C28A C29A C30A -0.2(4) . . . . ? C27A C28A C29A C32A 179.4(2) . . . . ? C28A C29A C30A C25A -0.2(4) . . . . ? C32A C29A C30A C25A -179.8(2) . . . . ? C26A C25A C30A C29A 0.4(4) . . . . ? B1A C25A C30A C29A 173.4(2) . . . . ? C28A C27A C31A F19' -26.4(4) . . . . ? C26A C27A C31A F19' 157.9(3) . . . . ? C28A C27A C31A F19A -168.4(5) . . . . ? C26A C27A C31A F19A 15.9(6) . . . . ? C28A C27A C31A F20A 65.0(5) . . . . ? C26A C27A C31A F20A -110.7(4) . . . . ? C28A C27A C31A F21' -151.5(5) . . . . ? C26A C27A C31A F21' 32.8(5) . . . . ? C28A C27A C31A F20' 94.4(4) . . . . ? C26A C27A C31A F20' -81.3(4) . . . . ? C28A C27A C31A F21A -51.3(4) . . . . ? C26A C27A C31A F21A 133.0(3) . . . . ? C30A C29A C32A F22A 170.9(2) . . . . ? C28A C29A C32A F22A -8.8(4) . . . . ? C30A C29A C32A F23A -68.6(3) . . . . ? C28A C29A C32A F23A 111.7(3) . . . . ? C30A C29A C32A F24A 50.2(3) . . . . ? C28A C29A C32A F24A -129.4(3) . . . . ?