# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 #TrackingRef 'FaulRotaxChemScistructures.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 ; Lanthanide appended rotaxanes respond to changing chloride concentration ; loop_ _publ_author_name _publ_author_address "Cl\'emence Allain" ; 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. ; 'Stephen Faulkner' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; 'Michael W. Jones' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; 'Alan M. Kenwright' ; Department of Chemistry, University of Durham, South Road, Durham, DH1 3LE, UK. ; ; N.L.Kilah ; ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford, OX1 3TA, UK. ; 'Richard C. Knighton' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford, OX1 3TA, UK. ; T.J.Sorensen ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford, OX1 3TA, UK. ; 'Manuel Tropiano' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford, OX1 3TA, UK. ; _publ_section_abstract ; YOUR PAPER ABSTRACT ; #============================================================================== data_4.Cl _database_code_depnum_ccdc_archive 'CCDC 903824' #TrackingRef 'FaulRotaxChemScistructures.cif' #============================================================================== # start Validation Reply Form _vrf_PLAT022_4.Cl ; PROBLEM: Ratio Unique / Expected Reflections (too) Low .. 0.751 RESPONSE: Crystals were extremely small and poorly diffracting. Synchrotron radiation was used but despite this the data were extremely weak with many reflections missed. ; _vrf_PLAT026_4.Cl ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 29 Perc. RESPONSE: Crystals were extremely small and poorly diffracting. Synchrotron radiation was used but despite this the data were extremely weak with many reflections missed. ; _vrf_PLAT029_4.Cl ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.797 RESPONSE: Crystals were extremely small and poorly diffracting. Synchrotron radiation was used but despite this the data were extremely weak with many reflections missed. ; # 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 -0.194 1.000 0.500 2722 275 ' ' 2 0.484 0.192 0.985 29 2 ' ' 3 0.516 0.808 0.015 29 3 ' ' _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 ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 13.2580(9) _cell_length_b 20.3837(18) _cell_length_c 26.4826(17) _cell_angle_alpha 85.599(6) _cell_angle_beta 81.344(5) _cell_angle_gamma 81.232(6) _cell_volume 6982.0(9) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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 2 # Given Formula = C106 H115 Cl1 N8 O11 # Dc = 0.81 Fooo = 1824.00 Mu = 0.71 M = 1712.58 # Found Formula = C106 H115 Cl1 N8 O11 # Dc = 0.81 FOOO = 1824.00 Mu = 0.71 M = 1712.58 _chemical_formula_sum 'C106 H115 Cl1 N8 O11' _chemical_formula_moiety 'C74 H78 N3 O2, C32 H37 N5 O9, Cl' _chemical_compound_source synthesised _chemical_formula_weight 1712.58 _cell_measurement_reflns_used 9798 _cell_measurement_theta_min 1.7551 _cell_measurement_theta_max 26.9166 _cell_measurement_temperature 100 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.1 _exptl_crystal_density_diffrn 0.815 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.071 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.31439 _exptl_absorpt_correction_T_max 1.0000 _diffrn_measurement_device_type synchrotron _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.68890 _diffrn_measurement_method \w/2\q # 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 'CrystalClear (Rigaku, 1997--2002)' _computing_data_reduction 'CrystalClear (Rigaku, 1997--2002)' _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 100 _diffrn_reflns_number 49935 _reflns_number_total 25858 _diffrn_reflns_av_R_equivalents 0.140 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 25858 # Theoretical number of reflections is about 66390 _diffrn_reflns_theta_min 1.755 _diffrn_reflns_theta_max 26.917 _diffrn_measured_fraction_theta_max 0.751 _diffrn_reflns_theta_full 25.032 _diffrn_measured_fraction_theta_full 0.797 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -16 _reflns_limit_h_max 17 _reflns_limit_k_min -25 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 4.99 _oxford_diffrn_Wilson_scale 0.04 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.39 _refine_diff_density_max 0.63 # 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 12858 _refine_ls_number_restraints 1441 _refine_ls_number_parameters 1150 _oxford_refine_ls_R_factor_ref 0.1601 _refine_ls_wR_factor_ref 0.3902 _refine_ls_goodness_of_fit_ref 1.1600 _refine_ls_shift/su_max 0.0003462 _refine_ls_shift/su_mean 0.0000372 # The values computed from all data _oxford_reflns_number_all 12858 _refine_ls_R_factor_all 0.1601 _refine_ls_wR_factor_all 0.3902 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7598 _refine_ls_R_factor_gt 0.1334 _refine_ls_wR_factor_gt 0.3575 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. CrystalClear: An Integrated Program for the Collection and Processing of Area Detector Data, Rigaku Corporation, 1997--2002. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C 0.1775(11) 0.7549(10) 0.5609(7) 0.2669 1.0000 Uani D U . . . . C2 C 0.2902(16) 0.8231(9) 0.5914(7) 0.2686 1.0000 Uani . U . . . . C3 C 0.3366(17) 0.7926(9) 0.5012(6) 0.2817 1.0000 Uani . U . . . . C4 C 0.2938(8) 0.7636(7) 0.5581(4) 0.1903 1.0000 Uani D U . . . . C5 C 0.3670(5) 0.7008(4) 0.5718(3) 0.1429 1.0000 Uani D U . . . . C6 C 0.4361(6) 0.7008(4) 0.6074(3) 0.1459 1.0000 Uani D U . . . . C7 C 0.5047(5) 0.6427(4) 0.6180(2) 0.1281 1.0000 Uani D U . . . . C8 C 0.5063(4) 0.5849(4) 0.5936(2) 0.1161 1.0000 Uani D U . . . . C9 C 0.4364(5) 0.5841(4) 0.5588(2) 0.1231 1.0000 Uani D U . . . . C10 C 0.3685(5) 0.6417(4) 0.5482(2) 0.1282 1.0000 Uani D U . . . . C11 C 0.9598(6) 0.5272(6) 0.4029(3) 0.1512 1.0000 Uani . U . . . . C12 C 1.0088(5) 0.4106(6) 0.4406(3) 0.1497 1.0000 Uani . U . . . . C13 C 0.8688(6) 0.4326(5) 0.3825(2) 0.1348 1.0000 Uani . U . . . . C14 C 0.9194(5) 0.4628(4) 0.4243(2) 0.1264 1.0000 Uani . U . . . . C15 C 0.8324(4) 0.4781(3) 0.4718(2) 0.1102 1.0000 Uani D U . . . . C16 C 0.8348(4) 0.4434(3) 0.5191(2) 0.1139 1.0000 Uani D U . . . . C17 C 0.7562(4) 0.4572(3) 0.5605(2) 0.1173 1.0000 Uani D U . . . . C18 C 0.6715(4) 0.5071(3) 0.5550(2) 0.1054 1.0000 Uani D U . . . . C19 C 0.6689(4) 0.5419(3) 0.5081(2) 0.1117 1.0000 Uani D U . . . . C20 C 0.7481(4) 0.5281(3) 0.4666(2) 0.1189 1.0000 Uani D U . . . . C21 C 0.3955(5) 0.3561(4) 0.6310(3) 0.1420 1.0000 Uani D U . . . . C22 C 0.3664(5) 0.4149(4) 0.6566(2) 0.1284 1.0000 Uani D U . . . . C23 C 0.4263(4) 0.4668(4) 0.6464(2) 0.1162 1.0000 Uani D U . . . . C24 C 0.5185(4) 0.4597(4) 0.6111(2) 0.1156 1.0000 Uani D U . . . . C25 C 0.5459(5) 0.4005(4) 0.5854(2) 0.1340 1.0000 Uani D U . . . . C26 C 0.4848(5) 0.3496(4) 0.5950(2) 0.1411 1.0000 Uani D U . . . . C27 C 0.5840(5) 0.5194(4) 0.6020(2) 0.1112 1.0000 Uani . U . . . . C28 C 0.6413(4) 0.5250(3) 0.6501(2) 0.1036 1.0000 Uani D U . . . . C29 C 0.7180(4) 0.5672(3) 0.6447(2) 0.1092 1.0000 Uani D U . . . . C30 C 0.7725(4) 0.5746(3) 0.68464(19) 0.1037 1.0000 Uani D U . . . . C31 C 0.7507(4) 0.5398(3) 0.73124(19) 0.0955 1.0000 Uani D U . . . . C32 C 0.6749(4) 0.4979(3) 0.7371(2) 0.1034 1.0000 Uani D U . . . . C33 C 0.6203(4) 0.4904(3) 0.6965(2) 0.1061 1.0000 Uani D U . . . . N34 N 0.8019(3) 0.5440(3) 0.77478(18) 0.0976 1.0000 Uani . U . . . . C35 C 0.8838(4) 0.5790(4) 0.7768(2) 0.1049 1.0000 Uani D U . . . . O36 O 0.9196(4) 0.6137(3) 0.74186(18) 0.1349 1.0000 Uani . U . . . . C37 C 0.9352(4) 0.5642(3) 0.82411(19) 0.0996 1.0000 Uani D U . . . . C38 C 1.0008(4) 0.6085(3) 0.8328(2) 0.0966 1.0000 Uani D U . . . . N39 N 1.0539(3) 0.5978(3) 0.87375(18) 0.0958 1.0000 Uani D U . . . . C40 C 1.1231(5) 0.6462(4) 0.8820(3) 0.1063 1.0000 Uani . U . . . . C41 C 1.0436(4) 0.5446(3) 0.9077(2) 0.0986 1.0000 Uani D U . . . . C42 C 0.9790(4) 0.4985(3) 0.90097(19) 0.0945 1.0000 Uani D U . . . . C43 C 0.9244(4) 0.5091(3) 0.8583(2) 0.0959 1.0000 Uani D U . . . . C44 C 0.6845(10) 0.0023(8) 0.8510(6) 0.2449 1.0000 Uani . U . . . . C45 C 0.5072(9) 0.0498(7) 0.8960(6) 0.2109 1.0000 Uani . U . . . . C46 C 0.5907(9) -0.0619(6) 0.9319(6) 0.2166 1.0000 Uani . U . . . . C47 C 0.6136(6) 0.0084(6) 0.9037(6) 0.1950 1.0000 Uani . U . . . . C48 C 0.6629(5) 0.0466(4) 0.9424(4) 0.1636 1.0000 Uani D U . . . . C49 C 0.6811(5) 0.0212(4) 0.9914(4) 0.1609 1.0000 Uani D U . . . . C50 C 0.7220(5) 0.0586(3) 1.0242(3) 0.1414 1.0000 Uani D U . . . . C51 C 0.7476(5) 0.1212(3) 1.0073(3) 0.1259 1.0000 Uani D U . . . . C52 C 0.7327(5) 0.1454(4) 0.9577(3) 0.1497 1.0000 Uani D U . . . . C53 C 0.6887(6) 0.1094(4) 0.9254(3) 0.1661 1.0000 Uani D U . . . . C54 C 0.3638(9) 0.2617(12) 1.2124(6) 0.2979 1.0000 Uani . U . . . . C55 C 0.4836(10) 0.3379(8) 1.2272(4) 0.2110 1.0000 Uani . U . . . . C56 C 0.5044(12) 0.2247(9) 1.2700(4) 0.2269 1.0000 Uani . U . . . . C57 C 0.4764(8) 0.2633(5) 1.2199(3) 0.1872 1.0000 Uani . U . . . . C58 C 0.5528(6) 0.2339(4) 1.1748(2) 0.1512 1.0000 Uani D U . . . . C59 C 0.5300(5) 0.1923(4) 1.1400(3) 0.1681 1.0000 Uani D U . . . . C60 C 0.6035(5) 0.1677(4) 1.0996(3) 0.1405 1.0000 Uani D U . . . . C61 C 0.7026(5) 0.1834(3) 1.0936(2) 0.1099 1.0000 Uani D U . . . . C62 C 0.7253(5) 0.2256(3) 1.1281(3) 0.1340 1.0000 Uani D U . . . . C63 C 0.6516(6) 0.2498(4) 1.1681(2) 0.1385 1.0000 Uani D U . . . . C64 C 1.0489(7) 0.0243(4) 1.0970(5) 0.1998 1.0000 Uani D U . . . . C65 C 1.0463(6) 0.0433(4) 1.0454(4) 0.1813 1.0000 Uani D U . . . . C66 C 0.9627(5) 0.0872(3) 1.0301(3) 0.1500 1.0000 Uani D U . . . . C67 C 0.8818(5) 0.1138(3) 1.0667(3) 0.1294 1.0000 Uani D U . . . . C68 C 0.8855(6) 0.0958(4) 1.1189(4) 0.1600 1.0000 Uani D U . . . . C69 C 0.9683(7) 0.0505(4) 1.1339(4) 0.2086 1.0000 Uani D U . . . . C70 C 0.7893(5) 0.1609(4) 1.0472(3) 0.1142 1.0000 Uani . U . . . . C71 C 0.8236(4) 0.2279(3) 1.0199(2) 0.1037 1.0000 Uani D U . . . . C72 C 0.7464(5) 0.2770(3) 1.0054(2) 0.1117 1.0000 Uani D U . . . . C73 C 0.7696(4) 0.3360(3) 0.9797(2) 0.1047 1.0000 Uani D U . . . . C74 C 0.8721(4) 0.3484(3) 0.9692(2) 0.0940 1.0000 Uani D U . . . . C75 C 0.9490(4) 0.3004(3) 0.9847(2) 0.1025 1.0000 Uani D U . . . . C76 C 0.9254(4) 0.2403(3) 1.0097(2) 0.1038 1.0000 Uani D U . . . . N77 N 0.8893(4) 0.4093(3) 0.94071(19) 0.0984 1.0000 Uani . U . . . . C78 C 0.9726(5) 0.4415(4) 0.9389(3) 0.0966 1.0000 Uani . U . . . . O79 O 1.0396(4) 0.4262(2) 0.96819(19) 0.1123 1.0000 Uani . U . . . . N80 N 0.226(2) 0.1556(16) 0.9381(6) 0.3491 0.5490 Uani D U . . 1 . N81 N 0.222(2) 0.2134(16) 0.9317(6) 0.2879 0.5490 Uani D U . . 1 . N82 N 0.220(2) 0.2711(16) 0.9266(6) 0.2213 0.5490 Uani D U . . 1 . C83 C 0.3039(7) 0.3065(6) 0.9124(3) 0.1624 1.0000 Uani . U . . . . C84 C 0.3985(8) 0.2758(6) 0.8903(3) 0.1731 1.0000 Uani . U . . . . C85 C 0.4846(7) 0.3086(6) 0.8749(3) 0.1474 1.0000 Uani . U . . . . C86 C 0.4719(6) 0.3763(5) 0.8823(2) 0.1239 1.0000 Uani . U . . . . C87 C 0.3801(6) 0.4111(5) 0.9046(2) 0.1228 1.0000 Uani . U . . . . C88 C 0.2950(6) 0.3772(5) 0.9193(2) 0.1481 1.0000 Uani . U . . . . C89 C 0.3637(6) 0.4848(5) 0.9136(2) 0.1278 1.0000 Uani . U . . . . O90 O 0.2779(4) 0.5135(3) 0.93022(19) 0.1421 1.0000 Uani . U . . . . N91 N 0.4511(5) 0.5151(4) 0.9067(3) 0.1357 1.0000 Uani . U . . . . C92 C 0.4467(7) 0.5879(5) 0.9205(4) 0.1492 1.0000 Uani . U . . . . C93 C 0.4773(8) 0.5928(7) 0.9740(4) 0.1743 1.0000 Uani . U . . . . O94 O 0.5798(5) 0.5742(4) 0.9730(2) 0.1879 1.0000 Uani D U . . . . C95 C 0.6485(6) 0.6196(5) 0.9580(3) 0.1853 1.0000 Uani D U . . . . C96 C 0.6178(7) 0.6841(6) 0.9411(3) 0.2205 1.0000 Uani D U . . . . C97 C 0.6935(7) 0.7268(5) 0.9275(3) 0.2187 1.0000 Uani D U . . . . C98 C 0.7941(7) 0.7030(5) 0.9325(3) 0.1895 1.0000 Uani D U . . . . C99 C 0.8209(7) 0.6390(5) 0.9498(3) 0.1774 1.0000 Uani D U . . . . C100 C 0.7480(7) 0.5978(4) 0.9631(3) 0.1670 1.0000 Uani D U . . . . O101 O 0.8791(4) 0.7364(4) 0.9235(2) 0.1814 1.0000 Uani D U . . . . C102 C 0.8632(8) 0.8022(4) 0.9058(4) 0.2009 1.0000 Uani D U . . . . C103 C 0.8701(7) 0.8143(6) 0.8494(4) 0.2211 1.0000 Uani D U . . . . O104 O 0.9601(6) 0.7846(4) 0.8204(3) 0.1975 1.0000 Uani D U . . . . C105 C 0.9744(8) 0.8004(6) 0.7695(4) 0.2286 1.0000 Uani D U . . . . C106 C 1.0800(9) 0.7802(5) 0.7423(4) 0.2259 1.0000 Uani D U . . . . O107 O 1.1227(6) 0.7155(3) 0.7515(2) 0.1799 1.0000 Uani D U . . . . C108 C 1.2010(8) 0.6891(4) 0.7167(3) 0.1933 1.0000 Uani D U . . . . C109 C 1.2483(9) 0.6189(4) 0.7267(2) 0.1745 1.0000 Uani D U . . . . O110 O 1.2698(5) 0.6013(3) 0.77597(17) 0.1583 1.0000 Uani D U . . . . C111 C 1.3274(5) 0.5391(4) 0.7855(3) 0.1638 1.0000 Uani D U . . . . C112 C 1.2682(6) 0.4812(4) 0.7968(3) 0.1569 1.0000 Uani D U . . . . O113 O 1.2033(4) 0.4730(3) 0.76051(16) 0.1484 1.0000 Uani D U . . . . C114 C 1.1269(5) 0.4326(4) 0.7728(3) 0.1437 1.0000 Uani D U . . . . C115 C 1.0526(6) 0.4406(4) 0.7399(2) 0.1397 1.0000 Uani D U . . . . C116 C 0.9707(6) 0.4028(4) 0.7498(3) 0.1518 1.0000 Uani D U . . . . C117 C 0.9618(6) 0.3577(4) 0.7920(3) 0.1643 1.0000 Uani D U . . . . C118 C 1.0376(7) 0.3500(4) 0.8246(3) 0.1656 1.0000 Uani D U . . . . C119 C 1.1198(6) 0.3876(4) 0.8149(3) 0.1527 1.0000 Uani D U . . . . O120 O 0.8740(6) 0.3243(4) 0.7965(4) 0.1905 1.0000 Uani D U . . . . C121 C 0.8603(8) 0.2835(7) 0.8346(5) 0.1931 1.0000 Uani D U . . . . C122 C 0.7699(7) 0.2500(6) 0.8268(5) 0.1790 1.0000 Uani D U . . . . N123 N 0.6712(5) 0.2916(4) 0.8469(3) 0.1498 1.0000 Uani . U . . . . C124 C 0.5802(7) 0.2651(6) 0.8511(3) 0.1418 1.0000 Uani . U . . . . O125 O 0.5828(6) 0.2043(4) 0.8430(2) 0.1976 1.0000 Uani . U . . . . Cl126 Cl 0.69499(12) 0.45336(11) 0.87377(6) 0.1149 1.0000 Uani . . . . . . H11 H 0.1745 0.7081 0.5694 0.3872 1.0000 Uiso R . . . . . H12 H 0.1339 0.7808 0.5867 0.3870 1.0000 Uiso R . . . . . H13 H 0.1523 0.7669 0.5286 0.3870 1.0000 Uiso R . . . . . H21 H 0.3536 0.8484 0.5759 0.3841 1.0000 Uiso R . . . . . H22 H 0.2950 0.8053 0.6301 0.3842 1.0000 Uiso R . . . . . H23 H 0.2178 0.8533 0.5884 0.3840 1.0000 Uiso R . . . . . H61 H 0.4348 0.7388 0.6252 0.1712 1.0000 Uiso R . . . . . H71 H 0.5508 0.6446 0.6412 0.1528 1.0000 Uiso R . . . . . H91 H 0.4348 0.5460 0.5426 0.1454 1.0000 Uiso R . . . . . H101 H 0.3225 0.6403 0.5248 0.1552 1.0000 Uiso R . . . . . H111 H 0.9029 0.5575 0.3917 0.2171 1.0000 Uiso R . . . . . H112 H 0.9858 0.5463 0.4302 0.2170 1.0000 Uiso R . . . . . H113 H 1.0137 0.5162 0.3748 0.2171 1.0000 Uiso R . . . . . H121 H 0.9890 0.3662 0.4460 0.2193 1.0000 Uiso R . . . . . H122 H 1.0262 0.4235 0.4719 0.2188 1.0000 Uiso R . . . . . H123 H 1.0655 0.4119 0.4134 0.2193 1.0000 Uiso R . . . . . H131 H 0.8369 0.3941 0.3967 0.1887 1.0000 Uiso R . . . . . H132 H 0.9222 0.4197 0.3550 0.1892 1.0000 Uiso R . . . . . H133 H 0.8191 0.4676 0.3701 0.1888 1.0000 Uiso R . . . . . H161 H 0.8899 0.4100 0.5225 0.1363 1.0000 Uiso R . . . . . H171 H 0.7607 0.4347 0.5924 0.1384 1.0000 Uiso R . . . . . H191 H 0.6135 0.5758 0.5038 0.1294 1.0000 Uiso R . . . . . H201 H 0.7424 0.5527 0.4345 0.1372 1.0000 Uiso R . . . . . H211 H 0.3567 0.3210 0.6375 0.1605 1.0000 Uiso R . . . . . H221 H 0.3073 0.4179 0.6806 0.1454 1.0000 Uiso R . . . . . H231 H 0.4050 0.5082 0.6623 0.1455 1.0000 Uiso R . . . . . H251 H 0.6069 0.3957 0.5621 0.1592 1.0000 Uiso R . . . . . H261 H 0.5042 0.3095 0.5768 0.1656 1.0000 Uiso R . . . . . H291 H 0.7323 0.5924 0.6136 0.1282 1.0000 Uiso R . . . . . H301 H 0.8228 0.6030 0.6803 0.1152 1.0000 Uiso R . . . . . H321 H 0.6583 0.4766 0.7681 0.1193 1.0000 Uiso R . . . . . H331 H 0.5715 0.4605 0.7006 0.1139 1.0000 Uiso R . . . . . H381 H 1.0095 0.6448 0.8104 0.1209 1.0000 Uiso R . . . . . H401 H 1.1814 0.6264 0.8978 0.1498 1.0000 Uiso R . . . . . H402 H 1.0856 0.6809 0.9027 0.1506 1.0000 Uiso R . . . . . H403 H 1.1481 0.6681 0.8498 0.1503 1.0000 Uiso R . . . . . H411 H 1.0799 0.5406 0.9367 0.1122 1.0000 Uiso R . . . . . H431 H 0.8817 0.4790 0.8537 0.1146 1.0000 Uiso R . . . . . H451 H 0.4545 0.0404 0.9256 0.2990 1.0000 Uiso R . . . . . H453 H 0.5150 0.0979 0.8930 0.2989 1.0000 Uiso R . . . . . H452 H 0.4892 0.0354 0.8637 0.2991 1.0000 Uiso R . . . . . H461 H 0.5253 -0.0555 0.9541 0.3109 1.0000 Uiso R . . . . . H463 H 0.6439 -0.0806 0.9519 0.3111 1.0000 Uiso R . . . . . H462 H 0.5875 -0.0921 0.9064 0.3112 1.0000 Uiso R . . . . . H491 H 0.6677 -0.0210 1.0033 0.1832 1.0000 Uiso R . . . . . H501 H 0.7319 0.0428 1.0577 0.1640 1.0000 Uiso R . . . . . H521 H 0.7512 0.1877 0.9454 0.1831 1.0000 Uiso R . . . . . H531 H 0.6781 0.1270 0.8928 0.2011 1.0000 Uiso R . . . . . H552 H 0.5557 0.3425 1.2191 0.2981 1.0000 Uiso R . . . . . H551 H 0.4593 0.3464 1.2625 0.2982 1.0000 Uiso R . . . . . H553 H 0.4439 0.3681 1.2054 0.2982 1.0000 Uiso R . . . . . H562 H 0.5789 0.2192 1.2687 0.3311 1.0000 Uiso R . . . . . H561 H 0.4731 0.2482 1.3000 0.3313 1.0000 Uiso R . . . . . H563 H 0.4823 0.1805 1.2717 0.3310 1.0000 Uiso R . . . . . H591 H 0.4631 0.1803 1.1443 0.1875 1.0000 Uiso R . . . . . H601 H 0.5851 0.1407 1.0761 0.1671 1.0000 Uiso R . . . . . H621 H 0.7917 0.2380 1.1233 0.1458 1.0000 Uiso R . . . . . H631 H 0.6684 0.2752 1.1927 0.1552 1.0000 Uiso R . . . . . H641 H 1.1019 -0.0064 1.1071 0.2283 1.0000 Uiso R . . . . . H651 H 1.1009 0.0267 1.0209 0.2101 1.0000 Uiso R . . . . . H661 H 0.9618 0.1003 0.9961 0.1714 1.0000 Uiso R . . . . . H681 H 0.8337 0.1144 1.1434 0.1909 1.0000 Uiso R . . . . . H691 H 0.9686 0.0370 1.1685 0.2374 1.0000 Uiso R . . . . . H721 H 0.6785 0.2691 1.0118 0.1294 1.0000 Uiso R . . . . . H731 H 0.7162 0.3694 0.9709 0.1229 1.0000 Uiso R . . . . . H751 H 1.0163 0.3100 0.9788 0.1164 1.0000 Uiso R . . . . . H761 H 0.9775 0.2068 1.0188 0.1182 1.0000 Uiso R . . . . . H841 H 0.4044 0.2298 0.8862 0.1972 1.0000 Uiso R . . . . . H861 H 0.5286 0.3981 0.8706 0.1407 1.0000 Uiso R . . . . . H881 H 0.2306 0.4006 0.9336 0.1662 1.0000 Uiso R . . . . . H922 H 0.4897 0.6116 0.8954 0.1757 1.0000 Uiso R . . . . . H921 H 0.3754 0.6086 0.9210 0.1751 1.0000 Uiso R . . . . . H931 H 0.4658 0.6387 0.9853 0.1955 1.0000 Uiso R . . . . . H932 H 0.4396 0.5624 0.9981 0.1966 1.0000 Uiso R . . . . . H961 H 0.5486 0.6978 0.9369 0.2687 1.0000 Uiso R . . . . . H971 H 0.6748 0.7706 0.9147 0.2931 1.0000 Uiso R . . . . . H991 H 0.8903 0.6247 0.9520 0.2054 1.0000 Uiso R . . . . . H1001 H 0.7657 0.5546 0.9763 0.1944 1.0000 Uiso R . . . . . H1022 H 0.9215 0.8233 0.9108 0.2304 1.0000 Uiso R . . . . . H1021 H 0.7992 0.8231 0.9251 0.2298 1.0000 Uiso R . . . . . H1062 H 1.1100 0.8064 0.7648 0.2631 1.0000 Uiso R . . . . . H1061 H 1.0939 0.7970 0.7064 0.2630 1.0000 Uiso R . . . . . H1081 H 1.2534 0.7141 0.7240 0.2226 1.0000 Uiso R . . . . . H1082 H 1.1855 0.6987 0.6813 0.2224 1.0000 Uiso R . . . . . H1092 H 1.3098 0.6065 0.7032 0.2032 1.0000 Uiso R . . . . . H1091 H 1.1935 0.5954 0.7201 0.2031 1.0000 Uiso R . . . . . H1111 H 1.3712 0.5409 0.8111 0.1728 1.0000 Uiso R . . . . . H1112 H 1.3686 0.5289 0.7524 0.1737 1.0000 Uiso R . . . . . H1121 H 1.2263 0.4873 0.8304 0.1764 1.0000 Uiso R . . . . . H1122 H 1.3157 0.4393 0.7993 0.1767 1.0000 Uiso R . . . . . H1151 H 1.0557 0.4726 0.7119 0.1632 1.0000 Uiso R . . . . . H1161 H 0.9216 0.4074 0.7264 0.1695 1.0000 Uiso R . . . . . H1181 H 1.0337 0.3193 0.8520 0.1941 1.0000 Uiso R . . . . . H1191 H 1.1701 0.3823 0.8364 0.1774 1.0000 Uiso R . . . . . H1221 H 0.7705 0.2060 0.8421 0.2082 1.0000 Uiso R . . . . . H1222 H 0.7737 0.2497 0.7899 0.2082 1.0000 Uiso R . . . . . H1211 H 0.8473 0.3023 0.8671 0.2179 1.0000 Uiso R . . . . . H1212 H 0.9192 0.2504 0.8335 0.2179 1.0000 Uiso R . . . . . H541 H 0.3512 0.2875 1.1820 0.3553 1.0000 Uiso R . . . . . H542 H 0.3184 0.2802 1.2406 0.3553 1.0000 Uiso R . . . . . H543 H 0.3525 0.2174 1.2093 0.3553 1.0000 Uiso R . . . . . H771 H 0.8356 0.4312 0.9214 0.1145 1.0000 Uiso R . . . . . H341 H 0.7758 0.5208 0.8069 0.1020 1.0000 Uiso R . . . . . H911 H 0.5162 0.4898 0.8926 0.1609 1.0000 Uiso R . . . . . H1231 H 0.6731 0.3359 0.8590 0.1791 1.0000 Uiso R . . . . . N180 N 0.250(2) 0.1744(12) 0.9650(6) 0.2274 0.4510 Uani D U . . 2 . N181 N 0.233(2) 0.2282(12) 0.9464(6) 0.2285 0.4510 Uani D U . . 2 . N182 N 0.213(2) 0.2827(12) 0.9298(6) 0.1671 0.4510 Uani D U . . 2 . H31 H 0.4076 0.7970 0.4978 0.3144 1.0000 Uiso R . . . . . H32 H 0.2974 0.8351 0.4963 0.3144 1.0000 Uiso R . . . . . H33 H 0.3260 0.7642 0.4763 0.3144 1.0000 Uiso R . . . . . H441 H 0.6949 0.0456 0.8373 0.2623 1.0000 Uiso R . . . . . H442 H 0.7491 -0.0231 0.8555 0.2623 1.0000 Uiso R . . . . . H443 H 0.6523 -0.0187 0.8283 0.2623 1.0000 Uiso R . . . . . H1051 H 0.9663 0.8476 0.7679 0.3540 1.0000 Uiso R . . . . . H1052 H 0.9239 0.7862 0.7526 0.3540 1.0000 Uiso R . . . . . H1031 H 0.8676 0.8610 0.8431 0.2824 1.0000 Uiso R . . . . . H1032 H 0.8122 0.8005 0.8383 0.2824 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 0.145(7) 0.38(2) 0.266(15) -0.064(13) -0.073(9) 0.054(8) C2 0.298(17) 0.277(11) 0.227(11) -0.090(11) -0.069(13) 0.041(12) C3 0.334(18) 0.290(16) 0.176(8) 0.010(7) -0.001(11) 0.051(14) C4 0.176(7) 0.254(8) 0.144(6) -0.031(6) -0.054(7) 0.002(7) C5 0.095(5) 0.241(6) 0.099(5) -0.042(4) -0.019(4) -0.024(5) C6 0.117(7) 0.227(6) 0.105(5) -0.048(5) -0.031(4) -0.028(5) C7 0.093(5) 0.221(6) 0.082(5) -0.042(4) -0.018(4) -0.040(4) C8 0.057(4) 0.232(5) 0.068(4) -0.051(3) -0.007(3) -0.029(3) C9 0.069(5) 0.239(6) 0.071(4) -0.045(4) -0.018(3) -0.027(4) C10 0.067(5) 0.245(7) 0.081(4) -0.037(4) -0.017(4) -0.027(4) C11 0.091(6) 0.301(7) 0.077(4) -0.038(5) 0.010(4) -0.086(5) C12 0.053(4) 0.304(8) 0.096(5) -0.062(5) 0.001(3) -0.025(4) C13 0.077(5) 0.274(9) 0.063(4) -0.059(4) 0.004(3) -0.045(5) C14 0.062(4) 0.264(7) 0.064(3) -0.046(4) 0.001(2) -0.047(3) C15 0.051(3) 0.231(7) 0.062(2) -0.044(3) -0.004(2) -0.047(3) C16 0.054(4) 0.241(7) 0.059(3) -0.045(3) -0.013(2) -0.035(4) C17 0.059(4) 0.241(7) 0.061(3) -0.041(4) -0.012(2) -0.028(3) C18 0.056(3) 0.211(6) 0.062(2) -0.045(3) -0.009(2) -0.040(3) C19 0.062(4) 0.220(7) 0.065(3) -0.040(3) -0.010(2) -0.038(4) C20 0.054(4) 0.251(8) 0.063(3) -0.033(4) -0.013(2) -0.041(3) C21 0.084(5) 0.236(7) 0.122(6) -0.056(5) 0.000(4) -0.065(5) C22 0.071(5) 0.246(7) 0.085(5) -0.054(4) -0.009(3) -0.055(4) C23 0.062(4) 0.230(6) 0.068(4) -0.054(4) -0.005(3) -0.042(4) C24 0.063(4) 0.233(5) 0.065(4) -0.052(3) -0.006(2) -0.045(3) C25 0.072(5) 0.242(7) 0.098(5) -0.069(5) 0.007(4) -0.047(4) C26 0.087(5) 0.231(7) 0.116(6) -0.062(5) 0.000(4) -0.046(5) C27 0.058(3) 0.224(4) 0.062(2) -0.041(3) -0.0073(18) -0.038(2) C28 0.054(4) 0.205(6) 0.061(2) -0.054(3) 0.000(2) -0.032(3) C29 0.053(4) 0.220(7) 0.065(3) -0.035(3) -0.008(3) -0.039(4) C30 0.051(4) 0.210(7) 0.060(3) -0.038(3) -0.002(3) -0.040(4) C31 0.047(4) 0.188(6) 0.060(2) -0.041(3) -0.007(2) -0.029(3) C32 0.062(4) 0.187(6) 0.074(3) -0.031(3) -0.018(3) -0.038(3) C33 0.050(4) 0.211(7) 0.068(3) -0.044(3) -0.008(3) -0.037(4) N34 0.057(3) 0.182(5) 0.065(3) -0.037(3) -0.016(2) -0.030(3) C35 0.063(4) 0.202(7) 0.062(3) -0.031(3) -0.013(3) -0.043(3) O36 0.096(4) 0.259(6) 0.073(3) -0.011(3) -0.025(3) -0.085(4) C37 0.057(4) 0.191(6) 0.062(3) -0.039(3) -0.012(3) -0.037(4) C38 0.071(4) 0.157(5) 0.072(3) -0.040(3) -0.019(3) -0.025(3) N39 0.065(3) 0.155(4) 0.079(3) -0.047(2) -0.021(2) -0.023(3) C40 0.070(4) 0.167(6) 0.097(4) -0.045(4) -0.024(4) -0.031(4) C41 0.059(4) 0.174(5) 0.076(4) -0.035(3) -0.025(3) -0.029(4) C42 0.053(4) 0.181(5) 0.060(3) -0.038(2) -0.008(2) -0.033(3) C43 0.050(4) 0.178(5) 0.072(3) -0.042(3) -0.015(3) -0.029(4) C44 0.165(8) 0.303(13) 0.304(10) -0.206(10) -0.034(8) -0.057(9) C45 0.135(7) 0.244(9) 0.283(14) -0.120(9) -0.085(7) -0.016(7) C46 0.132(8) 0.190(7) 0.369(13) -0.149(7) -0.089(8) -0.031(6) C47 0.112(6) 0.218(7) 0.286(8) -0.140(6) -0.059(5) -0.027(5) C48 0.103(6) 0.170(6) 0.241(7) -0.105(5) -0.045(6) -0.026(5) C49 0.097(6) 0.148(6) 0.261(8) -0.080(5) -0.054(7) -0.028(5) C50 0.090(5) 0.126(5) 0.221(7) -0.073(4) -0.034(5) -0.014(4) C51 0.074(5) 0.145(5) 0.173(5) -0.068(4) -0.023(4) -0.027(4) C52 0.119(7) 0.188(7) 0.168(6) -0.067(4) -0.033(6) -0.062(6) C53 0.141(8) 0.190(7) 0.195(7) -0.087(5) -0.053(7) -0.044(6) C54 0.114(5) 0.62(3) 0.187(10) -0.206(14) 0.024(6) -0.095(11) C55 0.169(10) 0.315(9) 0.146(8) -0.096(7) 0.007(8) -0.012(8) C56 0.221(12) 0.368(13) 0.111(5) -0.035(7) 0.020(7) -0.136(11) C57 0.124(5) 0.343(10) 0.114(5) -0.089(5) -0.004(4) -0.070(8) C58 0.097(4) 0.270(9) 0.102(4) -0.058(5) -0.025(4) -0.042(5) C59 0.081(5) 0.290(11) 0.154(7) -0.094(6) -0.011(4) -0.056(6) C60 0.078(4) 0.216(8) 0.145(6) -0.066(5) -0.016(4) -0.044(5) C61 0.077(3) 0.147(6) 0.119(4) -0.030(3) -0.029(3) -0.032(3) C62 0.103(5) 0.195(8) 0.122(6) -0.051(4) -0.016(4) -0.058(5) C63 0.116(5) 0.216(8) 0.101(5) -0.047(5) -0.019(4) -0.058(5) C64 0.107(7) 0.169(9) 0.343(12) -0.047(9) -0.104(8) 0.003(6) C65 0.096(6) 0.153(8) 0.314(10) -0.096(8) -0.069(7) 0.002(4) C66 0.091(5) 0.137(6) 0.239(7) -0.087(5) -0.047(5) -0.007(4) C67 0.077(4) 0.125(5) 0.203(5) -0.045(4) -0.042(4) -0.025(3) C68 0.094(6) 0.186(8) 0.215(6) -0.026(6) -0.065(5) -0.015(4) C69 0.139(9) 0.216(11) 0.281(9) -0.009(9) -0.095(7) 0.008(7) C70 0.070(3) 0.131(4) 0.154(4) -0.050(3) -0.025(2) -0.023(2) C71 0.066(3) 0.141(4) 0.114(5) -0.047(3) -0.018(3) -0.022(2) C72 0.061(3) 0.149(5) 0.131(6) -0.038(4) -0.011(4) -0.019(3) C73 0.056(3) 0.155(5) 0.106(5) -0.035(3) -0.010(3) -0.014(3) C74 0.058(3) 0.139(4) 0.094(4) -0.051(3) -0.015(3) -0.016(2) C75 0.061(3) 0.146(5) 0.108(5) -0.042(3) -0.017(3) -0.016(3) C76 0.061(3) 0.132(4) 0.126(5) -0.053(3) -0.018(4) -0.014(3) N77 0.058(3) 0.157(4) 0.089(3) -0.035(3) -0.022(3) -0.021(3) C78 0.056(4) 0.156(5) 0.086(4) -0.040(3) -0.016(3) -0.020(3) O79 0.076(3) 0.162(4) 0.114(3) -0.026(3) -0.039(2) -0.030(3) N80 0.40(4) 0.232(15) 0.42(5) -0.08(3) 0.02(4) -0.11(3) N81 0.27(2) 0.236(14) 0.38(3) -0.06(3) 0.00(3) -0.115(16) N82 0.127(11) 0.231(13) 0.30(2) -0.01(2) 0.029(17) -0.064(10) C83 0.107(5) 0.229(6) 0.155(7) -0.052(7) 0.021(6) -0.053(5) C84 0.107(5) 0.209(7) 0.203(10) -0.047(7) 0.011(6) -0.037(4) C85 0.081(4) 0.224(6) 0.151(7) -0.061(6) -0.024(4) -0.034(4) C86 0.067(4) 0.218(5) 0.097(5) -0.041(5) -0.014(4) -0.034(4) C87 0.063(3) 0.219(4) 0.093(5) -0.026(5) -0.013(4) -0.033(3) C88 0.073(4) 0.226(6) 0.148(7) -0.051(7) 0.014(5) -0.040(4) C89 0.062(3) 0.216(5) 0.106(5) -0.021(5) 0.002(4) -0.031(3) O90 0.055(3) 0.220(5) 0.150(5) -0.016(4) -0.004(3) -0.025(3) N91 0.056(3) 0.213(5) 0.139(5) -0.015(4) -0.009(4) -0.025(3) C92 0.095(5) 0.218(6) 0.135(5) -0.019(6) 0.012(4) -0.046(5) C93 0.110(4) 0.272(11) 0.135(5) -0.039(6) 0.009(6) -0.023(6) O94 0.110(4) 0.276(7) 0.182(6) -0.041(5) -0.005(4) -0.040(4) C95 0.147(5) 0.281(8) 0.154(8) -0.053(7) -0.041(7) -0.070(5) C96 0.134(6) 0.295(8) 0.259(10) -0.015(8) -0.061(8) -0.080(5) C97 0.124(5) 0.297(7) 0.250(9) -0.013(7) -0.033(7) -0.071(5) C98 0.131(5) 0.253(7) 0.204(8) -0.019(7) -0.042(7) -0.069(5) C99 0.146(6) 0.225(7) 0.162(9) -0.059(7) 0.030(7) -0.057(5) C100 0.132(5) 0.238(7) 0.144(7) -0.068(6) 0.002(6) -0.060(5) O101 0.105(4) 0.199(6) 0.249(7) -0.045(5) -0.029(5) -0.030(4) C102 0.142(9) 0.194(6) 0.266(8) -0.051(8) 0.001(8) -0.031(7) C103 0.175(10) 0.213(10) 0.270(9) -0.027(8) 0.000(9) -0.035(8) O104 0.193(6) 0.182(6) 0.219(6) -0.045(6) -0.041(6) -0.003(5) C105 0.235(8) 0.219(7) 0.225(7) -0.031(7) -0.024(7) -0.008(6) C106 0.231(9) 0.223(7) 0.221(8) -0.032(8) -0.026(7) -0.016(7) O107 0.193(7) 0.220(6) 0.136(5) -0.040(4) -0.040(4) -0.029(5) C108 0.211(11) 0.244(9) 0.123(7) -0.018(6) -0.021(6) -0.023(7) C109 0.207(10) 0.244(8) 0.077(4) -0.039(5) -0.033(5) -0.018(7) O110 0.136(5) 0.266(6) 0.080(3) -0.053(4) -0.035(3) -0.011(4) C111 0.118(8) 0.272(8) 0.111(6) -0.059(6) -0.046(5) -0.008(4) C112 0.110(6) 0.258(7) 0.108(6) -0.074(6) -0.031(4) 0.005(5) O113 0.114(4) 0.262(6) 0.076(3) -0.053(3) -0.016(3) -0.023(3) C114 0.099(5) 0.244(9) 0.085(5) -0.059(4) 0.005(4) -0.007(4) C115 0.103(5) 0.226(8) 0.090(5) -0.070(4) 0.002(4) -0.009(4) C116 0.092(5) 0.247(9) 0.112(5) -0.062(4) 0.010(5) -0.010(4) C117 0.127(7) 0.244(9) 0.114(6) -0.065(5) 0.028(4) -0.015(5) C118 0.134(7) 0.224(9) 0.123(6) -0.036(5) 0.018(5) 0.005(5) C119 0.115(6) 0.225(9) 0.105(5) -0.053(4) 0.008(5) 0.014(4) O120 0.136(5) 0.232(7) 0.189(6) -0.056(5) 0.039(5) -0.020(4) C121 0.105(5) 0.302(13) 0.170(9) -0.035(6) 0.007(7) -0.036(7) C122 0.097(4) 0.240(9) 0.191(9) -0.037(7) 0.007(6) -0.011(4) N123 0.090(3) 0.224(7) 0.142(5) -0.061(5) -0.013(4) -0.024(4) C124 0.093(3) 0.187(6) 0.146(7) -0.013(6) -0.018(5) -0.020(4) O125 0.146(6) 0.219(6) 0.241(8) -0.086(6) -0.023(5) -0.034(4) Cl126 0.0496(11) 0.218(2) 0.0840(12) -0.0234(11) -0.0109(8) -0.0326(11) N180 0.27(3) 0.26(3) 0.146(18) -0.058(19) -0.016(19) -0.03(3) N181 0.25(3) 0.23(2) 0.22(3) -0.079(19) -0.02(2) -0.05(2) N182 0.115(11) 0.198(19) 0.21(2) -0.108(16) 0.017(13) -0.068(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 8.0(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C4 . 1.570(17) yes C1 . H11 . 0.968 no C1 . H12 . 0.961 no C1 . H13 . 0.964 no C2 . C4 . 1.544(19) yes C2 . H21 . 1.066 no C2 . H22 . 1.067 no C2 . H23 . 1.070 no C3 . C4 . 1.627(17) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C3 . H33 . 0.950 no C4 . C5 . 1.540(14) yes C5 . C6 . 1.411(7) yes C5 . C10 . 1.396(8) yes C6 . C7 . 1.417(8) yes C6 . H61 . 0.932 no C7 . C8 . 1.381(10) yes C7 . H71 . 0.936 no C8 . C9 . 1.405(7) yes C8 . C27 . 1.581(10) yes C9 . C10 . 1.403(7) yes C9 . H91 . 0.919 no C10 . H101 . 0.936 no C11 . C14 . 1.530(12) yes C11 . H111 . 0.968 no C11 . H112 . 0.977 no C11 . H113 . 0.964 no C12 . C14 . 1.557(12) yes C12 . H121 . 0.974 no C12 . H122 . 0.957 no C12 . H123 . 0.962 no C13 . C14 . 1.583(9) yes C13 . H131 . 0.972 no C13 . H132 . 0.959 no C13 . H133 . 0.967 no C14 . C15 . 1.588(9) yes C15 . C16 . 1.393(7) yes C15 . C20 . 1.408(7) yes C16 . C17 . 1.409(6) yes C16 . H161 . 0.929 no C17 . C18 . 1.412(7) yes C17 . H171 . 0.936 no C18 . C19 . 1.383(7) yes C18 . C27 . 1.576(8) yes C19 . C20 . 1.413(7) yes C19 . H191 . 0.943 no C20 . H201 . 0.959 no C21 . C22 . 1.395(7) yes C21 . C26 . 1.399(7) yes C21 . H211 . 0.935 no C22 . C23 . 1.404(7) yes C22 . H221 . 0.929 no C23 . C24 . 1.419(7) yes C23 . H231 . 0.958 no C24 . C25 . 1.404(7) yes C24 . C27 . 1.582(10) yes C25 . C26 . 1.397(7) yes C25 . H251 . 0.938 no C26 . H261 . 0.962 no C27 . C28 . 1.599(8) yes C28 . C29 . 1.413(7) yes C28 . C33 . 1.381(7) yes C29 . C30 . 1.397(6) yes C29 . H291 . 0.947 no C30 . C31 . 1.389(7) yes C30 . H301 . 0.938 no C31 . C32 . 1.400(7) yes C31 . N34 . 1.437(7) yes C32 . C33 . 1.411(6) yes C32 . H321 . 0.913 no C33 . H331 . 0.945 no N34 . C35 . 1.397(8) yes N34 . H341 . 0.983 no C35 . O36 . 1.205(8) yes C35 . C37 . 1.503(7) yes C37 . C38 . 1.398(6) yes C37 . C43 . 1.399(7) yes C38 . N39 . 1.367(6) yes C38 . H381 . 0.923 no N39 . C40 . 1.494(8) yes N39 . C41 . 1.364(6) yes C40 . H401 . 0.956 no C40 . H402 . 0.959 no C40 . H403 . 0.967 no C41 . C42 . 1.403(7) yes C41 . H411 . 0.957 no C42 . C43 . 1.418(6) yes C42 . C78 . 1.481(9) yes C43 . H431 . 0.921 no C44 . C47 . 1.563(18) yes C44 . H441 . 0.950 no C44 . H442 . 0.950 no C44 . H443 . 0.950 no C45 . C47 . 1.563(14) yes C45 . H451 . 0.996 no C45 . H453 . 0.997 no C45 . H452 . 1.000 no C46 . C47 . 1.614(19) yes C46 . H461 . 0.968 no C46 . H463 . 0.961 no C46 . H462 . 0.958 no C47 . C48 . 1.600(12) yes C48 . C49 . 1.402(8) yes C48 . C53 . 1.398(8) yes C49 . C50 . 1.414(7) yes C49 . H491 . 0.927 no C50 . C51 . 1.394(7) yes C50 . H501 . 0.941 no C51 . C52 . 1.400(8) yes C51 . C70 . 1.588(9) yes C52 . C53 . 1.408(7) yes C52 . H521 . 0.953 no C53 . H531 . 0.931 no C54 . C57 . 1.542(15) yes C54 . H541 . 0.950 no C54 . H542 . 0.950 no C54 . H543 . 0.950 no C55 . C57 . 1.565(16) yes C55 . H552 . 0.965 no C55 . H551 . 0.963 no C55 . H553 . 0.962 no C56 . C57 . 1.554(16) yes C56 . H562 . 0.973 no C56 . H561 . 0.965 no C56 . H563 . 0.984 no C57 . C58 . 1.540(12) yes C58 . C59 . 1.392(7) yes C58 . C63 . 1.380(7) yes C59 . C60 . 1.404(7) yes C59 . H591 . 0.944 no C60 . C61 . 1.384(7) yes C60 . H601 . 0.942 no C61 . C62 . 1.394(7) yes C61 . C70 . 1.594(10) yes C62 . C63 . 1.394(7) yes C62 . H621 . 0.941 no C63 . H631 . 0.933 no C64 . C65 . 1.397(9) yes C64 . C69 . 1.405(9) yes C64 . H641 . 0.924 no C65 . C66 . 1.403(8) yes C65 . H651 . 0.936 no C66 . C67 . 1.405(8) yes C66 . H661 . 0.921 no C67 . C68 . 1.411(8) yes C67 . C70 . 1.564(10) yes C68 . C69 . 1.408(8) yes C68 . H681 . 0.926 no C69 . H691 . 0.936 no C70 . C71 . 1.593(10) yes C71 . C72 . 1.394(7) yes C71 . C76 . 1.394(7) yes C72 . C73 . 1.388(7) yes C72 . H721 . 0.926 no C73 . C74 . 1.403(7) yes C73 . H731 . 0.947 no C74 . C75 . 1.389(7) yes C74 . N77 . 1.433(8) yes C75 . C76 . 1.403(7) yes C75 . H751 . 0.931 no C76 . H761 . 0.938 no N77 . C78 . 1.361(8) yes N77 . H771 . 0.972 no C78 . O79 . 1.254(7) yes N80 . N81 . 1.17138(10) yes N81 . N82 . 1.16994(10) yes N82 . C83 . 1.41(3) yes C83 . C84 . 1.380(14) yes C83 . C88 . 1.450(13) yes C84 . C85 . 1.403(13) yes C84 . H841 . 0.941 no C85 . C86 . 1.389(12) yes C85 . C124 . 1.514(14) yes C86 . C87 . 1.385(11) yes C86 . H861 . 0.933 no C87 . C88 . 1.403(11) yes C87 . C89 . 1.517(12) yes C88 . H881 . 0.952 no C89 . O90 . 1.232(9) yes C89 . N91 . 1.376(10) yes N91 . C92 . 1.546(12) yes N91 . H911 . 0.972 no C92 . C93 . 1.544(14) yes C92 . H922 . 0.961 no C92 . H921 . 0.974 no C93 . O94 . 1.352(11) yes C93 . H931 . 0.986 no C93 . H932 . 0.990 no O94 . C95 . 1.392(8) yes C95 . C96 . 1.377(9) yes C95 . C100 . 1.349(8) yes C96 . C97 . 1.417(8) yes C96 . H961 . 0.938 no C97 . C98 . 1.370(8) yes C97 . H971 . 0.941 no C98 . C99 . 1.363(8) yes C98 . O101 . 1.385(7) yes C99 . C100 . 1.365(8) yes C99 . H991 . 0.931 no C100 . H1001 . 0.931 no O101 . C102 . 1.382(8) yes C102 . C103 . 1.487(5) yes C102 . H1022 . 0.970 no C102 . H1021 . 0.977 no C103 . O104 . 1.399(8) yes C103 . H1031 . 0.950 no C103 . H1032 . 0.950 no O104 . C105 . 1.352(8) yes C105 . C106 . 1.489(5) yes C105 . H1051 . 0.950 no C105 . H1052 . 0.950 no C106 . O107 . 1.372(8) yes C106 . H1062 . 0.992 no C106 . H1061 . 0.986 no O107 . C108 . 1.354(8) yes C108 . C109 . 1.493(5) yes C108 . H1081 . 0.971 no C108 . H1082 . 0.987 no C109 . O110 . 1.385(7) yes C109 . H1092 . 0.963 no C109 . H1091 . 0.973 no O110 . C111 . 1.403(7) yes C111 . C112 . 1.500(5) yes C111 . H1111 . 0.962 no C111 . H1112 . 0.979 no C112 . O113 . 1.418(7) yes C112 . H1121 . 0.981 no C112 . H1122 . 0.984 no O113 . C114 . 1.386(7) yes C114 . C115 . 1.395(7) yes C114 . C119 . 1.391(8) yes C115 . C116 . 1.407(8) yes C115 . H1151 . 0.951 no C116 . C117 . 1.394(8) yes C116 . H1161 . 0.953 no C117 . C118 . 1.404(8) yes C117 . O120 . 1.422(8) yes C118 . C119 . 1.407(8) yes C118 . H1181 . 0.922 no C119 . H1191 . 0.929 no O120 . C121 . 1.269(14) yes C121 . C122 . 1.514(5) yes C121 . H1211 . 0.950 no C121 . H1212 . 0.950 no C122 . N123 . 1.495(12) yes C122 . H1221 . 0.955 no C122 . H1222 . 0.970 no N123 . C124 . 1.381(11) yes N123 . H1231 . 0.987 no C124 . O125 . 1.268(11) yes N180 . N181 . 1.16974(10) yes N181 . N182 . 1.17018(10) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 . C1 . H11 . 105.7 no C4 . C1 . H12 . 112.1 no H11 . C1 . H12 . 109.4 no C4 . C1 . H13 . 112.0 no H11 . C1 . H13 . 109.2 no H12 . C1 . H13 . 108.3 no C4 . C2 . H21 . 107.1 no C4 . C2 . H22 . 109.5 no H21 . C2 . H22 . 111.7 no C4 . C2 . H23 . 105.7 no H21 . C2 . H23 . 111.9 no H22 . C2 . H23 . 110.7 no C4 . C3 . H31 . 112.0 no C4 . C3 . H32 . 106.6 no H31 . C3 . H32 . 109.5 no C4 . C3 . H33 . 109.8 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no C2 . C4 . C1 . 103.7(13) yes C2 . C4 . C3 . 102.8(13) yes C1 . C4 . C3 . 109.8(13) yes C2 . C4 . C5 . 115.3(10) yes C1 . C4 . C5 . 115.8(11) yes C3 . C4 . C5 . 108.7(9) yes C4 . C5 . C6 . 121.9(8) yes C4 . C5 . C10 . 120.5(7) yes C6 . C5 . C10 . 117.6(6) yes C5 . C6 . C7 . 120.4(6) yes C5 . C6 . H61 . 119.9 no C7 . C6 . H61 . 119.7 no C6 . C7 . C8 . 121.2(5) yes C6 . C7 . H71 . 118.4 no C8 . C7 . H71 . 120.4 no C7 . C8 . C9 . 118.7(6) yes C7 . C8 . C27 . 123.6(5) yes C9 . C8 . C27 . 117.7(6) yes C8 . C9 . C10 . 120.2(5) yes C8 . C9 . H91 . 120.5 no C10 . C9 . H91 . 119.3 no C9 . C10 . C5 . 121.8(5) yes C9 . C10 . H101 . 119.1 no C5 . C10 . H101 . 119.1 no C14 . C11 . H111 . 108.0 no C14 . C11 . H112 . 108.4 no H111 . C11 . H112 . 109.8 no C14 . C11 . H113 . 107.7 no H111 . C11 . H113 . 111.5 no H112 . C11 . H113 . 111.4 no C14 . C12 . H121 . 111.6 no C14 . C12 . H122 . 108.2 no H121 . C12 . H122 . 109.2 no C14 . C12 . H123 . 106.1 no H121 . C12 . H123 . 110.8 no H122 . C12 . H123 . 110.9 no C14 . C13 . H131 . 111.1 no C14 . C13 . H132 . 107.9 no H131 . C13 . H132 . 109.5 no C14 . C13 . H133 . 107.3 no H131 . C13 . H133 . 111.7 no H132 . C13 . H133 . 109.3 no C11 . C14 . C12 . 110.5(6) yes C11 . C14 . C13 . 110.4(6) yes C12 . C14 . C13 . 108.8(7) yes C11 . C14 . C15 . 109.5(6) yes C12 . C14 . C15 . 110.2(6) yes C13 . C14 . C15 . 107.4(5) yes C14 . C15 . C16 . 122.6(6) yes C14 . C15 . C20 . 119.8(5) yes C16 . C15 . C20 . 117.6(5) yes C15 . C16 . C17 . 121.7(5) yes C15 . C16 . H161 . 117.8 no C17 . C16 . H161 . 120.4 no C16 . C17 . C18 . 120.3(5) yes C16 . C17 . H171 . 120.5 no C18 . C17 . H171 . 119.1 no C17 . C18 . C19 . 118.1(5) yes C17 . C18 . C27 . 118.4(5) yes C19 . C18 . C27 . 123.5(6) yes C18 . C19 . C20 . 121.5(5) yes C18 . C19 . H191 . 119.3 no C20 . C19 . H191 . 119.2 no C19 . C20 . C15 . 120.7(5) yes C19 . C20 . H201 . 118.7 no C15 . C20 . H201 . 120.5 no C22 . C21 . C26 . 119.3(5) yes C22 . C21 . H211 . 121.4 no C26 . C21 . H211 . 119.2 no C21 . C22 . C23 . 120.3(5) yes C21 . C22 . H221 . 117.8 no C23 . C22 . H221 . 121.9 no C22 . C23 . C24 . 120.7(5) yes C22 . C23 . H231 . 121.0 no C24 . C23 . H231 . 118.3 no C23 . C24 . C25 . 118.1(5) yes C23 . C24 . C27 . 118.4(5) yes C25 . C24 . C27 . 123.5(5) yes C24 . C25 . C26 . 120.8(5) yes C24 . C25 . H251 . 118.2 no C26 . C25 . H251 . 121.0 no C21 . C26 . C25 . 120.7(5) yes C21 . C26 . H261 . 119.5 no C25 . C26 . H261 . 119.8 no C18 . C27 . C8 . 112.3(6) yes C18 . C27 . C24 . 110.4(5) yes C8 . C27 . C24 . 107.1(5) yes C18 . C27 . C28 . 106.1(4) yes C8 . C27 . C28 . 110.1(5) yes C24 . C27 . C28 . 110.9(5) yes C27 . C28 . C29 . 118.1(5) yes C27 . C28 . C33 . 123.4(5) yes C29 . C28 . C33 . 118.5(4) yes C28 . C29 . C30 . 121.9(5) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 118.1 no C29 . C30 . C31 . 119.4(5) yes C29 . C30 . H301 . 120.6 no C31 . C30 . H301 . 120.0 no C30 . C31 . C32 . 119.2(4) yes C30 . C31 . N34 . 123.8(5) yes C32 . C31 . N34 . 117.0(5) yes C31 . C32 . C33 . 121.2(5) yes C31 . C32 . H321 . 119.3 no C33 . C32 . H321 . 119.4 no C32 . C33 . C28 . 119.9(5) yes C32 . C33 . H331 . 120.1 no C28 . C33 . H331 . 120.0 no C31 . N34 . C35 . 126.9(5) yes C31 . N34 . H341 . 117.1 no C35 . N34 . H341 . 116.0 no N34 . C35 . O36 . 124.1(5) yes N34 . C35 . C37 . 115.2(6) yes O36 . C35 . C37 . 120.3(6) yes C35 . C37 . C38 . 116.3(5) yes C35 . C37 . C43 . 124.8(5) yes C38 . C37 . C43 . 118.9(4) yes C37 . C38 . N39 . 120.5(5) yes C37 . C38 . H381 . 120.0 no N39 . C38 . H381 . 119.5 no C38 . N39 . C40 . 119.1(5) yes C38 . N39 . C41 . 121.5(4) yes C40 . N39 . C41 . 119.4(5) yes N39 . C40 . H401 . 113.5 no N39 . C40 . H402 . 110.4 no H401 . C40 . H402 . 108.2 no N39 . C40 . H403 . 110.6 no H401 . C40 . H403 . 108.0 no H402 . C40 . H403 . 105.7 no N39 . C41 . C42 . 120.6(4) yes N39 . C41 . H411 . 118.1 no C42 . C41 . H411 . 121.3 no C41 . C42 . C43 . 118.2(5) yes C41 . C42 . C78 . 117.7(5) yes C43 . C42 . C78 . 124.1(5) yes C42 . C43 . C37 . 120.4(4) yes C42 . C43 . H431 . 118.6 no C37 . C43 . H431 . 121.0 no C47 . C44 . H441 . 108.9 no C47 . C44 . H442 . 109.9 no H441 . C44 . H442 . 109.5 no C47 . C44 . H443 . 109.6 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no C47 . C45 . H451 . 109.6 no C47 . C45 . H453 . 108.5 no H451 . C45 . H453 . 110.6 no C47 . C45 . H452 . 106.1 no H451 . C45 . H452 . 110.7 no H453 . C45 . H452 . 111.1 no C47 . C46 . H461 . 109.2 no C47 . C46 . H463 . 111.4 no H461 . C46 . H463 . 109.1 no C47 . C46 . H462 . 108.6 no H461 . C46 . H462 . 109.5 no H463 . C46 . H462 . 108.9 no C45 . C47 . C44 . 109.6(13) yes C45 . C47 . C46 . 107.2(9) yes C44 . C47 . C46 . 114.2(10) yes C45 . C47 . C48 . 107.2(7) yes C44 . C47 . C48 . 111.0(8) yes C46 . C47 . C48 . 107.4(11) yes C47 . C48 . C49 . 124.3(9) yes C47 . C48 . C53 . 116.9(9) yes C49 . C48 . C53 . 118.8(6) yes C48 . C49 . C50 . 121.3(6) yes C48 . C49 . H491 . 121.1 no C50 . C49 . H491 . 117.6 no C49 . C50 . C51 . 119.8(6) yes C49 . C50 . H501 . 121.9 no C51 . C50 . H501 . 118.3 no C50 . C51 . C52 . 118.7(5) yes C50 . C51 . C70 . 116.5(6) yes C52 . C51 . C70 . 124.8(6) yes C51 . C52 . C53 . 121.8(6) yes C51 . C52 . H521 . 119.4 no C53 . C52 . H521 . 118.8 no C52 . C53 . C48 . 119.5(6) yes C52 . C53 . H531 . 120.1 no C48 . C53 . H531 . 120.3 no C57 . C54 . H541 . 108.1 no C57 . C54 . H542 . 109.9 no H541 . C54 . H542 . 109.5 no C57 . C54 . H543 . 110.4 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no C57 . C55 . H552 . 106.0 no C57 . C55 . H551 . 107.7 no H552 . C55 . H551 . 110.3 no C57 . C55 . H553 . 112.7 no H552 . C55 . H553 . 110.1 no H551 . C55 . H553 . 109.9 no C57 . C56 . H562 . 108.1 no C57 . C56 . H561 . 112.0 no H562 . C56 . H561 . 108.6 no C57 . C56 . H563 . 108.9 no H562 . C56 . H563 . 108.9 no H561 . C56 . H563 . 110.2 no C54 . C57 . C56 . 112.4(12) yes C54 . C57 . C55 . 105.5(11) yes C56 . C57 . C55 . 105.7(9) yes C54 . C57 . C58 . 111.6(8) yes C56 . C57 . C58 . 108.1(9) yes C55 . C57 . C58 . 113.4(8) yes C57 . C58 . C59 . 125.1(7) yes C57 . C58 . C63 . 117.7(6) yes C59 . C58 . C63 . 117.2(5) yes C58 . C59 . C60 . 121.9(5) yes C58 . C59 . H591 . 118.5 no C60 . C59 . H591 . 119.6 no C59 . C60 . C61 . 120.3(5) yes C59 . C60 . H601 . 119.9 no C61 . C60 . H601 . 119.7 no C60 . C61 . C62 . 117.8(5) yes C60 . C61 . C70 . 123.8(5) yes C62 . C61 . C70 . 118.3(5) yes C61 . C62 . C63 . 121.4(5) yes C61 . C62 . H621 . 118.1 no C63 . C62 . H621 . 120.5 no C62 . C63 . C58 . 121.3(5) yes C62 . C63 . H631 . 121.3 no C58 . C63 . H631 . 117.3 no C65 . C64 . C69 . 119.6(6) yes C65 . C64 . H641 . 120.7 no C69 . C64 . H641 . 119.6 no C64 . C65 . C66 . 120.4(6) yes C64 . C65 . H651 . 119.5 no C66 . C65 . H651 . 120.1 no C65 . C66 . C67 . 120.4(6) yes C65 . C66 . H661 . 120.3 no C67 . C66 . H661 . 119.2 no C66 . C67 . C68 . 119.2(6) yes C66 . C67 . C70 . 118.1(7) yes C68 . C67 . C70 . 122.7(7) yes C67 . C68 . C69 . 120.1(6) yes C67 . C68 . H681 . 119.9 no C69 . C68 . H681 . 120.1 no C68 . C69 . C64 . 120.2(6) yes C68 . C69 . H691 . 119.8 no C64 . C69 . H691 . 120.0 no C67 . C70 . C51 . 106.5(5) yes C67 . C70 . C61 . 111.1(7) yes C51 . C70 . C61 . 112.4(5) yes C67 . C70 . C71 . 112.0(5) yes C51 . C70 . C71 . 109.4(6) yes C61 . C70 . C71 . 105.5(5) yes C70 . C71 . C72 . 117.5(5) yes C70 . C71 . C76 . 124.0(5) yes C72 . C71 . C76 . 118.5(5) yes C71 . C72 . C73 . 121.4(5) yes C71 . C72 . H721 . 119.0 no C73 . C72 . H721 . 119.6 no C72 . C73 . C74 . 120.3(5) yes C72 . C73 . H731 . 120.5 no C74 . C73 . H731 . 119.1 no C73 . C74 . C75 . 118.6(5) yes C73 . C74 . N77 . 116.5(5) yes C75 . C74 . N77 . 124.9(5) yes C74 . C75 . C76 . 121.0(5) yes C74 . C75 . H751 . 117.7 no C76 . C75 . H751 . 121.3 no C75 . C76 . C71 . 120.3(5) yes C75 . C76 . H761 . 121.3 no C71 . C76 . H761 . 118.4 no C74 . N77 . C78 . 126.7(6) yes C74 . N77 . H771 . 117.6 no C78 . N77 . H771 . 115.7 no C42 . C78 . N77 . 116.0(6) yes C42 . C78 . O79 . 120.5(6) yes N77 . C78 . O79 . 123.4(7) yes N80 . N81 . N82 . 177.651 yes N81 . N82 . C83 . 127.6(13) yes N82 . C83 . C84 . 121.4(16) yes N82 . C83 . C88 . 121.8(15) yes C84 . C83 . C88 . 116.7(9) yes C83 . C84 . C85 . 124.0(11) yes C83 . C84 . H841 . 116.6 no C85 . C84 . H841 . 119.4 no C84 . C85 . C86 . 117.0(9) yes C84 . C85 . C124 . 114.9(10) yes C86 . C85 . C124 . 128.1(9) yes C85 . C86 . C87 . 123.0(8) yes C85 . C86 . H861 . 116.4 no C87 . C86 . H861 . 120.5 no C86 . C87 . C88 . 118.8(9) yes C86 . C87 . C89 . 124.4(8) yes C88 . C87 . C89 . 116.8(7) yes C83 . C88 . C87 . 120.5(8) yes C83 . C88 . H881 . 119.5 no C87 . C88 . H881 . 120.0 no C87 . C89 . O90 . 120.8(8) yes C87 . C89 . N91 . 115.9(7) yes O90 . C89 . N91 . 122.9(9) yes C89 . N91 . C92 . 121.1(7) yes C89 . N91 . H911 . 118.7 no C92 . N91 . H911 . 120.3 no N91 . C92 . C93 . 112.4(9) yes N91 . C92 . H922 . 111.4 no C93 . C92 . H922 . 109.5 no N91 . C92 . H921 . 106.6 no C93 . C92 . H921 . 108.1 no H922 . C92 . H921 . 108.7 no C92 . C93 . O94 . 110.1(8) yes C92 . C93 . H931 . 113.3 no O94 . C93 . H931 . 103.7 no C92 . C93 . H932 . 107.6 no O94 . C93 . H932 . 109.4 no H931 . C93 . H932 . 112.6 no C93 . O94 . C95 . 120.7(9) yes O94 . C95 . C96 . 122.9(7) yes O94 . C95 . C100 . 116.0(8) yes C96 . C95 . C100 . 121.1(6) yes C95 . C96 . C97 . 118.5(6) yes C95 . C96 . H961 . 119.6 no C97 . C96 . H961 . 121.7 no C96 . C97 . C98 . 119.0(6) yes C96 . C97 . H971 . 120.2 no C98 . C97 . H971 . 120.8 no C97 . C98 . C99 . 120.4(6) yes C97 . C98 . O101 . 128.7(7) yes C99 . C98 . O101 . 110.8(7) yes C98 . C99 . C100 . 120.6(6) yes C98 . C99 . H991 . 117.4 no C100 . C99 . H991 . 122.0 no C99 . C100 . C95 . 120.2(6) yes C99 . C100 . H1001 . 120.8 no C95 . C100 . H1001 . 119.0 no C98 . O101 . C102 . 117.2(4) yes O101 . C102 . C103 . 116.0(4) yes O101 . C102 . H1022 . 109.0 no C103 . C102 . H1022 . 98.1 no O101 . C102 . H1021 . 107.5 no C103 . C102 . H1021 . 114.5 no H1022 . C102 . H1021 . 111.5 no C102 . C103 . O104 . 116.3(4) yes C102 . C103 . H1031 . 105.9 no O104 . C103 . H1031 . 107.0 no C102 . C103 . H1032 . 109.0 no O104 . C103 . H1032 . 109.0 no H1031 . C103 . H1032 . 109.5 no C103 . O104 . C105 . 117.9(4) yes O104 . C105 . C106 . 116.0(5) yes O104 . C105 . H1051 . 103.1 no C106 . C105 . H1051 . 104.4 no O104 . C105 . H1052 . 112.1 no C106 . C105 . H1052 . 111.0 no H1051 . C105 . H1052 . 109.5 no C105 . C106 . O107 . 116.1(4) yes C105 . C106 . H1062 . 91.2 no O107 . C106 . H1062 . 105.1 no C105 . C106 . H1061 . 116.5 no O107 . C106 . H1061 . 114.4 no H1062 . C106 . H1061 . 110.2 no C106 . O107 . C108 . 117.6(4) yes O107 . C108 . C109 . 117.8(4) yes O107 . C108 . H1081 . 98.0 no C109 . C108 . H1081 . 102.3 no O107 . C108 . H1082 . 111.9 no C109 . C108 . H1082 . 113.3 no H1081 . C108 . H1082 . 111.9 no C108 . C109 . O110 . 116.7(4) yes C108 . C109 . H1092 . 112.2 no O110 . C109 . H1092 . 108.4 no C108 . C109 . H1091 . 100.3 no O110 . C109 . H1091 . 108.9 no H1092 . C109 . H1091 . 109.9 no C109 . O110 . C111 . 118.7(4) yes O110 . C111 . C112 . 116.5(4) yes O110 . C111 . H1111 . 111.5 no C112 . C111 . H1111 . 111.1 no O110 . C111 . H1112 . 103.9 no C112 . C111 . H1112 . 102.5 no H1111 . C111 . H1112 . 110.7 no C111 . C112 . O113 . 115.6(4) yes C111 . C112 . H1121 . 107.1 no O113 . C112 . H1121 . 109.0 no C111 . C112 . H1122 . 110.5 no O113 . C112 . H1122 . 106.8 no H1121 . C112 . H1122 . 107.6 no C112 . O113 . C114 . 120.3(4) yes O113 . C114 . C115 . 115.2(6) yes O113 . C114 . C119 . 124.8(6) yes C115 . C114 . C119 . 120.0(6) yes C114 . C115 . C116 . 119.5(6) yes C114 . C115 . H1151 . 120.2 no C116 . C115 . H1151 . 120.3 no C115 . C116 . C117 . 121.3(6) yes C115 . C116 . H1161 . 118.9 no C117 . C116 . H1161 . 119.7 no C116 . C117 . C118 . 118.5(6) yes C116 . C117 . O120 . 113.9(9) yes C118 . C117 . O120 . 127.6(9) yes C117 . C118 . C119 . 120.4(6) yes C117 . C118 . H1181 . 119.1 no C119 . C118 . H1181 . 120.4 no C118 . C119 . C114 . 120.2(6) yes C118 . C119 . H1191 . 120.5 no C114 . C119 . H1191 . 119.3 no C117 . O120 . C121 . 117.2(10) yes O120 . C121 . C122 . 106.0(11) yes O120 . C121 . H1211 . 115.5 no C122 . C121 . H1211 . 109.8 no O120 . C121 . H1212 . 108.2 no C122 . C121 . H1212 . 107.5 no H1211 . C121 . H1212 . 109.5 no C121 . C122 . N123 . 109.7(9) yes C121 . C122 . H1221 . 114.5 no N123 . C122 . H1221 . 109.0 no C121 . C122 . H1222 . 104.5 no N123 . C122 . H1222 . 108.1 no H1221 . C122 . H1222 . 110.7 no C122 . N123 . C124 . 118.9(9) yes C122 . N123 . H1231 . 119.3 no C124 . N123 . H1231 . 121.7 no C85 . C124 . N123 . 115.7(10) yes C85 . C124 . O125 . 123.6(9) yes N123 . C124 . O125 . 119.7(9) yes N180 . N181 . N182 . 176.971 yes C83 . N182 . N181 . 107.8(10) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C7 . H71 . C29 . 124.9(2) 0.936 2.528 3.159(12) yes C19 . H191 . C9 . 124.5(2) 0.943 2.559 3.190(12) yes C22 . H221 . O113 1_455 147.95(19) 0.929 2.579 3.403(12) yes C25 . H251 . C17 . 126.23(19) 0.938 2.492 3.139(12) yes C30 . H301 . O36 . 122.7(2) 0.938 2.262 2.879(12) yes C33 . H331 . C23 . 124.2(2) 0.945 2.553 3.181(12) yes C38 . H381 . O107 . 151.4(2) 0.923 2.524 3.364(12) yes C41 . H411 . O90 1_655 123.51(16) 0.957 2.581 3.210(12) yes C52 . H521 . C72 . 121.0(2) 0.953 2.494 3.094(12) yes C53 . H531 . O125 . 147.7(3) 0.931 2.323 3.150(12) yes C60 . H601 . C50 . 121.3(2) 0.942 2.580 3.173(12) yes C68 . H681 . C62 . 122.6(3) 0.926 2.532 3.129(12) yes C76 . H761 . C66 . 125.0(2) 0.938 2.468 3.103(12) yes C88 . H881 . O79 1_455 160.9(3) 0.952 2.549 3.462(12) yes C99 . H991 . C41 . 139.3(2) 0.931 2.596 3.357(12) yes C99 . H991 . O79 2_767 124.7(2) 0.931 2.524 3.149(12) yes _iucr_refine_instruction_details_constraints ; # # Punched on 17/05/12 at 17:03:26 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE N ( 34,X'S) H ( 341,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 40,X'S) H ( 401,X'S) H ( 402,X'S) H ( 403,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 453,X'S) H ( 452,X'S) RIDE C ( 46,X'S) H ( 461,X'S) H ( 463,X'S) H ( 462,X'S) RIDE C ( 49,X'S) H ( 491,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) H ( 543,X'S) RIDE C ( 55,X'S) H ( 552,X'S) H ( 551,X'S) H ( 553,X'S) RIDE C ( 56,X'S) H ( 562,X'S) H ( 561,X'S) H ( 563,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE C ( 60,X'S) H ( 601,X'S) RIDE C ( 62,X'S) H ( 621,X'S) RIDE C ( 63,X'S) H ( 631,X'S) RIDE C ( 64,X'S) H ( 641,X'S) RIDE C ( 65,X'S) H ( 651,X'S) RIDE C ( 66,X'S) H ( 661,X'S) RIDE C ( 68,X'S) H ( 681,X'S) RIDE C ( 69,X'S) H ( 691,X'S) RIDE C ( 72,X'S) H ( 721,X'S) RIDE C ( 73,X'S) H ( 731,X'S) RIDE C ( 75,X'S) H ( 751,X'S) RIDE C ( 76,X'S) H ( 761,X'S) RIDE N ( 77,X'S) H ( 771,X'S) RIDE C ( 84,X'S) H ( 841,X'S) RIDE C ( 86,X'S) H ( 861,X'S) RIDE C ( 88,X'S) H ( 881,X'S) RIDE N ( 91,X'S) H ( 911,X'S) RIDE C ( 92,X'S) H ( 922,X'S) H ( 921,X'S) RIDE C ( 93,X'S) H ( 931,X'S) H ( 932,X'S) RIDE C ( 96,X'S) H ( 961,X'S) RIDE C ( 97,X'S) H ( 971,X'S) RIDE C ( 99,X'S) H ( 991,X'S) RIDE C ( 100,X'S) H (1001,X'S) RIDE C ( 102,X'S) H (1022,X'S) H (1021,X'S) RIDE C ( 103,X'S) H (1031,X'S) H (1032,X'S) RIDE C ( 105,X'S) H (1051,X'S) H (1052,X'S) RIDE C ( 106,X'S) H (1062,X'S) H (1061,X'S) RIDE C ( 108,X'S) H (1081,X'S) H (1082,X'S) RIDE C ( 109,X'S) H (1092,X'S) H (1091,X'S) RIDE C ( 111,X'S) H (1111,X'S) H (1112,X'S) RIDE C ( 112,X'S) H (1121,X'S) H (1122,X'S) RIDE C ( 115,X'S) H (1151,X'S) RIDE C ( 116,X'S) H (1161,X'S) RIDE C ( 118,X'S) H (1181,X'S) RIDE C ( 119,X'S) H (1191,X'S) RIDE C ( 121,X'S) H (1211,X'S) H (1212,X'S) RIDE C ( 122,X'S) H (1221,X'S) H (1222,X'S) RIDE N ( 123,X'S) H (1231,X'S) RIDE N ( 82,X'S) N (81,X'S) N(80,X'S) RIDE N ( 182,X'S) N (181,X'S) N(180,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 17/05/12 at 17:03:26 # #LIST 16 PLANAR C(21) C(22) C(23) C(24) C(25) C(26) PLANAR C(14) C(15) C(16) C(17) C(18) C(19) C(20) PLANAR C(4) C(5) C(6) C(7) C(8) C(9) C(10) PLANAR C(14) C(15) C(16) C(17) C(18) C(19) C(20) PLANAR C(28) C(29) C(30) C(31) C(32) C(33) N(34) PLANAR C(47) C(48) C(49) C(50) C(51) C(52) C(53) PLANAR C(57) C(58) C(59) C(60) C(61) C(62) C(63) PLANAR C(64) C(65) C(66) C(67) C(68) C(69) PLANAR C(71) C(72) C(73) C(74) C(75) C(76) N(77) PLANAR C(35) C(37) C(38) N(39) C(40) C(41) CONT C(42) C(43) C(78) PLANAR N(82) C(83) C(84) C(85) C(86) C(87) C(88) CONT C(89) O(90) C(124) O(125) PLANAR N(182) C(83) C(84) C(85) C(86) C(87) C(88) CONT C(89) O(90) C(124) O(125) PLANAR O(94) C(95) C(96) C(97) C(98) C(99) C(100) CONT O(101) PLANAR O(113) C(114) C(115) C(116) C(117) C(118) CONT C(119) O(120) DIST 1.4, 0.01 = C(98) TO C(99), C(99) TO C(100) CONT C(100) TO C(95), C(95) TO C(96), C(96) TO C(97) CONT C(97) TO C(98) DIST 1.4, 0.01 = C(114) TO C(115), C(115) TO C(116) CONT C(116) TO C(117), C(117) TO C(118), C(118) TO C(119) CONT C(119) TO C(114) ANGL 120, 1.0 = C(114) TO C(115) TO C(116) CONT C(115) TO C(116) TO C(117), C(116) TO C(117) TO C(118) CONT C(117) TO C(118) TO C(119), C(118) TO C(119) TO C(114) CONT C(119) TO C(114) TO C(115) ANGL 120, 1.0 = C(98) TO C(99) TO C(100) CONT C(99) TO C(100) TO C(95), C(100) TO C(95) TO C(96) CONT C(95) TO C(96) TO C(97), C(96) TO C(97) TO C(98) CONT C(97) TO C(98) TO C(99) DIST 1.40, 0.01 = C(5) TO C(6), C(6) TO C(7), C(8) TO C(9) CONT C(9) TO C(10), C(10) TO C(5), C(15) TO C(16) CONT C(16) TO C(17), C(17) TO C(18), C(18) TO C(19) CONT C(19) TO C(20), C(20) TO C(15), C(21) TO C(22) CONT C(22) TO C(23), C(23) TO C(24), C(24) TO C(25) CONT C(25) TO C(26), C(26) TO C(21), C(28) TO C(29) CONT C(29) TO C(30), C(30) TO C(31), C(31) TO C(32) CONT C(32) TO C(33), C(33) TO C(28) DIST 1.40, 0.01 = C(37) TO C(38), C(38) TO N(39) CONT N(39) TO C(41), C(41) TO C(42), C(42) TO C(43) CONT C(43) TO C(37) DIST 1.40, 0.01 = C(48) TO C(49), C(49) TO C(50) CONT C(50) TO C(51), C(51) TO C(52), C(52) TO C(53) CONT C(53) TO C(48), C(58) TO C(59), C(59) TO C(60) CONT C(60) TO C(61), C(61) TO C(62), C(62) TO C(63) CONT C(63) TO C(58), C(64) TO C(65), C(65) TO C(66) CONT C(66) TO C(67), C(67) TO C(68), C(68) TO C(69) CONT C(69) TO C(64), C(71) TO C(72), C(72) TO C(73) CONT C(73) TO C(74), C(74) TO C(75), C(75) TO C(76) CONT C(76) TO C(71) ANGLE 120, 1.0 = C(5) TO C(6) TO C(7), C(6) TO C(7) TO C(8) CONT C(7) TO C(8) TO C(9), C(8) TO C(9) TO C(10) CONT C(9) TO C(10) TO C(5), C(10) TO C(5) TO C(6) ANGLE 120, 1.0 = C(15) TO C(16) TO C(17) CONT C(16) TO C(17) TO C(18), C(17) TO C(18) TO C(19) CONT C(18) TO C(19) TO C(20), C(19) TO C(20) TO C(15) CONT C(20) TO C(15) TO C(16) ANGLE 120, 1.0 = C(21) TO C(22) TO C(23), CONT C(22) TO C(23) TO C(24), C(23) TO C(24) TO C(25) CONT C(24) TO C(25) TO C(26), C(25) TO C(26) TO C(21) CONT C(26) TO C(21) TO C(22) ANGLE 120, 1.0 = C(28) TO C(29) TO C(30), CONT C(29) TO C(30) TO C(31), C(30) TO C(31) TO C(32) CONT C(31) TO C(32) TO C(33), C(32) TO C(33) TO C(28) CONT C(33) TO C(28) TO C(29) ANGLE 120, 1.0 = C(48) TO C(49) TO C(50) CONT C(49) TO C(50) TO C(51), C(50) TO C(51) TO C(52) CONT C(51) TO C(52) TO C(53), C(52) TO C(53) TO C(48) CONT C(53) TO C(48) TO C(49) ANGLE 120, 1.0 = C(58) TO C(59) TO C(60) CONT C(59) TO C(60) TO C(61), C(60) TO C(61) TO C(62) CONT C(61) TO C(62) TO C(63), C(62) TO C(63) TO C(58) CONT C(63) TO C(58) TO C(59) ANGLE 120, 1.0 = C(64) TO C(65) TO C(66), CONT C(65) TO C(66) TO C(67), C(66) TO C(67) TO C(68) CONT C(67) TO C(68) TO C(69), C(68) TO C(69) TO C(64) CONT C(69) TO C(64) TO C(65) ANGLE 120, 1.0 = C(71) TO C(72) TO C(73) CONT C(72) TO C(73) TO C(74), C(73) TO C(74) TO C(75) CONT C(74) TO C(75) TO C(76), C(75) TO C(76) TO C(71) CONT C(76) TO C(71) TO C(72) ANGLE 120, 1.0 = C(37) TO C(38) TO N(39) CONT C(38) TO N(39) TO C(41), N(39) TO C(41) TO C(42) CONT C(41) TO C(42) TO C(43), C(42) TO C(43) TO C(37) CONT C(43) TO C(37) TO C(38) DISTANCE 1.520000 , 0.050000 = C(1) TO C(4) DIST 1.52, 0.005 = C(102) TO C(103), C(105) TO C(106) CONT C(108) TO C(109), C(111) TO C(112) DIST 1.43, 0.01 = O(101) TO C(102), C(103) TO O(104) CONT O(104) TO C(105), C(106) TO O(107) CONT O(107) TO C(108), C(109) TO O(110) CONT O(110) TO C(111), C(112) TO O(113) ANGL 120, 0.5 = C(98) TO O(101) TO C(102) CONT O(101) TO C(102) TO C(103), C(102) TO C(103) TO O(104) CONT C(103) TO O(104) TO C(105), O(104) TO C(105) TO C(106) CONT C(105) TO C(106) TO O(107), C(106) TO O(107) TO C(108) CONT O(107) TO C(108) TO C(109), C(108) TO C(109) TO O(110) CONT C(109) TO O(110) TO C(111), O(110) TO C(111) TO C(112) CONT C(111) TO C(112) TO O(113), C(112) TO O(113) TO C(114) DIST 1.39, 0.01 = C(98) TO O(101), C(114) TO O(113) CONT O(120) TO C(117), O(94) TO C(95) ANGL 120, 1.0 = O(94) TO C(95) TO C(96) ANGL 180, 1.0 = N(80) TO N(81) TO N(82) DIST 1.16, 0.01 = N(80) TO N(81), N(81) TO N(82) ANGL 180, 1.0 = N(180) TO N(181) TO N(182) DIST 1.16, 0.01 = N(180) TO N(181), N(181) TO N(182) DIST 1.48, 0.01 = C(35) TO C(37) DIST 1.52, 0.005 = C(121) TO C(122) REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE) REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(1) TO C(4) VIBR .0, 0.00200 = C(2) TO C(4) VIBR .0, 0.00200 = C(3) TO C(4) VIBR .0, 0.00200 = C(4) TO C(5) VIBR .0, 0.00500 = C(3) TO C(1) VIBR .0, 0.00500 = C(2) TO C(1) VIBR .0, 0.00500 = C(2) TO C(3) VIBR .0, 0.00500 = C(5) TO C(1) VIBR .0, 0.00500 = C(5) TO C(3) VIBR .0, 0.00500 = C(5) TO C(2) VIBR .0, 0.00200 = C(5) TO C(6) VIBR .0, 0.00200 = C(5) TO C(10) VIBR .0, 0.00500 = C(6) TO C(4) VIBR .0, 0.00500 = C(10) TO C(4) VIBR .0, 0.00500 = C(10) TO C(6) VIBR .0, 0.00200 = C(6) TO C(7) VIBR .0, 0.00500 = C(7) TO C(5) VIBR .0, 0.00200 = C(7) TO C(8) VIBR .0, 0.00500 = C(8) TO C(6) VIBR .0, 0.00200 = C(8) TO C(9) VIBR .0, 0.00200 = C(8) TO C(27) VIBR .0, 0.00500 = C(9) TO C(7) VIBR .0, 0.00500 = C(27) TO C(7) VIBR .0, 0.00500 = C(27) TO C(9) VIBR .0, 0.00200 = C(9) TO C(10) VIBR .0, 0.00500 = C(10) TO C(8) VIBR .0, 0.00500 = C(5) TO C(9) VIBR .0, 0.00200 = C(11) TO C(14) VIBR .0, 0.00200 = C(12) TO C(14) VIBR .0, 0.00200 = C(13) TO C(14) VIBR .0, 0.00200 = C(14) TO C(15) VIBR .0, 0.00500 = C(12) TO C(11) VIBR .0, 0.00500 = C(13) TO C(11) VIBR .0, 0.00500 = C(13) TO C(12) VIBR .0, 0.00500 = C(15) TO C(11) VIBR .0, 0.00500 = C(15) TO C(12) VIBR .0, 0.00500 = C(15) TO C(13) VIBR .0, 0.00200 = C(15) TO C(16) VIBR .0, 0.00200 = C(15) TO C(20) VIBR .0, 0.00500 = C(16) TO C(14) VIBR .0, 0.00500 = C(20) TO C(14) VIBR .0, 0.00500 = C(20) TO C(16) VIBR .0, 0.00200 = C(16) TO C(17) VIBR .0, 0.00500 = C(17) TO C(15) VIBR .0, 0.00200 = C(17) TO C(18) VIBR .0, 0.00500 = C(18) TO C(16) VIBR .0, 0.00200 = C(18) TO C(19) VIBR .0, 0.00200 = C(18) TO C(27) VIBR .0, 0.00500 = C(19) TO C(17) VIBR .0, 0.00500 = C(27) TO C(17) VIBR .0, 0.00500 = C(27) TO C(19) VIBR .0, 0.00200 = C(19) TO C(20) VIBR .0, 0.00500 = C(20) TO C(18) VIBR .0, 0.00500 = C(15) TO C(19) VIBR .0, 0.00200 = C(21) TO C(22) VIBR .0, 0.00200 = C(21) TO C(26) VIBR .0, 0.00500 = C(26) TO C(22) VIBR .0, 0.00200 = C(22) TO C(23) VIBR .0, 0.00500 = C(23) TO C(21) VIBR .0, 0.00200 = C(23) TO C(24) VIBR .0, 0.00500 = C(24) TO C(22) VIBR .0, 0.00200 = C(24) TO C(25) VIBR .0, 0.00200 = C(24) TO C(27) VIBR .0, 0.00500 = C(25) TO C(23) VIBR .0, 0.00500 = C(27) TO C(23) VIBR .0, 0.00500 = C(27) TO C(25) VIBR .0, 0.00200 = C(25) TO C(26) VIBR .0, 0.00500 = C(26) TO C(24) VIBR .0, 0.00500 = C(21) TO C(25) VIBR .0, 0.00200 = C(27) TO C(28) VIBR .0, 0.00500 = C(24) TO C(8) VIBR .0, 0.00500 = C(18) TO C(8) VIBR .0, 0.00500 = C(18) TO C(24) VIBR .0, 0.00500 = C(28) TO C(8) VIBR .0, 0.00500 = C(28) TO C(24) VIBR .0, 0.00500 = C(28) TO C(18) VIBR .0, 0.00200 = C(28) TO C(29) VIBR .0, 0.00200 = C(28) TO C(33) VIBR .0, 0.00500 = C(29) TO C(27) VIBR .0, 0.00500 = C(33) TO C(27) VIBR .0, 0.00500 = C(33) TO C(29) VIBR .0, 0.00200 = C(29) TO C(30) VIBR .0, 0.00500 = C(30) TO C(28) VIBR .0, 0.00200 = C(30) TO C(31) VIBR .0, 0.00500 = C(31) TO C(29) VIBR .0, 0.00200 = C(31) TO C(32) VIBR .0, 0.00200 = C(31) TO N(34) VIBR .0, 0.00500 = C(32) TO C(30) VIBR .0, 0.00500 = N(34) TO C(30) VIBR .0, 0.00500 = N(34) TO C(32) VIBR .0, 0.00200 = C(32) TO C(33) VIBR .0, 0.00500 = C(33) TO C(31) VIBR .0, 0.00500 = C(28) TO C(32) VIBR .0, 0.00200 = N(34) TO C(35) VIBR .0, 0.00500 = C(35) TO C(31) VIBR .0, 0.00200 = C(35) TO O(36) VIBR .0, 0.00200 = C(35) TO C(37) VIBR .0, 0.00500 = O(36) TO N(34) VIBR .0, 0.00500 = C(37) TO N(34) VIBR .0, 0.00500 = C(37) TO O(36) VIBR .0, 0.00200 = C(37) TO C(38) VIBR .0, 0.00200 = C(37) TO C(43) VIBR .0, 0.00500 = C(38) TO C(35) VIBR .0, 0.00500 = C(43) TO C(35) VIBR .0, 0.00500 = C(43) TO C(38) VIBR .0, 0.00200 = C(38) TO N(39) VIBR .0, 0.00500 = N(39) TO C(37) VIBR .0, 0.00200 = N(39) TO C(40) VIBR .0, 0.00200 = N(39) TO C(41) VIBR .0, 0.00500 = C(40) TO C(38) VIBR .0, 0.00500 = C(41) TO C(38) VIBR .0, 0.00500 = C(41) TO C(40) VIBR .0, 0.00200 = C(41) TO C(42) VIBR .0, 0.00500 = C(42) TO N(39) VIBR .0, 0.00200 = C(42) TO C(43) VIBR .0, 0.00200 = C(42) TO C(78) VIBR .0, 0.00500 = C(43) TO C(41) VIBR .0, 0.00500 = C(78) TO C(41) VIBR .0, 0.00500 = C(78) TO C(43) VIBR .0, 0.00500 = C(37) TO C(42) VIBR .0, 0.00200 = C(44) TO C(47) VIBR .0, 0.00200 = C(45) TO C(47) VIBR .0, 0.00200 = C(46) TO C(47) VIBR .0, 0.00200 = C(47) TO C(48) VIBR .0, 0.00500 = C(45) TO C(46) VIBR .0, 0.00500 = C(44) TO C(46) VIBR .0, 0.00500 = C(44) TO C(45) VIBR .0, 0.00500 = C(48) TO C(46) VIBR .0, 0.00500 = C(48) TO C(45) VIBR .0, 0.00500 = C(48) TO C(44) VIBR .0, 0.00200 = C(48) TO C(49) VIBR .0, 0.00200 = C(48) TO C(53) VIBR .0, 0.00500 = C(49) TO C(47) VIBR .0, 0.00500 = C(53) TO C(47) VIBR .0, 0.00500 = C(53) TO C(49) VIBR .0, 0.00200 = C(49) TO C(50) VIBR .0, 0.00500 = C(50) TO C(48) VIBR .0, 0.00200 = C(50) TO C(51) VIBR .0, 0.00500 = C(51) TO C(49) VIBR .0, 0.00200 = C(51) TO C(52) VIBR .0, 0.00200 = C(51) TO C(70) VIBR .0, 0.00500 = C(52) TO C(50) VIBR .0, 0.00500 = C(70) TO C(50) VIBR .0, 0.00500 = C(70) TO C(52) VIBR .0, 0.00200 = C(52) TO C(53) VIBR .0, 0.00500 = C(53) TO C(51) VIBR .0, 0.00500 = C(52) TO C(48) VIBR .0, 0.00200 = C(54) TO C(57) VIBR .0, 0.00200 = C(55) TO C(57) VIBR .0, 0.00200 = C(56) TO C(57) VIBR .0, 0.00200 = C(57) TO C(58) VIBR .0, 0.00500 = C(54) TO C(55) VIBR .0, 0.00500 = C(56) TO C(55) VIBR .0, 0.00500 = C(56) TO C(54) VIBR .0, 0.00500 = C(58) TO C(55) VIBR .0, 0.00500 = C(58) TO C(54) VIBR .0, 0.00500 = C(58) TO C(56) VIBR .0, 0.00200 = C(58) TO C(59) VIBR .0, 0.00200 = C(58) TO C(63) VIBR .0, 0.00500 = C(59) TO C(57) VIBR .0, 0.00500 = C(63) TO C(57) VIBR .0, 0.00500 = C(63) TO C(59) VIBR .0, 0.00200 = C(59) TO C(60) VIBR .0, 0.00500 = C(60) TO C(58) VIBR .0, 0.00200 = C(60) TO C(61) VIBR .0, 0.00500 = C(61) TO C(59) VIBR .0, 0.00200 = C(61) TO C(62) VIBR .0, 0.00200 = C(61) TO C(70) VIBR .0, 0.00500 = C(62) TO C(60) VIBR .0, 0.00500 = C(70) TO C(60) VIBR .0, 0.00500 = C(70) TO C(62) VIBR .0, 0.00200 = C(62) TO C(63) VIBR .0, 0.00500 = C(63) TO C(61) VIBR .0, 0.00500 = C(58) TO C(62) VIBR .0, 0.00200 = C(64) TO C(65) VIBR .0, 0.00200 = C(64) TO C(69) VIBR .0, 0.00500 = C(69) TO C(65) VIBR .0, 0.00200 = C(65) TO C(66) VIBR .0, 0.00500 = C(66) TO C(64) VIBR .0, 0.00200 = C(66) TO C(67) VIBR .0, 0.00500 = C(67) TO C(65) VIBR .0, 0.00200 = C(67) TO C(68) VIBR .0, 0.00200 = C(67) TO C(70) VIBR .0, 0.00500 = C(68) TO C(66) VIBR .0, 0.00500 = C(70) TO C(66) VIBR .0, 0.00500 = C(70) TO C(68) VIBR .0, 0.00200 = C(68) TO C(69) VIBR .0, 0.00500 = C(69) TO C(67) VIBR .0, 0.00500 = C(64) TO C(68) VIBR .0, 0.00200 = C(70) TO C(71) VIBR .0, 0.00500 = C(61) TO C(67) VIBR .0, 0.00500 = C(51) TO C(67) VIBR .0, 0.00500 = C(51) TO C(61) VIBR .0, 0.00500 = C(71) TO C(67) VIBR .0, 0.00500 = C(71) TO C(61) VIBR .0, 0.00500 = C(71) TO C(51) VIBR .0, 0.00200 = C(71) TO C(72) VIBR .0, 0.00200 = C(71) TO C(76) VIBR .0, 0.00500 = C(72) TO C(70) VIBR .0, 0.00500 = C(76) TO C(70) VIBR .0, 0.00500 = C(76) TO C(72) VIBR .0, 0.00200 = C(72) TO C(73) VIBR .0, 0.00500 = C(73) TO C(71) VIBR .0, 0.00200 = C(73) TO C(74) VIBR .0, 0.00500 = C(74) TO C(72) VIBR .0, 0.00200 = C(74) TO C(75) VIBR .0, 0.00200 = C(74) TO N(77) VIBR .0, 0.00500 = C(75) TO C(73) VIBR .0, 0.00500 = N(77) TO C(73) VIBR .0, 0.00500 = N(77) TO C(75) VIBR .0, 0.00200 = C(75) TO C(76) VIBR .0, 0.00500 = C(76) TO C(74) VIBR .0, 0.00500 = C(71) TO C(75) VIBR .0, 0.00200 = N(77) TO C(78) VIBR .0, 0.00500 = C(78) TO C(74) VIBR .0, 0.00200 = C(78) TO O(79) VIBR .0, 0.00500 = N(77) TO C(42) VIBR .0, 0.00500 = O(79) TO C(42) VIBR .0, 0.00500 = O(79) TO N(77) VIBR .0, 0.00200 = N(80) TO N(81) VIBR .0, 0.00200 = N(180) TO N(181) VIBR .0, 0.00200 = N(81) TO N(82) VIBR .0, 0.00500 = N(82) TO N(80) VIBR .0, 0.00500 = N(182) TO N(180) VIBR .0, 0.00200 = N(82) TO C(83) VIBR .0, 0.00200 = N(182) TO C(83) VIBR .0, 0.00500 = C(83) TO N(81) VIBR .0, 0.00200 = C(83) TO C(84) VIBR .0, 0.00200 = C(83) TO C(88) VIBR .0, 0.00500 = C(84) TO N(82) VIBR .0, 0.00500 = C(84) TO N(182) VIBR .0, 0.00500 = C(88) TO N(82) VIBR .0, 0.00500 = C(88) TO C(84) VIBR .0, 0.00200 = C(84) TO C(85) VIBR .0, 0.00500 = C(85) TO C(83) VIBR .0, 0.00200 = C(85) TO C(86) VIBR .0, 0.00200 = C(85) TO C(124) VIBR .0, 0.00500 = C(86) TO C(84) VIBR .0, 0.00500 = C(124) TO C(84) VIBR .0, 0.00500 = C(124) TO C(86) VIBR .0, 0.00200 = C(86) TO C(87) VIBR .0, 0.00500 = C(87) TO C(85) VIBR .0, 0.00200 = C(87) TO C(88) VIBR .0, 0.00200 = C(87) TO C(89) VIBR .0, 0.00500 = C(88) TO C(86) VIBR .0, 0.00500 = C(89) TO C(86) VIBR .0, 0.00500 = C(89) TO C(88) VIBR .0, 0.00500 = C(83) TO C(87) VIBR .0, 0.00200 = C(89) TO O(90) VIBR .0, 0.00200 = C(89) TO N(91) VIBR .0, 0.00500 = O(90) TO C(87) VIBR .0, 0.00500 = N(91) TO C(87) VIBR .0, 0.00500 = N(91) TO O(90) VIBR .0, 0.00200 = N(91) TO C(92) VIBR .0, 0.00500 = C(92) TO C(89) VIBR .0, 0.00200 = C(92) TO C(93) VIBR .0, 0.00500 = C(93) TO N(91) VIBR .0, 0.00200 = C(93) TO O(94) VIBR .0, 0.00500 = O(94) TO C(92) VIBR .0, 0.00200 = O(94) TO C(95) VIBR .0, 0.00500 = C(95) TO C(93) VIBR .0, 0.00200 = C(95) TO C(96) VIBR .0, 0.00200 = C(95) TO C(100) VIBR .0, 0.00500 = C(96) TO O(94) VIBR .0, 0.00500 = C(100) TO O(94) VIBR .0, 0.00500 = C(100) TO C(96) VIBR .0, 0.00200 = C(96) TO C(97) VIBR .0, 0.00500 = C(97) TO C(95) VIBR .0, 0.00200 = C(97) TO C(98) VIBR .0, 0.00500 = C(98) TO C(96) VIBR .0, 0.00200 = C(98) TO C(99) VIBR .0, 0.00200 = C(98) TO O(101) VIBR .0, 0.00500 = C(99) TO C(97) VIBR .0, 0.00500 = O(101) TO C(97) VIBR .0, 0.00500 = O(101) TO C(99) VIBR .0, 0.00200 = C(99) TO C(100) VIBR .0, 0.00500 = C(100) TO C(98) VIBR .0, 0.00500 = C(95) TO C(99) VIBR .0, 0.00200 = O(101) TO C(102) VIBR .0, 0.00500 = C(102) TO C(98) VIBR .0, 0.00200 = C(102) TO C(103) VIBR .0, 0.00500 = C(103) TO O(101) VIBR .0, 0.00200 = C(103) TO O(104) VIBR .0, 0.00500 = O(104) TO C(102) VIBR .0, 0.00200 = O(104) TO C(105) VIBR .0, 0.00500 = C(105) TO C(103) VIBR .0, 0.00200 = C(105) TO C(106) VIBR .0, 0.00500 = C(106) TO O(104) VIBR .0, 0.00200 = C(106) TO O(107) VIBR .0, 0.00500 = O(107) TO C(105) VIBR .0, 0.00200 = O(107) TO C(108) VIBR .0, 0.00500 = C(108) TO C(106) VIBR .0, 0.00200 = C(108) TO C(109) VIBR .0, 0.00500 = C(109) TO O(107) VIBR .0, 0.00200 = C(109) TO O(110) VIBR .0, 0.00500 = O(110) TO C(108) VIBR .0, 0.00200 = O(110) TO C(111) VIBR .0, 0.00500 = C(111) TO C(109) VIBR .0, 0.00200 = C(111) TO C(112) VIBR .0, 0.00500 = C(112) TO O(110) VIBR .0, 0.00200 = C(112) TO O(113) VIBR .0, 0.00500 = O(113) TO C(111) VIBR .0, 0.00200 = O(113) TO C(114) VIBR .0, 0.00500 = C(114) TO C(112) VIBR .0, 0.00200 = C(114) TO C(115) VIBR .0, 0.00200 = C(114) TO C(119) VIBR .0, 0.00500 = C(115) TO O(113) VIBR .0, 0.00500 = C(119) TO O(113) VIBR .0, 0.00500 = C(119) TO C(115) VIBR .0, 0.00200 = C(115) TO C(116) VIBR .0, 0.00500 = C(116) TO C(114) VIBR .0, 0.00200 = C(116) TO C(117) VIBR .0, 0.00500 = C(117) TO C(115) VIBR .0, 0.00200 = C(117) TO C(118) VIBR .0, 0.00200 = C(117) TO O(120) VIBR .0, 0.00500 = C(118) TO C(116) VIBR .0, 0.00500 = O(120) TO C(116) VIBR .0, 0.00500 = O(120) TO C(118) VIBR .0, 0.00200 = C(118) TO C(119) VIBR .0, 0.00500 = C(119) TO C(117) VIBR .0, 0.00500 = C(114) TO C(118) VIBR .0, 0.00200 = O(120) TO C(121) VIBR .0, 0.00500 = C(121) TO C(117) VIBR .0, 0.00200 = C(121) TO C(122) VIBR .0, 0.00500 = C(122) TO O(120) VIBR .0, 0.00200 = C(122) TO N(123) VIBR .0, 0.00500 = N(123) TO C(121) VIBR .0, 0.00200 = N(123) TO C(124) VIBR .0, 0.00500 = C(124) TO C(122) VIBR .0, 0.00200 = C(124) TO O(125) VIBR .0, 0.00500 = N(123) TO C(85) VIBR .0, 0.00500 = O(125) TO C(85) VIBR .0, 0.00500 = O(125) TO N(123) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(1) TO C(4) U(IJ) .0, 0.08000 = C(2) TO C(4) U(IJ) .0, 0.08000 = C(3) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(5) U(IJ) .0, 0.04000 = C(5) TO C(6) U(IJ) .0, 0.04000 = C(5) TO C(10) U(IJ) .0, 0.04000 = C(6) TO C(7) U(IJ) .0, 0.04000 = C(7) TO C(8) U(IJ) .0, 0.04000 = C(8) TO C(9) U(IJ) .0, 0.04000 = C(8) TO C(27) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.08000 = C(11) TO C(14) U(IJ) .0, 0.08000 = C(12) TO C(14) U(IJ) .0, 0.08000 = C(13) TO C(14) U(IJ) .0, 0.04000 = C(14) TO C(15) U(IJ) .0, 0.04000 = C(15) TO C(16) U(IJ) .0, 0.04000 = C(15) TO C(20) U(IJ) .0, 0.04000 = C(16) TO C(17) U(IJ) .0, 0.04000 = C(17) TO C(18) U(IJ) .0, 0.04000 = C(18) TO C(19) U(IJ) .0, 0.04000 = C(18) TO C(27) U(IJ) .0, 0.04000 = C(19) TO C(20) U(IJ) .0, 0.04000 = C(21) TO C(22) U(IJ) .0, 0.04000 = C(21) TO C(26) U(IJ) .0, 0.04000 = C(22) TO C(23) U(IJ) .0, 0.04000 = C(23) TO C(24) U(IJ) .0, 0.04000 = C(24) TO C(25) U(IJ) .0, 0.04000 = C(24) TO C(27) U(IJ) .0, 0.04000 = C(25) TO C(26) U(IJ) .0, 0.04000 = C(27) TO C(28) U(IJ) .0, 0.04000 = C(28) TO C(29) U(IJ) .0, 0.04000 = C(28) TO C(33) U(IJ) .0, 0.04000 = C(29) TO C(30) U(IJ) .0, 0.04000 = C(30) TO C(31) U(IJ) .0, 0.04000 = C(31) TO C(32) U(IJ) .0, 0.04000 = C(31) TO N(34) U(IJ) .0, 0.04000 = C(32) TO C(33) U(IJ) .0, 0.04000 = N(34) TO C(35) U(IJ) .0, 0.08000 = C(35) TO O(36) U(IJ) .0, 0.04000 = C(35) TO C(37) U(IJ) .0, 0.04000 = C(37) TO C(38) U(IJ) .0, 0.04000 = C(37) TO C(43) U(IJ) .0, 0.04000 = C(38) TO N(39) U(IJ) .0, 0.08000 = N(39) TO C(40) U(IJ) .0, 0.04000 = N(39) TO C(41) U(IJ) .0, 0.04000 = C(41) TO C(42) U(IJ) .0, 0.04000 = C(42) TO C(43) U(IJ) .0, 0.04000 = C(42) TO C(78) U(IJ) .0, 0.08000 = C(44) TO C(47) U(IJ) .0, 0.08000 = C(45) TO C(47) U(IJ) .0, 0.08000 = C(46) TO C(47) U(IJ) .0, 0.04000 = C(47) TO C(48) U(IJ) .0, 0.04000 = C(48) TO C(49) U(IJ) .0, 0.04000 = C(48) TO C(53) U(IJ) .0, 0.04000 = C(49) TO C(50) U(IJ) .0, 0.04000 = C(50) TO C(51) U(IJ) .0, 0.04000 = C(51) TO C(52) U(IJ) .0, 0.04000 = C(51) TO C(70) U(IJ) .0, 0.04000 = C(52) TO C(53) U(IJ) .0, 0.08000 = C(54) TO C(57) U(IJ) .0, 0.08000 = C(55) TO C(57) U(IJ) .0, 0.08000 = C(56) TO C(57) U(IJ) .0, 0.04000 = C(57) TO C(58) U(IJ) .0, 0.04000 = C(58) TO C(59) U(IJ) .0, 0.04000 = C(58) TO C(63) U(IJ) .0, 0.04000 = C(59) TO C(60) U(IJ) .0, 0.04000 = C(60) TO C(61) U(IJ) .0, 0.04000 = C(61) TO C(62) U(IJ) .0, 0.04000 = C(61) TO C(70) U(IJ) .0, 0.04000 = C(62) TO C(63) U(IJ) .0, 0.04000 = C(64) TO C(65) U(IJ) .0, 0.04000 = C(64) TO C(69) U(IJ) .0, 0.04000 = C(65) TO C(66) U(IJ) .0, 0.04000 = C(66) TO C(67) U(IJ) .0, 0.04000 = C(67) TO C(68) U(IJ) .0, 0.04000 = C(67) TO C(70) U(IJ) .0, 0.04000 = C(68) TO C(69) U(IJ) .0, 0.04000 = C(70) TO C(71) U(IJ) .0, 0.04000 = C(71) TO C(72) U(IJ) .0, 0.04000 = C(71) TO C(76) U(IJ) .0, 0.04000 = C(72) TO C(73) U(IJ) .0, 0.04000 = C(73) TO C(74) U(IJ) .0, 0.04000 = C(74) TO C(75) U(IJ) .0, 0.04000 = C(74) TO N(77) U(IJ) .0, 0.04000 = C(75) TO C(76) U(IJ) .0, 0.04000 = N(77) TO C(78) U(IJ) .0, 0.08000 = C(78) TO O(79) U(IJ) .0, 0.08000 = N(80) TO N(81) U(IJ) .0, 0.08000 = N(180) TO N(181) U(IJ) .0, 0.04000 = N(81) TO N(82) U(IJ) .0, 0.04000 = N(181) TO N(182) U(IJ) .0, 0.04000 = N(82) TO C(83) U(IJ) .0, 0.04000 = N(182) TO C(83) U(IJ) .0, 0.04000 = C(83) TO C(84) U(IJ) .0, 0.04000 = C(83) TO C(88) U(IJ) .0, 0.04000 = C(84) TO C(85) U(IJ) .0, 0.04000 = C(85) TO C(86) U(IJ) .0, 0.04000 = C(85) TO C(124) U(IJ) .0, 0.04000 = C(86) TO C(87) U(IJ) .0, 0.04000 = C(87) TO C(88) U(IJ) .0, 0.04000 = C(87) TO C(89) U(IJ) .0, 0.08000 = C(89) TO O(90) U(IJ) .0, 0.04000 = C(89) TO N(91) U(IJ) .0, 0.04000 = N(91) TO C(92) U(IJ) .0, 0.04000 = C(92) TO C(93) U(IJ) .0, 0.04000 = C(93) TO O(94) U(IJ) .0, 0.04000 = O(94) TO C(95) U(IJ) .0, 0.04000 = C(95) TO C(96) U(IJ) .0, 0.04000 = C(95) TO C(100) U(IJ) .0, 0.01000 = C(96) TO C(97) U(IJ) .0, 0.01000 = C(97) TO C(98) U(IJ) .0, 0.04000 = C(98) TO C(99) U(IJ) .0, 0.04000 = C(98) TO O(101) U(IJ) .0, 0.04000 = C(99) TO C(100) U(IJ) .0, 0.04000 = O(101) TO C(102) U(IJ) .0, 0.04000 = C(102) TO C(103) U(IJ) .0, 0.04000 = C(103) TO O(104) U(IJ) .0, 0.01000 = O(104) TO C(105) U(IJ) .0, 0.01000 = C(105) TO C(106) U(IJ) .0, 0.04000 = C(106) TO O(107) U(IJ) .0, 0.04000 = O(107) TO C(108) U(IJ) .0, 0.04000 = C(108) TO C(109) U(IJ) .0, 0.04000 = C(109) TO O(110) U(IJ) .0, 0.04000 = O(110) TO C(111) U(IJ) .0, 0.04000 = C(111) TO C(112) U(IJ) .0, 0.04000 = C(112) TO O(113) U(IJ) .0, 0.04000 = O(113) TO C(114) U(IJ) .0, 0.04000 = C(114) TO C(115) U(IJ) .0, 0.04000 = C(114) TO C(119) U(IJ) .0, 0.04000 = C(115) TO C(116) U(IJ) .0, 0.04000 = C(116) TO C(117) U(IJ) .0, 0.04000 = C(117) TO C(118) U(IJ) .0, 0.04000 = C(117) TO O(120) U(IJ) .0, 0.04000 = C(118) TO C(119) U(IJ) .0, 0.04000 = O(120) TO C(121) U(IJ) .0, 0.04000 = C(121) TO C(122) U(IJ) .0, 0.04000 = C(122) TO N(123) U(IJ) .0, 0.04000 = N(123) TO C(124) U(IJ) .0, 0.08000 = C(124) TO O(125) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details -1 6 3 x . 1 0 6 x . 3 -4 1 x . -2 -10 3 x . 1 -5 2 x . -1 5 7 x . -1 -5 1 x . 1 6 3 x . -1 -2 4 x . 0 -2 7 x . 3 7 3 x . 15 7 9 x . 15 7 8 x . 15 11 13 x . 16 -2 2 x . -11 -8 21 x . 4 -2 4 x . 2 -1 8 x . 1 2 9 x . 4 -2 2 x . 4 3 4 x . 3 7 8 x . -2 -2 7 x . 1 1 10 x . 4 6 7 x . 4 0 5 x . -2 6 1 x . 2 1 9 x . 4 4 2 x . -4 0 7 x . 0 -1 5 x . -4 1 5 x . 5 3 3 x . -3 3 6 x . 1 -5 7 x . -2 -2 8 x . 2 6 1 x . 2 2 11 x . 4 5 7 x . 4 -3 2 x . -4 6 1 x . 4 2 9 x . -3 1 7 x . -6 3 0 x . 3 0 8 x . 2 7 10 x . 4 -3 4 x . 4 1 6 x . 4 4 7 x . 1 0 10 x . 4 -6 1 x . -3 8 4 x . 5 5 9 x . -4 4 0 x . 0 4 11 x . 6 5 0 x . 2 -2 11 x . 1 -7 1 x . -1 7 3 x . 2 2 9 x . -3 -4 8 x . 3 -5 3 x . 2 7 4 x . 5 -1 3 x . 5 -3 1 x . -2 -5 5 x . 0 7 1 x . #============================================================================== data_Lu.5 _database_code_depnum_ccdc_archive 'CCDC 903825' #TrackingRef 'FaulRotaxChemScistructures.cif' #============================================================================== _audit_creation_date 2012-08-29 _audit_creation_method CRYSTALS_ver_14.43 _oxford_structure_analysis_title '043mwj11 At 16:48 on 3/ 8' _chemical_name_systematic . _chemical_melting_point 'not measured' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. ; _refine_special_details ; The crystals were present as merohedral twins in the approximate ratio of 70:30. The lutetium atoms lead to a high background level of diffuse electron density, apparent as 'ripples' around the lutetium atoms. This is not uncommon and has been seen in a number of other related structures within our laboratory and department. There was a high degree of symmetry in the structure, which meant that a number of the waters of crystallisation had their hydrogens across two sites or were either in or close to special positions. ; _cell_length_a 18.0616(2) _cell_length_b 14.9690(2) _cell_length_c 18.2262(3) _cell_angle_alpha 90 _cell_angle_beta 108.6904(8) _cell_angle_gamma 90 _cell_volume 4667.84(11) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c ' _symmetry_space_group_name_Hall '-P 2yc ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x,-y,z+1/2 -x,y,-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' Lu -0.4720 5.8584 28.9476 1.9018 15.2208 9.9852 15.1000 0.2610 3.7160 84.3298 7.9763 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C80 H108 Lu4 N16 Na4 O28 S4 # Dc = 1.89 Fooo = 2660.00 Mu = 43.88 M = 1330.97 # Found Formula = C70 H126 Lu4 N16 Na4 O43 # Dc = 1.90 FOOO = 2660.00 Mu = 43.13 M = 1335.85 _chemical_formula_sum 'C70 H126 Lu4 N16 Na4 O43' _chemical_formula_moiety 'C70 H102 Lu4 N16 Na4 O31, 12(H2 O)' _chemical_compound_source . _chemical_formula_weight 2671.69 _cell_measurement_reflns_used 10960 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_min 0.060 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2660 _exptl_absorpt_coefficient_mu 4.313 # Sheldrick geometric approximatio 0.65 0.77 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.77 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_ambient_pressure 105 _diffrn_reflns_number 84881 _reflns_number_total 10639 _diffrn_reflns_av_R_equivalents 0.040 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 10639 # Theoretical number of reflections is about 22104 _diffrn_reflns_theta_min 5.111 _diffrn_reflns_theta_max 27.499 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.949 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -23 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 1.19 _oxford_diffrn_Wilson_scale 70.16 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -3.05 _refine_diff_density_max 4.63 # 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 10631 _refine_ls_number_restraints 77 _refine_ls_number_parameters 640 _oxford_refine_ls_R_factor_ref 0.0723 _refine_ls_wR_factor_ref 0.1745 _refine_ls_goodness_of_fit_ref 0.9954 _refine_ls_shift/su_max 0.0067457 _refine_ls_shift/su_mean 0.0000459 # The values computed with all filters except I/sigma _oxford_reflns_number_all 10634 _refine_ls_R_factor_all 0.0723 _refine_ls_wR_factor_all 0.1746 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9306 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_gt 0.1680 # 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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +*****P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Lu1 Lu 0.71271(2) 0.38085(2) 0.71768(2) 0.0136 1.0000 Uani . . . . . . O2 O 0.7242(4) 0.2434(5) 0.6608(4) 0.0194 1.0000 Uani . . . . . . C4 C 0.7889(6) 0.2184(7) 0.6550(6) 0.0218 1.0000 Uani . . . . . . O5 O 0.8050(5) 0.1398(5) 0.6394(5) 0.0316 1.0000 Uani . . . . . . C6 C 0.8553(6) 0.2865(7) 0.6721(7) 0.0221 1.0000 Uani . . . . . . N7 N 0.8293(5) 0.3799(6) 0.6725(5) 0.0177 1.0000 Uani . . . . . . C8 C 0.8963(6) 0.4304(7) 0.7261(6) 0.0216 1.0000 Uani . . . . . . C9 C 0.8709(7) 0.5216(7) 0.7475(6) 0.0210 1.0000 Uani . . . . . . N10 N 0.8093(5) 0.5118(6) 0.7859(5) 0.0202 1.0000 Uani . . . . . . C11 C 0.7667(7) 0.5966(8) 0.7790(6) 0.0237 1.0000 Uani . . . . . . C12 C 0.7066(8) 0.6052(7) 0.6985(7) 0.0286 1.0000 Uani . . . . . . N13 N 0.6484(5) 0.5346(6) 0.6816(5) 0.0161 1.0000 Uani . . . . . . C14 C 0.5950(6) 0.5468(7) 0.7272(6) 0.0192 1.0000 Uani . . . . . . C15 C 0.6268(6) 0.5048(7) 0.8072(6) 0.0185 1.0000 Uani . . . . . . O16 O 0.6047(5) 0.5353(5) 0.8604(4) 0.0264 1.0000 Uani . . . . . . C17 C 0.6017(6) 0.5410(7) 0.5971(6) 0.0191 1.0000 Uani . . . . . . C18 C 0.6460(7) 0.5011(7) 0.5476(6) 0.0189 1.0000 Uani . . . . . . N19 N 0.6688(5) 0.4075(6) 0.5692(5) 0.0176 1.0000 Uani . U . . . . C20 C 0.5995(6) 0.3495(7) 0.5363(6) 0.0180 1.0000 Uani D . . . . . C21 C 0.5491(6) 0.3451(7) 0.5892(6) 0.0200 1.0000 Uani . . . . . . O22 O 0.5878(4) 0.3402(5) 0.6618(4) 0.0203 1.0000 Uani . . . . . . O23 O 0.4773(4) 0.3435(5) 0.5622(4) 0.0200 1.0000 Uani . . . . . . C24 C 0.7308(6) 0.3810(6) 0.5351(6) 0.0169 1.0000 Uani D U . . . . C25 C 0.8102(6) 0.4193(7) 0.5932(6) 0.0186 1.0000 Uani . U . . . . C26 C 0.8464(7) 0.4893(9) 0.8699(6) 0.0286 1.0000 Uani . . . . . . C27 C 0.8919(7) 0.5650(9) 0.9192(7) 0.0292 1.0000 Uani . . . . . . O28 O 0.6935(4) 0.2521(6) 0.8068(5) 0.0282 1.0000 Uani . . . . . . Lu29 Lu 0.71279(2) 0.11182(2) 0.91542(2) 0.0145 1.0000 Uani . . . . . . O30 O 0.6673(4) 0.0598(4) 0.7921(4) 0.0174 1.0000 Uani . U . . . . C31 C 0.6242(6) -0.0093(7) 0.7714(6) 0.0188 1.0000 Uani . U . . . . O32 O 0.6002(5) -0.0382(5) 0.7039(4) 0.0258 1.0000 Uani . . . . . . N34 N 0.6506(5) -0.0419(5) 0.9127(5) 0.0159 1.0000 Uani . U . . . . C35 C 0.6055(6) -0.0485(7) 0.9670(6) 0.0191 1.0000 Uani . . . . . . C36 C 0.6511(7) -0.0086(7) 1.0451(6) 0.0215 1.0000 Uani D . . . . . N37 N 0.6710(5) 0.0868(6) 1.0367(5) 0.0203 1.0000 Uani . U . . . . C38 C 0.7340(6) 0.1139(7) 1.1077(6) 0.0215 1.0000 Uani . U . . . . C39 C 0.8136(6) 0.0810(8) 1.1016(6) 0.0215 1.0000 Uani . U . . . . N40 N 0.8311(5) 0.1186(5) 1.0335(5) 0.0157 1.0000 Uani . . . . . . C41 C 0.8969(6) 0.0691(8) 1.0201(6) 0.0232 1.0000 Uani . . . . . . C42 C 0.8730(6) -0.0222(7) 0.9845(6) 0.0219 1.0000 Uani . . . . . . N43 N 0.8112(5) -0.0158(6) 0.9077(5) 0.0178 1.0000 Uani . . . . . . C44 C 0.8479(7) 0.0073(7) 0.8468(7) 0.0229 1.0000 Uani . . . . . . C45 C 0.8916(7) -0.0675(8) 0.8283(6) 0.0253 1.0000 Uani . . . . . . C46 C 0.9250(9) -0.1279(9) 0.8121(8) 0.0368 1.0000 Uani . . . . . . C48 C 0.7102(8) -0.1120(8) 0.9291(6) 0.0292 1.0000 Uani . U . . . . C49 C 0.8522(6) 0.2134(7) 1.0475(7) 0.0219 1.0000 Uani . . . . . . C50 C 0.7848(6) 0.2788(7) 1.0210(6) 0.0192 1.0000 Uani . . . . . . O51 O 0.7200(4) 0.2488(5) 0.9752(4) 0.0188 1.0000 Uani . . . . . . O52 O 0.7964(5) 0.3567(6) 1.0440(6) 0.0355 1.0000 Uani . . . . . . C53 C 0.6006(6) 0.1425(8) 1.0254(6) 0.0201 1.0000 Uani . . . . . . C54 C 0.5498(6) 0.1450(7) 0.9410(6) 0.0202 1.0000 Uani . . . . . . O55 O 0.5873(4) 0.1468(5) 0.8917(4) 0.0233 1.0000 Uani . . . . . . O56 O 0.4774(4) 0.1482(5) 0.9237(4) 0.0202 1.0000 Uani . . . . . . C58 C 0.7679(5) 0.2484(7) 0.8331(6) 0.0164 1.0000 Uani . . . . . . Na60 Na 0.6206(3) 0.3302(3) 0.8811(3) 0.0269 1.0000 Uani . U . . . . O63 O 0.5770(6) 0.7766(6) 0.6981(5) 0.0367 1.0000 Uani . . . . . . O66 O 0.0552(5) 0.4035(7) 0.3769(6) 0.0415 1.0000 Uani . . . . . . O67 O 1.000000(10) 0.7074(9) 0.750000(10) 0.0524 1.0000 Uani DS T . . . . O3 O 0.8077(5) 0.3099(5) 0.8127(4) 0.0220 1.0000 Uani . . . . . . O4 O 0.6695(4) 0.4369(5) 0.8124(4) 0.0201 1.0000 Uani . . . . . . C1 C 0.9249(8) 0.6210(10) 0.9586(8) 0.0407 1.0000 Uani . . . . . . O10 O 0.9737(6) 0.7494(10) 0.4027(9) 0.0699 1.0000 Uani D . . . . . O12 O 0.8029(5) 0.1843(5) 0.8767(4) 0.0216 1.0000 Uani . . . . . . Na1 Na 0.6213(2) 0.1698(3) 0.6934(2) 0.0241 1.0000 Uani D U . . . . H61 H 0.8921 0.2732 0.7230 0.0270 1.0000 Uiso R . . . . . H62 H 0.8817 0.2801 0.6332 0.0268 1.0000 Uiso R . . . . . H81 H 0.9187 0.3956 0.7725 0.0260 1.0000 Uiso R . . . . . H82 H 0.9346 0.4396 0.6996 0.0261 1.0000 Uiso R . . . . . H91 H 0.9160 0.5518 0.7829 0.0250 1.0000 Uiso R . . . . . H92 H 0.8494 0.5558 0.7015 0.0250 1.0000 Uiso R . . . . . H111 H 0.8035 0.6452 0.7875 0.0289 1.0000 Uiso R . . . . . H112 H 0.7401 0.5981 0.8168 0.0291 1.0000 Uiso R . . . . . H141 H 0.5869 0.6112 0.7332 0.0228 1.0000 Uiso R . . . . . H142 H 0.5448 0.5197 0.6998 0.0230 1.0000 Uiso R . . . . . H201 H 0.6165 0.2895 0.5296 0.0221 1.0000 Uiso R . . . . . H202 H 0.5680 0.3740 0.4868 0.0222 1.0000 Uiso DR . . . . . H241 H 0.7202 0.4044 0.4836 0.0202 1.0000 Uiso DR . . . . . H242 H 0.7340 0.3157 0.5332 0.0200 1.0000 Uiso R . . . . . H251 H 0.8073 0.4853 0.5972 0.0219 1.0000 Uiso R . . . . . H252 H 0.8529 0.4066 0.5737 0.0221 1.0000 Uiso R . . . . . H261 H 0.8820 0.4387 0.8746 0.0351 1.0000 Uiso R . . . . . H262 H 0.8053 0.4722 0.8912 0.0350 1.0000 Uiso R . . . . . H351 H 0.5943 -0.1113 0.9728 0.0231 1.0000 Uiso R . . . . . H352 H 0.5566 -0.0165 0.9456 0.0231 1.0000 Uiso R . . . . . H361 H 0.6993 -0.0423 1.0658 0.0261 1.0000 Uiso DR . . . . . H362 H 0.6205 -0.0132 1.0802 0.0260 1.0000 Uiso R . . . . . H381 H 0.7246 0.0907 1.1540 0.0262 1.0000 Uiso R . . . . . H382 H 0.7350 0.1790 1.1103 0.0258 1.0000 Uiso R . . . . . H391 H 0.8549 0.1002 1.1483 0.0260 1.0000 Uiso R . . . . . H392 H 0.8129 0.0167 1.0978 0.0259 1.0000 Uiso R . . . . . H411 H 0.9384 0.0625 1.0691 0.0271 1.0000 Uiso R . . . . . H412 H 0.9166 0.1050 0.9853 0.0270 1.0000 Uiso R . . . . . H421 H 0.9181 -0.0521 0.9780 0.0270 1.0000 Uiso R . . . . . H422 H 0.8529 -0.0575 1.0186 0.0270 1.0000 Uiso R . . . . . H441 H 0.8829 0.0573 0.8655 0.0280 1.0000 Uiso R . . . . . H442 H 0.8062 0.0258 0.8001 0.0280 1.0000 Uiso R . . . . . H461 H 0.9421 -0.1827 0.7960 0.0440 1.0000 Uiso R . . . . . H481 H 0.7384 -0.1117 0.9851 0.0348 1.0000 Uiso R . . . . . H482 H 0.6846 -0.1695 0.9146 0.0351 1.0000 Uiso R . . . . . H531 H 0.6162 0.2032 1.0420 0.0240 1.0000 Uiso R . . . . . H532 H 0.5699 0.1178 1.0557 0.0239 1.0000 Uiso R . . . . . H11 H 0.9508 0.6683 0.9898 0.0501 1.0000 Uiso R . . . . . H661 H 0.0959 0.4163 0.4091 0.0630 1.0000 Uiso R . . . . . H182 H 0.6926 0.5368 0.5537 0.0231 1.0000 Uiso R . . . . . H181 H 0.6131 0.5036 0.4933 0.0229 1.0000 Uiso R . . . . . H172 H 0.5905 0.6033 0.5836 0.0230 1.0000 Uiso R . . . . . H171 H 0.5525 0.5091 0.5882 0.0231 1.0000 Uiso R . . . . . H122 H 0.6790 0.6624 0.6958 0.0351 1.0000 Uiso R . . . . . H121 H 0.7329 0.6033 0.6605 0.0349 1.0000 Uiso R . . . . . O680 O 0.500000(10) 0.3763(12) 0.750000(10) 0.0418 0.7300 Uani S TU . . 8 . H492 H 0.8772 0.2215 1.1034 0.0261 1.0000 Uiso R . . . . . H491 H 0.8900 0.2275 1.0213 0.0261 1.0000 Uiso R . . . . . C2 C 0.7693(6) -0.1012(7) 0.8884(6) 0.0194 1.0000 Uani . U . . . . C3 C 0.5968(6) -0.0541(8) 0.8323(6) 0.0201 1.0000 Uani . . . . . . H31 H 0.5905 -0.1176 0.8207 0.0239 1.0000 Uiso R . . . . . H32 H 0.5464 -0.0290 0.8290 0.0240 1.0000 Uiso R . . . . . H21 H 0.8064 -0.1491 0.9031 0.0229 1.0000 Uiso R . . . . . H22 H 0.7428 -0.1026 0.8327 0.0229 1.0000 Uiso R . . . . . H631 H 0.5793 0.8318 0.6971 0.0561 1.0000 Uiso R . . . . . O700 O 0.500000(10) 0.119(4) 0.750000(10) 0.0645 0.2700 Uani DS TU . . 1 . O701 O 0.500000(10) 0.1895(12) 0.750000(10) 0.0526 0.7300 Uani S TU . . 2 . O65 O 0.4208(6) 0.2820(6) 0.1513(5) 0.0358 1.0000 Uani . . . . . . O681 O 0.500000(10) 0.302(3) 0.750000(10) 0.0303 0.2700 Uani S TU . . 7 . H671 H 1.0171 0.6781 0.7899 0.0790 1.0000 Uiso DR . . . . . H652 H 0.4128 0.3443 0.1474 0.0436 1.0000 Uiso R . . . . . H651 H 0.4225 0.2624 0.2015 0.0436 1.0000 Uiso R . . . . . H632 H 0.5245 0.7573 0.6827 0.0444 1.0000 Uiso R . . . . . H101 H 0.9189 0.7447 0.3721 0.0843 1.0000 Uiso DR . . . . . H103 H 1.0012 0.8108 0.4143 0.0843 1.0000 Uiso DR . . . . . H664 H 0.0165 0.4400 0.3836 0.0500 1.0000 Uiso R . . . . . H6809 H 0.4668 0.3319 0.7665 0.0500 0.2700 Uiso R . . . 7 . H7011 H 0.4685 0.1724 0.6988 0.0638 0.2700 Uiso R . . . 1 . O1501 O 0.9627(7) 0.1055(8) 0.6659(8) 0.0658 1.0000 Uani D . . . . . H1505 H 0.9189 0.1074 0.6527 0.0604 1.0000 Uiso DR . . . . . H1502 H 0.9885 0.1054 0.7145 0.0604 0.5000 Uiso DR . . . . . H7012 H 0.5314 0.1740 0.8010 0.0629 0.7300 Uiso R . . . 2 . H6801 H 0.5314 0.3637 0.7184 0.0499 0.7300 Uiso R . . . 8 . H1503 H 1.0004 0.0607 0.6673 0.0786 0.5000 Uiso DR . . . . . 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 Lu1 0.0159(2) 0.01399(19) 0.0123(2) -0.00069(13) 0.00645(16) -0.00189(14) O2 0.018(4) 0.019(3) 0.021(3) 0.002(3) 0.006(3) 0.001(3) C4 0.023(5) 0.027(5) 0.016(5) -0.003(4) 0.007(4) -0.004(4) O5 0.023(4) 0.023(4) 0.050(5) -0.016(4) 0.012(4) 0.003(3) C6 0.023(5) 0.017(5) 0.025(5) -0.002(4) 0.006(4) -0.001(4) N7 0.014(4) 0.022(4) 0.015(4) 0.004(3) 0.002(3) -0.005(3) C8 0.011(4) 0.027(5) 0.026(5) -0.002(4) 0.005(4) 0.000(4) C9 0.028(6) 0.019(5) 0.018(5) -0.001(4) 0.010(4) -0.005(4) N10 0.024(4) 0.018(4) 0.017(4) 0.006(3) 0.005(4) -0.004(3) C11 0.027(5) 0.020(5) 0.023(5) -0.002(4) 0.006(4) -0.002(4) C12 0.045(7) 0.020(5) 0.021(5) 0.001(4) 0.011(5) -0.013(5) N13 0.017(4) 0.020(4) 0.011(4) 0.003(3) 0.004(3) 0.000(3) C14 0.026(5) 0.018(5) 0.015(5) 0.003(4) 0.010(4) 0.002(4) C15 0.025(5) 0.018(5) 0.012(4) 0.002(4) 0.006(4) -0.002(4) O16 0.041(5) 0.026(4) 0.018(4) 0.002(3) 0.018(3) 0.010(3) C17 0.024(5) 0.022(5) 0.012(4) -0.001(4) 0.005(4) -0.002(4) C18 0.029(5) 0.020(5) 0.011(4) 0.003(4) 0.010(4) 0.000(4) N19 0.025(3) 0.017(3) 0.016(3) 0.000(2) 0.014(3) -0.004(2) C20 0.021(5) 0.018(5) 0.014(4) -0.005(4) 0.003(4) -0.005(4) C21 0.026(5) 0.014(5) 0.018(5) 0.003(4) 0.005(4) -0.004(4) O22 0.022(4) 0.024(4) 0.014(3) -0.001(3) 0.004(3) -0.004(3) O23 0.020(4) 0.023(4) 0.016(3) 0.004(3) 0.005(3) 0.000(3) C24 0.024(3) 0.017(3) 0.017(3) -0.001(2) 0.017(3) -0.004(2) C25 0.026(3) 0.018(3) 0.018(3) -0.001(2) 0.015(3) -0.003(3) C26 0.027(6) 0.046(7) 0.012(5) 0.003(5) 0.003(4) -0.007(5) C27 0.021(5) 0.037(7) 0.026(6) 0.002(5) 0.001(5) -0.006(5) O28 0.016(3) 0.029(4) 0.037(4) -0.018(3) 0.004(3) 0.001(3) Lu29 0.0158(2) 0.01539(19) 0.0128(2) -0.00086(13) 0.00550(16) 0.00039(14) O30 0.029(4) 0.010(3) 0.014(3) 0.000(2) 0.009(3) -0.007(3) C31 0.021(4) 0.019(4) 0.016(4) 0.003(4) 0.006(4) 0.000(4) O32 0.039(5) 0.024(4) 0.015(4) -0.002(3) 0.010(3) -0.013(3) N34 0.020(4) 0.018(4) 0.010(4) 0.001(3) 0.006(3) -0.001(3) C35 0.017(5) 0.023(5) 0.021(5) 0.006(4) 0.012(4) 0.000(4) C36 0.025(5) 0.021(5) 0.022(5) 0.002(4) 0.012(4) 0.001(4) N37 0.018(4) 0.025(4) 0.016(4) -0.003(3) 0.004(3) 0.004(3) C38 0.027(5) 0.021(4) 0.010(4) -0.006(3) -0.003(3) 0.007(3) C39 0.020(4) 0.027(5) 0.017(4) 0.004(4) 0.006(4) 0.001(4) N40 0.021(4) 0.010(4) 0.015(4) -0.001(3) 0.003(3) 0.004(3) C41 0.022(5) 0.026(6) 0.021(5) -0.006(4) 0.007(4) 0.003(4) C42 0.017(5) 0.026(5) 0.021(5) 0.003(4) 0.003(4) 0.004(4) N43 0.023(4) 0.017(4) 0.016(4) 0.001(3) 0.009(4) -0.002(3) C44 0.030(6) 0.018(5) 0.026(6) 0.005(4) 0.017(5) 0.002(4) C45 0.026(5) 0.030(6) 0.021(5) -0.002(4) 0.008(4) 0.002(5) C46 0.046(8) 0.032(7) 0.035(7) -0.004(5) 0.017(6) 0.010(6) C48 0.042(5) 0.035(5) 0.011(4) -0.003(3) 0.009(4) 0.002(4) C49 0.017(5) 0.021(5) 0.025(5) -0.003(4) 0.002(4) -0.003(4) C50 0.024(5) 0.015(5) 0.019(5) -0.002(4) 0.008(4) 0.001(4) O51 0.021(4) 0.017(3) 0.020(3) -0.002(3) 0.009(3) 0.003(3) O52 0.033(5) 0.022(4) 0.053(6) -0.013(4) 0.016(4) -0.001(3) C53 0.016(5) 0.026(5) 0.019(5) -0.006(4) 0.006(4) 0.003(4) C54 0.026(5) 0.020(5) 0.015(5) 0.003(4) 0.007(4) 0.003(4) O55 0.018(3) 0.034(4) 0.018(4) 0.002(3) 0.005(3) 0.005(3) O56 0.018(4) 0.024(4) 0.020(4) 0.005(3) 0.008(3) 0.001(3) C58 0.024(4) 0.011(4) 0.015(4) 0.000(3) 0.007(4) -0.003(4) Na60 0.026(2) 0.032(2) 0.029(2) 0.0085(18) 0.0168(19) 0.0062(17) O63 0.054(6) 0.021(4) 0.042(5) 0.001(4) 0.026(5) 0.002(4) O66 0.025(4) 0.053(6) 0.046(6) 0.013(5) 0.011(4) 0.007(4) O67 0.064(10) 0.019(6) 0.081(11) 0.0000 0.033(9) 0.0000 O3 0.034(4) 0.015(3) 0.016(3) 0.005(3) 0.007(3) -0.001(3) O4 0.027(4) 0.019(3) 0.017(3) 0.003(3) 0.010(3) 0.005(3) C1 0.034(7) 0.063(9) 0.032(7) -0.017(6) 0.020(6) -0.024(6) O10 0.026(5) 0.092(9) 0.083(8) 0.026(7) 0.005(6) 0.005(6) O12 0.026(4) 0.019(4) 0.024(4) 0.003(3) 0.014(3) 0.007(3) Na1 0.025(2) 0.027(2) 0.018(2) 0.0049(17) 0.0032(17) -0.0058(17) O680 0.044(7) 0.036(7) 0.057(8) 0.0000 0.033(6) 0.0000 C2 0.025(5) 0.020(4) 0.013(4) -0.001(3) 0.006(4) 0.000(4) C3 0.019(5) 0.033(6) 0.009(4) -0.002(4) 0.005(4) -0.006(4) O700 0.08(3) 0.03(3) 0.06(3) 0.0000 0.00(3) 0.0000 O701 0.089(16) 0.024(9) 0.026(9) 0.0000 -0.008(9) 0.0000 O65 0.058(6) 0.022(4) 0.031(5) 0.000(3) 0.019(4) 0.000(4) O681 0.033(9) 0.032(9) 0.033(9) 0.0000 0.020(8) 0.0000 O1501 0.035(6) 0.059(7) 0.090(10) -0.037(7) 0.002(6) 0.008(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.12582(7) loop_ _oxford_twin_element_scale_factors 0.700(2) 0.300(2) 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 Lu1 . O2 . 2.342(7) yes Lu1 . N7 . 2.496(9) yes Lu1 . N10 . 2.654(9) yes Lu1 . N13 . 2.567(8) yes Lu1 . N19 . 2.595(8) yes Lu1 . O22 . 2.242(7) yes Lu1 . O28 . 2.615(10) yes Lu1 . O3 . 2.273(7) yes Lu1 . O4 . 2.272(7) yes O2 . C4 . 1.264(13) yes O2 . Na1 . 2.393(8) yes C4 . O5 . 1.266(14) yes C4 . C6 . 1.529(14) yes C6 . N7 . 1.477(13) yes C6 . H61 . 0.974 no C6 . H62 . 0.977 no N7 . C8 . 1.493(13) yes N7 . C25 . 1.495(13) yes C8 . C9 . 1.531(15) yes C8 . H81 . 0.965 no C8 . H82 . 0.973 no C9 . N10 . 1.499(13) yes C9 . H91 . 0.973 no C9 . H92 . 0.952 no N10 . C11 . 1.469(14) yes N10 . C26 . 1.500(13) yes C11 . C12 . 1.526(16) yes C11 . H111 . 0.963 no C11 . H112 . 0.959 no C12 . N13 . 1.452(13) yes C12 . H122 . 0.983 no C12 . H121 . 0.958 no N13 . C14 . 1.474(13) yes N13 . C17 . 1.503(12) yes C14 . C15 . 1.520(13) yes C14 . H141 . 0.985 no C14 . H142 . 0.973 no C15 . O16 . 1.248(12) yes C15 . O4 . 1.261(12) yes C17 . C18 . 1.510(14) yes C17 . H172 . 0.969 no C17 . H171 . 0.975 no C18 . N19 . 1.479(13) yes C18 . H182 . 0.971 no C18 . H181 . 0.977 no N19 . C20 . 1.483(12) yes N19 . C24 . 1.498(12) yes C20 . C21 . 1.527(14) yes C20 . H201 . 0.968 no C20 . H202 . 0.971 no C21 . O22 . 1.285(12) yes C21 . O23 . 1.231(13) yes O22 . Na1 . 2.642(9) yes O23 . Na60 4_656 2.324(9) yes C24 . C25 . 1.591(14) yes C24 . H241 . 0.962 no C24 . H242 . 0.982 no C25 . H251 . 0.994 no C25 . H252 . 0.966 no C26 . C27 . 1.514(16) yes C26 . H261 . 0.980 no C26 . H262 . 0.975 no C27 . C1 . 1.141(18) yes O28 . Lu29 . 2.829(10) yes O28 . C58 . 1.276(11) yes O28 . Na60 . 2.465(9) yes O28 . Na1 . 2.400(9) yes Lu29 . O30 . 2.270(7) yes Lu29 . N34 . 2.553(8) yes Lu29 . N37 . 2.582(9) yes Lu29 . N40 . 2.503(8) yes Lu29 . N43 . 2.644(9) yes Lu29 . O51 . 2.306(7) yes Lu29 . O55 . 2.229(7) yes Lu29 . O12 . 2.250(8) yes O30 . C31 . 1.277(12) yes O30 . Na1 . 2.382(8) yes C31 . O32 . 1.244(13) yes C31 . C3 . 1.508(14) yes N34 . C35 . 1.474(12) yes N34 . C48 . 1.464(15) yes N34 . C3 . 1.488(12) yes C35 . C36 . 1.520(15) yes C35 . H351 . 0.975 no C35 . H352 . 0.970 no C36 . N37 . 1.492(14) yes C36 . H361 . 0.972 no C36 . H362 . 0.972 no N37 . C38 . 1.479(13) yes N37 . C53 . 1.479(13) yes C38 . C39 . 1.558(15) yes C38 . H381 . 0.975 no C38 . H382 . 0.976 no C39 . N40 . 1.486(13) yes C39 . H391 . 0.977 no C39 . H392 . 0.965 no N40 . C41 . 1.485(13) yes N40 . C49 . 1.470(12) yes C41 . C42 . 1.515(15) yes C41 . H411 . 0.969 no C41 . H412 . 0.981 no C42 . N43 . 1.488(13) yes C42 . H421 . 0.969 no C42 . H422 . 0.969 no N43 . C44 . 1.504(13) yes N43 . C2 . 1.470(13) yes C44 . C45 . 1.470(15) yes C44 . H441 . 0.968 no C44 . H442 . 0.978 no C45 . C46 . 1.178(17) yes C46 . H461 . 0.955 no C48 . H481 . 0.985 no C48 . H482 . 0.972 no C48 . C2 . 1.491(16) yes C49 . C50 . 1.516(14) yes C49 . H492 . 0.980 no C49 . H491 . 0.973 no C50 . O51 . 1.282(13) yes C50 . O52 . 1.233(13) yes O51 . Na60 . 2.381(8) yes C53 . C54 . 1.518(14) yes C53 . H531 . 0.969 no C53 . H532 . 0.973 no C54 . O55 . 1.287(13) yes C54 . O56 . 1.245(13) yes O56 . Na1 4_656 2.324(8) yes C58 . O3 . 1.294(12) yes C58 . O12 . 1.276(12) yes Na60 . O4 . 2.368(8) yes Na60 . O681 . 2.700(8) yes O63 . H631 . 0.827 no O63 . H632 . 0.944 no O66 . H661 . 0.802 no O66 . H664 . 0.925 no O67 . H671 4_756 0.820 no O67 . H671 . 0.820 no C1 . H11 . 0.935 no O10 . H101 . 0.970 no O10 . H103 . 1.034 no Na1 . O700 . 2.809(15) yes O680 . H6801 4_656 0.949 no O680 . H6801 . 0.949 no C2 . H21 . 0.959 no C2 . H22 . 0.975 no C3 . H31 . 0.972 no C3 . H32 . 0.968 no O700 . H7011 4_656 1.222 no O700 . H7011 . 1.222 no O701 . H7012 4_656 0.950 no O701 . H7012 . 0.950 no O65 . H652 . 0.943 no O65 . H651 . 0.952 no O681 . H6809 4_656 0.871 no O681 . H6809 . 0.871 no O1501 . H1505 . 0.751 no O1501 . H1502 . 0.858 no O1501 . H1503 . 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 O2 . Lu1 . N7 . 69.2(3) yes O2 . Lu1 . N10 . 135.9(3) yes N7 . Lu1 . N10 . 70.2(3) yes O2 . Lu1 . N13 . 140.4(3) yes N7 . Lu1 . N13 . 106.3(3) yes N10 . Lu1 . N13 . 68.5(3) yes O2 . Lu1 . N19 . 73.4(3) yes N7 . Lu1 . N19 . 70.4(3) yes N10 . Lu1 . N19 . 108.1(3) yes N13 . Lu1 . N19 . 68.5(3) yes O2 . Lu1 . O22 . 77.3(3) yes N7 . Lu1 . O22 . 133.0(3) yes N10 . Lu1 . O22 . 145.9(3) yes N13 . Lu1 . O22 . 79.6(3) yes N19 . Lu1 . O22 . 69.0(3) yes O2 . Lu1 . O28 . 71.1(2) yes N7 . Lu1 . O28 . 119.7(2) yes N10 . Lu1 . O28 . 116.9(2) yes N13 . Lu1 . O28 . 132.9(2) yes N19 . Lu1 . O28 . 134.7(2) yes O2 . Lu1 . O3 . 77.0(3) yes N7 . Lu1 . O3 . 74.8(3) yes N10 . Lu1 . O3 . 76.4(3) yes N13 . Lu1 . O3 . 141.6(3) yes N19 . Lu1 . O3 . 140.4(3) yes O2 . Lu1 . O4 . 139.6(2) yes N7 . Lu1 . O4 . 141.7(3) yes N10 . Lu1 . O4 . 72.9(3) yes N13 . Lu1 . O4 . 68.0(2) yes N19 . Lu1 . O4 . 132.2(3) yes O22 . Lu1 . O28 . 76.5(2) yes O22 . Lu1 . O3 . 128.6(3) yes O28 . Lu1 . O3 . 53.2(2) yes O22 . Lu1 . O4 . 84.5(3) yes O28 . Lu1 . O4 . 69.7(2) yes O3 . Lu1 . O4 . 87.3(3) yes Lu1 . O2 . C4 . 120.8(7) yes Lu1 . O2 . Na1 . 96.2(3) yes C4 . O2 . Na1 . 134.1(7) yes O2 . C4 . O5 . 125.5(10) yes O2 . C4 . C6 . 118.2(9) yes O5 . C4 . C6 . 116.3(9) yes C4 . C6 . N7 . 113.8(9) yes C4 . C6 . H61 . 108.0 no N7 . C6 . H61 . 108.0 no C4 . C6 . H62 . 108.7 no N7 . C6 . H62 . 109.1 no H61 . C6 . H62 . 109.3 no C6 . N7 . Lu1 . 108.1(6) yes C6 . N7 . C8 . 106.9(8) yes Lu1 . N7 . C8 . 111.9(6) yes C6 . N7 . C25 . 110.1(8) yes Lu1 . N7 . C25 . 111.0(6) yes C8 . N7 . C25 . 108.7(8) yes N7 . C8 . C9 . 111.8(8) yes N7 . C8 . H81 . 109.0 no C9 . C8 . H81 . 109.5 no N7 . C8 . H82 . 107.6 no C9 . C8 . H82 . 108.6 no H81 . C8 . H82 . 110.2 no C8 . C9 . N10 . 111.0(8) yes C8 . C9 . H91 . 109.1 no N10 . C9 . H91 . 108.9 no C8 . C9 . H92 . 109.0 no N10 . C9 . H92 . 108.1 no H91 . C9 . H92 . 110.7 no C9 . N10 . Lu1 . 109.2(6) yes C9 . N10 . C11 . 108.7(8) yes Lu1 . N10 . C11 . 110.5(6) yes C9 . N10 . C26 . 110.1(8) yes Lu1 . N10 . C26 . 108.9(6) yes C11 . N10 . C26 . 109.4(9) yes N10 . C11 . C12 . 110.3(9) yes N10 . C11 . H111 . 108.9 no C12 . C11 . H111 . 109.4 no N10 . C11 . H112 . 109.1 no C12 . C11 . H112 . 108.8 no H111 . C11 . H112 . 110.2 no C11 . C12 . N13 . 112.7(9) yes C11 . C12 . H122 . 108.3 no N13 . C12 . H122 . 107.7 no C11 . C12 . H121 . 109.1 no N13 . C12 . H121 . 108.5 no H122 . C12 . H121 . 110.6 no Lu1 . N13 . C12 . 111.2(7) yes Lu1 . N13 . C14 . 106.9(6) yes C12 . N13 . C14 . 110.5(9) yes Lu1 . N13 . C17 . 112.3(6) yes C12 . N13 . C17 . 107.5(8) yes C14 . N13 . C17 . 108.4(8) yes N13 . C14 . C15 . 112.0(8) yes N13 . C14 . H141 . 109.3 no C15 . C14 . H141 . 108.8 no N13 . C14 . H142 . 109.2 no C15 . C14 . H142 . 108.9 no H141 . C14 . H142 . 108.6 no C14 . C15 . O16 . 118.5(9) yes C14 . C15 . O4 . 116.2(9) yes O16 . C15 . O4 . 125.1(9) yes N13 . C17 . C18 . 110.9(8) yes N13 . C17 . H172 . 109.0 no C18 . C17 . H172 . 109.6 no N13 . C17 . H171 . 108.8 no C18 . C17 . H171 . 109.6 no H172 . C17 . H171 . 108.9 no C17 . C18 . N19 . 111.8(8) yes C17 . C18 . H182 . 108.6 no N19 . C18 . H182 . 109.5 no C17 . C18 . H181 . 108.8 no N19 . C18 . H181 . 109.5 no H182 . C18 . H181 . 108.7 no Lu1 . N19 . C18 . 113.0(6) yes Lu1 . N19 . C20 . 105.6(6) yes C18 . N19 . C20 . 108.7(8) yes Lu1 . N19 . C24 . 111.9(6) yes C18 . N19 . C24 . 108.7(7) yes C20 . N19 . C24 . 108.8(8) yes N19 . C20 . C21 . 111.5(8) yes N19 . C20 . H201 . 109.5 no C21 . C20 . H201 . 108.4 no N19 . C20 . H202 . 108.8 no C21 . C20 . H202 . 108.1 no H201 . C20 . H202 . 110.4 no C20 . C21 . O22 . 114.6(9) yes C20 . C21 . O23 . 121.0(9) yes O22 . C21 . O23 . 124.4(10) yes C21 . O22 . Lu1 . 126.0(6) yes C21 . O22 . Na1 . 106.9(6) yes Lu1 . O22 . Na1 . 92.0(3) yes Na60 4_656 O23 . C21 . 132.7(7) yes N19 . C24 . C25 . 105.2(7) yes N19 . C24 . H241 . 111.5 no C25 . C24 . H241 . 112.0 no N19 . C24 . H242 . 109.8 no C25 . C24 . H242 . 109.4 no H241 . C24 . H242 . 108.9 no N7 . C25 . C24 . 112.4(8) yes N7 . C25 . H251 . 108.8 no C24 . C25 . H251 . 110.5 no N7 . C25 . H252 . 108.3 no C24 . C25 . H252 . 109.9 no H251 . C25 . H252 . 106.8 no N10 . C26 . C27 . 114.7(10) yes N10 . C26 . H261 . 109.2 no C27 . C26 . H261 . 108.1 no N10 . C26 . H262 . 108.5 no C27 . C26 . H262 . 107.4 no H261 . C26 . H262 . 108.8 no C26 . C27 . C1 . 177.1(13) yes Lu1 . O28 . Lu29 . 166.1(3) yes Lu1 . O28 . C58 . 86.0(6) yes Lu29 . O28 . C58 . 80.0(6) yes Lu1 . O28 . Na60 . 101.1(3) yes Lu29 . O28 . Na60 . 86.3(3) yes C58 . O28 . Na60 . 119.8(7) yes Lu1 . O28 . Na1 . 89.2(3) yes Lu29 . O28 . Na1 . 97.7(3) yes C58 . O28 . Na1 . 121.2(7) yes Na60 . O28 . Na1 . 118.6(3) yes O28 . Lu29 . O30 . 68.7(2) yes O28 . Lu29 . N34 . 134.4(2) yes O30 . Lu29 . N34 . 69.8(2) yes O28 . Lu29 . N37 . 134.6(3) yes O30 . Lu29 . N37 . 133.3(3) yes N34 . Lu29 . N37 . 68.8(3) yes O28 . Lu29 . N40 . 116.8(2) yes O30 . Lu29 . N40 . 143.5(3) yes N34 . Lu29 . N40 . 107.6(3) yes N37 . Lu29 . N40 . 70.9(3) yes O28 . Lu29 . N43 . 115.7(2) yes O30 . Lu29 . N43 . 74.7(3) yes N34 . Lu29 . N43 . 69.3(3) yes N37 . Lu29 . N43 . 109.1(3) yes N40 . Lu29 . N43 . 70.8(3) yes O28 . Lu29 . O51 . 69.3(2) yes O30 . Lu29 . O51 . 136.1(2) yes N34 . Lu29 . O51 . 140.2(3) yes N37 . Lu29 . O51 . 73.3(3) yes N40 . Lu29 . O51 . 69.8(3) yes O28 . Lu29 . O55 . 78.5(2) yes O30 . Lu29 . O55 . 82.3(3) yes N34 . Lu29 . O55 . 78.2(3) yes N37 . Lu29 . O55 . 69.0(3) yes N40 . Lu29 . O55 . 133.8(3) yes O28 . Lu29 . O12 . 50.4(2) yes O30 . Lu29 . O12 . 85.6(3) yes N34 . Lu29 . O12 . 141.8(3) yes N37 . Lu29 . O12 . 141.1(3) yes N40 . Lu29 . O12 . 75.3(3) yes N43 . Lu29 . O51 . 136.9(3) yes N43 . Lu29 . O55 . 145.0(3) yes O51 . Lu29 . O55 . 77.4(3) yes N43 . Lu29 . O12 . 76.4(3) yes O51 . Lu29 . O12 . 77.4(3) yes O55 . Lu29 . O12 . 128.2(3) yes Lu29 . O30 . C31 . 124.2(6) yes Lu29 . O30 . Na1 . 116.0(3) yes C31 . O30 . Na1 . 107.8(6) yes O30 . C31 . O32 . 124.1(9) yes O30 . C31 . C3 . 117.2(9) yes O32 . C31 . C3 . 118.7(9) yes Lu29 . N34 . C35 . 112.4(6) yes Lu29 . N34 . C48 . 110.6(7) yes C35 . N34 . C48 . 110.1(8) yes Lu29 . N34 . C3 . 105.9(6) yes C35 . N34 . C3 . 109.0(8) yes C48 . N34 . C3 . 108.6(8) yes N34 . C35 . C36 . 110.7(8) yes N34 . C35 . H351 . 108.5 no C36 . C35 . H351 . 110.2 no N34 . C35 . H352 . 109.0 no C36 . C35 . H352 . 109.5 no H351 . C35 . H352 . 109.0 no C35 . C36 . N37 . 110.8(8) yes C35 . C36 . H361 . 108.0 no N37 . C36 . H361 . 108.7 no C35 . C36 . H362 . 109.7 no N37 . C36 . H362 . 110.0 no H361 . C36 . H362 . 109.6 no Lu29 . N37 . C36 . 111.9(6) yes Lu29 . N37 . C38 . 110.8(6) yes C36 . N37 . C38 . 108.4(8) yes Lu29 . N37 . C53 . 105.8(6) yes C36 . N37 . C53 . 109.2(8) yes C38 . N37 . C53 . 110.7(8) yes N37 . C38 . C39 . 108.6(8) yes N37 . C38 . H381 . 111.1 no C39 . C38 . H381 . 111.7 no N37 . C38 . H382 . 108.3 no C39 . C38 . H382 . 108.4 no H381 . C38 . H382 . 108.7 no C38 . C39 . N40 . 112.8(8) yes C38 . C39 . H391 . 108.0 no N40 . C39 . H391 . 108.0 no C38 . C39 . H392 . 109.2 no N40 . C39 . H392 . 108.7 no H391 . C39 . H392 . 110.2 no C39 . N40 . Lu29 . 110.5(6) yes C39 . N40 . C41 . 110.1(8) yes Lu29 . N40 . C41 . 110.3(6) yes C39 . N40 . C49 . 109.5(8) yes Lu29 . N40 . C49 . 106.9(6) yes C41 . N40 . C49 . 109.5(8) yes N40 . C41 . C42 . 112.8(9) yes N40 . C41 . H411 . 108.8 no C42 . C41 . H411 . 109.4 no N40 . C41 . H412 . 107.9 no C42 . C41 . H412 . 109.3 no H411 . C41 . H412 . 108.6 no C41 . C42 . N43 . 111.7(8) yes C41 . C42 . H421 . 109.5 no N43 . C42 . H421 . 108.7 no C41 . C42 . H422 . 109.3 no N43 . C42 . H422 . 108.4 no H421 . C42 . H422 . 109.2 no C42 . N43 . Lu29 . 108.1(6) yes C42 . N43 . C44 . 109.5(8) yes Lu29 . N43 . C44 . 109.6(6) yes C42 . N43 . C2 . 110.0(8) yes Lu29 . N43 . C2 . 109.7(6) yes C44 . N43 . C2 . 109.8(8) yes N43 . C44 . C45 . 112.9(9) yes N43 . C44 . H441 . 108.2 no C45 . C44 . H441 . 109.4 no N43 . C44 . H442 . 108.0 no C45 . C44 . H442 . 109.6 no H441 . C44 . H442 . 108.7 no C44 . C45 . C46 . 178.4(13) yes C45 . C46 . H461 . 168.4 no N34 . C48 . H481 . 108.1 no N34 . C48 . H482 . 109.0 no H481 . C48 . H482 . 109.2 no N34 . C48 . C2 . 114.7(9) yes H481 . C48 . C2 . 107.4 no H482 . C48 . C2 . 108.3 no N40 . C49 . C50 . 115.6(8) yes N40 . C49 . H492 . 107.9 no C50 . C49 . H492 . 107.8 no N40 . C49 . H491 . 107.9 no C50 . C49 . H491 . 108.8 no H492 . C49 . H491 . 108.7 no C49 . C50 . O51 . 117.0(9) yes C49 . C50 . O52 . 118.1(10) yes O51 . C50 . O52 . 124.9(10) yes C50 . O51 . Lu29 . 121.4(6) yes C50 . O51 . Na60 . 127.6(6) yes Lu29 . O51 . Na60 . 101.5(3) yes N37 . C53 . C54 . 111.6(8) yes N37 . C53 . H531 . 109.5 no C54 . C53 . H531 . 108.3 no N37 . C53 . H532 . 109.1 no C54 . C53 . H532 . 108.3 no H531 . C53 . H532 . 109.9 no C53 . C54 . O55 . 115.2(9) yes C53 . C54 . O56 . 120.2(9) yes O55 . C54 . O56 . 124.6(10) yes C54 . O55 . Lu29 . 126.1(7) yes Na1 4_656 O56 . C54 . 132.2(7) yes O28 . C58 . O3 . 118.5(10) yes O28 . C58 . O12 . 121.2(9) yes O3 . C58 . O12 . 120.3(8) yes O23 4_656 Na60 . O51 . 103.2(3) yes O23 4_656 Na60 . O28 . 154.3(3) yes O51 . Na60 . O28 . 75.0(3) yes O23 4_656 Na60 . O4 . 130.0(3) yes O51 . Na60 . O4 . 113.8(3) yes O28 . Na60 . O4 . 71.0(3) yes O23 4_656 Na60 . O681 . 83.9(2) yes O51 . Na60 . O681 . 140.1(10) yes O28 . Na60 . O681 . 82.1(5) yes O4 . Na60 . O681 . 88.1(7) yes H631 . O63 . H632 . 110.6 no H661 . O66 . H664 . 108.5 no H671 4_756 O67 . H671 . 115.5 no C58 . O3 . Lu1 . 101.4(6) yes Na60 . O4 . C15 . 105.2(6) yes Na60 . O4 . Lu1 . 115.4(3) yes C15 . O4 . Lu1 . 126.2(6) yes C27 . C1 . H11 . 178.1 no H101 . O10 . H103 . 121.1 no C58 . O12 . Lu29 . 107.1(6) yes O56 4_656 Na1 . O30 . 125.2(3) yes O56 4_656 Na1 . O2 . 105.3(3) yes O30 . Na1 . O2 . 113.3(3) yes O56 4_656 Na1 . O28 . 155.2(3) yes O30 . Na1 . O28 . 75.1(3) yes O2 . Na1 . O28 . 74.2(3) yes O56 4_656 Na1 . O22 . 83.1(3) yes O30 . Na1 . O22 . 146.3(3) yes O2 . Na1 . O22 . 69.1(3) yes O28 . Na1 . O22 . 73.5(3) yes O56 4_656 Na1 . O700 . 80.8(2) yes O30 . Na1 . O700 . 70.1(7) yes O2 . Na1 . O700 . 167.1(10) yes O28 . Na1 . O700 . 95.5(6) yes O22 . Na1 . O700 . 101.0(10) yes H6801 4_656 O680 . Na60 4_656 90.9 no H6801 4_656 O680 . Na60 . 83.3 no Na60 4_656 O680 . Na60 . 151.0(7) yes H6801 4_656 O680 . H6801 . 157.0 no Na60 4_656 O680 . H6801 . 83.3 no Na60 . O680 . H6801 . 90.9 no C48 . C2 . N43 . 111.8(9) yes C48 . C2 . H21 . 109.2 no N43 . C2 . H21 . 108.9 no C48 . C2 . H22 . 108.9 no N43 . C2 . H22 . 108.1 no H21 . C2 . H22 . 110.0 no C31 . C3 . N34 . 113.9(8) yes C31 . C3 . H31 . 108.6 no N34 . C3 . H31 . 109.1 no C31 . C3 . H32 . 107.8 no N34 . C3 . H32 . 108.5 no H31 . C3 . H32 . 108.9 no H7011 4_656 O700 . H7011 . 98.2 no H7011 4_656 O700 . Na1 . 82.9 no H7011 . O700 . Na1 . 76.7 no H7012 4_656 O701 . Na1 . 84.5 no H7012 4_656 O701 . Na1 4_656 92.5 no Na1 . O701 . Na1 4_656 167.6(8) yes H7012 4_656 O701 . H7012 . 151.9 no Na1 . O701 . H7012 . 92.5 no Na1 4_656 O701 . H7012 . 84.5 no H652 . O65 . H651 . 109.5 no H6809 4_656 O681 . Na60 . 77.2 no H6809 4_656 O681 . Na60 4_656 93.8 no Na60 . O681 . Na60 4_656 162.3(19) yes H6809 4_656 O681 . H6809 . 119.2 no Na60 . O681 . H6809 . 93.8 no Na60 4_656 O681 . H6809 . 77.2 no H1505 . O1501 . H1502 . 119.9 no H1505 . O1501 . H1503 . 135.1 no H1502 . O1501 . H1503 . 79.9 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 C11 . H112 . C15 . 122.6 0.959 2.436 3.061(16) yes C14 . H141 . O63 . 157.3 0.985 2.550 3.480(16) yes C14 . H142 . O16 4_656 149.0(3) 0.973 2.578 3.449(16) yes C14 . H142 . O680 . 121.0(2) 0.973 2.563 3.176(16) yes C24 . H242 . C4 . 123.0 0.982 2.574 3.215(16) yes C25 . H251 . O52 3_564 153.9(3) 0.994 2.540 3.460(16) yes C26 . H262 . O4 . 124.4 0.975 2.470 3.126(16) yes C35 . H352 . C54 . 122.4 0.970 2.421 3.053(16) yes C36 . H361 . O5 3_555 166.3(3) 0.972 2.437 3.389(16) yes C36 . H362 . O32 3_555 147.5(3) 0.972 2.519 3.379(16) yes C38 . H382 . C50 . 123.7 0.976 2.573 3.219(16) yes C39 . H392 . O5 3_555 157.1(3) 0.965 2.480 3.390(16) yes C44 . H442 . O30 . 125.6 0.978 2.519 3.189(16) yes C46 . H461 . O67 1_545 167.6(4) 0.955 2.250 3.189(16) yes C48 . H482 . O65 2_656 159.2(3) 0.972 2.537 3.463(16) yes C1 . H11 . O10 4_756 161.4(6) 0.935 2.335 3.235(16) yes O66 . H661 . O52 4_656 136.2(4) 0.802 2.060 2.697(16) yes C18 . H182 . O52 3_564 168.2(3) 0.971 2.511 3.468(16) yes C18 . H181 . O16 3_564 144.7(3) 0.977 2.449 3.295(16) yes C17 . H171 . C21 . 120.8 0.975 2.457 3.073(16) yes C12 . H122 . O63 . 161.7 0.983 2.524 3.471(16) yes C3 . H31 . O65 2_656 156.4(3) 0.972 2.536 3.449(16) yes C3 . H32 . O32 4_656 152.5(3) 0.968 2.524 3.412(16) yes C2 . H22 . C31 . 121.2 0.975 2.501 3.120(16) yes O63 . H631 . O32 1_565 172.0(4) 0.827 1.979 2.800(16) yes O67 . H671 . O66 3_665 173.3(4) 0.820 1.944 2.761(16) yes O65 . H652 . C15 2_666 153.2(3) 0.943 2.583 3.451(16) yes O65 . H652 . O16 2_666 178.9(4) 0.943 1.827 2.770(16) yes O65 . H651 . O63 2_666 178.5(5) 0.952 1.919 2.871(16) yes O63 . H632 . O65 3_565 179.3(4) 0.944 1.870 2.814(16) yes O10 . H101 . C58 3_564 160.9(4) 0.970 2.590 3.521(16) yes O10 . H101 . O3 3_564 161.3(4) 0.970 2.117 3.051(16) yes O10 . H101 . O12 3_564 134.2(4) 0.970 2.374 3.129(16) yes O10 . H103 . O1501 2_766 127.0(5) 1.034 2.178 2.920(16) yes O66 . H664 . C27 3_464 141.9(4) 0.925 2.535 3.312(16) yes O680 . H6809 . O22 4_656 131(3) 1.003 1.876 2.650(16) yes O681 . H6809 . O22 4_656 147.9(12) 0.871 1.876 2.655(16) yes O701 . H7011 . C54 4_656 151.7(8) 0.958 2.497 3.371(16) yes O701 . H7011 . O55 4_656 178(5) 0.958 1.680 2.637(16) yes O1501 . H1505 . O5 . 164.1 0.751 2.050 2.780(16) yes O1501 . H1502 . O1501 4_756 172.8(7) 0.858 2.074 2.927(16) yes O701 . H7012 . C54 . 152.0(3) 0.950 2.503 3.371(16) yes O701 . H7012 . O55 . 179.9(7) 0.950 1.687 2.637(16) yes O680 . H6801 . C21 . 151.5(3) 0.949 2.491 3.355(16) yes O680 . H6801 . O22 . 179.6(6) 0.949 1.701 2.650(16) yes _iucr_refine_instructions_details_constraints ; # # Punched on 29/08/12 at 16:51:25 # #LIST 12 BLOCK SCALE X'S, U'S SUMFIX ELEMENT SCALES RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) RIDE C ( 12,X'S) H ( 122,X'S) H ( 121,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) RIDE C ( 17,X'S) H ( 172,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 182,X'S) H ( 181,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,X'S) RIDE C ( 35,X'S) H ( 351,X'S) H ( 352,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S) RIDE C ( 38,X'S) H ( 381,X'S) H ( 382,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 492,X'S) H ( 491,X'S) RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S) RIDE O ( 63,X'S) H ( 631,X'S) H ( 632,X'S) RIDE O ( 66,X'S) H ( 661,X'S) H ( 664,X'S) RIDE O ( 67,X'S) H ( 671,X'S) RIDE C ( 1,X'S) H ( 11,X'S) RIDE O ( 10,X'S) H ( 101,X'S) H ( 103,X'S) RIDE O ( 680,X'S) H (6801,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) RIDE O ( 700,X'S) H (7011,X'S) RIDE O ( 701,X'S) H (7012,X'S) RIDE O ( 65,X'S) H ( 652,X'S) H ( 651,X'S) RIDE O ( 681,X'S) H (6809,X'S) RIDE O (1501,X'S) H (1505,X'S) H (1502,X'S) H (1503,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 29/08/12 at 16:51:25 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) U(IJ)'S 0.0, 0.010000 = N(37) TO C(38) U(IJ)'S 0.0, 0.010000 = C(38) TO C(39) U(IJ)'S 0.0, 0.010000 = C(48) TO C(2) U(IJ)'S 0.0, 0.010000 = N(34) TO C(48) U(IJ)'S 0.0, 0.0020000 = C(24) TO C(25) U(IJ)'S 0.0, 0.0020000 = N(19) TO C(24) VIBRATION 0.0, 0.020000 = C(24) TO C(25) VIBRATION 0.0, 0.020000 = N(19) TO C(24) DISTANCE 1.000000 , 0.200000 = C(36) TO H(361) DISTANCE 1.000000 , 0.200000 = C(20) TO H(202) DISTANCE 1.000000 , 0.200000 = C(24) TO H(241) VIBRATION 0.0, 0.050000 = NA(1) TO O(701) VIBRATION 0.0, 0.050000 = NA(1) TO O(700) U(IJ)'S 0.0, 0.050000 = NA(1) TO O(700) DISTANCE 2.700000 , 0.050000 = NA(1) TO O(700) DISTANCE 0.850000 , 0.050000 = O(67) TO H(671) ANGLE 120.000000 , 1.000000 = H(101) TO O(10) TO H(103) U(IJ)'S 0.0, 0.010000 = O(30) TO C(31) U(IJ)'S 0.0, 0.010000 = NA(60) TO O(681) U(IJ)'S 0.0, 0.010000 = NA(60) TO O(680) DISTANCE 0.90000 , 0.050000 = O(1501) TO H(1502) DISTANCE 0.90000 , 0.050000 = O(1501) TO H(1505) ANGLE 120.000000 , 1.000000 = H(1505) TO O(1501) TO H(1502) DISTANCE 0.850000 , 0.050000 = O(1501) TO H(1503) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details 0 0 6 x . 5 0 0 x . -1 5 2 x . -2 5 2 x . 1 5 2 x . # start Validation Reply Form _vrf_PLAT420_Lu.5 ; PROBLEM: D-H Without Acceptor O66 - H664 ... ? RESPONSE: There appears to be an interaction between the sp hybridised acetylene carbon-carbon triple bond and H664, with a close approach between the two of ca. 2.6 A. This is within the range of O-H ... pi interactions found in the literature. ; _vrf_PLAT417_Lu.5 ; PROBLEM: Short Inter D-H..H-D H632 .. H651 .. 2.04 Ang. RESPONSE: These atoms are part of a complex, tight three-dimensional hydrogen bonding network incorporating multiple water molecules closely related by symmetry. ; # end Validation Reply Form