# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 #TrackingRef 'CrystallographicData-revised.cif' #============================================================================== _publ_contact_author_name 'Paul D. Beer' _publ_contact_author_address ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; _publ_contact_author_email paul.beer@chem.ox.ac.uk _publ_section_title ; A meta-xylenediamide macrocycle containing rotaxane anion host system constructed by a new synthetic clipping methodology ; loop_ _publ_author_name _publ_author_address 'Nicholas H. Evans' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; 'Christopher J. Serpell' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford, OX1 3TA. UK. ; 'Paul D. Beer' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; _publ_section_abstract ; A novel rotaxane containing a meta-xylenediamide macrocycle is prepared by a new clipping methodology. Upon anion metathesis to the non-coordinating hexafluorophosphate salt, the rotaxane host system was shown to bind chloride and bromide anions more strongly than the basic oxoanions dihydrogen phosphate and acetate in the competitive solvent system 1:1 CDCl3:CD3OD. ; #============================================================================== data_5Cl _database_code_depnum_ccdc_archive 'CCDC 813286' #TrackingRef 'CrystallographicData-revised.cif' #============================================================================== _audit_creation_date 10-11-25 _audit_creation_method CRYSTALS_ver_14.07 _oxford_structure_analysis_title 009CJS10 _chemical_name_systematic . _chemical_melting_point . _refine_special_details ; After structure solution, the entire main residue could be modelled as well as a single chloroform molecule. No further structure could be resolved in the solvent cavity, and Platon SQUEEZE was therefore used to model this diffuse electron density. ; # start Validation Reply Form _vrf_PLAT027_5Cl ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 51.94 Deg. RESPONSE: The sample diffracted very weakly, and at high angles the reflections were completely absent, even when subjected to synchrotron radiation. This is ascribed to the large cavity containing disordered solvent. ; # 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 0.000 0.000 0.500 821 216 ' ' 2 1.500 0.500 0.000 821 218 ' ' _platon_squeeze_details ; The PLATON/SQUEEZE routine was used to model the disordered solvent cavity because there was no discernible structure in the Fourier difference map within this volume. It is therefore very difficult to know what proportion of the two solvents used in crystallisation occupy the cavity (even considering the electron count derived using SQUEEZE), and therefore it was deemed inappropriate to include such speculative information in the data reported in Supplementary Table 1. ; _cell_length_a 11.498(6) _cell_length_b 29.702(16) _cell_length_c 31.391(17) _cell_angle_alpha 90 _cell_angle_beta 97.333(5) _cell_angle_gamma 90 _cell_volume 10630(10) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 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 0.0311 0.0180 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 0.0492 0.0322 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 0.3639 0.7018 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 = C108 H118 Cl7 N5 O11 # Dc = 1.19 Fooo = 3680.37 Mu = 21.70 M = 1910.32 # Found Formula = C106.48 H116.48 Cl2.45 N5 O11 # Dc = 1.08 FOOO = 3680.37 Mu = 10.97 M = 1729.39 _chemical_formula_sum 'C106.48 H116.48 Cl2.45 N5 O11' _chemical_formula_moiety ; C74 H78 N3 O2, C32 H38 N2 O9, 0.48(C H Cl3), Cl ; _chemical_compound_source ? _chemical_formula_weight 1729.39 _cell_measurement_reflns_used 29790 _cell_measurement_theta_min 2 _cell_measurement_theta_max 59 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.027 _exptl_crystal_size_mid 0.031 _exptl_crystal_size_max 0.061 _exptl_crystal_density_diffrn 1.080 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3680.370 _exptl_absorpt_coefficient_mu 1.097 # Sheldrick geometric approximatio 0.97 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku, 1997--2009)' _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.97 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator 'Si(1 1 1) double-crystal monochromator' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.68890 _diffrn_measurement_method \w-scans # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'CrystalClear (Rigaku, 1997--2009)' _computing_cell_refinement 'CrystalClear (Rigaku, 1997--2009)' _computing_data_reduction 'CrystalClear (Rigaku, 1997--2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 293 _diffrn_reflns_number 23420 _reflns_number_total 23420 _diffrn_reflns_av_R_equivalents 0.162 # Number of reflections without Friedels Law is 23420 # Number of reflections with Friedels Law is 23420 # Theoretical number of reflections is about 24299 _diffrn_reflns_theta_min 2.056 _diffrn_reflns_theta_max 89.546 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 51.937 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 40 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 38 _reflns_limit_l_min 0 _reflns_limit_l_max 40 _oxford_diffrn_Wilson_B_factor 2.07 _oxford_diffrn_Wilson_scale 117.97 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.76 _refine_diff_density_max 1.20 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 11241 _refine_ls_number_restraints 106 _refine_ls_number_parameters 1145 _oxford_refine_ls_R_factor_ref 0.1371 _refine_ls_wR_factor_ref 0.0616 _refine_ls_goodness_of_fit_ref 1.1455 _refine_ls_shift/su_max 0.0002792 _refine_ls_shift/su_mean 0.0000188 # The values computed from all data _oxford_reflns_number_all 23332 _refine_ls_R_factor_all 0.2083 _refine_ls_wR_factor_all 0.0895 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11241 _refine_ls_R_factor_gt 0.1371 _refine_ls_wR_factor_gt 0.0616 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: -0.120 -1.84 -1.03 -0.959 -0.189 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Rigaku Americas and Rigaku Corporation. (2009). CrystalClear (Version 2.0). Rigaku Americas, 9009 TX, USA 77381-5209. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cl1 Cl 0.72426(14) 0.39622(6) 0.64807(5) 0.0539 1.0000 Uani . . . . . . . O2 O 0.3339(4) 0.41842(15) 0.53153(12) 0.0507 1.0000 Uani . . . . . . . O4 O 0.4510(5) 0.48469(18) 0.75077(14) 0.0691 1.0000 Uani . . . . . . . C5 C 0.6459(5) 0.3105(2) 0.47489(17) 0.0401 1.0000 Uani . . . . . . . N6 N 0.5177(4) 0.40020(16) 0.56345(14) 0.0401 1.0000 Uani . . . . . . . C7 C 0.4527(5) 0.43890(19) 0.64315(18) 0.0391 1.0000 Uani . . . . . . . N8 N 0.2652(5) 0.49643(18) 0.63240(15) 0.0467 1.0000 Uani . . . . . . . O9 O 0.4205(5) 0.58611(17) 0.65002(15) 0.0681 1.0000 Uani . . . . . . . O10 O 0.0669(6) 0.5362(2) 0.71701(18) 0.0874 1.0000 Uani . . . . . . . O11 O 0.7391(4) 0.48779(18) 0.57023(15) 0.0694 1.0000 Uani . . . . . . . O12 O 0.1953(5) 0.3648(2) 0.66962(19) 0.0920 1.0000 Uani . . . . . . . C13 C 0.5146(5) 0.2383(2) 0.40925(17) 0.0406 1.0000 Uani . . . . . . . C14 C 0.4929(6) 0.4644(2) 0.72171(19) 0.0489 1.0000 Uani . . . . . . . C15 C 0.8147(5) 0.2949(2) 0.43295(16) 0.0409 1.0000 Uani . . . . . . . C16 C 0.4234(5) 0.46376(19) 0.67764(17) 0.0373 1.0000 Uani . . . . . . . C17 C 0.4440(6) 0.2454(2) 0.33273(19) 0.0470 1.0000 Uani . . . . . . . C18 C 0.5572(5) 0.37145(19) 0.53126(18) 0.0397 1.0000 Uani . . . . . . . C19 C 0.3273(5) 0.4912(2) 0.67180(18) 0.0436 1.0000 Uani . . . . . . . C20 C 0.4828(5) 0.3529(2) 0.49731(18) 0.0413 1.0000 Uani . . . . . . . C21 C 0.6135(5) 0.26396(19) 0.40624(17) 0.0376 1.0000 Uani . . . . . . . O22 O 0.0827(5) 0.4438(2) 0.68776(18) 0.0841 1.0000 Uani . . . . . . . N23 N 0.5979(4) 0.44528(17) 0.72587(15) 0.0446 1.0000 Uani . . . . . . . C24 C 1.1810(6) 0.3517(2) 0.84220(18) 0.0521 1.0000 Uani . . . . . . . C25 C 0.6849(6) 0.4448(2) 0.76347(18) 0.0451 1.0000 Uani . . . . . . . C26 C 0.4114(6) 0.4192(2) 0.56239(17) 0.0404 1.0000 Uani . . . . . . . N28 N 0.8013(5) 0.2908(2) 0.63826(18) 0.0601 1.0000 Uani . . . . . . . O29 O 0.8548(5) 0.4636(2) 0.47396(16) 0.0883 1.0000 Uani . . . . . . . C30 C 0.6735(5) 0.3605(2) 0.53664(19) 0.0446 1.0000 Uani . . . . . . . O31 O 0.8274(5) 0.21616(19) 0.65149(17) 0.0743 1.0000 Uani . . . . . . . O32 O 0.2711(6) 0.58696(19) 0.71959(18) 0.0832 1.0000 Uani . . . . . . . C33 C 0.7183(6) 0.3302(2) 0.5091(2) 0.0488 1.0000 Uani . . . . . . . C34 C 0.7464(5) 0.1916(2) 0.44881(19) 0.0460 1.0000 Uani . . . . . . . C35 C 0.5303(5) 0.3228(2) 0.46973(18) 0.0417 1.0000 Uani . . . . . . . C36 C 0.9144(5) 0.2689(2) 0.42911(19) 0.0458 1.0000 Uani . . . . . . . C37 C 0.2954(5) 0.4735(2) 0.59833(19) 0.0458 1.0000 Uani . . . . . . . C38 C 0.4304(5) 0.2293(2) 0.37440(17) 0.0418 1.0000 Uani . . . . . . . C39 C 0.7278(5) 0.2300(2) 0.47113(17) 0.0398 1.0000 Uani . . . . . . . C40 C 0.7015(5) 0.2751(2) 0.44664(18) 0.0425 1.0000 Uani . . . . . . . O41 O 0.5736(4) 0.2785(2) 0.60905(15) 0.0753 1.0000 Uani . . . . . . . C42 C 0.8682(6) 0.4159(2) 0.79662(19) 0.0479 1.0000 Uani . . . . . . . C43 C 0.7819(5) 0.1513(2) 0.4685(2) 0.0527 1.0000 Uani . . . . . . . N44 N 0.9134(5) 0.4439(2) 0.54356(18) 0.0599 1.0000 Uani . . . . . . . C45 C 1.0134(5) 0.2877(2) 0.4146(2) 0.0481 1.0000 Uani . . . . . . . C46 C 0.9686(5) 0.3142(3) 0.6031(2) 0.0522 1.0000 Uani . . . . . . . C47 C 0.7801(6) 0.4172(2) 0.76237(19) 0.0506 1.0000 Uani . . . . . . . C48 C 0.9734(5) 0.3587(2) 0.59020(18) 0.0487 1.0000 Uani . . . . . . . C49 C 1.0102(5) 0.3698(2) 0.5499(2) 0.0500 1.0000 Uani . . . . . . . C50 C 0.7404(6) 0.2267(2) 0.51600(19) 0.0498 1.0000 Uani . . . . . . . C51 C 0.6280(6) 0.2795(2) 0.36538(19) 0.0519 1.0000 Uani . . . . . . . C52 C 1.0791(6) 0.3721(2) 0.85177(18) 0.0484 1.0000 Uani . . . . . . . C53 C 0.9967(7) 0.3925(2) 0.9417(2) 0.0583 1.0000 Uani . . . . . . . C54 C 0.9162(7) 0.4073(2) 0.9079(2) 0.0602 1.0000 Uani . U . . . . . C55 C 0.9643(7) 0.3636(2) 0.9728(2) 0.0581 1.0000 Uani . . . . . . . C56 C 0.7343(7) 0.4880(3) 0.5252(2) 0.0607 1.0000 Uani . . . . . . . C57 C 0.3897(5) 0.4441(2) 0.60247(18) 0.0390 1.0000 Uani . . . . . . . C58 C 0.8222(6) 0.3398(2) 0.4224(2) 0.0540 1.0000 Uani . . . . . . . C59 C 0.5438(6) 0.2699(2) 0.32991(19) 0.0521 1.0000 Uani . . . . . . . C60 C 0.9990(6) 0.2806(3) 0.5767(2) 0.0639 1.0000 Uani . . . . . . . C61 C 1.0204(6) 0.3328(2) 0.40407(19) 0.0482 1.0000 Uani . . . . . . . C62 C 0.7957(6) 0.1488(3) 0.5137(2) 0.0607 1.0000 Uani . . . . . . . C63 C 0.8034(7) 0.3919(3) 0.9071(2) 0.0650 1.0000 Uani . . . . . . . C64 C 0.7727(6) 0.1866(3) 0.5367(2) 0.0585 1.0000 Uani . . . . . . . C65 C 0.6578(6) 0.5130(2) 0.5882(2) 0.0590 1.0000 Uani . . . . . . . C66 C 0.3559(6) 0.2353(2) 0.2930(2) 0.0579 1.0000 Uani . . . . . . . C67 C 0.7626(6) 0.2480(3) 0.6409(2) 0.0592 1.0000 Uani . . . . . . . C68 C 0.3853(6) 0.3107(2) 0.6011(2) 0.0604 1.0000 Uani . . . . . . . C69 C 0.6779(7) 0.5178(2) 0.6322(2) 0.0611 1.0000 Uani . . . . . . . C70 C 0.9220(6) 0.3580(2) 0.4082(2) 0.0597 1.0000 Uani . . . . . . . C71 C 0.4849(7) 0.5585(3) 0.5879(3) 0.0664 1.0000 Uani . . . . . . . C72 C 0.5053(7) 0.5626(2) 0.6310(2) 0.0588 1.0000 Uani . . . . . . . C73 C 0.9247(6) 0.3034(3) 0.6448(2) 0.0570 1.0000 Uani . . . . . . . C74 C 1.0410(6) 0.3346(3) 0.5245(2) 0.0636 1.0000 Uani . . . . . . . C75 C 0.4181(7) 0.2092(3) 0.2606(2) 0.0696 1.0000 Uani . . . . . . . C76 C 1.0764(6) 0.4172(3) 0.8614(2) 0.0669 1.0000 Uani . U . . . . . C77 C 0.8425(6) 0.4638(3) 0.5128(2) 0.0589 1.0000 Uani . . . . . . . C78 C 0.4858(7) 0.2982(2) 0.6282(2) 0.0579 1.0000 Uani . . . . . . . C79 C 0.6777(7) 0.4715(2) 0.7995(2) 0.0646 1.0000 Uani . . . . . . . C80 C 1.0347(7) 0.2903(3) 0.5376(2) 0.0734 1.0000 Uani . . . . . . . C81 C 1.2866(7) 0.3754(3) 0.8419(2) 0.0637 1.0000 Uani . . . . . . . C82 C 0.9603(7) 0.4381(2) 0.8729(2) 0.0636 1.0000 Uani . U . . . . . C83 C 0.8505(7) 0.3484(3) 0.9726(2) 0.0615 1.0000 Uani . . . . . . . C84 C 0.2521(6) 0.2079(3) 0.3039(2) 0.0678 1.0000 Uani . . . . . . . C85 C 1.1284(7) 0.3537(3) 0.3905(2) 0.0650 1.0000 Uani . . . . . . . C86 C 1.0153(6) 0.4174(3) 0.5355(2) 0.0686 1.0000 Uani . . . . . . . C87 C 0.5615(6) 0.5334(2) 0.5654(2) 0.0567 1.0000 Uani . . . . . . . C88 C 0.0941(7) 0.4060(3) 0.7164(2) 0.0711 1.0000 Uani . . . . . . . C89 C 1.4009(7) 0.3525(3) 0.8350(2) 0.0755 1.0000 Uani . . . . . . . C90 C 0.3116(7) 0.2802(3) 0.2728(2) 0.0790 1.0000 Uani . . . . . . . C91 C 0.1683(7) 0.5287(3) 0.6258(2) 0.0678 1.0000 Uani . . . . . . . C92 C 0.6330(7) 0.2413(3) 0.6301(2) 0.0677 1.0000 Uani . . . . . . . C93 C 0.2933(8) 0.3322(3) 0.6155(3) 0.0714 1.0000 Uani . . . . . . . C95 C 0.7725(6) 0.3627(3) 0.9389(2) 0.0688 1.0000 Uani . . . . . . . C96 C 0.6034(7) 0.5430(3) 0.6535(2) 0.0666 1.0000 Uani . . . . . . . C97 C 0.7675(7) 0.4688(3) 0.8335(2) 0.0715 1.0000 Uani . . . . . . . C98 C -0.0234(7) 0.4688(3) 0.6898(3) 0.0858 1.0000 Uani . . . . . . . C99 C 0.2057(10) 0.3819(3) 0.7107(3) 0.1020 1.0000 Uani . . . . . . . C101 C 0.8126(7) 0.3140(3) 1.0056(2) 0.0682 1.0000 Uani . . . . . . . C102 C 0.2986(7) 0.3432(3) 0.6573(3) 0.0750 1.0000 Uani . . . . . . . C103 C 1.4822(7) 0.3500(3) 0.8778(2) 0.0838 1.0000 Uani . . . . . . . C104 C 0.1766(10) 0.6033(3) 0.7379(3) 0.1014 1.0000 Uani . . . . . . . C105 C 0.3942(9) 0.3334(3) 0.6856(3) 0.0856 1.0000 Uani . . . . . . . C106 C 0.3463(9) 0.6212(3) 0.7089(3) 0.0886 1.0000 Uani . . . . . . . C107 C 0.9781(12) 0.4869(3) 0.8906(3) 0.1278 1.0000 Uani . U . . . . . C108 C 0.8652(6) 0.4413(2) 0.8326(2) 0.0534 1.0000 Uani . . . . . . . C109 C 0.4525(8) 0.6010(3) 0.6936(3) 0.0791 1.0000 Uani . . . . . . . C110 C 1.4657(8) 0.3801(3) 0.8037(3) 0.0919 1.0000 Uani . . . . . . . C111 C 1.3833(7) 0.3054(3) 0.8167(3) 0.0856 1.0000 Uani . . . . . . . C112 C 0.4952(8) 0.3102(3) 0.6709(3) 0.0770 1.0000 Uani . . . . . . . C113 C 1.1814(7) 0.4414(3) 0.8622(3) 0.0828 1.0000 Uani . U . . . . . C114 C 1.2824(8) 0.4197(3) 0.8524(3) 0.0824 1.0000 Uani . U . . . . . C115 C 0.9160(8) 0.3005(3) 1.0388(3) 0.0885 1.0000 Uani . . . . . . . C116 C 0.7691(9) 0.2703(3) 0.9827(3) 0.1098 1.0000 Uani . . . . . . . C117 C 1.1704(9) 0.3920(4) 0.4215(3) 0.1077 1.0000 Uani . . . . . . . C118 C 0.7191(10) 0.3345(4) 1.0272(3) 0.1148 1.0000 Uani . . . . . . . C119 C 1.2319(8) 0.3211(3) 0.3917(3) 0.0938 1.0000 Uani . . . . . . . C120 C 0.1080(10) 0.5636(4) 0.7525(3) 0.1084 1.0000 Uani . . . . . . . C121 C 1.1030(8) 0.3729(4) 0.3457(3) 0.1042 1.0000 Uani . . . . . . . C122 C -0.0080(9) 0.5024(3) 0.7276(3) 0.1043 1.0000 Uani . . . . . . . C123 C 1.0031(13) 0.5214(3) 0.8629(3) 0.1347 1.0000 Uani . U . . . . . C125 C 0.9637(13) 0.4985(3) 0.9326(3) 0.1348 1.0000 Uani . U . . . . . C128 C 0.9832(14) 0.5427(3) 0.9465(3) 0.1440 1.0000 Uani . U . . . . . C129 C 1.0208(14) 0.5744(3) 0.9177(3) 0.1489 1.0000 Uani . U . . . . . C130 C 1.0221(14) 0.5648(3) 0.8758(3) 0.1433 1.0000 Uani . U . . . . . H71 H 0.5198 0.4183 0.6472 0.0450 1.0000 Uiso R . . . . . . H131 H 0.5044 0.2260 0.4370 0.0449 1.0000 Uiso R . . . . . . H191 H 0.3013 0.5073 0.6961 0.0434 1.0000 Uiso R . . . . . . H201 H 0.4020 0.3605 0.4935 0.0462 1.0000 Uiso R . . . . . . H241 H 1.1794 0.3196 0.8347 0.0578 1.0000 Uiso R . . . . . . H301 H 0.7258 0.3744 0.5592 0.0518 1.0000 Uiso R . . . . . . H331 H 0.8004 0.3223 0.5132 0.0507 1.0000 Uiso R . . . . . . H341 H 0.7389 0.1924 0.4175 0.0504 1.0000 Uiso R . . . . . . H351 H 0.4795 0.3107 0.4458 0.0444 1.0000 Uiso R . . . . . . H361 H 0.9128 0.2376 0.4360 0.0501 1.0000 Uiso R . . . . . . H371 H 0.2480 0.4781 0.5702 0.0510 1.0000 Uiso R . . . . . . H381 H 0.3621 0.2117 0.3784 0.0473 1.0000 Uiso R . . . . . . H421 H 0.9346 0.3961 0.7951 0.0494 1.0000 Uiso R . . . . . . H431 H 0.7933 0.1254 0.4518 0.0568 1.0000 Uiso R . . . . . . H451 H 1.0812 0.2684 0.4124 0.0549 1.0000 Uiso R . . . . . . H471 H 0.7867 0.3990 0.7376 0.0565 1.0000 Uiso R . . . . . . H481 H 0.9505 0.3819 0.6088 0.0563 1.0000 Uiso R . . . . . . H501 H 0.7274 0.2532 0.5325 0.0591 1.0000 Uiso R . . . . . . H511 H 0.6964 0.2971 0.3611 0.0595 1.0000 Uiso R . . . . . . H521 H 1.0084 0.3546 0.8513 0.0579 1.0000 Uiso R . . . . . . H531 H 1.0803 0.4027 0.9429 0.0625 1.0000 Uiso R . . . . . . H551 H 1.0254 0.3532 0.9953 0.0602 1.0000 Uiso R . . . . . . H561 H 0.7321 0.5179 0.5145 0.0673 1.0000 Uiso R . . . . . . H562 H 0.6640 0.4727 0.5121 0.0673 1.0000 Uiso R . . . . . . H581 H 0.7545 0.3587 0.4237 0.0620 1.0000 Uiso R . . . . . . H591 H 0.5577 0.2810 0.3018 0.0596 1.0000 Uiso R . . . . . . H601 H 0.9954 0.2494 0.5857 0.0659 1.0000 Uiso R . . . . . . H621 H 0.8186 0.1206 0.5275 0.0667 1.0000 Uiso R . . . . . . H631 H 0.7434 0.4018 0.8845 0.0719 1.0000 Uiso R . . . . . . H641 H 0.7805 0.1848 0.5675 0.0646 1.0000 Uiso R . . . . . . H681 H 0.3806 0.3044 0.5701 0.0632 1.0000 Uiso R . . . . . . H691 H 0.7462 0.5036 0.6484 0.0647 1.0000 Uiso R . . . . . . H701 H 0.9226 0.3895 0.4022 0.0609 1.0000 Uiso R . . . . . . H711 H 0.4167 0.5712 0.5716 0.0714 1.0000 Uiso R . . . . . . H731 H 0.9333 0.3292 0.6632 0.0675 1.0000 Uiso R . . . . . . H732 H 0.9693 0.2793 0.6588 0.0675 1.0000 Uiso R . . . . . . H741 H 1.0692 0.3421 0.4974 0.0666 1.0000 Uiso R . . . . . . H751 H 0.3655 0.2020 0.2356 0.0705 1.0000 Uiso R . . . . . . H752 H 0.4829 0.2258 0.2520 0.0705 1.0000 Uiso R . . . . . . H753 H 0.4494 0.1811 0.2730 0.0705 1.0000 Uiso R . . . . . . H791 H 0.6130 0.4911 0.8009 0.0748 1.0000 Uiso R . . . . . . H801 H 1.0565 0.2666 0.5185 0.0765 1.0000 Uiso R . . . . . . H841 H 0.1993 0.2022 0.2790 0.0714 1.0000 Uiso R . . . . . . H842 H 0.2117 0.2243 0.3241 0.0714 1.0000 Uiso R . . . . . . H843 H 0.2778 0.1800 0.3171 0.0714 1.0000 Uiso R . . . . . . H861 H 1.0829 0.4313 0.5491 0.0775 1.0000 Uiso R . . . . . . H862 H 1.0173 0.4175 0.5047 0.0775 1.0000 Uiso R . . . . . . H871 H 0.5451 0.5297 0.5336 0.0626 1.0000 Uiso R . . . . . . H881 H 0.0986 0.4153 0.7458 0.0808 1.0000 Uiso R . . . . . . H882 H 0.0312 0.3851 0.7107 0.0808 1.0000 Uiso R . . . . . . H911 H 0.1341 0.5289 0.5970 0.0758 1.0000 Uiso R . . . . . . H912 H 0.1970 0.5585 0.6336 0.0758 1.0000 Uiso R . . . . . . H913 H 0.1104 0.5213 0.6440 0.0758 1.0000 Uiso R . . . . . . H921 H 0.6007 0.2343 0.6555 0.0773 1.0000 Uiso R . . . . . . H922 H 0.6211 0.2152 0.6111 0.0773 1.0000 Uiso R . . . . . . H931 H 0.2219 0.3390 0.5960 0.0736 1.0000 Uiso R . . . . . . H951 H 0.6925 0.3514 0.9365 0.0757 1.0000 Uiso R . . . . . . H961 H 0.6166 0.5463 0.6843 0.0682 1.0000 Uiso R . . . . . . H971 H 0.7630 0.4870 0.8593 0.0763 1.0000 Uiso R . . . . . . H981 H -0.0403 0.4861 0.6634 0.0992 1.0000 Uiso R . . . . . . H982 H -0.0879 0.4494 0.6919 0.0992 1.0000 Uiso R . . . . . . H991 H 0.2670 0.4032 0.7156 0.0876 1.0000 Uiso R . . . . . . H992 H 0.2172 0.3585 0.7314 0.0876 1.0000 Uiso R . . . . . . H1031 H 1.5548 0.3355 0.8747 0.0872 1.0000 Uiso R . . . . . . H1032 H 1.4989 0.3797 0.8888 0.0872 1.0000 Uiso R . . . . . . H1033 H 1.4453 0.3336 0.8989 0.0872 1.0000 Uiso R . . . . . . H1041 H 0.1990 0.6243 0.7609 0.1145 1.0000 Uiso R . . . . . . H1042 H 0.1242 0.6202 0.7164 0.1145 1.0000 Uiso R . . . . . . H1051 H 0.3911 0.3437 0.7147 0.0883 1.0000 Uiso R . . . . . . H1061 H 0.3676 0.6411 0.7328 0.0937 1.0000 Uiso R . . . . . . H1062 H 0.3064 0.6392 0.6858 0.0937 1.0000 Uiso R . . . . . . H1091 H 0.5156 0.6222 0.6960 0.0831 1.0000 Uiso R . . . . . . H1092 H 0.4778 0.5759 0.7127 0.0831 1.0000 Uiso R . . . . . . H1101 H 1.5383 0.3651 0.7990 0.1020 1.0000 Uiso R . . . . . . H1102 H 1.4854 0.4088 0.8157 0.1020 1.0000 Uiso R . . . . . . H1103 H 1.4192 0.3833 0.7768 0.1020 1.0000 Uiso R . . . . . . H1111 H 1.4578 0.2911 0.8125 0.0899 1.0000 Uiso R . . . . . . H1112 H 1.3481 0.2861 0.8362 0.0899 1.0000 Uiso R . . . . . . H1113 H 1.3354 0.3051 0.7898 0.0899 1.0000 Uiso R . . . . . . H1121 H 0.5669 0.3044 0.6898 0.0831 1.0000 Uiso R . . . . . . H1131 H 1.1870 0.4734 0.8684 0.0924 1.0000 Uiso R . . . . . . H1141 H 1.3551 0.4378 0.8540 0.0901 1.0000 Uiso R . . . . . . H1151 H 0.8929 0.2793 1.0596 0.0931 1.0000 Uiso R . . . . . . H1152 H 0.9489 0.3264 1.0554 0.0931 1.0000 Uiso R . . . . . . H1153 H 0.9790 0.2871 1.0261 0.0931 1.0000 Uiso R . . . . . . H1161 H 0.7461 0.2482 1.0030 0.1108 1.0000 Uiso R . . . . . . H1162 H 0.8290 0.2563 0.9684 0.1108 1.0000 Uiso R . . . . . . H1163 H 0.7026 0.2755 0.9619 0.1108 1.0000 Uiso R . . . . . . H1171 H 1.2391 0.4066 0.4136 0.1206 1.0000 Uiso R . . . . . . H1172 H 1.1888 0.3803 0.4498 0.1206 1.0000 Uiso R . . . . . . H1173 H 1.1107 0.4146 0.4220 0.1206 1.0000 Uiso R . . . . . . H1181 H 0.6972 0.3124 1.0487 0.1200 1.0000 Uiso R . . . . . . H1182 H 0.7473 0.3602 1.0430 0.1200 1.0000 Uiso R . . . . . . H1183 H 0.6543 0.3403 1.0079 0.1200 1.0000 Uiso R . . . . . . H1191 H 1.2982 0.3352 0.3821 0.1027 1.0000 Uiso R . . . . . . H1192 H 1.2517 0.3090 0.4192 0.1027 1.0000 Uiso R . . . . . . H1193 H 1.2093 0.2961 0.3719 0.1027 1.0000 Uiso R . . . . . . H1201 H 0.1596 0.5466 0.7727 0.1083 1.0000 Uiso R . . . . . . H1202 H 0.0439 0.5740 0.7671 0.1083 1.0000 Uiso R . . . . . . H1211 H 1.1702 0.3870 0.3366 0.1117 1.0000 Uiso R . . . . . . H1212 H 1.0419 0.3954 0.3450 0.1117 1.0000 Uiso R . . . . . . H1213 H 1.0764 0.3498 0.3261 0.1117 1.0000 Uiso R . . . . . . H1221 H 0.0262 0.4869 0.7529 0.1123 1.0000 Uiso R . . . . . . H1222 H -0.0822 0.5143 0.7330 0.1123 1.0000 Uiso R . . . . . . H1231 H 1.0072 0.5129 0.8324 0.1071 1.0000 Uiso R . . . . . . H1251 H 0.9515 0.4741 0.9523 0.1239 1.0000 Uiso R . . . . . . H1281 H 0.9517 0.5506 0.9728 0.2028 1.0000 Uiso R . . . . . . H1291 H 1.0518 0.6031 0.9308 0.2214 1.0000 Uiso R . . . . . . H1301 H 1.0391 0.5872 0.8548 0.1737 1.0000 Uiso R . . . . . . H231 H 0.6181 0.4311 0.7034 0.0464 1.0000 Uiso R . . . . . . H61 H 0.5668 0.4052 0.5860 0.0436 1.0000 Uiso R . . . . . . H441 H 0.9000 0.4478 0.5698 0.0626 1.0000 Uiso R . . . . . . H281 H 0.7503 0.3113 0.6314 0.0671 1.0000 Uiso R . . . . . . Cl202 Cl 0.3388(10) 0.1844(3) 0.6590(4) 0.2482 0.484(9) Uani D . P . 1 . . Cl203 Cl 0.1658(10) 0.2222(3) 0.7016(4) 0.2544 0.484(9) Uani D . P . 1 . . Cl204 Cl 0.1390(11) 0.1341(3) 0.6677(4) 0.2789 0.484(9) Uani D . P . 1 . . C201 C 0.1862(13) 0.1885(4) 0.6574(5) 0.2584 0.484(9) Uani D . P . 1 . . H2011 H 0.1504 0.2001 0.6308 0.3169 0.484(9) Uiso R . P . 1 . . H901 H 0.2568 0.2742 0.2481 0.0963 1.0000 Uiso R . . . . . . H902 H 0.2743 0.2970 0.2929 0.0963 1.0000 Uiso R . . . . . . H903 H 0.3753 0.2971 0.2646 0.0963 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 Cl1 0.0489(10) 0.0664(10) 0.0449(8) -0.0125(7) 0.0002(7) 0.0146(8) O2 0.047(3) 0.067(3) 0.037(2) -0.007(2) 0.003(2) 0.020(2) O4 0.076(4) 0.089(4) 0.042(3) -0.009(2) 0.005(2) 0.028(3) C5 0.034(4) 0.051(4) 0.036(3) -0.005(3) 0.005(2) 0.004(3) N6 0.032(3) 0.050(3) 0.036(2) -0.006(2) -0.004(2) 0.014(2) C7 0.039(4) 0.037(3) 0.042(3) 0.003(3) 0.009(3) 0.005(3) N8 0.048(3) 0.053(3) 0.041(3) 0.009(2) 0.013(2) 0.019(3) O9 0.083(4) 0.063(3) 0.062(3) -0.003(2) 0.021(3) -0.001(3) O10 0.113(5) 0.082(4) 0.072(4) -0.008(3) 0.032(3) -0.010(4) O11 0.066(3) 0.092(4) 0.052(3) 0.021(3) 0.015(2) 0.024(3) O12 0.079(4) 0.112(5) 0.077(4) -0.010(3) -0.020(3) 0.009(4) C13 0.048(4) 0.044(3) 0.029(3) 0.000(2) -0.001(3) 0.008(3) C14 0.060(5) 0.050(4) 0.038(3) 0.005(3) 0.012(3) 0.009(3) C15 0.041(4) 0.056(4) 0.025(3) -0.005(3) 0.001(2) 0.001(3) C16 0.033(3) 0.042(3) 0.039(3) 0.004(3) 0.012(2) 0.008(3) C17 0.045(4) 0.056(4) 0.039(3) 0.002(3) 0.002(3) 0.007(3) C18 0.037(4) 0.040(3) 0.041(3) 0.000(3) 0.002(3) 0.004(3) C19 0.049(4) 0.048(4) 0.037(3) 0.000(3) 0.020(3) -0.003(3) C20 0.032(3) 0.046(4) 0.045(3) -0.006(3) -0.001(3) 0.008(3) C21 0.036(4) 0.043(3) 0.034(3) -0.006(2) 0.005(2) 0.014(3) O22 0.084(4) 0.090(4) 0.082(4) 0.002(3) 0.023(3) 0.003(3) N23 0.048(3) 0.051(3) 0.034(3) -0.004(2) 0.006(2) 0.012(3) C24 0.057(5) 0.067(4) 0.031(3) 0.008(3) 0.002(3) -0.013(4) C25 0.053(4) 0.044(4) 0.037(3) 0.011(3) 0.000(3) -0.002(3) C26 0.052(4) 0.040(3) 0.029(3) 0.003(2) 0.007(3) 0.006(3) N28 0.055(4) 0.064(4) 0.061(4) 0.006(3) 0.007(3) 0.018(3) O29 0.097(4) 0.119(5) 0.050(3) 0.016(3) 0.015(3) 0.047(4) C30 0.037(4) 0.051(4) 0.044(3) -0.012(3) -0.001(3) 0.005(3) O31 0.065(4) 0.074(4) 0.083(4) 0.008(3) 0.005(3) 0.020(3) O32 0.116(5) 0.067(4) 0.075(4) -0.007(3) 0.044(3) 0.006(3) C33 0.041(4) 0.052(4) 0.051(4) -0.010(3) -0.004(3) 0.023(3) C34 0.043(4) 0.056(4) 0.040(3) 0.008(3) 0.013(3) 0.011(3) C35 0.043(4) 0.046(4) 0.035(3) 0.000(3) -0.003(3) -0.002(3) C36 0.038(4) 0.050(4) 0.049(4) -0.005(3) 0.006(3) 0.020(3) C37 0.040(4) 0.059(4) 0.039(3) 0.005(3) 0.007(3) -0.002(3) C38 0.038(4) 0.047(4) 0.041(3) -0.002(3) 0.006(3) 0.011(3) C39 0.036(3) 0.049(4) 0.032(3) -0.005(3) -0.003(2) 0.013(3) C40 0.035(4) 0.050(4) 0.040(3) -0.001(3) -0.006(3) 0.005(3) O41 0.058(3) 0.111(4) 0.059(3) 0.014(3) 0.015(2) 0.026(3) C42 0.053(4) 0.046(4) 0.043(3) 0.000(3) 0.000(3) -0.003(3) C43 0.039(4) 0.068(5) 0.051(4) -0.005(3) 0.007(3) -0.001(3) N44 0.049(4) 0.082(4) 0.048(3) 0.010(3) 0.004(3) -0.001(3) C45 0.033(4) 0.061(4) 0.052(4) -0.002(3) 0.012(3) 0.013(3) C46 0.035(4) 0.076(5) 0.046(4) -0.002(3) 0.005(3) 0.021(3) C47 0.062(4) 0.051(4) 0.037(3) -0.001(3) 0.002(3) 0.010(3) C48 0.033(4) 0.077(5) 0.032(3) -0.006(3) -0.008(3) 0.011(3) C49 0.029(4) 0.075(5) 0.044(4) 0.006(3) -0.002(3) 0.006(3) C50 0.049(4) 0.057(4) 0.042(3) -0.003(3) 0.001(3) 0.011(3) C51 0.050(4) 0.061(4) 0.045(4) 0.004(3) 0.007(3) 0.003(3) C52 0.058(5) 0.047(4) 0.038(3) 0.004(3) -0.001(3) -0.013(3) C53 0.063(5) 0.059(4) 0.050(4) 0.003(3) -0.004(3) -0.004(4) C54 0.065(5) 0.067(3) 0.044(4) -0.011(3) -0.008(3) 0.005(3) C55 0.062(5) 0.063(5) 0.046(4) -0.012(3) -0.004(3) 0.003(4) C56 0.070(5) 0.067(5) 0.044(4) 0.011(3) 0.004(3) 0.016(4) C57 0.031(3) 0.046(3) 0.041(3) 0.005(3) 0.007(2) 0.005(3) C58 0.042(4) 0.054(4) 0.065(4) -0.001(3) 0.004(3) 0.010(3) C59 0.060(5) 0.062(4) 0.036(3) 0.007(3) 0.009(3) 0.003(4) C60 0.050(5) 0.080(5) 0.059(4) -0.004(4) -0.001(3) 0.016(4) C61 0.041(4) 0.063(4) 0.040(3) 0.003(3) 0.000(3) 0.010(3) C62 0.070(5) 0.065(5) 0.044(4) 0.015(3) -0.004(3) 0.010(4) C63 0.063(5) 0.085(6) 0.042(4) -0.005(4) -0.010(3) 0.003(4) C64 0.061(5) 0.073(5) 0.041(4) 0.000(3) 0.002(3) 0.021(4) C65 0.063(5) 0.062(5) 0.052(4) 0.015(3) 0.007(4) 0.004(4) C66 0.057(5) 0.066(5) 0.045(4) 0.004(3) -0.013(3) -0.002(4) C67 0.057(5) 0.082(6) 0.041(4) -0.010(4) 0.014(3) 0.015(4) C68 0.050(5) 0.069(5) 0.062(4) -0.003(4) 0.008(4) 0.000(4) C69 0.064(5) 0.064(5) 0.058(4) 0.020(4) 0.017(4) 0.014(4) C70 0.056(5) 0.050(4) 0.071(5) 0.013(3) 0.003(4) 0.005(4) C71 0.059(5) 0.058(5) 0.082(6) 0.019(4) 0.010(4) 0.011(4) C72 0.075(5) 0.060(4) 0.046(4) 0.002(3) 0.025(4) -0.009(4) C73 0.052(5) 0.072(5) 0.046(4) 0.009(3) 0.004(3) 0.021(4) C74 0.035(4) 0.111(7) 0.044(4) -0.005(4) 0.003(3) 0.010(4) C75 0.080(6) 0.083(6) 0.042(4) -0.005(4) -0.005(4) -0.012(4) C76 0.047(5) 0.100(5) 0.048(4) 0.022(3) -0.016(3) -0.018(4) C77 0.056(5) 0.070(5) 0.050(4) 0.011(3) 0.004(3) 0.003(4) C78 0.062(5) 0.065(5) 0.049(4) 0.003(3) 0.015(3) -0.003(4) C79 0.090(6) 0.058(4) 0.041(4) -0.007(3) -0.009(4) 0.026(4) C80 0.067(5) 0.095(7) 0.056(5) -0.020(4) 0.000(4) 0.019(5) C81 0.061(5) 0.077(5) 0.048(4) 0.021(4) -0.012(3) -0.013(4) C82 0.074(5) 0.064(3) 0.045(4) -0.007(2) -0.021(3) -0.017(4) C83 0.059(5) 0.082(5) 0.041(4) -0.009(3) -0.004(3) -0.007(4) C84 0.056(5) 0.095(6) 0.046(4) -0.010(4) -0.014(3) 0.004(4) C85 0.056(5) 0.076(5) 0.063(5) 0.002(4) 0.005(4) 0.011(4) C86 0.035(4) 0.105(6) 0.068(5) 0.017(4) 0.014(3) 0.013(4) C87 0.057(5) 0.066(5) 0.048(4) 0.014(3) 0.008(3) -0.001(4) C88 0.070(5) 0.084(6) 0.061(5) 0.010(4) 0.018(4) 0.001(5) C89 0.051(5) 0.117(7) 0.058(5) 0.027(5) 0.006(4) -0.015(5) C90 0.080(6) 0.087(6) 0.063(5) 0.012(4) -0.019(4) 0.005(5) C91 0.071(5) 0.080(5) 0.054(4) -0.002(4) 0.015(4) 0.044(4) C92 0.066(5) 0.072(5) 0.069(5) -0.001(4) 0.019(4) -0.005(4) C93 0.074(6) 0.065(5) 0.079(6) 0.000(4) 0.026(4) 0.000(4) C95 0.040(4) 0.106(6) 0.058(4) -0.007(4) -0.002(3) -0.006(4) C96 0.084(6) 0.061(5) 0.055(4) 0.017(4) 0.009(4) 0.002(4) C97 0.096(6) 0.061(5) 0.052(4) -0.019(3) -0.011(4) 0.013(4) C98 0.043(5) 0.091(6) 0.124(8) -0.004(6) 0.013(5) 0.012(4) C99 0.152(10) 0.085(7) 0.066(6) 0.002(5) 0.001(6) -0.034(7) C101 0.052(5) 0.096(6) 0.055(4) -0.007(4) 0.003(4) -0.017(4) C102 0.056(5) 0.067(5) 0.103(7) 0.017(5) 0.013(5) 0.016(4) C103 0.056(5) 0.135(8) 0.056(5) 0.015(5) -0.007(4) -0.001(5) C104 0.142(9) 0.085(7) 0.087(6) -0.019(5) 0.052(6) 0.008(7) C105 0.113(8) 0.076(6) 0.076(6) -0.005(5) 0.044(6) 0.006(6) C106 0.125(8) 0.075(6) 0.071(5) -0.011(5) 0.033(5) -0.007(6) C107 0.261(7) 0.050(2) 0.058(3) -0.0074(19) -0.035(4) -0.008(3) C108 0.068(5) 0.040(4) 0.050(4) 0.004(3) -0.001(3) 0.003(3) C109 0.099(7) 0.061(5) 0.081(6) -0.024(4) 0.023(5) -0.001(5) C110 0.103(7) 0.111(7) 0.061(5) 0.015(5) 0.008(5) -0.027(6) C111 0.056(5) 0.114(8) 0.085(6) 0.011(5) -0.001(4) 0.001(5) C112 0.081(6) 0.086(6) 0.061(5) 0.010(4) -0.006(4) -0.002(5) C113 0.066(4) 0.073(5) 0.103(5) 0.015(4) -0.013(4) -0.026(4) C114 0.061(4) 0.078(5) 0.102(5) 0.015(4) -0.014(4) -0.027(4) C115 0.086(7) 0.089(6) 0.089(6) 0.021(5) 0.008(5) -0.023(5) C116 0.122(9) 0.113(8) 0.099(7) -0.024(6) 0.030(6) -0.061(7) C117 0.097(8) 0.128(9) 0.102(7) -0.010(7) 0.025(6) -0.027(7) C118 0.126(9) 0.143(10) 0.078(6) -0.006(6) 0.023(6) 0.000(8) C119 0.069(6) 0.098(7) 0.115(8) 0.028(6) 0.013(5) 0.001(5) C120 0.121(9) 0.132(9) 0.082(6) -0.025(6) 0.050(6) -0.031(7) C121 0.074(6) 0.157(10) 0.080(6) 0.039(6) 0.007(5) 0.021(6) C122 0.116(8) 0.097(7) 0.113(8) -0.023(6) 0.063(7) -0.007(6) C123 0.268(7) 0.055(2) 0.068(3) -0.007(2) -0.031(4) -0.020(4) C125 0.275(7) 0.056(3) 0.059(3) -0.012(2) -0.035(4) -0.009(4) C128 0.289(7) 0.060(3) 0.070(3) -0.018(2) -0.030(4) -0.015(4) C129 0.292(7) 0.060(3) 0.081(3) -0.016(2) -0.029(4) -0.022(4) C130 0.282(7) 0.057(2) 0.078(3) -0.009(2) -0.030(4) -0.025(4) Cl202 0.313(11) 0.206(8) 0.261(10) 0.117(7) 0.175(8) 0.064(7) Cl203 0.295(11) 0.216(8) 0.290(10) 0.145(7) 0.182(8) 0.110(7) Cl204 0.340(11) 0.225(8) 0.298(10) 0.141(8) 0.141(9) 0.092(8) C201 0.315(10) 0.215(8) 0.278(10) 0.138(7) 0.165(8) 0.092(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1722(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 O2 . C26 . 1.230(7) yes O4 . C14 . 1.240(7) yes C5 . C33 . 1.400(8) yes C5 . C35 . 1.368(8) yes C5 . C40 . 1.562(8) yes N6 . C18 . 1.440(7) yes N6 . C26 . 1.343(7) yes N6 . H61 . 0.860 no C7 . C16 . 1.387(8) yes C7 . C57 . 1.394(8) yes C7 . H71 . 0.980 no N8 . C19 . 1.356(8) yes N8 . C37 . 1.350(8) yes N8 . C91 . 1.463(8) yes O9 . C72 . 1.393(8) yes O9 . C109 . 1.442(9) yes O10 . C120 . 1.411(10) yes O10 . C122 . 1.390(10) yes O11 . C56 . 1.406(8) yes O11 . C65 . 1.373(8) yes O12 . C99 . 1.376(10) yes O12 . C102 . 1.444(10) yes C13 . C21 . 1.382(8) yes C13 . C38 . 1.391(8) yes C13 . H131 . 0.966 no C14 . C16 . 1.507(8) yes C14 . N23 . 1.326(8) yes C15 . C36 . 1.400(8) yes C15 . C40 . 1.539(9) yes C15 . C58 . 1.380(9) yes C16 . C19 . 1.365(8) yes C17 . C38 . 1.421(8) yes C17 . C59 . 1.371(9) yes C17 . C66 . 1.532(8) yes C18 . C20 . 1.393(8) yes C18 . C30 . 1.366(8) yes C19 . H191 . 0.981 no C20 . C35 . 1.402(8) yes C20 . H201 . 0.949 no C21 . C40 . 1.554(8) yes C21 . C51 . 1.393(8) yes O22 . C88 . 1.434(9) yes O22 . C98 . 1.436(9) yes N23 . C25 . 1.447(7) yes N23 . H231 . 0.877 no C24 . C52 . 1.386(9) yes C24 . C81 . 1.404(10) yes C24 . H241 . 0.982 no C25 . C47 . 1.372(9) yes C25 . C79 . 1.390(9) yes C26 . C57 . 1.507(8) yes N28 . C67 . 1.354(10) yes N28 . C73 . 1.457(9) yes N28 . H281 . 0.854 no O29 . C77 . 1.245(8) yes C30 . C33 . 1.392(8) yes C30 . H301 . 0.960 no O31 . C67 . 1.223(8) yes O32 . C104 . 1.380(10) yes O32 . C106 . 1.402(10) yes C33 . H331 . 0.966 no C34 . C39 . 1.369(8) yes C34 . C43 . 1.386(9) yes C34 . H341 . 0.976 no C35 . H351 . 0.961 no C36 . C45 . 1.395(9) yes C36 . H361 . 0.954 no C37 . C57 . 1.386(8) yes C37 . H371 . 0.986 no C38 . H381 . 0.964 no C39 . C40 . 1.555(8) yes C39 . C50 . 1.401(8) yes O41 . C78 . 1.370(8) yes O41 . C92 . 1.419(9) yes C42 . C47 . 1.380(8) yes C42 . C108 . 1.361(9) yes C42 . H421 . 0.971 no C43 . C62 . 1.408(9) yes C43 . H431 . 0.949 no N44 . C77 . 1.321(8) yes N44 . C86 . 1.460(9) yes N44 . H441 . 0.865 no C45 . C61 . 1.385(9) yes C45 . H451 . 0.976 no C46 . C48 . 1.385(10) yes C46 . C60 . 1.370(10) yes C46 . C73 . 1.496(9) yes C47 . H471 . 0.959 no C48 . C49 . 1.421(9) yes C48 . H481 . 0.961 no C49 . C74 . 1.387(10) yes C49 . C86 . 1.487(10) yes C50 . C64 . 1.385(9) yes C50 . H501 . 0.962 no C51 . C59 . 1.408(9) yes C51 . H511 . 0.969 no C52 . C76 . 1.375(10) yes C52 . H521 . 0.963 no C53 . C54 . 1.386(9) yes C53 . C55 . 1.387(10) yes C53 . H531 . 1.005 no C54 . C63 . 1.373(10) yes C54 . C82 . 1.564(10) yes C55 . C83 . 1.383(10) yes C55 . H551 . 0.981 no C56 . C77 . 1.530(10) yes C56 . H561 . 0.949 no C56 . H562 . 0.972 no C58 . C70 . 1.392(10) yes C58 . H581 . 0.964 no C59 . H591 . 0.974 no C60 . C80 . 1.375(10) yes C60 . H601 . 0.968 no C61 . C70 . 1.376(9) yes C61 . C85 . 1.498(10) yes C62 . C64 . 1.377(10) yes C62 . H621 . 0.966 no C63 . C95 . 1.399(10) yes C63 . H631 . 0.971 no C64 . H641 . 0.962 no C65 . C69 . 1.380(10) yes C65 . C87 . 1.379(9) yes C66 . C75 . 1.529(10) yes C66 . C84 . 1.520(10) yes C66 . C90 . 1.537(10) yes C67 . C92 . 1.499(10) yes C68 . C78 . 1.394(10) yes C68 . C93 . 1.362(10) yes C68 . H681 . 0.985 no C69 . C96 . 1.373(10) yes C69 . H691 . 0.975 no C70 . H701 . 0.956 no C71 . C72 . 1.351(10) yes C71 . C87 . 1.410(10) yes C71 . H711 . 0.957 no C72 . C96 . 1.381(10) yes C73 . H731 . 0.958 no C73 . H732 . 0.956 no C74 . C80 . 1.385(11) yes C74 . H741 . 0.975 no C75 . H751 . 0.950 no C75 . H752 . 0.960 no C75 . H753 . 0.971 no C76 . C82 . 1.556(11) yes C76 . C113 . 1.402(10) yes C78 . C112 . 1.378(10) yes C79 . C97 . 1.390(10) yes C79 . H791 . 0.951 no C80 . H801 . 0.977 no C81 . C89 . 1.519(11) yes C81 . C114 . 1.360(11) yes C82 . C107 . 1.557(11) yes C82 . C108 . 1.567(9) yes C83 . C95 . 1.366(10) yes C83 . C101 . 1.556(11) yes C84 . H841 . 0.942 no C84 . H842 . 0.965 no C84 . H843 . 0.957 no C85 . C117 . 1.533(12) yes C85 . C119 . 1.533(11) yes C85 . C121 . 1.512(11) yes C86 . H861 . 0.933 no C86 . H862 . 0.971 no C87 . H871 . 0.997 no C88 . C99 . 1.501(13) yes C88 . H881 . 0.958 no C88 . H882 . 0.954 no C89 . C103 . 1.537(10) yes C89 . C110 . 1.543(10) yes C89 . C111 . 1.514(12) yes C90 . H901 . 0.950 no C90 . H902 . 0.950 no C90 . H903 . 0.950 no C91 . H911 . 0.940 no C91 . H912 . 0.967 no C91 . H913 . 0.956 no C92 . H921 . 0.945 no C92 . H922 . 0.976 no C93 . C102 . 1.346(11) yes C93 . H931 . 0.981 no C95 . H951 . 0.973 no C96 . H961 . 0.965 no C97 . C108 . 1.393(10) yes C97 . H971 . 0.979 no C98 . C122 . 1.544(12) yes C98 . H981 . 0.971 no C98 . H982 . 0.947 no C99 . H991 . 0.945 no C99 . H992 . 0.949 no C101 . C115 . 1.531(11) yes C101 . C116 . 1.535(11) yes C101 . C118 . 1.474(12) yes C102 . C105 . 1.354(12) yes C103 . H1031 . 0.955 no C103 . H1032 . 0.958 no C103 . H1033 . 0.963 no C104 . C120 . 1.523(13) yes C104 . H1041 . 0.964 no C104 . H1042 . 0.984 no C105 . C112 . 1.474(12) yes C105 . H1051 . 0.968 no C106 . C109 . 1.492(11) yes C106 . H1061 . 0.962 no C106 . H1062 . 0.967 no C107 . C123 . 1.397(13) yes C107 . C125 . 1.393(13) yes C109 . H1091 . 0.955 no C109 . H1092 . 0.977 no C110 . H1101 . 0.974 no C110 . H1102 . 0.947 no C110 . H1103 . 0.944 no C111 . H1111 . 0.981 no C111 . H1112 . 0.965 no C111 . H1113 . 0.947 no C112 . H1121 . 0.969 no C113 . C114 . 1.396(12) yes C113 . H1131 . 0.970 no C114 . H1141 . 0.990 no C115 . H1151 . 0.969 no C115 . H1152 . 0.977 no C115 . H1153 . 0.957 no C116 . H1161 . 0.973 no C116 . H1162 . 0.963 no C116 . H1163 . 0.953 no C117 . H1171 . 0.961 no C117 . H1172 . 0.954 no C117 . H1173 . 0.962 no C118 . H1181 . 0.997 no C118 . H1182 . 0.947 no C118 . H1183 . 0.914 no C119 . H1191 . 0.951 no C119 . H1192 . 0.936 no C119 . H1193 . 0.981 no C120 . H1201 . 0.955 no C120 . H1202 . 0.967 no C121 . H1211 . 0.954 no C121 . H1212 . 0.967 no C121 . H1213 . 0.948 no C122 . H1221 . 0.959 no C122 . H1222 . 0.958 no C123 . C130 . 1.361(12) yes C123 . H1231 . 0.995 no C125 . C128 . 1.392(12) yes C125 . H1251 . 0.974 no C128 . C129 . 1.410(16) yes C128 . H1281 . 0.973 no C129 . C130 . 1.349(14) yes C129 . H1291 . 0.993 no C130 . H1301 . 0.974 no Cl202 . C201 . 1.753(10) yes Cl203 . C201 . 1.751(10) yes Cl204 . C201 . 1.747(10) yes C201 . H2011 . 0.947 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 C33 . C5 . C35 . 116.9(5) yes C33 . C5 . C40 . 118.1(5) yes C35 . C5 . C40 . 125.1(5) yes C18 . N6 . C26 . 126.8(5) yes C18 . N6 . H61 . 116.6 no C26 . N6 . H61 . 116.6 no C16 . C7 . C57 . 120.4(5) yes C16 . C7 . H71 . 119.8 no C57 . C7 . H71 . 119.8 no C19 . N8 . C37 . 120.3(5) yes C19 . N8 . C91 . 120.5(5) yes C37 . N8 . C91 . 119.1(5) yes C72 . O9 . C109 . 116.9(6) yes C120 . O10 . C122 . 112.5(7) yes C56 . O11 . C65 . 117.9(5) yes C99 . O12 . C102 . 116.0(8) yes C21 . C13 . C38 . 123.3(5) yes C21 . C13 . H131 . 117.8 no C38 . C13 . H131 . 118.9 no O4 . C14 . C16 . 118.2(6) yes O4 . C14 . N23 . 124.7(6) yes C16 . C14 . N23 . 117.0(5) yes C36 . C15 . C40 . 122.9(6) yes C36 . C15 . C58 . 115.9(6) yes C40 . C15 . C58 . 121.2(6) yes C14 . C16 . C7 . 124.8(5) yes C14 . C16 . C19 . 116.1(5) yes C7 . C16 . C19 . 119.1(5) yes C38 . C17 . C59 . 115.5(6) yes C38 . C17 . C66 . 122.9(6) yes C59 . C17 . C66 . 121.6(6) yes N6 . C18 . C20 . 123.7(5) yes N6 . C18 . C30 . 116.5(5) yes C20 . C18 . C30 . 119.8(5) yes C16 . C19 . N8 . 120.9(5) yes C16 . C19 . H191 . 120.6 no N8 . C19 . H191 . 118.5 no C18 . C20 . C35 . 118.3(5) yes C18 . C20 . H201 . 119.8 no C35 . C20 . H201 . 121.8 no C13 . C21 . C40 . 121.2(5) yes C13 . C21 . C51 . 116.2(5) yes C40 . C21 . C51 . 122.6(6) yes C88 . O22 . C98 . 112.8(6) yes C14 . N23 . C25 . 127.6(5) yes C14 . N23 . H231 . 117.3 no C25 . N23 . H231 . 115.1 no C52 . C24 . C81 . 122.6(7) yes C52 . C24 . H241 . 119.0 no C81 . C24 . H241 . 118.4 no N23 . C25 . C47 . 117.1(5) yes N23 . C25 . C79 . 123.4(6) yes C47 . C25 . C79 . 119.5(6) yes N6 . C26 . O2 . 125.3(5) yes N6 . C26 . C57 . 115.6(5) yes O2 . C26 . C57 . 119.1(5) yes C67 . N28 . C73 . 123.7(6) yes C67 . N28 . H281 . 117.8 no C73 . N28 . H281 . 118.5 no C18 . C30 . C33 . 120.7(6) yes C18 . C30 . H301 . 120.1 no C33 . C30 . H301 . 119.2 no C104 . O32 . C106 . 112.7(7) yes C5 . C33 . C30 . 121.1(6) yes C5 . C33 . H331 . 118.4 no C30 . C33 . H331 . 120.5 no C39 . C34 . C43 . 123.2(6) yes C39 . C34 . H341 . 119.7 no C43 . C34 . H341 . 116.9 no C20 . C35 . C5 . 123.2(5) yes C20 . C35 . H351 . 118.3 no C5 . C35 . H351 . 118.5 no C15 . C36 . C45 . 121.2(6) yes C15 . C36 . H361 . 118.6 no C45 . C36 . H361 . 120.2 no N8 . C37 . C57 . 121.4(6) yes N8 . C37 . H371 . 118.0 no C57 . C37 . H371 . 120.5 no C17 . C38 . C13 . 120.8(6) yes C17 . C38 . H381 . 119.3 no C13 . C38 . H381 . 119.9 no C34 . C39 . C40 . 119.8(5) yes C34 . C39 . C50 . 117.0(6) yes C40 . C39 . C50 . 123.1(5) yes C15 . C40 . C21 . 109.8(5) yes C15 . C40 . C39 . 110.4(5) yes C21 . C40 . C39 . 106.6(5) yes C15 . C40 . C5 . 108.9(5) yes C21 . C40 . C5 . 109.6(4) yes C39 . C40 . C5 . 111.5(5) yes C78 . O41 . C92 . 117.9(6) yes C47 . C42 . C108 . 122.5(7) yes C47 . C42 . H421 . 118.8 no C108 . C42 . H421 . 118.7 no C34 . C43 . C62 . 118.9(6) yes C34 . C43 . H431 . 120.5 no C62 . C43 . H431 . 120.6 no C77 . N44 . C86 . 123.3(6) yes C77 . N44 . H441 . 117.8 no C86 . N44 . H441 . 118.8 no C36 . C45 . C61 . 122.6(6) yes C36 . C45 . H451 . 118.8 no C61 . C45 . H451 . 118.6 no C48 . C46 . C60 . 119.8(6) yes C48 . C46 . C73 . 119.3(6) yes C60 . C46 . C73 . 120.9(7) yes C42 . C47 . C25 . 120.4(6) yes C42 . C47 . H471 . 119.4 no C25 . C47 . H471 . 120.2 no C46 . C48 . C49 . 120.5(6) yes C46 . C48 . H481 . 118.8 no C49 . C48 . H481 . 120.6 no C48 . C49 . C74 . 117.6(7) yes C48 . C49 . C86 . 121.2(6) yes C74 . C49 . C86 . 121.2(6) yes C39 . C50 . C64 . 121.2(6) yes C39 . C50 . H501 . 118.6 no C64 . C50 . H501 . 120.1 no C21 . C51 . C59 . 120.7(6) yes C21 . C51 . H511 . 120.2 no C59 . C51 . H511 . 119.1 no C24 . C52 . C76 . 121.2(7) yes C24 . C52 . H521 . 119.8 no C76 . C52 . H521 . 119.1 no C54 . C53 . C55 . 121.5(7) yes C54 . C53 . H531 . 118.3 no C55 . C53 . H531 . 120.2 no C53 . C54 . C63 . 116.4(7) yes C53 . C54 . C82 . 118.6(7) yes C63 . C54 . C82 . 124.9(6) yes C53 . C55 . C83 . 122.5(7) yes C53 . C55 . H551 . 118.1 no C83 . C55 . H551 . 119.4 no O11 . C56 . C77 . 109.0(5) yes O11 . C56 . H561 . 110.9 no C77 . C56 . H561 . 109.6 no O11 . C56 . H562 . 110.4 no C77 . C56 . H562 . 109.3 no H561 . C56 . H562 . 107.7 no C26 . C57 . C7 . 126.1(5) yes C26 . C57 . C37 . 116.2(5) yes C7 . C57 . C37 . 117.7(5) yes C15 . C58 . C70 . 122.0(6) yes C15 . C58 . H581 . 118.4 no C70 . C58 . H581 . 119.5 no C51 . C59 . C17 . 123.6(6) yes C51 . C59 . H591 . 118.2 no C17 . C59 . H591 . 118.2 no C46 . C60 . C80 . 121.0(8) yes C46 . C60 . H601 . 119.8 no C80 . C60 . H601 . 119.2 no C45 . C61 . C70 . 115.5(6) yes C45 . C61 . C85 . 123.0(6) yes C70 . C61 . C85 . 121.5(7) yes C43 . C62 . C64 . 118.8(6) yes C43 . C62 . H621 . 119.1 no C64 . C62 . H621 . 122.1 no C54 . C63 . C95 . 121.2(7) yes C54 . C63 . H631 . 119.6 no C95 . C63 . H631 . 119.2 no C50 . C64 . C62 . 120.9(6) yes C50 . C64 . H641 . 120.3 no C62 . C64 . H641 . 118.9 no O11 . C65 . C69 . 115.6(6) yes O11 . C65 . C87 . 124.7(6) yes C69 . C65 . C87 . 119.6(7) yes C17 . C66 . C75 . 109.0(6) yes C17 . C66 . C84 . 112.3(6) yes C75 . C66 . C84 . 109.0(6) yes C17 . C66 . C90 . 108.5(6) yes C75 . C66 . C90 . 108.8(6) yes C84 . C66 . C90 . 109.2(6) yes N28 . C67 . O31 . 123.4(7) yes N28 . C67 . C92 . 115.9(7) yes O31 . C67 . C92 . 120.8(8) yes C78 . C68 . C93 . 122.7(7) yes C78 . C68 . H681 . 119.3 no C93 . C68 . H681 . 118.0 no C65 . C69 . C96 . 120.6(7) yes C65 . C69 . H691 . 119.8 no C96 . C69 . H691 . 119.6 no C58 . C70 . C61 . 122.8(7) yes C58 . C70 . H701 . 118.0 no C61 . C70 . H701 . 119.2 no C72 . C71 . C87 . 120.7(7) yes C72 . C71 . H711 . 121.6 no C87 . C71 . H711 . 117.6 no O9 . C72 . C71 . 115.7(7) yes O9 . C72 . C96 . 124.3(6) yes C71 . C72 . C96 . 120.0(7) yes C46 . C73 . N28 . 111.3(5) yes C46 . C73 . H731 . 109.8 no N28 . C73 . H731 . 108.3 no C46 . C73 . H732 . 110.1 no N28 . C73 . H732 . 109.1 no H731 . C73 . H732 . 108.3 no C49 . C74 . C80 . 121.3(7) yes C49 . C74 . H741 . 117.9 no C80 . C74 . H741 . 120.7 no C66 . C75 . H751 . 111.1 no C66 . C75 . H752 . 111.8 no H751 . C75 . H752 . 108.7 no C66 . C75 . H753 . 110.4 no H751 . C75 . H753 . 107.8 no H752 . C75 . H753 . 107.0 no C52 . C76 . C82 . 118.9(6) yes C52 . C76 . C113 . 117.3(8) yes C82 . C76 . C113 . 123.7(8) yes C56 . C77 . N44 . 118.0(6) yes C56 . C77 . O29 . 116.7(6) yes N44 . C77 . O29 . 125.3(7) yes C68 . C78 . O41 . 116.5(6) yes C68 . C78 . C112 . 118.7(7) yes O41 . C78 . C112 . 124.5(7) yes C25 . C79 . C97 . 118.4(7) yes C25 . C79 . H791 . 121.1 no C97 . C79 . H791 . 120.5 no C74 . C80 . C60 . 119.8(7) yes C74 . C80 . H801 . 118.5 no C60 . C80 . H801 . 121.7 no C24 . C81 . C89 . 122.8(8) yes C24 . C81 . C114 . 115.1(8) yes C89 . C81 . C114 . 121.8(8) yes C76 . C82 . C54 . 107.1(6) yes C76 . C82 . C107 . 112.1(8) yes C54 . C82 . C107 . 109.6(7) yes C76 . C82 . C108 . 111.5(6) yes C54 . C82 . C108 . 110.3(6) yes C107 . C82 . C108 . 106.2(6) yes C55 . C83 . C95 . 115.4(7) yes C55 . C83 . C101 . 123.8(6) yes C95 . C83 . C101 . 120.5(7) yes C66 . C84 . H841 . 110.5 no C66 . C84 . H842 . 109.5 no H841 . C84 . H842 . 108.9 no C66 . C84 . H843 . 110.7 no H841 . C84 . H843 . 109.6 no H842 . C84 . H843 . 107.6 no C61 . C85 . C117 . 109.5(6) yes C61 . C85 . C119 . 113.6(7) yes C117 . C85 . C119 . 105.9(7) yes C61 . C85 . C121 . 110.6(6) yes C117 . C85 . C121 . 108.6(8) yes C119 . C85 . C121 . 108.5(7) yes C49 . C86 . N44 . 113.3(6) yes C49 . C86 . H861 . 110.2 no N44 . C86 . H861 . 108.8 no C49 . C86 . H862 . 108.3 no N44 . C86 . H862 . 106.9 no H861 . C86 . H862 . 109.1 no C71 . C87 . C65 . 118.9(7) yes C71 . C87 . H871 . 120.5 no C65 . C87 . H871 . 120.6 no O22 . C88 . C99 . 108.1(7) yes O22 . C88 . H881 . 111.7 no C99 . C88 . H881 . 108.2 no O22 . C88 . H882 . 112.7 no C99 . C88 . H882 . 107.6 no H881 . C88 . H882 . 108.4 no C81 . C89 . C103 . 109.8(7) yes C81 . C89 . C110 . 110.4(7) yes C103 . C89 . C110 . 107.1(7) yes C81 . C89 . C111 . 113.0(7) yes C103 . C89 . C111 . 108.9(7) yes C110 . C89 . C111 . 107.6(7) yes C66 . C90 . H901 . 108.9 no C66 . C90 . H902 . 109.4 no H901 . C90 . H902 . 109.5 no C66 . C90 . H903 . 110.1 no H901 . C90 . H903 . 109.5 no H902 . C90 . H903 . 109.5 no N8 . C91 . H911 . 110.9 no N8 . C91 . H912 . 109.6 no H911 . C91 . H912 . 108.8 no N8 . C91 . H913 . 110.0 no H911 . C91 . H913 . 109.8 no H912 . C91 . H913 . 107.6 no C67 . C92 . O41 . 114.0(6) yes C67 . C92 . H921 . 108.9 no O41 . C92 . H921 . 110.3 no C67 . C92 . H922 . 107.6 no O41 . C92 . H922 . 108.1 no H921 . C92 . H922 . 107.6 no C68 . C93 . C102 . 119.9(8) yes C68 . C93 . H931 . 120.8 no C102 . C93 . H931 . 119.2 no C63 . C95 . C83 . 122.9(7) yes C63 . C95 . H951 . 118.8 no C83 . C95 . H951 . 118.3 no C72 . C96 . C69 . 120.1(7) yes C72 . C96 . H961 . 118.8 no C69 . C96 . H961 . 121.0 no C79 . C97 . C108 . 122.7(7) yes C79 . C97 . H971 . 119.4 no C108 . C97 . H971 . 117.9 no O22 . C98 . C122 . 110.7(8) yes O22 . C98 . H981 . 108.3 no C122 . C98 . H981 . 107.7 no O22 . C98 . H982 . 111.4 no C122 . C98 . H982 . 110.7 no H981 . C98 . H982 . 107.9 no C88 . C99 . O12 . 108.4(8) yes C88 . C99 . H991 . 106.9 no O12 . C99 . H991 . 111.9 no C88 . C99 . H992 . 108.3 no O12 . C99 . H992 . 111.1 no H991 . C99 . H992 . 110.0 no C83 . C101 . C115 . 111.4(6) yes C83 . C101 . C116 . 110.4(6) yes C115 . C101 . C116 . 106.0(8) yes C83 . C101 . C118 . 108.4(8) yes C115 . C101 . C118 . 110.1(7) yes C116 . C101 . C118 . 110.5(8) yes O12 . C102 . C93 . 115.6(8) yes O12 . C102 . C105 . 123.2(9) yes C93 . C102 . C105 . 121.2(8) yes C89 . C103 . H1031 . 112.1 no C89 . C103 . H1032 . 110.0 no H1031 . C103 . H1032 . 108.4 no C89 . C103 . H1033 . 110.7 no H1031 . C103 . H1033 . 107.9 no H1032 . C103 . H1033 . 107.7 no O32 . C104 . C120 . 108.5(8) yes O32 . C104 . H1041 . 113.0 no C120 . C104 . H1041 . 111.9 no O32 . C104 . H1042 . 109.9 no C120 . C104 . H1042 . 107.8 no H1041 . C104 . H1042 . 105.6 no C102 . C105 . C112 . 120.1(8) yes C102 . C105 . H1051 . 115.2 no C112 . C105 . H1051 . 124.7 no O32 . C106 . C109 . 110.0(7) yes O32 . C106 . H1061 . 111.2 no C109 . C106 . H1061 . 111.0 no O32 . C106 . H1062 . 109.5 no C109 . C106 . H1062 . 108.1 no H1061 . C106 . H1062 . 107.1 no C82 . C107 . C123 . 119.2(8) yes C82 . C107 . C125 . 122.8(9) yes C123 . C107 . C125 . 117.9(8) yes C82 . C108 . C97 . 120.0(6) yes C82 . C108 . C42 . 123.3(6) yes C97 . C108 . C42 . 116.6(6) yes C106 . C109 . O9 . 107.9(7) yes C106 . C109 . H1091 . 110.9 no O9 . C109 . H1091 . 112.1 no C106 . C109 . H1092 . 107.6 no O9 . C109 . H1092 . 111.5 no H1091 . C109 . H1092 . 106.8 no C89 . C110 . H1101 . 110.3 no C89 . C110 . H1102 . 109.5 no H1101 . C110 . H1102 . 107.7 no C89 . C110 . H1103 . 111.0 no H1101 . C110 . H1103 . 108.0 no H1102 . C110 . H1103 . 110.3 no C89 . C111 . H1111 . 112.0 no C89 . C111 . H1112 . 110.8 no H1111 . C111 . H1112 . 105.7 no C89 . C111 . H1113 . 112.5 no H1111 . C111 . H1113 . 107.1 no H1112 . C111 . H1113 . 108.4 no C105 . C112 . C78 . 117.3(8) yes C105 . C112 . H1121 . 122.3 no C78 . C112 . H1121 . 120.3 no C76 . C113 . C114 . 119.9(9) yes C76 . C113 . H1131 . 122.7 no C114 . C113 . H1131 . 117.4 no C113 . C114 . C81 . 123.8(8) yes C113 . C114 . H1141 . 117.3 no C81 . C114 . H1141 . 118.9 no C101 . C115 . H1151 . 111.9 no C101 . C115 . H1152 . 111.8 no H1151 . C115 . H1152 . 105.8 no C101 . C115 . H1153 . 112.9 no H1151 . C115 . H1153 . 107.4 no H1152 . C115 . H1153 . 106.7 no C101 . C116 . H1161 . 111.4 no C101 . C116 . H1162 . 111.9 no H1161 . C116 . H1162 . 106.5 no C101 . C116 . H1163 . 111.5 no H1161 . C116 . H1163 . 107.2 no H1162 . C116 . H1163 . 108.1 no C85 . C117 . H1171 . 112.0 no C85 . C117 . H1172 . 109.6 no H1171 . C117 . H1172 . 108.2 no C85 . C117 . H1173 . 111.2 no H1171 . C117 . H1173 . 107.6 no H1172 . C117 . H1173 . 108.1 no C101 . C118 . H1181 . 107.7 no C101 . C118 . H1182 . 110.8 no H1181 . C118 . H1182 . 105.9 no C101 . C118 . H1183 . 110.8 no H1181 . C118 . H1183 . 108.5 no H1182 . C118 . H1183 . 112.9 no C85 . C119 . H1191 . 111.4 no C85 . C119 . H1192 . 111.1 no H1191 . C119 . H1192 . 110.6 no C85 . C119 . H1193 . 108.7 no H1191 . C119 . H1193 . 106.8 no H1192 . C119 . H1193 . 108.1 no C104 . C120 . O10 . 110.1(8) yes C104 . C120 . H1201 . 107.9 no O10 . C120 . H1201 . 109.6 no C104 . C120 . H1202 . 110.4 no O10 . C120 . H1202 . 111.1 no H1201 . C120 . H1202 . 107.6 no C85 . C121 . H1211 . 112.0 no C85 . C121 . H1212 . 109.6 no H1211 . C121 . H1212 . 107.7 no C85 . C121 . H1213 . 109.8 no H1211 . C121 . H1213 . 109.4 no H1212 . C121 . H1213 . 108.2 no C98 . C122 . O10 . 107.2(7) yes C98 . C122 . H1221 . 108.7 no O10 . C122 . H1221 . 110.2 no C98 . C122 . H1222 . 111.0 no O10 . C122 . H1222 . 111.7 no H1221 . C122 . H1222 . 108.1 no C107 . C123 . C130 . 123.1(10) yes C107 . C123 . H1231 . 116.8 no C130 . C123 . H1231 . 120.1 no C107 . C125 . C128 . 119.7(10) yes C107 . C125 . H1251 . 117.4 no C128 . C125 . H1251 . 122.3 no C125 . C128 . C129 . 118.7(10) yes C125 . C128 . H1281 . 115.4 no C129 . C128 . H1281 . 124.3 no C128 . C129 . C130 . 121.7(9) yes C128 . C129 . H1291 . 115.4 no C130 . C129 . H1291 . 122.7 no C123 . C130 . C129 . 118.0(11) yes C123 . C130 . H1301 . 119.0 no C129 . C130 . H1301 . 123.0 no Cl202 . C201 . Cl203 . 104.6(7) yes Cl202 . C201 . Cl204 . 105.3(7) yes Cl203 . C201 . Cl204 . 107.7(8) yes Cl202 . C201 . H2011 . 111.9 no Cl203 . C201 . H2011 . 113.7 no Cl204 . C201 . H2011 . 113.0 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 C19 . H191 . O32 . 139 0.98 2.51 3.319(11) yes C20 . H201 . O2 . 121 0.95 2.29 2.889(11) yes C35 . H351 . C13 . 124 0.96 2.49 3.138(11) yes C36 . H361 . C34 . 129 0.95 2.43 3.112(11) yes C37 . H371 . O29 2_666 142 0.99 2.43 3.259(11) yes C42 . H421 . C52 . 128 0.97 2.38 3.082(11) yes C50 . H501 . C33 . 128 0.96 2.40 3.088(11) yes C51 . H511 . C58 . 123 0.97 2.59 3.222(11) yes C56 . H561 . O2 2_666 158 0.95 2.44 3.341(11) yes C63 . H631 . C97 . 124 0.97 2.59 3.239(11) yes C91 . H911 . O29 2_666 152 0.94 2.26 3.118(11) yes C91 . H913 . O10 . 139 0.96 2.45 3.233(11) yes C113 . H1131 . C123 . 120 0.97 2.54 3.141(11) yes C125 . H1251 . C53 . 126 0.97 2.51 3.182(11) yes _chemical_name_common .