# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_7PF6 _database_code_depnum_ccdc_archive 'CCDC 911205' #TrackingRef 'White_Beer_OBC.cif' #============================================================================== # start Validation Reply Form _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.904 RESPONSE: Crystals were very small and weakly-diffracting. It was necessary to use synchrotron radiation to collect diffraction data, but despite this, some reflections were too weak to be separated from background noise. ; # end Validation Reply Form _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; Crystals were twinned. Twin laws were found and applied using the ROTAX feature of CRYSTALS. ; _cell_length_a 19.4982(4) _cell_length_b 13.3380(3) _cell_length_c 43.2785(11) _cell_angle_alpha 90 _cell_angle_beta 95.832(2) _cell_angle_gamma 90 _cell_volume 11197.1(4) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z x,-y,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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C58 H64 Cl1 F3 N5 O5 P0.50 # Dc = 0.60 Fooo = 4488.00 Mu = 0.72 M = 1019.11 # Found Formula = C121 H144.40 Cl2 F6 N9 O10.70 P1 # Dc = 1.25 FOOO = 4488.00 Mu = 1.46 M = 2112.00 _chemical_formula_sum 'C121 H144.40 Cl2 F6 N9 O10.70 P1' _chemical_formula_moiety ; C116 H 131 N9 O9, F6 P, C4 H10 O, C H2 Cl2, 0.7 (H2 O) ; _chemical_compound_source synthesized _chemical_formula_weight 2112.00 _cell_measurement_reflns_used 12672 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 26.19 _cell_measurement_temperature 100 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4488.000 _exptl_absorpt_coefficient_mu 0.146 # Sheldrick geometric approximatio 0.86 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Oxford Diffraction, 2011)' _exptl_absorpt_correction_T_min 0.563 _exptl_absorpt_correction_T_max 1.00 _diffrn_measurement_device_type synchrotron _diffrn_measurement_device Area _diffrn_radiation_monochromator synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.68890 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Crystal Clear (Rigaku, 1997--2002)' _computing_cell_refinement 'CrysAlisPro, (Oxford Diffraction, 2011)' _computing_data_reduction 'CrysAlisPro, (Oxford Diffraction, 2011)' _computing_structure_solution 'Superflip, (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 38822 _reflns_number_total 10792 _diffrn_reflns_av_R_equivalents 0.064 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 10792 # Theoretical number of reflections is about 20103 _diffrn_reflns_theta_min 1.828 _diffrn_reflns_theta_max 26.190 _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 25.142 _diffrn_measured_fraction_theta_full 0.904 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 55 _reflns_limit_h_min -24 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 55 _oxford_diffrn_Wilson_B_factor 3.42 _oxford_diffrn_Wilson_scale 0.06 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.49 _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 9747 _refine_ls_number_restraints 1370 _refine_ls_number_parameters 1353 _oxford_refine_ls_R_factor_ref 0.1293 _refine_ls_wR_factor_ref 0.2919 _refine_ls_goodness_of_fit_ref 1.0601 _refine_ls_shift/su_max 0.0004470 _refine_ls_shift/su_mean 0.0000369 # The values computed with all filters except I/sigma _oxford_reflns_number_all 9747 _refine_ls_R_factor_all 0.1293 _refine_ls_wR_factor_all 0.2919 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9344 _refine_ls_R_factor_gt 0.1264 _refine_ls_wR_factor_gt 0.2908 # 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 unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #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: 0.678E+04 0.103E+05 0.572E+04 0.290E+04 ; # Insert your own references if required - in alphabetical order loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.3392(9) 0.4740(14) 0.7563(4) 0.0587 1.0000 Uani . U . . . . C2 C 0.3134(10) 0.5686(14) 0.7661(4) 0.0631 1.0000 Uani . U . . . . C3 C 0.3549(11) 0.6479(15) 0.7701(4) 0.0663 1.0000 Uani . U . . . . C4 C 0.4236(10) 0.6448(13) 0.7641(4) 0.0610 1.0000 Uani . U . . . . C5 C 0.4509(9) 0.5549(13) 0.7527(4) 0.0570 1.0000 Uani . U . . . . C6 C 0.4058(9) 0.4712(13) 0.7499(3) 0.0537 1.0000 Uani . U . . . . O7 O 0.5645(8) 0.6183(10) 0.7554(3) 0.0809 1.0000 Uani . U . . . . C8 C 0.5220(10) 0.5477(13) 0.7471(4) 0.0606 1.0000 Uani . U . . . . N9 N 0.5481(7) 0.4665(11) 0.7316(3) 0.0599 1.0000 Uani . U . . . . C10 C 0.6168(9) 0.4623(14) 0.7240(4) 0.0638 1.0000 Uani . U . . . . C11 C 0.6217(10) 0.3809(14) 0.7000(5) 0.0664 1.0000 Uani . U . . . . O12 O 0.6192(6) 0.2864(9) 0.7140(3) 0.0608 1.0000 Uani . U . . . . C13 C 0.6289(8) 0.1998(14) 0.6967(4) 0.0574 1.0000 Uani . U . . . . C14 C 0.6312(8) 0.2031(14) 0.6649(4) 0.0582 1.0000 Uani . U . . . . C15 C 0.6440(8) 0.1128(14) 0.6501(4) 0.0597 1.0000 Uani . U . . . . C16 C 0.6564(8) 0.0275(13) 0.6664(4) 0.0550 1.0000 Uani . U . . . . C17 C 0.6566(8) 0.0256(13) 0.6972(4) 0.0561 1.0000 Uani . U . . . . C18 C 0.6426(7) 0.1160(13) 0.7134(4) 0.0542 1.0000 Uani . U . . . . O19 O 0.6690(6) -0.0564(9) 0.6492(3) 0.0625 1.0000 Uani . U . . . . C20 C 0.6836(9) -0.1482(12) 0.6661(4) 0.0630 1.0000 Uani D U . . . . C21 C 0.7029(6) -0.2223(13) 0.6419(4) 0.0646 1.0000 Uani D U . . . . O22 O 0.6417(5) -0.2471(8) 0.6223(3) 0.0580 1.0000 Uani D U . . . . C23 C 0.6529(7) -0.3275(11) 0.6014(4) 0.0617 1.0000 Uani D U . . . . C24 C 0.5884(6) -0.3317(13) 0.5784(3) 0.0629 1.0000 Uani D U . . . . O25 O 0.5328(5) -0.3692(8) 0.5942(2) 0.0565 1.0000 Uani D U . . . . C26 C 0.4701(6) -0.3703(13) 0.5738(4) 0.0642 1.0000 Uani D U . . . . C27 C 0.4133(8) -0.4261(12) 0.5883(4) 0.0659 1.0000 Uani D U . . . . O28 O 0.3975(6) -0.3668(8) 0.6139(3) 0.0642 1.0000 Uani D U . . . . C29 C 0.3389(7) -0.4055(12) 0.6274(4) 0.0641 1.0000 Uani D U . . . . C30 C 0.3292(9) -0.3476(12) 0.6569(4) 0.0589 1.0000 Uani D U . . . . O31 O 0.3114(6) -0.2488(9) 0.6464(3) 0.0613 1.0000 Uani . U . . . . C32 C 0.3072(10) -0.1806(11) 0.6694(3) 0.0628 1.0000 Uani D U . . . . C33 C 0.3060(9) -0.2037(13) 0.7008(3) 0.0631 1.0000 Uani D U . . . . C34 C 0.3040(9) -0.1266(10) 0.7224(4) 0.0662 1.0000 Uani D U . . . . C35 C 0.2987(9) -0.0279(12) 0.7123(4) 0.0662 1.0000 Uani D U . . . . C36 C 0.2949(9) -0.0028(12) 0.6809(3) 0.0638 1.0000 Uani D U . . . . C37 C 0.2992(9) -0.0807(9) 0.6596(4) 0.0629 1.0000 Uani D U . . . . O38 O 0.2894(7) 0.0426(10) 0.7359(3) 0.0751 1.0000 Uani . U . . . . C39 C 0.2865(11) 0.1415(15) 0.7276(5) 0.0731 1.0000 Uani . U . . . . C40 C 0.2834(11) 0.2049(16) 0.7571(5) 0.0758 1.0000 Uani . U . . . . N41 N 0.3227(9) 0.2993(12) 0.7559(4) 0.0706 1.0000 Uani . U . . . . C42 C 0.2916(9) 0.3905(15) 0.7549(4) 0.0623 1.0000 Uani . U . . . . O43 O 0.2283(7) 0.3969(12) 0.7548(4) 0.0837 1.0000 Uani . U . . . . P1 P 0.4181(2) 0.3052(3) 0.66593(11) 0.0498 1.0000 Uani . U . . . . F2 F 0.4840(6) 0.2652(10) 0.6512(3) 0.0874 1.0000 Uani . U . . . . F3 F 0.4536(5) 0.2864(6) 0.7012(2) 0.0607 1.0000 Uani . U . . . . F4 F 0.3524(6) 0.3414(10) 0.6803(3) 0.0881 1.0000 Uani . U . . . . F5 F 0.4490(6) 0.4140(7) 0.6678(3) 0.0769 1.0000 Uani . U . . . . F6 F 0.3908(6) 0.1946(7) 0.6649(3) 0.0802 1.0000 Uani . U . . . . F7 F 0.3800(6) 0.3261(8) 0.6323(3) 0.0751 1.0000 Uani . U . . . . N10 N 0.4840(5) 0.0724(7) 0.5728(2) 0.0305 1.0000 Uani . U . . . . C190 C 0.4781(6) 0.0677(9) 0.6032(3) 0.0310 1.0000 Uani . U . . . . C12 C 0.4900(7) -0.0293(9) 0.6114(3) 0.0358 1.0000 Uani . U . . . . N13 N 0.5033(7) -0.0807(8) 0.5849(3) 0.0401 1.0000 Uani . U . . . . N14 N 0.4987(6) -0.0176(8) 0.5618(2) 0.0385 1.0000 Uani . U . . . . C191 C 0.4901(7) -0.0818(9) 0.6408(3) 0.0326 1.0000 Uani . U . . . . C192 C 0.5022(6) -0.1856(9) 0.6415(3) 0.0298 1.0000 Uani . U . . . . N17 N 0.5054(5) -0.2337(7) 0.6684(2) 0.0318 1.0000 Uani . U . . . . C19 C 0.4988(7) -0.1883(9) 0.6959(3) 0.0331 1.0000 Uani . U . . . . C193 C 0.4854(7) -0.0863(9) 0.6962(3) 0.0338 1.0000 Uani . U . . . . C194 C 0.4827(7) -0.0335(9) 0.6690(3) 0.0338 1.0000 Uani . U . . . . C22 C 0.4774(7) -0.0396(10) 0.7260(3) 0.0367 1.0000 Uani . U . . . . N23 N 0.4698(7) -0.0939(8) 0.7518(3) 0.0428 1.0000 Uani . U . . . . N24 N 0.4645(7) -0.0334(8) 0.7750(3) 0.0412 1.0000 Uani . U . . . . N25 N 0.4666(6) 0.0620(8) 0.7639(2) 0.0343 1.0000 Uani . U . . . . C195 C 0.4754(6) 0.0606(10) 0.7340(3) 0.0320 1.0000 Uani . U . . . . C196 C 0.4580(6) 0.1422(9) 0.7849(3) 0.0290 1.0000 Uani . U . . . . C28 C 0.4145(6) 0.1298(9) 0.8084(3) 0.0310 1.0000 Uani . U . . . . C197 C 0.4127(6) 0.2054(9) 0.8302(3) 0.0321 1.0000 Uani . U . . . . C198 C 0.4494(6) 0.2912(9) 0.8299(3) 0.0290 1.0000 Uani . U . . . . C31 C 0.4925(6) 0.3037(9) 0.8051(3) 0.0284 1.0000 Uani . U . . . . C199 C 0.4959(6) 0.2298(9) 0.7833(3) 0.0288 1.0000 Uani . U . . . . C200 C 0.4471(6) 0.3714(9) 0.8556(3) 0.0312 1.0000 Uani . U . . . . C201 C 0.3808(6) 0.4380(8) 0.8503(3) 0.0277 1.0000 Uani . U . . . . C202 C 0.3795(6) 0.5325(8) 0.8653(3) 0.0291 1.0000 Uani . U . . . . C203 C 0.3209(6) 0.5914(9) 0.8625(3) 0.0335 1.0000 Uani . U . . . . C204 C 0.2607(6) 0.5593(10) 0.8463(3) 0.0376 1.0000 Uani . U . . . . C38 C 0.2623(7) 0.4673(10) 0.8309(3) 0.0386 1.0000 Uani . U . . . . C205 C 0.3198(6) 0.4091(9) 0.8331(3) 0.0338 1.0000 Uani . U . . . . C41 C 0.1329(8) 0.5717(12) 0.8281(5) 0.0644 1.0000 Uani . U . . . . C207 C 0.2068(8) 0.7216(12) 0.8243(5) 0.0702 1.0000 Uani . U . . . . C43 C 0.4395(6) 0.3084(9) 0.8864(3) 0.0290 1.0000 Uani . U . . . . C44 C 0.3889(6) 0.3290(9) 0.9063(3) 0.0289 1.0000 Uani . U . . . . C45 C 0.3892(6) 0.2731(9) 0.9333(3) 0.0292 1.0000 Uani . U . . . . C46 C 0.4329(6) 0.1939(9) 0.9411(3) 0.0306 1.0000 Uani . U . . . . C47 C 0.4833(7) 0.1734(9) 0.9208(3) 0.0332 1.0000 Uani . U . . . . C48 C 0.4840(6) 0.2284(8) 0.8936(3) 0.0299 1.0000 Uani . U . . . . C49 C 0.4270(8) 0.1310(10) 0.9705(3) 0.0391 1.0000 Uani . U . . . . C50 C 0.4302(10) 0.2005(13) 0.9991(4) 0.0581 1.0000 Uani . U . . . . C51 C 0.5108(6) 0.4323(9) 0.8584(3) 0.0291 1.0000 Uani . U . . . . C52 C 0.5210(7) 0.5067(9) 0.8357(3) 0.0334 1.0000 Uani . U . . . . C53 C 0.5835(7) 0.5526(10) 0.8349(3) 0.0383 1.0000 Uani . U . . . . C54 C 0.6384(7) 0.5405(10) 0.8565(3) 0.0413 1.0000 Uani . U . . . . C55 C 0.6275(7) 0.4720(10) 0.8815(3) 0.0373 1.0000 Uani . U . . . . C56 C 0.5657(6) 0.4227(9) 0.8822(3) 0.0319 1.0000 Uani . U . . . . C57 C 0.7097(8) 0.5864(12) 0.8546(4) 0.0569 1.0000 Uani D U . . . . C58 C 0.5260(9) -0.3417(10) 0.6686(3) 0.0463 1.0000 Uani . U . . . . C59 C 0.4745(6) 0.1581(8) 0.5514(3) 0.0276 1.0000 Uani . U . . . . C60 C 0.5198(6) 0.1568(8) 0.5282(3) 0.0268 1.0000 Uani . U . . . . C61 C 0.5096(6) 0.2317(8) 0.5054(3) 0.0282 1.0000 Uani . U . . . . C62 C 0.4597(6) 0.3066(9) 0.5063(3) 0.0289 1.0000 Uani . U . . . . C63 C 0.4175(6) 0.3034(9) 0.5304(3) 0.0309 1.0000 Uani . U . . . . C64 C 0.4258(6) 0.2279(8) 0.5532(3) 0.0280 1.0000 Uani . U . . . . C65 C 0.4545(6) 0.3845(9) 0.4795(3) 0.0294 1.0000 Uani . U . . . . C66 C 0.5143(6) 0.4633(9) 0.4850(3) 0.0268 1.0000 Uani . U . . . . C67 C 0.5092(6) 0.5483(9) 0.4666(3) 0.0294 1.0000 Uani . U . . . . C68 C 0.5656(6) 0.6152(9) 0.4674(3) 0.0337 1.0000 Uani . U . . . . C69 C 0.6260(6) 0.5994(9) 0.4862(3) 0.0342 1.0000 Uani . U . . . . C70 C 0.6845(7) 0.6756(12) 0.4865(4) 0.0501 1.0000 Uani . U . . . . C71 C 0.6300(6) 0.5156(9) 0.5060(3) 0.0325 1.0000 Uani . U . . . . C72 C 0.5726(6) 0.4473(9) 0.5042(3) 0.0291 1.0000 Uani . U . . . . C73 C 0.4632(6) 0.3243(9) 0.4491(3) 0.0276 1.0000 Uani . U . . . . C74 C 0.5090(6) 0.3468(8) 0.4286(3) 0.0266 1.0000 Uani . U . . . . C75 C 0.5117(6) 0.2921(9) 0.4009(3) 0.0290 1.0000 Uani . U . . . . C76 C 0.4688(6) 0.2099(8) 0.3937(3) 0.0293 1.0000 Uani . U . . . . C77 C 0.4222(6) 0.1863(9) 0.4148(3) 0.0318 1.0000 Uani . U . . . . C78 C 0.4188(6) 0.2415(9) 0.4429(3) 0.0300 1.0000 Uani . U . . . . C79 C 0.4704(6) 0.1493(9) 0.3636(3) 0.0318 1.0000 Uani . U . . . . C80 C 0.3988(6) 0.1578(9) 0.3452(3) 0.0349 1.0000 Uani . U . . . . C81 C 0.5265(7) 0.1815(10) 0.3441(3) 0.0423 1.0000 Uani . U . . . . C82 C 0.4834(7) 0.0393(9) 0.3727(3) 0.0390 1.0000 Uani . U . . . . C83 C 0.3869(6) 0.4421(8) 0.4764(3) 0.0268 1.0000 Uani . U . . . . C84 C 0.3702(6) 0.5100(9) 0.4990(3) 0.0317 1.0000 Uani . U . . . . C85 C 0.3113(6) 0.5653(9) 0.4967(3) 0.0334 1.0000 Uani . U . . . . C86 C 0.2630(6) 0.5605(9) 0.4696(3) 0.0355 1.0000 Uani . U . . . . C87 C 0.2785(6) 0.4933(9) 0.4467(3) 0.0303 1.0000 Uani . U . . . . C88 C 0.3384(6) 0.4359(9) 0.4496(3) 0.0313 1.0000 Uani . U . . . . C127 C 0.1371(7) 0.5578(11) 0.4659(4) 0.0503 1.0000 Uani . U . . . . C128 C 0.1989(7) 0.6254(11) 0.4648(4) 0.0475 1.0000 Uani . U . . . . C129 C 0.1931(8) 0.6775(13) 0.4330(5) 0.0637 1.0000 Uani . U . . . . C130 C 0.1977(7) 0.7109(11) 0.4891(4) 0.0547 1.0000 Uani . U . . . . C132 C 0.4761(9) 0.0479(11) 0.9750(4) 0.0572 1.0000 Uani . U . . . . C135 C 0.7036(10) 0.7004(13) 0.8509(5) 0.0693 1.0000 Uani . U . . . . C141 C 0.7064(9) 0.6850(17) 0.4537(5) 0.0753 1.0000 Uani . U . . . . C144 C 0.6562(9) 0.7819(12) 0.4929(5) 0.0703 1.0000 Uani . U . . . . C159 C 0.7434(8) 0.6545(14) 0.5100(5) 0.0641 1.0000 Uani . U . . . . C160 C 0.1810(9) 0.6485(16) 0.8773(5) 0.0733 1.0000 Uani . U . . . . C174 C 0.7614(8) 0.5597(15) 0.8814(5) 0.0677 1.0000 Uani . U . . . . C185 C 0.3551(9) 0.0801(11) 0.9677(4) 0.0589 1.0000 Uani . U . . . . Cl56 Cl 0.2603(3) 0.3771(5) 0.56922(18) 0.1004 1.0000 Uani . U . . . . Cl91 Cl 0.1817(3) 0.5625(4) 0.56559(16) 0.0918 1.0000 Uani . U . . . . C187 C 0.1780(11) 0.4385(16) 0.5713(6) 0.0861 1.0000 Uani . U . . . . C186 C 0.7389(7) 0.5394(14) 0.8266(4) 0.0658 1.0000 Uani D U . . . . O303 O 0.7059(6) 0.4035(10) 0.5781(3) 0.0722 1.0000 Uani D U . . . . C305 C 0.5935(8) 0.3797(14) 0.5932(4) 0.0667 1.0000 Uani D U . . . . C304 C 0.6569(7) 0.3274(11) 0.5839(5) 0.0679 1.0000 Uani D U . . . . C302 C 0.7701(7) 0.3670(13) 0.5690(5) 0.0773 1.0000 Uani D U . . . . C301 C 0.8218(11) 0.4512(17) 0.5674(5) 0.0921 1.0000 Uani D U . . . . H21 H 0.2680 0.5753 0.7705 0.0800 1.0000 Uiso R . . . . . H31 H 0.3369 0.7071 0.7772 0.0810 1.0000 Uiso R . . . . . H41 H 0.4511 0.7017 0.7678 0.0720 1.0000 Uiso R . . . . . H61 H 0.4241 0.4113 0.7435 0.0681 1.0000 Uiso R . . . . . H101 H 0.6469 0.4481 0.7427 0.0781 1.0000 Uiso R . . . . . H102 H 0.6291 0.5261 0.7155 0.0780 1.0000 Uiso R . . . . . H111 H 0.6666 0.3866 0.6925 0.0851 1.0000 Uiso R . . . . . H112 H 0.5859 0.3874 0.6827 0.0850 1.0000 Uiso R . . . . . H141 H 0.6248 0.2634 0.6542 0.0700 1.0000 Uiso R . . . . . H151 H 0.6438 0.1116 0.6286 0.0790 1.0000 Uiso R . . . . . H171 H 0.6661 -0.0338 0.7081 0.0681 1.0000 Uiso R . . . . . H181 H 0.6422 0.1173 0.7349 0.0649 1.0000 Uiso R . . . . . H202 H 0.7228 -0.1370 0.6813 0.0780 1.0000 Uiso R . . . . . H201 H 0.6444 -0.1699 0.6765 0.0781 1.0000 Uiso R . . . . . H211 H 0.7203 -0.2825 0.6524 0.0890 1.0000 Uiso R . . . . . H212 H 0.7372 -0.1958 0.6294 0.0891 1.0000 Uiso R . . . . . H231 H 0.6564 -0.3905 0.6127 0.0770 1.0000 Uiso R . . . . . H232 H 0.6943 -0.3171 0.5912 0.0770 1.0000 Uiso R . . . . . H241 H 0.5783 -0.2642 0.5707 0.0750 1.0000 Uiso R . . . . . H242 H 0.5955 -0.3758 0.5611 0.0750 1.0000 Uiso R . . . . . H261 H 0.4546 -0.3025 0.5688 0.0869 1.0000 Uiso R . . . . . H262 H 0.4796 -0.4044 0.5549 0.0871 1.0000 Uiso R . . . . . H271 H 0.4308 -0.4908 0.5955 0.0970 1.0000 Uiso R . . . . . H272 H 0.3732 -0.4355 0.5733 0.0971 1.0000 Uiso R . . . . . H291 H 0.3439 -0.4761 0.6324 0.0840 1.0000 Uiso R . . . . . H292 H 0.2986 -0.3956 0.6127 0.0840 1.0000 Uiso R . . . . . H301 H 0.3723 -0.3464 0.6702 0.0750 1.0000 Uiso R . . . . . H302 H 0.2937 -0.3776 0.6681 0.0750 1.0000 Uiso R . . . . . H331 H 0.3085 -0.2702 0.7071 0.0731 1.0000 Uiso R . . . . . H341 H 0.3040 -0.1422 0.7434 0.0800 1.0000 Uiso R . . . . . H361 H 0.2914 0.0646 0.6756 0.0810 1.0000 Uiso R . . . . . H371 H 0.2972 -0.0666 0.6384 0.0789 1.0000 Uiso R . . . . . H401 H 0.3009 0.1660 0.7752 0.0990 1.0000 Uiso R . . . . . H402 H 0.2353 0.2214 0.7586 0.0990 1.0000 Uiso R . . . . . H1901 H 0.4680 0.1202 0.6161 0.0400 1.0000 Uiso R . . . . . H1921 H 0.5053 -0.2209 0.6231 0.0409 1.0000 Uiso R . . . . . H191 H 0.5023 -0.2252 0.7141 0.0441 1.0000 Uiso R . . . . . H1941 H 0.4791 0.0357 0.6696 0.0461 1.0000 Uiso R . . . . . H1951 H 0.4780 0.1152 0.7209 0.0431 1.0000 Uiso R . . . . . H281 H 0.3876 0.0723 0.8091 0.0462 1.0000 Uiso R . . . . . H1971 H 0.3849 0.1959 0.8462 0.0481 1.0000 Uiso R . . . . . H311 H 0.5195 0.3612 0.8042 0.0359 1.0000 Uiso R . . . . . H1991 H 0.5229 0.2396 0.7671 0.0411 1.0000 Uiso R . . . . . H2021 H 0.4190 0.5561 0.8768 0.0390 1.0000 Uiso R . . . . . H2031 H 0.3226 0.6541 0.8719 0.0461 1.0000 Uiso R . . . . . H381 H 0.2228 0.4457 0.8186 0.0520 1.0000 Uiso R . . . . . H2051 H 0.3187 0.3472 0.8230 0.0451 1.0000 Uiso R . . . . . H414 H 0.0961 0.6179 0.8222 0.1251 1.0000 Uiso R . . . . . H412 H 0.1174 0.5221 0.8419 0.1250 1.0000 Uiso R . . . . . H413 H 0.1464 0.5393 0.8098 0.1250 1.0000 Uiso R . . . . . H2071 H 0.1641 0.7528 0.8167 0.1300 1.0000 Uiso R . . . . . H2073 H 0.2330 0.7660 0.8384 0.1301 1.0000 Uiso R . . . . . H2072 H 0.2327 0.7064 0.8071 0.1299 1.0000 Uiso R . . . . . H441 H 0.3583 0.3821 0.9019 0.0419 1.0000 Uiso R . . . . . H451 H 0.3560 0.2877 0.9465 0.0360 1.0000 Uiso R . . . . . H471 H 0.5153 0.1225 0.9253 0.0450 1.0000 Uiso R . . . . . H481 H 0.5159 0.2104 0.8798 0.0419 1.0000 Uiso R . . . . . H503 H 0.4456 0.1619 1.0172 0.0840 1.0000 Uiso R . . . . . H502 H 0.4613 0.2552 0.9970 0.0841 1.0000 Uiso R . . . . . H501 H 0.3851 0.2267 1.0012 0.0840 1.0000 Uiso R . . . . . H521 H 0.4851 0.5206 0.8204 0.0421 1.0000 Uiso R . . . . . H531 H 0.5879 0.5986 0.8191 0.0460 1.0000 Uiso R . . . . . H551 H 0.6613 0.4621 0.8981 0.0490 1.0000 Uiso R . . . . . H561 H 0.5602 0.3800 0.8986 0.0440 1.0000 Uiso R . . . . . H582 H 0.5572 -0.3566 0.6867 0.0771 1.0000 Uiso R . . . . . H581 H 0.5475 -0.3587 0.6503 0.0769 1.0000 Uiso R . . . . . H583 H 0.4849 -0.3814 0.6692 0.0769 1.0000 Uiso R . . . . . H601 H 0.5549 0.1095 0.5276 0.0421 1.0000 Uiso R . . . . . H611 H 0.5370 0.2312 0.4891 0.0441 1.0000 Uiso R . . . . . H631 H 0.3824 0.3507 0.5310 0.0401 1.0000 Uiso R . . . . . H641 H 0.3967 0.2274 0.5689 0.0391 1.0000 Uiso R . . . . . H671 H 0.4693 0.5611 0.4537 0.0401 1.0000 Uiso R . . . . . H681 H 0.5621 0.6709 0.4544 0.0490 1.0000 Uiso R . . . . . H711 H 0.6695 0.5023 0.5192 0.0461 1.0000 Uiso R . . . . . H721 H 0.5751 0.3921 0.5176 0.0401 1.0000 Uiso R . . . . . H741 H 0.5410 0.3974 0.4334 0.0361 1.0000 Uiso R . . . . . H751 H 0.5421 0.3112 0.3867 0.0411 1.0000 Uiso R . . . . . H771 H 0.3922 0.1328 0.4107 0.0511 1.0000 Uiso R . . . . . H781 H 0.3884 0.2218 0.4570 0.0421 1.0000 Uiso R . . . . . H802 H 0.3971 0.1177 0.3266 0.0700 1.0000 Uiso R . . . . . H801 H 0.3638 0.1358 0.3577 0.0701 1.0000 Uiso R . . . . . H803 H 0.3903 0.2263 0.3395 0.0701 1.0000 Uiso R . . . . . H812 H 0.5387 0.1277 0.3311 0.0800 1.0000 Uiso R . . . . . H811 H 0.5662 0.2011 0.3579 0.0799 1.0000 Uiso R . . . . . H813 H 0.5107 0.2372 0.3312 0.0800 1.0000 Uiso R . . . . . H821 H 0.4761 -0.0013 0.3544 0.0779 1.0000 Uiso R . . . . . H822 H 0.5298 0.0291 0.3820 0.0780 1.0000 Uiso R . . . . . H823 H 0.4518 0.0184 0.3871 0.0778 1.0000 Uiso R . . . . . H841 H 0.4009 0.5142 0.5169 0.0449 1.0000 Uiso R . . . . . H851 H 0.3029 0.6094 0.5126 0.0441 1.0000 Uiso R . . . . . H871 H 0.2474 0.4884 0.4289 0.0460 1.0000 Uiso R . . . . . H881 H 0.3471 0.3936 0.4335 0.0481 1.0000 Uiso R . . . . . H1271 H 0.0957 0.5970 0.4622 0.0849 1.0000 Uiso R . . . . . H1272 H 0.1401 0.5295 0.4864 0.0850 1.0000 Uiso R . . . . . H1273 H 0.1368 0.5053 0.4508 0.0850 1.0000 Uiso R . . . . . H1291 H 0.1739 0.7437 0.4339 0.1111 1.0000 Uiso R . . . . . H1293 H 0.2384 0.6816 0.4262 0.1110 1.0000 Uiso R . . . . . H1292 H 0.1642 0.6377 0.4184 0.1110 1.0000 Uiso R . . . . . H1301 H 0.1520 0.7457 0.4856 0.1009 1.0000 Uiso R . . . . . H1302 H 0.2039 0.6799 0.5104 0.1010 1.0000 Uiso R . . . . . H1303 H 0.2361 0.7588 0.4860 0.1010 1.0000 Uiso R . . . . . H1321 H 0.4759 0.0083 0.9927 0.0700 1.0000 Uiso R . . . . . H1322 H 0.5054 0.0325 0.9599 0.0700 1.0000 Uiso R . . . . . H1351 H 0.7474 0.7286 0.8582 0.1101 1.0000 Uiso R . . . . . H1352 H 0.6691 0.7253 0.8633 0.1100 1.0000 Uiso R . . . . . H1353 H 0.6919 0.7199 0.8298 0.1100 1.0000 Uiso R . . . . . H1412 H 0.7431 0.7424 0.4540 0.1440 1.0000 Uiso R . . . . . H1411 H 0.7279 0.6149 0.4494 0.1440 1.0000 Uiso R . . . . . H1413 H 0.6626 0.7009 0.4383 0.1440 1.0000 Uiso R . . . . . H1442 H 0.6807 0.8343 0.4833 0.1100 1.0000 Uiso R . . . . . H1441 H 0.6620 0.7903 0.5151 0.1100 1.0000 Uiso R . . . . . H1443 H 0.6081 0.7855 0.4856 0.1101 1.0000 Uiso R . . . . . H1591 H 0.7800 0.7011 0.5076 0.0900 1.0000 Uiso R . . . . . H1592 H 0.7285 0.6618 0.5303 0.0900 1.0000 Uiso R . . . . . H1593 H 0.7599 0.5872 0.5074 0.0900 1.0000 Uiso R . . . . . H1602 H 0.1325 0.6413 0.8792 0.1560 1.0000 Uiso R . . . . . H1601 H 0.1952 0.7156 0.8830 0.1560 1.0000 Uiso R . . . . . H1603 H 0.2066 0.6016 0.8909 0.1560 1.0000 Uiso R . . . . . H1742 H 0.7891 0.6191 0.8849 0.1070 1.0000 Uiso R . . . . . H1741 H 0.7382 0.5453 0.8995 0.1070 1.0000 Uiso R . . . . . H1743 H 0.7905 0.5042 0.8773 0.1070 1.0000 Uiso R . . . . . H1851 H 0.3450 0.0547 0.9875 0.0900 1.0000 Uiso R . . . . . H1852 H 0.3211 0.1297 0.9607 0.0901 1.0000 Uiso R . . . . . H1853 H 0.3538 0.0258 0.9529 0.0901 1.0000 Uiso R . . . . . H1872 H 0.1637 0.4266 0.5918 0.1041 1.0000 Uiso R . . . . . H1871 H 0.1450 0.4087 0.5556 0.1041 1.0000 Uiso R . . . . . H1861 H 0.7835 0.5749 0.8250 0.1171 1.0000 Uiso R . . . . . H1863 H 0.7467 0.4661 0.8305 0.1170 1.0000 Uiso R . . . . . H1862 H 0.7063 0.5510 0.8076 0.1170 1.0000 Uiso R . . . . . H391 H 0.3271 0.1581 0.7183 0.0971 1.0000 Uiso R . . . . . H392 H 0.2472 0.1535 0.7132 0.0971 1.0000 Uiso R . . . . . H91 H 0.5190 0.4159 0.7260 0.0702 1.0000 Uiso R . . . . . H411 H 0.3694 0.2962 0.7572 0.0947 1.0000 Uiso R . . . . . C7 C 0.1952(8) 0.6247(11) 0.8434(4) 0.0521 1.0000 Uani . U . . . . O401 O 0.1319(12) 0.2539(19) 0.7281(6) 0.1174 0.7000 Uani . . . . . . H4011 H 0.1611 0.2965 0.7360 0.1770 0.7000 Uiso R . . . . . H4012 H 0.1110 0.2083 0.7372 0.1770 0.7000 Uiso R . . . . . H3051 H 0.5598 0.3310 0.5971 0.0878 1.0000 Uiso R . . . . . H3053 H 0.6059 0.4172 0.6116 0.0878 1.0000 Uiso R . . . . . H3052 H 0.5750 0.4234 0.5772 0.0878 1.0000 Uiso R . . . . . H3042 H 0.6760 0.2838 0.5999 0.0859 1.0000 Uiso R . . . . . H3041 H 0.6452 0.2901 0.5655 0.0859 1.0000 Uiso R . . . . . H3022 H 0.7873 0.3189 0.5840 0.1073 1.0000 Uiso R . . . . . H3021 H 0.7619 0.3357 0.5493 0.1073 1.0000 Uiso R . . . . . H3011 H 0.8630 0.4216 0.5616 0.1520 1.0000 Uiso R . . . . . H3012 H 0.8310 0.4828 0.5871 0.1520 1.0000 Uiso R . . . . . H3013 H 0.8056 0.4996 0.5523 0.1520 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 C1 0.061(4) 0.063(3) 0.050(5) 0.007(5) -0.001(5) 0.003(3) C2 0.073(5) 0.064(4) 0.052(6) 0.010(5) 0.007(5) 0.006(4) C3 0.084(5) 0.062(4) 0.051(6) 0.009(5) -0.001(6) 0.005(4) C4 0.078(5) 0.050(4) 0.051(6) 0.013(5) -0.011(5) -0.001(4) C5 0.068(4) 0.051(4) 0.048(5) 0.013(4) -0.009(4) -0.003(3) C6 0.062(4) 0.055(4) 0.043(6) 0.006(5) 0.000(5) -0.003(3) O7 0.086(5) 0.070(7) 0.087(8) -0.017(6) 0.006(7) -0.029(5) C8 0.066(4) 0.051(5) 0.062(6) 0.007(4) -0.010(5) -0.011(3) N9 0.054(4) 0.049(5) 0.074(6) 0.005(4) -0.009(4) -0.014(4) C10 0.053(4) 0.059(4) 0.076(7) 0.008(4) -0.009(5) -0.015(5) C11 0.058(6) 0.060(3) 0.079(6) 0.009(4) -0.004(5) -0.007(5) O12 0.047(5) 0.060(3) 0.075(5) 0.008(3) 0.002(4) -0.004(4) C13 0.040(5) 0.060(3) 0.070(4) 0.007(3) -0.005(5) -0.008(5) C14 0.039(6) 0.063(4) 0.071(4) 0.009(4) -0.003(5) -0.005(5) C15 0.044(6) 0.064(4) 0.070(4) 0.006(3) -0.004(5) -0.009(5) C16 0.036(5) 0.057(3) 0.070(4) 0.004(3) 0.000(5) -0.018(4) C17 0.040(5) 0.056(4) 0.070(4) 0.004(3) -0.004(5) -0.016(5) C18 0.033(5) 0.059(4) 0.068(4) 0.006(3) -0.004(5) -0.008(5) O19 0.050(5) 0.063(4) 0.074(5) 0.001(3) -0.001(5) -0.012(4) C20 0.049(6) 0.058(4) 0.080(6) -0.001(3) -0.002(5) -0.015(5) C21 0.039(5) 0.064(4) 0.091(7) -0.004(5) 0.006(4) -0.015(5) O22 0.038(4) 0.050(5) 0.085(6) -0.008(4) 0.006(4) -0.003(4) C23 0.049(4) 0.053(6) 0.085(6) -0.008(4) 0.016(4) -0.005(5) C24 0.054(4) 0.054(6) 0.082(6) -0.014(5) 0.014(4) -0.009(5) O25 0.050(4) 0.048(5) 0.072(6) -0.016(4) 0.010(3) -0.006(4) C26 0.052(4) 0.058(6) 0.082(6) -0.015(6) 0.005(3) -0.007(5) C27 0.050(4) 0.058(6) 0.089(7) -0.012(5) 0.003(4) -0.007(5) O28 0.055(5) 0.053(5) 0.085(6) -0.004(4) 0.008(4) -0.005(4) C29 0.054(6) 0.050(5) 0.088(6) 0.007(4) 0.006(5) -0.002(5) C30 0.048(6) 0.049(4) 0.080(6) 0.013(4) 0.005(4) -0.008(5) O31 0.057(5) 0.053(4) 0.073(5) 0.011(3) 0.007(5) 0.005(4) C32 0.063(6) 0.054(4) 0.072(4) 0.011(3) 0.005(5) 0.002(5) C33 0.056(6) 0.061(4) 0.072(4) 0.012(3) 0.007(6) 0.004(6) C34 0.058(6) 0.067(4) 0.075(4) 0.008(3) 0.016(6) 0.003(6) C35 0.056(6) 0.063(3) 0.081(4) 0.004(3) 0.015(5) -0.005(5) C36 0.054(6) 0.055(4) 0.083(5) 0.007(3) 0.015(6) 0.002(6) C37 0.059(6) 0.053(4) 0.077(4) 0.010(3) 0.009(6) 0.001(6) O38 0.070(6) 0.070(3) 0.087(5) -0.002(4) 0.015(5) -0.002(5) C39 0.065(7) 0.067(3) 0.089(6) -0.007(4) 0.014(6) -0.012(5) C40 0.070(7) 0.072(3) 0.086(7) -0.007(5) 0.012(6) -0.010(5) N41 0.067(6) 0.065(3) 0.081(6) -0.007(5) 0.012(6) -0.003(3) C42 0.055(4) 0.071(3) 0.061(6) -0.002(5) 0.006(5) 0.000(3) O43 0.053(4) 0.101(7) 0.095(9) 0.002(8) -0.002(6) 0.002(4) P1 0.0433(19) 0.0410(18) 0.066(2) -0.0063(18) 0.0077(16) -0.0060(16) F2 0.068(4) 0.104(6) 0.095(5) -0.023(6) 0.027(4) 0.013(4) F3 0.077(5) 0.034(4) 0.070(3) -0.001(3) 0.001(3) 0.008(4) F4 0.053(4) 0.110(6) 0.101(6) -0.030(6) 0.010(3) 0.018(4) F5 0.101(6) 0.040(3) 0.084(6) 0.008(3) -0.017(5) -0.017(3) F6 0.109(7) 0.045(3) 0.086(6) -0.003(3) 0.003(5) -0.023(4) F7 0.089(6) 0.058(5) 0.074(3) -0.001(4) -0.011(3) -0.009(5) N10 0.033(4) 0.020(2) 0.039(2) 0.0002(17) 0.006(3) 0.005(3) C190 0.034(5) 0.022(3) 0.036(2) -0.0026(19) 0.000(4) 0.002(4) C12 0.049(5) 0.024(3) 0.035(2) -0.0006(18) 0.003(4) 0.006(4) N13 0.066(5) 0.019(2) 0.035(2) 0.000(2) 0.008(4) 0.003(4) N14 0.061(5) 0.019(3) 0.036(2) 0.000(2) 0.005(4) 0.005(4) C191 0.040(5) 0.023(2) 0.0352(18) -0.0019(16) 0.004(4) -0.005(4) C192 0.034(5) 0.023(2) 0.033(3) -0.001(2) 0.005(4) -0.007(4) N17 0.037(4) 0.026(2) 0.032(2) -0.0005(15) 0.004(4) -0.004(3) C19 0.042(5) 0.025(3) 0.033(3) -0.001(2) 0.006(4) -0.008(4) C193 0.039(4) 0.028(3) 0.0345(18) -0.0013(17) 0.002(4) 0.000(4) C194 0.044(5) 0.022(3) 0.036(2) -0.0022(18) 0.006(4) -0.006(4) C22 0.048(5) 0.028(2) 0.034(2) -0.0020(18) 0.001(4) 0.000(4) N23 0.067(5) 0.026(2) 0.036(2) -0.003(2) 0.009(4) 0.000(4) N24 0.064(5) 0.023(2) 0.038(2) -0.003(2) 0.011(4) 0.000(4) N25 0.042(4) 0.025(2) 0.037(2) -0.0012(18) 0.006(3) -0.001(3) C195 0.034(5) 0.027(2) 0.033(3) -0.0022(19) -0.002(4) -0.004(4) C196 0.028(4) 0.022(3) 0.038(3) 0.000(2) 0.007(3) -0.001(2) C28 0.025(4) 0.028(4) 0.041(4) 0.000(3) 0.007(3) -0.004(3) C197 0.031(5) 0.030(4) 0.037(4) 0.001(3) 0.011(3) -0.007(3) C198 0.027(4) 0.025(3) 0.036(3) 0.003(2) 0.007(3) -0.001(2) C31 0.020(4) 0.028(3) 0.038(4) -0.002(3) 0.005(3) -0.007(3) C199 0.026(4) 0.022(3) 0.039(4) 0.002(3) 0.007(3) 0.000(3) C200 0.032(2) 0.025(3) 0.038(3) 0.0022(16) 0.008(2) 0.0000(16) C201 0.029(2) 0.019(3) 0.037(4) 0.006(2) 0.009(3) -0.004(2) C202 0.025(3) 0.021(3) 0.044(5) 0.002(3) 0.015(3) -0.007(2) C203 0.033(3) 0.022(4) 0.047(5) 0.006(3) 0.013(4) 0.000(2) C204 0.031(3) 0.028(3) 0.054(5) 0.010(3) 0.008(3) 0.003(3) C38 0.031(3) 0.033(4) 0.051(5) 0.005(4) 0.003(4) -0.002(3) C205 0.033(3) 0.027(4) 0.041(5) 0.001(3) 0.004(3) -0.003(3) C41 0.030(4) 0.047(7) 0.116(10) 0.017(7) 0.006(6) 0.010(4) C207 0.037(7) 0.045(6) 0.132(11) 0.039(7) 0.021(8) 0.016(5) C43 0.029(4) 0.022(3) 0.037(3) 0.001(2) 0.007(3) 0.003(2) C44 0.027(4) 0.022(4) 0.039(4) 0.003(3) 0.007(3) 0.004(3) C45 0.026(4) 0.023(4) 0.039(4) 0.003(3) 0.008(3) 0.004(3) C46 0.030(4) 0.020(4) 0.043(4) 0.005(3) 0.010(3) 0.003(3) C47 0.033(4) 0.025(4) 0.043(4) 0.003(3) 0.009(3) 0.010(3) C48 0.030(4) 0.020(4) 0.042(4) 0.000(3) 0.010(3) 0.003(3) C49 0.051(5) 0.026(5) 0.042(4) 0.007(3) 0.011(4) 0.008(3) C50 0.084(10) 0.047(7) 0.043(4) -0.001(5) 0.009(7) 0.018(6) C51 0.029(2) 0.022(3) 0.038(4) -0.002(2) 0.011(2) 0.003(2) C52 0.043(4) 0.024(4) 0.035(4) -0.004(3) 0.012(3) -0.005(3) C53 0.046(4) 0.029(5) 0.042(5) -0.004(3) 0.016(3) -0.008(4) C54 0.035(3) 0.035(4) 0.056(4) -0.004(3) 0.018(3) 0.000(3) C55 0.031(3) 0.030(5) 0.052(5) -0.005(3) 0.007(3) 0.001(3) C56 0.032(3) 0.025(4) 0.040(4) -0.006(3) 0.008(3) 0.002(3) C57 0.042(4) 0.049(5) 0.083(6) 0.000(4) 0.019(4) -0.010(4) C58 0.077(9) 0.032(4) 0.031(5) 0.002(2) 0.005(6) 0.012(6) C59 0.025(4) 0.018(3) 0.040(3) -0.001(2) 0.005(3) 0.001(2) C60 0.019(4) 0.020(4) 0.042(4) 0.000(3) 0.003(3) 0.000(3) C61 0.024(4) 0.022(4) 0.039(4) 0.000(3) 0.005(3) 0.003(3) C62 0.028(4) 0.020(3) 0.039(3) 0.002(2) 0.008(3) 0.004(2) C63 0.029(4) 0.023(4) 0.042(4) 0.004(3) 0.009(3) 0.005(3) C64 0.027(4) 0.020(4) 0.039(4) 0.001(3) 0.007(3) 0.002(3) C65 0.026(2) 0.023(2) 0.039(2) 0.0037(16) 0.004(2) 0.0005(16) C66 0.022(2) 0.023(3) 0.036(4) 0.001(2) 0.009(3) 0.002(2) C67 0.027(3) 0.023(4) 0.038(5) 0.002(3) 0.006(3) 0.000(3) C68 0.033(4) 0.022(4) 0.047(5) 0.000(3) 0.005(3) -0.003(3) C69 0.023(3) 0.030(4) 0.052(5) 0.000(3) 0.012(3) -0.001(3) C70 0.033(4) 0.045(4) 0.073(6) 0.005(4) 0.009(4) -0.014(3) C71 0.022(3) 0.029(4) 0.047(5) -0.002(3) 0.007(3) 0.002(3) C72 0.024(3) 0.026(4) 0.038(5) 0.001(3) 0.006(3) 0.002(3) C73 0.023(3) 0.021(3) 0.039(3) 0.005(2) 0.004(2) 0.000(2) C74 0.018(4) 0.020(4) 0.042(4) 0.000(3) 0.004(3) 0.000(3) C75 0.025(4) 0.019(4) 0.043(4) 0.000(3) 0.006(3) 0.002(3) C76 0.026(4) 0.020(3) 0.043(3) -0.001(3) 0.006(3) 0.001(3) C77 0.029(4) 0.024(4) 0.043(4) 0.001(3) 0.006(3) -0.002(3) C78 0.026(4) 0.024(4) 0.041(4) 0.003(3) 0.007(3) -0.003(3) C79 0.026(4) 0.021(3) 0.049(4) -0.006(3) 0.008(3) 0.005(3) C80 0.033(4) 0.015(5) 0.056(6) -0.013(5) -0.001(4) 0.005(4) C81 0.041(5) 0.034(6) 0.054(6) -0.017(5) 0.018(5) -0.009(5) C82 0.044(7) 0.023(3) 0.050(7) -0.004(3) 0.003(5) 0.010(4) C83 0.024(2) 0.017(3) 0.040(3) 0.004(2) 0.005(2) -0.003(2) C84 0.031(4) 0.020(4) 0.045(4) 0.000(3) 0.008(3) -0.002(3) C85 0.030(4) 0.019(4) 0.053(4) 0.000(3) 0.012(3) -0.003(3) C86 0.022(3) 0.023(4) 0.062(4) 0.002(3) 0.009(3) -0.006(3) C87 0.016(3) 0.026(4) 0.049(4) 0.007(3) 0.007(3) -0.008(3) C88 0.024(3) 0.027(4) 0.043(4) 0.003(3) 0.003(3) -0.002(3) C127 0.022(3) 0.033(6) 0.098(10) -0.022(6) 0.017(6) -0.001(4) C128 0.023(4) 0.036(5) 0.085(6) -0.003(3) 0.008(3) -0.001(3) C129 0.038(7) 0.050(8) 0.101(7) 0.018(6) 0.003(6) 0.015(6) C130 0.022(6) 0.029(6) 0.114(8) -0.013(6) 0.010(6) -0.004(4) C132 0.080(7) 0.034(6) 0.061(8) 0.019(5) 0.022(7) 0.025(6) C135 0.060(9) 0.047(5) 0.101(11) -0.001(6) 0.009(8) -0.019(5) C141 0.053(9) 0.093(11) 0.084(6) 0.015(7) 0.023(6) -0.037(8) C144 0.048(8) 0.038(4) 0.123(12) -0.003(7) -0.003(8) -0.019(4) C159 0.037(6) 0.059(8) 0.095(8) 0.005(8) -0.005(6) -0.018(5) C160 0.043(8) 0.086(11) 0.094(7) 0.009(6) 0.021(6) 0.036(7) C174 0.034(5) 0.071(9) 0.099(8) 0.006(8) 0.013(5) -0.010(7) C185 0.067(6) 0.031(7) 0.081(9) 0.021(6) 0.024(6) -0.010(5) Cl56 0.075(3) 0.084(3) 0.145(5) -0.006(4) 0.024(4) 0.004(3) Cl91 0.089(4) 0.074(3) 0.111(4) 0.007(3) 0.005(3) 0.000(3) C187 0.071(7) 0.069(4) 0.118(11) -0.008(9) 0.014(9) -0.002(6) C186 0.027(6) 0.073(8) 0.103(8) -0.019(8) 0.029(6) -0.026(7) O303 0.061(5) 0.077(7) 0.079(7) 0.010(6) 0.012(5) -0.011(5) C305 0.061(7) 0.061(9) 0.079(11) -0.010(8) 0.011(7) -0.017(6) C304 0.065(6) 0.064(8) 0.076(8) -0.002(7) 0.011(6) -0.010(5) C302 0.057(6) 0.089(9) 0.086(8) 0.004(8) 0.004(6) -0.008(6) C301 0.070(8) 0.125(13) 0.083(11) 0.005(12) 0.014(9) -0.032(9) C7 0.038(4) 0.037(4) 0.082(6) 0.018(4) 0.008(4) 0.011(3) O401 0.075(14) 0.12(2) 0.15(2) 0.073(18) -0.022(14) -0.029(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 3.89(16) loop_ _oxford_twin_element_scale_factors 0.572(6) 0.275(4) 0.153(8) 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 C1 . C2 . 1.44(2) yes C1 . C6 . 1.35(2) yes C1 . C42 . 1.45(3) yes C2 . C3 . 1.33(3) yes C2 . H21 . 0.929 no C3 . C4 . 1.39(3) yes C3 . H31 . 0.929 no C4 . C5 . 1.42(2) yes C4 . H41 . 0.933 no C5 . C6 . 1.42(2) yes C5 . C8 . 1.44(3) yes C6 . H61 . 0.929 no O7 . C8 . 1.28(2) yes C8 . N9 . 1.40(2) yes N9 . C10 . 1.41(2) yes N9 . H91 . 0.900 no C10 . C11 . 1.51(3) yes C10 . H101 . 0.966 no C10 . H102 . 0.967 no C11 . O12 . 1.40(2) yes C11 . H111 . 0.969 no C11 . H112 . 0.974 no O12 . C13 . 1.40(2) yes C13 . C14 . 1.38(2) yes C13 . C18 . 1.34(2) yes C14 . C15 . 1.40(3) yes C14 . H141 . 0.930 no C15 . C16 . 1.35(2) yes C15 . H151 . 0.928 no C16 . C17 . 1.33(2) yes C16 . O19 . 1.38(2) yes C17 . C18 . 1.43(2) yes C17 . H171 . 0.931 no C18 . H181 . 0.931 no O19 . C20 . 1.44(2) yes C20 . C21 . 1.515(9) yes C20 . H202 . 0.969 no C20 . H201 . 0.970 no C21 . O22 . 1.431(8) yes C21 . H211 . 0.967 no C21 . H212 . 0.969 no O22 . C23 . 1.434(9) yes C23 . C24 . 1.523(9) yes C23 . H231 . 0.972 no C23 . H232 . 0.969 no C24 . O25 . 1.430(9) yes C24 . H241 . 0.974 no C24 . H242 . 0.971 no O25 . C26 . 1.433(9) yes C26 . C27 . 1.520(9) yes C26 . H261 . 0.972 no C26 . H262 . 0.972 no C27 . O28 . 1.423(9) yes C27 . H271 . 0.968 no C27 . H272 . 0.970 no O28 . C29 . 1.431(9) yes C29 . C30 . 1.520(9) yes C29 . H291 . 0.969 no C29 . H292 . 0.968 no C30 . O31 . 1.424(19) yes C30 . H301 . 0.969 no C30 . H302 . 0.972 no O31 . C32 . 1.354(19) yes C32 . C33 . 1.397(9) yes C32 . C37 . 1.401(9) yes C33 . C34 . 1.396(9) yes C33 . H331 . 0.928 no C34 . C35 . 1.388(9) yes C34 . H341 . 0.930 no C35 . C36 . 1.395(9) yes C35 . O38 . 1.41(2) yes C36 . C37 . 1.395(9) yes C36 . H361 . 0.928 no C37 . H371 . 0.934 no O38 . C39 . 1.37(2) yes C39 . C40 . 1.54(3) yes C39 . H391 . 0.950 no C39 . H392 . 0.950 no C40 . N41 . 1.48(2) yes C40 . H401 . 0.973 no C40 . H402 . 0.972 no N41 . C42 . 1.36(2) yes N41 . H411 . 0.908 no C42 . O43 . 1.24(2) yes P1 . F2 . 1.582(11) yes P1 . F3 . 1.629(11) yes P1 . F4 . 1.558(11) yes P1 . F5 . 1.570(10) yes P1 . F6 . 1.568(10) yes P1 . F7 . 1.590(11) yes N10 . C190 . 1.332(16) yes N10 . N14 . 1.333(14) yes N10 . C59 . 1.469(15) yes C190 . C12 . 1.356(17) yes C190 . H1901 . 0.930 no C12 . N13 . 1.380(16) yes C12 . C191 . 1.452(17) yes N13 . N14 . 1.304(15) yes C191 . C192 . 1.403(17) yes C191 . C194 . 1.402(18) yes C192 . N17 . 1.326(15) yes C192 . H1921 . 0.930 no N17 . C19 . 1.354(16) yes N17 . C58 . 1.495(16) yes C19 . C193 . 1.386(18) yes C19 . H191 . 0.924 no C193 . C194 . 1.366(18) yes C193 . C22 . 1.457(18) yes C194 . H1941 . 0.925 no C22 . N23 . 1.353(17) yes C22 . C195 . 1.382(18) yes N23 . N24 . 1.298(15) yes N24 . N25 . 1.361(15) yes N25 . C195 . 1.323(16) yes N25 . C196 . 1.423(15) yes C195 . H1951 . 0.928 no C196 . C28 . 1.397(16) yes C196 . C199 . 1.388(16) yes C28 . C197 . 1.385(17) yes C28 . H281 . 0.932 no C197 . C198 . 1.350(17) yes C197 . H1971 . 0.931 no C198 . C31 . 1.441(16) yes C198 . C200 . 1.546(17) yes C31 . C199 . 1.371(17) yes C31 . H311 . 0.933 no C199 . H1991 . 0.925 no C200 . C201 . 1.566(16) yes C200 . C43 . 1.597(17) yes C200 . C51 . 1.480(17) yes C201 . C202 . 1.420(16) yes C201 . C205 . 1.391(17) yes C202 . C203 . 1.381(17) yes C202 . H2021 . 0.928 no C203 . C204 . 1.374(18) yes C203 . H2031 . 0.929 no C204 . C38 . 1.399(19) yes C204 . C7 . 1.541(18) yes C38 . C205 . 1.360(18) yes C38 . H381 . 0.935 no C205 . H2051 . 0.933 no C41 . H414 . 0.960 no C41 . H412 . 0.960 no C41 . H413 . 0.961 no C41 . C7 . 1.50(2) yes C207 . H2071 . 0.957 no C207 . H2073 . 0.961 no C207 . H2072 . 0.963 no C207 . C7 . 1.56(2) yes C43 . C44 . 1.402(16) yes C43 . C48 . 1.390(16) yes C44 . C45 . 1.386(17) yes C44 . H441 . 0.934 no C45 . C46 . 1.377(16) yes C45 . H451 . 0.927 no C46 . C47 . 1.410(17) yes C46 . C49 . 1.538(17) yes C47 . C48 . 1.386(18) yes C47 . H471 . 0.930 no C48 . H481 . 0.935 no C49 . C50 . 1.54(2) yes C49 . C132 . 1.464(19) yes C49 . C185 . 1.55(2) yes C50 . H503 . 0.959 no C50 . H502 . 0.959 no C50 . H501 . 0.959 no C51 . C52 . 1.426(17) yes C51 . C56 . 1.412(18) yes C52 . C53 . 1.367(18) yes C52 . H521 . 0.931 no C53 . C54 . 1.36(2) yes C53 . H531 . 0.927 no C54 . C55 . 1.45(2) yes C54 . C57 . 1.529(19) yes C55 . C56 . 1.377(18) yes C55 . H551 . 0.934 no C56 . H561 . 0.925 no C57 . C135 . 1.53(2) yes C57 . C174 . 1.50(2) yes C57 . C186 . 1.526(9) yes C58 . H582 . 0.960 no C58 . H581 . 0.962 no C58 . H583 . 0.963 no C59 . C60 . 1.404(16) yes C59 . C64 . 1.337(16) yes C60 . C61 . 1.406(16) yes C60 . H601 . 0.934 no C61 . C62 . 1.396(16) yes C61 . H611 . 0.930 no C62 . C63 . 1.394(17) yes C62 . C65 . 1.550(16) yes C63 . C64 . 1.408(16) yes C63 . H631 . 0.934 no C64 . H641 . 0.929 no C65 . C66 . 1.569(16) yes C65 . C73 . 1.568(17) yes C65 . C83 . 1.520(16) yes C66 . C67 . 1.382(16) yes C66 . C72 . 1.356(16) yes C67 . C68 . 1.413(17) yes C67 . H671 . 0.927 no C68 . C69 . 1.377(18) yes C68 . H681 . 0.930 no C69 . C70 . 1.528(18) yes C69 . C71 . 1.407(18) yes C70 . C141 . 1.53(2) yes C70 . C144 . 1.56(2) yes C70 . C159 . 1.48(2) yes C71 . C72 . 1.438(16) yes C71 . H711 . 0.929 no C72 . H721 . 0.934 no C73 . C74 . 1.353(16) yes C73 . C78 . 1.412(16) yes C74 . C75 . 1.410(17) yes C74 . H741 . 0.928 no C75 . C76 . 1.394(16) yes C75 . H751 . 0.930 no C76 . C77 . 1.387(17) yes C76 . C79 . 1.536(17) yes C77 . C78 . 1.430(17) yes C77 . H771 . 0.929 no C78 . H781 . 0.932 no C79 . C80 . 1.542(17) yes C79 . C81 . 1.510(17) yes C79 . C82 . 1.535(17) yes C80 . H802 . 0.962 no C80 . H801 . 0.958 no C80 . H803 . 0.956 no C81 . H812 . 0.955 no C81 . H811 . 0.963 no C81 . H813 . 0.960 no C82 . H821 . 0.960 no C82 . H822 . 0.961 no C82 . H823 . 0.959 no C83 . C84 . 1.395(17) yes C83 . C88 . 1.425(17) yes C84 . C85 . 1.359(17) yes C84 . H841 . 0.931 no C85 . C86 . 1.428(19) yes C85 . H851 . 0.932 no C86 . C87 . 1.393(18) yes C86 . C128 . 1.518(18) yes C87 . C88 . 1.392(16) yes C87 . H871 . 0.933 no C88 . H881 . 0.923 no C127 . C128 . 1.510(18) yes C127 . H1271 . 0.961 no C127 . H1272 . 0.961 no C127 . H1273 . 0.958 no C128 . C129 . 1.54(2) yes C128 . C130 . 1.55(2) yes C129 . H1291 . 0.962 no C129 . H1293 . 0.961 no C129 . H1292 . 0.960 no C130 . H1301 . 1.002 no C130 . H1302 . 1.006 no C130 . H1303 . 1.005 no C132 . H1321 . 0.932 no C132 . H1322 . 0.933 no C135 . H1351 . 0.958 no C135 . H1352 . 0.961 no C135 . H1353 . 0.957 no C141 . H1412 . 1.047 no C141 . H1411 . 1.048 no C141 . H1413 . 1.051 no C144 . H1442 . 0.964 no C144 . H1441 . 0.965 no C144 . H1443 . 0.960 no C159 . H1591 . 0.958 no C159 . H1592 . 0.961 no C159 . H1593 . 0.964 no C160 . H1602 . 0.962 no C160 . H1601 . 0.961 no C160 . H1603 . 0.963 no C160 . C7 . 1.55(2) yes C174 . H1742 . 0.962 no C174 . H1741 . 0.961 no C174 . H1743 . 0.961 no C185 . H1851 . 0.960 no C185 . H1852 . 0.964 no C185 . H1853 . 0.966 no Cl56 . C187 . 1.81(2) yes Cl91 . C187 . 1.67(2) yes C187 . H1872 . 0.972 no C187 . H1871 . 0.970 no C186 . H1861 . 0.999 no C186 . H1863 . 1.002 no C186 . H1862 . 0.999 no O303 . C304 . 1.433(9) yes O303 . C302 . 1.436(9) yes C305 . C304 . 1.510(9) yes C305 . H3051 . 0.950 no C305 . H3053 . 0.950 no C305 . H3052 . 0.950 no C304 . H3042 . 0.950 no C304 . H3041 . 0.950 no C302 . C301 . 1.516(9) yes C302 . H3022 . 0.950 no C302 . H3021 . 0.950 no C301 . H3011 . 0.950 no C301 . H3012 . 0.950 no C301 . H3013 . 0.950 no O401 . H4011 . 0.850 no O401 . H4012 . 0.850 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 C2 . C1 . C6 . 117.1(17) yes C2 . C1 . C42 . 116.3(16) yes C6 . C1 . C42 . 126.5(18) yes C1 . C2 . C3 . 120.6(18) yes C1 . C2 . H21 . 121.1 no C3 . C2 . H21 . 118.3 no C2 . C3 . C4 . 122.4(19) yes C2 . C3 . H31 . 118.2 no C4 . C3 . H31 . 119.5 no C3 . C4 . C5 . 119.5(17) yes C3 . C4 . H41 . 119.4 no C5 . C4 . H41 . 121.1 no C4 . C5 . C6 . 116.4(17) yes C4 . C5 . C8 . 121.2(16) yes C6 . C5 . C8 . 122.2(17) yes C5 . C6 . C1 . 124.0(17) yes C5 . C6 . H61 . 116.8 no C1 . C6 . H61 . 119.2 no C5 . C8 . O7 . 120.8(18) yes C5 . C8 . N9 . 122.6(15) yes O7 . C8 . N9 . 116.6(17) yes C8 . N9 . C10 . 122.9(14) yes C8 . N9 . H91 . 117.4 no C10 . N9 . H91 . 119.7 no N9 . C10 . C11 . 108.4(14) yes N9 . C10 . H101 . 108.9 no C11 . C10 . H101 . 111.0 no N9 . C10 . H102 . 109.3 no C11 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.8 no C10 . C11 . O12 . 109.9(15) yes C10 . C11 . H111 . 107.3 no O12 . C11 . H111 . 106.7 no C10 . C11 . H112 . 112.1 no O12 . C11 . H112 . 111.0 no H111 . C11 . H112 . 109.7 no C11 . O12 . C13 . 119.8(14) yes O12 . C13 . C14 . 121.8(16) yes O12 . C13 . C18 . 115.3(16) yes C14 . C13 . C18 . 122.6(18) yes C13 . C14 . C15 . 117.1(17) yes C13 . C14 . H141 . 120.4 no C15 . C14 . H141 . 122.5 no C14 . C15 . C16 . 121.1(17) yes C14 . C15 . H151 . 119.5 no C16 . C15 . H151 . 119.5 no C15 . C16 . C17 . 121.5(18) yes C15 . C16 . O19 . 115.7(16) yes C17 . C16 . O19 . 122.8(16) yes C16 . C17 . C18 . 119.5(16) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 120.5 no C17 . C18 . C13 . 118.2(17) yes C17 . C18 . H181 . 121.6 no C13 . C18 . H181 . 120.2 no C16 . O19 . C20 . 116.9(13) yes O19 . C20 . C21 . 104.7(14) yes O19 . C20 . H202 . 108.4 no C21 . C20 . H202 . 109.7 no O19 . C20 . H201 . 111.4 no C21 . C20 . H201 . 112.9 no H202 . C20 . H201 . 109.5 no C20 . C21 . O22 . 108.0(12) yes C20 . C21 . H211 . 108.5 no O22 . C21 . H211 . 108.6 no C20 . C21 . H212 . 112.4 no O22 . C21 . H212 . 109.6 no H211 . C21 . H212 . 109.5 no C21 . O22 . C23 . 112.1(11) yes O22 . C23 . C24 . 105.8(12) yes O22 . C23 . H231 . 109.6 no C24 . C23 . H231 . 108.0 no O22 . C23 . H232 . 111.6 no C24 . C23 . H232 . 112.3 no H231 . C23 . H232 . 109.5 no C23 . C24 . O25 . 108.4(12) yes C23 . C24 . H241 . 108.3 no O25 . C24 . H241 . 110.5 no C23 . C24 . H242 . 110.6 no O25 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.7 no C24 . O25 . C26 . 110.4(11) yes O25 . C26 . C27 . 111.4(13) yes O25 . C26 . H261 . 110.8 no C27 . C26 . H261 . 109.0 no O25 . C26 . H262 . 107.6 no C27 . C26 . H262 . 109.0 no H261 . C26 . H262 . 109.1 no C26 . C27 . O28 . 105.9(12) yes C26 . C27 . H271 . 108.8 no O28 . C27 . H271 . 109.9 no C26 . C27 . H272 . 111.2 no O28 . C27 . H272 . 111.6 no H271 . C27 . H272 . 109.4 no C27 . O28 . C29 . 111.3(11) yes O28 . C29 . C30 . 109.4(12) yes O28 . C29 . H291 . 112.0 no C30 . C29 . H291 . 108.8 no O28 . C29 . H292 . 108.2 no C30 . C29 . H292 . 108.8 no H291 . C29 . H292 . 109.6 no C29 . C30 . O31 . 104.5(13) yes C29 . C30 . H301 . 109.4 no O31 . C30 . H301 . 109.9 no C29 . C30 . H302 . 111.5 no O31 . C30 . H302 . 112.2 no H301 . C30 . H302 . 109.2 no C30 . O31 . C32 . 114.9(11) yes O31 . C32 . C33 . 124.9(13) yes O31 . C32 . C37 . 115.6(13) yes C33 . C32 . C37 . 119.3(16) yes C32 . C33 . C34 . 119.7(16) yes C32 . C33 . H331 . 119.6 no C34 . C33 . H331 . 120.6 no C33 . C34 . C35 . 119.5(16) yes C33 . C34 . H341 . 119.5 no C35 . C34 . H341 . 120.9 no C34 . C35 . C36 . 122.1(17) yes C34 . C35 . O38 . 114.4(13) yes C36 . C35 . O38 . 123.1(13) yes C35 . C36 . C37 . 117.5(16) yes C35 . C36 . H361 . 117.8 no C37 . C36 . H361 . 124.7 no C32 . C37 . C36 . 121.5(16) yes C32 . C37 . H371 . 118.6 no C36 . C37 . H371 . 119.9 no C35 . O38 . C39 . 117.3(14) yes O38 . C39 . C40 . 108.6(17) yes O38 . C39 . H391 . 108.8 no C40 . C39 . H391 . 109.1 no O38 . C39 . H392 . 110.1 no C40 . C39 . H392 . 110.7 no H391 . C39 . H392 . 109.5 no C39 . C40 . N41 . 112.2(16) yes C39 . C40 . H401 . 109.5 no N41 . C40 . H401 . 109.9 no C39 . C40 . H402 . 107.5 no N41 . C40 . H402 . 108.5 no H401 . C40 . H402 . 109.3 no C40 . N41 . C42 . 122.2(16) yes C40 . N41 . H411 . 118.6 no C42 . N41 . H411 . 119.1 no C1 . C42 . N41 . 113.9(16) yes C1 . C42 . O43 . 125.7(19) yes N41 . C42 . O43 . 120.3(19) yes F2 . P1 . F3 . 92.3(6) yes F2 . P1 . F4 . 178.3(8) yes F3 . P1 . F4 . 87.8(6) yes F2 . P1 . F5 . 90.6(7) yes F3 . P1 . F5 . 88.2(6) yes F4 . P1 . F5 . 91.1(7) yes F2 . P1 . F6 . 87.7(7) yes F3 . P1 . F6 . 89.6(6) yes F4 . P1 . F6 . 90.7(7) yes F5 . P1 . F6 . 177.1(7) yes F2 . P1 . F7 . 90.8(7) yes F3 . P1 . F7 . 176.9(6) yes F4 . P1 . F7 . 89.1(7) yes F5 . P1 . F7 . 91.5(6) yes F6 . P1 . F7 . 90.8(6) yes C190 . N10 . N14 . 110.7(10) yes C190 . N10 . C59 . 129.7(10) yes N14 . N10 . C59 . 119.6(10) yes N10 . C190 . C12 . 105.9(11) yes N10 . C190 . H1901 . 127.2 no C12 . C190 . H1901 . 127.0 no C190 . C12 . N13 . 107.3(11) yes C190 . C12 . C191 . 132.4(12) yes N13 . C12 . C191 . 120.2(11) yes C12 . N13 . N14 . 108.2(10) yes N10 . N14 . N13 . 107.9(10) yes C12 . C191 . C192 . 118.6(11) yes C12 . C191 . C194 . 123.4(11) yes C192 . C191 . C194 . 117.8(11) yes C191 . C192 . N17 . 119.3(12) yes C191 . C192 . H1921 . 120.4 no N17 . C192 . H1921 . 120.2 no C192 . N17 . C19 . 123.8(11) yes C192 . N17 . C58 . 117.5(10) yes C19 . N17 . C58 . 118.3(10) yes N17 . C19 . C193 . 118.8(12) yes N17 . C19 . H191 . 120.3 no C193 . C19 . H191 . 120.9 no C19 . C193 . C194 . 119.3(12) yes C19 . C193 . C22 . 117.7(12) yes C194 . C193 . C22 . 123.0(11) yes C191 . C194 . C193 . 120.9(11) yes C191 . C194 . H1941 . 119.9 no C193 . C194 . H1941 . 119.0 no C193 . C22 . N23 . 122.3(12) yes C193 . C22 . C195 . 130.2(12) yes N23 . C22 . C195 . 107.6(11) yes C22 . N23 . N24 . 109.1(11) yes N23 . N24 . N25 . 107.7(10) yes N24 . N25 . C195 . 109.9(10) yes N24 . N25 . C196 . 118.0(10) yes C195 . N25 . C196 . 132.1(11) yes C22 . C195 . N25 . 105.7(11) yes C22 . C195 . H1951 . 126.9 no N25 . C195 . H1951 . 127.4 no N25 . C196 . C28 . 119.6(11) yes N25 . C196 . C199 . 120.1(11) yes C28 . C196 . C199 . 120.2(11) yes C196 . C28 . C197 . 118.0(11) yes C196 . C28 . H281 . 120.7 no C197 . C28 . H281 . 121.4 no C28 . C197 . C198 . 124.1(11) yes C28 . C197 . H1971 . 117.9 no C198 . C197 . H1971 . 118.1 no C197 . C198 . C31 . 117.1(11) yes C197 . C198 . C200 . 121.7(11) yes C31 . C198 . C200 . 121.2(10) yes C198 . C31 . C199 . 120.2(11) yes C198 . C31 . H311 . 120.0 no C199 . C31 . H311 . 119.8 no C196 . C199 . C31 . 120.5(11) yes C196 . C199 . H1991 . 120.2 no C31 . C199 . H1991 . 119.3 no C198 . C200 . C201 . 111.8(10) yes C198 . C200 . C43 . 104.3(9) yes C201 . C200 . C43 . 106.0(9) yes C198 . C200 . C51 . 110.7(10) yes C201 . C200 . C51 . 112.1(9) yes C43 . C200 . C51 . 111.6(10) yes C200 . C201 . C202 . 119.3(10) yes C200 . C201 . C205 . 124.7(11) yes C202 . C201 . C205 . 115.9(11) yes C201 . C202 . C203 . 121.2(12) yes C201 . C202 . H2021 . 119.6 no C203 . C202 . H2021 . 119.2 no C202 . C203 . C204 . 121.5(12) yes C202 . C203 . H2031 . 118.8 no C204 . C203 . H2031 . 119.7 no C203 . C204 . C38 . 117.3(12) yes C203 . C204 . C7 . 121.6(13) yes C38 . C204 . C7 . 121.0(13) yes C204 . C38 . C205 . 121.6(13) yes C204 . C38 . H381 . 119.1 no C205 . C38 . H381 . 119.2 no C201 . C205 . C38 . 122.3(12) yes C201 . C205 . H2051 . 118.2 no C38 . C205 . H2051 . 119.5 no H414 . C41 . H412 . 109.5 no H414 . C41 . H413 . 109.2 no H412 . C41 . H413 . 109.4 no H414 . C41 . C7 . 111.4 no H412 . C41 . C7 . 110.0 no H413 . C41 . C7 . 107.3 no H2071 . C207 . H2073 . 109.7 no H2071 . C207 . H2072 . 109.5 no H2073 . C207 . H2072 . 109.6 no H2071 . C207 . C7 . 111.9 no H2073 . C207 . C7 . 105.5 no H2072 . C207 . C7 . 110.5 no C200 . C43 . C44 . 122.7(10) yes C200 . C43 . C48 . 118.9(10) yes C44 . C43 . C48 . 118.4(11) yes C43 . C44 . C45 . 118.0(11) yes C43 . C44 . H441 . 119.9 no C45 . C44 . H441 . 122.0 no C44 . C45 . C46 . 124.6(11) yes C44 . C45 . H451 . 117.5 no C46 . C45 . H451 . 117.8 no C45 . C46 . C47 . 116.7(11) yes C45 . C46 . C49 . 121.6(11) yes C47 . C46 . C49 . 121.8(11) yes C46 . C47 . C48 . 119.6(11) yes C46 . C47 . H471 . 120.4 no C48 . C47 . H471 . 120.0 no C43 . C48 . C47 . 122.4(11) yes C43 . C48 . H481 . 119.6 no C47 . C48 . H481 . 118.0 no C46 . C49 . C50 . 109.7(11) yes C46 . C49 . C132 . 114.8(12) yes C50 . C49 . C132 . 112.1(13) yes C46 . C49 . C185 . 108.5(11) yes C50 . C49 . C185 . 106.7(13) yes C132 . C49 . C185 . 104.6(12) yes C49 . C50 . H503 . 108.4 no C49 . C50 . H502 . 110.7 no H503 . C50 . H502 . 109.8 no C49 . C50 . H501 . 109.4 no H503 . C50 . H501 . 109.4 no H502 . C50 . H501 . 109.1 no C200 . C51 . C52 . 120.0(11) yes C200 . C51 . C56 . 125.3(11) yes C52 . C51 . C56 . 114.7(11) yes C51 . C52 . C53 . 121.1(13) yes C51 . C52 . H521 . 118.7 no C53 . C52 . H521 . 120.1 no C52 . C53 . C54 . 124.8(13) yes C52 . C53 . H531 . 117.7 no C54 . C53 . H531 . 117.4 no C53 . C54 . C55 . 115.2(12) yes C53 . C54 . C57 . 124.9(13) yes C55 . C54 . C57 . 119.7(13) yes C54 . C55 . C56 . 120.8(13) yes C54 . C55 . H551 . 121.4 no C56 . C55 . H551 . 117.8 no C51 . C56 . C55 . 122.8(12) yes C51 . C56 . H561 . 118.6 no C55 . C56 . H561 . 118.6 no C54 . C57 . C135 . 110.0(13) yes C54 . C57 . C174 . 114.0(13) yes C135 . C57 . C174 . 110.8(15) yes C54 . C57 . C186 . 107.0(11) yes C135 . C57 . C186 . 110.8(15) yes C174 . C57 . C186 . 104.0(15) yes N17 . C58 . H582 . 110.7 no N17 . C58 . H581 . 111.1 no H582 . C58 . H581 . 109.2 no N17 . C58 . H583 . 107.8 no H582 . C58 . H583 . 109.1 no H581 . C58 . H583 . 108.9 no N10 . C59 . C60 . 113.1(10) yes N10 . C59 . C64 . 123.4(11) yes C60 . C59 . C64 . 123.4(11) yes C59 . C60 . C61 . 116.1(10) yes C59 . C60 . H601 . 123.1 no C61 . C60 . H601 . 120.9 no C60 . C61 . C62 . 122.6(11) yes C60 . C61 . H611 . 118.5 no C62 . C61 . H611 . 118.9 no C61 . C62 . C63 . 117.7(11) yes C61 . C62 . C65 . 116.9(10) yes C63 . C62 . C65 . 125.4(10) yes C62 . C63 . C64 . 120.8(11) yes C62 . C63 . H631 . 119.5 no C64 . C63 . H631 . 119.7 no C63 . C64 . C59 . 119.4(11) yes C63 . C64 . H641 . 118.8 no C59 . C64 . H641 . 121.8 no C62 . C65 . C66 . 110.2(10) yes C62 . C65 . C73 . 106.3(9) yes C66 . C65 . C73 . 109.1(9) yes C62 . C65 . C83 . 113.3(10) yes C66 . C65 . C83 . 107.3(9) yes C73 . C65 . C83 . 110.6(10) yes C65 . C66 . C67 . 117.1(10) yes C65 . C66 . C72 . 123.4(10) yes C67 . C66 . C72 . 119.2(11) yes C66 . C67 . C68 . 119.6(11) yes C66 . C67 . H671 . 120.3 no C68 . C67 . H671 . 120.1 no C67 . C68 . C69 . 122.3(12) yes C67 . C68 . H681 . 118.8 no C69 . C68 . H681 . 118.9 no C68 . C69 . C70 . 119.8(12) yes C68 . C69 . C71 . 118.1(11) yes C70 . C69 . C71 . 121.9(12) yes C69 . C70 . C141 . 109.0(13) yes C69 . C70 . C144 . 109.2(12) yes C141 . C70 . C144 . 103.2(15) yes C69 . C70 . C159 . 114.0(13) yes C141 . C70 . C159 . 112.4(14) yes C144 . C70 . C159 . 108.4(15) yes C69 . C71 . C72 . 118.4(11) yes C69 . C71 . H711 . 121.1 no C72 . C71 . H711 . 120.4 no C71 . C72 . C66 . 122.2(11) yes C71 . C72 . H721 . 118.3 no C66 . C72 . H721 . 119.4 no C65 . C73 . C74 . 124.8(10) yes C65 . C73 . C78 . 116.3(10) yes C74 . C73 . C78 . 118.9(11) yes C73 . C74 . C75 . 121.7(11) yes C73 . C74 . H741 . 119.3 no C75 . C74 . H741 . 118.9 no C74 . C75 . C76 . 121.5(11) yes C74 . C75 . H751 . 120.0 no C76 . C75 . H751 . 118.5 no C75 . C76 . C77 . 116.7(11) yes C75 . C76 . C79 . 122.6(11) yes C77 . C76 . C79 . 120.6(10) yes C76 . C77 . C78 . 122.2(11) yes C76 . C77 . H771 . 119.4 no C78 . C77 . H771 . 118.4 no C77 . C78 . C73 . 118.8(11) yes C77 . C78 . H781 . 120.1 no C73 . C78 . H781 . 121.0 no C76 . C79 . C80 . 107.8(9) yes C76 . C79 . C81 . 113.8(10) yes C80 . C79 . C81 . 111.0(11) yes C76 . C79 . C82 . 107.6(11) yes C80 . C79 . C82 . 108.7(10) yes C81 . C79 . C82 . 107.8(11) yes C79 . C80 . H802 . 110.1 no C79 . C80 . H801 . 110.1 no H802 . C80 . H801 . 109.5 no C79 . C80 . H803 . 109.1 no H802 . C80 . H803 . 109.1 no H801 . C80 . H803 . 108.8 no C79 . C81 . H812 . 110.7 no C79 . C81 . H811 . 108.1 no H812 . C81 . H811 . 109.6 no C79 . C81 . H813 . 109.6 no H812 . C81 . H813 . 109.0 no H811 . C81 . H813 . 109.9 no C79 . C82 . H821 . 108.6 no C79 . C82 . H822 . 111.5 no H821 . C82 . H822 . 108.6 no C79 . C82 . H823 . 110.1 no H821 . C82 . H823 . 108.8 no H822 . C82 . H823 . 109.2 no C65 . C83 . C84 . 121.9(11) yes C65 . C83 . C88 . 122.7(11) yes C84 . C83 . C88 . 115.2(11) yes C83 . C84 . C85 . 123.8(12) yes C83 . C84 . H841 . 116.4 no C85 . C84 . H841 . 119.8 no C84 . C85 . C86 . 121.2(12) yes C84 . C85 . H851 . 119.9 no C86 . C85 . H851 . 118.9 no C85 . C86 . C87 . 116.2(11) yes C85 . C86 . C128 . 123.5(12) yes C87 . C86 . C128 . 120.2(12) yes C86 . C87 . C88 . 121.9(12) yes C86 . C87 . H871 . 117.7 no C88 . C87 . H871 . 120.4 no C83 . C88 . C87 . 121.6(12) yes C83 . C88 . H881 . 119.5 no C87 . C88 . H881 . 118.9 no C128 . C127 . H1271 . 109.2 no C128 . C127 . H1272 . 106.8 no H1271 . C127 . H1272 . 109.9 no C128 . C127 . H1273 . 111.3 no H1271 . C127 . H1273 . 109.6 no H1272 . C127 . H1273 . 109.9 no C86 . C128 . C127 . 107.7(11) yes C86 . C128 . C129 . 111.5(13) yes C127 . C128 . C129 . 108.2(13) yes C86 . C128 . C130 . 113.3(12) yes C127 . C128 . C130 . 110.4(12) yes C129 . C128 . C130 . 105.7(13) yes C128 . C129 . H1291 . 111.8 no C128 . C129 . H1293 . 108.3 no H1291 . C129 . H1293 . 109.5 no C128 . C129 . H1292 . 108.8 no H1291 . C129 . H1292 . 109.2 no H1293 . C129 . H1292 . 109.2 no C128 . C130 . H1301 . 108.2 no C128 . C130 . H1302 . 108.1 no H1301 . C130 . H1302 . 110.6 no C128 . C130 . H1303 . 108.2 no H1301 . C130 . H1303 . 110.4 no H1302 . C130 . H1303 . 111.3 no C49 . C132 . H1321 . 118.7 no C49 . C132 . H1322 . 120.9 no H1321 . C132 . H1322 . 120.3 no C57 . C135 . H1351 . 107.3 no C57 . C135 . H1352 . 109.6 no H1351 . C135 . H1352 . 109.4 no C57 . C135 . H1353 . 112.3 no H1351 . C135 . H1353 . 109.0 no H1352 . C135 . H1353 . 109.2 no C70 . C141 . H1412 . 107.6 no C70 . C141 . H1411 . 104.3 no H1412 . C141 . H1411 . 111.8 no C70 . C141 . H1413 . 108.6 no H1412 . C141 . H1413 . 111.7 no H1411 . C141 . H1413 . 112.4 no C70 . C144 . H1442 . 112.5 no C70 . C144 . H1441 . 105.9 no H1442 . C144 . H1441 . 109.4 no C70 . C144 . H1443 . 109.9 no H1442 . C144 . H1443 . 109.5 no H1441 . C144 . H1443 . 109.5 no C70 . C159 . H1591 . 109.6 no C70 . C159 . H1592 . 108.9 no H1591 . C159 . H1592 . 109.3 no C70 . C159 . H1593 . 110.0 no H1591 . C159 . H1593 . 109.4 no H1592 . C159 . H1593 . 109.5 no H1602 . C160 . H1601 . 109.5 no H1602 . C160 . H1603 . 109.7 no H1601 . C160 . H1603 . 109.3 no H1602 . C160 . C7 . 109.2 no H1601 . C160 . C7 . 110.8 no H1603 . C160 . C7 . 108.2 no C57 . C174 . H1742 . 104.5 no C57 . C174 . H1741 . 110.0 no H1742 . C174 . H1741 . 109.8 no C57 . C174 . H1743 . 113.7 no H1742 . C174 . H1743 . 109.3 no H1741 . C174 . H1743 . 109.4 no C49 . C185 . H1851 . 110.4 no C49 . C185 . H1852 . 108.2 no H1851 . C185 . H1852 . 109.1 no C49 . C185 . H1853 . 110.0 no H1851 . C185 . H1853 . 109.5 no H1852 . C185 . H1853 . 109.6 no Cl56 . C187 . Cl91 . 112.8(12) yes Cl56 . C187 . H1872 . 108.0 no Cl91 . C187 . H1872 . 108.4 no Cl56 . C187 . H1871 . 108.0 no Cl91 . C187 . H1871 . 109.7 no H1872 . C187 . H1871 . 110.1 no C57 . C186 . H1861 . 105.1 no C57 . C186 . H1863 . 109.2 no H1861 . C186 . H1863 . 110.9 no C57 . C186 . H1862 . 109.5 no H1861 . C186 . H1862 . 110.7 no H1863 . C186 . H1862 . 111.2 no C304 . O303 . C302 . 115.1(12) yes C304 . C305 . H3051 . 109.4 no C304 . C305 . H3053 . 108.7 no H3051 . C305 . H3053 . 109.5 no C304 . C305 . H3052 . 110.3 no H3051 . C305 . H3052 . 109.5 no H3053 . C305 . H3052 . 109.5 no C305 . C304 . O303 . 107.4(12) yes C305 . C304 . H3042 . 111.1 no O303 . C304 . H3042 . 110.0 no C305 . C304 . H3041 . 109.5 no O303 . C304 . H3041 . 109.3 no H3042 . C304 . H3041 . 109.5 no O303 . C302 . C301 . 111.4(15) yes O303 . C302 . H3022 . 107.4 no C301 . C302 . H3022 . 110.0 no O303 . C302 . H3021 . 108.9 no C301 . C302 . H3021 . 109.6 no H3022 . C302 . H3021 . 109.5 no C302 . C301 . H3011 . 106.7 no C302 . C301 . H3012 . 110.6 no H3011 . C301 . H3012 . 109.5 no C302 . C301 . H3013 . 111.0 no H3011 . C301 . H3013 . 109.5 no H3012 . C301 . H3013 . 109.5 no C204 . C7 . C160 . 105.3(12) yes C204 . C7 . C207 . 110.4(12) yes C160 . C7 . C207 . 112.4(15) yes C204 . C7 . C41 . 113.4(13) yes C160 . C7 . C41 . 107.4(15) yes C207 . C7 . C41 . 108.0(14) yes H4011 . O401 . H4012 . 128.7 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 C17 . H171 . O43 2_545 143.2(5) 0.931 2.434 3.23(2) yes C20 . H201 . O401 2_545 133.8(6) 0.970 2.490 3.24(2) yes C40 . H401 . C28 . 140.0(5) 0.973 2.561 3.36(2) yes C40 . H402 . O401 . 142.0(9) 0.972 2.334 3.16(2) yes C192 . H1921 . O25 . 152.7(4) 0.930 2.429 3.28(2) yes C31 . H311 . C52 . 128.7(4) 0.933 2.369 3.04(2) yes C56 . H561 . C48 . 122.9(4) 0.925 2.507 3.11(2) yes C58 . H581 . O25 . 145.6(5) 0.962 2.417 3.26(2) yes C63 . H631 . C84 . 125.4(4) 0.934 2.534 3.17(2) yes C72 . H721 . C61 . 123.1(4) 0.934 2.520 3.13(2) yes C88 . H881 . C78 . 121.4(4) 0.923 2.474 3.06(2) yes C187 . H1872 . O19 2_455 156.0(6) 0.972 2.483 3.39(2) yes O401 . H4011 . O43 . 179.3(10) 0.850 1.990 2.84(2) yes O401 . H4012 . O7 2_445 177.2(10) 0.850 1.741 2.59(2) yes data_9Cl _database_code_depnum_ccdc_archive 'CCDC 911206' #TrackingRef 'White_Beer_OBC.cif' #============================================================================== # start Validation Reply Form _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Crystals were extremely small and weakly diffracting, and required the use of synchrotron radiation. Despite this, data could only be collected to a resolution of approximately 1.0 A. ; _vrf_PLAT022_I ; PROBLEM: Ratio Unique / Expected Reflections (too) Low .. 0.844 RESPONSE: Crystals were extremely small and weakly diffracting, and required the use of synchrotron radiation. Despite this, data could only be collected to a resolution of approximately 1.0 A. ; _vrf_PLAT023_I ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 38.31 Deg. RESPONSE: Crystals were extremely small and weakly diffracting, and required the use of synchrotron radiation. Despite this, data could only be collected to a resolution of approximately 1.0 A. ; _vrf_PLAT027_I ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 25.28 Deg. RESPONSE: Crystals were extremely small and weakly diffracting, and required the use of synchrotron radiation. Despite this, data could only be collected to a resolution of approximately 1.0 A. ; _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.939 RESPONSE: Crystals were extremely small and weakly diffracting, and required the use of synchrotron radiation. Despite this, data could only be collected to a resolution of approximately 1.0 A. ; # end Validation Reply Form # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.016 0.000 0.000 1751 330 ' ' 2 0.234 0.218 0.635 45 2 ' ' 3 0.395 0.643 0.227 10 0 ' ' 4 0.604 0.357 0.773 10 0 ' ' 5 0.765 0.781 0.365 45 4 ' ' _platon_squeeze_details ; ; _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; ? ; _cell_length_a 11.7586(5) _cell_length_b 23.4082(13) _cell_length_c 23.5471(12) _cell_angle_alpha 93.401(4) _cell_angle_beta 98.295(4) _cell_angle_gamma 92.975(4) _cell_volume 6390.2(6) _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 0.0100 0.0050 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' N 0.0170 0.0100 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0290 0.0190 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' Cl 0.2770 0.4370 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C120 H130 Cl1 N12 O15 # Dc = 1.05 Fooo = 1984.00 Mu = 0.90 M = 2015.88 # Found Formula = C116 H129 Cl1 N10 O10 # Dc = 0.97 FOOO = 1984.00 Mu = 0.82 M = 1858.81 _chemical_formula_sum 'C116 H129 Cl1 N10 O10' _chemical_formula_moiety 'C84 H94 N7, C32 H35 N3 O10, Cl' _chemical_compound_source synthesized _chemical_formula_weight 1858.81 _cell_measurement_reflns_used 3685 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 38.32 _cell_measurement_temperature 100 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 0.966 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.082 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Oxford Diffraction, 2011)' _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 1.00 _diffrn_measurement_device_type synchrotron _diffrn_measurement_device Area _diffrn_radiation_monochromator synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 1.19490 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'CrystalClear, (Rigaku, 1997--2002)' _computing_cell_refinement 'CrysAlisPro, (Oxford Diffraction, 2011)' _computing_data_reduction 'CrysAlisPro, (Oxford Diffraction, 2011)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 26680 _reflns_number_total 12622 _diffrn_reflns_av_R_equivalents 0.089 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 12622 # Theoretical number of reflections is about 24847 _diffrn_reflns_theta_min 1.468 _diffrn_reflns_theta_max 38.306 _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 25.282 _diffrn_measured_fraction_theta_full 0.939 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -24 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 3.18 _oxford_diffrn_Wilson_scale 0.28 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.49 _refine_diff_density_max 0.44 # 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 11194 _refine_ls_number_restraints 107 _refine_ls_number_parameters 1261 _oxford_refine_ls_R_factor_ref 0.1102 _refine_ls_wR_factor_ref 0.2640 _refine_ls_goodness_of_fit_ref 1.0041 _refine_ls_shift/su_max 0.0001628 _refine_ls_shift/su_mean 0.0000126 # The values computed with all filters except I/sigma _oxford_reflns_number_all 11194 _refine_ls_R_factor_all 0.1102 _refine_ls_wR_factor_all 0.2640 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6808 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_gt 0.1947 # 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 #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: 0.329E+04 0.545E+04 0.330E+04 0.132E+04 271. ; # Insert your own references if required - in alphabetical order loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens O101 O 0.3614(7) 0.2306(4) 0.8742(3) 0.1278 1.0000 Uani . . . . . . O102 O 0.5011(8) 0.2660(3) 0.8334(3) 0.1281 1.0000 Uani . . . . . . N103 N 0.3999(10) 0.2590(4) 0.8378(4) 0.1047 1.0000 Uani . . . . . . C104 C 0.3130(10) 0.2828(4) 0.7945(4) 0.0858 1.0000 Uani . . . . . . C105 C 0.3541(7) 0.3110(4) 0.7525(4) 0.0814 1.0000 Uani . . . . . . C106 C 0.2819(8) 0.3355(4) 0.7096(4) 0.0789 1.0000 Uani . . . . . . C107 C 0.1612(8) 0.3295(3) 0.7142(3) 0.0698 1.0000 Uani . . . . . . C108 C 0.1214(7) 0.2999(3) 0.7578(3) 0.0671 1.0000 Uani . . . . . . C109 C 0.1991(9) 0.2768(4) 0.7983(3) 0.0854 1.0000 Uani . . . . . . O110 O 0.4304(6) 0.3774(4) 0.6670(3) 0.1243 1.0000 Uani . . . . . . C111 C 0.3252(9) 0.3644(4) 0.6625(4) 0.0865 1.0000 Uani . . . . . . N112 N 0.2511(6) 0.3729(3) 0.6159(3) 0.0845 1.0000 Uani D . . . . . C113 C 0.2931(8) 0.3881(6) 0.5641(4) 0.1359 1.0000 Uani D . . . . . C114 C 0.2025(8) 0.4096(6) 0.5229(4) 0.1377 1.0000 Uani D . . . . . O115 O 0.2375(5) 0.4118(3) 0.4671(2) 0.1017 1.0000 Uani D . . . . . C116 C 0.1487(8) 0.4278(4) 0.4262(4) 0.0779 1.0000 Uani . . . . . . C117 C 0.1563(8) 0.4097(3) 0.3694(4) 0.0832 1.0000 Uani . . . . . . C118 C 0.0695(8) 0.4221(4) 0.3257(4) 0.0793 1.0000 Uani . . . . . . C119 C -0.0181(7) 0.4533(3) 0.3375(3) 0.0741 1.0000 Uani . . . . . . C120 C -0.0208(7) 0.4737(3) 0.3933(3) 0.0741 1.0000 Uani . . . . . . C121 C 0.0621(8) 0.4602(4) 0.4378(3) 0.0816 1.0000 Uani . . . . . . O122 O -0.1102(4) 0.4671(2) 0.2981(2) 0.0765 1.0000 Uani D . . . . . C123 C -0.1113(7) 0.4499(3) 0.2379(3) 0.0860 1.0000 Uani D . . . . . C124 C -0.1597(7) 0.3884(3) 0.2236(3) 0.0805 1.0000 Uani D . . . . . O125 O -0.2775(5) 0.3859(2) 0.2331(2) 0.0814 1.0000 Uani D . . . . . C126 C -0.3359(7) 0.3307(3) 0.2159(4) 0.1007 1.0000 Uani D . . . . . C127 C -0.4435(8) 0.3290(4) 0.2449(4) 0.0986 1.0000 Uani D . . . . . C128 C -0.5459(9) 0.3391(5) 0.2177(3) 0.1082 1.0000 Uani D . . . . . C129 C -0.6522(8) 0.3445(5) 0.2476(3) 0.1248 1.0000 Uani D . . . . . O130 O -0.6236(5) 0.3445(3) 0.3095(2) 0.1003 1.0000 Uani D . . . . . C131 C -0.6498(7) 0.2906(3) 0.3313(3) 0.0973 1.0000 Uani D . . . . . C132 C -0.6094(6) 0.2956(4) 0.3958(3) 0.0789 1.0000 Uani D . . . . . O133 O -0.4886(4) 0.2888(2) 0.4053(2) 0.0729 1.0000 Uani D . . . . . C134 C -0.4416(7) 0.2830(3) 0.4632(3) 0.0672 1.0000 Uani . . . . . . C135 C -0.4790(7) 0.3097(3) 0.5081(4) 0.0710 1.0000 Uani . . . . . . C136 C -0.4249(7) 0.3048(3) 0.5651(3) 0.0741 1.0000 Uani . . . . . . C137 C -0.3285(7) 0.2740(3) 0.5727(3) 0.0665 1.0000 Uani . . . . . . C138 C -0.2901(7) 0.2460(3) 0.5267(3) 0.0721 1.0000 Uani . . . . . . C139 C -0.3438(6) 0.2512(3) 0.4702(3) 0.0656 1.0000 Uani . . . . . . O140 O -0.2690(4) 0.2639(2) 0.6271(2) 0.0721 1.0000 Uani D . . . . . C141 C -0.2877(7) 0.3014(3) 0.6740(3) 0.0794 1.0000 Uani D . . . . . C142 C -0.2038(7) 0.2870(3) 0.7263(3) 0.0809 1.0000 Uani D . . . . . N143 N -0.0834(5) 0.2978(2) 0.7191(3) 0.0681 1.0000 Uani D . . . . . C144 C -0.0036(8) 0.2919(3) 0.7650(4) 0.0741 1.0000 Uani . . . . . . O145 O -0.0285(5) 0.2801(3) 0.8122(3) 0.0962 1.0000 Uani . . . . . . Cl1 Cl -0.01947(15) 0.33370(8) 0.58699(7) 0.0661 1.0000 Uani . . . . . . N51 N 0.0123(5) 0.2700(2) 0.4038(2) 0.0509 1.0000 Uani . . . . . . N52 N -0.0221(5) 0.2794(2) 0.3467(2) 0.0565 1.0000 Uani . . . . . . N53 N -0.1058(5) 0.3143(3) 0.3458(2) 0.0609 1.0000 Uani . . . . . . C54 C -0.1244(6) 0.3283(3) 0.4010(3) 0.0546 1.0000 Uani . . . . . . C55 C -0.0473(6) 0.3003(3) 0.4369(3) 0.0572 1.0000 Uani . . . . . . C56 C -0.2105(6) 0.3681(3) 0.4135(3) 0.0617 1.0000 Uani . . . . . . C57 C -0.2241(6) 0.3830(3) 0.4692(3) 0.0540 1.0000 Uani . . . . . . C58 C -0.3049(6) 0.4221(3) 0.4808(3) 0.0534 1.0000 Uani . . . . . . C59 C -0.3706(6) 0.4451(3) 0.4358(3) 0.0627 1.0000 Uani . . . . . . N60 N -0.3526(5) 0.4313(3) 0.3818(2) 0.0721 1.0000 Uani . . . . . . C61 C -0.2769(7) 0.3941(3) 0.3701(3) 0.0665 1.0000 Uani . . . . . . C62 C -0.4214(8) 0.4586(4) 0.3317(3) 0.0902 1.0000 Uani . . . . . . C63 C -0.3179(7) 0.4397(3) 0.5412(3) 0.0586 1.0000 Uani . . . . . . N64 N -0.4016(5) 0.4710(3) 0.5574(2) 0.0591 1.0000 Uani . . . . . . N65 N -0.3856(5) 0.4792(3) 0.6142(2) 0.0641 1.0000 Uani . . . . . . N66 N -0.2866(5) 0.4535(2) 0.6332(2) 0.0521 1.0000 Uani . . . . . . C67 C -0.2426(6) 0.4279(3) 0.5899(3) 0.0587 1.0000 Uani . . . . . . C68 C -0.2424(6) 0.4547(3) 0.6936(3) 0.0545 1.0000 Uani . . . . . . C69 C -0.1294(6) 0.4405(3) 0.7090(3) 0.0547 1.0000 Uani . . . . . . C70 C -0.0837(6) 0.4435(3) 0.7667(3) 0.0567 1.0000 Uani . . . . . . C71 C -0.1466(6) 0.4624(3) 0.8084(3) 0.0575 1.0000 Uani . . . . . . C72 C -0.0971(6) 0.4692(3) 0.8750(3) 0.0590 1.0000 Uani . . . . . . C73 C 0.0372(6) 0.4728(3) 0.8823(3) 0.0570 1.0000 Uani . . . . . . C74 C 0.0939(7) 0.4243(3) 0.8693(3) 0.0597 1.0000 Uani . . . . . . C75 C 0.2115(7) 0.4265(3) 0.8692(3) 0.0603 1.0000 Uani . . . . . . C76 C 0.2795(7) 0.4781(4) 0.8851(3) 0.0670 1.0000 Uani . . . . . . C77 C 0.4078(7) 0.4813(4) 0.8792(3) 0.0788 1.0000 Uani . . . . . . C78 C 0.4704(8) 0.4360(4) 0.9124(4) 0.1039 1.0000 Uani . . . . . . C79 C 0.4642(7) 0.5404(4) 0.8991(4) 0.0937 1.0000 Uani . . . . . . C80 C 0.4170(8) 0.4700(5) 0.8148(3) 0.1066 1.0000 Uani . . . . . . C81 C 0.2227(7) 0.5248(3) 0.9029(3) 0.0608 1.0000 Uani . . . . . . C82 C 0.1042(7) 0.5228(3) 0.9014(2) 0.0571 1.0000 Uani . . . . . . C83 C -0.1416(6) 0.5253(3) 0.9002(3) 0.0633 1.0000 Uani . . . . . . C84 C -0.1910(6) 0.5294(3) 0.9503(3) 0.0626 1.0000 Uani . . . . . . C85 C -0.2252(6) 0.5816(4) 0.9720(3) 0.0677 1.0000 Uani . . . . . . C86 C -0.2113(6) 0.6326(3) 0.9433(3) 0.0655 1.0000 Uani . . . . . . C87 C -0.2489(7) 0.6886(3) 0.9693(3) 0.0723 1.0000 Uani . . . . . . C88 C -0.2231(9) 0.7397(4) 0.9336(4) 0.0978 1.0000 Uani . . . . . . C89 C -0.1789(8) 0.7034(4) 1.0296(4) 0.0963 1.0000 Uani . . . . . . C90 C -0.3755(8) 0.6853(4) 0.9731(4) 0.0998 1.0000 Uani . . . . . . C91 C -0.1648(6) 0.6277(4) 0.8929(3) 0.0687 1.0000 Uani . . . . . . C92 C -0.1314(6) 0.5753(4) 0.8715(3) 0.0650 1.0000 Uani . . . . . . C93 C -0.1376(6) 0.4174(3) 0.9052(3) 0.0594 1.0000 Uani . . . . . . C94 C -0.2295(6) 0.3780(3) 0.8831(3) 0.0635 1.0000 Uani . . . . . . C95 C -0.2622(7) 0.3321(3) 0.9123(3) 0.0680 1.0000 Uani . U . . . . C96 C -0.2065(6) 0.3220(3) 0.9677(3) 0.0659 1.0000 Uani . U . . . . C97 C -0.1135(7) 0.3607(4) 0.9891(3) 0.0694 1.0000 Uani . U . . . . C98 C -0.0802(6) 0.4062(3) 0.9599(3) 0.0661 1.0000 Uani . . . . . . C201 C -0.2411(6) 0.2725(3) 1.0012(3) 0.0746 1.0000 Uani D U . . . . C202 C -0.1392(9) 0.2366(5) 1.0180(6) 0.1027 0.7500 Uani D U . . 1 . C204 C -0.3393(10) 0.2333(5) 0.9689(5) 0.1095 0.7500 Uani D U . . 1 . C102 C -0.2616(6) 0.4758(3) 0.7917(3) 0.0687 1.0000 Uani . . . . . . C103 C -0.3084(6) 0.4714(3) 0.7339(3) 0.0644 1.0000 Uani . . . . . . C145 C 0.1015(6) 0.2319(3) 0.4184(3) 0.0535 1.0000 Uani . . . . . . C146 C 0.1539(6) 0.2324(3) 0.4749(3) 0.0620 1.0000 Uani . . . . . . C147 C 0.2371(6) 0.1922(3) 0.4891(3) 0.0566 1.0000 Uani . . . . . . C148 C 0.2629(6) 0.1513(3) 0.4500(3) 0.0550 1.0000 Uani . . . . . . C149 C 0.3450(6) 0.1034(3) 0.4656(3) 0.0551 1.0000 Uani . . . . . . C150 C 0.2737(7) 0.0456(3) 0.4442(3) 0.0606 1.0000 Uani . . . . . . C110 C 0.3165(7) 0.0010(3) 0.4155(3) 0.0664 1.0000 Uani . . . . . . C151 C 0.2477(8) -0.0493(3) 0.3955(3) 0.0688 1.0000 Uani . . . . . . C112 C 0.1332(7) -0.0556(3) 0.4043(3) 0.0591 1.0000 Uani . . . . . . C152 C 0.0935(6) -0.0113(3) 0.4353(3) 0.0600 1.0000 Uani . . . . . . C153 C 0.1611(7) 0.0383(3) 0.4540(3) 0.0647 1.0000 Uani . . . . . . C115 C 0.0558(7) -0.1089(3) 0.3825(4) 0.0740 1.0000 Uani . . . . . . C154 C 0.0301(9) -0.1414(4) 0.4339(5) 0.1045 1.0000 Uani . . . . . . C155 C 0.1099(8) -0.1500(4) 0.3429(4) 0.0890 1.0000 Uani . . . . . . C156 C -0.0592(7) -0.0911(4) 0.3488(5) 0.1013 1.0000 Uani . . . . . . C157 C 0.4527(6) 0.1081(3) 0.4366(3) 0.0554 1.0000 Uani . . . . . . C158 C 0.5555(8) 0.0830(3) 0.4586(4) 0.0730 1.0000 Uani . . . . . . C159 C 0.6521(8) 0.0847(3) 0.4331(4) 0.0713 1.0000 Uani . . . . . . C122 C 0.6562(6) 0.1091(3) 0.3816(4) 0.0679 1.0000 Uani . . . . . . C160 C 0.5566(8) 0.1357(3) 0.3599(4) 0.0749 1.0000 Uani . . . . . . C161 C 0.4606(7) 0.1358(3) 0.3859(3) 0.0693 1.0000 Uani . . . . . . C125 C 0.7618(7) 0.1095(3) 0.3513(4) 0.0804 1.0000 Uani . . . . . . C162 C 0.7320(9) 0.0754(5) 0.2915(5) 0.1214 1.0000 Uani . . . . . . C163 C 0.7968(9) 0.1692(4) 0.3371(5) 0.1191 1.0000 Uani . . . . . . C164 C 0.8628(9) 0.0822(6) 0.3817(6) 0.1440 1.0000 Uani . . . . . . C165 C 0.3829(6) 0.1054(3) 0.5316(3) 0.0552 1.0000 Uani . . . . . . C130 C 0.4621(6) 0.1505(3) 0.5584(3) 0.0622 1.0000 Uani . . . . . . C166 C 0.4969(6) 0.1534(3) 0.6168(3) 0.0660 1.0000 Uani . . . . . . C167 C 0.4599(7) 0.1143(3) 0.6520(3) 0.0683 1.0000 Uani . . . . . . C133 C 0.4944(8) 0.1158(4) 0.7183(3) 0.0783 1.0000 Uani . . . . . . C168 C 0.3887(8) 0.1236(4) 0.7476(4) 0.0948 1.0000 Uani . . . . . . C169 C 0.5507(8) 0.0607(4) 0.7349(4) 0.0963 1.0000 Uani . . . . . . C170 C 0.5835(8) 0.1664(4) 0.7386(3) 0.0960 1.0000 Uani . . . . . . C171 C 0.3820(7) 0.0694(3) 0.6255(3) 0.0731 1.0000 Uani . . . . . . C172 C 0.3453(7) 0.0658(3) 0.5664(3) 0.0687 1.0000 Uani . . . . . . C173 C 0.2041(6) 0.1516(3) 0.3936(3) 0.0654 1.0000 Uani . . . . . . C140 C 0.1238(6) 0.1905(3) 0.3786(3) 0.0592 1.0000 Uani . . . . . . C203 C -0.2797(12) 0.2975(5) 1.0563(4) 0.1089 0.7500 Uani D U . . 1 . H1051 H 0.4324 0.3154 0.7513 0.0990 1.0000 Uiso R . . . . . H1071 H 0.1069 0.3473 0.6857 0.0849 1.0000 Uiso R . . . . . H1091 H 0.1761 0.2573 0.8295 0.1180 1.0000 Uiso R . . . . . H1132 H 0.3611 0.4158 0.5738 0.1652 1.0000 Uiso R . . . . . H1131 H 0.3147 0.3535 0.5435 0.1655 1.0000 Uiso R . . . . . H1141 H 0.1871 0.4471 0.5390 0.1674 1.0000 Uiso R . . . . . H1142 H 0.1366 0.3831 0.5209 0.1672 1.0000 Uiso R . . . . . H1171 H 0.2184 0.3873 0.3625 0.1107 1.0000 Uiso R . . . . . H1181 H 0.0735 0.4095 0.2868 0.1046 1.0000 Uiso R . . . . . H1201 H -0.0827 0.4965 0.4022 0.1045 1.0000 Uiso R . . . . . H1211 H 0.0618 0.4745 0.4754 0.1109 1.0000 Uiso R . . . . . H1231 H -0.1631 0.4743 0.2165 0.1185 1.0000 Uiso R . . . . . H1232 H -0.0306 0.4534 0.2290 0.1182 1.0000 Uiso R . . . . . H1242 H -0.1145 0.3628 0.2476 0.0953 1.0000 Uiso R . . . . . H1241 H -0.1580 0.3768 0.1835 0.0950 1.0000 Uiso R . . . . . H1261 H -0.3576 0.3263 0.1729 0.1233 1.0000 Uiso R . . . . . H1262 H -0.2902 0.2989 0.2290 0.1232 1.0000 Uiso R . . . . . H1271 H -0.4389 0.3194 0.2833 0.1457 1.0000 Uiso R . . . . . H1281 H -0.5540 0.3461 0.1779 0.1380 1.0000 Uiso R . . . . . H1291 H -0.6863 0.3805 0.2400 0.1562 1.0000 Uiso R . . . . . H1292 H -0.7068 0.3131 0.2316 0.1564 1.0000 Uiso R . . . . . H1312 H -0.7351 0.2812 0.3262 0.1311 1.0000 Uiso R . . . . . H1311 H -0.6081 0.2595 0.3146 0.1312 1.0000 Uiso R . . . . . H1321 H -0.6229 0.3349 0.4102 0.1053 1.0000 Uiso R . . . . . H1322 H -0.6543 0.2671 0.4142 0.1061 1.0000 Uiso R . . . . . H1351 H -0.5425 0.3331 0.5026 0.0914 1.0000 Uiso R . . . . . H1361 H -0.4561 0.3230 0.5948 0.0999 1.0000 Uiso R . . . . . H1381 H -0.2253 0.2234 0.5330 0.0913 1.0000 Uiso R . . . . . H1391 H -0.3134 0.2349 0.4375 0.0818 1.0000 Uiso R . . . . . H1411 H -0.3677 0.2968 0.6815 0.1015 1.0000 Uiso R . . . . . H1412 H -0.2708 0.3418 0.6681 0.1016 1.0000 Uiso R . . . . . H1421 H -0.2169 0.3116 0.7588 0.1063 1.0000 Uiso R . . . . . H1422 H -0.2153 0.2468 0.7326 0.1066 1.0000 Uiso R . . . . . H551 H -0.0386 0.3032 0.4769 0.0711 1.0000 Uiso R . . . . . H571 H -0.1790 0.3673 0.4982 0.0648 1.0000 Uiso R . . . . . H591 H -0.4270 0.4702 0.4436 0.0885 1.0000 Uiso R . . . . . H611 H -0.2701 0.3840 0.3306 0.0846 1.0000 Uiso R . . . . . H622 H -0.3739 0.4664 0.3037 0.1495 1.0000 Uiso R . . . . . H621 H -0.4497 0.4931 0.3477 0.1489 1.0000 Uiso R . . . . . H623 H -0.4837 0.4308 0.3172 0.1488 1.0000 Uiso R . . . . . H671 H -0.1757 0.4060 0.5939 0.0710 1.0000 Uiso R . . . . . H691 H -0.0835 0.4294 0.6790 0.0723 1.0000 Uiso R . . . . . H701 H -0.0088 0.4315 0.7784 0.0784 1.0000 Uiso R . . . . . H741 H 0.0525 0.3900 0.8612 0.0794 1.0000 Uiso R . . . . . H751 H 0.2469 0.3949 0.8566 0.0771 1.0000 Uiso R . . . . . H781 H 0.5535 0.4393 0.9078 0.1587 1.0000 Uiso R . . . . . H782 H 0.4581 0.4415 0.9524 0.1596 1.0000 Uiso R . . . . . H783 H 0.4341 0.3996 0.8942 0.1590 1.0000 Uiso R . . . . . H791 H 0.5451 0.5396 0.8990 0.1631 1.0000 Uiso R . . . . . H793 H 0.4512 0.5498 0.9389 0.1630 1.0000 Uiso R . . . . . H792 H 0.4355 0.5694 0.8734 0.1631 1.0000 Uiso R . . . . . H801 H 0.4980 0.4699 0.8064 0.1693 1.0000 Uiso R . . . . . H803 H 0.3791 0.5008 0.7933 0.1692 1.0000 Uiso R . . . . . H802 H 0.3755 0.4329 0.8016 0.1694 1.0000 Uiso R . . . . . H811 H 0.2644 0.5593 0.9172 0.0785 1.0000 Uiso R . . . . . H821 H 0.0692 0.5563 0.9129 0.0710 1.0000 Uiso R . . . . . H841 H -0.1977 0.4978 0.9703 0.0828 1.0000 Uiso R . . . . . H851 H -0.2579 0.5830 1.0053 0.0875 1.0000 Uiso R . . . . . H881 H -0.2348 0.7735 0.9571 0.1610 1.0000 Uiso R . . . . . H883 H -0.1425 0.7387 0.9269 0.1615 1.0000 Uiso R . . . . . H882 H -0.2778 0.7355 0.8984 0.1614 1.0000 Uiso R . . . . . H891 H -0.2122 0.7357 1.0480 0.1466 1.0000 Uiso R . . . . . H892 H -0.1853 0.6709 1.0538 0.1459 1.0000 Uiso R . . . . . H893 H -0.0987 0.7123 1.0235 0.1466 1.0000 Uiso R . . . . . H901 H -0.3936 0.7246 0.9848 0.1568 1.0000 Uiso R . . . . . H902 H -0.3940 0.6572 1.0018 0.1563 1.0000 Uiso R . . . . . H903 H -0.4151 0.6740 0.9335 0.1566 1.0000 Uiso R . . . . . H911 H -0.1554 0.6598 0.8732 0.0909 1.0000 Uiso R . . . . . H921 H -0.0990 0.5740 0.8378 0.0834 1.0000 Uiso R . . . . . H941 H -0.2702 0.3822 0.8468 0.0811 1.0000 Uiso R . . . . . H951 H -0.3239 0.3071 0.8957 0.0884 1.0000 Uiso R . . . . . H971 H -0.0697 0.3559 1.0262 0.0788 1.0000 Uiso R . . . . . H981 H -0.0200 0.4314 0.9753 0.0839 1.0000 Uiso R . . . . . H1021 H -0.3053 0.4879 0.8201 0.0919 1.0000 Uiso R . . . . . H1031 H -0.3865 0.4802 0.7225 0.0833 1.0000 Uiso R . . . . . H1461 H 0.1323 0.2599 0.5009 0.0757 1.0000 Uiso R . . . . . H1471 H 0.2755 0.1931 0.5286 0.0693 1.0000 Uiso R . . . . . H1101 H 0.3932 0.0044 0.4075 0.0852 1.0000 Uiso R . . . . . H1511 H 0.2770 -0.0801 0.3774 0.0842 1.0000 Uiso R . . . . . H1521 H 0.0196 -0.0151 0.4430 0.0859 1.0000 Uiso R . . . . . H1531 H 0.1295 0.0679 0.4742 0.0868 1.0000 Uiso R . . . . . H1541 H 0.0207 -0.1832 0.4248 0.1553 1.0000 Uiso R . . . . . H1543 H 0.0896 -0.1355 0.4673 0.1551 1.0000 Uiso R . . . . . H1542 H -0.0407 -0.1292 0.4475 0.1555 1.0000 Uiso R . . . . . H1551 H 0.0547 -0.1817 0.3289 0.1316 1.0000 Uiso R . . . . . H1553 H 0.1780 -0.1651 0.3631 0.1322 1.0000 Uiso R . . . . . H1552 H 0.1307 -0.1298 0.3106 0.1326 1.0000 Uiso R . . . . . H1561 H -0.1101 -0.1258 0.3361 0.1631 1.0000 Uiso R . . . . . H1562 H -0.0945 -0.0655 0.3748 0.1628 1.0000 Uiso R . . . . . H1563 H -0.0390 -0.0707 0.3156 0.1635 1.0000 Uiso R . . . . . H1581 H 0.5559 0.0630 0.4933 0.0871 1.0000 Uiso R . . . . . H1591 H 0.7165 0.0681 0.4501 0.0955 1.0000 Uiso R . . . . . H1601 H 0.5561 0.1552 0.3250 0.0923 1.0000 Uiso R . . . . . H1611 H 0.3935 0.1536 0.3702 0.0883 1.0000 Uiso R . . . . . H1622 H 0.7984 0.0771 0.2730 0.1810 1.0000 Uiso R . . . . . H1621 H 0.7080 0.0364 0.2971 0.1814 1.0000 Uiso R . . . . . H1623 H 0.6698 0.0931 0.2705 0.1811 1.0000 Uiso R . . . . . H1631 H 0.8617 0.1660 0.3176 0.1895 1.0000 Uiso R . . . . . H1633 H 0.8136 0.1917 0.3734 0.1892 1.0000 Uiso R . . . . . H1632 H 0.7317 0.1830 0.3137 0.1893 1.0000 Uiso R . . . . . H1641 H 0.9185 0.0802 0.3544 0.2242 1.0000 Uiso R . . . . . H1643 H 0.8913 0.1088 0.4155 0.2242 1.0000 Uiso R . . . . . H1642 H 0.8383 0.0437 0.3929 0.2240 1.0000 Uiso R . . . . . H1301 H 0.4902 0.1776 0.5357 0.0811 1.0000 Uiso R . . . . . H1661 H 0.5489 0.1845 0.6329 0.0837 1.0000 Uiso R . . . . . H1681 H 0.4031 0.1221 0.7899 0.1523 1.0000 Uiso R . . . . . H1683 H 0.3535 0.1596 0.7371 0.1522 1.0000 Uiso R . . . . . H1682 H 0.3310 0.0920 0.7330 0.1523 1.0000 Uiso R . . . . . H1691 H 0.5773 0.0625 0.7759 0.1579 1.0000 Uiso R . . . . . H1693 H 0.6131 0.0592 0.7131 0.1579 1.0000 Uiso R . . . . . H1692 H 0.4977 0.0287 0.7234 0.1584 1.0000 Uiso R . . . . . H1701 H 0.6060 0.1665 0.7789 0.1490 1.0000 Uiso R . . . . . H1702 H 0.6495 0.1605 0.7200 0.1494 1.0000 Uiso R . . . . . H1703 H 0.5481 0.2017 0.7305 0.1493 1.0000 Uiso R . . . . . H1711 H 0.3519 0.0416 0.6478 0.0893 1.0000 Uiso R . . . . . H1721 H 0.2915 0.0357 0.5495 0.0812 1.0000 Uiso R . . . . . H1731 H 0.2226 0.1230 0.3667 0.0794 1.0000 Uiso R . . . . . H1401 H 0.0834 0.1887 0.3402 0.0741 1.0000 Uiso R . . . . . H1431 H -0.0641 0.3082 0.6854 0.0918 1.0000 Uiso R . . . . . H1121 H 0.1746 0.3694 0.6161 0.1109 1.0000 Uiso R . . . . . C302 C -0.166(2) 0.2717(14) 1.0593(8) 0.1120 0.2500 Uani D U . . 2 . C303 C -0.3658(12) 0.2775(15) 1.0096(13) 0.1029 0.2500 Uani D U . . 2 . C304 C -0.230(3) 0.2174(9) 0.9651(12) 0.0935 0.2500 Uani D U . . 2 . H2021 H -0.1630 0.2056 1.0388 0.1340 0.7500 Uiso R . . . 1 . H2022 H -0.0799 0.2597 1.0416 0.1340 0.7500 Uiso R . . . 1 . H2023 H -0.1110 0.2219 0.9846 0.1340 0.7500 Uiso R . . . 1 . H2041 H -0.3573 0.2033 0.9922 0.1437 0.7500 Uiso R . . . 1 . H2042 H -0.4048 0.2551 0.9600 0.1437 0.7500 Uiso R . . . 1 . H2043 H -0.3176 0.2174 0.9342 0.1437 0.7500 Uiso R . . . 1 . H2031 H -0.3030 0.2671 1.0779 0.1358 0.7500 Uiso R . . . 1 . H2032 H -0.2172 0.3198 1.0784 0.1358 0.7500 Uiso R . . . 1 . H2033 H -0.3423 0.3209 1.0470 0.1358 0.7500 Uiso R . . . 1 . H3021 H -0.1886 0.2406 1.0802 0.1329 0.2500 Uiso R . . . 2 . H3022 H -0.1690 0.3068 1.0814 0.1329 0.2500 Uiso R . . . 2 . H3023 H -0.0896 0.2676 1.0515 0.1329 0.2500 Uiso R . . . 2 . H3031 H -0.3886 0.2464 1.0304 0.1279 0.2500 Uiso R . . . 2 . H3032 H -0.3702 0.3125 1.0314 0.1279 0.2500 Uiso R . . . 2 . H3033 H -0.4154 0.2773 0.9739 0.1279 0.2500 Uiso R . . . 2 . H3041 H -0.2525 0.1853 0.9847 0.1371 0.2500 Uiso R . . . 2 . H3042 H -0.1535 0.2141 0.9575 0.1371 0.2500 Uiso R . . . 2 . H3043 H -0.2804 0.2185 0.9299 0.1371 0.2500 Uiso R . . . 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 O101 0.120(7) 0.169(7) 0.088(5) 0.019(5) -0.029(5) 0.057(5) O102 0.088(6) 0.152(6) 0.123(6) -0.007(4) -0.058(5) 0.024(5) N103 0.096(8) 0.134(7) 0.072(6) -0.001(5) -0.035(6) 0.032(6) C104 0.096(9) 0.093(6) 0.056(6) -0.006(5) -0.036(6) 0.029(6) C105 0.056(6) 0.107(6) 0.069(6) -0.015(5) -0.029(5) 0.018(5) C106 0.064(7) 0.098(6) 0.066(6) -0.012(5) -0.018(5) 0.023(5) C107 0.074(7) 0.084(5) 0.044(4) -0.006(4) -0.014(4) 0.008(4) C108 0.052(6) 0.084(5) 0.058(5) 0.002(4) -0.022(4) 0.011(4) C109 0.078(8) 0.105(7) 0.060(5) -0.013(4) -0.028(5) 0.021(5) O110 0.064(5) 0.220(8) 0.074(4) -0.003(4) -0.026(4) -0.016(5) C111 0.074(8) 0.120(7) 0.053(6) -0.010(5) -0.024(6) -0.006(5) N112 0.049(4) 0.147(6) 0.057(4) 0.017(4) 0.001(4) 0.005(4) C113 0.065(7) 0.259(15) 0.077(7) 0.028(8) -0.008(6) -0.018(8) C114 0.111(9) 0.209(13) 0.086(7) 0.088(8) -0.032(7) -0.023(8) O115 0.103(5) 0.116(5) 0.077(4) 0.024(3) -0.023(4) 0.006(4) C116 0.072(6) 0.085(6) 0.067(6) 0.020(5) -0.028(5) 0.003(5) C117 0.084(7) 0.079(5) 0.079(6) 0.006(5) -0.010(5) -0.003(4) C118 0.073(6) 0.092(6) 0.069(5) 0.019(4) -0.013(5) 0.019(5) C119 0.068(6) 0.082(5) 0.065(6) 0.017(4) -0.023(5) 0.013(5) C120 0.078(6) 0.085(5) 0.054(5) 0.010(4) -0.010(4) 0.002(4) C121 0.093(7) 0.083(6) 0.063(5) 0.014(4) -0.012(5) 0.007(5) O122 0.070(4) 0.091(4) 0.063(3) 0.006(3) -0.010(3) 0.007(3) C123 0.102(7) 0.096(6) 0.051(5) -0.001(4) -0.017(4) 0.011(5) C124 0.078(7) 0.115(7) 0.043(4) 0.000(4) -0.006(4) 0.007(5) O125 0.077(5) 0.109(4) 0.052(3) 0.007(3) -0.010(3) -0.001(3) C126 0.104(9) 0.122(8) 0.067(6) -0.006(5) -0.007(6) -0.009(6) C127 0.079(8) 0.117(7) 0.094(7) 0.011(5) -0.005(7) 0.002(6) C128 0.084(8) 0.158(10) 0.077(6) 0.016(6) -0.003(6) -0.015(7) C129 0.107(9) 0.184(11) 0.073(7) 0.036(7) -0.028(6) -0.011(8) O130 0.095(5) 0.132(5) 0.070(4) 0.028(4) -0.010(3) 0.005(4) C131 0.078(7) 0.118(7) 0.088(6) 0.033(6) -0.026(5) 0.007(5) C132 0.055(6) 0.108(6) 0.072(5) 0.030(5) -0.006(4) 0.005(4) O133 0.058(4) 0.097(4) 0.060(3) 0.011(3) -0.011(3) 0.013(3) C134 0.055(6) 0.069(5) 0.072(6) 0.007(4) -0.009(4) 0.006(4) C135 0.052(5) 0.079(5) 0.077(6) 0.002(4) -0.009(5) 0.015(4) C136 0.058(6) 0.080(5) 0.076(6) 0.001(4) -0.019(4) 0.015(4) C137 0.053(5) 0.064(5) 0.074(6) 0.018(4) -0.024(4) -0.006(4) C138 0.072(6) 0.068(5) 0.071(6) 0.003(4) -0.011(5) 0.012(4) C139 0.050(5) 0.077(5) 0.066(5) 0.014(4) -0.009(4) 0.004(4) O140 0.064(4) 0.078(3) 0.067(3) 0.002(3) -0.015(3) 0.004(3) C141 0.076(6) 0.072(5) 0.081(6) 0.007(5) -0.017(5) 0.000(4) C142 0.074(7) 0.077(5) 0.080(6) 0.005(4) -0.025(5) -0.005(4) N143 0.052(5) 0.077(4) 0.068(4) 0.008(3) -0.016(4) -0.001(3) C144 0.078(8) 0.078(5) 0.055(5) 0.004(4) -0.025(5) 0.003(4) O145 0.090(5) 0.131(5) 0.059(4) 0.019(3) -0.020(3) 0.004(4) Cl1 0.0541(12) 0.0876(12) 0.0511(10) 0.0085(9) -0.0152(8) 0.0133(9) N51 0.044(4) 0.062(3) 0.048(4) 0.012(3) 0.003(3) 0.018(3) N52 0.050(4) 0.074(4) 0.042(3) 0.008(3) -0.012(3) 0.022(3) N53 0.046(4) 0.083(4) 0.051(4) 0.010(3) -0.009(3) 0.020(3) C54 0.054(5) 0.066(4) 0.041(4) 0.011(3) -0.011(3) 0.017(4) C55 0.049(5) 0.061(4) 0.058(4) 0.015(4) -0.012(4) 0.012(4) C56 0.062(5) 0.068(5) 0.047(5) 0.013(4) -0.023(4) 0.005(4) C57 0.047(5) 0.062(4) 0.048(5) 0.014(3) -0.017(3) 0.013(4) C58 0.048(5) 0.072(4) 0.034(4) 0.013(3) -0.017(3) 0.002(4) C59 0.066(5) 0.094(5) 0.026(4) 0.008(3) -0.007(3) 0.026(4) N60 0.073(5) 0.102(5) 0.042(4) 0.021(3) -0.011(3) 0.044(4) C61 0.067(6) 0.078(5) 0.051(4) 0.008(4) -0.012(4) 0.022(4) C62 0.101(7) 0.129(7) 0.045(4) 0.029(4) -0.004(4) 0.059(6) C63 0.060(5) 0.067(4) 0.046(5) 0.016(3) -0.006(4) 0.008(4) N64 0.051(4) 0.086(4) 0.038(4) 0.005(3) -0.011(3) 0.022(3) N65 0.051(4) 0.088(4) 0.049(4) 0.008(3) -0.019(3) 0.033(3) N66 0.048(4) 0.067(3) 0.037(3) 0.001(3) -0.010(3) 0.014(3) C67 0.054(5) 0.068(4) 0.045(4) 0.013(4) -0.027(4) 0.013(4) C68 0.058(5) 0.074(4) 0.030(4) 0.006(3) -0.005(4) 0.018(4) C69 0.049(5) 0.074(4) 0.038(4) 0.001(3) -0.010(3) 0.019(4) C70 0.055(5) 0.070(4) 0.040(4) 0.001(3) -0.010(4) 0.013(4) C71 0.046(5) 0.084(5) 0.037(4) 0.008(3) -0.014(4) 0.004(4) C72 0.050(5) 0.089(5) 0.033(4) 0.011(4) -0.017(3) 0.012(4) C73 0.048(5) 0.091(6) 0.029(3) 0.013(3) -0.010(3) 0.019(5) C74 0.039(6) 0.093(6) 0.042(4) 0.011(4) -0.011(3) 0.007(4) C75 0.057(6) 0.090(6) 0.030(4) -0.002(3) -0.009(3) 0.014(4) C76 0.067(7) 0.094(6) 0.034(4) 0.007(4) -0.016(4) 0.014(5) C77 0.050(6) 0.117(7) 0.063(5) 0.003(5) -0.014(4) 0.011(5) C78 0.062(6) 0.137(8) 0.105(7) 0.015(6) -0.022(5) 0.017(6) C79 0.061(6) 0.115(7) 0.095(6) -0.010(5) -0.009(5) -0.006(5) C80 0.077(7) 0.186(10) 0.053(5) -0.002(6) 0.008(4) -0.008(6) C81 0.051(6) 0.081(5) 0.044(4) 0.016(4) -0.017(4) 0.002(4) C82 0.058(6) 0.080(5) 0.027(3) 0.002(3) -0.015(3) 0.006(4) C83 0.047(5) 0.094(6) 0.042(4) 0.018(4) -0.027(4) 0.010(4) C84 0.055(5) 0.095(6) 0.032(4) 0.001(4) -0.016(4) 0.013(4) C85 0.047(5) 0.109(7) 0.042(4) 0.004(4) -0.013(3) 0.020(4) C86 0.051(5) 0.087(6) 0.050(5) 0.005(4) -0.023(4) 0.008(4) C87 0.066(6) 0.093(6) 0.052(4) 0.008(4) -0.017(4) 0.020(4) C88 0.109(8) 0.108(7) 0.069(5) 0.001(5) -0.016(5) 0.018(6) C89 0.108(8) 0.099(6) 0.072(6) -0.010(5) -0.018(5) 0.011(5) C90 0.085(8) 0.116(7) 0.093(6) -0.006(5) -0.010(5) 0.032(5) C91 0.059(5) 0.099(6) 0.045(5) 0.017(4) -0.010(4) 0.009(4) C92 0.045(5) 0.095(6) 0.050(4) 0.003(4) -0.012(3) 0.013(4) C93 0.052(5) 0.085(5) 0.037(4) 0.005(4) -0.013(4) 0.019(4) C94 0.052(5) 0.096(6) 0.036(4) 0.006(4) -0.016(4) 0.008(4) C95 0.060(5) 0.091(5) 0.048(4) 0.007(3) -0.008(4) 0.003(4) C96 0.051(5) 0.087(4) 0.053(4) 0.007(3) -0.019(3) 0.009(3) C97 0.062(6) 0.097(5) 0.045(4) 0.011(4) -0.010(4) 0.009(4) C98 0.052(5) 0.094(6) 0.045(4) 0.005(4) -0.022(4) 0.005(4) C201 0.071(4) 0.090(4) 0.056(3) 0.011(2) -0.016(3) 0.007(3) C202 0.079(6) 0.098(8) 0.130(10) 0.047(7) -0.004(6) 0.012(5) C204 0.108(8) 0.126(10) 0.079(7) 0.028(5) -0.031(7) -0.035(6) C102 0.051(5) 0.108(6) 0.043(5) 0.006(4) -0.008(4) 0.016(4) C103 0.053(5) 0.096(5) 0.038(4) 0.007(4) -0.019(4) 0.019(4) C145 0.049(5) 0.057(4) 0.050(4) 0.003(3) -0.009(4) 0.010(4) C146 0.059(5) 0.075(5) 0.050(4) 0.002(3) -0.005(4) 0.022(4) C147 0.043(5) 0.069(5) 0.053(4) 0.005(4) -0.013(3) 0.011(4) C148 0.049(5) 0.060(4) 0.053(4) 0.005(4) -0.006(4) 0.009(3) C149 0.037(5) 0.062(4) 0.063(4) 0.008(3) -0.008(4) 0.010(3) C150 0.041(6) 0.073(5) 0.063(4) 0.015(4) -0.017(4) 0.019(4) C110 0.050(5) 0.069(5) 0.074(5) 0.007(4) -0.014(4) 0.014(4) C151 0.063(7) 0.071(5) 0.069(5) -0.001(4) -0.009(4) 0.023(4) C112 0.054(6) 0.058(5) 0.059(4) 0.002(4) -0.019(4) 0.019(4) C152 0.050(5) 0.059(5) 0.065(4) 0.004(4) -0.011(4) 0.008(4) C153 0.054(6) 0.068(5) 0.069(5) 0.001(4) -0.004(4) 0.020(4) C115 0.055(5) 0.077(5) 0.086(6) -0.009(5) 0.002(4) 0.008(4) C154 0.116(8) 0.075(6) 0.127(8) -0.009(6) 0.043(7) -0.002(5) C155 0.078(6) 0.083(6) 0.098(6) -0.011(5) -0.005(5) 0.000(5) C156 0.041(5) 0.104(7) 0.145(8) -0.021(6) -0.020(5) 0.006(4) C157 0.034(5) 0.062(4) 0.064(5) -0.002(4) -0.011(4) 0.006(3) C158 0.050(6) 0.075(5) 0.087(6) 0.006(4) -0.017(5) 0.012(4) C159 0.042(6) 0.076(5) 0.091(6) 0.003(5) -0.012(5) 0.016(4) C122 0.035(5) 0.071(5) 0.093(6) 0.003(4) -0.007(5) 0.014(4) C160 0.055(6) 0.085(6) 0.084(5) 0.016(4) 0.002(5) 0.007(4) C161 0.044(6) 0.093(6) 0.067(5) 0.010(4) -0.010(4) 0.011(4) C125 0.046(6) 0.079(6) 0.114(7) 0.002(5) 0.004(5) 0.011(4) C162 0.094(8) 0.134(9) 0.136(9) 0.009(7) 0.022(7) -0.015(6) C163 0.080(8) 0.104(8) 0.180(11) 0.027(7) 0.034(7) 0.003(6) C164 0.062(7) 0.205(13) 0.180(12) 0.072(10) 0.032(7) 0.043(8) C165 0.040(5) 0.072(5) 0.053(4) 0.015(4) -0.005(4) 0.019(4) C130 0.054(5) 0.069(5) 0.060(5) 0.011(4) -0.010(4) 0.013(4) C166 0.059(5) 0.075(5) 0.060(5) 0.006(4) -0.005(4) 0.001(4) C167 0.065(5) 0.071(5) 0.062(5) 0.010(4) -0.017(4) 0.005(4) C133 0.075(7) 0.092(6) 0.062(5) 0.013(4) -0.011(5) 0.001(5) C168 0.075(7) 0.125(7) 0.079(6) 0.009(5) -0.006(5) 0.007(5) C169 0.102(7) 0.107(7) 0.073(6) 0.027(5) -0.021(5) 0.009(5) C170 0.109(8) 0.113(7) 0.054(5) -0.001(5) -0.017(5) -0.016(6) C171 0.070(6) 0.074(5) 0.071(6) 0.016(4) -0.006(4) 0.001(4) C172 0.069(6) 0.071(5) 0.057(5) 0.013(4) -0.023(4) 0.005(4) C173 0.063(5) 0.076(5) 0.055(5) 0.005(4) -0.007(4) 0.023(4) C140 0.043(5) 0.081(5) 0.049(4) 0.010(4) -0.012(3) 0.011(4) C203 0.142(12) 0.118(9) 0.068(6) 0.012(5) 0.016(6) 0.014(7) C302 0.111(16) 0.10(2) 0.103(14) 0.047(8) -0.063(14) -0.006(13) C303 0.069(8) 0.14(2) 0.10(2) 0.048(12) -0.007(10) 0.005(12) C304 0.07(2) 0.087(6) 0.122(18) 0.002(11) 0.021(11) 0.010(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.57(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 O101 . N103 . 1.238(11) yes O102 . N103 . 1.213(11) yes N103 . C104 . 1.488(12) yes C104 . C105 . 1.355(13) yes C104 . C109 . 1.356(13) yes C105 . C106 . 1.393(12) yes C105 . H1051 . 0.925 no C106 . C107 . 1.440(11) yes C106 . C111 . 1.468(13) yes C107 . C108 . 1.393(11) yes C107 . H1071 . 0.985 no C108 . C109 . 1.378(11) yes C108 . C144 . 1.507(12) yes C109 . H1091 . 0.951 no O110 . C111 . 1.247(10) yes C111 . N112 . 1.332(10) yes N112 . C113 . 1.436(9) yes N112 . H1121 . 0.900 no C113 . C114 . 1.466(8) yes C113 . H1132 . 0.993 no C113 . H1131 . 0.982 no C114 . O115 . 1.435(8) yes C114 . H1141 . 0.971 no C114 . H1142 . 0.960 no O115 . C116 . 1.397(9) yes C116 . C117 . 1.395(12) yes C116 . C121 . 1.351(12) yes C117 . C118 . 1.395(11) yes C117 . H1171 . 0.948 no C118 . C119 . 1.345(11) yes C118 . H1181 . 0.955 no C119 . C120 . 1.377(11) yes C119 . O122 . 1.385(9) yes C120 . C121 . 1.387(11) yes C120 . H1201 . 0.964 no C121 . H1211 . 0.930 no O122 . C123 . 1.451(7) yes C123 . C124 . 1.519(7) yes C123 . H1231 . 0.966 no C123 . H1232 . 1.001 no C124 . O125 . 1.432(7) yes C124 . H1242 . 0.974 no C124 . H1241 . 0.970 no O125 . C126 . 1.440(7) yes C126 . C127 . 1.522(8) yes C126 . H1261 . 1.004 no C126 . H1262 . 0.980 no C127 . C128 . 1.319(10) yes C127 . H1271 . 0.939 no C128 . C129 . 1.528(8) yes C128 . H1281 . 0.952 no C129 . O130 . 1.448(7) yes C129 . H1291 . 0.966 no C129 . H1292 . 0.970 no O130 . C131 . 1.427(7) yes C131 . C132 . 1.521(7) yes C131 . H1312 . 1.004 no C131 . H1311 . 0.992 no C132 . O133 . 1.425(6) yes C132 . H1321 . 0.992 no C132 . H1322 . 0.987 no O133 . C134 . 1.412(9) yes C134 . C135 . 1.337(10) yes C134 . C139 . 1.398(10) yes C135 . C136 . 1.412(10) yes C135 . H1351 . 0.947 no C136 . C137 . 1.370(10) yes C136 . H1361 . 0.930 no C137 . C138 . 1.375(11) yes C137 . O140 . 1.409(8) yes C138 . C139 . 1.403(10) yes C138 . H1381 . 0.949 no C139 . H1391 . 0.961 no O140 . C141 . 1.419(7) yes C141 . C142 . 1.528(7) yes C141 . H1411 . 0.983 no C141 . H1412 . 0.978 no C142 . N143 . 1.461(8) yes C142 . H1421 . 0.965 no C142 . H1422 . 0.967 no N143 . C144 . 1.343(9) yes N143 . H1431 . 0.900 no C144 . O145 . 1.232(10) yes N51 . N52 . 1.381(7) yes N51 . C55 . 1.323(9) yes N51 . C145 . 1.430(8) yes N52 . N53 . 1.311(7) yes N53 . C54 . 1.372(8) yes C54 . C55 . 1.368(9) yes C54 . C56 . 1.461(10) yes C55 . H551 . 0.930 no C56 . C57 . 1.371(10) yes C56 . C61 . 1.385(9) yes C57 . C58 . 1.396(9) yes C57 . H571 . 0.910 no C58 . C59 . 1.372(9) yes C58 . C63 . 1.490(10) yes C59 . N60 . 1.344(8) yes C59 . H591 . 0.938 no N60 . C61 . 1.322(9) yes N60 . C62 . 1.523(8) yes C61 . H611 . 0.963 no C62 . H622 . 0.944 no C62 . H621 . 0.964 no C62 . H623 . 0.964 no C63 . N64 . 1.341(9) yes C63 . C67 . 1.393(9) yes N64 . N65 . 1.325(7) yes N65 . N66 . 1.369(7) yes N66 . C67 . 1.333(9) yes N66 . C68 . 1.440(8) yes C67 . H671 . 0.959 no C68 . C69 . 1.389(9) yes C68 . C103 . 1.364(10) yes C69 . C70 . 1.385(9) yes C69 . H691 . 0.980 no C70 . C71 . 1.377(10) yes C70 . H701 . 0.946 no C71 . C72 . 1.587(9) yes C71 . C102 . 1.410(10) yes C72 . C73 . 1.561(10) yes C72 . C83 . 1.555(10) yes C72 . C93 . 1.531(10) yes C73 . C74 . 1.387(10) yes C73 . C82 . 1.391(10) yes C74 . C75 . 1.382(10) yes C74 . H741 . 0.912 no C75 . C76 . 1.413(10) yes C75 . H751 . 0.924 no C76 . C77 . 1.534(11) yes C76 . C81 . 1.385(10) yes C77 . C78 . 1.514(12) yes C77 . C79 . 1.518(12) yes C77 . C80 . 1.544(11) yes C78 . H781 . 0.997 no C78 . H782 . 0.976 no C78 . H783 . 0.979 no C79 . H791 . 0.952 no C79 . H793 . 0.987 no C79 . H792 . 0.978 no C80 . H801 . 1.001 no C80 . H803 . 0.992 no C80 . H802 . 0.984 no C81 . C82 . 1.387(10) yes C81 . H811 . 0.941 no C82 . H821 . 0.947 no C83 . C84 . 1.390(10) yes C83 . C92 . 1.395(10) yes C84 . C85 . 1.396(10) yes C84 . H841 . 0.906 no C85 . C86 . 1.420(11) yes C85 . H851 . 0.921 no C86 . C87 . 1.527(11) yes C86 . C91 . 1.378(10) yes C87 . C88 . 1.545(12) yes C87 . C89 . 1.546(10) yes C87 . C90 . 1.503(12) yes C88 . H881 . 0.966 no C88 . H883 . 0.984 no C88 . H882 . 0.970 no C89 . H891 . 0.977 no C89 . H892 . 0.984 no C89 . H893 . 0.987 no C90 . H901 . 0.987 no C90 . H902 . 1.007 no C90 . H903 . 0.995 no C91 . C92 . 1.395(10) yes C91 . H911 . 0.917 no C92 . H921 . 0.928 no C93 . C94 . 1.402(10) yes C93 . C98 . 1.410(9) yes C94 . C95 . 1.377(10) yes C94 . H941 . 0.931 no C95 . C96 . 1.411(9) yes C95 . H951 . 0.932 no C96 . C97 . 1.397(10) yes C96 . C201 . 1.511(10) yes C97 . C98 . 1.373(10) yes C97 . H971 . 0.964 no C98 . H981 . 0.915 no C201 . C202 . 1.519(8) yes C201 . C204 . 1.518(8) yes C201 . C203 . 1.530(8) yes C202 . H2021 . 0.950 no C202 . H2022 . 0.950 no C202 . H2023 . 0.950 no C204 . H2041 . 0.950 no C204 . H2042 . 0.950 no C204 . H2043 . 0.950 no C102 . C103 . 1.388(9) yes C102 . H1021 . 0.939 no C103 . H1031 . 0.956 no C145 . C146 . 1.382(9) yes C145 . C140 . 1.368(9) yes C146 . C147 . 1.412(9) yes C146 . H1461 . 0.932 no C147 . C148 . 1.362(9) yes C147 . H1471 . 0.972 no C148 . C149 . 1.544(9) yes C148 . C173 . 1.407(9) yes C149 . C150 . 1.570(10) yes C149 . C157 . 1.525(10) yes C149 . C165 . 1.550(9) yes C150 . C110 . 1.366(10) yes C150 . C153 . 1.381(10) yes C110 . C151 . 1.411(10) yes C110 . H1101 . 0.949 no C151 . C112 . 1.394(10) yes C151 . H1511 . 0.923 no C112 . C152 . 1.373(10) yes C112 . C115 . 1.524(10) yes C152 . C153 . 1.383(10) yes C152 . H1521 . 0.913 no C153 . H1531 . 0.940 no C115 . C154 . 1.525(12) yes C115 . C155 . 1.528(11) yes C115 . C156 . 1.555(11) yes C154 . H1541 . 0.986 no C154 . H1543 . 0.971 no C154 . H1542 . 0.984 no C155 . H1551 . 0.968 no C155 . H1553 . 0.964 no C155 . H1552 . 0.971 no C156 . H1561 . 0.988 no C156 . H1562 . 0.981 no C156 . H1563 . 0.991 no C157 . C158 . 1.414(10) yes C157 . C161 . 1.404(10) yes C158 . C159 . 1.360(11) yes C158 . H1581 . 0.966 no C159 . C122 . 1.377(11) yes C159 . H1591 . 0.919 no C122 . C160 . 1.401(11) yes C122 . C125 . 1.518(12) yes C160 . C161 . 1.359(11) yes C160 . H1601 . 0.964 no C161 . H1611 . 0.949 no C125 . C162 . 1.561(13) yes C125 . C163 . 1.506(12) yes C125 . C164 . 1.491(12) yes C162 . H1622 . 0.948 no C162 . H1621 . 0.963 no C162 . H1623 . 0.950 no C163 . H1631 . 0.949 no C163 . H1633 . 0.966 no C163 . H1632 . 0.959 no C164 . H1641 . 0.983 no C164 . H1643 . 0.988 no C164 . H1642 . 0.993 no C165 . C130 . 1.425(10) yes C165 . C172 . 1.372(10) yes C130 . C166 . 1.374(10) yes C130 . H1301 . 0.930 no C166 . C167 . 1.366(10) yes C166 . H1661 . 0.950 no C167 . C133 . 1.553(11) yes C167 . C171 . 1.411(10) yes C133 . C168 . 1.520(12) yes C133 . C169 . 1.526(11) yes C133 . C170 . 1.545(11) yes C168 . H1681 . 0.990 no C168 . H1683 . 0.987 no C168 . H1682 . 0.988 no C169 . H1691 . 0.967 no C169 . H1693 . 0.956 no C169 . H1692 . 0.950 no C170 . H1701 . 0.947 no C170 . H1702 . 0.958 no C170 . H1703 . 0.960 no C171 . C172 . 1.390(10) yes C171 . H1711 . 0.947 no C172 . H1721 . 0.952 no C173 . C140 . 1.371(9) yes C173 . H1731 . 0.949 no C140 . H1401 . 0.956 no C203 . H2031 . 0.950 no C203 . H2032 . 0.950 no C203 . H2033 . 0.950 no C302 . H3021 . 0.950 no C302 . H3022 . 0.950 no C302 . H3023 . 0.950 no C303 . H3031 . 0.950 no C303 . H3032 . 0.950 no C303 . H3033 . 0.950 no C304 . H3041 . 0.950 no C304 . H3042 . 0.950 no C304 . H3043 . 0.950 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 O101 . N103 . O102 . 124.8(9) yes O101 . N103 . C104 . 116.1(11) yes O102 . N103 . C104 . 118.9(11) yes N103 . C104 . C105 . 116.5(11) yes N103 . C104 . C109 . 120.9(11) yes C105 . C104 . C109 . 122.5(8) yes C104 . C105 . C106 . 122.2(9) yes C104 . C105 . H1051 . 121.0 no C106 . C105 . H1051 . 116.7 no C105 . C106 . C107 . 114.9(9) yes C105 . C106 . C111 . 122.7(9) yes C107 . C106 . C111 . 122.4(7) yes C106 . C107 . C108 . 121.6(7) yes C106 . C107 . H1071 . 117.9 no C108 . C107 . H1071 . 120.5 no C107 . C108 . C109 . 119.6(9) yes C107 . C108 . C144 . 124.2(7) yes C109 . C108 . C144 . 116.2(9) yes C108 . C109 . C104 . 119.2(9) yes C108 . C109 . H1091 . 122.5 no C104 . C109 . H1091 . 118.3 no C106 . C111 . O110 . 118.4(8) yes C106 . C111 . N112 . 118.5(9) yes O110 . C111 . N112 . 123.0(9) yes C111 . N112 . C113 . 119.9(7) yes C111 . N112 . H1121 . 121.2 no C113 . N112 . H1121 . 119.0 no N112 . C113 . C114 . 111.8(7) yes N112 . C113 . H1132 . 109.9 no C114 . C113 . H1132 . 112.4 no N112 . C113 . H1131 . 109.7 no C114 . C113 . H1131 . 103.2 no H1132 . C113 . H1131 . 109.7 no C113 . C114 . O115 . 111.0(8) yes C113 . C114 . H1141 . 105.9 no O115 . C114 . H1141 . 112.6 no C113 . C114 . H1142 . 106.3 no O115 . C114 . H1142 . 109.7 no H1141 . C114 . H1142 . 111.1 no C114 . O115 . C116 . 111.7(7) yes O115 . C116 . C117 . 115.2(9) yes O115 . C116 . C121 . 125.0(8) yes C117 . C116 . C121 . 119.8(7) yes C116 . C117 . C118 . 119.3(9) yes C116 . C117 . H1171 . 118.0 no C118 . C117 . H1171 . 122.6 no C117 . C118 . C119 . 120.8(8) yes C117 . C118 . H1181 . 119.9 no C119 . C118 . H1181 . 119.3 no C118 . C119 . C120 . 119.2(7) yes C118 . C119 . O122 . 126.0(8) yes C120 . C119 . O122 . 114.8(8) yes C119 . C120 . C121 . 121.1(8) yes C119 . C120 . H1201 . 120.0 no C121 . C120 . H1201 . 118.8 no C120 . C121 . C116 . 119.7(8) yes C120 . C121 . H1211 . 121.5 no C116 . C121 . H1211 . 118.8 no C119 . O122 . C123 . 118.4(6) yes O122 . C123 . C124 . 111.4(5) yes O122 . C123 . H1231 . 106.0 no C124 . C123 . H1231 . 107.4 no O122 . C123 . H1232 . 108.8 no C124 . C123 . H1232 . 109.4 no H1231 . C123 . H1232 . 113.9 no C123 . C124 . O125 . 107.7(5) yes C123 . C124 . H1242 . 109.8 no O125 . C124 . H1242 . 111.5 no C123 . C124 . H1241 . 110.9 no O125 . C124 . H1241 . 108.1 no H1242 . C124 . H1241 . 108.8 no C124 . O125 . C126 . 112.7(5) yes O125 . C126 . C127 . 105.9(6) yes O125 . C126 . H1261 . 110.4 no C127 . C126 . H1261 . 110.2 no O125 . C126 . H1262 . 112.8 no C127 . C126 . H1262 . 107.7 no H1261 . C126 . H1262 . 109.8 no C126 . C127 . C128 . 122.6(6) yes C126 . C127 . H1271 . 119.9 no C128 . C127 . H1271 . 117.5 no C127 . C128 . C129 . 123.4(6) yes C127 . C128 . H1281 . 119.2 no C129 . C128 . H1281 . 117.3 no C128 . C129 . O130 . 111.8(6) yes C128 . C129 . H1291 . 110.4 no O130 . C129 . H1291 . 106.1 no C128 . C129 . H1292 . 107.0 no O130 . C129 . H1292 . 112.4 no H1291 . C129 . H1292 . 109.2 no C129 . O130 . C131 . 113.3(6) yes O130 . C131 . C132 . 107.7(5) yes O130 . C131 . H1312 . 111.4 no C132 . C131 . H1312 . 106.1 no O130 . C131 . H1311 . 111.8 no C132 . C131 . H1311 . 107.3 no H1312 . C131 . H1311 . 112.2 no C131 . C132 . O133 . 108.2(5) yes C131 . C132 . H1321 . 107.4 no O133 . C132 . H1321 . 108.1 no C131 . C132 . H1322 . 109.1 no O133 . C132 . H1322 . 113.5 no H1321 . C132 . H1322 . 110.3 no C132 . O133 . C134 . 114.7(5) yes O133 . C134 . C135 . 124.0(7) yes O133 . C134 . C139 . 114.3(7) yes C135 . C134 . C139 . 121.4(7) yes C134 . C135 . C136 . 121.7(7) yes C134 . C135 . H1351 . 120.6 no C136 . C135 . H1351 . 117.7 no C135 . C136 . C137 . 117.6(8) yes C135 . C136 . H1361 . 118.2 no C137 . C136 . H1361 . 124.2 no C136 . C137 . C138 . 121.1(7) yes C136 . C137 . O140 . 123.4(8) yes C138 . C137 . O140 . 115.2(7) yes C137 . C138 . C139 . 121.0(7) yes C137 . C138 . H1381 . 120.0 no C139 . C138 . H1381 . 119.0 no C138 . C139 . C134 . 117.1(7) yes C138 . C139 . H1391 . 121.8 no C134 . C139 . H1391 . 121.0 no C137 . O140 . C141 . 116.7(6) yes O140 . C141 . C142 . 107.1(6) yes O140 . C141 . H1411 . 111.1 no C142 . C141 . H1411 . 110.7 no O140 . C141 . H1412 . 113.0 no C142 . C141 . H1412 . 106.6 no H1411 . C141 . H1412 . 108.2 no C141 . C142 . N143 . 112.8(7) yes C141 . C142 . H1421 . 108.1 no N143 . C142 . H1421 . 106.7 no C141 . C142 . H1422 . 109.2 no N143 . C142 . H1422 . 107.7 no H1421 . C142 . H1422 . 112.3 no C142 . N143 . C144 . 117.1(7) yes C142 . N143 . H1431 . 121.0 no C144 . N143 . H1431 . 121.9 no C108 . C144 . N143 . 118.1(8) yes C108 . C144 . O145 . 119.1(7) yes N143 . C144 . O145 . 122.8(9) yes N52 . N51 . C55 . 110.2(5) yes N52 . N51 . C145 . 119.3(5) yes C55 . N51 . C145 . 130.5(5) yes N51 . N52 . N53 . 106.3(5) yes N52 . N53 . C54 . 109.5(5) yes N53 . C54 . C55 . 107.3(6) yes N53 . C54 . C56 . 121.9(5) yes C55 . C54 . C56 . 130.8(7) yes C54 . C55 . N51 . 106.6(6) yes C54 . C55 . H551 . 125.8 no N51 . C55 . H551 . 127.6 no C54 . C56 . C57 . 120.7(6) yes C54 . C56 . C61 . 121.5(7) yes C57 . C56 . C61 . 117.8(7) yes C56 . C57 . C58 . 120.3(6) yes C56 . C57 . H571 . 118.7 no C58 . C57 . H571 . 121.1 no C57 . C58 . C59 . 119.2(6) yes C57 . C58 . C63 . 120.5(6) yes C59 . C58 . C63 . 120.3(6) yes C58 . C59 . N60 . 119.3(6) yes C58 . C59 . H591 . 119.2 no N60 . C59 . H591 . 121.5 no C59 . N60 . C61 . 122.1(6) yes C59 . N60 . C62 . 119.7(6) yes C61 . N60 . C62 . 118.2(6) yes C56 . C61 . N60 . 121.3(7) yes C56 . C61 . H611 . 119.6 no N60 . C61 . H611 . 119.1 no N60 . C62 . H622 . 109.8 no N60 . C62 . H621 . 106.5 no H622 . C62 . H621 . 111.9 no N60 . C62 . H623 . 105.0 no H622 . C62 . H623 . 112.0 no H621 . C62 . H623 . 111.3 no C58 . C63 . N64 . 125.5(6) yes C58 . C63 . C67 . 125.2(7) yes N64 . C63 . C67 . 109.2(6) yes C63 . N64 . N65 . 109.2(5) yes N64 . N65 . N66 . 106.0(5) yes N65 . N66 . C67 . 111.8(5) yes N65 . N66 . C68 . 121.0(6) yes C67 . N66 . C68 . 127.2(5) yes C63 . C67 . N66 . 103.7(6) yes C63 . C67 . H671 . 131.0 no N66 . C67 . H671 . 125.3 no N66 . C68 . C69 . 117.7(6) yes N66 . C68 . C103 . 120.8(6) yes C69 . C68 . C103 . 121.5(6) yes C68 . C69 . C70 . 118.7(6) yes C68 . C69 . H691 . 119.7 no C70 . C69 . H691 . 121.6 no C69 . C70 . C71 . 121.2(6) yes C69 . C70 . H701 . 120.2 no C71 . C70 . H701 . 118.5 no C70 . C71 . C72 . 123.5(6) yes C70 . C71 . C102 . 118.9(6) yes C72 . C71 . C102 . 117.6(6) yes C71 . C72 . C73 . 109.0(5) yes C71 . C72 . C83 . 107.5(5) yes C73 . C72 . C83 . 110.7(6) yes C71 . C72 . C93 . 110.2(6) yes C73 . C72 . C93 . 108.7(5) yes C83 . C72 . C93 . 110.7(6) yes C72 . C73 . C74 . 119.4(7) yes C72 . C73 . C82 . 123.1(7) yes C74 . C73 . C82 . 117.6(7) yes C73 . C74 . C75 . 121.6(7) yes C73 . C74 . H741 . 119.1 no C75 . C74 . H741 . 119.3 no C74 . C75 . C76 . 120.9(7) yes C74 . C75 . H751 . 120.7 no C76 . C75 . H751 . 118.3 no C75 . C76 . C77 . 120.2(7) yes C75 . C76 . C81 . 116.5(7) yes C77 . C76 . C81 . 123.2(8) yes C76 . C77 . C78 . 111.1(8) yes C76 . C77 . C79 . 111.4(7) yes C78 . C77 . C79 . 110.0(7) yes C76 . C77 . C80 . 107.4(6) yes C78 . C77 . C80 . 108.5(8) yes C79 . C77 . C80 . 108.3(8) yes C77 . C78 . H781 . 109.1 no C77 . C78 . H782 . 107.7 no H781 . C78 . H782 . 112.8 no C77 . C78 . H783 . 104.5 no H781 . C78 . H783 . 110.6 no H782 . C78 . H783 . 111.7 no C77 . C79 . H791 . 109.2 no C77 . C79 . H793 . 108.9 no H791 . C79 . H793 . 107.9 no C77 . C79 . H792 . 111.6 no H791 . C79 . H792 . 107.7 no H793 . C79 . H792 . 111.5 no C77 . C80 . H801 . 113.8 no C77 . C80 . H803 . 108.5 no H801 . C80 . H803 . 107.4 no C77 . C80 . H802 . 107.6 no H801 . C80 . H802 . 110.3 no H803 . C80 . H802 . 109.2 no C76 . C81 . C82 . 122.3(7) yes C76 . C81 . H811 . 120.3 no C82 . C81 . H811 . 117.5 no C73 . C82 . C81 . 120.7(7) yes C73 . C82 . H821 . 120.3 no C81 . C82 . H821 . 119.0 no C72 . C83 . C84 . 124.3(7) yes C72 . C83 . C92 . 118.9(7) yes C84 . C83 . C92 . 116.8(7) yes C83 . C84 . C85 . 121.6(7) yes C83 . C84 . H841 . 118.9 no C85 . C84 . H841 . 119.5 no C84 . C85 . C86 . 121.0(7) yes C84 . C85 . H851 . 119.8 no C86 . C85 . H851 . 119.2 no C85 . C86 . C87 . 118.9(7) yes C85 . C86 . C91 . 116.9(7) yes C87 . C86 . C91 . 124.2(7) yes C86 . C87 . C88 . 111.7(7) yes C86 . C87 . C89 . 110.0(6) yes C88 . C87 . C89 . 105.3(7) yes C86 . C87 . C90 . 111.6(7) yes C88 . C87 . C90 . 108.1(7) yes C89 . C87 . C90 . 110.0(7) yes C87 . C88 . H881 . 105.4 no C87 . C88 . H883 . 107.7 no H881 . C88 . H883 . 111.4 no C87 . C88 . H882 . 106.9 no H881 . C88 . H882 . 111.7 no H883 . C88 . H882 . 113.2 no C87 . C89 . H891 . 108.8 no C87 . C89 . H892 . 109.9 no H891 . C89 . H892 . 107.0 no C87 . C89 . H893 . 106.3 no H891 . C89 . H893 . 112.7 no H892 . C89 . H893 . 112.2 no C87 . C90 . H901 . 105.6 no C87 . C90 . H902 . 110.9 no H901 . C90 . H902 . 111.6 no C87 . C90 . H903 . 105.9 no H901 . C90 . H903 . 110.0 no H902 . C90 . H903 . 112.5 no C86 . C91 . C92 . 121.6(7) yes C86 . C91 . H911 . 119.0 no C92 . C91 . H911 . 119.5 no C91 . C92 . C83 . 122.0(7) yes C91 . C92 . H921 . 119.0 no C83 . C92 . H921 . 119.0 no C72 . C93 . C94 . 125.6(5) yes C72 . C93 . C98 . 119.7(7) yes C94 . C93 . C98 . 114.6(7) yes C93 . C94 . C95 . 123.1(6) yes C93 . C94 . H941 . 119.3 no C95 . C94 . H941 . 117.5 no C94 . C95 . C96 . 122.0(7) yes C94 . C95 . H951 . 119.7 no C96 . C95 . H951 . 118.3 no C95 . C96 . C97 . 114.7(7) yes C95 . C96 . C201 . 123.4(7) yes C97 . C96 . C201 . 121.9(6) yes C96 . C97 . C98 . 123.3(6) yes C96 . C97 . H971 . 119.6 no C98 . C97 . H971 . 117.1 no C93 . C98 . C97 . 122.2(7) yes C93 . C98 . H981 . 116.5 no C97 . C98 . H981 . 121.3 no C96 . C201 . C202 . 110.6(7) yes C96 . C201 . C204 . 113.7(6) yes C202 . C201 . C204 . 108.4(7) yes C96 . C201 . C203 . 107.8(7) yes C202 . C201 . C203 . 108.2(6) yes C204 . C201 . C203 . 108.1(7) yes C201 . C202 . H2021 . 109.1 no C201 . C202 . H2022 . 109.3 no H2021 . C202 . H2022 . 109.5 no C201 . C202 . H2023 . 110.0 no H2021 . C202 . H2023 . 109.5 no H2022 . C202 . H2023 . 109.5 no C201 . C204 . H2041 . 109.6 no C201 . C204 . H2042 . 108.9 no H2041 . C204 . H2042 . 109.5 no C201 . C204 . H2043 . 109.8 no H2041 . C204 . H2043 . 109.5 no H2042 . C204 . H2043 . 109.5 no C71 . C102 . C103 . 119.9(7) yes C71 . C102 . H1021 . 119.2 no C103 . C102 . H1021 . 120.9 no C102 . C103 . C68 . 119.7(7) yes C102 . C103 . H1031 . 120.2 no C68 . C103 . H1031 . 120.1 no N51 . C145 . C146 . 119.1(6) yes N51 . C145 . C140 . 120.0(6) yes C146 . C145 . C140 . 120.4(6) yes C145 . C146 . C147 . 118.2(6) yes C145 . C146 . H1461 . 117.1 no C147 . C146 . H1461 . 124.7 no C146 . C147 . C148 . 122.6(6) yes C146 . C147 . H1471 . 118.3 no C148 . C147 . H1471 . 119.1 no C147 . C148 . C149 . 123.6(6) yes C147 . C148 . C173 . 116.7(6) yes C149 . C148 . C173 . 119.5(6) yes C148 . C149 . C150 . 105.6(5) yes C148 . C149 . C157 . 112.4(6) yes C150 . C149 . C157 . 109.9(6) yes C148 . C149 . C165 . 110.4(5) yes C150 . C149 . C165 . 110.2(6) yes C157 . C149 . C165 . 108.3(5) yes C149 . C150 . C110 . 123.7(7) yes C149 . C150 . C153 . 119.6(7) yes C110 . C150 . C153 . 116.7(7) yes C150 . C110 . C151 . 121.5(8) yes C150 . C110 . H1101 . 119.5 no C151 . C110 . H1101 . 118.9 no C110 . C151 . C112 . 121.2(7) yes C110 . C151 . H1511 . 121.8 no C112 . C151 . H1511 . 116.9 no C151 . C112 . C152 . 116.3(7) yes C151 . C112 . C115 . 122.7(7) yes C152 . C112 . C115 . 121.0(7) yes C112 . C152 . C153 . 122.0(7) yes C112 . C152 . H1521 . 117.9 no C153 . C152 . H1521 . 120.1 no C152 . C153 . C150 . 122.2(7) yes C152 . C153 . H1531 . 118.9 no C150 . C153 . H1531 . 118.9 no C112 . C115 . C154 . 108.9(7) yes C112 . C115 . C155 . 113.4(7) yes C154 . C115 . C155 . 107.6(7) yes C112 . C115 . C156 . 109.7(6) yes C154 . C115 . C156 . 109.2(8) yes C155 . C115 . C156 . 108.0(7) yes C115 . C154 . H1541 . 112.2 no C115 . C154 . H1543 . 114.0 no H1541 . C154 . H1543 . 105.9 no C115 . C154 . H1542 . 111.4 no H1541 . C154 . H1542 . 107.6 no H1543 . C154 . H1542 . 105.2 no C115 . C155 . H1551 . 108.9 no C115 . C155 . H1553 . 111.0 no H1551 . C155 . H1553 . 108.7 no C115 . C155 . H1552 . 109.3 no H1551 . C155 . H1552 . 109.8 no H1553 . C155 . H1552 . 109.0 no C115 . C156 . H1561 . 109.2 no C115 . C156 . H1562 . 107.6 no H1561 . C156 . H1562 . 110.8 no C115 . C156 . H1563 . 106.7 no H1561 . C156 . H1563 . 111.6 no H1562 . C156 . H1563 . 110.7 no C149 . C157 . C158 . 121.9(7) yes C149 . C157 . C161 . 124.8(6) yes C158 . C157 . C161 . 113.3(8) yes C157 . C158 . C159 . 123.7(8) yes C157 . C158 . H1581 . 117.7 no C159 . C158 . H1581 . 118.6 no C158 . C159 . C122 . 122.2(7) yes C158 . C159 . H1591 . 119.2 no C122 . C159 . H1591 . 118.5 no C159 . C122 . C160 . 114.9(8) yes C159 . C122 . C125 . 123.1(7) yes C160 . C122 . C125 . 122.0(8) yes C122 . C160 . C161 . 123.3(8) yes C122 . C160 . H1601 . 118.5 no C161 . C160 . H1601 . 118.2 no C157 . C161 . C160 . 122.3(7) yes C157 . C161 . H1611 . 115.6 no C160 . C161 . H1611 . 122.1 no C122 . C125 . C162 . 109.6(7) yes C122 . C125 . C163 . 111.4(7) yes C162 . C125 . C163 . 104.3(9) yes C122 . C125 . C164 . 115.1(8) yes C162 . C125 . C164 . 105.4(9) yes C163 . C125 . C164 . 110.2(9) yes C125 . C162 . H1622 . 108.1 no C125 . C162 . H1621 . 109.3 no H1622 . C162 . H1621 . 111.4 no C125 . C162 . H1623 . 107.1 no H1622 . C162 . H1623 . 111.6 no H1621 . C162 . H1623 . 109.2 no C125 . C163 . H1631 . 106.7 no C125 . C163 . H1633 . 106.1 no H1631 . C163 . H1633 . 113.4 no C125 . C163 . H1632 . 106.7 no H1631 . C163 . H1632 . 113.0 no H1633 . C163 . H1632 . 110.4 no C125 . C164 . H1641 . 105.4 no C125 . C164 . H1643 . 104.8 no H1641 . C164 . H1643 . 111.8 no C125 . C164 . H1642 . 109.8 no H1641 . C164 . H1642 . 112.3 no H1643 . C164 . H1642 . 112.2 no C149 . C165 . C130 . 119.0(6) yes C149 . C165 . C172 . 123.9(6) yes C130 . C165 . C172 . 117.0(6) yes C165 . C130 . C166 . 120.2(7) yes C165 . C130 . H1301 . 118.9 no C166 . C130 . H1301 . 120.9 no C130 . C166 . C167 . 123.3(7) yes C130 . C166 . H1661 . 117.2 no C167 . C166 . H1661 . 119.6 no C166 . C167 . C133 . 125.7(7) yes C166 . C167 . C171 . 116.6(7) yes C133 . C167 . C171 . 117.7(7) yes C167 . C133 . C168 . 109.8(7) yes C167 . C133 . C169 . 109.9(7) yes C168 . C133 . C169 . 110.8(7) yes C167 . C133 . C170 . 109.8(7) yes C168 . C133 . C170 . 108.9(7) yes C169 . C133 . C170 . 107.6(7) yes C133 . C168 . H1681 . 114.3 no C133 . C168 . H1683 . 110.4 no H1681 . C168 . H1683 . 110.3 no C133 . C168 . H1682 . 108.2 no H1681 . C168 . H1682 . 106.4 no H1683 . C168 . H1682 . 106.8 no C133 . C169 . H1691 . 110.3 no C133 . C169 . H1693 . 103.8 no H1691 . C169 . H1693 . 111.9 no C133 . C169 . H1692 . 109.7 no H1691 . C169 . H1692 . 111.2 no H1693 . C169 . H1692 . 109.7 no C133 . C170 . H1701 . 109.5 no C133 . C170 . H1702 . 107.6 no H1701 . C170 . H1702 . 108.7 no C133 . C170 . H1703 . 108.9 no H1701 . C170 . H1703 . 108.2 no H1702 . C170 . H1703 . 114.0 no C167 . C171 . C172 . 121.1(7) yes C167 . C171 . H1711 . 120.4 no C172 . C171 . H1711 . 118.5 no C171 . C172 . C165 . 121.8(7) yes C171 . C172 . H1721 . 119.8 no C165 . C172 . H1721 . 118.4 no C148 . C173 . C140 . 121.8(7) yes C148 . C173 . H1731 . 116.2 no C140 . C173 . H1731 . 122.0 no C173 . C140 . C145 . 120.1(6) yes C173 . C140 . H1401 . 119.7 no C145 . C140 . H1401 . 120.1 no C201 . C203 . H2031 . 109.4 no C201 . C203 . H2032 . 109.1 no H2031 . C203 . H2032 . 109.5 no C201 . C203 . H2033 . 109.9 no H2031 . C203 . H2033 . 109.5 no H2032 . C203 . H2033 . 109.5 no C201 . C302 . H3021 . 111.7 no C201 . C302 . H3022 . 110.4 no H3021 . C302 . H3022 . 109.5 no C201 . C302 . H3023 . 106.3 no H3021 . C302 . H3023 . 109.5 no H3022 . C302 . H3023 . 109.5 no C201 . C303 . H3031 . 109.0 no C201 . C303 . H3032 . 107.5 no H3031 . C303 . H3032 . 109.5 no C201 . C303 . H3033 . 111.9 no H3031 . C303 . H3033 . 109.5 no H3032 . C303 . H3033 . 109.5 no C201 . C304 . H3041 . 109.7 no C201 . C304 . H3042 . 111.3 no H3041 . C304 . H3042 . 109.5 no C201 . C304 . H3043 . 107.5 no H3041 . C304 . H3043 . 109.5 no H3042 . C304 . H3043 . 109.5 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 C117 . H1171 . O130 1_655 159.4(2) 0.948 2.593 3.497(12) yes C59 . H591 . N64 2_466 167.37(19) 0.938 2.498 3.419(12) yes C61 . H611 . O125 . 162.7(2) 0.963 2.287 3.220(12) yes C62 . H621 . N65 2_466 137.9(3) 0.964 2.354 3.137(12) yes C62 . H623 . O130 . 161.38(18) 0.964 2.518 3.446(12) yes C70 . H701 . C74 . 131.1(3) 0.946 2.320 3.027(12) yes C82 . H821 . C92 . 121.5(2) 0.947 2.493 3.095(12) yes C95 . H951 . O102 1_455 162.3(3) 0.932 2.464 3.364(12) yes C147 . H1471 . C130 . 124.2(2) 0.972 2.483 3.135(12) yes C161 . H1611 . C173 . 132.2(2) 0.949 2.368 3.087(12) yes C172 . H1721 . C153 . 125.0(3) 0.952 2.536 3.180(12) yes