# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 177 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Jonathan Steed' _publ_contact_author_name 'Jonathan Steed' _publ_contact_author_email JON.STEED@DUR.AC.UK _publ_section_title ; Allosteric Effects in a Tetrapodal Imidazolium-Derived Calix[4]arene Anion Receptor ; # Attachment 'Br.CIF' data_c:\rawdat~1\charlo~1\08srv453\work\sad _database_code_depnum_ccdc_archive 'CCDC 722205' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 N8, 2(C2 H3 N), 7(H2 O), 4(Br)' _chemical_formula_sum 'C64 H92 Br4 N10 O7' _chemical_formula_weight 1433.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7428(4) _cell_length_b 17.2842(6) _cell_length_c 18.1320(6) _cell_angle_alpha 117.9510(10) _cell_angle_beta 97.0620(10) _cell_angle_gamma 99.8510(10) _cell_volume 3379.69(19) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 2.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852221 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 6k' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36796 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 29.16 _reflns_number_total 18180 _reflns_number_gt 13552 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-seed _computing_publication_material X-Seed _refine_special_details ; Some water and solvent molecules are disordered. Hydrogen atoms for some water molecules have not been included. The water hydrogens which are included were found in the difference map and then restrained using DFIX Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.8189P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18180 _refine_ls_number_parameters 883 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.97430(2) 1.706955(17) 0.064373(16) 0.02899(6) Uani 1 1 d . . . Br2 Br 1.17638(2) 1.065758(17) -0.377328(15) 0.02928(7) Uani 1 1 d . . . Br3 Br 1.22108(2) 1.096625(16) 0.205666(16) 0.02645(6) Uani 1 1 d . . . Br4 Br 1.79050(2) 1.294643(16) 0.441665(15) 0.02505(6) Uani 1 1 d . . . O1W O 1.2612(6) 1.0850(6) 0.3882(5) 0.044(2) Uani 0.63(4) 1 d PD A 1 O2W O 1.3915(3) 1.0164(2) 0.4725(2) 0.0602(13) Uani 0.668(6) 1 d P B 1 O3W O 1.5626(2) 1.15600(19) 0.60712(16) 0.0489(6) Uani 1 1 d D . . O4W O 1.1986(2) 0.86580(17) 0.09244(16) 0.0564(6) Uani 1 1 d . . . O5W O 1.77391(18) 1.07946(13) 0.30780(13) 0.0357(5) Uani 1 1 d D . . O7W O 1.0786(4) 1.0849(8) 0.4545(5) 0.044(2) Uani 0.61(2) 1 d PD C 1 O9W O 1.6599(2) 1.30424(18) 0.59012(15) 0.0534(6) Uani 1 1 d D . . O1W' O 1.250(3) 1.122(4) 0.4003(18) 0.135(11) Uani 0.37(4) 1 d P A 2 O2W' O 1.3486(6) 1.1535(9) 0.5543(6) 0.103(5) Uani 0.332(6) 1 d P B 2 O7W' O 1.0766(6) 1.0256(16) 0.4227(9) 0.056(5) Uani 0.39(2) 1 d PD C 2 N1 N 1.09008(16) 1.30809(13) 0.36191(13) 0.0229(4) Uani 1 1 d . . . N2 N 1.22570(15) 1.41096(12) 0.37647(11) 0.0174(4) Uani 1 1 d . . . N3 N 1.92250(15) 0.95731(12) 0.14122(12) 0.0169(4) Uani 1 1 d . . . N4 N 1.83430(15) 1.00080(12) 0.06485(12) 0.0170(4) Uani 1 1 d . . . N5 N 2.12908(19) 1.82854(14) 0.32652(14) 0.0302(5) Uani 1 1 d . . . N6 N 1.99426(17) 1.76737(12) 0.35954(12) 0.0243(4) Uani 1 1 d . . . N7 N 1.49987(17) 0.98259(13) -0.31619(14) 0.0251(4) Uani 1 1 d . . . N8 N 1.48996(16) 1.12030(12) -0.24331(12) 0.0181(4) Uani 1 1 d . . . N1S N 1.8364(2) 1.37683(17) 0.73838(17) 0.0399(6) Uani 1 1 d . . . N4S N 1.2738(8) 1.3578(10) 0.5294(9) 0.059(2) Uani 0.619(12) 1 d P D 1 N4S' N 1.295(3) 1.386(2) 0.5346(19) 0.122(11) Uani 0.381(12) 1 d P D 2 C1 C 1.36940(18) 1.39058(14) 0.29332(14) 0.0168(4) Uani 1 1 d . . . C2 C 1.44017(18) 1.34058(15) 0.30407(14) 0.0176(4) Uani 1 1 d . . . C3 C 1.47536(17) 1.28107(14) 0.23248(14) 0.0157(4) Uani 1 1 d . . . C4 C 1.43689(17) 1.27097(14) 0.15186(13) 0.0147(4) Uani 1 1 d . . . C5 C 1.36908(17) 1.32333(14) 0.14181(14) 0.0149(4) Uani 1 1 d . . . C6 C 1.33136(18) 1.38034(14) 0.21237(15) 0.0179(4) Uani 1 1 d . . . C7 C 1.2474(2) 1.42887(17) 0.20115(16) 0.0253(5) Uani 1 1 d . . . H7A H 1.2847 1.4848 0.2035 0.038 Uiso 1 1 calc R . . H7B H 1.2081 1.4438 0.2472 0.038 Uiso 1 1 calc R . . H7C H 1.1953 1.3893 0.1455 0.038 Uiso 1 1 calc R . . C8 C 1.4720(2) 1.34528(19) 0.38966(15) 0.0291(6) Uani 1 1 d . . . H8A H 1.4305 1.3809 0.4289 0.044 Uiso 1 1 calc R . . H8B H 1.5506 1.3741 0.4142 0.044 Uiso 1 1 calc R . . H8C H 1.4556 1.2838 0.3812 0.044 Uiso 1 1 calc R . . C9 C 1.46157(19) 1.19808(14) 0.07325(14) 0.0185(4) Uani 1 1 d . . . H9A H 1.5305 1.2228 0.0638 0.028 Uiso 1 1 calc R . . H9B H 1.4021 1.1771 0.0231 0.028 Uiso 1 1 calc R . . H9C H 1.4682 1.1470 0.0818 0.028 Uiso 1 1 calc R . . C10 C 1.33146(17) 1.31497(15) 0.05459(14) 0.0173(4) Uani 1 1 d . . . H10A H 1.2926 1.3624 0.0631 0.021 Uiso 1 1 calc R . . H10B H 1.2772 1.2555 0.0175 0.021 Uiso 1 1 calc R . . C11 C 1.41839(17) 1.32265(14) 0.00543(13) 0.0145(4) Uani 1 1 d . . . C12 C 1.50877(17) 1.39971(14) 0.04437(13) 0.0141(4) Uani 1 1 d . . . C13 C 1.58854(17) 1.40790(14) -0.00006(13) 0.0146(4) Uani 1 1 d . . . C14 C 1.57326(17) 1.34301(14) -0.08771(13) 0.0154(4) Uani 1 1 d . . . C15 C 1.47995(18) 1.26931(14) -0.12753(13) 0.0152(4) Uani 1 1 d . . . C16 C 1.40482(17) 1.25662(14) -0.08132(13) 0.0151(4) Uani 1 1 d . . . C17 C 1.51722(18) 1.47578(14) 0.13410(14) 0.0183(4) Uani 1 1 d . . . H17A H 1.5643 1.4681 0.1759 0.027 Uiso 1 1 calc R . . H17B H 1.4441 1.4743 0.1458 0.027 Uiso 1 1 calc R . . H17C H 1.5487 1.5342 0.1387 0.027 Uiso 1 1 calc R . . C18 C 1.30757(19) 1.17379(15) -0.12565(15) 0.0212(5) Uani 1 1 d . . . H18A H 1.3070 1.1410 -0.0938 0.032 Uiso 1 1 calc R . . H18B H 1.3132 1.1339 -0.1843 0.032 Uiso 1 1 calc R . . H18C H 1.2397 1.1929 -0.1275 0.032 Uiso 1 1 calc R . . C19 C 1.65613(19) 1.35334(16) -0.13758(15) 0.0224(5) Uani 1 1 d . . . H19A H 1.6355 1.3006 -0.1957 0.034 Uiso 1 1 calc R . . H19B H 1.7288 1.3576 -0.1085 0.034 Uiso 1 1 calc R . . H19C H 1.6578 1.4085 -0.1409 0.034 Uiso 1 1 calc R . . C20 C 1.68778(17) 1.49012(14) 0.04462(14) 0.0162(4) Uani 1 1 d . . . H20A H 1.6616 1.5443 0.0549 0.019 Uiso 1 1 calc R . . H20B H 1.7362 1.4821 0.0043 0.019 Uiso 1 1 calc R . . C21 C 1.75728(17) 1.51055(14) 0.12962(14) 0.0148(4) Uani 1 1 d . . . C22 C 1.79654(17) 1.44258(14) 0.13731(13) 0.0145(4) Uani 1 1 d . . . C23 C 1.86174(17) 1.46279(14) 0.21593(14) 0.0144(4) Uani 1 1 d . . . C24 C 1.89215(18) 1.55149(14) 0.28564(14) 0.0163(4) Uani 1 1 d . . . C25 C 1.85444(18) 1.61953(14) 0.27696(14) 0.0160(4) Uani 1 1 d . . . C26 C 1.78831(17) 1.60001(14) 0.19944(14) 0.0156(4) Uani 1 1 d . . . C27 C 1.7549(2) 1.67412(14) 0.18795(15) 0.0212(5) Uani 1 1 d . . . H27A H 1.7920 1.7332 0.2387 0.032 Uiso 1 1 calc R . . H27B H 1.6754 1.6648 0.1807 0.032 Uiso 1 1 calc R . . H27C H 1.7755 1.6724 0.1370 0.032 Uiso 1 1 calc R . . C28 C 1.77606(19) 1.34971(14) 0.05937(14) 0.0185(4) Uani 1 1 d . . . H28A H 1.8389 1.3249 0.0630 0.028 Uiso 1 1 calc R . . H28B H 1.7661 1.3546 0.0074 0.028 Uiso 1 1 calc R . . H28C H 1.7100 1.3094 0.0571 0.028 Uiso 1 1 calc R . . C29 C 1.9682(2) 1.57691(16) 0.36908(15) 0.0265(5) Uani 1 1 d . . . H29A H 2.0123 1.6397 0.3955 0.040 Uiso 1 1 calc R . . H29B H 2.0166 1.5363 0.3576 0.040 Uiso 1 1 calc R . . H29C H 1.9248 1.5712 0.4082 0.040 Uiso 1 1 calc R . . C30 C 1.90460(18) 1.38872(14) 0.22313(15) 0.0176(4) Uani 1 1 d . . . H30A H 1.9587 1.3734 0.1873 0.021 Uiso 1 1 calc R . . H30B H 1.9444 1.4145 0.2834 0.021 Uiso 1 1 calc R . . C31 C 1.82139(18) 1.30092(14) 0.19756(14) 0.0161(4) Uani 1 1 d . . . C32 C 1.83934(18) 1.21783(14) 0.14059(14) 0.0174(4) Uani 1 1 d . . . C33 C 1.75907(18) 1.13684(14) 0.11207(14) 0.0174(4) Uani 1 1 d . . . C34 C 1.66658(18) 1.13731(14) 0.14681(14) 0.0168(4) Uani 1 1 d . . . C35 C 1.64923(17) 1.22087(14) 0.20503(13) 0.0145(4) Uani 1 1 d . . . C36 C 1.72739(17) 1.30230(14) 0.23095(13) 0.0150(4) Uani 1 1 d . . . C37 C 1.71350(19) 1.39051(14) 0.29919(14) 0.0184(4) Uani 1 1 d . . . H37A H 1.6704 1.4162 0.2722 0.028 Uiso 1 1 calc R . . H37B H 1.7856 1.4331 0.3312 0.028 Uiso 1 1 calc R . . H37C H 1.6755 1.3796 0.3386 0.028 Uiso 1 1 calc R . . C38 C 1.54811(18) 1.22357(14) 0.24240(14) 0.0158(4) Uani 1 1 d . . . H38A H 1.5024 1.1605 0.2156 0.019 Uiso 1 1 calc R . . H38B H 1.5728 1.2457 0.3045 0.019 Uiso 1 1 calc R . . C39 C 1.5898(2) 1.04838(15) 0.12551(16) 0.0218(5) Uani 1 1 d . . . H39A H 1.5782 1.0504 0.1788 0.033 Uiso 1 1 calc R . . H39B H 1.6222 0.9983 0.0943 0.033 Uiso 1 1 calc R . . H39C H 1.5195 1.0390 0.0897 0.033 Uiso 1 1 calc R . . C40 C 1.9463(2) 1.21474(16) 0.11199(17) 0.0240(5) Uani 1 1 d . . . H40A H 1.9470 1.2358 0.0704 0.036 Uiso 1 1 calc R . . H40B H 1.9534 1.1523 0.0853 0.036 Uiso 1 1 calc R . . H40C H 2.0077 1.2541 0.1619 0.036 Uiso 1 1 calc R . . C41 C 1.0200(2) 1.21863(18) 0.3361(2) 0.0406(7) Uani 1 1 d . . . H41A H 1.0437 1.1714 0.2901 0.061 Uiso 1 1 calc R . . H41B H 0.9438 1.2156 0.3154 0.061 Uiso 1 1 calc R . . H41C H 1.0257 1.2091 0.3855 0.061 Uiso 1 1 calc R . . C42 C 1.18381(19) 1.32194(15) 0.34001(15) 0.0214(5) Uani 1 1 d . . . H42 H 1.2157 1.2762 0.3044 0.026 Uiso 1 1 calc R . . C43 C 1.0711(2) 1.39018(16) 0.41476(14) 0.0223(5) Uani 1 1 d . . . H43 H 1.0097 1.3995 0.4396 0.027 Uiso 1 1 calc R . . C44 C 1.15682(19) 1.45510(16) 0.42456(14) 0.0204(5) Uani 1 1 d . . . H44 H 1.1676 1.5189 0.4581 0.025 Uiso 1 1 calc R . . C45 C 1.33111(19) 1.45523(15) 0.36945(15) 0.0208(5) Uani 1 1 d . . . H45A H 1.3873 1.4779 0.4228 0.025 Uiso 1 1 calc R . . H45B H 1.3227 1.5080 0.3634 0.025 Uiso 1 1 calc R . . C46 C 1.9730(2) 0.95263(16) 0.21570(15) 0.0229(5) Uani 1 1 d . . . H46A H 2.0505 0.9861 0.2355 0.034 Uiso 1 1 calc R . . H46B H 1.9670 0.8891 0.1994 0.034 Uiso 1 1 calc R . . H46C H 1.9354 0.9796 0.2620 0.034 Uiso 1 1 calc R . . C47 C 1.86419(18) 1.01498(14) 0.14362(14) 0.0176(4) Uani 1 1 d . . . H47 H 1.8469 1.0589 0.1934 0.021 Uiso 1 1 calc R . . C48 C 1.9294(2) 0.90434(16) 0.05825(15) 0.0227(5) Uani 1 1 d . . . H48 H 1.9664 0.8576 0.0386 0.027 Uiso 1 1 calc R . . C49 C 1.8740(2) 0.93092(15) 0.00964(15) 0.0213(5) Uani 1 1 d . . . H49 H 1.8641 0.9065 -0.0506 0.026 Uiso 1 1 calc R . . C50 C 1.7687(2) 1.04975(15) 0.03799(14) 0.0202(5) Uani 1 1 d . . . H50A H 1.6943 1.0094 0.0063 0.024 Uiso 1 1 calc R . . H50B H 1.8024 1.0642 -0.0019 0.024 Uiso 1 1 calc R . . C51 C 2.1979(2) 1.84958(19) 0.27659(18) 0.0361(6) Uani 1 1 d . . . H51A H 2.1609 1.8135 0.2156 0.054 Uiso 1 1 calc R . . H51B H 2.2678 1.8351 0.2855 0.054 Uiso 1 1 calc R . . H51C H 2.2114 1.9143 0.2951 0.054 Uiso 1 1 calc R . . C52 C 2.0287(2) 1.77274(15) 0.29592(15) 0.0228(5) Uani 1 1 d . . . H52 H 1.9885 1.7419 0.2379 0.027 Uiso 1 1 calc R . . C53 C 2.1584(3) 1.8598(3) 0.4131(2) 0.0687(13) Uani 1 1 d . . . H53 H 2.2256 1.9008 0.4515 0.082 Uiso 1 1 calc R . . C54 C 2.0742(3) 1.8217(3) 0.43311(19) 0.0657(13) Uani 1 1 d . . . H54 H 2.0708 1.8308 0.4886 0.079 Uiso 1 1 calc R . . C55 C 1.88642(19) 1.71512(15) 0.35390(14) 0.0210(5) Uani 1 1 d . . . H55A H 1.8304 1.7469 0.3494 0.025 Uiso 1 1 calc R . . H55B H 1.8882 1.7118 0.4071 0.025 Uiso 1 1 calc R . . C56 C 1.4718(3) 0.88607(17) -0.38430(19) 0.0389(7) Uani 1 1 d . . . H56A H 1.4230 0.8493 -0.3682 0.058 Uiso 1 1 calc R . . H56B H 1.5390 0.8656 -0.3913 0.058 Uiso 1 1 calc R . . H56C H 1.4350 0.8794 -0.4385 0.058 Uiso 1 1 calc R . . C57 C 1.4475(2) 1.04202(15) -0.31611(15) 0.0242(5) Uani 1 1 d . . . H57 H 1.3890 1.0308 -0.3607 0.029 Uiso 1 1 calc R . . C58 C 1.5791(2) 1.02289(16) -0.24183(17) 0.0256(5) Uani 1 1 d . . . H58 H 1.6285 0.9952 -0.2256 0.031 Uiso 1 1 calc R . . C59 C 1.57377(19) 1.11017(16) -0.19558(16) 0.0222(5) Uani 1 1 d . . . H59 H 1.6190 1.1554 -0.1410 0.027 Uiso 1 1 calc R . . C60 C 1.45642(19) 1.20442(14) -0.22307(13) 0.0182(4) Uani 1 1 d . . . H60A H 1.3770 1.1887 -0.2479 0.022 Uiso 1 1 calc R . . H60B H 1.4958 1.2348 -0.2501 0.022 Uiso 1 1 calc R . . C2S C 1.8889(2) 1.41787(17) 0.80635(19) 0.0283(6) Uani 1 1 d . . . C3S C 1.9541(2) 1.46971(19) 0.89343(19) 0.0348(6) Uani 1 1 d . . . H3S1 H 1.9478 1.4321 0.9205 0.052 Uiso 1 1 calc R . . H3S2 H 1.9278 1.5233 0.9258 0.052 Uiso 1 1 calc R . . H3S3 H 2.0309 1.4889 0.8931 0.052 Uiso 1 1 calc R . . C5S C 1.3318(9) 1.3395(8) 0.5677(8) 0.051(2) Uani 0.619(12) 1 d P D 1 C6S C 1.3928(6) 1.3062(7) 0.6140(5) 0.071(3) Uani 0.619(12) 1 d P D 1 H6S1 H 1.3598 1.2413 0.5901 0.106 Uiso 0.619(12) 1 calc PR D 1 H6S2 H 1.3910 1.3392 0.6748 0.106 Uiso 0.619(12) 1 calc PR D 1 H6S3 H 1.4688 1.3156 0.6086 0.106 Uiso 0.619(12) 1 calc PR D 1 C5S' C 1.346(2) 1.3767(11) 0.5764(14) 0.048(4) Uani 0.381(12) 1 d P D 2 C6S' C 1.4379(9) 1.3800(9) 0.6378(7) 0.062(4) Uani 0.381(12) 1 d P D 2 H6S4 H 1.4712 1.4431 0.6832 0.093 Uiso 0.381(12) 1 calc PR D 2 H6S5 H 1.4931 1.3550 0.6075 0.093 Uiso 0.381(12) 1 calc PR D 2 H6S6 H 1.4098 1.3442 0.6634 0.093 Uiso 0.381(12) 1 calc PR D 2 H1W1 H 1.253(3) 1.108(3) 0.353(2) 0.067(13) Uiso 1 1 d D . . H3W1 H 1.516(7) 1.106(4) 0.560(4) 0.30(6) Uiso 1 1 d D . . H5W1 H 1.777(3) 1.1282(15) 0.3470(16) 0.046(10) Uiso 1 1 d D . . H7W1 H 1.106(4) 1.056(2) 0.4808(16) 0.113(19) Uiso 1 1 d D . . H9W1 H 1.720(2) 1.327(2) 0.6310(19) 0.062(12) Uiso 1 1 d D . . H1W2 H 1.196(2) 1.081(3) 0.403(3) 0.093(17) Uiso 1 1 d D . . H3W2 H 1.578(5) 1.195(3) 0.588(4) 0.14(2) Uiso 1 1 d D . . H5W2 H 1.780(2) 1.0608(16) 0.3408(14) 0.013(6) Uiso 1 1 d D . . H7W2 H 1.0137(14) 1.042(2) 0.429(5) 0.26(5) Uiso 1 1 d D . . H9W2 H 1.690(3) 1.306(3) 0.5486(19) 0.070(13) Uiso 1 1 d D . . 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 Br1 0.03761(15) 0.02506(12) 0.02855(13) 0.01519(11) 0.00939(11) 0.01174(11) Br2 0.03370(14) 0.03092(13) 0.02097(12) 0.01122(11) 0.00216(10) 0.01147(11) Br3 0.03040(13) 0.02442(12) 0.02646(12) 0.01246(10) 0.00909(10) 0.01091(10) Br4 0.02538(13) 0.02167(11) 0.02340(12) 0.00884(10) 0.00278(10) 0.00447(9) O1W 0.033(3) 0.067(4) 0.041(3) 0.033(3) 0.017(2) 0.015(3) O2W 0.068(3) 0.048(2) 0.061(2) 0.0262(19) 0.029(2) -0.0016(18) O3W 0.0493(14) 0.0673(16) 0.0439(13) 0.0362(13) 0.0177(11) 0.0180(12) O4W 0.0500(15) 0.0626(15) 0.0557(15) 0.0311(13) 0.0063(12) 0.0127(12) O5W 0.0505(13) 0.0230(10) 0.0358(11) 0.0136(9) 0.0166(10) 0.0137(9) O7W 0.033(2) 0.064(5) 0.041(3) 0.033(4) 0.0080(18) 0.006(2) O9W 0.0397(14) 0.0724(17) 0.0375(13) 0.0211(13) 0.0143(11) 0.0048(12) O1W' 0.128(14) 0.18(3) 0.061(10) 0.084(14) -0.035(8) -0.074(13) O2W' 0.035(5) 0.216(13) 0.092(7) 0.117(9) 0.001(4) 0.001(6) O7W' 0.036(4) 0.102(13) 0.038(5) 0.046(7) 0.004(3) 0.008(4) N1 0.0223(10) 0.0213(10) 0.0234(10) 0.0092(8) 0.0095(8) 0.0049(8) N2 0.0199(10) 0.0168(9) 0.0161(9) 0.0070(8) 0.0071(8) 0.0077(7) N3 0.0164(9) 0.0156(9) 0.0191(9) 0.0086(8) 0.0051(7) 0.0050(7) N4 0.0200(10) 0.0141(8) 0.0198(9) 0.0091(8) 0.0072(8) 0.0073(7) N5 0.0375(13) 0.0189(10) 0.0281(11) 0.0106(9) 0.0057(10) -0.0017(9) N6 0.0318(12) 0.0143(9) 0.0174(9) 0.0053(8) -0.0014(8) -0.0033(8) N7 0.0283(11) 0.0171(9) 0.0305(11) 0.0108(9) 0.0117(9) 0.0075(8) N8 0.0205(10) 0.0178(9) 0.0182(9) 0.0100(8) 0.0053(8) 0.0062(8) N1S 0.0416(15) 0.0362(13) 0.0420(15) 0.0160(12) 0.0170(13) 0.0160(12) N4S 0.051(4) 0.106(6) 0.062(5) 0.068(4) 0.025(3) 0.037(4) N4S' 0.20(2) 0.19(3) 0.110(14) 0.124(18) 0.123(16) 0.15(2) C1 0.0173(11) 0.0154(10) 0.0189(10) 0.0079(9) 0.0097(9) 0.0056(8) C2 0.0168(11) 0.0191(10) 0.0184(10) 0.0101(9) 0.0067(9) 0.0046(8) C3 0.0139(10) 0.0172(10) 0.0185(10) 0.0103(9) 0.0057(8) 0.0045(8) C4 0.0136(10) 0.0130(9) 0.0177(10) 0.0076(8) 0.0055(8) 0.0032(8) C5 0.0128(10) 0.0143(9) 0.0190(10) 0.0098(9) 0.0035(8) 0.0023(8) C6 0.0155(10) 0.0175(10) 0.0243(11) 0.0119(9) 0.0084(9) 0.0063(8) C7 0.0281(13) 0.0306(13) 0.0328(13) 0.0219(11) 0.0168(11) 0.0197(11) C8 0.0349(14) 0.0412(15) 0.0196(12) 0.0163(11) 0.0142(11) 0.0209(12) C9 0.0233(12) 0.0175(10) 0.0157(10) 0.0078(9) 0.0051(9) 0.0091(9) C10 0.0131(10) 0.0194(10) 0.0193(10) 0.0101(9) 0.0023(8) 0.0037(8) C11 0.0125(10) 0.0172(10) 0.0175(10) 0.0116(9) 0.0023(8) 0.0049(8) C12 0.0143(10) 0.0141(9) 0.0150(9) 0.0083(8) 0.0016(8) 0.0048(8) C13 0.0132(10) 0.0160(10) 0.0160(10) 0.0092(8) 0.0016(8) 0.0049(8) C14 0.0151(10) 0.0192(10) 0.0142(10) 0.0097(9) 0.0037(8) 0.0055(8) C15 0.0189(11) 0.0142(10) 0.0119(9) 0.0059(8) 0.0016(8) 0.0060(8) C16 0.0130(10) 0.0160(10) 0.0166(10) 0.0092(9) 0.0001(8) 0.0039(8) C17 0.0179(11) 0.0150(10) 0.0196(11) 0.0067(9) 0.0055(9) 0.0042(8) C18 0.0197(11) 0.0192(11) 0.0199(11) 0.0090(9) 0.0002(9) -0.0008(9) C19 0.0201(12) 0.0271(12) 0.0178(11) 0.0099(10) 0.0067(9) 0.0033(9) C20 0.0162(10) 0.0148(10) 0.0176(10) 0.0102(9) 0.0010(8) 0.0000(8) C21 0.0116(10) 0.0156(10) 0.0182(10) 0.0105(9) 0.0015(8) 0.0014(8) C22 0.0121(10) 0.0138(9) 0.0165(10) 0.0073(8) 0.0031(8) 0.0020(8) C23 0.0124(10) 0.0151(10) 0.0186(10) 0.0104(9) 0.0041(8) 0.0042(8) C24 0.0158(10) 0.0161(10) 0.0172(10) 0.0099(9) 0.0011(8) 0.0020(8) C25 0.0170(10) 0.0119(9) 0.0166(10) 0.0065(8) 0.0026(8) 0.0009(8) C26 0.0137(10) 0.0146(10) 0.0198(10) 0.0099(9) 0.0036(8) 0.0032(8) C27 0.0228(12) 0.0141(10) 0.0258(12) 0.0101(9) 0.0007(10) 0.0059(9) C28 0.0208(11) 0.0154(10) 0.0166(10) 0.0061(9) 0.0016(9) 0.0056(9) C29 0.0317(14) 0.0200(11) 0.0219(12) 0.0105(10) -0.0059(10) 0.0014(10) C30 0.0153(10) 0.0179(10) 0.0227(11) 0.0127(9) 0.0035(9) 0.0049(8) C31 0.0182(11) 0.0151(10) 0.0191(10) 0.0110(9) 0.0041(9) 0.0063(8) C32 0.0201(11) 0.0173(10) 0.0219(11) 0.0128(9) 0.0087(9) 0.0097(9) C33 0.0218(11) 0.0160(10) 0.0198(10) 0.0107(9) 0.0067(9) 0.0111(9) C34 0.0173(11) 0.0154(10) 0.0192(10) 0.0100(9) 0.0027(9) 0.0049(8) C35 0.0161(10) 0.0159(10) 0.0153(10) 0.0098(8) 0.0035(8) 0.0071(8) C36 0.0169(10) 0.0147(10) 0.0160(10) 0.0093(8) 0.0026(8) 0.0069(8) C37 0.0206(11) 0.0154(10) 0.0197(11) 0.0082(9) 0.0070(9) 0.0058(9) C38 0.0173(10) 0.0172(10) 0.0177(10) 0.0113(9) 0.0063(9) 0.0064(8) C39 0.0243(12) 0.0158(10) 0.0277(12) 0.0118(10) 0.0085(10) 0.0067(9) C40 0.0251(12) 0.0203(11) 0.0363(13) 0.0168(11) 0.0181(11) 0.0136(10) C41 0.0364(16) 0.0266(14) 0.0495(18) 0.0115(13) 0.0226(14) 0.0007(12) C42 0.0212(12) 0.0201(11) 0.0205(11) 0.0075(9) 0.0087(9) 0.0054(9) C43 0.0229(12) 0.0272(12) 0.0188(11) 0.0102(10) 0.0100(10) 0.0118(10) C44 0.0243(12) 0.0217(11) 0.0175(10) 0.0080(9) 0.0097(9) 0.0133(9) C45 0.0196(11) 0.0170(10) 0.0228(11) 0.0065(9) 0.0100(9) 0.0047(9) C46 0.0233(12) 0.0263(12) 0.0226(11) 0.0144(10) 0.0036(10) 0.0095(10) C47 0.0189(11) 0.0142(10) 0.0199(10) 0.0080(9) 0.0063(9) 0.0058(8) C48 0.0281(13) 0.0206(11) 0.0243(12) 0.0107(10) 0.0127(10) 0.0147(10) C49 0.0277(12) 0.0204(11) 0.0200(11) 0.0101(9) 0.0112(10) 0.0126(9) C50 0.0275(12) 0.0171(10) 0.0195(11) 0.0095(9) 0.0075(10) 0.0117(9) C51 0.0388(16) 0.0364(15) 0.0349(15) 0.0189(13) 0.0131(13) 0.0073(12) C52 0.0270(13) 0.0182(11) 0.0209(11) 0.0076(9) 0.0035(10) 0.0087(10) C53 0.069(3) 0.070(2) 0.0244(15) 0.0168(16) -0.0130(16) -0.048(2) C54 0.067(2) 0.070(2) 0.0191(14) 0.0153(15) -0.0123(15) -0.044(2) C55 0.0246(12) 0.0159(10) 0.0184(11) 0.0065(9) 0.0027(9) 0.0036(9) C56 0.0498(18) 0.0162(12) 0.0425(16) 0.0071(12) 0.0136(14) 0.0101(12) C57 0.0265(13) 0.0207(11) 0.0206(11) 0.0077(10) 0.0042(10) 0.0036(10) C58 0.0271(13) 0.0275(12) 0.0351(13) 0.0217(11) 0.0151(11) 0.0140(10) C59 0.0201(11) 0.0243(12) 0.0243(12) 0.0140(10) 0.0042(10) 0.0062(9) C60 0.0225(11) 0.0160(10) 0.0139(10) 0.0061(9) 0.0007(9) 0.0066(9) C2S 0.0276(14) 0.0251(12) 0.0421(16) 0.0197(12) 0.0173(12) 0.0148(11) C3S 0.0276(14) 0.0393(15) 0.0460(17) 0.0281(14) 0.0089(13) 0.0079(12) C5S 0.049(5) 0.086(7) 0.053(5) 0.050(7) 0.033(4) 0.038(6) C6S 0.042(4) 0.121(8) 0.084(5) 0.073(6) 0.018(4) 0.034(5) C5S' 0.076(10) 0.052(8) 0.044(6) 0.032(8) 0.041(7) 0.039(9) C6S' 0.051(6) 0.069(8) 0.049(6) 0.018(5) 0.013(5) 0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C42 1.323(3) . ? N1 C43 1.374(3) . ? N1 C41 1.467(3) . ? N2 C42 1.330(3) . ? N2 C44 1.381(3) . ? N2 C45 1.479(3) . ? N3 C47 1.330(3) . ? N3 C48 1.370(3) . ? N3 C46 1.467(3) . ? N4 C47 1.323(3) . ? N4 C49 1.384(3) . ? N4 C50 1.477(3) . ? N5 C52 1.333(3) . ? N5 C53 1.373(4) . ? N5 C51 1.455(3) . ? N6 C52 1.320(3) . ? N6 C54 1.365(3) . ? N6 C55 1.473(3) . ? N7 C57 1.317(3) . ? N7 C58 1.366(3) . ? N7 C56 1.481(3) . ? N8 C57 1.329(3) . ? N8 C59 1.378(3) . ? N8 C60 1.477(3) . ? N1S C2S 1.134(4) . ? N4S C5S 1.135(18) . ? N4S' C5S' 1.03(4) . ? C1 C6 1.405(3) . ? C1 C2 1.407(3) . ? C1 C45 1.516(3) . ? C2 C3 1.412(3) . ? C2 C8 1.515(3) . ? C3 C4 1.401(3) . ? C3 C38 1.524(3) . ? C4 C5 1.408(3) . ? C4 C9 1.510(3) . ? C5 C6 1.404(3) . ? C5 C10 1.526(3) . ? C6 C7 1.517(3) . ? C10 C11 1.531(3) . ? C11 C16 1.410(3) . ? C11 C12 1.411(3) . ? C12 C13 1.401(3) . ? C12 C17 1.513(3) . ? C13 C14 1.414(3) . ? C13 C20 1.526(3) . ? C14 C15 1.402(3) . ? C14 C19 1.512(3) . ? C15 C16 1.402(3) . ? C15 C60 1.512(3) . ? C16 C18 1.517(3) . ? C20 C21 1.527(3) . ? C21 C26 1.408(3) . ? C21 C22 1.410(3) . ? C22 C23 1.410(3) . ? C22 C28 1.510(3) . ? C23 C24 1.399(3) . ? C23 C30 1.527(3) . ? C24 C25 1.410(3) . ? C24 C29 1.514(3) . ? C25 C26 1.402(3) . ? C25 C55 1.520(3) . ? C26 C27 1.510(3) . ? C30 C31 1.520(3) . ? C31 C32 1.401(3) . ? C31 C36 1.406(3) . ? C32 C33 1.405(3) . ? C32 C40 1.518(3) . ? C33 C34 1.402(3) . ? C33 C50 1.514(3) . ? C34 C35 1.410(3) . ? C34 C39 1.518(3) . ? C35 C36 1.407(3) . ? C35 C38 1.526(3) . ? C36 C37 1.505(3) . ? C43 C44 1.352(3) . ? C48 C49 1.351(3) . ? C53 C54 1.339(4) . ? C58 C59 1.359(3) . ? C2S C3S 1.443(4) . ? C5S C6S 1.443(13) . ? C5S' C6S' 1.48(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C42 N1 C43 109.4(2) . . ? C42 N1 C41 124.8(2) . . ? C43 N1 C41 125.7(2) . . ? C42 N2 C44 108.81(19) . . ? C42 N2 C45 125.45(19) . . ? C44 N2 C45 125.69(18) . . ? C47 N3 C48 108.94(19) . . ? C47 N3 C46 125.40(19) . . ? C48 N3 C46 125.65(19) . . ? C47 N4 C49 108.92(18) . . ? C47 N4 C50 126.69(19) . . ? C49 N4 C50 124.38(19) . . ? C52 N5 C53 108.1(2) . . ? C52 N5 C51 126.1(2) . . ? C53 N5 C51 125.7(2) . . ? C52 N6 C54 108.4(2) . . ? C52 N6 C55 126.4(2) . . ? C54 N6 C55 125.2(2) . . ? C57 N7 C58 109.3(2) . . ? C57 N7 C56 124.7(2) . . ? C58 N7 C56 125.9(2) . . ? C57 N8 C59 108.50(19) . . ? C57 N8 C60 123.98(19) . . ? C59 N8 C60 127.33(19) . . ? C6 C1 C2 121.0(2) . . ? C6 C1 C45 119.0(2) . . ? C2 C1 C45 120.0(2) . . ? C1 C2 C3 119.1(2) . . ? C1 C2 C8 120.6(2) . . ? C3 C2 C8 120.1(2) . . ? C4 C3 C2 119.6(2) . . ? C4 C3 C38 120.65(19) . . ? C2 C3 C38 119.64(19) . . ? C3 C4 C5 121.17(19) . . ? C3 C4 C9 119.57(19) . . ? C5 C4 C9 119.11(19) . . ? C6 C5 C4 119.08(19) . . ? C6 C5 C10 119.90(19) . . ? C4 C5 C10 120.93(19) . . ? C5 C6 C1 119.8(2) . . ? C5 C6 C7 120.4(2) . . ? C1 C6 C7 119.9(2) . . ? C5 C10 C11 118.07(18) . . ? C16 C11 C12 119.10(19) . . ? C16 C11 C10 120.49(18) . . ? C12 C11 C10 120.21(19) . . ? C13 C12 C11 120.81(19) . . ? C13 C12 C17 119.71(18) . . ? C11 C12 C17 119.44(19) . . ? C12 C13 C14 119.81(19) . . ? C12 C13 C20 119.82(19) . . ? C14 C13 C20 120.24(19) . . ? C15 C14 C13 118.92(19) . . ? C15 C14 C19 120.68(19) . . ? C13 C14 C19 120.40(19) . . ? C16 C15 C14 121.37(19) . . ? C16 C15 C60 118.91(19) . . ? C14 C15 C60 119.66(19) . . ? C15 C16 C11 119.60(19) . . ? C15 C16 C18 119.86(19) . . ? C11 C16 C18 120.51(19) . . ? C13 C20 C21 117.90(16) . . ? C26 C21 C22 119.70(19) . . ? C26 C21 C20 119.23(18) . . ? C22 C21 C20 120.94(19) . . ? C23 C22 C21 120.26(19) . . ? C23 C22 C28 119.68(19) . . ? C21 C22 C28 119.89(18) . . ? C24 C23 C22 120.12(19) . . ? C24 C23 C30 120.08(19) . . ? C22 C23 C30 119.71(18) . . ? C23 C24 C25 119.28(19) . . ? C23 C24 C29 121.53(19) . . ? C25 C24 C29 119.14(19) . . ? C26 C25 C24 121.12(19) . . ? C26 C25 C55 120.32(19) . . ? C24 C25 C55 118.56(19) . . ? C25 C26 C21 119.44(19) . . ? C25 C26 C27 121.14(19) . . ? C21 C26 C27 119.33(19) . . ? C31 C30 C23 117.59(18) . . ? C32 C31 C36 119.81(19) . . ? C32 C31 C30 119.4(2) . . ? C36 C31 C30 120.76(19) . . ? C31 C32 C33 119.6(2) . . ? C31 C32 C40 120.35(19) . . ? C33 C32 C40 119.99(19) . . ? C34 C33 C32 120.7(2) . . ? C34 C33 C50 120.0(2) . . ? C32 C33 C50 119.1(2) . . ? C33 C34 C35 119.33(19) . . ? C33 C34 C39 119.97(19) . . ? C35 C34 C39 120.6(2) . . ? C36 C35 C34 119.8(2) . . ? C36 C35 C38 119.68(19) . . ? C34 C35 C38 120.51(18) . . ? C31 C36 C35 120.38(19) . . ? C31 C36 C37 120.05(19) . . ? C35 C36 C37 119.4(2) . . ? C3 C38 C35 117.76(17) . . ? N1 C42 N2 108.2(2) . . ? C44 C43 N1 106.7(2) . . ? C43 C44 N2 106.9(2) . . ? N2 C45 C1 111.80(18) . . ? N4 C47 N3 108.35(19) . . ? C49 C48 N3 107.3(2) . . ? C48 C49 N4 106.5(2) . . ? N4 C50 C33 113.63(18) . . ? N6 C52 N5 108.8(2) . . ? C54 C53 N5 107.0(3) . . ? C53 C54 N6 107.8(3) . . ? N6 C55 C25 111.84(19) . . ? N7 C57 N8 108.7(2) . . ? C59 C58 N7 106.9(2) . . ? C58 C59 N8 106.6(2) . . ? N8 C60 C15 112.37(17) . . ? N1S C2S C3S 179.0(3) . . ? N4S C5S C6S 172.1(11) . . ? N4S' C5S' C6S' 168(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.648 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.081 # Attachment 'Cl.CIF' data_c:\rawdat~1\charlo~1\08srv4~1\work\sad _database_code_depnum_ccdc_archive 'CCDC 722206' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 N8, 4(Cl), 13.25 (H2 O),' _chemical_formula_sum 'C60 H102.50 Cl4 N8 O13.25' _chemical_formula_weight 1289.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.8228(7) _cell_length_b 18.0014(7) _cell_length_c 25.5431(10) _cell_angle_alpha 77.1510(10) _cell_angle_beta 82.016(2) _cell_angle_gamma 60.6060(10) _cell_volume 6957.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2770 _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859378 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 6k' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 118706 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 0.82 _diffrn_reflns_theta_max 29.21 _reflns_number_total 37617 _reflns_number_gt 17339 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _refine_special_details ; The solvent and counterion region is very diffuse which has caused problems with the data and the refinement. The crystal was only weakly diffracting causing problems with the intensities. The solvent/counterion region has been assigned as best as possible however some unrefineable disorder still remains and the location of the counterions is not fixed as the large thermal parameters of some O and Cl atoms will attest. The large residual electron density peaks are an artefact of the poor data quality and diffuse nature of the solvent. The configuration of the host is not in question however. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 37617 _refine_ls_number_parameters 1621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2244 _refine_ls_R_factor_gt 0.1233 _refine_ls_wR_factor_ref 0.4138 _refine_ls_wR_factor_gt 0.3534 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.251 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.17565(11) 0.35650(12) 0.74790(8) 0.0607(5) Uani 1 1 d . . . Cl2 Cl 0.2000(3) 0.4858(2) 0.54304(15) 0.1466(14) Uani 1 1 d . . . Cl3 Cl 0.2433(2) 0.41357(17) 0.66036(10) 0.0981(8) Uani 1 1 d . . . Cl4 Cl 0.2881(3) 0.5710(2) 0.46217(14) 0.1324(12) Uani 1 1 d . . . Cl5 Cl 0.57150(13) 0.43517(14) 0.22571(8) 0.0709(6) Uani 1 1 d . . . Cl6 Cl 0.46237(10) -0.28559(10) 0.11253(9) 0.0601(5) Uani 1 1 d . . . Cl7 Cl 1.38477(10) -0.57844(10) 0.08229(6) 0.0475(4) Uani 1 1 d . . . Cl8 Cl 1.0205(2) -0.5075(3) 0.18524(14) 0.0585(13) Uani 0.481(5) 1 d P A 2 Cl8' Cl 1.1875(4) -0.5232(4) 0.2335(2) 0.107(2) Uani 0.519(5) 1 d P A 1 O1W O 1.0545(11) -0.0964(11) -0.3682(7) 0.126(5) Uiso 0.50 1 d P . . O2W O 0.9995(9) -0.0186(9) -0.2788(6) 0.097(4) Uiso 0.50 1 d P . . O3W O 1.0799(3) -0.2354(6) -0.1951(2) 0.131(4) Uani 1 1 d . . . O4W O 0.1171(8) -0.0704(7) 0.5134(6) 0.083(4) Uani 0.50 1 d P B 1 O5W O 1.0705(3) -0.4978(4) 0.0579(2) 0.0725(15) Uani 1 1 d . . . O6W O 0.7753(3) -0.4847(3) -0.0178(2) 0.0684(14) Uani 1 1 d . . . O7W O 0.7100(8) 0.0672(8) 0.6714(4) 0.053(3) Uani 0.50 1 d P C 1 O8W O 0.075(2) 0.538(3) 0.7103(14) 0.120(13) Uani 0.50 1 d P D 1 O9W O 0.6450(4) -0.3475(3) 0.8033(2) 0.0769(16) Uani 1 1 d . . . O10W O 0.0746(7) -0.2814(6) 0.7011(3) 0.070(3) Uani 0.50 1 d P E 1 O11W O -0.0821(4) -0.1579(6) 0.6199(3) 0.127(3) Uani 1 1 d . . . O12W O 0.1451(3) 0.0279(3) 0.4307(2) 0.0644(14) Uani 1 1 d . . . O13W O 0.0195(5) 0.1116(4) 0.5107(3) 0.106(2) Uani 1 1 d . . . O16W O 0.5145(4) 0.2906(4) 0.2415(2) 0.0774(17) Uani 1 1 d . . . O17W O 0.7451(3) 0.3366(3) 0.1614(2) 0.0672(14) Uani 1 1 d . . . O18W O 0.4397(10) 0.3477(10) -0.3221(5) 0.106(5) Uani 0.50 1 d P . . O19W O 0.5762(8) 0.2200(7) -0.3751(6) 0.099(5) Uani 0.50 1 d P . . O20W O 0.5111(6) 0.6290(5) 0.2276(3) 0.125(3) Uani 1 1 d . . . O21W O 0.5523(14) 0.5524(11) 0.4341(10) 0.192(11) Uani 0.50 1 d P . . O22W O 0.4897(8) 0.4243(6) 0.4371(4) 0.167(4) Uani 1 1 d . . . O23W O 0.1962(3) 0.3627(4) 0.3378(2) 0.0699(15) Uani 1 1 d . . . O24W O 0.3588(10) 0.6784(7) 0.4746(3) 0.196(6) Uani 1 1 d . . . O25W O 0.0144(4) 0.7362(4) 0.4494(2) 0.0775(16) Uani 1 1 d . . . O26W O 0.0188(3) 0.6081(4) 0.5329(2) 0.0684(14) Uani 1 1 d . . . O27W O -0.0514(4) 0.6555(6) 0.6295(2) 0.115(3) Uani 1 1 d . . . O28W O -0.1518(5) 0.3543(4) 0.6242(2) 0.088(2) Uani 1 1 d . . . O29W O 1.0352(3) -0.3739(3) 0.8717(2) 0.0680(14) Uani 1 1 d . . . O30W O 0.7896(3) -0.5512(3) 0.0891(2) 0.0642(13) Uani 1 1 d . . . O31W O 0.9564(3) -0.3776(3) -0.0242(2) 0.0707(15) Uani 1 1 d . . . O1W' O 1.0157(11) -0.0268(11) -0.3356(7) 0.124(5) Uiso 0.50 1 d P . . O4W' O 0.1651(9) -0.1431(10) 0.5014(5) 0.092(4) Uani 0.50 1 d P F 2 O7W' O 0.7420(6) 0.0477(7) 0.6473(6) 0.061(4) Uani 0.50 1 d P G 2 O8W' O 0.0845(19) 0.573(3) 0.6985(14) 0.131(15) Uani 0.50 1 d P H 2 N1 N 0.8341(3) -0.1498(4) 0.7583(2) 0.0470(13) Uani 1 1 d . . . N2 N 0.7400(3) -0.1850(3) 0.74740(16) 0.0298(9) Uani 1 1 d . . . N3 N 0.3696(3) 0.3947(3) 0.3584(2) 0.0454(12) Uani 1 1 d . . . N4 N 0.3215(3) 0.3321(3) 0.42507(16) 0.0280(9) Uani 1 1 d . . . N5 N -0.0097(3) 0.4280(3) 0.61035(18) 0.0368(10) Uani 1 1 d . . . N6 N 0.0586(3) 0.3454(3) 0.68193(17) 0.0301(9) Uani 1 1 d . . . N7 N 0.2193(4) -0.3244(4) 0.5966(3) 0.0648(17) Uani 1 1 d . . . N8 N 0.3152(3) -0.3106(3) 0.6304(2) 0.0447(12) Uani 1 1 d . . . N9 N 0.8059(9) 0.1898(9) -0.3368(3) 0.119(4) Uani 1 1 d . . . N10 N 0.7455(4) 0.2046(4) -0.2585(2) 0.0543(15) Uani 1 1 d . . . N11 N 1.1793(2) -0.3297(2) 0.08444(16) 0.0233(8) Uani 1 1 d . . . N12 N 1.2938(2) -0.3778(3) 0.12844(17) 0.0290(9) Uani 1 1 d . . . N13 N 0.7101(3) -0.3372(3) 0.07352(17) 0.0290(9) Uani 1 1 d . . . N14 N 0.7531(3) -0.4125(3) 0.15188(19) 0.0416(11) Uani 1 1 d . . . N15 N 0.5921(3) 0.4432(3) 0.05735(19) 0.0347(10) Uani 1 1 d . . . N16 N 0.6050(2) 0.3155(2) 0.08435(16) 0.0256(8) Uani 1 1 d . . . C1 C 0.5916(3) -0.0914(3) 0.71305(19) 0.0253(10) Uani 1 1 d . . . C2 C 0.5266(3) -0.0550(3) 0.75218(18) 0.0252(10) Uani 1 1 d . . . C3 C 0.4559(3) 0.0270(3) 0.73708(18) 0.0238(9) Uani 1 1 d . . . C4 C 0.4527(3) 0.0722(3) 0.68418(18) 0.0246(10) Uani 1 1 d . . . C5 C 0.5176(3) 0.0350(3) 0.64641(18) 0.0231(9) Uani 1 1 d . . . C6 C 0.5894(3) -0.0463(3) 0.66100(19) 0.0253(10) Uani 1 1 d . . . C7 C 0.6657(3) -0.0825(3) 0.6218(2) 0.0311(11) Uani 1 1 d . . . H7A H 0.7135 -0.1340 0.6408 0.047 Uiso 1 1 calc R . . H7B H 0.6838 -0.0386 0.6067 0.047 Uiso 1 1 calc R . . H7C H 0.6488 -0.0984 0.5928 0.047 Uiso 1 1 calc R . . C8 C 0.5367(3) -0.1042(3) 0.80920(19) 0.0300(11) Uani 1 1 d . . . H8A H 0.5101 -0.0632 0.8342 0.045 Uiso 1 1 calc R . . H8B H 0.5981 -0.1410 0.8164 0.045 Uiso 1 1 calc R . . H8C H 0.5086 -0.1405 0.8140 0.045 Uiso 1 1 calc R . . C9 C 0.3813(3) 0.1644(3) 0.6693(2) 0.0326(11) Uani 1 1 d . . . H9A H 0.4020 0.1961 0.6400 0.049 Uiso 1 1 calc R . . H9B H 0.3643 0.1931 0.7006 0.049 Uiso 1 1 calc R . . H9C H 0.3316 0.1637 0.6576 0.049 Uiso 1 1 calc R . . C10 C 0.3831(3) 0.0675(3) 0.77822(18) 0.0248(10) Uani 1 1 d . . . H10A H 0.3940 0.0241 0.8117 0.030 Uiso 1 1 calc R . . H10B H 0.3861 0.1170 0.7867 0.030 Uiso 1 1 calc R . . C11 C 0.2915(3) 0.0996(3) 0.76164(18) 0.0254(10) Uani 1 1 d . . . C12 C 0.2718(3) 0.0398(3) 0.74804(17) 0.0230(9) Uani 1 1 d . . . C13 C 0.1892(3) 0.0660(3) 0.73127(18) 0.0254(10) Uani 1 1 d . . . C14 C 0.1240(3) 0.1520(3) 0.73072(18) 0.0275(10) Uani 1 1 d . . . C15 C 0.1439(3) 0.2112(3) 0.74403(19) 0.0293(11) Uani 1 1 d . . . C16 C 0.2261(3) 0.1867(3) 0.76049(18) 0.0260(10) Uani 1 1 d . . . C17 C 0.2419(3) 0.2527(3) 0.7780(2) 0.0333(11) Uani 1 1 d . . . H17A H 0.2282 0.3026 0.7487 0.050 Uiso 1 1 calc R . . H17B H 0.3025 0.2264 0.7868 0.050 Uiso 1 1 calc R . . H17C H 0.2051 0.2719 0.8097 0.050 Uiso 1 1 calc R . . C18 C 0.3386(3) -0.0547(3) 0.7538(2) 0.0268(10) Uani 1 1 d . . . H18A H 0.3776 -0.0637 0.7219 0.040 Uiso 1 1 calc R . . H18B H 0.3099 -0.0902 0.7572 0.040 Uiso 1 1 calc R . . H18C H 0.3717 -0.0714 0.7858 0.040 Uiso 1 1 calc R . . C19 C 0.0326(3) 0.1819(4) 0.7167(2) 0.0349(12) Uani 1 1 d . . . H19A H -0.0073 0.2310 0.7343 0.052 Uiso 1 1 calc R . . H19B H 0.0188 0.1342 0.7290 0.052 Uiso 1 1 calc R . . H19C H 0.0270 0.1998 0.6777 0.052 Uiso 1 1 calc R . . C20 C 0.1708(3) 0.0004(3) 0.7144(2) 0.0289(10) Uani 1 1 d . . . H20A H 0.1764 -0.0447 0.7462 0.035 Uiso 1 1 calc R . . H20B H 0.1100 0.0305 0.7038 0.035 Uiso 1 1 calc R . . C21 C 0.2273(3) -0.0449(3) 0.66860(19) 0.0266(10) Uani 1 1 d . . . C22 C 0.2367(3) 0.0037(3) 0.61939(19) 0.0265(10) Uani 1 1 d . . . C23 C 0.2891(3) -0.0368(3) 0.5776(2) 0.0305(11) Uani 1 1 d . . . C24 C 0.3295(3) -0.1278(3) 0.5834(2) 0.0317(11) Uani 1 1 d . . . C25 C 0.3202(3) -0.1762(3) 0.6324(2) 0.0320(11) Uani 1 1 d . . . C26 C 0.2680(3) -0.1358(3) 0.6752(2) 0.0295(11) Uani 1 1 d . . . C27 C 0.2545(4) -0.1909(3) 0.7253(2) 0.0367(12) Uani 1 1 d . . . H27A H 0.2996 -0.2092 0.7505 0.055 Uiso 1 1 calc R . . H27B H 0.2571 -0.2421 0.7160 0.055 Uiso 1 1 calc R . . H27C H 0.1979 -0.1573 0.7419 0.055 Uiso 1 1 calc R . . C28 C 0.1857(3) 0.1014(3) 0.6098(2) 0.0327(11) Uani 1 1 d . . . H28A H 0.2186 0.1250 0.6214 0.049 Uiso 1 1 calc R . . H28B H 0.1308 0.1192 0.6304 0.049 Uiso 1 1 calc R . . H28C H 0.1745 0.1234 0.5715 0.049 Uiso 1 1 calc R . . C29 C 0.3787(4) -0.1727(4) 0.5366(3) 0.0465(15) Uani 1 1 d . . . H29A H 0.4333 -0.1707 0.5300 0.070 Uiso 1 1 calc R . . H29B H 0.3442 -0.1432 0.5044 0.070 Uiso 1 1 calc R . . H29C H 0.3905 -0.2332 0.5451 0.070 Uiso 1 1 calc R . . C30 C 0.2988(3) 0.0172(3) 0.52431(19) 0.0301(11) Uani 1 1 d . . . H30A H 0.2427 0.0485 0.5066 0.036 Uiso 1 1 calc R . . H30B H 0.3409 -0.0230 0.5009 0.036 Uiso 1 1 calc R . . C31 C 0.3279(3) 0.0839(3) 0.52720(18) 0.0237(9) Uani 1 1 d . . . C32 C 0.2822(3) 0.1704(3) 0.50102(18) 0.0266(10) Uani 1 1 d . . . C33 C 0.3130(3) 0.2279(3) 0.50364(19) 0.0275(10) Uani 1 1 d . . . C34 C 0.3843(3) 0.2036(3) 0.53340(19) 0.0291(10) Uani 1 1 d . . . C35 C 0.4309(3) 0.1160(3) 0.55834(18) 0.0245(10) Uani 1 1 d . . . C36 C 0.4038(3) 0.0564(3) 0.55307(18) 0.0260(10) Uani 1 1 d . . . C37 C 0.4605(3) -0.0388(3) 0.5738(2) 0.0290(10) Uani 1 1 d . . . H37A H 0.5199 -0.0500 0.5756 0.044 Uiso 1 1 calc R . . H37B H 0.4590 -0.0731 0.5495 0.044 Uiso 1 1 calc R . . H37C H 0.4395 -0.0549 0.6097 0.044 Uiso 1 1 calc R . . C38 C 0.2012(3) 0.2024(4) 0.4705(2) 0.0339(12) Uani 1 1 d . . . H38A H 0.1950 0.1527 0.4667 0.051 Uiso 1 1 calc R . . H38B H 0.2057 0.2344 0.4349 0.051 Uiso 1 1 calc R . . H38C H 0.1508 0.2406 0.4904 0.051 Uiso 1 1 calc R . . C39 C 0.4087(3) 0.2718(3) 0.5367(2) 0.0306(11) Uani 1 1 d . . . H39A H 0.4173 0.2992 0.5004 0.046 Uiso 1 1 calc R . . H39B H 0.4621 0.2446 0.5562 0.046 Uiso 1 1 calc R . . H39C H 0.3624 0.3157 0.5557 0.046 Uiso 1 1 calc R . . C40 C 0.5128(3) 0.0844(3) 0.58797(19) 0.0263(10) Uani 1 1 d . . . H40A H 0.5201 0.1353 0.5884 0.032 Uiso 1 1 calc R . . H40B H 0.5624 0.0461 0.5669 0.032 Uiso 1 1 calc R . . C41 C 0.8800(4) -0.0977(6) 0.7528(3) 0.064(2) Uani 1 1 d . . . H41A H 0.9384 -0.1297 0.7379 0.096 Uiso 1 1 calc R . . H41B H 0.8830 -0.0869 0.7882 0.096 Uiso 1 1 calc R . . H41C H 0.8486 -0.0424 0.7287 0.096 Uiso 1 1 calc R . . C42 C 0.7595(3) -0.1208(4) 0.7380(2) 0.0345(12) Uani 1 1 d . . . H42 H 0.7250 -0.0636 0.7197 0.041 Uiso 1 1 calc R . . C43 C 0.8645(4) -0.2367(5) 0.7826(3) 0.0537(17) Uani 1 1 d . . . H43 H 0.9169 -0.2732 0.8008 0.064 Uiso 1 1 calc R . . C44 C 0.8064(4) -0.2581(4) 0.7752(2) 0.0473(15) Uani 1 1 d . . . H44 H 0.8093 -0.3133 0.7868 0.057 Uiso 1 1 calc R . . C45 C 0.6638(3) -0.1830(3) 0.7282(2) 0.0276(10) Uani 1 1 d . . . H45A H 0.6424 -0.2158 0.7569 0.033 Uiso 1 1 calc R . . H45B H 0.6815 -0.2121 0.6966 0.033 Uiso 1 1 calc R . . C46 C 0.3818(5) 0.4636(5) 0.3202(3) 0.078(3) Uani 1 1 d . . . H46A H 0.3519 0.4776 0.2871 0.118 Uiso 1 1 calc R . . H46B H 0.4434 0.4432 0.3118 0.118 Uiso 1 1 calc R . . H46C H 0.3580 0.5155 0.3365 0.118 Uiso 1 1 calc R . . C47 C 0.3167(4) 0.4061(4) 0.4015(2) 0.0439(14) Uani 1 1 d . . . H47 H 0.2810 0.4599 0.4133 0.053 Uiso 1 1 calc R . . C48 C 0.4101(4) 0.3089(4) 0.3547(2) 0.0396(13) Uani 1 1 d . . . H48 H 0.4516 0.2822 0.3279 0.048 Uiso 1 1 calc R . . C49 C 0.3797(3) 0.2696(3) 0.3961(2) 0.0341(12) Uani 1 1 d . . . H49 H 0.3955 0.2098 0.4040 0.041 Uiso 1 1 calc R . . C50 C 0.2682(3) 0.3201(3) 0.4726(2) 0.0319(11) Uani 1 1 d . . . H50A H 0.2118 0.3327 0.4610 0.038 Uiso 1 1 calc R . . H50B H 0.2577 0.3612 0.4963 0.038 Uiso 1 1 calc R . . C51 C -0.0811(4) 0.4912(4) 0.5754(2) 0.0467(15) Uani 1 1 d . . . H51A H -0.0953 0.4608 0.5543 0.070 Uiso 1 1 calc R . . H51B H -0.0640 0.5312 0.5511 0.070 Uiso 1 1 calc R . . H51C H -0.1316 0.5239 0.5974 0.070 Uiso 1 1 calc R . . C52 C -0.0185(3) 0.4028(3) 0.6631(2) 0.0354(12) Uani 1 1 d . . . H52 H -0.0712 0.4227 0.6837 0.042 Uiso 1 1 calc R . . C53 C 0.0752(4) 0.3831(4) 0.5959(2) 0.0482(16) Uani 1 1 d . . . H53 H 0.0999 0.3869 0.5606 0.058 Uiso 1 1 calc R . . C54 C 0.1175(4) 0.3331(4) 0.6400(2) 0.0423(14) Uani 1 1 d . . . H54 H 0.1779 0.2956 0.6420 0.051 Uiso 1 1 calc R . . C55 C 0.0744(4) 0.3056(3) 0.7392(2) 0.0360(12) Uani 1 1 d . . . H55A H 0.0205 0.3090 0.7578 0.043 Uiso 1 1 calc R . . H55B H 0.0930 0.3376 0.7566 0.043 Uiso 1 1 calc R . . C56 C 0.1463(6) -0.3037(7) 0.5654(5) 0.102(4) Uani 1 1 d . . . H56A H 0.1332 -0.2510 0.5386 0.152 Uiso 1 1 calc R . . H56B H 0.0959 -0.2945 0.5895 0.152 Uiso 1 1 calc R . . H56C H 0.1611 -0.3519 0.5471 0.152 Uiso 1 1 calc R . . C57 C 0.2491(4) -0.2701(4) 0.5972(3) 0.0490(15) Uani 1 1 d . . . H57 H 0.2274 -0.2126 0.5776 0.059 Uiso 1 1 calc R . . C58 C 0.2678(6) -0.4017(6) 0.6309(5) 0.096(3) Uani 1 1 d . . . H58 H 0.2615 -0.4523 0.6368 0.115 Uiso 1 1 calc R . . C59 C 0.3254(6) -0.3924(5) 0.6542(4) 0.082(3) Uani 1 1 d . . . H59 H 0.3645 -0.4329 0.6811 0.098 Uiso 1 1 calc R . . C60 C 0.3691(4) -0.2744(3) 0.6414(2) 0.0372(12) Uani 1 1 d . . . H60A H 0.4214 -0.2933 0.6176 0.045 Uiso 1 1 calc R . . H60B H 0.3874 -0.2971 0.6791 0.045 Uiso 1 1 calc R . . C61 C 0.7743(3) 0.0997(3) -0.17132(19) 0.0259(10) Uani 1 1 d . . . C62 C 0.8540(3) 0.0595(3) -0.14730(18) 0.0241(9) Uani 1 1 d . . . C63 C 0.8823(3) -0.0221(3) -0.11365(18) 0.0236(9) Uani 1 1 d . . . C64 C 0.8330(3) -0.0658(3) -0.10747(18) 0.0224(9) Uani 1 1 d . . . C65 C 0.7530(3) -0.0243(3) -0.13232(18) 0.0226(9) Uani 1 1 d . . . C66 C 0.7247(3) 0.0566(3) -0.16534(18) 0.0264(10) Uani 1 1 d . . . C67 C 0.6415(3) 0.1001(4) -0.1959(2) 0.0349(12) Uani 1 1 d . . . H67A H 0.6321 0.0557 -0.2056 0.052 Uiso 1 1 calc R . . H67B H 0.6460 0.1385 -0.2285 0.052 Uiso 1 1 calc R . . H67C H 0.5930 0.1340 -0.1731 0.052 Uiso 1 1 calc R . . C68 C 0.9118(3) 0.1015(4) -0.1579(2) 0.0312(11) Uani 1 1 d . . . H68A H 0.8874 0.1532 -0.1859 0.047 Uiso 1 1 calc R . . H68B H 0.9693 0.0604 -0.1698 0.047 Uiso 1 1 calc R . . H68C H 0.9160 0.1181 -0.1248 0.047 Uiso 1 1 calc R . . C69 C 0.8686(3) -0.1579(3) -0.0782(2) 0.0287(10) Uani 1 1 d . . . H69A H 0.9316 -0.1873 -0.0822 0.043 Uiso 1 1 calc R . . H69B H 0.8458 -0.1881 -0.0933 0.043 Uiso 1 1 calc R . . H69C H 0.8516 -0.1585 -0.0400 0.043 Uiso 1 1 calc R . . C70 C 0.9693(3) -0.0658(3) -0.08702(19) 0.0257(10) Uani 1 1 d . . . H70A H 1.0111 -0.1109 -0.1077 0.031 Uiso 1 1 calc R . . H70B H 0.9886 -0.0218 -0.0912 0.031 Uiso 1 1 calc R . . C71 C 0.9755(3) -0.1080(3) -0.02790(18) 0.0218(9) Uani 1 1 d . . . C72 C 0.9242(3) -0.0572(3) 0.01084(19) 0.0220(9) Uani 1 1 d . . . C73 C 0.9258(3) -0.0945(3) 0.06568(19) 0.0212(9) Uani 1 1 d . . . C74 C 0.9835(3) -0.1831(3) 0.08202(18) 0.0210(9) Uani 1 1 d . . . C75 C 1.0380(3) -0.2316(3) 0.04401(19) 0.0232(9) Uani 1 1 d . . . C76 C 1.0345(3) -0.1962(3) -0.01091(19) 0.0242(10) Uani 1 1 d . . . C77 C 1.0945(3) -0.2544(3) -0.0497(2) 0.0302(11) Uani 1 1 d . . . H77A H 1.0896 -0.2200 -0.0858 0.045 Uiso 1 1 calc R . . H77B H 1.0788 -0.2995 -0.0499 0.045 Uiso 1 1 calc R . . H77C H 1.1540 -0.2816 -0.0383 0.045 Uiso 1 1 calc R . . C78 C 0.8697(3) 0.0392(3) -0.00625(19) 0.0242(9) Uani 1 1 d . . . H78A H 0.8136 0.0516 -0.0172 0.036 Uiso 1 1 calc R . . H78B H 0.8987 0.0603 -0.0365 0.036 Uiso 1 1 calc R . . H78C H 0.8615 0.0683 0.0239 0.036 Uiso 1 1 calc R . . C79 C 0.9894(3) -0.2278(3) 0.1403(2) 0.0280(10) Uani 1 1 d . . . H79A H 0.9750 -0.2747 0.1438 0.042 Uiso 1 1 calc R . . H79B H 0.9489 -0.1858 0.1626 0.042 Uiso 1 1 calc R . . H79C H 1.0482 -0.2518 0.1522 0.042 Uiso 1 1 calc R . . C80 C 0.8710(3) -0.0393(3) 0.10743(19) 0.0239(9) Uani 1 1 d . . . H80A H 0.8956 -0.0018 0.1107 0.029 Uiso 1 1 calc R . . H80B H 0.8778 -0.0787 0.1424 0.029 Uiso 1 1 calc R . . C81 C 0.7742(3) 0.0190(3) 0.09908(17) 0.0192(9) Uani 1 1 d . . . C82 C 0.7234(3) -0.0145(3) 0.08700(17) 0.0187(8) Uani 1 1 d . . . C83 C 0.6366(3) 0.0409(3) 0.07443(17) 0.0185(8) Uani 1 1 d . . . C84 C 0.5993(3) 0.1285(3) 0.07900(17) 0.0180(8) Uani 1 1 d . . . C85 C 0.6467(3) 0.1572(3) 0.09998(18) 0.0205(9) Uani 1 1 d . . . C86 C 0.7354(3) 0.1040(3) 0.10801(18) 0.0216(9) Uani 1 1 d . . . C87 C 0.7872(3) 0.1380(3) 0.1268(2) 0.0283(10) Uani 1 1 d . . . H87A H 0.8122 0.1030 0.1614 0.042 Uiso 1 1 calc R . . H87B H 0.7497 0.1984 0.1311 0.042 Uiso 1 1 calc R . . H87C H 0.8336 0.1348 0.1003 0.042 Uiso 1 1 calc R . . C88 C 0.7626(3) -0.1116(3) 0.08970(19) 0.0211(9) Uani 1 1 d . . . H88A H 0.7800 -0.1250 0.0534 0.032 Uiso 1 1 calc R . . H88B H 0.7199 -0.1304 0.1053 0.032 Uiso 1 1 calc R . . H88C H 0.8131 -0.1419 0.1122 0.032 Uiso 1 1 calc R . . C89 C 0.5078(3) 0.1928(3) 0.06139(19) 0.0249(10) Uani 1 1 d . . . H89A H 0.4667 0.1822 0.0873 0.037 Uiso 1 1 calc R . . H89B H 0.5003 0.1857 0.0258 0.037 Uiso 1 1 calc R . . H89C H 0.4976 0.2520 0.0597 0.037 Uiso 1 1 calc R . . C90 C 0.5792(3) 0.0065(3) 0.06284(18) 0.0199(9) Uani 1 1 d . . . H90A H 0.5253 0.0569 0.0482 0.024 Uiso 1 1 calc R . . H90B H 0.5635 -0.0207 0.0977 0.024 Uiso 1 1 calc R . . C91 C 0.6123(3) -0.0584(3) 0.02490(17) 0.0186(8) Uani 1 1 d . . . C92 C 0.6142(3) -0.1387(3) 0.04155(17) 0.0197(9) Uani 1 1 d . . . C93 C 0.6504(3) -0.1993(3) 0.00711(18) 0.0210(9) Uani 1 1 d . . . C94 C 0.6826(3) -0.1802(3) -0.04438(18) 0.0207(9) Uani 1 1 d . . . C95 C 0.6743(3) -0.0967(3) -0.06303(18) 0.0199(9) Uani 1 1 d . . . C96 C 0.6396(3) -0.0359(3) -0.02816(18) 0.0201(9) Uani 1 1 d . . . C97 C 0.6277(3) 0.0539(3) -0.04649(19) 0.0241(9) Uani 1 1 d . . . H97A H 0.6805 0.0548 -0.0407 0.036 Uiso 1 1 calc R . . H97B H 0.5795 0.0935 -0.0260 0.036 Uiso 1 1 calc R . . H97C H 0.6154 0.0723 -0.0848 0.036 Uiso 1 1 calc R . . C98 C 0.5784(3) -0.1601(3) 0.09663(19) 0.0263(10) Uani 1 1 d . . . H98A H 0.6242 -0.1875 0.1226 0.039 Uiso 1 1 calc R . . H98B H 0.5562 -0.1998 0.0956 0.039 Uiso 1 1 calc R . . H98C H 0.5316 -0.1067 0.1074 0.039 Uiso 1 1 calc R . . C99 C 0.7262(3) -0.2510(3) -0.07903(19) 0.0254(10) Uani 1 1 d . . . H99A H 0.6838 -0.2657 -0.0876 0.038 Uiso 1 1 calc R . . H99B H 0.7729 -0.3026 -0.0592 0.038 Uiso 1 1 calc R . . H99C H 0.7499 -0.2298 -0.1124 0.038 Uiso 1 1 calc R . . C100 C 0.6957(3) -0.0684(3) -0.12110(18) 0.0229(9) Uani 1 1 d . . . H10C H 0.6407 -0.0280 -0.1392 0.027 Uiso 1 1 calc R . . H10D H 0.7242 -0.1201 -0.1385 0.027 Uiso 1 1 calc R . . C101 C 0.8516(13) 0.1646(12) -0.3837(5) 0.210(10) Uani 1 1 d . . . H10E H 0.9087 0.1153 -0.3750 0.315 Uiso 1 1 calc R . . H10F H 0.8581 0.2130 -0.4062 0.315 Uiso 1 1 calc R . . H10G H 0.8205 0.1476 -0.4032 0.315 Uiso 1 1 calc R . . C102 C 0.8168(7) 0.1542(6) -0.2853(3) 0.073(3) Uani 1 1 d . . . H102 H 0.8656 0.1031 -0.2701 0.088 Uiso 1 1 calc R . . C103 C 0.7270(13) 0.2572(13) -0.3434(4) 0.156(9) Uani 1 1 d . . . H103 H 0.7023 0.2892 -0.3771 0.187 Uiso 1 1 calc R . . C104 C 0.6853(7) 0.2738(7) -0.2924(3) 0.090(3) Uani 1 1 d . . . H104 H 0.6311 0.3197 -0.2840 0.108 Uiso 1 1 calc R . . C105 C 0.7359(4) 0.1927(4) -0.2000(2) 0.0365(12) Uani 1 1 d . . . H10H H 0.6737 0.2224 -0.1900 0.044 Uiso 1 1 calc R . . H10I H 0.7630 0.2214 -0.1870 0.044 Uiso 1 1 calc R . . C106 C 1.3632(3) -0.4328(3) 0.1667(2) 0.0358(12) Uani 1 1 d . . . H10J H 1.3386 -0.4316 0.2035 0.054 Uiso 1 1 calc R . . H10K H 1.4049 -0.4110 0.1621 0.054 Uiso 1 1 calc R . . H10L H 1.3923 -0.4925 0.1601 0.054 Uiso 1 1 calc R . . C107 C 1.2318(3) -0.3942(3) 0.1199(2) 0.0275(10) Uani 1 1 d . . . H107 H 1.2263 -0.4441 0.1365 0.033 Uiso 1 1 calc R . . C108 C 1.2805(3) -0.3001(3) 0.0971(2) 0.0289(11) Uani 1 1 d . . . H108 H 1.3148 -0.2726 0.0953 0.035 Uiso 1 1 calc R . . C109 C 1.2085(3) -0.2701(3) 0.0689(2) 0.0297(11) Uani 1 1 d . . . H109 H 1.1834 -0.2180 0.0435 0.036 Uiso 1 1 calc R . . C110 C 1.1037(3) -0.3255(3) 0.0628(2) 0.0269(10) Uani 1 1 d . . . H11A H 1.0769 -0.3535 0.0910 0.032 Uiso 1 1 calc R . . H11B H 1.1227 -0.3571 0.0323 0.032 Uiso 1 1 calc R . . C111 C 0.7547(5) -0.4652(5) 0.2046(3) 0.0616(19) Uani 1 1 d . . . H11C H 0.6975 -0.4603 0.2141 0.092 Uiso 1 1 calc R . . H11D H 0.7708 -0.4447 0.2315 0.092 Uiso 1 1 calc R . . H11E H 0.7969 -0.5259 0.2037 0.092 Uiso 1 1 calc R . . C112 C 0.6873(4) -0.3727(3) 0.1188(2) 0.0334(11) Uani 1 1 d . . . H112 H 0.6327 -0.3706 0.1269 0.040 Uiso 1 1 calc R . . C113 C 0.8195(4) -0.4016(4) 0.1252(3) 0.0438(15) Uani 1 1 d . . . H113 H 0.8749 -0.4242 0.1389 0.053 Uiso 1 1 calc R . . C114 C 0.7939(3) -0.3534(4) 0.0760(3) 0.0397(13) Uani 1 1 d . . . H114 H 0.8264 -0.3347 0.0489 0.048 Uiso 1 1 calc R . . C115 C 0.6540(3) -0.2868(3) 0.02715(19) 0.0238(9) Uani 1 1 d . . . H11F H 0.5950 -0.2780 0.0377 0.029 Uiso 1 1 calc R . . H11G H 0.6756 -0.3204 -0.0025 0.029 Uiso 1 1 calc R . . C116 C 0.5773(4) 0.5305(4) 0.0590(3) 0.0445(14) Uani 1 1 d . . . H11H H 0.5379 0.5522 0.0894 0.067 Uiso 1 1 calc R . . H11I H 0.5518 0.5695 0.0254 0.067 Uiso 1 1 calc R . . H11J H 0.6322 0.5281 0.0633 0.067 Uiso 1 1 calc R . . C117 C 0.5854(3) 0.3874(3) 0.0999(2) 0.0311(11) Uani 1 1 d . . . H117 H 0.5692 0.3985 0.1356 0.037 Uiso 1 1 calc R . . C118 C 0.6166(4) 0.4032(4) 0.0134(2) 0.0444(15) Uani 1 1 d . . . H118 H 0.6268 0.4268 -0.0222 0.053 Uiso 1 1 calc R . . C119 C 0.6234(4) 0.3241(3) 0.0307(2) 0.0405(13) Uani 1 1 d . . . H119 H 0.6383 0.2817 0.0092 0.049 Uiso 1 1 calc R . . C120 C 0.5987(3) 0.2426(3) 0.1210(2) 0.0251(10) Uani 1 1 d . . . H12A H 0.5372 0.2577 0.1273 0.030 Uiso 1 1 calc R . . H12B H 0.6221 0.2344 0.1560 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0393(8) 0.0567(10) 0.0734(12) -0.0128(9) 0.0138(8) -0.0168(7) Cl2 0.168(4) 0.120(3) 0.124(3) -0.034(2) 0.008(2) -0.046(2) Cl3 0.145(2) 0.0885(17) 0.0779(15) 0.0045(13) -0.0290(15) -0.0701(17) Cl4 0.164(3) 0.134(3) 0.117(2) -0.038(2) 0.032(2) -0.088(3) Cl5 0.0568(11) 0.0729(12) 0.0580(11) -0.0105(9) -0.0053(9) -0.0115(9) Cl6 0.0319(7) 0.0401(8) 0.1173(16) -0.0263(9) 0.0165(8) -0.0237(6) Cl7 0.0406(8) 0.0391(8) 0.0520(9) -0.0039(7) 0.0024(7) -0.0135(6) Cl8 0.0340(17) 0.073(3) 0.046(2) -0.0067(17) -0.0196(14) -0.0047(16) Cl8' 0.126(5) 0.103(4) 0.103(4) -0.023(3) 0.041(3) -0.071(4) O3W 0.041(3) 0.285(10) 0.029(3) 0.024(4) -0.008(2) -0.069(5) O4W 0.075(8) 0.047(6) 0.127(10) 0.020(7) -0.063(8) -0.028(6) O5W 0.068(3) 0.071(3) 0.095(4) -0.008(3) -0.010(3) -0.047(3) O6W 0.050(3) 0.062(3) 0.082(4) -0.023(3) -0.001(3) -0.014(2) O7W 0.074(9) 0.059(7) 0.043(6) -0.018(5) 0.009(5) -0.045(7) O8W 0.076(12) 0.22(3) 0.094(19) -0.08(2) 0.003(11) -0.069(16) O9W 0.081(4) 0.047(3) 0.086(4) 0.002(3) 0.015(3) -0.027(3) O10W 0.090(8) 0.054(6) 0.030(5) -0.024(4) -0.005(5) 0.002(5) O11W 0.086(5) 0.233(9) 0.126(6) -0.122(6) 0.016(4) -0.094(6) O12W 0.068(3) 0.081(4) 0.065(3) -0.005(3) -0.018(3) -0.051(3) O13W 0.126(6) 0.094(5) 0.131(6) -0.015(4) -0.029(5) -0.074(5) O16W 0.082(4) 0.070(3) 0.044(3) -0.011(3) 0.018(3) -0.014(3) O17W 0.065(3) 0.066(3) 0.077(4) -0.021(3) -0.006(3) -0.032(3) O18W 0.143(13) 0.136(12) 0.082(9) -0.047(8) -0.023(8) -0.083(10) O19W 0.104(9) 0.059(7) 0.161(12) 0.004(7) -0.085(9) -0.050(7) O20W 0.129(7) 0.104(5) 0.127(6) -0.038(5) -0.045(5) -0.029(5) O21W 0.20(2) 0.107(13) 0.27(3) -0.080(15) 0.151(19) -0.093(14) O22W 0.214(11) 0.124(7) 0.165(9) -0.074(7) 0.058(8) -0.078(7) O23W 0.047(3) 0.101(4) 0.054(3) -0.021(3) -0.003(2) -0.026(3) O24W 0.423(19) 0.204(10) 0.066(5) -0.038(6) -0.012(8) -0.224(12) O25W 0.070(4) 0.074(4) 0.067(3) 0.008(3) -0.022(3) -0.021(3) O26W 0.063(3) 0.088(4) 0.062(3) -0.003(3) -0.002(3) -0.046(3) O27W 0.052(3) 0.207(8) 0.053(3) 0.011(4) -0.003(3) -0.050(4) O28W 0.144(6) 0.124(5) 0.050(3) -0.006(3) 0.000(3) -0.110(5) O29W 0.046(3) 0.056(3) 0.067(3) 0.000(2) -0.015(2) 0.001(2) O30W 0.060(3) 0.040(2) 0.085(4) -0.021(2) -0.008(3) -0.013(2) O31W 0.055(3) 0.053(3) 0.094(4) -0.001(3) 0.000(3) -0.024(2) O4W' 0.100(10) 0.112(11) 0.069(8) -0.009(8) -0.007(7) -0.055(9) O7W' 0.032(5) 0.032(5) 0.128(12) -0.007(6) -0.011(6) -0.023(4) O8W' 0.060(14) 0.20(3) 0.079(14) -0.035(16) -0.043(12) -0.012(15) N1 0.029(2) 0.070(4) 0.044(3) -0.026(3) 0.010(2) -0.022(3) N2 0.021(2) 0.035(2) 0.022(2) -0.0052(17) -0.0014(16) -0.0049(17) N3 0.042(3) 0.034(3) 0.042(3) 0.007(2) 0.005(2) -0.012(2) N4 0.029(2) 0.026(2) 0.021(2) -0.0004(16) -0.0034(16) -0.0080(17) N5 0.033(2) 0.038(3) 0.034(2) 0.003(2) -0.0042(19) -0.016(2) N6 0.025(2) 0.027(2) 0.029(2) 0.0024(17) -0.0018(17) -0.0082(17) N7 0.049(3) 0.073(4) 0.094(5) -0.050(4) -0.001(3) -0.031(3) N8 0.042(3) 0.035(3) 0.064(3) -0.015(2) 0.000(2) -0.022(2) N9 0.214(12) 0.211(12) 0.040(4) -0.031(6) 0.035(6) -0.191(11) N10 0.082(4) 0.075(4) 0.032(3) 0.013(3) -0.014(3) -0.063(4) N11 0.0166(18) 0.0184(18) 0.030(2) -0.0018(16) 0.0014(15) -0.0064(15) N12 0.0179(19) 0.029(2) 0.033(2) -0.0029(18) -0.0005(16) -0.0068(17) N13 0.027(2) 0.022(2) 0.037(2) -0.0075(18) -0.0023(17) -0.0101(17) N14 0.048(3) 0.032(2) 0.040(3) -0.006(2) -0.014(2) -0.012(2) N15 0.036(2) 0.023(2) 0.044(3) -0.0068(19) 0.005(2) -0.0151(19) N16 0.023(2) 0.0212(19) 0.031(2) -0.0050(16) 0.0018(16) -0.0102(16) C1 0.021(2) 0.027(2) 0.025(2) -0.0068(19) -0.0009(18) -0.0081(19) C2 0.026(2) 0.028(2) 0.021(2) -0.0024(19) -0.0024(18) -0.013(2) C3 0.022(2) 0.026(2) 0.024(2) -0.0070(19) -0.0005(18) -0.0113(19) C4 0.024(2) 0.024(2) 0.024(2) -0.0038(19) 0.0011(18) -0.0105(19) C5 0.024(2) 0.025(2) 0.019(2) -0.0009(18) -0.0024(17) -0.0106(19) C6 0.024(2) 0.029(2) 0.022(2) -0.0056(19) -0.0008(18) -0.011(2) C7 0.028(3) 0.031(3) 0.025(2) -0.008(2) 0.0021(19) -0.006(2) C8 0.027(2) 0.032(3) 0.025(2) 0.000(2) -0.0013(19) -0.011(2) C9 0.035(3) 0.024(2) 0.026(3) 0.000(2) 0.002(2) -0.007(2) C10 0.024(2) 0.029(2) 0.019(2) -0.0041(19) -0.0024(17) -0.0103(19) C11 0.027(2) 0.030(2) 0.015(2) -0.0027(18) 0.0038(17) -0.012(2) C12 0.023(2) 0.025(2) 0.016(2) 0.0003(17) 0.0004(17) -0.0092(19) C13 0.022(2) 0.031(3) 0.022(2) -0.0019(19) 0.0027(18) -0.013(2) C14 0.024(2) 0.033(3) 0.018(2) -0.0016(19) 0.0027(18) -0.010(2) C15 0.028(2) 0.025(2) 0.022(2) -0.0020(19) 0.0020(19) -0.004(2) C16 0.027(2) 0.026(2) 0.019(2) -0.0042(18) 0.0007(18) -0.0079(19) C17 0.032(3) 0.027(3) 0.032(3) -0.008(2) 0.000(2) -0.007(2) C18 0.025(2) 0.022(2) 0.028(2) -0.0018(19) -0.0040(19) -0.0075(19) C19 0.023(2) 0.039(3) 0.033(3) -0.003(2) 0.000(2) -0.008(2) C20 0.022(2) 0.033(3) 0.031(3) -0.003(2) 0.0001(19) -0.014(2) C21 0.025(2) 0.029(2) 0.028(2) -0.005(2) -0.0012(19) -0.015(2) C22 0.026(2) 0.026(2) 0.028(2) -0.004(2) -0.0053(19) -0.012(2) C23 0.029(3) 0.036(3) 0.029(3) -0.006(2) -0.003(2) -0.016(2) C24 0.030(3) 0.030(3) 0.035(3) -0.010(2) -0.002(2) -0.013(2) C25 0.035(3) 0.027(3) 0.040(3) -0.005(2) -0.007(2) -0.018(2) C26 0.029(3) 0.028(3) 0.034(3) 0.001(2) -0.009(2) -0.016(2) C27 0.040(3) 0.031(3) 0.038(3) -0.001(2) -0.003(2) -0.018(2) C28 0.032(3) 0.029(3) 0.027(3) -0.004(2) 0.001(2) -0.008(2) C29 0.056(4) 0.044(3) 0.047(4) -0.022(3) 0.013(3) -0.027(3) C30 0.033(3) 0.033(3) 0.024(2) -0.005(2) -0.001(2) -0.015(2) C31 0.024(2) 0.026(2) 0.018(2) -0.0072(18) 0.0030(17) -0.0097(19) C32 0.023(2) 0.030(2) 0.019(2) -0.0044(19) -0.0004(18) -0.007(2) C33 0.025(2) 0.022(2) 0.024(2) -0.0018(19) 0.0009(19) -0.0040(19) C34 0.030(3) 0.027(2) 0.022(2) -0.0044(19) 0.0012(19) -0.008(2) C35 0.026(2) 0.024(2) 0.019(2) -0.0025(18) 0.0002(18) -0.0087(19) C36 0.029(2) 0.026(2) 0.017(2) -0.0034(18) 0.0010(18) -0.010(2) C37 0.029(3) 0.025(2) 0.030(3) -0.004(2) -0.002(2) -0.011(2) C38 0.029(3) 0.034(3) 0.028(3) 0.000(2) -0.008(2) -0.007(2) C39 0.031(3) 0.025(2) 0.030(3) -0.001(2) -0.005(2) -0.009(2) C40 0.022(2) 0.028(2) 0.024(2) -0.0012(19) 0.0012(18) -0.0099(19) C41 0.036(3) 0.104(6) 0.071(5) -0.040(4) 0.009(3) -0.040(4) C42 0.030(3) 0.046(3) 0.027(3) -0.008(2) 0.004(2) -0.019(2) C43 0.024(3) 0.070(5) 0.051(4) -0.021(3) -0.007(3) -0.004(3) C44 0.032(3) 0.042(3) 0.042(3) -0.005(3) -0.010(3) 0.003(3) C45 0.023(2) 0.026(2) 0.027(2) -0.005(2) -0.0003(19) -0.0068(19) C46 0.069(5) 0.045(4) 0.082(6) 0.023(4) 0.023(4) -0.018(4) C47 0.042(3) 0.024(3) 0.050(4) 0.001(2) 0.003(3) -0.008(2) C48 0.030(3) 0.046(3) 0.032(3) -0.006(2) 0.002(2) -0.011(2) C49 0.034(3) 0.029(3) 0.034(3) -0.008(2) 0.003(2) -0.011(2) C50 0.027(3) 0.028(3) 0.032(3) -0.003(2) 0.002(2) -0.008(2) C51 0.035(3) 0.048(4) 0.041(3) 0.007(3) -0.011(3) -0.011(3) C52 0.027(3) 0.035(3) 0.034(3) 0.000(2) 0.000(2) -0.009(2) C53 0.037(3) 0.044(3) 0.038(3) 0.010(3) 0.005(3) -0.008(3) C54 0.024(3) 0.042(3) 0.042(3) 0.002(3) 0.004(2) -0.006(2) C55 0.034(3) 0.030(3) 0.027(3) 0.000(2) -0.004(2) -0.003(2) C56 0.065(6) 0.139(9) 0.145(9) -0.083(8) 0.005(6) -0.061(6) C57 0.047(4) 0.050(4) 0.063(4) -0.028(3) 0.003(3) -0.027(3) C58 0.076(6) 0.066(6) 0.178(11) -0.055(7) 0.010(6) -0.049(5) C59 0.083(6) 0.035(4) 0.137(8) -0.012(4) -0.023(6) -0.032(4) C60 0.037(3) 0.033(3) 0.047(3) -0.011(2) 0.000(2) -0.020(2) C61 0.027(2) 0.030(2) 0.022(2) 0.0006(19) -0.0030(18) -0.016(2) C62 0.027(2) 0.031(2) 0.020(2) -0.0066(19) 0.0040(18) -0.019(2) C63 0.018(2) 0.031(2) 0.025(2) -0.0059(19) 0.0023(17) -0.0143(19) C64 0.015(2) 0.028(2) 0.026(2) -0.0080(19) 0.0050(17) -0.0109(18) C65 0.019(2) 0.033(2) 0.021(2) -0.0075(19) 0.0045(17) -0.0161(19) C66 0.023(2) 0.040(3) 0.019(2) -0.002(2) -0.0010(18) -0.019(2) C67 0.032(3) 0.046(3) 0.029(3) 0.007(2) -0.011(2) -0.023(2) C68 0.031(3) 0.040(3) 0.029(3) 0.001(2) 0.000(2) -0.025(2) C69 0.019(2) 0.029(3) 0.040(3) -0.003(2) -0.003(2) -0.015(2) C70 0.018(2) 0.032(3) 0.030(2) -0.005(2) 0.0043(18) -0.0155(19) C71 0.0132(19) 0.028(2) 0.028(2) -0.0049(19) -0.0002(17) -0.0130(18) C72 0.014(2) 0.024(2) 0.031(2) -0.0032(19) -0.0040(17) -0.0114(18) C73 0.0122(19) 0.022(2) 0.032(2) -0.0076(19) 0.0013(17) -0.0098(17) C74 0.0137(19) 0.024(2) 0.027(2) -0.0053(18) -0.0015(17) -0.0102(17) C75 0.016(2) 0.020(2) 0.033(3) -0.0037(19) -0.0020(18) -0.0092(17) C76 0.013(2) 0.027(2) 0.032(3) -0.007(2) 0.0032(18) -0.0096(18) C77 0.023(2) 0.024(2) 0.036(3) -0.009(2) 0.006(2) -0.0060(19) C78 0.021(2) 0.022(2) 0.028(2) -0.0013(19) -0.0021(18) -0.0099(18) C79 0.021(2) 0.023(2) 0.033(3) -0.001(2) 0.0031(19) -0.0071(19) C80 0.013(2) 0.027(2) 0.030(2) -0.007(2) -0.0026(17) -0.0074(18) C81 0.0109(18) 0.023(2) 0.024(2) -0.0042(18) -0.0005(16) -0.0090(17) C82 0.016(2) 0.019(2) 0.020(2) -0.0016(17) -0.0003(16) -0.0088(17) C83 0.0150(19) 0.018(2) 0.019(2) -0.0005(16) -0.0015(16) -0.0068(16) C84 0.0149(19) 0.021(2) 0.018(2) -0.0021(17) 0.0006(15) -0.0093(17) C85 0.019(2) 0.019(2) 0.023(2) -0.0054(17) 0.0040(17) -0.0094(17) C86 0.020(2) 0.026(2) 0.022(2) -0.0052(18) -0.0009(17) -0.0132(18) C87 0.020(2) 0.027(2) 0.042(3) -0.009(2) -0.004(2) -0.013(2) C88 0.017(2) 0.018(2) 0.030(2) -0.0043(18) -0.0024(17) -0.0100(17) C89 0.017(2) 0.026(2) 0.027(2) -0.0044(19) -0.0007(18) -0.0072(18) C90 0.0147(19) 0.023(2) 0.023(2) -0.0044(18) 0.0007(16) -0.0099(17) C91 0.0100(18) 0.022(2) 0.023(2) -0.0036(17) -0.0020(16) -0.0064(16) C92 0.0147(19) 0.025(2) 0.023(2) -0.0049(18) 0.0012(16) -0.0124(17) C93 0.020(2) 0.021(2) 0.026(2) -0.0019(18) -0.0025(17) -0.0131(18) C94 0.016(2) 0.023(2) 0.026(2) -0.0049(18) -0.0041(17) -0.0109(17) C95 0.0135(19) 0.023(2) 0.026(2) -0.0036(18) -0.0011(16) -0.0102(17) C96 0.0130(19) 0.024(2) 0.025(2) -0.0006(18) -0.0050(16) -0.0110(17) C97 0.021(2) 0.023(2) 0.026(2) -0.0014(19) 0.0006(18) -0.0103(18) C98 0.026(2) 0.031(3) 0.030(2) -0.005(2) 0.0024(19) -0.020(2) C99 0.024(2) 0.029(2) 0.028(2) -0.011(2) 0.0031(19) -0.015(2) C100 0.020(2) 0.030(2) 0.025(2) -0.0069(19) 0.0017(17) -0.0167(19) C101 0.41(3) 0.31(2) 0.099(9) -0.128(12) 0.149(13) -0.32(2) C102 0.123(7) 0.116(7) 0.039(4) -0.021(4) 0.022(4) -0.105(7) C103 0.27(2) 0.29(2) 0.046(5) 0.057(9) -0.052(9) -0.26(2) C104 0.121(8) 0.123(8) 0.060(5) 0.049(5) -0.051(5) -0.098(7) C105 0.041(3) 0.037(3) 0.034(3) 0.002(2) -0.008(2) -0.023(3) C106 0.023(2) 0.035(3) 0.045(3) 0.000(2) -0.009(2) -0.011(2) C107 0.019(2) 0.023(2) 0.037(3) -0.003(2) 0.0027(19) -0.0096(19) C108 0.026(2) 0.029(3) 0.034(3) -0.001(2) 0.002(2) -0.018(2) C109 0.028(2) 0.030(3) 0.031(3) -0.002(2) 0.003(2) -0.016(2) C110 0.017(2) 0.026(2) 0.038(3) -0.009(2) -0.0014(19) -0.0094(19) C111 0.078(5) 0.061(4) 0.038(4) -0.002(3) -0.015(3) -0.026(4) C112 0.037(3) 0.034(3) 0.028(3) -0.006(2) -0.005(2) -0.014(2) C113 0.035(3) 0.031(3) 0.063(4) -0.007(3) -0.024(3) -0.008(2) C114 0.027(3) 0.031(3) 0.058(4) -0.007(3) -0.011(2) -0.009(2) C115 0.026(2) 0.023(2) 0.026(2) -0.0028(19) -0.0043(18) -0.0146(19) C116 0.051(4) 0.031(3) 0.056(4) -0.015(3) 0.005(3) -0.021(3) C117 0.030(3) 0.030(3) 0.037(3) -0.010(2) 0.003(2) -0.016(2) C118 0.068(4) 0.032(3) 0.034(3) -0.009(2) 0.010(3) -0.027(3) C119 0.058(4) 0.028(3) 0.038(3) -0.010(2) 0.011(3) -0.023(3) C120 0.022(2) 0.019(2) 0.034(3) -0.0057(19) 0.0021(19) -0.0094(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W O1W' 1.48(2) . ? O2W O1W' 1.47(2) . ? N1 C42 1.304(7) . ? N1 C43 1.398(9) . ? N1 C41 1.492(9) . ? N2 C42 1.326(7) . ? N2 C44 1.388(7) . ? N2 C45 1.489(6) . ? N3 C47 1.329(8) . ? N3 C48 1.368(8) . ? N3 C46 1.484(8) . ? N4 C47 1.301(7) . ? N4 C49 1.379(6) . ? N4 C50 1.479(6) . ? N5 C52 1.337(7) . ? N5 C53 1.363(7) . ? N5 C51 1.468(7) . ? N6 C52 1.326(6) . ? N6 C54 1.365(7) . ? N6 C55 1.478(6) . ? N7 C57 1.324(8) . ? N7 C58 1.392(12) . ? N7 C56 1.466(10) . ? N8 C57 1.340(8) . ? N8 C59 1.394(9) . ? N8 C60 1.481(7) . ? N9 C102 1.324(11) . ? N9 C103 1.33(2) . ? N9 C101 1.384(14) . ? N10 C102 1.345(11) . ? N10 C104 1.385(10) . ? N10 C105 1.459(7) . ? N11 C107 1.321(6) . ? N11 C109 1.371(6) . ? N11 C110 1.488(6) . ? N12 C107 1.332(6) . ? N12 C108 1.371(6) . ? N12 C106 1.473(6) . ? N13 C112 1.308(7) . ? N13 C114 1.381(7) . ? N13 C115 1.479(6) . ? N14 C112 1.336(7) . ? N14 C113 1.359(8) . ? N14 C111 1.461(8) . ? N15 C117 1.341(7) . ? N15 C118 1.372(7) . ? N15 C116 1.471(7) . ? N16 C117 1.305(6) . ? N16 C119 1.356(7) . ? N16 C120 1.478(6) . ? C1 C6 1.389(7) . ? C1 C2 1.413(7) . ? C1 C45 1.516(6) . ? C2 C3 1.403(7) . ? C2 C8 1.511(6) . ? C3 C4 1.407(6) . ? C3 C10 1.534(6) . ? C4 C5 1.391(6) . ? C4 C9 1.516(6) . ? C5 C6 1.403(6) . ? C5 C40 1.548(6) . ? C6 C7 1.522(6) . ? C10 C11 1.529(7) . ? C11 C12 1.405(7) . ? C11 C16 1.419(7) . ? C12 C13 1.405(6) . ? C12 C18 1.511(6) . ? C13 C14 1.406(7) . ? C13 C20 1.529(7) . ? C14 C15 1.395(7) . ? C14 C19 1.513(7) . ? C15 C16 1.403(7) . ? C15 C55 1.524(7) . ? C16 C17 1.512(7) . ? C20 C21 1.529(7) . ? C21 C22 1.403(7) . ? C21 C26 1.406(7) . ? C22 C23 1.393(7) . ? C22 C28 1.510(7) . ? C23 C24 1.410(7) . ? C23 C30 1.530(7) . ? C24 C25 1.398(7) . ? C24 C29 1.515(8) . ? C25 C26 1.411(8) . ? C25 C60 1.517(7) . ? C26 C27 1.506(7) . ? C30 C31 1.541(7) . ? C31 C36 1.400(7) . ? C31 C32 1.407(7) . ? C32 C33 1.406(7) . ? C32 C38 1.523(7) . ? C33 C34 1.398(7) . ? C33 C50 1.519(7) . ? C34 C35 1.413(7) . ? C34 C39 1.511(7) . ? C35 C36 1.410(7) . ? C35 C40 1.527(7) . ? C36 C37 1.511(7) . ? C43 C44 1.316(10) . ? C48 C49 1.340(8) . ? C53 C54 1.328(8) . ? C58 C59 1.349(12) . ? C61 C62 1.398(7) . ? C61 C66 1.410(7) . ? C61 C105 1.509(7) . ? C62 C63 1.408(7) . ? C62 C68 1.518(6) . ? C63 C64 1.414(6) . ? C63 C70 1.530(6) . ? C64 C65 1.411(6) . ? C64 C69 1.503(7) . ? C65 C66 1.392(7) . ? C65 C100 1.539(6) . ? C66 C67 1.526(6) . ? C70 C71 1.525(6) . ? C71 C72 1.408(6) . ? C71 C76 1.412(6) . ? C72 C73 1.410(6) . ? C72 C78 1.507(6) . ? C73 C74 1.411(6) . ? C73 C80 1.520(6) . ? C74 C75 1.389(6) . ? C74 C79 1.518(7) . ? C75 C76 1.402(7) . ? C75 C110 1.520(6) . ? C76 C77 1.513(6) . ? C80 C81 1.532(6) . ? C81 C86 1.395(6) . ? C81 C82 1.405(6) . ? C82 C83 1.404(6) . ? C82 C88 1.520(6) . ? C83 C84 1.405(6) . ? C83 C90 1.519(6) . ? C84 C85 1.395(6) . ? C84 C89 1.523(6) . ? C85 C86 1.406(6) . ? C85 C120 1.527(6) . ? C86 C87 1.506(6) . ? C90 C91 1.522(6) . ? C91 C92 1.398(6) . ? C91 C96 1.415(6) . ? C92 C93 1.400(6) . ? C92 C98 1.512(6) . ? C93 C94 1.400(6) . ? C93 C115 1.515(6) . ? C94 C95 1.411(6) . ? C94 C99 1.532(6) . ? C95 C96 1.411(6) . ? C95 C100 1.518(6) . ? C96 C97 1.494(6) . ? C103 C104 1.422(18) . ? C108 C109 1.362(7) . ? C113 C114 1.352(8) . ? C118 C119 1.342(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W O1W' O1W 138.5(15) . . ? C42 N1 C43 109.2(5) . . ? C42 N1 C41 123.9(6) . . ? C43 N1 C41 126.9(6) . . ? C42 N2 C44 108.6(5) . . ? C42 N2 C45 126.8(4) . . ? C44 N2 C45 124.4(5) . . ? C47 N3 C48 108.4(5) . . ? C47 N3 C46 125.9(6) . . ? C48 N3 C46 125.7(5) . . ? C47 N4 C49 108.3(4) . . ? C47 N4 C50 124.7(4) . . ? C49 N4 C50 126.9(4) . . ? C52 N5 C53 107.8(4) . . ? C52 N5 C51 124.6(5) . . ? C53 N5 C51 127.7(5) . . ? C52 N6 C54 108.2(4) . . ? C52 N6 C55 123.8(4) . . ? C54 N6 C55 128.1(4) . . ? C57 N7 C58 108.5(6) . . ? C57 N7 C56 124.5(8) . . ? C58 N7 C56 127.0(7) . . ? C57 N8 C59 109.7(6) . . ? C57 N8 C60 126.0(5) . . ? C59 N8 C60 124.3(6) . . ? C102 N9 C103 109.7(10) . . ? C102 N9 C101 134.0(16) . . ? C103 N9 C101 115.3(14) . . ? C102 N10 C104 112.4(7) . . ? C102 N10 C105 123.8(6) . . ? C104 N10 C105 123.6(7) . . ? C107 N11 C109 108.9(4) . . ? C107 N11 C110 125.1(4) . . ? C109 N11 C110 125.9(4) . . ? C107 N12 C108 108.6(4) . . ? C107 N12 C106 125.3(4) . . ? C108 N12 C106 126.0(4) . . ? C112 N13 C114 109.6(5) . . ? C112 N13 C115 124.8(4) . . ? C114 N13 C115 125.6(4) . . ? C112 N14 C113 107.4(5) . . ? C112 N14 C111 125.1(6) . . ? C113 N14 C111 127.1(5) . . ? C117 N15 C118 107.8(4) . . ? C117 N15 C116 125.0(5) . . ? C118 N15 C116 127.2(5) . . ? C117 N16 C119 109.0(4) . . ? C117 N16 C120 122.4(4) . . ? C119 N16 C120 128.4(4) . . ? C6 C1 C2 121.6(4) . . ? C6 C1 C45 119.7(4) . . ? C2 C1 C45 118.6(4) . . ? C3 C2 C1 118.9(4) . . ? C3 C2 C8 122.2(4) . . ? C1 C2 C8 118.9(4) . . ? C2 C3 C4 119.6(4) . . ? C2 C3 C10 120.2(4) . . ? C4 C3 C10 120.2(4) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 C9 119.7(4) . . ? C3 C4 C9 119.7(4) . . ? C4 C5 C6 120.7(4) . . ? C4 C5 C40 120.2(4) . . ? C6 C5 C40 119.1(4) . . ? C1 C6 C5 118.7(4) . . ? C1 C6 C7 120.3(4) . . ? C5 C6 C7 120.9(4) . . ? C11 C10 C3 116.5(4) . . ? C12 C11 C16 119.4(4) . . ? C12 C11 C10 118.3(4) . . ? C16 C11 C10 122.2(4) . . ? C11 C12 C13 120.8(4) . . ? C11 C12 C18 119.8(4) . . ? C13 C12 C18 119.3(4) . . ? C12 C13 C14 119.8(5) . . ? C12 C13 C20 119.6(4) . . ? C14 C13 C20 120.5(4) . . ? C15 C14 C13 119.0(4) . . ? C15 C14 C19 119.1(4) . . ? C13 C14 C19 121.8(5) . . ? C14 C15 C16 122.0(4) . . ? C14 C15 C55 118.4(5) . . ? C16 C15 C55 119.5(5) . . ? C15 C16 C11 118.7(5) . . ? C15 C16 C17 119.4(4) . . ? C11 C16 C17 121.9(4) . . ? C21 C20 C13 117.0(4) . . ? C22 C21 C26 119.7(5) . . ? C22 C21 C20 120.5(4) . . ? C26 C21 C20 119.8(4) . . ? C23 C22 C21 121.1(4) . . ? C23 C22 C28 118.8(4) . . ? C21 C22 C28 120.1(4) . . ? C22 C23 C24 119.8(5) . . ? C22 C23 C30 120.4(5) . . ? C24 C23 C30 119.7(5) . . ? C25 C24 C23 119.0(5) . . ? C25 C24 C29 120.1(5) . . ? C23 C24 C29 120.9(5) . . ? C24 C25 C26 121.5(5) . . ? C24 C25 C60 120.1(5) . . ? C26 C25 C60 118.4(5) . . ? C21 C26 C25 118.9(4) . . ? C21 C26 C27 122.1(5) . . ? C25 C26 C27 119.0(5) . . ? C23 C30 C31 116.7(4) . . ? C36 C31 C32 119.8(4) . . ? C36 C31 C30 119.4(4) . . ? C32 C31 C30 120.7(4) . . ? C33 C32 C31 118.3(4) . . ? C33 C32 C38 120.0(4) . . ? C31 C32 C38 121.7(5) . . ? C34 C33 C32 122.6(4) . . ? C34 C33 C50 118.2(5) . . ? C32 C33 C50 119.2(4) . . ? C33 C34 C35 118.4(5) . . ? C33 C34 C39 118.5(4) . . ? C35 C34 C39 123.0(4) . . ? C36 C35 C34 119.4(4) . . ? C36 C35 C40 119.9(4) . . ? C34 C35 C40 120.6(4) . . ? C31 C36 C35 121.1(4) . . ? C31 C36 C37 120.2(4) . . ? C35 C36 C37 118.7(4) . . ? C35 C40 C5 117.0(4) . . ? N1 C42 N2 108.2(5) . . ? C44 C43 N1 106.6(5) . . ? C43 C44 N2 107.4(6) . . ? N2 C45 C1 112.1(4) . . ? N4 C47 N3 109.2(5) . . ? C49 C48 N3 106.7(5) . . ? C48 C49 N4 107.4(5) . . ? N4 C50 C33 110.7(4) . . ? N6 C52 N5 108.5(5) . . ? C54 C53 N5 107.9(5) . . ? C53 C54 N6 107.7(5) . . ? N6 C55 C15 109.7(4) . . ? N7 C57 N8 108.0(6) . . ? C59 C58 N7 108.3(7) . . ? C58 C59 N8 105.2(8) . . ? N8 C60 C25 111.4(4) . . ? C62 C61 C66 120.6(4) . . ? C62 C61 C105 120.8(4) . . ? C66 C61 C105 118.4(4) . . ? C61 C62 C63 119.8(4) . . ? C61 C62 C68 121.0(4) . . ? C63 C62 C68 119.1(4) . . ? C62 C63 C64 119.8(4) . . ? C62 C63 C70 119.9(4) . . ? C64 C63 C70 120.2(4) . . ? C65 C64 C63 119.3(4) . . ? C65 C64 C69 120.3(4) . . ? C63 C64 C69 120.2(4) . . ? C66 C65 C64 120.8(4) . . ? C66 C65 C100 120.1(4) . . ? C64 C65 C100 119.1(4) . . ? C65 C66 C61 119.4(4) . . ? C65 C66 C67 121.9(4) . . ? C61 C66 C67 118.7(4) . . ? C71 C70 C63 119.1(4) . . ? C72 C71 C76 119.3(4) . . ? C72 C71 C70 119.3(4) . . ? C76 C71 C70 121.3(4) . . ? C71 C72 C73 121.0(4) . . ? C71 C72 C78 119.5(4) . . ? C73 C72 C78 119.5(4) . . ? C72 C73 C74 119.1(4) . . ? C72 C73 C80 120.9(4) . . ? C74 C73 C80 119.9(4) . . ? C75 C74 C73 119.5(4) . . ? C75 C74 C79 118.3(4) . . ? C73 C74 C79 122.2(4) . . ? C74 C75 C76 121.9(4) . . ? C74 C75 C110 118.8(4) . . ? C76 C75 C110 119.3(4) . . ? C75 C76 C71 119.0(4) . . ? C75 C76 C77 118.3(4) . . ? C71 C76 C77 122.7(4) . . ? C73 C80 C81 119.1(4) . . ? C86 C81 C82 120.0(4) . . ? C86 C81 C80 119.2(4) . . ? C82 C81 C80 120.6(4) . . ? C83 C82 C81 120.3(4) . . ? C83 C82 C88 120.4(4) . . ? C81 C82 C88 119.2(4) . . ? C82 C83 C84 119.0(4) . . ? C82 C83 C90 121.7(4) . . ? C84 C83 C90 118.9(4) . . ? C85 C84 C83 119.5(4) . . ? C85 C84 C89 119.3(4) . . ? C83 C84 C89 121.1(4) . . ? C84 C85 C86 120.9(4) . . ? C84 C85 C120 118.8(4) . . ? C86 C85 C120 119.8(4) . . ? C81 C86 C85 118.8(4) . . ? C81 C86 C87 120.7(4) . . ? C85 C86 C87 120.5(4) . . ? C83 C90 C91 119.4(3) . . ? C92 C91 C96 119.9(4) . . ? C92 C91 C90 120.7(4) . . ? C96 C91 C90 119.3(4) . . ? C91 C92 C93 119.5(4) . . ? C91 C92 C98 120.1(4) . . ? C93 C92 C98 120.4(4) . . ? C94 C93 C92 121.2(4) . . ? C94 C93 C115 120.7(4) . . ? C92 C93 C115 118.1(4) . . ? C93 C94 C95 119.4(4) . . ? C93 C94 C99 118.9(4) . . ? C95 C94 C99 121.7(4) . . ? C96 C95 C94 119.6(4) . . ? C96 C95 C100 118.9(4) . . ? C94 C95 C100 121.4(4) . . ? C95 C96 C91 120.0(4) . . ? C95 C96 C97 121.4(4) . . ? C91 C96 C97 118.5(4) . . ? C95 C100 C65 118.2(4) . . ? N9 C102 N10 106.7(10) . . ? N9 C103 C104 109.8(9) . . ? N10 C104 C103 100.9(11) . . ? N10 C105 C61 115.3(5) . . ? N11 C107 N12 108.7(4) . . ? C109 C108 N12 106.8(4) . . ? C108 C109 N11 106.9(4) . . ? N11 C110 C75 110.0(4) . . ? N13 C112 N14 109.0(5) . . ? C114 C113 N14 109.0(5) . . ? C113 C114 N13 105.0(5) . . ? N13 C115 C93 112.6(4) . . ? N16 C117 N15 108.7(5) . . ? C119 C118 N15 106.6(5) . . ? C118 C119 N16 107.9(5) . . ? N16 C120 C85 113.8(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.21 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.456 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.140 # Attachment 'NO31.CIF' data_c:\rawdat~1\charlo~1\08srv469\work\sad _database_code_depnum_ccdc_archive 'CCDC 722207' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 N8, 4(N O3), (C2H3N)0.66, (H2 O)1.34' _chemical_formula_sum 'C61.33 H80.68 N12.66 O13.34' _chemical_formula_weight 1205.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2373(3) _cell_length_b 16.0639(5) _cell_length_c 19.0982(6) _cell_angle_alpha 114.2490(10) _cell_angle_beta 97.9090(10) _cell_angle_gamma 99.5570(10) _cell_volume 3017.42(16) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1283 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.884897 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 6k' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51679 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 29.18 _reflns_number_total 16296 _reflns_number_gt 7770 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _refine_special_details ; One nitrate anion is disordered over two positions. There is also disorder where an acetonitrile and water molecule share a site. No water hydrogen atoms were refined. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^+0.4341P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16296 _refine_ls_number_parameters 848 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1660 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2765 _refine_ls_wR_factor_gt 0.2197 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.1443(4) 0.2377(3) 0.1562(2) 0.1088(14) Uani 1 1 d . . . O2 O 1.2813(3) 0.1742(3) 0.1858(2) 0.0880(11) Uani 1 1 d . . . O3 O 1.1417(5) 0.1025(3) 0.0752(2) 0.1138(15) Uani 1 1 d . . . O4 O 0.6956(3) 0.7138(2) 0.55855(19) 0.0734(9) Uani 1 1 d . . . O5 O 0.8904(3) 0.7240(2) 0.59799(18) 0.0753(9) Uani 1 1 d . . . O6 O 0.7719(2) 0.59393(17) 0.50947(15) 0.0475(6) Uani 1 1 d . . . O7 O 0.7299(4) 0.2562(3) 0.4488(3) 0.1189(17) Uani 1 1 d . . . O8 O 0.7486(3) 0.1389(2) 0.4699(2) 0.0711(8) Uani 1 1 d . . . O9 O 0.6415(3) 0.2273(3) 0.5309(3) 0.1193(17) Uani 1 1 d . . . O10 O 0.5156(16) 0.0871(12) -0.2058(10) 0.130(8) Uani 0.454(18) 1 d P A 2 O11 O 0.3643(18) 0.1352(12) -0.208(3) 0.31(2) Uani 0.454(18) 1 d P A 2 O12 O 0.3728(19) 0.060(2) -0.1497(14) 0.203(10) Uani 0.454(18) 1 d P A 2 O10' O 0.5458(9) 0.0764(7) -0.1574(10) 0.104(4) Uani 0.546(18) 1 d P A 1 O11' O 0.4267(19) 0.1056(7) -0.2475(5) 0.153(8) Uani 0.546(18) 1 d P A 1 O12' O 0.3714(5) 0.1134(6) -0.1443(3) 0.057(3) Uani 0.546(18) 1 d P A 1 O1W O 1.8512(15) 0.2539(12) 0.3530(7) 0.126(6) Uani 0.336(8) 1 d P B 2 O2W O 0.5907(6) -0.0415(8) -0.0941(4) 0.249(5) Uani 1 1 d . . . N1 N 0.5973(3) 0.9255(2) 0.61482(16) 0.0416(7) Uani 1 1 d . . . N2 N 0.6488(2) 0.93810(18) 0.51377(15) 0.0359(6) Uani 1 1 d . . . N3 N 0.9298(4) 1.0176(3) 0.2631(2) 0.0756(11) Uani 1 1 d . . . N4 N 0.9947(3) 0.9387(2) 0.16040(18) 0.0469(7) Uani 1 1 d . . . N5 N 1.4721(2) 0.4247(2) 0.38052(15) 0.0373(6) Uani 1 1 d . . . N6 N 1.2926(2) 0.44663(19) 0.34794(15) 0.0340(6) Uani 1 1 d . . . N7 N 0.7680(5) 0.1308(4) 0.0767(3) 0.0937(15) Uani 1 1 d . . . N8 N 0.6544(3) 0.2182(2) 0.05653(19) 0.0550(8) Uani 1 1 d . . . N9 N 1.1867(4) 0.1729(3) 0.1402(2) 0.0655(10) Uani 1 1 d . . . N10 N 0.7856(3) 0.6781(2) 0.55526(17) 0.0426(7) Uani 1 1 d . . . N11 N 0.7042(3) 0.2064(2) 0.4830(2) 0.0512(8) Uani 1 1 d . . . N12 N 0.4389(6) 0.0965(3) -0.1886(3) 0.0873(15) Uani 1 1 d . . . N1S N 1.6508(6) 0.1811(6) 0.2292(4) 0.092(3) Uani 0.664(8) 1 d P B 1 C1 C 0.7055(3) 0.8172(2) 0.40145(17) 0.0340(7) Uani 1 1 d . . . C2 C 0.6122(3) 0.7411(2) 0.34340(17) 0.0332(7) Uani 1 1 d . . . C3 C 0.6378(3) 0.6525(2) 0.30818(16) 0.0290(6) Uani 1 1 d . . . C4 C 0.7512(3) 0.6383(2) 0.33613(16) 0.0272(6) Uani 1 1 d . . . C5 C 0.8445(3) 0.7149(2) 0.39432(16) 0.0300(6) Uani 1 1 d . . . C6 C 0.8215(3) 0.8041(2) 0.42776(17) 0.0326(6) Uani 1 1 d . . . C7 C 0.9167(3) 0.8854(2) 0.4966(2) 0.0454(8) Uani 1 1 d . . . H7A H 0.9349 0.8683 0.5399 0.068 Uiso 1 1 calc R . . H7B H 0.8836 0.9415 0.5146 0.068 Uiso 1 1 calc R . . H7C H 0.9930 0.8988 0.4795 0.068 Uiso 1 1 calc R . . C8 C 0.4840(3) 0.7541(3) 0.3218(2) 0.0445(8) Uani 1 1 d . . . H8A H 0.4769 0.7655 0.2750 0.067 Uiso 1 1 calc R . . H8B H 0.4707 0.8080 0.3659 0.067 Uiso 1 1 calc R . . H8C H 0.4215 0.6971 0.3106 0.067 Uiso 1 1 calc R . . C9 C 0.7690(3) 0.5401(2) 0.30858(17) 0.0319(6) Uani 1 1 d . . . H9A H 0.8126 0.5264 0.2656 0.048 Uiso 1 1 calc R . . H9B H 0.6880 0.4949 0.2897 0.048 Uiso 1 1 calc R . . H9C H 0.8181 0.5348 0.3525 0.048 Uiso 1 1 calc R . . C10 C 0.6820(3) 0.9152(2) 0.43655(18) 0.0385(7) Uani 1 1 d . . . H10A H 0.7573 0.9624 0.4435 0.046 Uiso 1 1 calc R . . H10B H 0.6137 0.9184 0.3997 0.046 Uiso 1 1 calc R . . C11 C 0.6238(3) 0.8791(2) 0.5454(2) 0.0435(8) Uani 1 1 d . . . H11 H 0.6246 0.8144 0.5222 0.052 Uiso 1 1 calc R . . C12 C 0.6378(3) 1.0256(2) 0.5650(2) 0.0412(8) Uani 1 1 d . . . H12 H 0.6509 1.0812 0.5577 0.049 Uiso 1 1 calc R . . C13 C 0.6047(3) 1.0169(2) 0.6277(2) 0.0434(8) Uani 1 1 d . . . H13 H 0.5895 1.0653 0.6724 0.052 Uiso 1 1 calc R . . C14 C 0.5637(4) 0.8853(3) 0.6678(2) 0.0567(10) Uani 1 1 d . . . H14A H 0.4741 0.8577 0.6530 0.085 Uiso 1 1 calc R . . H14B H 0.5867 0.9350 0.7223 0.085 Uiso 1 1 calc R . . H14C H 0.6078 0.8363 0.6637 0.085 Uiso 1 1 calc R . . C15 C 0.5383(3) 0.5713(2) 0.24129(16) 0.0311(6) Uani 1 1 d . . . H15A H 0.4728 0.5984 0.2251 0.037 Uiso 1 1 calc R . . H15B H 0.5003 0.5301 0.2633 0.037 Uiso 1 1 calc R . . C16 C 0.5754(2) 0.5086(2) 0.16663(16) 0.0276(6) Uani 1 1 d . . . C17 C 0.6294(2) 0.5507(2) 0.12273(16) 0.0280(6) Uani 1 1 d . . . C18 C 0.6564(2) 0.4946(2) 0.05131(16) 0.0272(6) Uani 1 1 d . . . C19 C 0.6221(3) 0.3963(2) 0.02011(17) 0.0310(6) Uani 1 1 d . . . C20 C 0.5713(3) 0.3553(2) 0.06483(17) 0.0295(6) Uani 1 1 d . . . C21 C 0.5491(3) 0.4113(2) 0.13876(16) 0.0303(6) Uani 1 1 d . . . C22 C 0.4960(3) 0.3608(2) 0.18369(18) 0.0364(7) Uani 1 1 d . . . H22A H 0.5012 0.4068 0.2378 0.055 Uiso 1 1 calc R . . H22B H 0.5434 0.3152 0.1847 0.055 Uiso 1 1 calc R . . H22C H 0.4091 0.3278 0.1576 0.055 Uiso 1 1 calc R . . C23 C 0.6551(3) 0.6558(2) 0.15148(17) 0.0329(7) Uani 1 1 d . . . H23A H 0.7388 0.6855 0.1854 0.049 Uiso 1 1 calc R . . H23B H 0.5944 0.6802 0.1815 0.049 Uiso 1 1 calc R . . H23C H 0.6490 0.6703 0.1062 0.049 Uiso 1 1 calc R . . C24 C 0.6416(3) 0.3354(2) -0.06033(18) 0.0406(8) Uani 1 1 d . . . H24A H 0.7303 0.3391 -0.0570 0.061 Uiso 1 1 calc R . . H24B H 0.6102 0.3577 -0.0982 0.061 Uiso 1 1 calc R . . H24C H 0.5969 0.2699 -0.0778 0.061 Uiso 1 1 calc R . . C25 C 0.5426(3) 0.2444(2) 0.03354(18) 0.0345(7) Uani 1 1 d . . . H25A H 0.4760 0.2236 0.0560 0.041 Uiso 1 1 calc R . . H25B H 0.5139 0.2130 -0.0246 0.041 Uiso 1 1 calc R . . C26 C 0.6514(6) 0.1380(4) 0.0595(4) 0.0965(19) Uani 1 1 d . . . H26 H 0.5785 0.0923 0.0509 0.116 Uiso 1 1 calc R . . C27 C 0.7735(5) 0.2599(4) 0.0699(4) 0.0919(18) Uani 1 1 d . . . H27 H 0.8033 0.3187 0.0697 0.110 Uiso 1 1 calc R . . C28 C 0.8452(6) 0.2068(5) 0.0837(4) 0.0926(18) Uani 1 1 d . . . H28 H 0.9332 0.2210 0.0959 0.111 Uiso 1 1 calc R . . C29 C 0.8012(8) 0.0498(5) 0.0849(5) 0.164(4) Uani 1 1 d . . . H29A H 0.8583 0.0268 0.0511 0.247 Uiso 1 1 calc R . . H29B H 0.7260 -0.0005 0.0690 0.247 Uiso 1 1 calc R . . H29C H 0.8413 0.0693 0.1400 0.247 Uiso 1 1 calc R . . C30 C 0.7216(3) 0.5410(2) 0.00618(16) 0.0313(6) Uani 1 1 d . . . H30A H 0.7378 0.4905 -0.0402 0.038 Uiso 1 1 calc R . . H30B H 0.6630 0.5701 -0.0140 0.038 Uiso 1 1 calc R . . C31 C 0.8429(3) 0.6156(2) 0.05057(16) 0.0285(6) Uani 1 1 d . . . C32 C 0.8622(3) 0.7026(2) 0.04751(16) 0.0304(6) Uani 1 1 d . . . C33 C 0.9774(3) 0.7689(2) 0.08705(17) 0.0328(7) Uani 1 1 d . . . C34 C 1.0709(3) 0.7506(2) 0.13226(17) 0.0320(6) Uani 1 1 d . . . C35 C 1.0501(3) 0.6650(2) 0.13641(16) 0.0299(6) Uani 1 1 d . . . C36 C 0.9392(3) 0.5960(2) 0.09222(16) 0.0288(6) Uani 1 1 d . . . C37 C 0.9265(3) 0.4985(2) 0.08695(18) 0.0344(7) Uani 1 1 d . . . H37A H 0.8953 0.4961 0.1317 0.052 Uiso 1 1 calc R . . H37B H 1.0076 0.4836 0.0882 0.052 Uiso 1 1 calc R . . H37C H 0.8684 0.4525 0.0376 0.052 Uiso 1 1 calc R . . C38 C 0.7635(3) 0.7265(2) 0.00182(19) 0.0369(7) Uani 1 1 d . . . H38A H 0.7346 0.7782 0.0386 0.055 Uiso 1 1 calc R . . H38B H 0.6937 0.6710 -0.0276 0.055 Uiso 1 1 calc R . . H38C H 0.7982 0.7457 -0.0351 0.055 Uiso 1 1 calc R . . C39 C 1.0008(3) 0.8644(2) 0.08539(19) 0.0400(8) Uani 1 1 d . . . H39A H 1.0835 0.8789 0.0747 0.048 Uiso 1 1 calc R . . H39B H 0.9379 0.8618 0.0423 0.048 Uiso 1 1 calc R . . C40 C 0.9050(4) 0.9373(3) 0.1992(2) 0.0532(9) Uani 1 1 d . . . H40 H 0.8344 0.8865 0.1831 0.064 Uiso 1 1 calc R . . C41 C 1.0816(4) 1.0233(3) 0.2032(3) 0.0657(12) Uani 1 1 d . . . H41 H 1.1554 1.0429 0.1892 0.079 Uiso 1 1 calc R . . C42 C 1.0438(5) 1.0730(4) 0.2678(3) 0.0808(15) Uani 1 1 d . . . H42 H 1.0857 1.1337 0.3086 0.097 Uiso 1 1 calc R . . C43 C 0.8529(6) 1.0426(6) 0.3207(3) 0.127(3) Uani 1 1 d . . . H43A H 0.7655 1.0124 0.2939 0.191 Uiso 1 1 calc R . . H43B H 0.8647 1.1111 0.3465 0.191 Uiso 1 1 calc R . . H43C H 0.8769 1.0210 0.3605 0.191 Uiso 1 1 calc R . . C44 C 1.1913(3) 0.8265(2) 0.1750(2) 0.0393(7) Uani 1 1 d . . . H44A H 1.1800 0.8745 0.2240 0.059 Uiso 1 1 calc R . . H44B H 1.2146 0.8557 0.1412 0.059 Uiso 1 1 calc R . . H44C H 1.2570 0.7980 0.1873 0.059 Uiso 1 1 calc R . . C45 C 1.1493(3) 0.6433(2) 0.18534(18) 0.0322(7) Uani 1 1 d . . . H45A H 1.1818 0.5935 0.1481 0.039 Uiso 1 1 calc R . . H45B H 1.2186 0.7005 0.2129 0.039 Uiso 1 1 calc R . . C46 C 1.1145(2) 0.6118(2) 0.24690(16) 0.0302(6) Uani 1 1 d . . . C47 C 1.1438(2) 0.5312(2) 0.24808(17) 0.0304(6) Uani 1 1 d . . . C48 C 1.1221(3) 0.5093(2) 0.31042(18) 0.0327(7) Uani 1 1 d . . . C49 C 1.0699(3) 0.5658(2) 0.36993(17) 0.0323(7) Uani 1 1 d . . . C50 C 1.0335(3) 0.6427(2) 0.36495(16) 0.0299(6) Uani 1 1 d . . . C51 C 1.0616(2) 0.6688(2) 0.30637(16) 0.0299(6) Uani 1 1 d . . . C52 C 1.0421(3) 0.7608(2) 0.31020(19) 0.0367(7) Uani 1 1 d . . . H52A H 1.1079 0.7887 0.2918 0.055 Uiso 1 1 calc R . . H52B H 1.0444 0.8040 0.3648 0.055 Uiso 1 1 calc R . . H52C H 0.9614 0.7498 0.2765 0.055 Uiso 1 1 calc R . . C53 C 1.2009(3) 0.4677(2) 0.18622(18) 0.0348(7) Uani 1 1 d . . . H53A H 1.1351 0.4211 0.1411 0.052 Uiso 1 1 calc R . . H53B H 1.2490 0.4354 0.2087 0.052 Uiso 1 1 calc R . . H53C H 1.2556 0.5056 0.1687 0.052 Uiso 1 1 calc R . . C54 C 1.1584(3) 0.4245(2) 0.3136(2) 0.0381(7) Uani 1 1 d . . . H54A H 1.1106 0.4037 0.3458 0.046 Uiso 1 1 calc R . . H54B H 1.1379 0.3723 0.2596 0.046 Uiso 1 1 calc R . . C55 C 1.3700(3) 0.5338(2) 0.39746(18) 0.0382(7) Uani 1 1 d . . . H55 H 1.3482 0.5925 0.4142 0.046 Uiso 1 1 calc R . . C56 C 1.4825(3) 0.5204(2) 0.41784(18) 0.0382(7) Uani 1 1 d . . . H56 H 1.5550 0.5677 0.4514 0.046 Uiso 1 1 calc R . . C57 C 1.3571(3) 0.3809(2) 0.33840(18) 0.0355(7) Uani 1 1 d . . . H57 H 1.3260 0.3149 0.3071 0.043 Uiso 1 1 calc R . . C58 C 1.5720(4) 0.3777(3) 0.3873(2) 0.0503(9) Uani 1 1 d . . . H58A H 1.5612 0.3509 0.4245 0.075 Uiso 1 1 calc R . . H58B H 1.6524 0.4237 0.4066 0.075 Uiso 1 1 calc R . . H58C H 1.5690 0.3273 0.3355 0.075 Uiso 1 1 calc R . . C59 C 1.0551(3) 0.5443(3) 0.4387(2) 0.0462(9) Uani 1 1 d . . . H59A H 1.0706 0.6034 0.4868 0.069 Uiso 1 1 calc R . . H59B H 1.1145 0.5084 0.4455 0.069 Uiso 1 1 calc R . . H59C H 0.9706 0.5072 0.4283 0.069 Uiso 1 1 calc R . . C60 C 0.9675(3) 0.7002(2) 0.42541(17) 0.0328(7) Uani 1 1 d . . . H60A H 0.9529 0.6691 0.4598 0.039 Uiso 1 1 calc R . . H60B H 1.0245 0.7630 0.4590 0.039 Uiso 1 1 calc R . . C2S C 1.7440(9) 0.2344(7) 0.2666(5) 0.085(3) Uani 0.664(8) 1 d P B 1 C3S C 1.8550(8) 0.3010(7) 0.3112(7) 0.107(4) Uani 0.664(8) 1 d P B 1 H3S1 H 1.8850 0.3340 0.2813 0.161 Uiso 0.664(8) 1 calc PR B 1 H3S2 H 1.9169 0.2693 0.3229 0.161 Uiso 0.664(8) 1 calc PR B 1 H3S3 H 1.8413 0.3465 0.3606 0.161 Uiso 0.664(8) 1 calc PR B 1 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 O1 0.145(4) 0.076(3) 0.092(3) 0.025(2) 0.009(3) 0.038(3) O2 0.077(2) 0.099(3) 0.078(2) 0.042(2) 0.0074(19) -0.003(2) O3 0.180(4) 0.085(3) 0.052(2) 0.016(2) -0.010(2) 0.039(3) O4 0.102(2) 0.087(2) 0.092(2) 0.0673(19) 0.068(2) 0.068(2) O5 0.081(2) 0.071(2) 0.0541(18) 0.0189(16) 0.0124(17) -0.0070(17) O6 0.0557(15) 0.0478(15) 0.0473(14) 0.0237(12) 0.0182(12) 0.0212(12) O7 0.108(3) 0.107(3) 0.155(4) 0.102(3) -0.029(3) -0.008(2) O8 0.080(2) 0.0506(17) 0.088(2) 0.0289(16) 0.0266(18) 0.0282(16) O9 0.063(2) 0.099(3) 0.141(4) -0.006(3) 0.050(2) 0.016(2) O10 0.096(10) 0.157(13) 0.101(12) 0.010(10) 0.084(10) 0.014(9) O11 0.174(15) 0.109(11) 0.72(6) 0.18(2) 0.27(3) 0.068(11) O12 0.180(16) 0.25(3) 0.226(19) 0.143(19) 0.102(14) 0.040(16) O10' 0.057(5) 0.074(5) 0.153(11) 0.023(7) 0.039(6) 0.007(3) O11' 0.29(2) 0.102(7) 0.058(5) 0.034(5) 0.066(8) -0.008(10) O12' 0.034(3) 0.080(5) 0.035(3) 0.007(3) 0.016(2) 0.002(3) O1W 0.149(13) 0.158(14) 0.061(7) 0.047(8) 0.033(8) 0.006(10) O2W 0.152(6) 0.453(13) 0.124(5) 0.082(7) 0.047(4) 0.140(7) N1 0.0490(17) 0.0429(16) 0.0351(14) 0.0168(13) 0.0112(13) 0.0169(13) N2 0.0392(15) 0.0365(15) 0.0333(14) 0.0149(12) 0.0075(11) 0.0152(12) N3 0.078(3) 0.081(3) 0.048(2) 0.007(2) 0.0044(19) 0.035(2) N4 0.0489(17) 0.0458(17) 0.0506(18) 0.0275(15) 0.0073(14) 0.0103(14) N5 0.0407(15) 0.0557(17) 0.0332(13) 0.0275(13) 0.0166(12) 0.0292(13) N6 0.0376(14) 0.0479(16) 0.0308(13) 0.0256(13) 0.0140(11) 0.0207(12) N7 0.122(4) 0.114(4) 0.084(3) 0.054(3) 0.036(3) 0.086(3) N8 0.067(2) 0.061(2) 0.0545(19) 0.0325(17) 0.0231(17) 0.0352(18) N9 0.086(3) 0.062(2) 0.047(2) 0.029(2) 0.009(2) 0.007(2) N10 0.0544(18) 0.0508(18) 0.0408(16) 0.0294(15) 0.0260(15) 0.0225(15) N11 0.0400(17) 0.0480(18) 0.066(2) 0.0254(17) 0.0082(16) 0.0144(14) N12 0.095(4) 0.054(3) 0.071(3) -0.009(2) 0.038(3) -0.007(3) N1S 0.055(4) 0.127(6) 0.070(4) 0.031(4) 0.004(3) 0.004(4) C1 0.0366(16) 0.0421(18) 0.0290(15) 0.0177(14) 0.0111(13) 0.0158(14) C2 0.0338(15) 0.0451(18) 0.0271(14) 0.0174(14) 0.0118(12) 0.0179(14) C3 0.0252(14) 0.0417(17) 0.0222(13) 0.0139(13) 0.0083(11) 0.0118(12) C4 0.0271(14) 0.0395(16) 0.0220(13) 0.0166(12) 0.0111(11) 0.0139(12) C5 0.0281(14) 0.0420(17) 0.0261(14) 0.0188(13) 0.0104(12) 0.0112(13) C6 0.0308(15) 0.0396(17) 0.0285(15) 0.0148(13) 0.0089(12) 0.0104(13) C7 0.0409(18) 0.043(2) 0.046(2) 0.0148(17) 0.0064(15) 0.0105(15) C8 0.0398(18) 0.053(2) 0.0398(18) 0.0147(16) 0.0082(15) 0.0266(16) C9 0.0298(15) 0.0411(17) 0.0263(14) 0.0144(13) 0.0066(12) 0.0139(13) C10 0.0445(18) 0.0441(19) 0.0320(16) 0.0178(15) 0.0116(14) 0.0197(15) C11 0.053(2) 0.0414(19) 0.0394(18) 0.0167(16) 0.0162(16) 0.0182(16) C12 0.0450(19) 0.0323(17) 0.0401(18) 0.0096(15) 0.0041(15) 0.0157(15) C13 0.0452(19) 0.0422(19) 0.0377(18) 0.0109(15) 0.0051(15) 0.0194(16) C14 0.074(3) 0.061(2) 0.044(2) 0.027(2) 0.023(2) 0.023(2) C15 0.0244(14) 0.0456(18) 0.0264(14) 0.0168(13) 0.0084(11) 0.0123(13) C16 0.0231(13) 0.0404(17) 0.0232(13) 0.0165(13) 0.0059(11) 0.0112(12) C17 0.0241(13) 0.0385(16) 0.0242(13) 0.0159(13) 0.0045(11) 0.0104(12) C18 0.0224(13) 0.0396(17) 0.0227(13) 0.0162(12) 0.0050(11) 0.0094(12) C19 0.0252(14) 0.0433(18) 0.0251(14) 0.0145(13) 0.0072(11) 0.0103(13) C20 0.0239(14) 0.0352(16) 0.0302(15) 0.0145(13) 0.0058(11) 0.0091(12) C21 0.0232(13) 0.0455(18) 0.0257(14) 0.0187(13) 0.0051(11) 0.0099(12) C22 0.0357(16) 0.0439(18) 0.0349(16) 0.0220(15) 0.0114(13) 0.0082(14) C23 0.0337(16) 0.0416(18) 0.0298(15) 0.0194(14) 0.0098(12) 0.0143(13) C24 0.0384(17) 0.0460(19) 0.0311(16) 0.0113(15) 0.0115(14) 0.0070(15) C25 0.0315(15) 0.0469(19) 0.0295(15) 0.0204(14) 0.0079(12) 0.0113(14) C26 0.112(5) 0.071(3) 0.105(4) 0.036(3) 0.004(4) 0.047(3) C27 0.069(3) 0.112(4) 0.138(5) 0.087(4) 0.030(3) 0.045(3) C28 0.092(4) 0.132(5) 0.113(5) 0.089(4) 0.045(4) 0.069(4) C29 0.204(9) 0.126(6) 0.171(8) 0.057(6) -0.001(7) 0.120(6) C30 0.0296(15) 0.0430(17) 0.0228(13) 0.0161(13) 0.0060(11) 0.0081(13) C31 0.0269(14) 0.0418(17) 0.0204(13) 0.0154(12) 0.0083(11) 0.0108(12) C32 0.0289(14) 0.0462(18) 0.0250(14) 0.0218(13) 0.0092(12) 0.0137(13) C33 0.0310(15) 0.0440(18) 0.0301(15) 0.0218(14) 0.0104(12) 0.0094(13) C34 0.0269(14) 0.0455(18) 0.0264(14) 0.0182(14) 0.0081(12) 0.0081(13) C35 0.0256(14) 0.0438(17) 0.0266(14) 0.0196(13) 0.0092(11) 0.0119(13) C36 0.0302(14) 0.0434(17) 0.0224(13) 0.0198(13) 0.0124(11) 0.0142(13) C37 0.0338(16) 0.0444(18) 0.0317(15) 0.0207(14) 0.0099(13) 0.0146(14) C38 0.0335(16) 0.0464(19) 0.0372(17) 0.0253(15) 0.0043(13) 0.0117(14) C39 0.0356(17) 0.059(2) 0.0359(17) 0.0325(17) 0.0073(14) 0.0091(15) C40 0.050(2) 0.061(2) 0.043(2) 0.0174(19) 0.0054(17) 0.0155(19) C41 0.063(3) 0.051(2) 0.077(3) 0.034(2) -0.006(2) 0.001(2) C42 0.089(4) 0.059(3) 0.072(3) 0.015(3) -0.009(3) 0.019(3) C43 0.100(5) 0.191(7) 0.053(3) 0.006(4) 0.013(3) 0.073(5) C44 0.0304(16) 0.049(2) 0.0416(18) 0.0243(16) 0.0071(14) 0.0073(14) C45 0.0240(14) 0.0497(19) 0.0348(16) 0.0271(15) 0.0108(12) 0.0136(13) C46 0.0204(13) 0.0495(18) 0.0273(14) 0.0228(14) 0.0059(11) 0.0098(13) C47 0.0204(13) 0.0479(18) 0.0272(14) 0.0195(14) 0.0062(11) 0.0113(12) C48 0.0259(14) 0.0472(18) 0.0330(15) 0.0228(14) 0.0099(12) 0.0133(13) C49 0.0267(14) 0.0507(19) 0.0309(15) 0.0253(15) 0.0116(12) 0.0154(13) C50 0.0238(14) 0.0436(17) 0.0254(14) 0.0177(13) 0.0048(11) 0.0101(12) C51 0.0216(13) 0.0443(17) 0.0260(14) 0.0179(13) 0.0038(11) 0.0087(12) C52 0.0360(16) 0.0432(18) 0.0360(16) 0.0207(15) 0.0116(14) 0.0118(14) C53 0.0332(16) 0.0490(19) 0.0308(15) 0.0220(15) 0.0117(13) 0.0174(14) C54 0.0335(16) 0.053(2) 0.0418(18) 0.0296(16) 0.0163(14) 0.0159(15) C55 0.0460(19) 0.048(2) 0.0340(16) 0.0249(16) 0.0144(14) 0.0225(16) C56 0.0434(18) 0.048(2) 0.0295(15) 0.0194(15) 0.0104(13) 0.0200(15) C57 0.0420(18) 0.0466(19) 0.0339(16) 0.0262(15) 0.0196(14) 0.0206(15) C58 0.055(2) 0.068(2) 0.044(2) 0.0307(19) 0.0157(17) 0.039(2) C59 0.050(2) 0.072(2) 0.0465(19) 0.0428(19) 0.0267(17) 0.0343(19) C60 0.0309(15) 0.0464(18) 0.0261(14) 0.0190(14) 0.0077(12) 0.0133(13) C2S 0.090(6) 0.102(7) 0.074(5) 0.030(5) 0.044(5) 0.055(5) C3S 0.070(6) 0.129(8) 0.102(7) 0.040(7) 0.014(5) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N9 1.160(5) . ? O2 N9 1.270(5) . ? O3 N9 1.249(5) . ? O4 N10 1.239(4) . ? O5 N10 1.245(4) . ? O6 N10 1.240(4) . ? O7 N11 1.247(5) . ? O8 N11 1.216(4) . ? O9 N11 1.205(5) . ? O10 N12 0.977(13) . ? O11 N12 1.23(3) . ? O12 N12 1.35(2) . ? O10' N12 1.412(12) . ? O11' N12 1.187(11) . ? O12' N12 1.191(8) . ? N1 C11 1.332(4) . ? N1 C13 1.371(4) . ? N1 C14 1.465(5) . ? N2 C11 1.330(4) . ? N2 C12 1.382(4) . ? N2 C10 1.483(4) . ? N3 C40 1.314(5) . ? N3 C42 1.401(7) . ? N3 C43 1.461(7) . ? N4 C40 1.333(5) . ? N4 C41 1.376(5) . ? N4 C39 1.460(4) . ? N5 C57 1.327(4) . ? N5 C56 1.378(4) . ? N5 C58 1.473(4) . ? N6 C57 1.344(4) . ? N6 C55 1.376(4) . ? N6 C54 1.480(4) . ? N7 C28 1.321(8) . ? N7 C26 1.342(7) . ? N7 C29 1.472(7) . ? N8 C26 1.308(6) . ? N8 C27 1.331(6) . ? N8 C25 1.457(4) . ? N1S C2S 1.155(11) . ? C1 C2 1.402(4) . ? C1 C6 1.412(4) . ? C1 C10 1.523(4) . ? C2 C3 1.401(4) . ? C2 C8 1.515(4) . ? C3 C4 1.405(4) . ? C3 C15 1.528(4) . ? C4 C5 1.406(4) . ? C4 C9 1.502(4) . ? C5 C6 1.394(4) . ? C5 C60 1.521(4) . ? C6 C7 1.523(5) . ? C12 C13 1.353(5) . ? C15 C16 1.531(4) . ? C16 C21 1.390(4) . ? C16 C17 1.414(4) . ? C17 C18 1.400(4) . ? C17 C23 1.506(4) . ? C18 C19 1.401(4) . ? C18 C30 1.534(4) . ? C19 C20 1.400(4) . ? C19 C24 1.515(4) . ? C20 C21 1.412(4) . ? C20 C25 1.586(4) . ? C21 C22 1.518(4) . ? C27 C28 1.342(6) . ? C30 C31 1.523(4) . ? C31 C32 1.405(4) . ? C31 C36 1.408(4) . ? C32 C33 1.411(4) . ? C32 C38 1.513(4) . ? C33 C34 1.412(4) . ? C33 C39 1.527(4) . ? C34 C35 1.394(4) . ? C34 C44 1.521(4) . ? C35 C36 1.406(4) . ? C35 C45 1.532(4) . ? C36 C37 1.509(4) . ? C41 C42 1.337(7) . ? C45 C46 1.529(4) . ? C46 C47 1.397(4) . ? C46 C51 1.413(4) . ? C47 C48 1.413(4) . ? C47 C53 1.511(4) . ? C48 C49 1.405(4) . ? C48 C54 1.505(4) . ? C49 C50 1.399(4) . ? C49 C59 1.512(4) . ? C50 C51 1.402(4) . ? C50 C60 1.524(4) . ? C51 C52 1.504(4) . ? C55 C56 1.350(4) . ? C2S C3S 1.394(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 N1 C13 108.4(3) . . ? C11 N1 C14 125.8(3) . . ? C13 N1 C14 125.8(3) . . ? C11 N2 C12 108.3(3) . . ? C11 N2 C10 126.6(3) . . ? C12 N2 C10 125.1(3) . . ? C40 N3 C42 108.6(4) . . ? C40 N3 C43 125.2(5) . . ? C42 N3 C43 126.2(5) . . ? C40 N4 C41 108.1(4) . . ? C40 N4 C39 126.5(3) . . ? C41 N4 C39 125.4(3) . . ? C57 N5 C56 109.5(3) . . ? C57 N5 C58 124.9(3) . . ? C56 N5 C58 125.6(3) . . ? C57 N6 C55 108.7(3) . . ? C57 N6 C54 123.7(3) . . ? C55 N6 C54 127.4(3) . . ? C28 N7 C26 108.7(5) . . ? C28 N7 C29 126.8(6) . . ? C26 N7 C29 124.5(7) . . ? C26 N8 C27 106.5(4) . . ? C26 N8 C25 122.5(4) . . ? C27 N8 C25 130.6(4) . . ? O1 N9 O3 119.2(5) . . ? O1 N9 O2 121.2(4) . . ? O3 N9 O2 119.5(4) . . ? O4 N10 O6 119.9(3) . . ? O4 N10 O5 121.8(4) . . ? O6 N10 O5 118.2(3) . . ? O9 N11 O8 120.5(4) . . ? O9 N11 O7 120.6(4) . . ? O8 N11 O7 118.8(4) . . ? O10 N12 O11' 75.9(14) . . ? O10 N12 O12' 157.5(15) . . ? O11' N12 O12' 125.0(12) . . ? O10 N12 O11 127.7(19) . . ? O11' N12 O11 54.8(16) . . ? O12' N12 O11 70.7(16) . . ? O10 N12 O12 132.1(18) . . ? O11' N12 O12 140.6(14) . . ? O12' N12 O12 37.5(12) . . ? O11 N12 O12 99.3(15) . . ? O10 N12 O10' 46.9(11) . . ? O11' N12 O10' 122.8(13) . . ? O12' N12 O10' 111.7(9) . . ? O11 N12 O10' 164.5(10) . . ? O12 N12 O10' 90.0(11) . . ? C2 C1 C6 120.7(3) . . ? C2 C1 C10 119.8(3) . . ? C6 C1 C10 119.5(3) . . ? C3 C2 C1 119.1(3) . . ? C3 C2 C8 120.7(3) . . ? C1 C2 C8 120.1(3) . . ? C2 C3 C4 120.2(3) . . ? C2 C3 C15 118.8(2) . . ? C4 C3 C15 120.9(3) . . ? C3 C4 C5 120.1(3) . . ? C3 C4 C9 119.9(3) . . ? C5 C4 C9 119.9(2) . . ? C6 C5 C4 119.9(3) . . ? C6 C5 C60 119.5(3) . . ? C4 C5 C60 120.5(3) . . ? C5 C6 C1 119.7(3) . . ? C5 C6 C7 120.4(3) . . ? C1 C6 C7 119.8(3) . . ? N2 C10 C1 111.1(3) . . ? N2 C11 N1 108.9(3) . . ? C13 C12 N2 106.8(3) . . ? C12 C13 N1 107.5(3) . . ? C3 C15 C16 119.0(2) . . ? C21 C16 C17 119.9(3) . . ? C21 C16 C15 121.3(2) . . ? C17 C16 C15 118.6(3) . . ? C18 C17 C16 120.1(3) . . ? C18 C17 C23 119.7(2) . . ? C16 C17 C23 120.2(2) . . ? C17 C18 C19 120.3(3) . . ? C17 C18 C30 119.9(3) . . ? C19 C18 C30 119.8(2) . . ? C20 C19 C18 119.0(3) . . ? C20 C19 C24 120.6(3) . . ? C18 C19 C24 120.3(3) . . ? C19 C20 C21 121.0(3) . . ? C19 C20 C25 119.6(3) . . ? C21 C20 C25 119.3(3) . . ? C16 C21 C20 119.4(3) . . ? C16 C21 C22 123.3(3) . . ? C20 C21 C22 117.3(3) . . ? N8 C25 C20 109.5(3) . . ? N8 C26 N7 109.0(6) . . ? N8 C27 C28 110.1(5) . . ? N7 C28 C27 105.7(5) . . ? C31 C30 C18 117.7(2) . . ? C32 C31 C36 119.3(3) . . ? C32 C31 C30 120.6(2) . . ? C36 C31 C30 120.0(3) . . ? C31 C32 C33 119.1(3) . . ? C31 C32 C38 121.7(3) . . ? C33 C32 C38 119.1(3) . . ? C34 C33 C32 121.0(3) . . ? C34 C33 C39 118.5(3) . . ? C32 C33 C39 120.4(3) . . ? C35 C34 C33 119.5(3) . . ? C35 C34 C44 122.5(3) . . ? C33 C34 C44 118.1(3) . . ? C34 C35 C36 119.5(3) . . ? C34 C35 C45 120.7(3) . . ? C36 C35 C45 119.7(3) . . ? C35 C36 C31 121.1(3) . . ? C35 C36 C37 118.8(3) . . ? C31 C36 C37 120.0(3) . . ? N4 C39 C33 110.9(2) . . ? N3 C40 N4 109.0(4) . . ? C42 C41 N4 108.1(4) . . ? C41 C42 N3 106.2(4) . . ? C46 C45 C35 119.1(2) . . ? C47 C46 C51 120.0(3) . . ? C47 C46 C45 120.2(3) . . ? C51 C46 C45 119.6(3) . . ? C46 C47 C48 118.9(3) . . ? C46 C47 C53 122.4(3) . . ? C48 C47 C53 118.7(3) . . ? C49 C48 C47 121.4(3) . . ? C49 C48 C54 119.7(3) . . ? C47 C48 C54 118.9(3) . . ? C50 C49 C48 119.0(3) . . ? C50 C49 C59 120.7(3) . . ? C48 C49 C59 120.3(3) . . ? C49 C50 C51 120.1(3) . . ? C49 C50 C60 119.6(2) . . ? C51 C50 C60 120.2(3) . . ? C50 C51 C46 120.3(3) . . ? C50 C51 C52 119.5(3) . . ? C46 C51 C52 120.2(3) . . ? N6 C54 C48 111.0(3) . . ? C56 C55 N6 107.3(3) . . ? C55 C56 N5 106.8(3) . . ? N5 C57 N6 107.7(3) . . ? C5 C60 C50 117.5(2) . . ? N1S C2S C3S 178.1(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.825 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.071