# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sean Bew' _publ_contact_author_email a.d.burrows@bath.ac.uk loop_ _publ_author_name A.Burrows S.Bew T.Duren M.Mahon P.Moghadam V.Sebestyenb S.Thurston data_k09adb11 _database_code_depnum_ccdc_archive 'CCDC 866579' #TrackingRef '- calix-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H53 Cu1 N1 O9' _chemical_formula_weight 815.43 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4670(2) _cell_length_b 26.3310(5) _cell_length_c 17.6480(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.7890(10) _cell_angle_gamma 90.00 _cell_volume 4290.08(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 83799 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47644 _diffrn_reflns_av_R_equivalents 0.1632 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 24.93 _reflns_number_total 7394 _reflns_number_gt 4673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; 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. The asymmetric unit consists of one copper centre, one DMF, and one calixarene diananion. Carbons 6-8 of the n-propoxy functionality are modeled as being disordered over two sites. This approach yielded that optimal convergence, but the disorder is somewhat smeared. Hence, C-C distance restraints and ADP restraints were applied to these partial carbon atoms ; _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^)+(0.0921P)^2^+7.8357P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7394 _refine_ls_number_parameters 537 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1955 _refine_ls_wR_factor_gt 0.1644 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _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 Cu1 Cu 1.07955(6) -0.498002(19) 0.44787(3) 0.0251(2) Uani 1 1 d . . . O1 O 0.9087(4) -0.47188(12) 0.37349(19) 0.0332(8) Uani 1 1 d . . . O2 O 0.7724(4) -0.47657(12) 0.46258(19) 0.0339(8) Uani 1 1 d . . . O3 O 1.2195(4) -0.51239(13) 0.3673(2) 0.0373(9) Uani 1 1 d . . . O4 O 0.2974(4) -0.40069(14) 0.1754(2) 0.0443(10) Uani 1 1 d D . . O5 O 0.0280(4) -0.33891(12) 0.26254(19) 0.0313(8) Uani 1 1 d . . . O6 O 0.1097(4) -0.30001(11) 0.0920(2) 0.0351(9) Uani 1 1 d . . . O7 O 0.3218(4) -0.37189(12) 0.00116(19) 0.0354(9) Uani 1 1 d . . . O8 O 0.1348(4) -0.07173(11) -0.01724(19) 0.0297(8) Uani 1 1 d . . . O9 O 0.0002(4) -0.06643(12) 0.0726(2) 0.0352(8) Uani 1 1 d . . . N1 N 1.4041(6) -0.5626(2) 0.3482(3) 0.0551(14) Uani 1 1 d . . . C1 C 0.7905(6) -0.46711(16) 0.3948(3) 0.0285(11) Uani 1 1 d . . . C2 C 0.6613(6) -0.44882(16) 0.3358(3) 0.0288(11) Uani 1 1 d . . . C3 C 0.6645(6) -0.44392(17) 0.2577(3) 0.0333(12) Uani 1 1 d . A . H3 H 0.7507 -0.4521 0.2412 0.040 Uiso 1 1 calc R . . C4 C 0.5436(6) -0.42731(18) 0.2034(3) 0.0339(12) Uani 1 1 d . . . C5 C 0.4170(6) -0.41668(18) 0.2288(3) 0.0345(12) Uani 1 1 d . A . C6 C 0.2049(15) -0.4398(5) 0.1288(7) 0.066(4) Uani 0.50 1 d PDU A 1 H6A H 0.2642 -0.4696 0.1212 0.079 Uiso 0.50 1 calc PR A 1 H6B H 0.1587 -0.4260 0.0771 0.079 Uiso 0.50 1 calc PR A 1 C7 C 0.0895(18) -0.4556(7) 0.1721(9) 0.096(6) Uani 0.50 1 d PDU A 1 H7A H 0.1311 -0.4773 0.2173 0.116 Uiso 0.50 1 calc PR A 1 H7B H 0.0435 -0.4255 0.1902 0.116 Uiso 0.50 1 calc PR A 1 C8 C -0.019(3) -0.4850(9) 0.1115(13) 0.125(8) Uani 0.50 1 d PDU A 1 H8A H -0.0997 -0.4959 0.1338 0.188 Uiso 0.50 1 calc PR A 1 H8B H 0.0290 -0.5148 0.0952 0.188 Uiso 0.50 1 calc PR A 1 H8C H -0.0549 -0.4632 0.0664 0.188 Uiso 0.50 1 calc PR A 1 C9 C 0.4142(6) -0.41681(18) 0.3080(3) 0.0316(12) Uani 1 1 d . . . C10 C 0.5372(6) -0.43404(17) 0.3602(3) 0.0316(12) Uani 1 1 d . A . H10 H 0.5366 -0.4357 0.4139 0.038 Uiso 1 1 calc R . . C11 C 0.2895(6) -0.39296(18) 0.3359(3) 0.0361(13) Uani 1 1 d . A . H11A H 0.3024 -0.3985 0.3925 0.043 Uiso 1 1 calc R . . H11B H 0.1974 -0.4091 0.3094 0.043 Uiso 1 1 calc R . . C12 C 0.2832(6) -0.33620(18) 0.3188(3) 0.0303(11) Uani 1 1 d . . . C13 C 0.4111(6) -0.3079(2) 0.3357(3) 0.0399(13) Uani 1 1 d . A . H13 H 0.4984 -0.3237 0.3621 0.048 Uiso 1 1 calc R . . C14 C 0.4129(6) -0.2572(2) 0.3145(3) 0.0396(13) Uani 1 1 d . . . H14 H 0.5001 -0.2382 0.3275 0.048 Uiso 1 1 calc R A . C15 C 0.2869(6) -0.23476(19) 0.2744(3) 0.0335(12) Uani 1 1 d . A . H15 H 0.2885 -0.2003 0.2585 0.040 Uiso 1 1 calc R . . C16 C 0.1572(6) -0.26174(17) 0.2568(3) 0.0295(11) Uani 1 1 d . . . C17 C 0.1566(5) -0.31184(18) 0.2816(3) 0.0284(11) Uani 1 1 d . A . C18 C -0.0426(6) -0.34618(18) 0.3272(3) 0.0353(12) Uani 1 1 d . . . H18A H 0.0299 -0.3587 0.3727 0.042 Uiso 1 1 calc R . . H18B H -0.1182 -0.3726 0.3130 0.042 Uiso 1 1 calc R . . C19 C -0.1108(6) -0.2987(2) 0.3499(3) 0.0372(13) Uani 1 1 d . . . H19A H -0.1803 -0.2850 0.3041 0.045 Uiso 1 1 calc R . . H19B H -0.0350 -0.2727 0.3675 0.045 Uiso 1 1 calc R . . C20 C -0.1900(7) -0.3093(2) 0.4150(3) 0.0491(15) Uani 1 1 d . . . H20A H -0.2554 -0.3382 0.4005 0.074 Uiso 1 1 calc R . . H20B H -0.2460 -0.2793 0.4231 0.074 Uiso 1 1 calc R . . H20C H -0.1191 -0.3171 0.4631 0.074 Uiso 1 1 calc R . . C21 C 0.0238(6) -0.23767(18) 0.2063(3) 0.0333(12) Uani 1 1 d . A . H21A H -0.0538 -0.2634 0.1924 0.040 Uiso 1 1 calc R . . H21B H -0.0118 -0.2102 0.2355 0.040 Uiso 1 1 calc R . . C22 C 0.0583(6) -0.21631(18) 0.1334(3) 0.0302(11) Uani 1 1 d . . . C23 C 0.0547(6) -0.16466(17) 0.1188(3) 0.0295(11) Uani 1 1 d . A . H23 H 0.0140 -0.1425 0.1506 0.035 Uiso 1 1 calc R . . C24 C 0.1102(6) -0.14443(17) 0.0576(3) 0.0293(11) Uani 1 1 d . . . C25 C 0.0810(5) -0.08991(17) 0.0363(3) 0.0269(11) Uani 1 1 d . A . C26 C 0.1802(5) -0.17649(17) 0.0152(3) 0.0279(11) Uani 1 1 d . A . H26 H 0.2262 -0.1624 -0.0227 0.033 Uiso 1 1 calc R . . C27 C 0.1841(6) -0.22870(17) 0.0271(3) 0.0295(11) Uani 1 1 d . . . C28 C 0.1146(5) -0.24802(17) 0.0832(3) 0.0299(11) Uani 1 1 d . A . C29 C -0.0353(7) -0.3212(2) 0.0674(3) 0.0448(14) Uani 1 1 d . . . H29A H -0.1070 -0.2957 0.0761 0.054 Uiso 1 1 calc R . . H29B H -0.0441 -0.3513 0.0996 0.054 Uiso 1 1 calc R . . C30 C -0.0692(8) -0.3362(3) -0.0164(4) 0.0599(18) Uani 1 1 d . . . H30A H 0.0033 -0.3612 -0.0255 0.072 Uiso 1 1 calc R . . H30B H -0.0632 -0.3059 -0.0489 0.072 Uiso 1 1 calc R . . C31 C -0.2194(9) -0.3591(4) -0.0398(5) 0.087(3) Uani 1 1 d . . . H31A H -0.2237 -0.3901 -0.0096 0.131 Uiso 1 1 calc R . . H31B H -0.2405 -0.3674 -0.0953 0.131 Uiso 1 1 calc R . . H31C H -0.2910 -0.3347 -0.0296 0.131 Uiso 1 1 calc R . . C32 C 0.2638(6) -0.26434(18) -0.0161(3) 0.0333(12) Uani 1 1 d . A . H32A H 0.2934 -0.2457 -0.0587 0.040 Uiso 1 1 calc R . . H32B H 0.1982 -0.2922 -0.0393 0.040 Uiso 1 1 calc R . . C33 C 0.3972(6) -0.28656(18) 0.0381(3) 0.0309(12) Uani 1 1 d . . . C34 C 0.4975(6) -0.25448(19) 0.0834(3) 0.0379(13) Uani 1 1 d . A . H34 H 0.4863 -0.2188 0.0771 0.046 Uiso 1 1 calc R . . C35 C 0.6138(7) -0.2737(2) 0.1378(3) 0.0426(14) Uani 1 1 d . . . H35 H 0.6821 -0.2511 0.1680 0.051 Uiso 1 1 calc R A . C36 C 0.6307(6) -0.3254(2) 0.1481(3) 0.0393(13) Uani 1 1 d . A . H36 H 0.7095 -0.3382 0.1863 0.047 Uiso 1 1 calc R . . C37 C 0.5335(6) -0.35898(19) 0.1032(3) 0.0326(12) Uani 1 1 d . . . C38 C 0.4187(6) -0.33862(17) 0.0473(3) 0.0290(11) Uani 1 1 d . A . C39 C 0.3558(8) -0.3808(2) -0.0729(3) 0.0490(16) Uani 1 1 d . . . H39A H 0.4449 -0.4015 -0.0662 0.059 Uiso 1 1 calc R . . H39B H 0.3732 -0.3480 -0.0968 0.059 Uiso 1 1 calc R . . C40 C 0.2344(11) -0.4075(3) -0.1237(4) 0.089(3) Uani 1 1 d . . . H40A H 0.1482 -0.3852 -0.1333 0.107 Uiso 1 1 calc R . . H40B H 0.2111 -0.4382 -0.0964 0.107 Uiso 1 1 calc R . . C41 C 0.2648(12) -0.4233(3) -0.2010(4) 0.095(3) Uani 1 1 d . . . H41A H 0.2729 -0.3929 -0.2319 0.143 Uiso 1 1 calc R . . H41B H 0.1855 -0.4446 -0.2289 0.143 Uiso 1 1 calc R . . H41C H 0.3558 -0.4424 -0.1922 0.143 Uiso 1 1 calc R . . C42 C 0.5506(6) -0.41575(19) 0.1198(3) 0.0378(13) Uani 1 1 d . A . H42A H 0.4727 -0.4345 0.0840 0.045 Uiso 1 1 calc R . . H42B H 0.6447 -0.4274 0.1105 0.045 Uiso 1 1 calc R . . C43 C 1.3340(7) -0.5345(2) 0.3904(3) 0.0432(14) Uani 1 1 d . . . H43 H 1.3775 -0.5313 0.4441 0.052 Uiso 1 1 calc R . . C44 C 1.3526(12) -0.5626(5) 0.2642(5) 0.127(5) Uani 1 1 d . . . H44A H 1.2580 -0.5457 0.2505 0.190 Uiso 1 1 calc R . . H44B H 1.3433 -0.5976 0.2451 0.190 Uiso 1 1 calc R . . H44C H 1.4218 -0.5443 0.2403 0.190 Uiso 1 1 calc R . . C45 C 1.5455(8) -0.5841(3) 0.3804(5) 0.071(2) Uani 1 1 d . . . H45A H 1.5753 -0.5751 0.4355 0.106 Uiso 1 1 calc R . . H45B H 1.6159 -0.5705 0.3525 0.106 Uiso 1 1 calc R . . H45C H 1.5410 -0.6211 0.3751 0.106 Uiso 1 1 calc R . . C6A C 0.1659(10) -0.4326(5) 0.1667(9) 0.060(4) Uani 0.50 1 d PDU A 2 H6A1 H 0.0773 -0.4114 0.1543 0.072 Uiso 0.50 1 calc PR A 2 H6A2 H 0.1667 -0.4519 0.2150 0.072 Uiso 0.50 1 calc PR A 2 C7A C 0.172(4) -0.4685(10) 0.1000(14) 0.170(12) Uani 0.50 1 d PDU A 2 H7A1 H 0.1539 -0.4496 0.0502 0.204 Uiso 0.50 1 calc PR A 2 H7A2 H 0.2685 -0.4847 0.1082 0.204 Uiso 0.50 1 calc PR A 2 C8A C 0.055(4) -0.5083(16) 0.098(3) 0.25(2) Uani 0.50 1 d PDU A 2 H8A1 H 0.0752 -0.5379 0.0688 0.374 Uiso 0.50 1 calc PR A 2 H8A2 H -0.0393 -0.4940 0.0739 0.374 Uiso 0.50 1 calc PR A 2 H8A3 H 0.0548 -0.5186 0.1518 0.374 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0290(3) 0.0208(3) 0.0258(3) 0.0022(2) 0.0066(2) 0.0032(2) O1 0.035(2) 0.0335(19) 0.0308(19) 0.0068(14) 0.0063(17) 0.0042(15) O2 0.038(2) 0.0347(19) 0.029(2) 0.0062(15) 0.0078(16) 0.0100(15) O3 0.033(2) 0.042(2) 0.039(2) 0.0046(16) 0.0134(17) 0.0102(17) O4 0.032(2) 0.060(2) 0.039(2) 0.0155(18) 0.0050(18) 0.0103(18) O5 0.029(2) 0.0313(18) 0.0325(19) 0.0052(14) 0.0053(15) -0.0016(14) O6 0.043(2) 0.0237(17) 0.039(2) 0.0045(14) 0.0100(17) 0.0023(15) O7 0.041(2) 0.0330(19) 0.0298(19) 0.0008(14) 0.0040(17) 0.0051(16) O8 0.033(2) 0.0249(17) 0.0332(19) -0.0012(14) 0.0107(16) -0.0002(14) O9 0.046(2) 0.0254(17) 0.037(2) 0.0007(15) 0.0161(18) 0.0020(16) N1 0.047(3) 0.060(3) 0.056(3) -0.012(3) 0.006(3) 0.018(3) C1 0.031(3) 0.020(2) 0.035(3) 0.001(2) 0.009(2) 0.003(2) C2 0.034(3) 0.021(2) 0.029(3) 0.0042(19) 0.002(2) 0.002(2) C3 0.038(3) 0.022(2) 0.040(3) 0.001(2) 0.009(3) 0.007(2) C4 0.044(4) 0.027(3) 0.029(3) 0.004(2) 0.005(2) 0.004(2) C5 0.030(3) 0.033(3) 0.038(3) 0.010(2) 0.003(3) 0.007(2) C6 0.063(6) 0.074(6) 0.062(5) 0.010(4) 0.016(4) -0.004(4) C7 0.102(7) 0.098(7) 0.090(7) 0.005(5) 0.023(5) -0.007(5) C8 0.120(9) 0.124(9) 0.131(9) 0.002(5) 0.027(5) -0.008(5) C9 0.030(3) 0.030(3) 0.035(3) 0.006(2) 0.007(2) 0.004(2) C10 0.036(3) 0.029(3) 0.029(3) 0.010(2) 0.007(2) 0.004(2) C11 0.036(3) 0.036(3) 0.037(3) 0.013(2) 0.009(3) 0.006(2) C12 0.031(3) 0.033(3) 0.031(3) 0.003(2) 0.015(2) 0.003(2) C13 0.033(3) 0.049(3) 0.037(3) 0.006(2) 0.006(3) 0.007(2) C14 0.034(3) 0.047(3) 0.040(3) -0.001(3) 0.012(3) -0.009(3) C15 0.039(3) 0.032(3) 0.032(3) 0.003(2) 0.014(2) -0.002(2) C16 0.034(3) 0.029(3) 0.026(3) 0.001(2) 0.009(2) 0.001(2) C17 0.027(3) 0.032(3) 0.026(3) 0.003(2) 0.008(2) -0.001(2) C18 0.037(3) 0.034(3) 0.033(3) 0.010(2) 0.004(2) -0.002(2) C19 0.032(3) 0.042(3) 0.036(3) 0.004(2) 0.006(2) 0.007(2) C20 0.031(3) 0.069(4) 0.048(3) 0.008(3) 0.010(3) 0.003(3) C21 0.036(3) 0.027(3) 0.039(3) 0.005(2) 0.014(2) 0.009(2) C22 0.031(3) 0.031(3) 0.030(3) 0.004(2) 0.008(2) 0.004(2) C23 0.035(3) 0.024(2) 0.030(3) 0.001(2) 0.008(2) 0.005(2) C24 0.030(3) 0.026(2) 0.029(3) 0.000(2) 0.002(2) 0.000(2) C25 0.027(3) 0.024(2) 0.028(3) 0.000(2) 0.004(2) -0.005(2) C26 0.027(3) 0.027(3) 0.028(3) 0.004(2) 0.003(2) -0.002(2) C27 0.032(3) 0.026(3) 0.029(3) 0.000(2) 0.005(2) 0.003(2) C28 0.027(3) 0.027(3) 0.033(3) 0.009(2) 0.000(2) 0.005(2) C29 0.057(4) 0.032(3) 0.050(3) 0.000(2) 0.023(3) -0.004(3) C30 0.061(5) 0.071(4) 0.051(4) -0.013(3) 0.017(3) -0.013(3) C31 0.072(6) 0.123(7) 0.066(5) -0.032(5) 0.014(4) -0.042(5) C32 0.043(3) 0.028(3) 0.030(3) 0.001(2) 0.011(2) 0.006(2) C33 0.036(3) 0.033(3) 0.026(3) 0.003(2) 0.013(2) 0.005(2) C34 0.036(3) 0.033(3) 0.045(3) 0.002(2) 0.010(3) 0.002(2) C35 0.039(4) 0.042(3) 0.045(3) -0.003(3) 0.004(3) -0.006(3) C36 0.030(3) 0.052(3) 0.033(3) 0.007(2) 0.001(2) 0.003(3) C37 0.031(3) 0.038(3) 0.029(3) 0.004(2) 0.010(2) 0.009(2) C38 0.029(3) 0.031(3) 0.028(3) -0.002(2) 0.007(2) 0.000(2) C39 0.073(5) 0.040(3) 0.036(3) -0.004(2) 0.016(3) 0.006(3) C40 0.111(8) 0.097(6) 0.059(5) -0.028(4) 0.018(5) -0.026(5) C41 0.155(10) 0.071(5) 0.060(5) -0.021(4) 0.027(5) -0.001(5) C42 0.043(4) 0.038(3) 0.029(3) 0.004(2) 0.003(2) 0.011(2) C43 0.046(4) 0.050(3) 0.036(3) -0.003(3) 0.013(3) 0.000(3) C44 0.098(8) 0.188(11) 0.083(6) -0.048(7) -0.003(6) 0.076(8) C45 0.041(4) 0.081(5) 0.088(5) -0.002(4) 0.008(4) 0.020(4) C6A 0.063(5) 0.057(5) 0.056(5) -0.009(4) 0.003(4) 0.008(4) C7A 0.172(13) 0.170(12) 0.169(12) -0.002(5) 0.038(6) -0.004(5) C8A 0.25(2) 0.25(2) 0.25(2) 0.001(5) 0.055(7) -0.002(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 Cu1 O9 1.956(3) 2_645 ? Cu1 O1 1.968(3) . ? Cu1 O8 1.970(3) 4_656 ? Cu1 O2 1.982(3) 3_746 ? Cu1 O3 2.181(4) . ? Cu1 Cu1 2.6254(11) 3_746 ? O1 C1 1.264(6) . ? O2 C1 1.270(6) . ? O2 Cu1 1.982(3) 3_746 ? O3 C43 1.219(7) . ? O4 C5 1.370(6) . ? O4 C6 1.479(5) . ? O4 C6A 1.481(5) . ? O5 C17 1.387(6) . ? O5 C18 1.457(6) . ? O6 C28 1.380(5) . ? O6 C29 1.456(7) . ? O7 C38 1.393(6) . ? O7 C39 1.433(7) . ? O8 C25 1.262(6) . ? O8 Cu1 1.970(3) 4_455 ? O9 C25 1.263(6) . ? O9 Cu1 1.956(3) 2_655 ? N1 C43 1.326(8) . ? N1 C45 1.449(8) . ? N1 C44 1.455(10) . ? C1 C2 1.499(7) . ? C2 C3 1.392(7) . ? C2 C10 1.393(7) . ? C3 C4 1.391(7) . ? C3 H3 0.9500 . ? C4 C5 1.398(8) . ? C4 C42 1.522(7) . ? C5 C9 1.403(7) . ? C6 C7 1.523(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.392(7) . ? C9 C11 1.512(7) . ? C10 H10 0.9500 . ? C11 C12 1.523(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.390(7) . ? C12 C13 1.396(8) . ? C13 C14 1.389(8) . ? C13 H13 0.9500 . ? C14 C15 1.378(8) . ? C14 H14 0.9500 . ? C15 C16 1.392(7) . ? C15 H15 0.9500 . ? C16 C17 1.390(7) . ? C16 C21 1.515(7) . ? C18 C19 1.502(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.529(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.504(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.383(6) . ? C22 C28 1.406(7) . ? C23 C24 1.406(7) . ? C23 H23 0.9500 . ? C24 C26 1.390(7) . ? C24 C25 1.495(6) . ? C26 C27 1.390(6) . ? C26 H26 0.9500 . ? C27 C28 1.400(7) . ? C27 C32 1.512(7) . ? C29 C30 1.495(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.516(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.522(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.385(7) . ? C33 C38 1.390(7) . ? C34 C35 1.386(8) . ? C34 H34 0.9500 . ? C35 C36 1.380(8) . ? C35 H35 0.9500 . ? C36 C37 1.391(7) . ? C36 H36 0.9500 . ? C37 C38 1.403(7) . ? C37 C42 1.525(7) . ? C39 C40 1.471(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.513(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C6A C7A 1.520(5) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.518(5) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? 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 O9 Cu1 O1 88.42(15) 2_645 . ? O9 Cu1 O8 168.84(14) 2_645 4_656 ? O1 Cu1 O8 90.28(14) . 4_656 ? O9 Cu1 O2 90.67(15) 2_645 3_746 ? O1 Cu1 O2 168.98(15) . 3_746 ? O8 Cu1 O2 88.49(14) 4_656 3_746 ? O9 Cu1 O3 89.13(14) 2_645 . ? O1 Cu1 O3 98.84(14) . . ? O8 Cu1 O3 102.02(14) 4_656 . ? O2 Cu1 O3 92.12(14) 3_746 . ? O9 Cu1 Cu1 80.48(10) 2_645 3_746 ? O1 Cu1 Cu1 88.13(11) . 3_746 ? O8 Cu1 Cu1 88.40(10) 4_656 3_746 ? O2 Cu1 Cu1 80.90(10) 3_746 3_746 ? O3 Cu1 Cu1 167.36(10) . 3_746 ? C1 O1 Cu1 119.2(3) . . ? C1 O2 Cu1 126.7(3) . 3_746 ? C43 O3 Cu1 119.3(3) . . ? C5 O4 C6 117.8(7) . . ? C5 O4 C6A 116.4(7) . . ? C6 O4 C6A 33.5(6) . . ? C17 O5 C18 114.1(4) . . ? C28 O6 C29 113.5(4) . . ? C38 O7 C39 112.6(4) . . ? C25 O8 Cu1 117.7(3) . 4_455 ? C25 O9 Cu1 127.6(3) . 2_655 ? C43 N1 C45 122.1(6) . . ? C43 N1 C44 118.3(6) . . ? C45 N1 C44 118.2(6) . . ? O1 C1 O2 125.0(5) . . ? O1 C1 C2 117.8(4) . . ? O2 C1 C2 117.2(5) . . ? C3 C2 C10 119.0(5) . . ? C3 C2 C1 121.6(5) . . ? C10 C2 C1 119.3(4) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 118.4(5) . . ? C3 C4 C42 121.6(5) . . ? C5 C4 C42 119.7(5) . . ? O4 C5 C4 118.5(5) . . ? O4 C5 C9 119.4(5) . . ? C4 C5 C9 121.7(5) . . ? O4 C6 C7 108.2(10) . . ? O4 C6 H6A 110.1 . . ? C7 C6 H6A 110.1 . . ? O4 C6 H6B 110.1 . . ? C7 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C8 C7 C6 103.5(14) . . ? C8 C7 H7A 111.1 . . ? C6 C7 H7A 111.1 . . ? C8 C7 H7B 111.1 . . ? C6 C7 H7B 111.1 . . ? H7A C7 H7B 109.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C5 117.6(5) . . ? C10 C9 C11 121.2(5) . . ? C5 C9 C11 120.8(4) . . ? C9 C10 C2 121.7(5) . . ? C9 C10 H10 119.2 . . ? C2 C10 H10 119.2 . . ? C9 C11 C12 110.0(4) . . ? C9 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C9 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C17 C12 C13 118.1(5) . . ? C17 C12 C11 122.6(5) . . ? C13 C12 C11 119.1(5) . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 119.3(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 121.0(5) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 118.6(5) . . ? C17 C16 C21 121.4(4) . . ? C15 C16 C21 119.8(4) . . ? O5 C17 C12 119.8(4) . . ? O5 C17 C16 118.4(4) . . ? C12 C17 C16 121.6(5) . . ? O5 C18 C19 113.5(4) . . ? O5 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? O5 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C18 C19 C20 111.0(4) . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C16 110.4(4) . . ? C22 C21 H21A 109.6 . . ? C16 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C16 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C28 117.6(4) . . ? C23 C22 C21 121.8(4) . . ? C28 C22 C21 120.1(4) . . ? C22 C23 C24 121.2(4) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C26 C24 C23 119.2(4) . . ? C26 C24 C25 122.1(4) . . ? C23 C24 C25 118.5(4) . . ? O9 C25 O8 125.7(4) . . ? O9 C25 C24 116.2(4) . . ? O8 C25 C24 118.0(4) . . ? C27 C26 C24 121.3(5) . . ? C27 C26 H26 119.4 . . ? C24 C26 H26 119.4 . . ? C26 C27 C28 117.7(4) . . ? C26 C27 C32 122.5(4) . . ? C28 C27 C32 119.7(4) . . ? O6 C28 C27 118.3(4) . . ? O6 C28 C22 119.4(4) . . ? C27 C28 C22 122.2(4) . . ? O6 C29 C30 112.2(5) . . ? O6 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? O6 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C29 C30 C31 111.0(6) . . ? C29 C30 H30A 109.4 . . ? C31 C30 H30A 109.4 . . ? C29 C30 H30B 109.4 . . ? C31 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 C33 111.0(4) . . ? C27 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C27 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C38 118.1(5) . . ? C34 C33 C32 119.7(4) . . ? C38 C33 C32 122.1(5) . . ? C35 C34 C33 121.0(5) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 120.2(5) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C37 120.6(5) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C38 118.0(5) . . ? C36 C37 C42 119.0(5) . . ? C38 C37 C42 122.9(5) . . ? C33 C38 O7 119.5(4) . . ? C33 C38 C37 122.0(5) . . ? O7 C38 C37 118.5(4) . . ? O7 C39 C40 109.3(6) . . ? O7 C39 H39A 109.8 . . ? C40 C39 H39A 109.8 . . ? O7 C39 H39B 109.8 . . ? C40 C39 H39B 109.8 . . ? H39A C39 H39B 108.3 . . ? C39 C40 C41 113.7(8) . . ? C39 C40 H40A 108.8 . . ? C41 C40 H40A 108.8 . . ? C39 C40 H40B 108.8 . . ? C41 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 C37 110.9(4) . . ? C4 C42 H42A 109.5 . . ? C37 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 108.0 . . ? O3 C43 N1 126.7(5) . . ? O3 C43 H43 116.7 . . ? N1 C43 H43 116.7 . . ? N1 C44 H44A 109.5 . . ? N1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N1 C45 H45A 109.5 . . ? N1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O4 C6A C7A 104.9(15) . . ? O4 C6A H6A1 110.8 . . ? C7A C6A H6A1 110.8 . . ? O4 C6A H6A2 110.8 . . ? C7A C6A H6A2 110.8 . . ? H6A1 C6A H6A2 108.8 . . ? C8A C7A C6A 107(2) . . ? C8A C7A H7A1 110.4 . . ? C6A C7A H7A1 110.4 . . ? C8A C7A H7A2 110.4 . . ? C6A C7A H7A2 110.4 . . ? H7A1 C7A H7A2 108.6 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Cu1 O1 C1 78.7(3) 2_645 . . . ? O8 Cu1 O1 C1 -90.2(3) 4_656 . . . ? O2 Cu1 O1 C1 -6.7(9) 3_746 . . . ? O3 Cu1 O1 C1 167.6(3) . . . . ? Cu1 Cu1 O1 C1 -1.8(3) 3_746 . . . ? O9 Cu1 O3 C43 -83.9(4) 2_645 . . . ? O1 Cu1 O3 C43 -172.2(4) . . . . ? O8 Cu1 O3 C43 95.7(4) 4_656 . . . ? O2 Cu1 O3 C43 6.8(4) 3_746 . . . ? Cu1 Cu1 O3 C43 -49.3(7) 3_746 . . . ? Cu1 O1 C1 O2 2.2(6) . . . . ? Cu1 O1 C1 C2 -177.9(3) . . . . ? Cu1 O2 C1 O1 -1.0(7) 3_746 . . . ? Cu1 O2 C1 C2 179.1(3) 3_746 . . . ? O1 C1 C2 C3 8.8(6) . . . . ? O2 C1 C2 C3 -171.3(4) . . . . ? O1 C1 C2 C10 -168.0(4) . . . . ? O2 C1 C2 C10 11.9(6) . . . . ? C10 C2 C3 C4 -3.7(7) . . . . ? C1 C2 C3 C4 179.5(4) . . . . ? C2 C3 C4 C5 -1.4(7) . . . . ? C2 C3 C4 C42 172.6(4) . . . . ? C6 O4 C5 C4 82.8(8) . . . . ? C6A O4 C5 C4 120.6(7) . . . . ? C6 O4 C5 C9 -103.8(8) . . . . ? C6A O4 C5 C9 -66.0(8) . . . . ? C3 C4 C5 O4 -179.5(4) . . . . ? C42 C4 C5 O4 6.4(7) . . . . ? C3 C4 C5 C9 7.3(7) . . . . ? C42 C4 C5 C9 -166.9(4) . . . . ? C5 O4 C6 C7 90.1(13) . . . . ? C6A O4 C6 C7 -6.6(14) . . . . ? O4 C6 C7 C8 166.5(15) . . . . ? O4 C5 C9 C10 179.1(4) . . . . ? C4 C5 C9 C10 -7.8(7) . . . . ? O4 C5 C9 C11 -8.4(7) . . . . ? C4 C5 C9 C11 164.7(5) . . . . ? C5 C9 C10 C2 2.4(7) . . . . ? C11 C9 C10 C2 -170.0(5) . . . . ? C3 C2 C10 C9 3.1(7) . . . . ? C1 C2 C10 C9 -179.9(4) . . . . ? C10 C9 C11 C12 109.2(5) . . . . ? C5 C9 C11 C12 -63.0(6) . . . . ? C9 C11 C12 C17 129.8(5) . . . . ? C9 C11 C12 C13 -45.2(6) . . . . ? C17 C12 C13 C14 -1.4(8) . . . . ? C11 C12 C13 C14 173.9(5) . . . . ? C12 C13 C14 C15 -1.6(8) . . . . ? C13 C14 C15 C16 1.8(8) . . . . ? C14 C15 C16 C17 1.0(7) . . . . ? C14 C15 C16 C21 -174.3(5) . . . . ? C18 O5 C17 C12 80.1(5) . . . . ? C18 O5 C17 C16 -105.3(5) . . . . ? C13 C12 C17 O5 178.8(4) . . . . ? C11 C12 C17 O5 3.7(7) . . . . ? C13 C12 C17 C16 4.3(7) . . . . ? C11 C12 C17 C16 -170.8(4) . . . . ? C15 C16 C17 O5 -178.7(4) . . . . ? C21 C16 C17 O5 -3.5(7) . . . . ? C15 C16 C17 C12 -4.1(7) . . . . ? C21 C16 C17 C12 171.1(4) . . . . ? C17 O5 C18 C19 72.8(5) . . . . ? O5 C18 C19 C20 176.9(4) . . . . ? C17 C16 C21 C22 -125.0(5) . . . . ? C15 C16 C21 C22 50.1(6) . . . . ? C16 C21 C22 C23 -113.7(5) . . . . ? C16 C21 C22 C28 57.5(6) . . . . ? C28 C22 C23 C24 -2.3(8) . . . . ? C21 C22 C23 C24 169.2(5) . . . . ? C22 C23 C24 C26 -5.2(8) . . . . ? C22 C23 C24 C25 169.8(5) . . . . ? Cu1 O9 C25 O8 5.7(7) 2_655 . . . ? Cu1 O9 C25 C24 -172.2(3) 2_655 . . . ? Cu1 O8 C25 O9 -3.9(6) 4_455 . . . ? Cu1 O8 C25 C24 174.0(3) 4_455 . . . ? C26 C24 C25 O9 170.9(5) . . . . ? C23 C24 C25 O9 -3.9(7) . . . . ? C26 C24 C25 O8 -7.2(7) . . . . ? C23 C24 C25 O8 178.0(4) . . . . ? C23 C24 C26 C27 6.2(7) . . . . ? C25 C24 C26 C27 -168.6(5) . . . . ? C24 C26 C27 C28 0.3(7) . . . . ? C24 C26 C27 C32 -177.8(5) . . . . ? C29 O6 C28 C27 -111.7(5) . . . . ? C29 O6 C28 C22 72.2(6) . . . . ? C26 C27 C28 O6 175.8(4) . . . . ? C32 C27 C28 O6 -6.0(7) . . . . ? C26 C27 C28 C22 -8.1(7) . . . . ? C32 C27 C28 C22 170.0(5) . . . . ? C23 C22 C28 O6 -174.9(4) . . . . ? C21 C22 C28 O6 13.5(7) . . . . ? C23 C22 C28 C27 9.1(8) . . . . ? C21 C22 C28 C27 -162.5(5) . . . . ? C28 O6 C29 C30 90.3(6) . . . . ? O6 C29 C30 C31 178.7(6) . . . . ? C26 C27 C32 C33 110.3(5) . . . . ? C28 C27 C32 C33 -67.7(6) . . . . ? C27 C32 C33 C34 -52.5(6) . . . . ? C27 C32 C33 C38 123.8(5) . . . . ? C38 C33 C34 C35 -1.7(8) . . . . ? C32 C33 C34 C35 174.8(5) . . . . ? C33 C34 C35 C36 -0.6(9) . . . . ? C34 C35 C36 C37 1.4(9) . . . . ? C35 C36 C37 C38 0.1(8) . . . . ? C35 C36 C37 C42 -176.3(5) . . . . ? C34 C33 C38 O7 -178.4(4) . . . . ? C32 C33 C38 O7 5.3(7) . . . . ? C34 C33 C38 C37 3.3(8) . . . . ? C32 C33 C38 C37 -173.0(5) . . . . ? C39 O7 C38 C33 84.5(6) . . . . ? C39 O7 C38 C37 -97.1(5) . . . . ? C36 C37 C38 C33 -2.6(8) . . . . ? C42 C37 C38 C33 173.7(5) . . . . ? C36 C37 C38 O7 179.1(5) . . . . ? C42 C37 C38 O7 -4.6(7) . . . . ? C38 O7 C39 C40 -168.7(5) . . . . ? O7 C39 C40 C41 -174.5(6) . . . . ? C3 C4 C42 C37 -111.4(5) . . . . ? C5 C4 C42 C37 62.6(6) . . . . ? C36 C37 C42 C4 58.0(7) . . . . ? C38 C37 C42 C4 -118.3(6) . . . . ? Cu1 O3 C43 N1 152.8(5) . . . . ? C45 N1 C43 O3 175.1(6) . . . . ? C44 N1 C43 O3 8.8(11) . . . . ? C5 O4 C6A C7A -94.0(16) . . . . ? C6 O4 C6A C7A 7.1(19) . . . . ? O4 C6A C7A C8A 170(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.114 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.109 #===end data_h10adb8 _database_code_depnum_ccdc_archive 'CCDC 866580' #TrackingRef '- calix-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H127 Cd2 N5 O21' _chemical_formula_weight 1947.86 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.5500(3) _cell_length_b 24.9210(2) _cell_length_c 25.2820(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.005(1) _cell_angle_gamma 90.00 _cell_volume 9797.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 157897 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74270 _diffrn_reflns_av_R_equivalents 0.1147 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 17143 _reflns_number_gt 12798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; 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. Notes: Several of the n-propyl groups appended to the calixarenes exhibited 60:40 disorder, as did the DMF moiety ligated to Cd1. Only major atom fractions in these disordered moieties were refined anisotropically, with the exception of the group containing O11, where the electron density was very smeared. O-C and C-C distance restraints were applied in disordered n-propyl functionalities to assist convergence. There is also 'free' solvent in the asymmetric unit of this structure. This consists of one area of well defined solvent, and 2 areas where it is more diffuse. Strenuous efforts could not successfully render a credible model that would converge for the diffuse regions - which each approximated to one molecule of DMF. Hence, Platon SQUEEZE was employed, and this also suggested the presence of 2 molecules of DMF in terms of void volume. Data presented herein takes account of this 'pre-squeeze' solvent. Data were truncated to a max Bragg angle of 25o for this needle-like crystal. A fall off in diffraction intensity was noted - probably a function of the disordered solvent present and the small size of 2 of the sample dimensions. ; _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^)+(0.1408P)^2^+4.0683P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17143 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2163 _refine_ls_wR_factor_gt 0.1999 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _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 Cd1 Cd 0.93157(2) 0.052584(14) 0.915861(14) 0.03865(14) Uani 1 1 d . . . Cd2 Cd 1.15318(2) 0.007521(14) 0.957327(14) 0.03983(14) Uani 1 1 d . . . O1 O 0.8782(2) 0.07283(13) 1.00507(14) 0.0436(8) Uani 1 1 d . . . O2 O 0.8442(2) 0.12464(14) 0.93780(14) 0.0472(8) Uani 1 1 d . . . O3 O 0.6181(3) 0.23903(16) 1.11283(15) 0.0568(10) Uani 1 1 d D . . O4 O 0.4545(2) 0.28614(14) 1.05002(16) 0.0527(9) Uani 1 1 d . . . O5 O 0.3938(3) 0.20947(16) 1.14310(16) 0.0580(10) Uani 1 1 d . C . O6 O 0.1771(2) -0.00394(15) 1.11912(16) 0.0505(9) Uani 1 1 d . . . O7 O 0.1407(2) 0.03576(16) 1.04430(15) 0.0498(9) Uani 1 1 d . . . O8 O 0.5496(3) 0.18101(19) 1.21719(14) 0.0629(11) Uani 1 1 d D . . O9 O 1.0297(2) -0.01382(14) 0.89585(14) 0.0459(8) Uani 1 1 d . . . O10 O 1.1650(2) -0.01872(15) 0.86998(13) 0.0467(8) Uani 1 1 d . . . O11 O 0.9837(3) -0.0630(2) 0.65068(16) 0.0692(12) Uani 1 1 d D . . O12 O 1.1268(3) -0.11728(16) 0.56941(15) 0.0602(10) Uani 1 1 d . F . O13 O 0.9181(3) -0.16155(15) 0.56798(18) 0.0645(11) Uani 1 1 d D . . O14 O 0.9403(2) -0.41612(14) 0.55140(15) 0.0492(9) Uani 1 1 d . . . O15 O 0.8021(2) -0.40426(14) 0.56542(15) 0.0490(9) Uani 1 1 d . . . O16 O 0.7721(2) -0.09192(15) 0.63318(15) 0.0509(9) Uani 1 1 d D . . O17 O 0.9561(3) 0.0930(2) 0.83618(18) 0.0753(13) Uani 1 1 d . . . O21 O 1.2910(2) -0.01275(15) 0.97744(17) 0.0537(9) Uani 1 1 d . . . O22 O 0.6710(4) 0.0280(3) 0.7572(3) 0.112(2) Uani 1 1 d . . . N1 N 1.0359(8) 0.1198(5) 0.7649(4) 0.073(3) Uani 0.60 1 d P A 1 N2 N 1.3992(3) 0.01634(19) 1.02999(18) 0.0504(11) Uani 1 1 d . . . N4 N 0.6801(4) 0.1057(3) 0.8034(2) 0.0776(16) Uani 1 1 d . . . N1A N 0.9947(13) 0.1406(7) 0.7692(8) 0.075(5) Uiso 0.40 1 d P B 2 C1 C 0.8362(3) 0.11210(19) 0.9856(2) 0.0398(11) Uani 1 1 d . . . C2 C 0.7780(3) 0.14484(18) 1.01924(19) 0.0388(11) Uani 1 1 d . . . C3 C 0.7701(3) 0.1345(2) 1.07355(19) 0.0401(11) Uani 1 1 d . C . H3 H 0.8015 0.1057 1.0888 0.048 Uiso 1 1 calc R . . C4 C 0.7175(3) 0.1657(2) 1.1053(2) 0.0428(11) Uani 1 1 d . . . C5 C 0.6713(3) 0.2081(2) 1.0820(2) 0.0421(11) Uani 1 1 d . C . C6 C 0.6624(9) 0.2762(4) 1.1482(5) 0.078(4) Uani 0.60 1 d PD C 1 H6A H 0.7123 0.2580 1.1646 0.093 Uiso 0.60 1 calc PR C 1 H6B H 0.6229 0.2875 1.1768 0.093 Uiso 0.60 1 calc PR C 1 C7 C 0.6934(12) 0.3259(6) 1.1176(6) 0.119(6) Uani 0.60 1 d PD C 1 H7A H 0.6431 0.3440 1.1015 0.142 Uiso 0.60 1 calc PR C 1 H7B H 0.7318 0.3142 1.0886 0.142 Uiso 0.60 1 calc PR C 1 C8 C 0.742(3) 0.3664(10) 1.1527(12) 0.186(17) Uani 0.60 1 d PD C 1 H8A H 0.7598 0.3972 1.1312 0.279 Uiso 0.60 1 calc PR C 1 H8B H 0.7927 0.3491 1.1680 0.279 Uiso 0.60 1 calc PR C 1 H8C H 0.7039 0.3787 1.1811 0.279 Uiso 0.60 1 calc PR C 1 C9 C 0.6748(3) 0.21675(19) 1.0276(2) 0.0390(11) Uani 1 1 d . . . C10 C 0.7297(3) 0.18595(19) 0.9974(2) 0.0397(11) Uani 1 1 d . C . H10 H 0.7345 0.1931 0.9606 0.048 Uiso 1 1 calc R . . C11 C 0.6144(3) 0.2568(2) 1.0007(2) 0.0472(12) Uani 1 1 d . C . H11A H 0.6043 0.2878 1.0245 0.057 Uiso 1 1 calc R . . H11B H 0.6412 0.2703 0.9678 0.057 Uiso 1 1 calc R . . C12 C 0.5291(3) 0.22989(19) 0.9878(2) 0.0426(11) Uani 1 1 d . . . C13 C 0.5250(3) 0.1904(2) 0.9502(2) 0.0443(12) Uani 1 1 d . C . H13 H 0.5755 0.1815 0.9309 0.053 Uiso 1 1 calc R . . C14 C 0.4493(4) 0.1631(2) 0.9395(2) 0.0493(13) Uani 1 1 d . . . H14 H 0.4465 0.1380 0.9113 0.059 Uiso 1 1 calc R C . C15 C 0.3784(3) 0.1732(2) 0.9703(2) 0.0454(12) Uani 1 1 d . C . H15 H 0.3273 0.1532 0.9645 0.054 Uiso 1 1 calc R . . C16 C 0.3794(3) 0.2121(2) 1.0101(2) 0.0443(12) Uani 1 1 d . . . C17 C 0.4544(3) 0.2426(2) 1.0161(2) 0.0454(12) Uani 1 1 d . C . C18 C 0.4285(5) 0.3347(2) 1.0238(3) 0.076(2) Uani 1 1 d . . . H18A H 0.3698 0.3304 1.0091 0.091 Uiso 1 1 calc R . . H18B H 0.4682 0.3426 0.9942 0.091 Uiso 1 1 calc R . . C19 C 0.4298(7) 0.3799(3) 1.0627(4) 0.107(3) Uani 1 1 d . . . H19A H 0.4878 0.3823 1.0787 0.129 Uiso 1 1 calc R . . H19B H 0.3883 0.3722 1.0914 0.129 Uiso 1 1 calc R . . C20 C 0.4075(9) 0.4328(3) 1.0380(6) 0.138(5) Uani 1 1 d . . . H20A H 0.4555 0.4449 1.0158 0.207 Uiso 1 1 calc R . . H20B H 0.3967 0.4593 1.0658 0.207 Uiso 1 1 calc R . . H20C H 0.3559 0.4287 1.0161 0.207 Uiso 1 1 calc R . . C21 C 0.3021(3) 0.2181(2) 1.0469(2) 0.0528(13) Uani 1 1 d . C . H21A H 0.3088 0.2510 1.0685 0.063 Uiso 1 1 calc R . . H21B H 0.2490 0.2219 1.0255 0.063 Uiso 1 1 calc R . . C22 C 0.2939(3) 0.1703(2) 1.0826(2) 0.0454(12) Uani 1 1 d . . . C23 C 0.2430(3) 0.1261(2) 1.0698(2) 0.0470(12) Uani 1 1 d . C . H23 H 0.2106 0.1268 1.0379 0.056 Uiso 1 1 calc R . . C24 C 0.2382(3) 0.0813(2) 1.10176(19) 0.0408(11) Uani 1 1 d . . . C25 C 0.1822(3) 0.0346(2) 1.0871(2) 0.0433(12) Uani 1 1 d . C . C26 C 0.2862(3) 0.0797(2) 1.1477(2) 0.0457(12) Uani 1 1 d . C . H26 H 0.2839 0.0485 1.1693 0.055 Uiso 1 1 calc R . . C27 C 0.3374(3) 0.1219(2) 1.1632(2) 0.0447(12) Uani 1 1 d . . . C28 C 0.3406(3) 0.1675(2) 1.1304(2) 0.0491(13) Uani 1 1 d . C . C29 C 0.3545(5) 0.2472(3) 1.1770(4) 0.088(2) Uani 1 1 d DU . . H29A H 0.3333 0.2292 1.2093 0.105 Uiso 1 1 calc R D 1 H29B H 0.3051 0.2643 1.1590 0.105 Uiso 1 1 calc R D 1 C30 C 0.4224(5) 0.2896(3) 1.1913(4) 0.107(2) Uani 1 1 d DU E 1 H30A H 0.4744 0.2720 1.2058 0.128 Uiso 1 1 calc R E 1 H30B H 0.4392 0.3101 1.1594 0.128 Uiso 1 1 calc R E 1 C31 C 0.3830(8) 0.3273(5) 1.2326(5) 0.162(5) Uani 1 1 d DU E 1 H31A H 0.3381 0.3491 1.2160 0.243 Uiso 1 1 calc R E 1 H31B H 0.4279 0.3508 1.2469 0.243 Uiso 1 1 calc R E 1 H31C H 0.3580 0.3060 1.2614 0.243 Uiso 1 1 calc R E 1 C32 C 0.3925(4) 0.1184(3) 1.2118(2) 0.0567(15) Uani 1 1 d . C . H32A H 0.3651 0.0942 1.2379 0.068 Uiso 1 1 calc R . . H32B H 0.3981 0.1544 1.2280 0.068 Uiso 1 1 calc R . . C33 C 0.4824(4) 0.0967(3) 1.1970(2) 0.0539(14) Uani 1 1 d . . . C34 C 0.4910(4) 0.0449(3) 1.1804(2) 0.0579(15) Uani 1 1 d . C . H34 H 0.4429 0.0214 1.1823 0.069 Uiso 1 1 calc R . . C35 C 0.5678(4) 0.0258(3) 1.1607(3) 0.0617(16) Uani 1 1 d . . . H35 H 0.5739 -0.0110 1.1519 0.074 Uiso 1 1 calc R C . C36 C 0.6372(4) 0.0616(2) 1.1539(3) 0.0574(15) Uani 1 1 d . C . H36 H 0.6885 0.0499 1.1370 0.069 Uiso 1 1 calc R . . C37 C 0.6302(3) 0.1137(2) 1.17200(19) 0.0463(12) Uani 1 1 d . . . C38 C 0.5544(3) 0.1309(2) 1.19578(19) 0.0498(13) Uani 1 1 d . C . C39 C 0.5671(10) 0.1761(6) 1.2760(2) 0.169(4) Uani 1 1 d DU . . H39A H 0.5137 0.1859 1.2950 0.203 Uiso 1 1 calc R . . H39B H 0.5789 0.1379 1.2837 0.203 Uiso 1 1 calc R . . C40 C 0.6281(11) 0.2037(7) 1.2955(4) 0.178(4) Uani 1 1 d DU . . H40A H 0.6243 0.2409 1.2819 0.214 Uiso 1 1 calc R . . H40B H 0.6837 0.1885 1.2836 0.214 Uiso 1 1 calc R . . C41 C 0.6264(9) 0.2050(5) 1.3556(3) 0.137(4) Uani 1 1 d DU . . H41A H 0.5791 0.1826 1.3685 0.205 Uiso 1 1 calc R . . H41B H 0.6180 0.2420 1.3676 0.205 Uiso 1 1 calc R . . H41C H 0.6810 0.1913 1.3694 0.205 Uiso 1 1 calc R . . C42 C 0.7070(3) 0.1513(2) 1.1636(2) 0.0462(12) Uani 1 1 d . C . H42A H 0.6985 0.1845 1.1844 0.055 Uiso 1 1 calc R . . H42B H 0.7601 0.1336 1.1764 0.055 Uiso 1 1 calc R . . C43 C 1.0291(9) 0.1043(6) 0.8154(5) 0.071(3) Uani 0.60 1 d P A 1 H43 H 1.0796 0.1017 0.8364 0.086 Uiso 0.60 1 calc PR A 1 C44 C 0.9611(12) 0.1223(10) 0.7303(8) 0.109(6) Uani 0.60 1 d P A 1 H44A H 0.9787 0.1348 0.6952 0.164 Uiso 0.60 1 calc PR A 1 H44B H 0.9188 0.1473 0.7452 0.164 Uiso 0.60 1 calc PR A 1 H44C H 0.9354 0.0865 0.7273 0.164 Uiso 0.60 1 calc PR A 1 C45 C 1.1247(11) 0.1235(8) 0.7403(7) 0.118(6) Uani 0.60 1 d P A 1 H45A H 1.1196 0.1354 0.7034 0.177 Uiso 0.60 1 calc PR A 1 H45B H 1.1523 0.0881 0.7413 0.177 Uiso 0.60 1 calc PR A 1 H45C H 1.1597 0.1493 0.7601 0.177 Uiso 0.60 1 calc PR A 1 C46 C 1.0861(3) -0.0214(2) 0.8599(2) 0.0419(11) Uani 1 1 d . . . C47 C 1.0587(4) -0.0347(2) 0.8057(2) 0.0473(12) Uani 1 1 d . . . C48 C 0.9723(3) -0.0357(2) 0.7924(2) 0.0457(12) Uani 1 1 d . F . H48 H 0.9304 -0.0292 0.8190 0.055 Uiso 1 1 calc R . . C49 C 0.9461(4) -0.0459(2) 0.7410(2) 0.0507(13) Uani 1 1 d . . . C50 C 1.0094(4) -0.0546(2) 0.7022(2) 0.0540(14) Uani 1 1 d . F . C51 C 1.0048(12) -0.0158(6) 0.6140(8) 0.102(6) Uiso 0.60 1 d PD F 1 H51C H 1.0132 -0.0285 0.5773 0.122 Uiso 0.60 1 calc PR F 1 H51D H 1.0581 0.0024 0.6258 0.122 Uiso 0.60 1 calc PR F 1 C52 C 0.9277(16) 0.0230(10) 0.6170(14) 0.194(11) Uiso 0.60 1 d PD F 1 H52C H 0.8796 0.0075 0.5964 0.232 Uiso 0.60 1 calc PR F 1 H52D H 0.9088 0.0255 0.6543 0.232 Uiso 0.60 1 calc PR F 1 C53 C 0.945(3) 0.0801(12) 0.5964(16) 0.237(16) Uiso 0.60 1 d PD F 1 H53D H 0.9964 0.0947 0.6141 0.356 Uiso 0.60 1 calc PR F 1 H53E H 0.8958 0.1030 0.6038 0.356 Uiso 0.60 1 calc PR F 1 H53F H 0.9556 0.0788 0.5581 0.356 Uiso 0.60 1 calc PR F 1 C54 C 1.0960(4) -0.0576(2) 0.7148(2) 0.0513(13) Uani 1 1 d . . . C55 C 1.1205(4) -0.0471(2) 0.7668(2) 0.0487(13) Uani 1 1 d . F . H55 H 1.1797 -0.0483 0.7761 0.058 Uiso 1 1 calc R . . C56 C 1.1605(4) -0.0772(3) 0.6740(2) 0.0566(15) Uani 1 1 d . F . H56A H 1.2195 -0.0720 0.6877 0.068 Uiso 1 1 calc R . . H56B H 1.1544 -0.0558 0.6413 0.068 Uiso 1 1 calc R . . C57 C 1.1465(3) -0.1362(2) 0.6615(2) 0.0507(13) Uani 1 1 d . . . C58 C 1.1489(4) -0.1734(3) 0.7010(3) 0.0689(17) Uani 1 1 d . F . H58 H 1.1627 -0.1622 0.7359 0.083 Uiso 1 1 calc R . . C59 C 1.1317(5) -0.2275(3) 0.6916(3) 0.0763(19) Uani 1 1 d . . . H59 H 1.1355 -0.2528 0.7196 0.092 Uiso 1 1 calc R F . C60 C 1.1095(4) -0.2439(3) 0.6421(3) 0.0657(16) Uani 1 1 d . F . H60 H 1.0977 -0.2807 0.6356 0.079 Uiso 1 1 calc R . . C61 C 1.1040(3) -0.2066(2) 0.6004(2) 0.0498(13) Uani 1 1 d . . . C62 C 1.1268(3) -0.1538(2) 0.6103(2) 0.0486(13) Uani 1 1 d . F . C63 C 1.2011(6) -0.1200(4) 0.5365(3) 0.102(3) Uani 1 1 d D . . H63A H 1.1863 -0.1403 0.5041 0.123 Uiso 1 1 calc R G 1 H63B H 1.2463 -0.1404 0.5554 0.123 Uiso 1 1 calc R G 1 C64 C 1.2377(13) -0.0652(6) 0.5204(14) 0.28(3) Uani 0.60 1 d PD H 1 H64A H 1.2391 -0.0404 0.5510 0.336 Uiso 0.60 1 calc PR H 1 H64B H 1.2029 -0.0489 0.4918 0.336 Uiso 0.60 1 calc PR H 1 C65 C 1.3293(17) -0.0780(16) 0.5010(17) 0.22(3) Uani 0.60 1 d PD H 1 H65A H 1.3576 -0.0447 0.4898 0.326 Uiso 0.60 1 calc PR H 1 H65B H 1.3263 -0.1028 0.4710 0.326 Uiso 0.60 1 calc PR H 1 H65C H 1.3622 -0.0945 0.5297 0.326 Uiso 0.60 1 calc PR H 1 C66 C 1.0691(4) -0.2250(2) 0.5473(2) 0.0535(14) Uani 1 1 d . F . H66A H 1.0664 -0.1941 0.5227 0.064 Uiso 1 1 calc R . . H66B H 1.1082 -0.2522 0.5318 0.064 Uiso 1 1 calc R . . C67 C 0.9808(4) -0.2487(2) 0.5540(2) 0.0494(13) Uani 1 1 d . . . C68 C 0.9692(4) -0.3042(2) 0.5531(2) 0.0471(12) Uani 1 1 d . F . H68 H 1.0158 -0.3269 0.5437 0.057 Uiso 1 1 calc R . . C69 C 0.8898(3) -0.3266(2) 0.5657(2) 0.0426(11) Uani 1 1 d . . . C70 C 0.8763(4) -0.3856(2) 0.5608(2) 0.0448(12) Uani 1 1 d . . . C71 C 0.8227(4) -0.2944(2) 0.5837(2) 0.0475(12) Uani 1 1 d . F . H71 H 0.7706 -0.3103 0.5956 0.057 Uiso 1 1 calc R . . C72 C 0.8323(4) -0.2384(2) 0.5843(2) 0.0496(13) Uani 1 1 d . . . C73 C 0.9094(4) -0.2163(2) 0.5671(2) 0.0515(13) Uani 1 1 d . F . C74 C 0.9230(6) -0.1379(4) 0.5124(3) 0.126(3) Uani 1 1 d DU I 1 H74A H 0.9549 -0.1625 0.4888 0.151 Uiso 1 1 calc R I 1 H74B H 0.9535 -0.1030 0.5133 0.151 Uiso 1 1 calc R I 1 C75 C 0.8312(6) -0.1302(5) 0.4922(4) 0.141(3) Uani 1 1 d DU I 1 H75A H 0.7984 -0.1070 0.5168 0.169 Uiso 1 1 calc R I 1 H75B H 0.8016 -0.1653 0.4897 0.169 Uiso 1 1 calc R I 1 C76 C 0.8366(9) -0.1039(7) 0.4372(5) 0.171(5) Uani 1 1 d DU I 1 H76A H 0.8679 -0.0698 0.4400 0.256 Uiso 1 1 calc R I 1 H76B H 0.7784 -0.0971 0.4239 0.256 Uiso 1 1 calc R I 1 H76C H 0.8670 -0.1279 0.4129 0.256 Uiso 1 1 calc R I 1 C77 C 0.7595(4) -0.2033(2) 0.6074(2) 0.0555(14) Uani 1 1 d . F . H77A H 0.7481 -0.1725 0.5836 0.067 Uiso 1 1 calc R . . H77B H 0.7060 -0.2246 0.6103 0.067 Uiso 1 1 calc R . . C78 C 0.7855(3) -0.1832(2) 0.6609(2) 0.0531(13) Uani 1 1 d . . . C79 C 0.8070(4) -0.2203(3) 0.7012(3) 0.0645(16) Uani 1 1 d . F . H79 H 0.8010 -0.2577 0.6953 0.077 Uiso 1 1 calc R . . C80 C 0.8367(5) -0.2015(3) 0.7490(3) 0.0681(17) Uani 1 1 d . . . H80 H 0.8485 -0.2265 0.7765 0.082 Uiso 1 1 calc R F . C81 C 0.8497(4) -0.1481(3) 0.7580(2) 0.0600(15) Uani 1 1 d . F . H81 H 0.8718 -0.1366 0.7912 0.072 Uiso 1 1 calc R . . C82 C 0.8306(3) -0.1103(2) 0.7190(2) 0.0471(12) Uani 1 1 d . . . C83 C 0.7950(3) -0.1287(2) 0.6719(2) 0.0437(12) Uani 1 1 d . F . C84 C 0.6867(8) -0.0726(7) 0.6435(6) 0.067(4) Uani 0.60 1 d PD J 1 H84A H 0.6812 -0.0609 0.6807 0.080 Uiso 0.60 1 calc PR J 1 H84B H 0.6438 -0.1011 0.6365 0.080 Uiso 0.60 1 calc PR J 1 C85 C 0.6732(10) -0.0249(8) 0.6056(6) 0.123(7) Uani 0.60 1 d PD J 1 H85A H 0.7187 0.0021 0.6117 0.148 Uiso 0.60 1 calc PR J 1 H85B H 0.6782 -0.0375 0.5686 0.148 Uiso 0.60 1 calc PR J 1 C86 C 0.5845(13) 0.0013(13) 0.6138(14) 0.208(14) Uani 0.60 1 d PD J 1 H86A H 0.5397 -0.0226 0.6000 0.311 Uiso 0.60 1 calc PR J 1 H86B H 0.5825 0.0356 0.5949 0.311 Uiso 0.60 1 calc PR J 1 H86C H 0.5749 0.0074 0.6516 0.311 Uiso 0.60 1 calc PR J 1 C87 C 0.8512(4) -0.0521(2) 0.7283(2) 0.0561(15) Uani 1 1 d . F . H87A H 0.8162 -0.0383 0.7580 0.067 Uiso 1 1 calc R . . H87B H 0.8369 -0.0310 0.6963 0.067 Uiso 1 1 calc R . . C88 C 1.3452(4) 0.0222(2) 0.9911(2) 0.0527(14) Uani 1 1 d . . . H88 H 1.3468 0.0549 0.9718 0.063 Uiso 1 1 calc R . . C89 C 1.3961(4) -0.0322(3) 1.0631(3) 0.0625(16) Uani 1 1 d . . . H89A H 1.3721 -0.0232 1.0978 0.094 Uiso 1 1 calc R . . H89B H 1.4544 -0.0465 1.0675 0.094 Uiso 1 1 calc R . . H89C H 1.3598 -0.0593 1.0460 0.094 Uiso 1 1 calc R . . C90 C 1.4564(4) 0.0597(2) 1.0461(2) 0.0537(14) Uani 1 1 d . . . H90A H 1.4553 0.0882 1.0194 0.081 Uiso 1 1 calc R . . H90B H 1.5151 0.0459 1.0497 0.081 Uiso 1 1 calc R . . H90C H 1.4372 0.0742 1.0802 0.081 Uiso 1 1 calc R . . C91 C 0.7321(7) 0.1421(5) 0.8326(4) 0.126(4) Uani 1 1 d . . . H91A H 0.7156 0.1410 0.8700 0.188 Uiso 1 1 calc R . . H91B H 0.7239 0.1785 0.8189 0.188 Uiso 1 1 calc R . . H91C H 0.7927 0.1319 0.8290 0.188 Uiso 1 1 calc R . . C92 C 0.7116(6) 0.0601(3) 0.7839(3) 0.077(2) Uani 1 1 d . . . H92 H 0.7701 0.0520 0.7912 0.092 Uiso 1 1 calc R . . C93 C 0.5923(6) 0.1194(4) 0.7961(5) 0.121(4) Uani 1 1 d . . . H93A H 0.5696 0.1004 0.7652 0.181 Uiso 1 1 calc R . . H93B H 0.5872 0.1582 0.7906 0.181 Uiso 1 1 calc R . . H93C H 0.5594 0.1091 0.8276 0.181 Uiso 1 1 calc R . . C6A C 0.6502(14) 0.2941(7) 1.1193(9) 0.086(6) Uiso 0.40 1 d PD C 2 H6A1 H 0.6010 0.3188 1.1248 0.103 Uiso 0.40 1 calc PR C 2 H6A2 H 0.6805 0.3054 1.0867 0.103 Uiso 0.40 1 calc PR C 2 C7A C 0.7120(16) 0.2980(10) 1.1667(9) 0.107(7) Uiso 0.40 1 d PD C 2 H7A1 H 0.7649 0.2767 1.1610 0.129 Uiso 0.40 1 calc PR C 2 H7A2 H 0.6841 0.2867 1.2001 0.129 Uiso 0.40 1 calc PR C 2 C8A C 0.730(2) 0.3587(10) 1.1661(17) 0.103(11) Uiso 0.40 1 d PD C 2 H8A1 H 0.7703 0.3677 1.1948 0.155 Uiso 0.40 1 calc PR C 2 H8A2 H 0.6766 0.3785 1.1709 0.155 Uiso 0.40 1 calc PR C 2 H8A3 H 0.7564 0.3686 1.1321 0.155 Uiso 0.40 1 calc PR C 2 C43A C 0.9862(16) 0.1232(9) 0.8187(9) 0.071(6) Uiso 0.40 1 d P B 2 H43A H 1.0164 0.1451 0.8432 0.085 Uiso 0.40 1 calc PR B 2 C44A C 0.984(4) 0.110(3) 0.709(2) 0.21(3) Uiso 0.40 1 d P B 2 H44D H 0.9955 0.1361 0.6807 0.317 Uiso 0.40 1 calc PR B 2 H44E H 0.9248 0.0966 0.7051 0.317 Uiso 0.40 1 calc PR B 2 H44F H 1.0242 0.0802 0.7062 0.317 Uiso 0.40 1 calc PR B 2 C45A C 1.0549(17) 0.1863(11) 0.7603(11) 0.113(8) Uiso 0.40 1 d P B 2 H45D H 1.0553 0.1957 0.7226 0.170 Uiso 0.40 1 calc PR B 2 H45E H 1.1130 0.1758 0.7712 0.170 Uiso 0.40 1 calc PR B 2 H45F H 1.0361 0.2173 0.7811 0.170 Uiso 0.40 1 calc PR B 2 C51A C 0.990(4) -0.0087(14) 0.6239(19) 0.23(3) Uiso 0.40 1 d PD F 2 H51A H 1.0493 -0.0020 0.6109 0.272 Uiso 0.40 1 calc PR F 2 H51B H 0.9733 0.0206 0.6483 0.272 Uiso 0.40 1 calc PR F 2 C52A C 0.926(3) -0.0139(13) 0.5777(15) 0.199(18) Uiso 0.40 1 d PD F 2 H52A H 0.9463 -0.0403 0.5512 0.238 Uiso 0.40 1 calc PR F 2 H52B H 0.8683 -0.0244 0.5903 0.238 Uiso 0.40 1 calc PR F 2 C53A C 0.927(3) 0.0434(14) 0.5554(17) 0.21(2) Uiso 0.40 1 d PD F 2 H53A H 0.9276 0.0693 0.5846 0.319 Uiso 0.40 1 calc PR F 2 H53B H 0.8748 0.0491 0.5340 0.319 Uiso 0.40 1 calc PR F 2 H53C H 0.9777 0.0485 0.5332 0.319 Uiso 0.40 1 calc PR F 2 C64A C 1.2741(8) -0.0826(5) 0.5536(6) 0.052(3) Uiso 0.40 1 d PD H 2 H64C H 1.2951 -0.0940 0.5888 0.063 Uiso 0.40 1 calc PR H 2 H64D H 1.2513 -0.0457 0.5570 0.063 Uiso 0.40 1 calc PR H 2 C65A C 1.350(2) -0.082(3) 0.5146(15) 0.118(12) Uiso 0.40 1 d PD H 2 H65D H 1.3947 -0.0577 0.5275 0.178 Uiso 0.40 1 calc PR H 2 H65E H 1.3301 -0.0702 0.4798 0.178 Uiso 0.40 1 calc PR H 2 H65F H 1.3739 -0.1185 0.5116 0.178 Uiso 0.40 1 calc PR H 2 C84A C 0.6991(11) -0.0582(8) 0.6364(14) 0.070(9) Uiso 0.40 1 d PD J 2 H84C H 0.7026 -0.0304 0.6085 0.084 Uiso 0.40 1 calc PR J 2 H84D H 0.6988 -0.0397 0.6711 0.084 Uiso 0.40 1 calc PR J 2 C85A C 0.6152(13) -0.0901(8) 0.6299(10) 0.100(7) Uiso 0.40 1 d PD J 2 H85C H 0.6125 -0.1198 0.6559 0.120 Uiso 0.40 1 calc PR J 2 H85D H 0.6113 -0.1055 0.5939 0.120 Uiso 0.40 1 calc PR J 2 C86A C 0.5413(18) -0.0500(11) 0.6394(14) 0.132(10) Uiso 0.40 1 d PD J 2 H86D H 0.5622 -0.0202 0.6612 0.197 Uiso 0.40 1 calc PR J 2 H86E H 0.4940 -0.0681 0.6577 0.197 Uiso 0.40 1 calc PR J 2 H86F H 0.5209 -0.0361 0.6054 0.197 Uiso 0.40 1 calc PR J 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0343(2) 0.0439(2) 0.0378(2) 0.00043(14) -0.00031(15) 0.00066(14) Cd2 0.0410(2) 0.0403(2) 0.0382(2) 0.00112(14) -0.00249(16) 0.00147(15) O1 0.0399(19) 0.0416(18) 0.049(2) 0.0018(16) 0.0016(16) 0.0019(16) O2 0.052(2) 0.0449(19) 0.045(2) 0.0035(15) 0.0056(16) 0.0114(16) O3 0.052(2) 0.065(2) 0.054(2) -0.0051(19) 0.0090(18) 0.0115(19) O4 0.047(2) 0.0391(19) 0.072(3) -0.0092(17) 0.0009(18) 0.0010(16) O5 0.050(2) 0.064(2) 0.060(2) -0.0170(19) 0.0003(18) -0.0163(19) O6 0.042(2) 0.055(2) 0.055(2) -0.0034(18) -0.0063(17) -0.0013(17) O7 0.0389(19) 0.060(2) 0.051(2) -0.0104(18) -0.0060(17) -0.0017(17) O8 0.050(2) 0.092(3) 0.047(2) -0.027(2) 0.0073(18) -0.019(2) O9 0.044(2) 0.049(2) 0.045(2) -0.0049(16) 0.0023(16) 0.0065(16) O10 0.044(2) 0.058(2) 0.0384(19) -0.0009(16) -0.0004(15) 0.0012(17) O11 0.066(3) 0.100(3) 0.042(2) -0.022(2) -0.0035(19) -0.006(2) O12 0.070(3) 0.061(2) 0.049(2) -0.0065(19) 0.0128(19) -0.017(2) O13 0.059(2) 0.042(2) 0.093(3) -0.012(2) -0.006(2) -0.0015(18) O14 0.043(2) 0.0414(19) 0.063(2) -0.0015(17) -0.0104(17) 0.0067(16) O15 0.049(2) 0.0449(19) 0.053(2) -0.0009(16) -0.0075(17) 0.0036(17) O16 0.053(2) 0.051(2) 0.049(2) -0.0117(17) -0.0089(17) 0.0077(17) O17 0.070(3) 0.094(3) 0.061(3) 0.027(2) 0.019(2) 0.027(3) O21 0.042(2) 0.049(2) 0.069(3) -0.0018(18) -0.0039(18) 0.0039(18) O22 0.090(4) 0.081(4) 0.164(6) 0.003(4) 0.003(4) -0.013(3) N1 0.091(8) 0.078(6) 0.049(5) 0.022(5) 0.011(5) -0.003(6) N2 0.048(3) 0.057(3) 0.047(3) 0.002(2) 0.003(2) 0.008(2) N4 0.070(4) 0.093(4) 0.069(4) 0.013(3) -0.002(3) 0.011(3) C1 0.034(3) 0.041(3) 0.045(3) -0.001(2) 0.000(2) -0.004(2) C2 0.035(3) 0.036(2) 0.045(3) 0.002(2) -0.002(2) -0.002(2) C3 0.038(3) 0.040(2) 0.042(3) 0.002(2) -0.001(2) 0.000(2) C4 0.037(3) 0.049(3) 0.042(3) 0.000(2) -0.002(2) -0.006(2) C5 0.032(2) 0.047(3) 0.047(3) -0.008(2) 0.002(2) -0.002(2) C6 0.101(10) 0.058(6) 0.073(8) -0.014(7) 0.023(7) 0.003(7) C7 0.139(14) 0.104(11) 0.113(12) -0.018(9) 0.001(10) -0.075(11) C8 0.31(4) 0.105(15) 0.14(3) -0.043(15) -0.05(2) -0.08(2) C9 0.035(3) 0.035(2) 0.048(3) 0.003(2) -0.002(2) -0.003(2) C10 0.034(3) 0.041(2) 0.044(3) 0.001(2) -0.003(2) -0.004(2) C11 0.042(3) 0.042(3) 0.058(3) 0.000(2) 0.004(2) 0.003(2) C12 0.041(3) 0.039(3) 0.048(3) 0.007(2) -0.004(2) 0.001(2) C13 0.041(3) 0.049(3) 0.043(3) 0.005(2) 0.003(2) 0.005(2) C14 0.057(3) 0.050(3) 0.041(3) 0.000(2) -0.003(2) 0.001(3) C15 0.041(3) 0.043(3) 0.051(3) 0.004(2) -0.010(2) -0.005(2) C16 0.039(3) 0.040(3) 0.054(3) 0.004(2) -0.004(2) 0.005(2) C17 0.041(3) 0.040(3) 0.055(3) -0.003(2) -0.006(2) 0.006(2) C18 0.082(5) 0.036(3) 0.109(6) -0.002(3) -0.007(4) 0.007(3) C19 0.121(7) 0.060(4) 0.141(8) -0.017(5) -0.023(6) 0.021(5) C20 0.158(10) 0.053(4) 0.204(13) -0.016(6) -0.035(9) 0.018(6) C21 0.036(3) 0.057(3) 0.065(4) -0.010(3) 0.001(2) 0.005(2) C22 0.029(2) 0.055(3) 0.052(3) -0.009(2) 0.007(2) 0.005(2) C23 0.033(3) 0.061(3) 0.047(3) -0.012(3) -0.002(2) 0.003(2) C24 0.031(2) 0.053(3) 0.038(3) -0.011(2) 0.003(2) 0.001(2) C25 0.028(2) 0.056(3) 0.045(3) -0.013(3) 0.002(2) 0.003(2) C26 0.034(3) 0.061(3) 0.042(3) -0.006(2) 0.008(2) -0.002(2) C27 0.026(2) 0.069(3) 0.039(3) -0.008(2) 0.004(2) -0.005(2) C28 0.033(3) 0.065(3) 0.050(3) -0.022(3) 0.008(2) -0.004(2) C29 0.077(4) 0.079(4) 0.107(5) -0.037(4) -0.014(4) -0.001(4) C30 0.102(5) 0.080(4) 0.140(6) -0.039(4) -0.034(5) -0.004(4) C31 0.146(9) 0.103(7) 0.236(11) -0.085(7) -0.048(9) 0.003(6) C32 0.045(3) 0.087(4) 0.038(3) -0.009(3) 0.007(2) -0.016(3) C33 0.044(3) 0.086(4) 0.031(3) 0.004(3) -0.005(2) -0.012(3) C34 0.046(3) 0.074(4) 0.053(3) 0.016(3) -0.009(3) -0.015(3) C35 0.050(3) 0.059(3) 0.076(4) 0.017(3) -0.003(3) -0.007(3) C36 0.040(3) 0.066(4) 0.067(4) 0.010(3) -0.004(3) 0.000(3) C37 0.044(3) 0.063(3) 0.033(3) 0.007(2) -0.009(2) -0.010(3) C38 0.045(3) 0.074(4) 0.030(3) 0.000(2) -0.007(2) -0.012(3) C39 0.234(11) 0.208(10) 0.066(5) -0.034(6) -0.024(6) -0.104(9) C40 0.236(10) 0.214(10) 0.085(6) -0.010(6) -0.031(6) -0.085(8) C41 0.177(10) 0.172(9) 0.062(5) -0.027(6) -0.023(6) 0.003(8) C42 0.036(3) 0.063(3) 0.040(3) 0.000(2) -0.001(2) -0.014(2) C43 0.069(8) 0.087(8) 0.058(7) 0.003(6) -0.004(6) -0.017(7) C44 0.089(11) 0.162(17) 0.077(11) 0.051(12) 0.001(9) 0.004(11) C45 0.096(11) 0.160(16) 0.099(11) 0.020(10) 0.050(9) 0.016(10) C46 0.046(3) 0.040(3) 0.039(3) -0.002(2) -0.002(2) 0.002(2) C47 0.052(3) 0.051(3) 0.039(3) -0.006(2) 0.000(2) -0.001(3) C48 0.045(3) 0.053(3) 0.040(3) -0.007(2) 0.003(2) 0.009(2) C49 0.051(3) 0.053(3) 0.048(3) -0.013(2) -0.004(2) 0.008(3) C50 0.059(4) 0.063(4) 0.040(3) -0.017(2) -0.003(3) -0.008(3) C54 0.055(3) 0.055(3) 0.044(3) -0.009(2) 0.005(3) -0.007(3) C55 0.045(3) 0.053(3) 0.049(3) -0.010(2) 0.000(2) -0.003(2) C56 0.050(3) 0.075(4) 0.045(3) -0.008(3) 0.009(3) -0.021(3) C57 0.038(3) 0.069(4) 0.045(3) -0.013(3) 0.003(2) -0.002(3) C58 0.069(4) 0.081(5) 0.057(4) -0.001(3) -0.007(3) 0.000(4) C59 0.091(5) 0.065(4) 0.073(5) 0.013(3) -0.010(4) 0.004(4) C60 0.063(4) 0.066(4) 0.068(4) -0.005(3) -0.014(3) 0.002(3) C61 0.036(3) 0.061(3) 0.053(3) -0.002(3) 0.005(2) 0.004(2) C62 0.031(3) 0.059(3) 0.056(3) -0.010(3) 0.012(2) -0.003(2) C63 0.105(7) 0.121(7) 0.080(5) 0.004(5) 0.036(5) -0.029(6) C64 0.091(16) 0.53(8) 0.22(3) 0.13(4) 0.063(19) -0.01(3) C65 0.15(3) 0.124(19) 0.38(6) -0.05(3) 0.19(4) -0.04(2) C66 0.050(3) 0.054(3) 0.057(3) -0.016(3) 0.006(3) -0.006(3) C67 0.053(3) 0.048(3) 0.047(3) -0.009(2) -0.002(2) 0.000(3) C68 0.053(3) 0.049(3) 0.040(3) -0.005(2) -0.006(2) 0.009(2) C69 0.042(3) 0.043(3) 0.043(3) -0.006(2) -0.011(2) 0.000(2) C70 0.047(3) 0.045(3) 0.042(3) 0.001(2) -0.012(2) 0.005(3) C71 0.046(3) 0.043(3) 0.054(3) -0.008(2) -0.014(2) 0.002(2) C72 0.048(3) 0.047(3) 0.054(3) -0.013(2) -0.015(2) 0.004(2) C73 0.056(3) 0.039(3) 0.059(3) -0.006(2) -0.012(3) 0.005(3) C74 0.117(7) 0.094(6) 0.165(8) 0.034(6) -0.013(6) 0.012(5) C75 0.117(7) 0.135(7) 0.171(8) 0.030(6) -0.002(6) 0.016(6) C76 0.145(9) 0.202(11) 0.165(10) 0.077(9) -0.015(8) 0.019(9) C77 0.050(3) 0.049(3) 0.067(4) -0.016(3) -0.017(3) 0.006(3) C78 0.039(3) 0.056(3) 0.065(4) -0.009(3) -0.003(3) 0.004(2) C79 0.060(4) 0.056(3) 0.078(4) 0.001(3) -0.004(3) -0.009(3) C80 0.074(4) 0.074(4) 0.055(4) 0.015(3) 0.001(3) 0.004(3) C81 0.055(3) 0.079(4) 0.047(3) -0.008(3) 0.006(3) 0.000(3) C82 0.035(3) 0.067(3) 0.039(3) -0.011(2) 0.006(2) 0.005(2) C83 0.034(3) 0.050(3) 0.047(3) -0.008(2) 0.001(2) 0.009(2) C84 0.046(7) 0.081(9) 0.074(9) 0.017(8) 0.003(6) 0.031(7) C85 0.110(12) 0.186(17) 0.072(9) 0.024(10) 0.003(8) 0.091(13) C86 0.14(2) 0.23(3) 0.26(4) 0.04(3) -0.04(2) 0.11(2) C87 0.054(3) 0.065(4) 0.049(3) -0.026(3) -0.006(3) 0.014(3) C88 0.048(3) 0.055(3) 0.056(3) 0.005(3) 0.007(3) 0.013(3) C89 0.064(4) 0.064(4) 0.059(4) 0.014(3) 0.000(3) 0.010(3) C90 0.049(3) 0.061(3) 0.050(3) -0.004(3) 0.000(3) 0.007(3) C91 0.120(8) 0.161(10) 0.095(7) -0.045(7) -0.043(6) 0.034(7) C92 0.072(5) 0.078(5) 0.081(5) 0.013(4) 0.011(4) 0.012(4) C93 0.069(5) 0.119(7) 0.174(10) -0.024(7) -0.024(6) 0.038(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 Cd1 O6 2.259(4) 3_657 ? Cd1 O17 2.285(4) . ? Cd1 O14 2.294(4) 2_756 ? Cd1 O9 2.307(3) . ? Cd1 O2 2.319(3) . ? Cd1 O1 2.456(3) . ? Cd2 O21 2.259(4) . ? Cd2 O1 2.270(3) 3_757 ? Cd2 O10 2.311(3) . ? Cd2 O7 2.317(4) 1_655 ? Cd2 O15 2.377(4) 2_756 ? Cd2 O14 2.405(4) 2_756 ? Cd2 O9 2.527(4) . ? Cd2 C70 2.742(5) 2_756 ? O1 C1 1.276(6) . ? O1 Cd2 2.270(3) 3_757 ? O2 C1 1.254(6) . ? O3 C5 1.374(6) . ? O3 C6 1.461(12) . ? O3 C6A 1.470(17) . ? O4 C17 1.384(6) . ? O4 C18 1.438(7) . ? O5 C28 1.372(7) . ? O5 C29 1.410(8) . ? O6 C25 1.260(7) . ? O6 Cd1 2.259(4) 3_657 ? O7 C25 1.260(6) . ? O7 Cd2 2.317(4) 1_455 ? O8 C38 1.363(7) . ? O8 C39 1.516(5) . ? O9 C46 1.277(6) . ? O10 C46 1.255(6) . ? O11 C50 1.378(7) . ? O11 C51A 1.52(2) . ? O11 C51 1.534(15) . ? O12 C62 1.376(7) . ? O12 C63 1.425(9) . ? O13 C73 1.372(7) . ? O13 C74 1.524(5) . ? O14 C70 1.275(6) . ? O14 Cd1 2.294(3) 2_746 ? O14 Cd2 2.405(4) 2_746 ? O15 C70 1.250(7) . ? O15 Cd2 2.377(4) 2_746 ? O16 C83 1.387(7) . ? O16 C84A 1.415(16) . ? O16 C84 1.435(10) . ? O17 C43A 0.99(2) . ? O17 C43 1.282(14) . ? O21 C88 1.261(7) . ? O22 C92 1.224(10) . ? N1 C43 1.340(14) . ? N1 C44 1.46(2) . ? N1 C45 1.517(18) . ? N2 C88 1.301(8) . ? N2 C90 1.458(8) . ? N2 C89 1.472(8) . ? N4 C92 1.332(10) . ? N4 C93 1.420(10) . ? N4 C91 1.421(12) . ? N1A C43A 1.33(3) . ? N1A C45A 1.49(3) . ? N1A C44A 1.71(6) . ? C1 C2 1.487(7) . ? C2 C10 1.385(7) . ? C2 C3 1.402(7) . ? C3 C4 1.385(7) . ? C3 H3 0.9500 . ? C4 C5 1.408(7) . ? C4 C42 1.524(7) . ? C5 C9 1.392(7) . ? C6 C7 1.537(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.540(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.379(7) . ? C9 C11 1.531(7) . ? C10 H10 0.9500 . ? C11 C12 1.522(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.370(7) . ? C12 C17 1.400(8) . ? C13 C14 1.386(8) . ? C13 H13 0.9500 . ? C14 C15 1.374(8) . ? C14 H14 0.9500 . ? C15 C16 1.397(7) . ? C15 H15 0.9500 . ? C16 C17 1.399(7) . ? C16 C21 1.528(7) . ? C18 C19 1.496(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.498(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.502(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.395(8) . ? C22 C28 1.410(8) . ? C23 C24 1.380(8) . ? C23 H23 0.9500 . ? C24 C26 1.382(7) . ? C24 C25 1.499(7) . ? C26 C27 1.377(8) . ? C26 H26 0.9500 . ? C27 C28 1.406(8) . ? C27 C32 1.500(8) . ? C29 C30 1.538(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.533(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.544(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.364(9) . ? C33 C38 1.408(8) . ? C34 C35 1.379(9) . ? C34 H34 0.9500 . ? C35 C36 1.410(9) . ? C35 H35 0.9500 . ? C36 C37 1.381(8) . ? C36 H36 0.9500 . ? C37 C38 1.391(8) . ? C37 C42 1.534(7) . ? C39 C40 1.271(13) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.520(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.472(7) . ? C47 C48 1.385(8) . ? C47 C55 1.410(7) . ? C48 C49 1.385(8) . ? C48 H48 0.9500 . ? C49 C50 1.408(8) . ? C49 C87 1.519(8) . ? C50 C54 1.385(9) . ? C51 C52 1.542(5) . ? C51 H51C 0.9900 . ? C51 H51D 0.9900 . ? C52 C53 1.539(5) . ? C52 H52C 0.9900 . ? C52 H52D 0.9900 . ? C53 H53D 0.9800 . ? C53 H53E 0.9800 . ? C53 H53F 0.9800 . ? C54 C55 1.393(8) . ? C54 C56 1.519(8) . ? C55 H55 0.9500 . ? C56 C57 1.521(8) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.362(9) . ? C57 C62 1.401(8) . ? C58 C59 1.395(10) . ? C58 H58 0.9500 . ? C59 C60 1.361(10) . ? C59 H59 0.9500 . ? C60 C61 1.406(9) . ? C60 H60 0.9500 . ? C61 C62 1.387(8) . ? C61 C66 1.520(8) . ? C63 C64A 1.532(5) . ? C63 C64 1.535(5) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.540(5) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.505(8) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.397(7) . ? C67 C73 1.410(8) . ? C68 C69 1.391(8) . ? C68 H68 0.9500 . ? C69 C71 1.393(7) . ? C69 C70 1.490(7) . ? C70 Cd2 2.742(5) 2_746 ? C71 C72 1.405(7) . ? C71 H71 0.9500 . ? C72 C73 1.389(8) . ? C72 C77 1.545(8) . ? C74 C75 1.529(5) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.539(5) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.498(8) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C83 1.394(8) . ? C78 C79 1.415(9) . ? C79 C80 1.375(9) . ? C79 H79 0.9500 . ? C80 C81 1.367(9) . ? C80 H80 0.9500 . ? C81 C82 1.396(9) . ? C81 H81 0.9500 . ? C82 C83 1.391(7) . ? C82 C87 1.502(8) . ? C84 C85 1.541(5) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.539(5) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88 0.9500 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92 0.9500 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C6A C7A 1.540(5) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.540(5) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C43A H43A 0.9500 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C45A H45D 0.9800 . ? C45A H45E 0.9800 . ? C45A H45F 0.9800 . ? C51A C52A 1.540(5) . ? C51A H51A 0.9900 . ? C51A H51B 0.9900 . ? C52A C53A 1.537(5) . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? C64A C65A 1.540(5) . ? C64A H64C 0.9900 . ? C64A H64D 0.9900 . ? C65A H65D 0.9800 . ? C65A H65E 0.9800 . ? C65A H65F 0.9800 . ? C84A C85A 1.539(5) . ? C84A H84C 0.9900 . ? C84A H84D 0.9900 . ? C85A C86A 1.543(5) . ? C85A H85C 0.9900 . ? C85A H85D 0.9900 . ? C86A H86D 0.9800 . ? C86A H86E 0.9800 . ? C86A H86F 0.9800 . ? 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 O6 Cd1 O17 90.93(18) 3_657 . ? O6 Cd1 O14 166.63(13) 3_657 2_756 ? O17 Cd1 O14 91.34(17) . 2_756 ? O6 Cd1 O9 91.37(13) 3_657 . ? O17 Cd1 O9 90.73(15) . . ? O14 Cd1 O9 75.43(13) 2_756 . ? O6 Cd1 O2 94.09(14) 3_657 . ? O17 Cd1 O2 88.10(15) . . ? O14 Cd1 O2 99.15(13) 2_756 . ? O9 Cd1 O2 174.43(13) . . ? O6 Cd1 O1 102.53(13) 3_657 . ? O17 Cd1 O1 140.86(15) . . ? O14 Cd1 O1 83.82(13) 2_756 . ? O9 Cd1 O1 124.92(12) . . ? O2 Cd1 O1 54.77(12) . . ? O21 Cd2 O1 84.97(13) . 3_757 ? O21 Cd2 O10 94.37(14) . . ? O1 Cd2 O10 99.66(13) 3_757 . ? O21 Cd2 O7 86.22(14) . 1_655 ? O1 Cd2 O7 81.51(13) 3_757 1_655 ? O10 Cd2 O7 178.73(14) . 1_655 ? O21 Cd2 O15 89.06(14) . 2_756 ? O1 Cd2 O15 168.64(13) 3_757 2_756 ? O10 Cd2 O15 90.41(13) . 2_756 ? O7 Cd2 O15 88.47(13) 1_655 2_756 ? O21 Cd2 O14 140.43(13) . 2_756 ? O1 Cd2 O14 127.34(12) 3_757 2_756 ? O10 Cd2 O14 100.63(13) . 2_756 ? O7 Cd2 O14 78.22(13) 1_655 2_756 ? O15 Cd2 O14 54.75(13) 2_756 2_756 ? O21 Cd2 O9 144.28(13) . . ? O1 Cd2 O9 84.76(12) 3_757 . ? O10 Cd2 O9 54.06(12) . . ? O7 Cd2 O9 125.73(12) 1_655 . ? O15 Cd2 O9 105.57(12) 2_756 . ? O14 Cd2 O9 69.57(12) 2_756 . ? O21 Cd2 C70 114.44(15) . 2_756 ? O1 Cd2 C70 153.04(14) 3_757 2_756 ? O10 Cd2 C70 97.36(14) . 2_756 ? O7 Cd2 C70 81.36(15) 1_655 2_756 ? O15 Cd2 C70 27.10(14) 2_756 2_756 ? O14 Cd2 C70 27.70(14) 2_756 2_756 ? O9 Cd2 C70 88.52(13) . 2_756 ? C1 O1 Cd2 136.8(3) . 3_757 ? C1 O1 Cd1 88.6(3) . . ? Cd2 O1 Cd1 106.03(13) 3_757 . ? C1 O2 Cd1 95.5(3) . . ? C5 O3 C6 114.8(6) . . ? C5 O3 C6A 112.5(10) . . ? C6 O3 C6A 34.8(8) . . ? C17 O4 C18 111.9(5) . . ? C28 O5 C29 112.9(4) . . ? C25 O6 Cd1 101.8(3) . 3_657 ? C25 O7 Cd2 139.9(3) . 1_455 ? C38 O8 C39 107.8(7) . . ? C46 O9 Cd1 135.8(3) . . ? C46 O9 Cd2 87.0(3) . . ? Cd1 O9 Cd2 102.52(13) . . ? C46 O10 Cd2 97.5(3) . . ? C50 O11 C51A 105.5(16) . . ? C50 O11 C51 113.1(9) . . ? C51A O11 C51 14(3) . . ? C62 O12 C63 114.0(6) . . ? C73 O13 C74 112.0(6) . . ? C70 O14 Cd1 144.4(3) . 2_746 ? C70 O14 Cd2 91.0(3) . 2_746 ? Cd1 O14 Cd2 106.80(14) 2_746 2_746 ? C70 O15 Cd2 92.9(3) . 2_746 ? C83 O16 C84A 124.0(14) . . ? C83 O16 C84 109.4(7) . . ? C84A O16 C84 18.0(12) . . ? C43A O17 C43 39.8(12) . . ? C43A O17 Cd1 143.8(14) . . ? C43 O17 Cd1 127.2(7) . . ? C88 O21 Cd2 122.8(3) . . ? C43 N1 C44 121.4(12) . . ? C43 N1 C45 118.7(13) . . ? C44 N1 C45 118.6(12) . . ? C88 N2 C90 121.4(5) . . ? C88 N2 C89 120.0(5) . . ? C90 N2 C89 118.1(5) . . ? C92 N4 C93 120.7(8) . . ? C92 N4 C91 121.8(7) . . ? C93 N4 C91 117.5(8) . . ? C43A N1A C45A 117(2) . . ? C43A N1A C44A 133(3) . . ? C45A N1A C44A 106(3) . . ? O2 C1 O1 120.8(4) . . ? O2 C1 C2 118.4(4) . . ? O1 C1 C2 120.8(4) . . ? C10 C2 C3 118.6(4) . . ? C10 C2 C1 120.5(4) . . ? C3 C2 C1 120.9(4) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 118.7(5) . . ? C3 C4 C42 119.4(5) . . ? C5 C4 C42 121.8(5) . . ? O3 C5 C9 119.8(5) . . ? O3 C5 C4 119.4(5) . . ? C9 C5 C4 120.7(4) . . ? O3 C6 C7 110.5(9) . . ? O3 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? O3 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 113.0(16) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C5 119.0(5) . . ? C10 C9 C11 119.8(5) . . ? C5 C9 C11 121.1(4) . . ? C9 C10 C2 121.8(5) . . ? C9 C10 H10 119.1 . . ? C2 C10 H10 119.1 . . ? C12 C11 C9 110.0(4) . . ? C12 C11 H11A 109.7 . . ? C9 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? C9 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C13 C12 C17 118.6(5) . . ? C13 C12 C11 120.4(5) . . ? C17 C12 C11 120.9(5) . . ? C12 C13 C14 121.8(5) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 118.8(5) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 121.8(5) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C17 117.6(5) . . ? C15 C16 C21 119.8(5) . . ? C17 C16 C21 122.5(5) . . ? O4 C17 C16 119.6(5) . . ? O4 C17 C12 119.5(5) . . ? C16 C17 C12 120.9(5) . . ? O4 C18 C19 109.0(7) . . ? O4 C18 H18A 109.9 . . ? C19 C18 H18A 109.9 . . ? O4 C18 H18B 109.9 . . ? C19 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C18 C19 C20 112.6(9) . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C16 110.8(4) . . ? C22 C21 H21A 109.5 . . ? C16 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C28 116.9(5) . . ? C23 C22 C21 122.3(5) . . ? C28 C22 C21 120.8(5) . . ? C24 C23 C22 122.2(5) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C26 119.1(5) . . ? C23 C24 C25 120.9(5) . . ? C26 C24 C25 120.0(5) . . ? O6 C25 O7 122.4(5) . . ? O6 C25 C24 118.0(5) . . ? O7 C25 C24 119.5(5) . . ? C27 C26 C24 121.9(5) . . ? C27 C26 H26 119.0 . . ? C24 C26 H26 119.0 . . ? C26 C27 C28 118.1(5) . . ? C26 C27 C32 121.1(5) . . ? C28 C27 C32 120.7(5) . . ? O5 C28 C27 119.9(5) . . ? O5 C28 C22 118.2(5) . . ? C27 C28 C22 121.8(5) . . ? O5 C29 C30 107.6(6) . . ? O5 C29 H29A 110.2 . . ? C30 C29 H29A 110.2 . . ? O5 C29 H29B 110.2 . . ? C30 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? C31 C30 C29 107.9(7) . . ? C31 C30 H30A 110.1 . . ? C29 C30 H30A 110.1 . . ? C31 C30 H30B 110.1 . . ? C29 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C27 C32 C33 109.9(4) . . ? C27 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? C27 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C38 119.2(6) . . ? C34 C33 C32 119.6(5) . . ? C38 C33 C32 120.9(6) . . ? C33 C34 C35 121.5(6) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C34 C35 C36 119.3(6) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 119.5(6) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.0(5) . . ? C36 C37 C42 117.8(5) . . ? C38 C37 C42 122.1(5) . . ? O8 C38 C37 120.1(5) . . ? O8 C38 C33 120.1(5) . . ? C37 C38 C33 119.8(6) . . ? C40 C39 O8 118.1(9) . . ? C40 C39 H39A 107.8 . . ? O8 C39 H39A 107.8 . . ? C40 C39 H39B 107.8 . . ? O8 C39 H39B 107.8 . . ? H39A C39 H39B 107.1 . . ? C39 C40 C41 112.7(11) . . ? C39 C40 H40A 109.0 . . ? C41 C40 H40A 109.0 . . ? C39 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 C37 111.2(4) . . ? C4 C42 H42A 109.4 . . ? C37 C42 H42A 109.4 . . ? C4 C42 H42B 109.4 . . ? C37 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? O17 C43 N1 121.6(12) . . ? O17 C43 H43 119.2 . . ? N1 C43 H43 119.2 . . ? N1 C44 H44A 109.5 . . ? N1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N1 C45 H45A 109.5 . . ? N1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O10 C46 O9 121.3(5) . . ? O10 C46 C47 118.9(5) . . ? O9 C46 C47 119.8(5) . . ? C48 C47 C55 119.3(5) . . ? C48 C47 C46 120.7(5) . . ? C55 C47 C46 120.1(5) . . ? C47 C48 C49 121.1(5) . . ? C47 C48 H48 119.5 . . ? C49 C48 H48 119.5 . . ? C48 C49 C50 118.5(5) . . ? C48 C49 C87 120.3(5) . . ? C50 C49 C87 121.1(5) . . ? O11 C50 C54 119.5(5) . . ? O11 C50 C49 118.7(5) . . ? C54 C50 C49 121.8(5) . . ? O11 C51 C52 106.6(16) . . ? O11 C51 H51C 110.4 . . ? C52 C51 H51C 110.4 . . ? O11 C51 H51D 110.4 . . ? C52 C51 H51D 110.4 . . ? H51C C51 H51D 108.6 . . ? C53 C52 C51 115(2) . . ? C53 C52 H52C 108.5 . . ? C51 C52 H52C 108.5 . . ? C53 C52 H52D 108.5 . . ? C51 C52 H52D 108.5 . . ? H52C C52 H52D 107.5 . . ? C50 C54 C55 118.3(5) . . ? C50 C54 C56 120.1(5) . . ? C55 C54 C56 121.3(5) . . ? C54 C55 C47 120.8(5) . . ? C54 C55 H55 119.6 . . ? C47 C55 H55 119.6 . . ? C54 C56 C57 110.9(4) . . ? C54 C56 H56A 109.4 . . ? C57 C56 H56A 109.4 . . ? C54 C56 H56B 109.4 . . ? C57 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C58 C57 C62 118.1(6) . . ? C58 C57 C56 120.1(5) . . ? C62 C57 C56 121.7(5) . . ? C57 C58 C59 121.8(6) . . ? C57 C58 H58 119.1 . . ? C59 C58 H58 119.1 . . ? C60 C59 C58 119.7(6) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 120.4(6) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? C62 C61 C60 118.5(6) . . ? C62 C61 C66 122.4(5) . . ? C60 C61 C66 119.0(5) . . ? O12 C62 C61 119.5(5) . . ? O12 C62 C57 119.2(5) . . ? C61 C62 C57 121.2(5) . . ? O12 C63 C64A 114.0(8) . . ? O12 C63 C64 114.4(9) . . ? C64A C63 C64 42.1(13) . . ? O12 C63 H63A 108.7 . . ? C64A C63 H63A 135.7 . . ? C64 C63 H63A 108.7 . . ? O12 C63 H63B 108.7 . . ? C64A C63 H63B 69.4 . . ? C64 C63 H63B 108.7 . . ? H63A C63 H63B 107.6 . . ? C63 C64 C65 104.1(15) . . ? C63 C64 H64A 110.9 . . ? C65 C64 H64A 110.9 . . ? C63 C64 H64B 110.9 . . ? C65 C64 H64B 110.9 . . ? H64A C64 H64B 108.9 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 C61 110.1(4) . . ? C67 C66 H66A 109.6 . . ? C61 C66 H66A 109.6 . . ? C67 C66 H66B 109.6 . . ? C61 C66 H66B 109.6 . . ? H66A C66 H66B 108.2 . . ? C68 C67 C73 117.9(5) . . ? C68 C67 C66 120.3(5) . . ? C73 C67 C66 121.4(5) . . ? C69 C68 C67 120.6(5) . . ? C69 C68 H68 119.7 . . ? C67 C68 H68 119.7 . . ? C68 C69 C71 120.6(5) . . ? C68 C69 C70 120.1(5) . . ? C71 C69 C70 119.3(5) . . ? O15 C70 O14 121.1(5) . . ? O15 C70 C69 119.3(5) . . ? O14 C70 C69 119.6(5) . . ? O15 C70 Cd2 60.0(3) . 2_746 ? O14 C70 Cd2 61.3(3) . 2_746 ? C69 C70 Cd2 174.8(4) . 2_746 ? C69 C71 C72 119.8(5) . . ? C69 C71 H71 120.1 . . ? C72 C71 H71 120.1 . . ? C73 C72 C71 118.8(5) . . ? C73 C72 C77 121.8(5) . . ? C71 C72 C77 119.3(5) . . ? O13 C73 C72 118.2(5) . . ? O13 C73 C67 119.7(5) . . ? C72 C73 C67 121.8(5) . . ? O13 C74 C75 108.1(7) . . ? O13 C74 H74A 110.1 . . ? C75 C74 H74A 110.1 . . ? O13 C74 H74B 110.1 . . ? C75 C74 H74B 110.1 . . ? H74A C74 H74B 108.4 . . ? C74 C75 C76 107.7(8) . . ? C74 C75 H75A 110.2 . . ? C76 C75 H75A 110.2 . . ? C74 C75 H75B 110.2 . . ? C76 C75 H75B 110.2 . . ? H75A C75 H75B 108.5 . . ? C78 C77 C72 109.3(4) . . ? C78 C77 H77A 109.8 . . ? C72 C77 H77A 109.8 . . ? C78 C77 H77B 109.8 . . ? C72 C77 H77B 109.8 . . ? H77A C77 H77B 108.3 . . ? C83 C78 C79 117.9(5) . . ? C83 C78 C77 122.3(5) . . ? C79 C78 C77 119.7(5) . . ? C80 C79 C78 119.3(6) . . ? C80 C79 H79 120.3 . . ? C78 C79 H79 120.3 . . ? C81 C80 C79 121.8(6) . . ? C81 C80 H80 119.1 . . ? C79 C80 H80 119.1 . . ? C80 C81 C82 120.6(6) . . ? C80 C81 H81 119.7 . . ? C82 C81 H81 119.7 . . ? C83 C82 C81 117.8(5) . . ? C83 C82 C87 122.5(5) . . ? C81 C82 C87 119.7(5) . . ? O16 C83 C82 119.3(5) . . ? O16 C83 C78 118.4(5) . . ? C82 C83 C78 122.3(5) . . ? O16 C84 C85 105.8(9) . . ? O16 C84 H84A 110.6 . . ? C85 C84 H84A 110.6 . . ? O16 C84 H84B 110.6 . . ? C85 C84 H84B 110.6 . . ? H84A C84 H84B 108.7 . . ? C86 C85 C84 111.5(13) . . ? C86 C85 H85A 109.3 . . ? C84 C85 H85A 109.3 . . ? C86 C85 H85B 109.3 . . ? C84 C85 H85B 109.3 . . ? H85A C85 H85B 108.0 . . ? C82 C87 C49 109.8(5) . . ? C82 C87 H87A 109.7 . . ? C49 C87 H87A 109.7 . . ? C82 C87 H87B 109.7 . . ? C49 C87 H87B 109.7 . . ? H87A C87 H87B 108.2 . . ? O21 C88 N2 124.1(5) . . ? O21 C88 H88 117.9 . . ? N2 C88 H88 117.9 . . ? N2 C89 H89A 109.5 . . ? N2 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? N2 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N2 C90 H90A 109.5 . . ? N2 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? N2 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N4 C91 H91A 109.5 . . ? N4 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? N4 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? O22 C92 N4 125.0(8) . . ? O22 C92 H92 117.5 . . ? N4 C92 H92 117.5 . . ? N4 C93 H93A 109.5 . . ? N4 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? N4 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O3 C6A C7A 110.9(16) . . ? O3 C6A H6A1 109.5 . . ? C7A C6A H6A1 109.5 . . ? O3 C6A H6A2 109.5 . . ? C7A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 108.0 . . ? C6A C7A C8A 99.8(19) . . ? C6A C7A H7A1 111.8 . . ? C8A C7A H7A1 111.8 . . ? C6A C7A H7A2 111.8 . . ? C8A C7A H7A2 111.8 . . ? H7A1 C7A H7A2 109.5 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? O17 C43A N1A 135(2) . . ? O17 C43A H43A 112.3 . . ? N1A C43A H43A 112.3 . . ? N1A C44A H44D 109.5 . . ? N1A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? N1A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? N1A C45A H45D 109.5 . . ? N1A C45A H45E 109.5 . . ? H45D C45A H45E 109.5 . . ? N1A C45A H45F 109.5 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? O11 C51A C52A 102.7(15) . . ? O11 C51A H51A 111.2 . . ? C52A C51A H51A 111.2 . . ? O11 C51A H51B 111.2 . . ? C52A C51A H51B 111.2 . . ? H51A C51A H51B 109.1 . . ? C53A C52A C51A 101.4(12) . . ? C53A C52A H52A 111.5 . . ? C51A C52A H52A 111.5 . . ? C53A C52A H52B 111.5 . . ? C51A C52A H52B 111.5 . . ? H52A C52A H52B 109.3 . . ? C52A C53A H53A 109.5 . . ? C52A C53A H53B 109.5 . . ? H53A C53A H53B 109.5 . . ? C52A C53A H53C 109.5 . . ? H53A C53A H53C 109.5 . . ? H53B C53A H53C 109.5 . . ? C63 C64A C65A 113(2) . . ? C63 C64A H64C 109.0 . . ? C65A C64A H64C 109.0 . . ? C63 C64A H64D 109.0 . . ? C65A C64A H64D 109.0 . . ? H64C C64A H64D 107.8 . . ? C64A C65A H65D 109.5 . . ? C64A C65A H65E 109.5 . . ? H65D C65A H65E 109.5 . . ? C64A C65A H65F 109.5 . . ? H65D C65A H65F 109.5 . . ? H65E C65A H65F 109.5 . . ? O16 C84A C85A 111.5(15) . . ? O16 C84A H84C 109.3 . . ? C85A C84A H84C 109.3 . . ? O16 C84A H84D 109.3 . . ? C85A C84A H84D 109.3 . . ? H84C C84A H84D 108.0 . . ? C84A C85A C86A 106.2(18) . . ? C84A C85A H85C 110.5 . . ? C86A C85A H85C 110.5 . . ? C84A C85A H85D 110.5 . . ? C86A C85A H85D 110.5 . . ? H85C C85A H85D 108.7 . . ? C85A C86A H86D 109.5 . . ? C85A C86A H86E 109.5 . . ? H86D C86A H86E 109.5 . . ? C85A C86A H86F 109.5 . . ? H86D C86A H86F 109.5 . . ? H86E C86A H86F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Cd1 O1 C1 -83.1(3) 3_657 . . . ? O17 Cd1 O1 C1 24.3(4) . . . . ? O14 Cd1 O1 C1 108.8(3) 2_756 . . . ? O9 Cd1 O1 C1 176.2(3) . . . . ? O2 Cd1 O1 C1 3.0(3) . . . . ? O6 Cd1 O1 Cd2 55.60(16) 3_657 . . 3_757 ? O17 Cd1 O1 Cd2 163.0(2) . . . 3_757 ? O14 Cd1 O1 Cd2 -112.47(15) 2_756 . . 3_757 ? O9 Cd1 O1 Cd2 -45.06(19) . . . 3_757 ? O2 Cd1 O1 Cd2 141.7(2) . . . 3_757 ? O6 Cd1 O2 C1 99.4(3) 3_657 . . . ? O17 Cd1 O2 C1 -169.8(3) . . . . ? O14 Cd1 O2 C1 -78.8(3) 2_756 . . . ? O9 Cd1 O2 C1 -91.8(13) . . . . ? O1 Cd1 O2 C1 -3.1(3) . . . . ? O6 Cd1 O9 C46 101.4(5) 3_657 . . . ? O17 Cd1 O9 C46 10.4(5) . . . . ? O14 Cd1 O9 C46 -80.7(5) 2_756 . . . ? O2 Cd1 O9 C46 -67.4(15) . . . . ? O1 Cd1 O9 C46 -152.3(4) . . . . ? O6 Cd1 O9 Cd2 -159.90(15) 3_657 . . . ? O17 Cd1 O9 Cd2 109.14(18) . . . . ? O14 Cd1 O9 Cd2 17.95(13) 2_756 . . . ? O2 Cd1 O9 Cd2 31.3(14) . . . . ? O1 Cd1 O9 Cd2 -53.56(18) . . . . ? O21 Cd2 O9 C46 -34.3(4) . . . . ? O1 Cd2 O9 C46 -108.2(3) 3_757 . . . ? O10 Cd2 O9 C46 -2.2(3) . . . . ? O7 Cd2 O9 C46 176.2(3) 1_655 . . . ? O15 Cd2 O9 C46 76.7(3) 2_756 . . . ? O14 Cd2 O9 C46 118.7(3) 2_756 . . . ? C70 Cd2 O9 C46 98.0(3) 2_756 . . . ? O21 Cd2 O9 Cd1 -170.67(18) . . . . ? O1 Cd2 O9 Cd1 115.49(14) 3_757 . . . ? O10 Cd2 O9 Cd1 -138.6(2) . . . . ? O7 Cd2 O9 Cd1 39.9(2) 1_655 . . . ? O15 Cd2 O9 Cd1 -59.68(16) 2_756 . . . ? O14 Cd2 O9 Cd1 -17.68(13) 2_756 . . . ? C70 Cd2 O9 Cd1 -38.37(16) 2_756 . . . ? O21 Cd2 O10 C46 164.1(3) . . . . ? O1 Cd2 O10 C46 78.5(3) 3_757 . . . ? O7 Cd2 O10 C46 -79(6) 1_655 . . . ? O15 Cd2 O10 C46 -106.8(3) 2_756 . . . ? O14 Cd2 O10 C46 -52.6(3) 2_756 . . . ? O9 Cd2 O10 C46 2.3(3) . . . . ? C70 Cd2 O10 C46 -80.5(3) 2_756 . . . ? O6 Cd1 O17 C43A 167(2) 3_657 . . . ? O14 Cd1 O17 C43A -27(2) 2_756 . . . ? O9 Cd1 O17 C43A -102(2) . . . . ? O2 Cd1 O17 C43A 72(2) . . . . ? O1 Cd1 O17 C43A 55(2) . . . . ? O6 Cd1 O17 C43 -140.1(9) 3_657 . . . ? O14 Cd1 O17 C43 26.8(9) 2_756 . . . ? O9 Cd1 O17 C43 -48.7(9) . . . . ? O2 Cd1 O17 C43 125.9(9) . . . . ? O1 Cd1 O17 C43 108.6(9) . . . . ? O1 Cd2 O21 C88 -145.0(4) 3_757 . . . ? O10 Cd2 O21 C88 115.6(4) . . . . ? O7 Cd2 O21 C88 -63.2(4) 1_655 . . . ? O15 Cd2 O21 C88 25.3(4) 2_756 . . . ? O14 Cd2 O21 C88 3.1(5) 2_756 . . . ? O9 Cd2 O21 C88 141.2(4) . . . . ? C70 Cd2 O21 C88 15.5(5) 2_756 . . . ? Cd1 O2 C1 O1 5.6(5) . . . . ? Cd1 O2 C1 C2 -175.7(4) . . . . ? Cd2 O1 C1 O2 -117.5(5) 3_757 . . . ? Cd1 O1 C1 O2 -5.3(5) . . . . ? Cd2 O1 C1 C2 63.9(6) 3_757 . . . ? Cd1 O1 C1 C2 176.0(4) . . . . ? O2 C1 C2 C10 4.1(7) . . . . ? O1 C1 C2 C10 -177.2(4) . . . . ? O2 C1 C2 C3 -176.4(4) . . . . ? O1 C1 C2 C3 2.2(7) . . . . ? C10 C2 C3 C4 -2.1(7) . . . . ? C1 C2 C3 C4 178.5(5) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C2 C3 C4 C42 176.7(4) . . . . ? C6 O3 C5 C9 -110.8(7) . . . . ? C6A O3 C5 C9 -72.7(10) . . . . ? C6 O3 C5 C4 73.3(7) . . . . ? C6A O3 C5 C4 111.4(10) . . . . ? C3 C4 C5 O3 179.3(4) . . . . ? C42 C4 C5 O3 3.0(7) . . . . ? C3 C4 C5 C9 3.5(7) . . . . ? C42 C4 C5 C9 -172.9(4) . . . . ? C5 O3 C6 C7 78.5(13) . . . . ? C6A O3 C6 C7 -15.8(19) . . . . ? O3 C6 C7 C8 -179(2) . . . . ? O3 C5 C9 C10 178.9(4) . . . . ? C4 C5 C9 C10 -5.3(7) . . . . ? O3 C5 C9 C11 -5.5(7) . . . . ? C4 C5 C9 C11 170.4(4) . . . . ? C5 C9 C10 C2 3.5(7) . . . . ? C11 C9 C10 C2 -172.2(4) . . . . ? C3 C2 C10 C9 0.2(7) . . . . ? C1 C2 C10 C9 179.6(4) . . . . ? C10 C9 C11 C12 90.4(6) . . . . ? C5 C9 C11 C12 -85.3(6) . . . . ? C9 C11 C12 C13 -67.9(6) . . . . ? C9 C11 C12 C17 108.3(5) . . . . ? C17 C12 C13 C14 0.2(8) . . . . ? C11 C12 C13 C14 176.5(5) . . . . ? C12 C13 C14 C15 -5.1(8) . . . . ? C13 C14 C15 C16 3.5(8) . . . . ? C14 C15 C16 C17 2.8(8) . . . . ? C14 C15 C16 C21 -174.0(5) . . . . ? C18 O4 C17 C16 -89.1(6) . . . . ? C18 O4 C17 C12 90.3(6) . . . . ? C15 C16 C17 O4 171.5(5) . . . . ? C21 C16 C17 O4 -11.8(8) . . . . ? C15 C16 C17 C12 -7.9(8) . . . . ? C21 C16 C17 C12 168.9(5) . . . . ? C13 C12 C17 O4 -172.9(5) . . . . ? C11 C12 C17 O4 10.8(8) . . . . ? C13 C12 C17 C16 6.4(8) . . . . ? C11 C12 C17 C16 -169.9(5) . . . . ? C17 O4 C18 C19 179.8(6) . . . . ? O4 C18 C19 C20 177.2(9) . . . . ? C15 C16 C21 C22 68.6(6) . . . . ? C17 C16 C21 C22 -108.1(6) . . . . ? C16 C21 C22 C23 -92.8(6) . . . . ? C16 C21 C22 C28 85.0(6) . . . . ? C28 C22 C23 C24 -0.3(7) . . . . ? C21 C22 C23 C24 177.5(5) . . . . ? C22 C23 C24 C26 -1.0(7) . . . . ? C22 C23 C24 C25 179.4(4) . . . . ? Cd1 O6 C25 O7 -8.3(5) 3_657 . . . ? Cd1 O6 C25 C24 169.9(3) 3_657 . . . ? Cd2 O7 C25 O6 -87.2(6) 1_455 . . . ? Cd2 O7 C25 C24 94.6(6) 1_455 . . . ? C23 C24 C25 O6 -176.5(4) . . . . ? C26 C24 C25 O6 3.9(7) . . . . ? C23 C24 C25 O7 1.7(7) . . . . ? C26 C24 C25 O7 -177.8(4) . . . . ? C23 C24 C26 C27 1.5(7) . . . . ? C25 C24 C26 C27 -178.9(4) . . . . ? C24 C26 C27 C28 -0.7(7) . . . . ? C24 C26 C27 C32 -176.9(5) . . . . ? C29 O5 C28 C27 -87.8(7) . . . . ? C29 O5 C28 C22 95.6(6) . . . . ? C26 C27 C28 O5 -177.0(4) . . . . ? C32 C27 C28 O5 -0.8(7) . . . . ? C26 C27 C28 C22 -0.6(7) . . . . ? C32 C27 C28 C22 175.6(5) . . . . ? C23 C22 C28 O5 177.6(4) . . . . ? C21 C22 C28 O5 -0.3(7) . . . . ? C23 C22 C28 C27 1.1(7) . . . . ? C21 C22 C28 C27 -176.8(5) . . . . ? C28 O5 C29 C30 175.9(7) . . . . ? O5 C29 C30 C31 -174.1(9) . . . . ? C26 C27 C32 C33 90.7(6) . . . . ? C28 C27 C32 C33 -85.3(6) . . . . ? C27 C32 C33 C34 -67.8(7) . . . . ? C27 C32 C33 C38 106.2(6) . . . . ? C38 C33 C34 C35 -2.1(8) . . . . ? C32 C33 C34 C35 171.9(5) . . . . ? C33 C34 C35 C36 -4.9(9) . . . . ? C34 C35 C36 C37 6.6(9) . . . . ? C35 C36 C37 C38 -1.3(8) . . . . ? C35 C36 C37 C42 -179.7(5) . . . . ? C39 O8 C38 C37 -96.5(8) . . . . ? C39 O8 C38 C33 84.4(8) . . . . ? C36 C37 C38 O8 175.1(5) . . . . ? C42 C37 C38 O8 -6.6(7) . . . . ? C36 C37 C38 C33 -5.8(8) . . . . ? C42 C37 C38 C33 172.6(5) . . . . ? C34 C33 C38 O8 -173.3(5) . . . . ? C32 C33 C38 O8 12.7(7) . . . . ? C34 C33 C38 C37 7.5(8) . . . . ? C32 C33 C38 C37 -166.5(5) . . . . ? C38 O8 C39 C40 123.5(16) . . . . ? O8 C39 C40 C41 167.1(13) . . . . ? C3 C4 C42 C37 -91.5(6) . . . . ? C5 C4 C42 C37 84.8(6) . . . . ? C36 C37 C42 C4 70.5(6) . . . . ? C38 C37 C42 C4 -107.9(6) . . . . ? C43A O17 C43 N1 -59(2) . . . . ? Cd1 O17 C43 N1 168.6(9) . . . . ? C44 N1 C43 O17 -3(2) . . . . ? C45 N1 C43 O17 -169.8(14) . . . . ? Cd2 O10 C46 O9 -4.3(5) . . . . ? Cd2 O10 C46 C47 176.9(4) . . . . ? Cd1 O9 C46 O10 108.8(5) . . . . ? Cd2 O9 C46 O10 3.9(5) . . . . ? Cd1 O9 C46 C47 -72.4(6) . . . . ? Cd2 O9 C46 C47 -177.3(4) . . . . ? O10 C46 C47 C48 -177.0(5) . . . . ? O9 C46 C47 C48 4.2(8) . . . . ? O10 C46 C47 C55 3.6(8) . . . . ? O9 C46 C47 C55 -175.2(5) . . . . ? C55 C47 C48 C49 -3.3(8) . . . . ? C46 C47 C48 C49 177.3(5) . . . . ? C47 C48 C49 C50 -0.9(8) . . . . ? C47 C48 C49 C87 174.1(5) . . . . ? C51A O11 C50 C54 -87(3) . . . . ? C51 O11 C50 C54 -74.0(10) . . . . ? C51A O11 C50 C49 96(3) . . . . ? C51 O11 C50 C49 109.2(10) . . . . ? C48 C49 C50 O11 -177.8(5) . . . . ? C87 C49 C50 O11 7.3(9) . . . . ? C48 C49 C50 C54 5.5(9) . . . . ? C87 C49 C50 C54 -169.5(6) . . . . ? C50 O11 C51 C52 -88.2(18) . . . . ? C51A O11 C51 C52 -28(5) . . . . ? O11 C51 C52 C53 163(2) . . . . ? O11 C50 C54 C55 177.7(5) . . . . ? C49 C50 C54 C55 -5.6(9) . . . . ? O11 C50 C54 C56 -8.0(9) . . . . ? C49 C50 C54 C56 168.6(5) . . . . ? C50 C54 C55 C47 1.2(8) . . . . ? C56 C54 C55 C47 -173.0(5) . . . . ? C48 C47 C55 C54 3.2(8) . . . . ? C46 C47 C55 C54 -177.4(5) . . . . ? C50 C54 C56 C57 -67.1(7) . . . . ? C55 C54 C56 C57 106.9(6) . . . . ? C54 C56 C57 C58 -57.0(8) . . . . ? C54 C56 C57 C62 119.9(6) . . . . ? C62 C57 C58 C59 -0.6(9) . . . . ? C56 C57 C58 C59 176.4(6) . . . . ? C57 C58 C59 C60 -1.9(11) . . . . ? C58 C59 C60 C61 0.1(11) . . . . ? C59 C60 C61 C62 4.0(9) . . . . ? C59 C60 C61 C66 -173.0(6) . . . . ? C63 O12 C62 C61 -79.6(7) . . . . ? C63 O12 C62 C57 103.0(6) . . . . ? C60 C61 C62 O12 176.2(5) . . . . ? C66 C61 C62 O12 -7.0(8) . . . . ? C60 C61 C62 C57 -6.5(8) . . . . ? C66 C61 C62 C57 170.3(5) . . . . ? C58 C57 C62 O12 -177.9(5) . . . . ? C56 C57 C62 O12 5.2(8) . . . . ? C58 C57 C62 C61 4.8(8) . . . . ? C56 C57 C62 C61 -172.1(5) . . . . ? C62 O12 C63 C64A -91.7(10) . . . . ? C62 O12 C63 C64 -138.1(16) . . . . ? O12 C63 C64 C65 163(2) . . . . ? C64A C63 C64 C65 64(2) . . . . ? C62 C61 C66 C67 -120.4(6) . . . . ? C60 C61 C66 C67 56.4(7) . . . . ? C61 C66 C67 C68 -103.3(6) . . . . ? C61 C66 C67 C73 69.8(7) . . . . ? C73 C67 C68 C69 -1.3(8) . . . . ? C66 C67 C68 C69 172.1(5) . . . . ? C67 C68 C69 C71 -5.3(8) . . . . ? C67 C68 C69 C70 175.6(5) . . . . ? Cd2 O15 C70 O14 -4.9(5) 2_746 . . . ? Cd2 O15 C70 C69 174.1(4) 2_746 . . . ? Cd1 O14 C70 O15 -116.5(6) 2_746 . . . ? Cd2 O14 C70 O15 4.9(5) 2_746 . . . ? Cd1 O14 C70 C69 64.4(8) 2_746 . . . ? Cd2 O14 C70 C69 -174.2(4) 2_746 . . . ? Cd1 O14 C70 Cd2 -121.4(6) 2_746 . . 2_746 ? C68 C69 C70 O15 -170.5(5) . . . . ? C71 C69 C70 O15 10.4(7) . . . . ? C68 C69 C70 O14 8.6(7) . . . . ? C71 C69 C70 O14 -170.5(5) . . . . ? C68 C69 C70 Cd2 -90(4) . . . 2_746 ? C71 C69 C70 Cd2 91(4) . . . 2_746 ? C68 C69 C71 C72 6.2(8) . . . . ? C70 C69 C71 C72 -174.7(5) . . . . ? C69 C71 C72 C73 -0.4(8) . . . . ? C69 C71 C72 C77 -176.5(5) . . . . ? C74 O13 C73 C72 -112.2(6) . . . . ? C74 O13 C73 C67 74.2(7) . . . . ? C71 C72 C73 O13 -179.8(5) . . . . ? C77 C72 C73 O13 -3.8(8) . . . . ? C71 C72 C73 C67 -6.4(8) . . . . ? C77 C72 C73 C67 169.7(5) . . . . ? C68 C67 C73 O13 -179.4(5) . . . . ? C66 C67 C73 O13 7.3(8) . . . . ? C68 C67 C73 C72 7.2(8) . . . . ? C66 C67 C73 C72 -166.1(5) . . . . ? C73 O13 C74 C75 84.3(10) . . . . ? O13 C74 C75 C76 177.4(10) . . . . ? C73 C72 C77 C78 -71.3(7) . . . . ? C71 C72 C77 C78 104.7(6) . . . . ? C72 C77 C78 C83 117.8(6) . . . . ? C72 C77 C78 C79 -57.9(7) . . . . ? C83 C78 C79 C80 -0.5(9) . . . . ? C77 C78 C79 C80 175.5(6) . . . . ? C78 C79 C80 C81 -2.9(10) . . . . ? C79 C80 C81 C82 1.8(10) . . . . ? C80 C81 C82 C83 2.6(8) . . . . ? C80 C81 C82 C87 -175.7(6) . . . . ? C84A O16 C83 C82 -74.0(13) . . . . ? C84 O16 C83 C82 -85.8(10) . . . . ? C84A O16 C83 C78 109.3(13) . . . . ? C84 O16 C83 C78 97.4(10) . . . . ? C81 C82 C83 O16 177.3(5) . . . . ? C87 C82 C83 O16 -4.5(7) . . . . ? C81 C82 C83 C78 -6.1(8) . . . . ? C87 C82 C83 C78 172.2(5) . . . . ? C79 C78 C83 O16 -178.3(5) . . . . ? C77 C78 C83 O16 5.9(8) . . . . ? C79 C78 C83 C82 5.0(8) . . . . ? C77 C78 C83 C82 -170.8(5) . . . . ? C83 O16 C84 C85 169.5(11) . . . . ? C84A O16 C84 C85 23(5) . . . . ? O16 C84 C85 C86 -178(2) . . . . ? C83 C82 C87 C49 -122.0(5) . . . . ? C81 C82 C87 C49 56.2(7) . . . . ? C48 C49 C87 C82 -105.5(6) . . . . ? C50 C49 C87 C82 69.4(7) . . . . ? Cd2 O21 C88 N2 136.3(5) . . . . ? C90 N2 C88 O21 -175.8(5) . . . . ? C89 N2 C88 O21 -3.5(8) . . . . ? C93 N4 C92 O22 2.8(13) . . . . ? C91 N4 C92 O22 -177.8(9) . . . . ? C5 O3 C6A C7A -87.6(19) . . . . ? C6 O3 C6A C7A 13.8(15) . . . . ? O3 C6A C7A C8A -177(2) . . . . ? C43 O17 C43A N1A 91(4) . . . . ? Cd1 O17 C43A N1A 178.2(16) . . . . ? C45A N1A C43A O17 -174(3) . . . . ? C44A N1A C43A O17 -22(5) . . . . ? C50 O11 C51A C52A -156(4) . . . . ? C51 O11 C51A C52A 80(6) . . . . ? O11 C51A C52A C53A 174(4) . . . . ? O12 C63 C64A C65A -174(2) . . . . ? C64 C63 C64A C65A -74(3) . . . . ? C83 O16 C84A C85A -71(3) . . . . ? C84 O16 C84A C85A -32(5) . . . . ? O16 C84A C85A C86A 175(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.163 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.122 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.218 0.113 157 21 ' ' 2 0.000 0.282 0.613 157 20 ' ' 3 0.000 0.718 0.387 157 21 ' ' 4 0.000 0.782 0.887 157 20 ' ' 5 0.341 0.049 0.731 126 18 ' ' 6 0.341 0.451 0.231 126 18 ' ' 7 0.448 0.254 0.859 26 2 ' ' 8 0.448 0.246 0.359 26 2 ' ' 9 0.659 0.549 0.769 126 18 ' ' 10 0.659 0.951 0.269 126 18 ' ' 11 0.552 0.754 0.641 26 2 ' ' 12 0.552 0.746 0.141 26 2 ' ' #===end data_p10adb2 _database_code_depnum_ccdc_archive 'CCDC 866581' #TrackingRef '- calix-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H125 Co2.50 N4 O23' _chemical_formula_weight 1850.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _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 13.7658(3) _cell_length_b 16.0409(5) _cell_length_c 22.3491(10) _cell_angle_alpha 104.894(3) _cell_angle_beta 89.547(3) _cell_angle_gamma 92.223(2) _cell_volume 4765.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9254 _cell_measurement_theta_min 2.9237 _cell_measurement_theta_max 27.5238 _exptl_crystal_description tabloid _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1961 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_T_min 0.84060 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Atlas (Gemini ultra Mo) ; _diffrn_detector_area_resol_mean 10.3795 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31341 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.1159 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.37 _reflns_number_total 18857 _reflns_number_gt 9096 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; 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. Tricky structure to refine in the way that calixarene pendant groups often exhibit disorder. 2 data collections were effected in order to get optimal data. Asymmetric unit contains 2.5 x cobalt centres (Co1 located at an inversion centre), 2 fully deprotonated calixarene ligands, 2 DMFs, and a mixture of oxygens/hydroxide anions (O1, O2 and O3). Core is well resolved, with the exception of the hydroxide/water hydrogens atoms. The latter could not be credibly located and hence were omitted from the refinement. One of the DMFs exhibited disorder of 3 atoms therein - namely C89, C90 and C91 - in a 50:50 ratio. The electron density is generally smeared in the calixarene pendant group regions. The extent of this smearing led to disorder modeling for C35, C36 and C42. A considerable number of distance restraints pertaining to the n-propoxy groups plus some ADP restraints were necessary in order to facilitate convergence of this structure. Based on residual electron density and void volume calculations, it was evident that the lattice contained some diffuse solvent. This has been included as 2 molecules of DMF per asymmetric unit following implementation of PLATON SQUEEZE.. ; _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^)+(0.1416P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18857 _refine_ls_number_parameters 1044 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2299 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.000 _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 Co1 Co 0.0000 0.0000 0.0000 0.0373(3) Uani 1 2 d S . . Co2 Co -0.27513(4) -0.01990(4) 0.00835(3) 0.0365(2) Uani 1 1 d . . . Co3 Co -0.49821(4) -0.09455(4) 0.00515(3) 0.0385(2) Uani 1 1 d . . . O1 O 0.0546(2) 0.11003(19) 0.06593(16) 0.0455(9) Uani 1 1 d . . . O2 O -0.1272(2) -0.01919(19) 0.05482(16) 0.0400(8) Uani 1 1 d . . . O3 O -0.4104(2) -0.01275(17) -0.02791(15) 0.0359(8) Uani 1 1 d . . . O4 O -0.0710(2) 0.07690(19) -0.04464(17) 0.0433(9) Uani 1 1 d . . . O5 O -0.2146(2) 0.00470(18) -0.06885(15) 0.0387(8) Uani 1 1 d . . . O6 O -0.4107(2) 0.80246(18) -0.01954(18) 0.0491(10) Uani 1 1 d . . . O7 O -0.2621(2) 0.85079(18) -0.03951(17) 0.0449(9) Uani 1 1 d . . . O8 O -0.2359(3) 0.2621(3) -0.2396(3) 0.0802(14) Uani 1 1 d D . . O9 O -0.4626(3) 0.3285(2) -0.23800(19) 0.0622(12) Uani 1 1 d D B . O10 O -0.2898(3) 0.4799(2) -0.23067(18) 0.0570(11) Uani 1 1 d D . . O11 O -0.0605(2) 0.4083(2) -0.25690(15) 0.0457(9) Uani 1 1 d D . . O12 O -0.3186(2) -0.0440(2) 0.09080(16) 0.0479(9) Uani 1 1 d . . . O13 O -0.4793(2) -0.06669(19) 0.09785(16) 0.0429(9) Uani 1 1 d . . . O14 O -0.4078(3) 0.1609(2) 0.05575(18) 0.0588(11) Uani 1 1 d . . . O15 O -0.2594(2) 0.10908(19) 0.05943(16) 0.0455(9) Uani 1 1 d . . . O16 O -0.3645(4) 0.0257(3) 0.38111(19) 0.0788(14) Uani 1 1 d D . . O17 O -0.2101(3) 0.1697(3) 0.3380(2) 0.0785(14) Uani 1 1 d D . . O18 O -0.2958(3) 0.3620(2) 0.32955(18) 0.0676(12) Uani 1 1 d D . . O19 O -0.4608(4) 0.2084(3) 0.3497(2) 0.0781(14) Uani 1 1 d D . . O20 O -0.0255(3) 0.2642(2) 0.0920(2) 0.0742(14) Uani 1 1 d . . . O21 O -0.1375(3) 0.8332(3) 0.0930(2) 0.0768(13) Uani 1 1 d . . . N1 N -0.1551(4) 0.3272(3) 0.0652(3) 0.0681(15) Uani 1 1 d . . . N2 N -0.2355(4) 0.7109(3) 0.0779(3) 0.0639(14) Uani 1 1 d . . . C1 C -0.1509(3) 0.0621(3) -0.0729(2) 0.0377(13) Uani 1 1 d . . . C2 C -0.1736(3) 0.1158(3) -0.1174(3) 0.0416(13) Uani 1 1 d . . . C3 C -0.0994(4) 0.1603(3) -0.1394(3) 0.0436(13) Uani 1 1 d . . . H3 H -0.0345 0.1571 -0.1263 0.052 Uiso 1 1 calc R . . C4 C -0.1191(4) 0.2102(3) -0.1806(3) 0.0500(15) Uani 1 1 d . . . C5 C -0.2153(4) 0.2138(3) -0.1979(3) 0.0553(16) Uani 1 1 d . . . C6 C -0.2920(4) 0.1748(3) -0.1726(3) 0.0559(16) Uani 1 1 d . . . C7 C -0.2700(4) 0.1236(3) -0.1328(3) 0.0462(14) Uani 1 1 d . . . H7 H -0.3206 0.0943 -0.1163 0.055 Uiso 1 1 calc R . . C8 C -0.3973(4) 0.1945(3) -0.1836(3) 0.0653(19) Uani 1 1 d . . . H8A H -0.4074 0.1896 -0.2282 0.078 Uiso 1 1 calc R . . H8B H -0.4418 0.1518 -0.1714 0.078 Uiso 1 1 calc R . . C9 C -0.4206(3) 0.2852(3) -0.1462(3) 0.0537(16) Uani 1 1 d . . . C10 C -0.4462(3) 0.3488(3) -0.1757(3) 0.0445(14) Uani 1 1 d . . . C11 C -0.4555(3) 0.4357(3) -0.1413(3) 0.0430(13) Uani 1 1 d . . . C12 C -0.4438(4) 0.4547(4) -0.0774(3) 0.0609(17) Uani 1 1 d . . . H12 H -0.4495 0.5125 -0.0535 0.073 Uiso 1 1 calc R . . C13 C -0.4238(5) 0.3907(5) -0.0473(3) 0.075(2) Uani 1 1 d . . . H13 H -0.4192 0.4043 -0.0035 0.090 Uiso 1 1 calc R . . C14 C -0.4109(4) 0.3071(4) -0.0827(3) 0.0651(18) Uani 1 1 d . . . H14 H -0.3949 0.2639 -0.0627 0.078 Uiso 1 1 calc R . . C15 C -0.4715(4) 0.5081(3) -0.1713(3) 0.0482(14) Uani 1 1 d . . . H15A H -0.5330 0.5360 -0.1560 0.058 Uiso 1 1 calc R . . H15B H -0.4773 0.4844 -0.2167 0.058 Uiso 1 1 calc R . . C16 C -0.3884(4) 0.5747(3) -0.1572(3) 0.0473(14) Uani 1 1 d . . . C17 C -0.2981(4) 0.5558(3) -0.1859(3) 0.0491(14) Uani 1 1 d . . . C18 C -0.2168(4) 0.6100(3) -0.1676(3) 0.0472(14) Uani 1 1 d . . . C19 C -0.2275(4) 0.6870(3) -0.1222(3) 0.0471(14) Uani 1 1 d . . . H19 H -0.1724 0.7249 -0.1098 0.057 Uiso 1 1 calc R . . C20 C -0.3169(4) 0.7093(3) -0.0948(2) 0.0442(13) Uani 1 1 d . . . C21 C -0.3965(4) 0.6515(3) -0.1123(3) 0.0477(14) Uani 1 1 d . . . H21 H -0.4576 0.6653 -0.0930 0.057 Uiso 1 1 calc R . . C22 C -0.3308(4) 0.7936(3) -0.0479(3) 0.0430(13) Uani 1 1 d . . . C23 C -0.1153(4) 0.5795(3) -0.1888(3) 0.0507(15) Uani 1 1 d . . . H23A H -0.1143 0.5571 -0.2344 0.061 Uiso 1 1 calc R . . H23B H -0.0673 0.6285 -0.1770 0.061 Uiso 1 1 calc R . . C24 C -0.0894(3) 0.5093(3) -0.1586(2) 0.0411(13) Uani 1 1 d . . . C25 C -0.0671(3) 0.4265(3) -0.1919(3) 0.0425(13) Uani 1 1 d . . . C26 C -0.0540(4) 0.3602(3) -0.1635(3) 0.0448(13) Uani 1 1 d . . . C27 C -0.0597(5) 0.3792(4) -0.1003(3) 0.0685(18) Uani 1 1 d . . . H27 H -0.0519 0.3345 -0.0800 0.082 Uiso 1 1 calc R . . C28 C -0.0766(5) 0.4614(4) -0.0655(3) 0.076(2) Uani 1 1 d . . . H28 H -0.0768 0.4741 -0.0215 0.091 Uiso 1 1 calc R . . C29 C -0.0935(4) 0.5264(4) -0.0956(3) 0.0641(18) Uani 1 1 d . . . H29 H -0.1078 0.5827 -0.0719 0.077 Uiso 1 1 calc R . . C30 C -0.0406(4) 0.2665(3) -0.1998(3) 0.0538(15) Uani 1 1 d . . . H30A H -0.0451 0.2614 -0.2448 0.065 Uiso 1 1 calc R . . H30B H 0.0243 0.2479 -0.1910 0.065 Uiso 1 1 calc R . . C31 C -0.2295(12) 0.1996(8) -0.3040(4) 0.251(7) Uani 1 1 d DU . . H31A H -0.1624 0.1989 -0.3203 0.301 Uiso 1 1 calc R . . H31B H -0.2506 0.1403 -0.3029 0.301 Uiso 1 1 calc R . . C32 C -0.2988(14) 0.2360(11) -0.3430(4) 0.284(8) Uani 1 1 d DU . . H32A H -0.2738 0.2923 -0.3483 0.341 Uiso 1 1 calc R . . H32B H -0.3642 0.2431 -0.3241 0.341 Uiso 1 1 calc R . . C33 C -0.3016(14) 0.1674(11) -0.4049(5) 0.300(13) Uani 1 1 d D . . H33A H -0.3554 0.1780 -0.4302 0.449 Uiso 1 1 calc R . . H33B H -0.3111 0.1101 -0.3975 0.449 Uiso 1 1 calc R . . H33C H -0.2401 0.1703 -0.4269 0.449 Uiso 1 1 calc R . . C34 C -0.5621(6) 0.3127(6) -0.2523(3) 0.127(4) Uani 1 1 d D . . H34A H -0.5996 0.3604 -0.2268 0.152 Uiso 0.60 1 calc PR A 1 H34B H -0.5845 0.2586 -0.2420 0.152 Uiso 0.60 1 calc PR A 1 H34C H -0.5705 0.2977 -0.2978 0.152 Uiso 0.40 1 calc PR A 2 H34D H -0.5974 0.3660 -0.2346 0.152 Uiso 0.40 1 calc PR A 2 C35 C -0.5814(6) 0.3049(11) -0.3202(4) 0.121(5) Uiso 0.60 1 d PD B 1 H35A H -0.5443 0.2578 -0.3469 0.145 Uiso 0.60 1 calc PR B 1 H35B H -0.5640 0.3596 -0.3312 0.145 Uiso 0.60 1 calc PR B 1 C36 C -0.6920(6) 0.2842(9) -0.3266(5) 0.102(4) Uiso 0.60 1 d PD B 1 H36A H -0.7112 0.2745 -0.3701 0.152 Uiso 0.60 1 calc PR B 1 H36B H -0.7270 0.3328 -0.3012 0.152 Uiso 0.60 1 calc PR B 1 H36C H -0.7078 0.2322 -0.3126 0.152 Uiso 0.60 1 calc PR B 1 C37 C -0.2733(6) 0.4938(6) -0.2913(4) 0.142(4) Uani 1 1 d DU . . H37A H -0.2189 0.4587 -0.3115 0.170 Uiso 1 1 calc R . . H37B H -0.2551 0.5553 -0.2872 0.170 Uiso 1 1 calc R . . C38 C -0.3634(6) 0.4693(8) -0.3307(3) 0.174(4) Uani 1 1 d DU . . H38A H -0.4160 0.5095 -0.3150 0.209 Uiso 1 1 calc R . . H38B H -0.3869 0.4097 -0.3322 0.209 Uiso 1 1 calc R . . C39 C -0.3277(9) 0.4769(9) -0.3955(3) 0.174(5) Uani 1 1 d DU . . H39A H -0.3811 0.4600 -0.4254 0.261 Uiso 1 1 calc R . . H39B H -0.2734 0.4387 -0.4090 0.261 Uiso 1 1 calc R . . H39C H -0.3061 0.5367 -0.3929 0.261 Uiso 1 1 calc R . . C40 C 0.0344(5) 0.4217(4) -0.2790(2) 0.0662(18) Uani 1 1 d D D . H40A H 0.0810 0.3878 -0.2624 0.079 Uiso 1 1 calc R . . H40B H 0.0546 0.4835 -0.2644 0.079 Uiso 1 1 calc R . . C41 C 0.0363(6) 0.3945(5) -0.3492(2) 0.098(3) Uani 1 1 d D . . H41A H 0.0964 0.4169 -0.3652 0.118 Uiso 0.55 1 calc PR C 1 H41B H -0.0207 0.4157 -0.3668 0.118 Uiso 0.55 1 calc PR C 1 H41C H -0.0079 0.3436 -0.3653 0.118 Uiso 0.45 1 calc PR C 2 H41D H 0.1029 0.3800 -0.3644 0.118 Uiso 0.45 1 calc PR C 2 C42 C 0.0333(12) 0.2953(5) -0.3652(5) 0.123(6) Uani 0.55 1 d PD D 1 H42A H 0.0323 0.2722 -0.4103 0.184 Uiso 0.55 1 calc PR D 1 H42B H -0.0253 0.2746 -0.3474 0.184 Uiso 0.55 1 calc PR D 1 H42C H 0.0910 0.2758 -0.3481 0.184 Uiso 0.55 1 calc PR D 1 C43 C -0.3956(4) -0.0490(3) 0.1199(2) 0.0448(13) Uani 1 1 d D . . C44 C -0.3891(4) -0.0301(3) 0.1895(2) 0.0469(14) Uani 1 1 d D . . C45 C -0.2930(4) -0.0313(3) 0.2192(3) 0.0594(16) Uani 1 1 d D . . H45 H -0.2359 -0.0435 0.1949 0.071 Uiso 1 1 calc R . . C46 C -0.2890(5) -0.0144(4) 0.2818(3) 0.0622(17) Uani 1 1 d . . . C47 C -0.3726(5) 0.0061(3) 0.3172(3) 0.0612(17) Uani 1 1 d . . . C48 C -0.4624(5) 0.0114(3) 0.2901(3) 0.0562(16) Uani 1 1 d . . . C49 C -0.4680(4) -0.0087(3) 0.2261(3) 0.0496(14) Uani 1 1 d . . . H49 H -0.5294 -0.0075 0.2072 0.059 Uiso 1 1 calc R . . C50 C -0.5527(5) 0.0451(4) 0.3279(3) 0.071(2) Uani 1 1 d . . . H50A H -0.6021 -0.0025 0.3246 0.085 Uiso 1 1 calc R . . H50B H -0.5351 0.0682 0.3721 0.085 Uiso 1 1 calc R . . C51 C -0.5934(5) 0.1154(4) 0.3029(3) 0.0625(18) Uani 1 1 d . . . C52 C -0.6739(5) 0.1004(4) 0.2627(4) 0.077(2) Uani 1 1 d . . . H52 H -0.7119 0.0482 0.2568 0.092 Uiso 1 1 calc R . . C53 C -0.6983(5) 0.1603(5) 0.2319(4) 0.082(2) Uani 1 1 d . . . H53 H -0.7544 0.1509 0.2061 0.098 Uiso 1 1 calc R . . C54 C -0.6396(5) 0.2357(4) 0.2387(3) 0.0684(19) Uani 1 1 d . . . H54 H -0.6556 0.2761 0.2162 0.082 Uiso 1 1 calc R . . C55 C -0.5597(4) 0.2528(3) 0.2770(3) 0.0580(17) Uani 1 1 d . . . C56 C -0.5392(5) 0.1937(4) 0.3112(3) 0.0604(17) Uani 1 1 d . . . C57 C -0.4882(4) 0.3273(3) 0.2766(3) 0.0584(16) Uani 1 1 d . . . H57A H -0.4716 0.3586 0.3198 0.070 Uiso 1 1 calc R . . H57B H -0.5190 0.3682 0.2568 0.070 Uiso 1 1 calc R . . C59 C -0.3044(4) 0.3093(3) 0.2684(3) 0.0529(15) Uani 1 1 d D . . C60 C -0.2215(4) 0.2716(3) 0.2389(3) 0.0524(15) Uani 1 1 d . . . C61 C -0.2314(4) 0.2215(3) 0.1793(3) 0.0503(15) Uani 1 1 d . . . H61 H -0.1760 0.1943 0.1586 0.060 Uiso 1 1 calc R . . C62 C -0.3191(4) 0.2094(3) 0.1488(3) 0.0444(14) Uani 1 1 d . . . C63 C -0.4018(4) 0.2457(3) 0.1813(3) 0.0478(14) Uani 1 1 d . . . H63 H -0.4634 0.2359 0.1613 0.057 Uiso 1 1 calc R . . C64 C -0.3953(4) 0.2951(3) 0.2415(3) 0.0494(14) Uani 1 1 d . . . C65 C -0.3291(4) 0.1555(3) 0.0834(2) 0.0449(14) Uani 1 1 d . . . C66 C -0.1226(4) 0.2788(4) 0.2711(3) 0.0640(18) Uani 1 1 d . . . H66A H -0.0754 0.3112 0.2512 0.077 Uiso 1 1 calc R . . H66B H -0.1288 0.3108 0.3151 0.077 Uiso 1 1 calc R . . C67 C -0.0862(5) 0.1902(4) 0.2671(3) 0.0619(17) Uani 1 1 d . . . C68 C -0.0127(5) 0.1550(4) 0.2266(3) 0.0728(19) Uani 1 1 d . . . H68 H 0.0230 0.1907 0.2057 0.087 Uiso 1 1 calc R . . C69 C 0.0096(6) 0.0696(5) 0.2161(4) 0.084(2) Uani 1 1 d . . . H69 H 0.0615 0.0474 0.1892 0.101 Uiso 1 1 calc R . . C70 C -0.0435(6) 0.0164(5) 0.2448(3) 0.081(2) Uani 1 1 d . . . H70 H -0.0293 -0.0430 0.2369 0.097 Uiso 1 1 calc R . . C71 C -0.1175(5) 0.0493(4) 0.2852(3) 0.0695(18) Uani 1 1 d . . . C72 C -0.1349(4) 0.1370(4) 0.2978(3) 0.0621(17) Uani 1 1 d . . . C73 C -0.1874(6) -0.0101(4) 0.3110(3) 0.080(2) Uani 1 1 d . . . H73A H -0.1616 -0.0688 0.3020 0.096 Uiso 1 1 calc R . . H73B H -0.1922 0.0122 0.3565 0.096 Uiso 1 1 calc R . . C74 C -0.3765(10) -0.0448(7) 0.4067(3) 0.150(4) Uani 1 1 d DU . . H74A H -0.3352 -0.0922 0.3847 0.180 Uiso 1 1 calc R . . H74B H -0.4451 -0.0663 0.4030 0.180 Uiso 1 1 calc R . . C75 C -0.3466(11) -0.0145(6) 0.4759(3) 0.178(4) Uani 1 1 d DU . . H75A H -0.2774 0.0054 0.4806 0.214 Uiso 1 1 calc R . . H75B H -0.3876 0.0325 0.4989 0.214 Uiso 1 1 calc R . . C76 C -0.3641(15) -0.0963(8) 0.4979(5) 0.277(8) Uani 1 1 d DU . . H76A H -0.3447 -0.0851 0.5414 0.415 Uiso 1 1 calc R . . H76B H -0.3255 -0.1427 0.4728 0.415 Uiso 1 1 calc R . . H76C H -0.4332 -0.1138 0.4937 0.415 Uiso 1 1 calc R . . C77 C -0.1910(9) 0.1781(6) 0.4059(5) 0.179(6) Uani 1 1 d D . . H77A H -0.1432 0.1359 0.4110 0.214 Uiso 1 1 calc R . . H77B H -0.2518 0.1681 0.4273 0.214 Uiso 1 1 calc R . . C78 C -0.1511(12) 0.2695(7) 0.4316(4) 0.218(7) Uani 1 1 d D . . H78A H -0.1950 0.3119 0.4221 0.262 Uiso 1 1 calc R . . H78B H -0.0859 0.2777 0.4145 0.262 Uiso 1 1 calc R . . C79 C -0.1460(13) 0.2783(9) 0.5021(3) 0.251(10) Uani 1 1 d D . . H79A H -0.1218 0.3366 0.5233 0.376 Uiso 1 1 calc R . . H79B H -0.1019 0.2359 0.5101 0.376 Uiso 1 1 calc R . . H79C H -0.2110 0.2680 0.5175 0.376 Uiso 1 1 calc R . . C80 C -0.4869(14) 0.2660(9) 0.4081(4) 0.222(6) Uani 1 1 d DU . . H80A H -0.5576 0.2753 0.4088 0.267 Uiso 1 1 calc R . . H80B H -0.4522 0.3226 0.4130 0.267 Uiso 1 1 calc R . . C81 C -0.4605(14) 0.2284(8) 0.4606(3) 0.232(6) Uani 1 1 d DU . . H81A H -0.3896 0.2207 0.4616 0.278 Uiso 1 1 calc R . . H81B H -0.4948 0.1718 0.4567 0.278 Uiso 1 1 calc R . . C82 C -0.4934(12) 0.2948(9) 0.5192(4) 0.226(7) Uani 1 1 d DU . . H82A H -0.4745 0.2765 0.5559 0.340 Uiso 1 1 calc R . . H82B H -0.5642 0.2989 0.5184 0.340 Uiso 1 1 calc R . . H82C H -0.4624 0.3513 0.5206 0.340 Uiso 1 1 calc R . . C83 C -0.2864(6) 0.4530(3) 0.3318(3) 0.097(3) Uani 1 1 d DU . . H83A H -0.3444 0.4711 0.3131 0.117 Uiso 1 1 calc R . . H83B H -0.2283 0.4646 0.3084 0.117 Uiso 1 1 calc R . . C84 C -0.2767(6) 0.5032(4) 0.4001(3) 0.120(3) Uani 1 1 d DU . . H84A H -0.2279 0.4774 0.4214 0.144 Uiso 1 1 calc R . . H84B H -0.2569 0.5643 0.4036 0.144 Uiso 1 1 calc R . . C85 C -0.3769(8) 0.4967(7) 0.4278(4) 0.177(5) Uani 1 1 d DU . . H85A H -0.3755 0.5275 0.4718 0.266 Uiso 1 1 calc R . . H85B H -0.3956 0.4358 0.4235 0.266 Uiso 1 1 calc R . . H85C H -0.4242 0.5225 0.4062 0.266 Uiso 1 1 calc R . . C86 C -0.0914(5) 0.2674(4) 0.0549(3) 0.0664(19) Uani 1 1 d . . . H86 H -0.0954 0.2238 0.0170 0.080 Uiso 1 1 calc R . . C87 C -0.1565(5) 0.3964(4) 0.1214(3) 0.076(2) Uani 1 1 d . . . H87A H -0.2097 0.4344 0.1192 0.114 Uiso 1 1 calc R . . H87B H -0.0945 0.4296 0.1259 0.114 Uiso 1 1 calc R . . H87C H -0.1663 0.3721 0.1571 0.114 Uiso 1 1 calc R . . C88 C -0.2325(6) 0.3217(5) 0.0219(4) 0.091(2) Uani 1 1 d . . . H88A H -0.2735 0.3716 0.0359 0.136 Uiso 1 1 calc R . . H88B H -0.2718 0.2685 0.0190 0.136 Uiso 1 1 calc R . . H88C H -0.2054 0.3212 -0.0189 0.136 Uiso 1 1 calc R . . C89 C -0.1727(12) 0.7681(10) 0.0626(8) 0.078(4) Uiso 0.50 1 d P E 3 H89 H -0.1535 0.7537 0.0204 0.094 Uiso 0.60 1 calc PR E 3 C90 C -0.2714(15) 0.6334(11) 0.0404(8) 0.109(6) Uiso 0.50 1 d P E 3 H90A H -0.3145 0.6046 0.0646 0.163 Uiso 0.60 1 calc PR E 3 H90B H -0.2173 0.5963 0.0241 0.163 Uiso 0.60 1 calc PR E 3 H90C H -0.3079 0.6444 0.0059 0.163 Uiso 0.60 1 calc PR E 3 C91 C -0.2655(15) 0.7325(12) 0.1419(9) 0.120(6) Uiso 0.50 1 d P E 3 H91A H -0.3102 0.6870 0.1489 0.181 Uiso 0.60 1 calc PR E 3 H91B H -0.2984 0.7875 0.1515 0.181 Uiso 0.60 1 calc PR E 3 H91C H -0.2083 0.7377 0.1686 0.181 Uiso 0.60 1 calc PR E 3 C35A C -0.6060(9) 0.2402(13) -0.2275(13) 0.150 Uiso 0.40 1 d PD B 2 H35C H -0.5914 0.2496 -0.1829 0.180 Uiso 0.40 1 calc PR B 2 H35D H -0.5818 0.1836 -0.2504 0.180 Uiso 0.40 1 calc PR B 2 C36A C -0.7164(8) 0.2458(19) -0.2385(17) 0.205 Uiso 0.40 1 d PD B 2 H36D H -0.7526 0.2043 -0.2207 0.307 Uiso 0.40 1 calc PR B 2 H36E H -0.7293 0.2325 -0.2831 0.307 Uiso 0.40 1 calc PR B 2 H36F H -0.7370 0.3043 -0.2188 0.307 Uiso 0.40 1 calc PR B 2 C42A C 0.0022(13) 0.4728(9) -0.3693(5) 0.113(7) Uani 0.45 1 d PD D 2 H42D H 0.0001 0.4593 -0.4146 0.169 Uiso 0.45 1 calc PR D 2 H42E H 0.0475 0.5221 -0.3535 0.169 Uiso 0.45 1 calc PR D 2 H42F H -0.0628 0.4872 -0.3526 0.169 Uiso 0.45 1 calc PR D 2 C89A C -0.2185(10) 0.7927(8) 0.0809(5) 0.053(3) Uiso 0.50 1 d P E 1 H89A H -0.2719 0.8245 0.0734 0.063 Uiso 0.40 1 calc PR E 1 C90A C -0.1614(15) 0.6492(12) 0.0718(9) 0.118(6) Uiso 0.50 1 d P E 1 H90D H -0.1913 0.5924 0.0708 0.177 Uiso 0.40 1 calc PR E 1 H90E H -0.1167 0.6669 0.1071 0.177 Uiso 0.40 1 calc PR E 1 H90F H -0.1254 0.6459 0.0333 0.177 Uiso 0.40 1 calc PR E 1 C91A C -0.3350(10) 0.6721(8) 0.0639(6) 0.069(3) Uiso 0.50 1 d P E 1 H91D H -0.3349 0.6106 0.0629 0.103 Uiso 0.40 1 calc PR E 1 H91E H -0.3558 0.6784 0.0235 0.103 Uiso 0.40 1 calc PR E 1 H91F H -0.3799 0.7015 0.0959 0.103 Uiso 0.40 1 calc PR E 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 Co1 0.0216(5) 0.0235(4) 0.0634(7) 0.0051(4) 0.0051(4) 0.0008(3) Co2 0.0217(3) 0.0262(3) 0.0538(4) -0.0028(3) 0.0057(3) -0.0037(2) Co3 0.0227(3) 0.0270(3) 0.0560(5) -0.0062(3) 0.0056(3) -0.0057(2) O1 0.035(2) 0.0353(17) 0.060(2) 0.0011(16) 0.0040(17) 0.0028(14) O2 0.0216(17) 0.0390(17) 0.057(2) 0.0082(15) 0.0005(15) -0.0014(13) O3 0.0192(16) 0.0257(15) 0.057(2) 0.0015(14) 0.0054(15) -0.0039(12) O4 0.0239(18) 0.0309(17) 0.073(3) 0.0095(16) -0.0016(17) -0.0008(13) O5 0.0274(18) 0.0285(16) 0.056(2) 0.0043(15) 0.0053(15) -0.0060(13) O6 0.031(2) 0.0264(16) 0.081(3) -0.0018(16) 0.0097(18) -0.0031(13) O7 0.0278(18) 0.0240(16) 0.073(2) -0.0038(16) 0.0109(17) -0.0049(13) O8 0.056(3) 0.064(3) 0.127(4) 0.038(3) -0.021(3) -0.008(2) O9 0.048(2) 0.043(2) 0.083(3) -0.009(2) -0.033(2) 0.0055(17) O10 0.061(3) 0.0330(19) 0.064(3) -0.0106(18) 0.001(2) 0.0041(16) O11 0.042(2) 0.0400(18) 0.052(2) 0.0062(16) 0.0060(17) 0.0060(15) O12 0.0284(19) 0.061(2) 0.052(2) 0.0130(18) 0.0028(17) -0.0087(16) O13 0.0286(19) 0.0385(18) 0.053(2) -0.0018(16) 0.0059(16) -0.0073(14) O14 0.039(2) 0.042(2) 0.076(3) -0.0215(19) -0.011(2) 0.0030(16) O15 0.0296(18) 0.0308(17) 0.061(2) -0.0141(16) 0.0037(16) -0.0028(14) O16 0.110(4) 0.067(3) 0.054(3) 0.008(2) 0.003(3) -0.002(2) O17 0.067(3) 0.075(3) 0.077(3) -0.010(2) 0.003(2) -0.003(2) O18 0.072(3) 0.048(2) 0.067(3) -0.015(2) 0.006(2) -0.0004(19) O19 0.104(4) 0.057(3) 0.064(3) 0.001(2) -0.003(3) -0.006(2) O20 0.050(3) 0.031(2) 0.122(4) -0.015(2) -0.001(3) 0.0018(17) O21 0.039(2) 0.074(3) 0.128(4) 0.046(3) -0.012(2) -0.010(2) N1 0.055(3) 0.044(3) 0.097(4) 0.003(3) -0.010(3) -0.003(2) N2 0.045(3) 0.054(3) 0.096(4) 0.025(3) 0.004(3) 0.002(2) C1 0.031(3) 0.018(2) 0.057(3) -0.003(2) 0.015(2) 0.0038(19) C2 0.029(3) 0.017(2) 0.070(4) -0.003(2) 0.005(2) 0.0045(18) C3 0.030(3) 0.030(2) 0.066(4) 0.004(3) 0.002(3) 0.005(2) C4 0.035(3) 0.029(3) 0.083(4) 0.011(3) 0.003(3) 0.000(2) C5 0.052(4) 0.022(2) 0.089(5) 0.009(3) -0.009(3) 0.000(2) C6 0.034(3) 0.028(3) 0.096(5) -0.001(3) -0.007(3) 0.000(2) C7 0.034(3) 0.022(2) 0.077(4) 0.003(3) -0.002(3) -0.002(2) C8 0.036(3) 0.031(3) 0.130(6) 0.020(3) -0.025(3) -0.006(2) C9 0.018(3) 0.033(3) 0.110(5) 0.020(3) 0.000(3) -0.002(2) C10 0.022(3) 0.030(3) 0.076(4) 0.004(3) -0.007(3) -0.0095(19) C11 0.025(3) 0.032(3) 0.069(4) 0.006(2) -0.006(2) -0.0002(19) C12 0.047(4) 0.051(3) 0.078(5) 0.004(3) 0.007(3) 0.013(3) C13 0.075(5) 0.087(5) 0.070(4) 0.027(4) 0.019(4) 0.038(4) C14 0.052(4) 0.066(4) 0.085(5) 0.033(4) 0.018(4) 0.019(3) C15 0.035(3) 0.029(2) 0.076(4) 0.005(3) -0.013(3) -0.001(2) C16 0.040(3) 0.027(2) 0.070(4) 0.004(2) -0.004(3) -0.004(2) C17 0.051(3) 0.025(2) 0.064(4) -0.003(2) 0.001(3) 0.004(2) C18 0.043(3) 0.031(3) 0.062(4) 0.001(2) 0.010(3) 0.001(2) C19 0.032(3) 0.028(2) 0.074(4) 0.001(2) 0.004(3) -0.007(2) C20 0.043(3) 0.022(2) 0.061(3) 0.000(2) 0.009(3) -0.001(2) C21 0.033(3) 0.033(3) 0.072(4) 0.005(3) 0.006(3) -0.001(2) C22 0.032(3) 0.032(3) 0.062(4) 0.008(2) 0.001(3) -0.003(2) C23 0.048(3) 0.032(3) 0.062(4) -0.004(2) 0.017(3) -0.005(2) C24 0.032(3) 0.038(3) 0.048(3) 0.003(2) 0.006(2) -0.011(2) C25 0.028(3) 0.040(3) 0.056(3) 0.007(3) 0.005(2) -0.007(2) C26 0.035(3) 0.040(3) 0.060(4) 0.014(3) -0.001(3) -0.007(2) C27 0.082(5) 0.053(4) 0.073(5) 0.022(3) -0.012(4) -0.020(3) C28 0.092(5) 0.079(5) 0.050(4) 0.009(4) 0.000(4) -0.035(4) C29 0.060(4) 0.052(3) 0.068(4) -0.004(3) 0.011(3) -0.019(3) C30 0.045(3) 0.045(3) 0.074(4) 0.020(3) 0.007(3) 0.006(2) C31 0.35(2) 0.262(15) 0.207(14) 0.164(11) 0.022(13) 0.103(14) C32 0.35(2) 0.289(16) 0.240(15) 0.108(12) 0.053(14) 0.114(14) C33 0.35(3) 0.32(2) 0.169(15) -0.031(15) -0.005(16) -0.12(2) C34 0.086(6) 0.162(9) 0.117(7) 0.014(6) -0.039(5) -0.052(6) C37 0.129(8) 0.099(6) 0.160(9) -0.038(6) -0.014(7) 0.011(6) C38 0.167(9) 0.138(7) 0.194(9) -0.002(7) 0.023(8) 0.007(7) C39 0.180(11) 0.215(11) 0.112(8) 0.024(8) 0.002(8) -0.040(9) C40 0.061(4) 0.063(4) 0.066(4) 0.003(3) 0.019(3) -0.004(3) C41 0.102(7) 0.092(6) 0.086(6) -0.001(5) 0.034(5) 0.003(5) C42 0.108(13) 0.177(17) 0.064(9) -0.009(10) 0.022(9) 0.043(12) C43 0.034(3) 0.035(3) 0.059(4) 0.000(2) 0.007(3) -0.003(2) C44 0.045(3) 0.036(3) 0.056(4) 0.007(2) 0.003(3) -0.011(2) C45 0.060(4) 0.044(3) 0.065(4) -0.002(3) 0.002(3) -0.007(3) C46 0.070(4) 0.048(3) 0.060(4) -0.001(3) -0.003(3) 0.000(3) C47 0.081(5) 0.038(3) 0.059(4) 0.003(3) 0.005(4) -0.008(3) C48 0.063(4) 0.039(3) 0.062(4) 0.006(3) 0.011(3) -0.011(3) C49 0.047(3) 0.036(3) 0.061(4) 0.006(3) 0.009(3) -0.009(2) C50 0.084(5) 0.050(3) 0.066(4) -0.004(3) 0.028(4) -0.014(3) C51 0.067(5) 0.047(3) 0.070(4) 0.009(3) 0.033(4) 0.004(3) C52 0.060(5) 0.055(4) 0.108(6) 0.008(4) 0.035(4) -0.006(3) C53 0.043(4) 0.077(5) 0.120(6) 0.018(5) 0.015(4) -0.001(3) C54 0.052(4) 0.057(4) 0.094(5) 0.014(3) 0.023(4) 0.013(3) C55 0.051(4) 0.043(3) 0.070(4) -0.003(3) 0.024(3) 0.010(3) C56 0.058(4) 0.053(4) 0.060(4) -0.005(3) 0.013(3) 0.004(3) C57 0.057(4) 0.039(3) 0.071(4) -0.001(3) 0.017(3) 0.007(2) C59 0.059(4) 0.031(3) 0.057(4) -0.008(2) 0.012(3) -0.004(2) C60 0.045(3) 0.039(3) 0.061(4) -0.008(3) -0.003(3) -0.008(2) C61 0.036(3) 0.035(3) 0.067(4) -0.009(3) 0.006(3) -0.005(2) C62 0.035(3) 0.025(2) 0.063(4) -0.005(2) 0.002(3) -0.007(2) C63 0.037(3) 0.032(3) 0.067(4) 0.000(3) 0.005(3) -0.001(2) C64 0.049(3) 0.025(2) 0.066(4) -0.002(2) 0.010(3) 0.000(2) C65 0.044(3) 0.023(2) 0.056(3) -0.009(2) 0.004(3) -0.005(2) C66 0.046(4) 0.062(4) 0.067(4) -0.014(3) -0.009(3) -0.009(3) C67 0.054(4) 0.057(4) 0.063(4) -0.006(3) -0.009(3) -0.006(3) C68 0.058(4) 0.075(4) 0.074(5) -0.002(4) -0.001(4) 0.000(3) C69 0.069(5) 0.086(5) 0.085(5) -0.004(4) -0.001(4) 0.022(4) C70 0.073(5) 0.068(4) 0.086(5) -0.012(4) -0.012(4) 0.017(4) C71 0.067(4) 0.063(4) 0.068(4) -0.001(3) -0.016(4) -0.004(3) C72 0.052(4) 0.063(4) 0.056(4) -0.013(3) -0.009(3) 0.003(3) C73 0.093(6) 0.064(4) 0.072(5) -0.006(3) -0.020(4) 0.018(4) C74 0.256(12) 0.130(7) 0.069(5) 0.032(5) 0.021(7) 0.025(7) C75 0.291(12) 0.162(8) 0.093(6) 0.051(6) 0.033(7) 0.021(8) C76 0.369(19) 0.309(17) 0.158(12) 0.069(12) 0.057(13) 0.040(16) C77 0.156(11) 0.181(12) 0.145(11) -0.057(9) 0.039(9) 0.021(9) C78 0.26(2) 0.185(14) 0.176(14) -0.008(11) -0.017(13) -0.030(13) C79 0.35(2) 0.293(19) 0.061(7) -0.033(9) -0.001(10) -0.095(17) C80 0.285(14) 0.204(12) 0.141(10) -0.031(9) -0.044(11) 0.053(10) C81 0.297(14) 0.211(11) 0.152(10) -0.024(9) 0.002(11) 0.050(10) C82 0.283(16) 0.203(12) 0.143(10) -0.041(9) 0.013(11) -0.021(12) C83 0.126(6) 0.045(4) 0.094(5) -0.026(3) 0.029(5) -0.028(4) C84 0.153(7) 0.061(4) 0.116(6) -0.027(4) 0.048(5) -0.021(4) C85 0.240(13) 0.114(8) 0.144(9) -0.028(7) 0.021(9) -0.003(8) C86 0.051(4) 0.037(3) 0.097(5) -0.007(3) -0.003(4) -0.005(3) C87 0.060(4) 0.039(3) 0.116(6) -0.004(3) -0.005(4) 0.001(3) C88 0.078(5) 0.077(5) 0.107(6) 0.007(4) -0.020(5) -0.008(4) C42A 0.101(15) 0.107(14) 0.108(15) -0.011(12) 0.041(12) -0.012(11) _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 Co1 O4 2.053(3) . ? Co1 O4 2.053(3) 2 ? Co1 O1 2.105(3) . ? Co1 O1 2.105(3) 2 ? Co1 O2 2.187(3) . ? Co1 O2 2.187(3) 2 ? Co2 O5 2.032(3) . ? Co2 O3 2.055(3) . ? Co2 O12 2.058(4) . ? Co2 O7 2.089(3) 1_545 ? Co2 O15 2.094(3) . ? Co2 O2 2.291(3) . ? Co3 O14 1.958(4) 2_455 ? Co3 O13 2.021(4) . ? Co3 O3 2.023(3) . ? Co3 O6 2.040(3) 1_545 ? Co3 O3 2.124(3) 2_455 ? O3 Co3 2.124(3) 2_455 ? O4 C1 1.256(6) . ? O5 C1 1.267(5) . ? O6 C22 1.259(6) . ? O6 Co3 2.040(3) 1_565 ? O7 C22 1.272(5) . ? O7 Co2 2.089(3) 1_565 ? O8 C5 1.395(7) . ? O8 C31 1.531(5) . ? O9 C10 1.365(7) . ? O9 C34 1.407(8) . ? O10 C17 1.370(6) . ? O10 C37 1.443(10) . ? O11 C25 1.408(6) . ? O11 C40 1.422(6) . ? O12 C43 1.250(6) . ? O13 C43 1.250(6) . ? O14 C65 1.268(6) . ? O14 Co3 1.958(4) 2_455 ? O15 C65 1.267(6) . ? O16 C47 1.387(7) . ? O16 C74 1.397(9) . ? O17 C72 1.392(7) . ? O17 C77 1.512(12) . ? O18 C59 1.413(6) . ? O18 C83 1.449(7) . ? O19 C56 1.361(8) . ? O19 C80 1.443(11) . ? O20 C86 1.245(8) . ? O21 C89 1.179(15) . ? O21 C89A 1.264(13) . ? N1 C86 1.300(8) . ? N1 C88 1.430(9) . ? N1 C87 1.447(7) . ? N2 C89A 1.308(12) . ? N2 C89 1.341(16) . ? N2 C90 1.385(17) . ? N2 C90A 1.43(2) . ? N2 C91 1.443(18) . ? N2 C91A 1.485(14) . ? C1 C2 1.515(8) . ? C2 C3 1.380(7) . ? C2 C7 1.392(7) . ? C3 C4 1.401(8) . ? C3 H3 0.9500 . ? C4 C5 1.391(8) . ? C4 C30 1.512(7) . ? C5 C6 1.395(8) . ? C6 C7 1.399(8) . ? C6 C8 1.530(8) . ? C7 H7 0.9500 . ? C8 C9 1.525(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.377(9) . ? C9 C10 1.406(8) . ? C10 C11 1.418(7) . ? C11 C12 1.391(8) . ? C11 C15 1.506(8) . ? C12 C13 1.399(9) . ? C12 H12 0.9500 . ? C13 C14 1.388(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.512(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.382(7) . ? C16 C17 1.401(7) . ? C17 C18 1.388(7) . ? C18 C19 1.394(7) . ? C18 C23 1.529(7) . ? C19 C20 1.389(7) . ? C19 H19 0.9500 . ? C20 C21 1.398(7) . ? C20 C22 1.501(6) . ? C21 H21 0.9500 . ? C23 C24 1.509(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.365(8) . ? C24 C25 1.390(7) . ? C25 C26 1.390(8) . ? C26 C27 1.369(8) . ? C26 C30 1.531(7) . ? C27 C28 1.375(9) . ? C27 H27 0.9500 . ? C28 C29 1.406(10) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.527(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.530(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35A 1.514(5) . ? C34 C35 1.516(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 H34C 0.9900 . ? C34 H34D 0.9900 . ? C35 C36 1.545(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.506(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.558(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.516(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42A 1.530(5) . ? C41 C42 1.537(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 H41C 0.9900 . ? C41 H41D 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.508(4) . ? C44 C49 1.355(7) . ? C44 C45 1.487(4) . ? C45 C46 1.358(8) . ? C45 H45 0.9500 . ? C46 C47 1.392(9) . ? C46 C73 1.539(9) . ? C47 C48 1.395(9) . ? C48 C49 1.386(8) . ? C48 C50 1.534(8) . ? C49 H49 0.9500 . ? C50 C51 1.508(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.407(10) . ? C51 C56 1.407(8) . ? C52 C53 1.370(11) . ? C52 H52 0.9500 . ? C53 C54 1.403(9) . ? C53 H53 0.9500 . ? C54 C55 1.374(9) . ? C54 H54 0.9500 . ? C55 C56 1.400(9) . ? C55 C57 1.519(8) . ? C57 C64 1.532(7) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C59 C64 1.377(8) . ? C59 C60 1.393(7) . ? C60 C61 1.372(7) . ? C60 C66 1.532(8) . ? C61 C62 1.374(7) . ? C61 H61 0.9500 . ? C62 C63 1.409(7) . ? C62 C65 1.497(7) . ? C63 C64 1.376(7) . ? C63 H63 0.9500 . ? C66 C67 1.505(9) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C72 1.379(9) . ? C67 C68 1.388(8) . ? C68 C69 1.376(9) . ? C68 H68 0.9500 . ? C69 C70 1.379(10) . ? C69 H69 0.9500 . ? C70 C71 1.382(9) . ? C70 H70 0.9500 . ? C71 C72 1.392(9) . ? C71 C73 1.539(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.550(5) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.526(5) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.513(5) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.548(5) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.503(5) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.537(5) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.535(5) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.519(5) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86 0.9500 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89 0.9500 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C35A C36A 1.552(5) . ? C35A H35C 0.9900 . ? C35A H35D 0.9900 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C89A H89A 0.9500 . ? C90A H90D 0.9800 . ? C90A H90E 0.9800 . ? C90A H90F 0.9800 . ? C91A H91D 0.9800 . ? C91A H91E 0.9800 . ? C91A H91F 0.9800 . ? 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 O4 Co1 O4 180.0 . 2 ? O4 Co1 O1 90.39(13) . . ? O4 Co1 O1 89.61(13) 2 . ? O4 Co1 O1 89.61(13) . 2 ? O4 Co1 O1 90.39(13) 2 2 ? O1 Co1 O1 180.0 . 2 ? O4 Co1 O2 93.57(13) . . ? O4 Co1 O2 86.43(13) 2 . ? O1 Co1 O2 94.72(12) . . ? O1 Co1 O2 85.28(12) 2 . ? O4 Co1 O2 86.43(13) . 2 ? O4 Co1 O2 93.57(13) 2 2 ? O1 Co1 O2 85.28(12) . 2 ? O1 Co1 O2 94.72(12) 2 2 ? O2 Co1 O2 180.0 . 2 ? O5 Co2 O3 89.04(13) . . ? O5 Co2 O12 172.67(14) . . ? O3 Co2 O12 98.26(13) . . ? O5 Co2 O7 84.33(13) . 1_545 ? O3 Co2 O7 93.21(12) . 1_545 ? O12 Co2 O7 95.84(14) . 1_545 ? O5 Co2 O15 93.19(13) . . ? O3 Co2 O15 97.52(12) . . ? O12 Co2 O15 85.26(14) . . ? O7 Co2 O15 168.95(13) 1_545 . ? O5 Co2 O2 93.00(13) . . ? O3 Co2 O2 175.67(11) . . ? O12 Co2 O2 79.67(13) . . ? O7 Co2 O2 90.79(12) 1_545 . ? O15 Co2 O2 78.57(12) . . ? O14 Co3 O13 137.14(15) 2_455 . ? O14 Co3 O3 113.62(16) 2_455 . ? O13 Co3 O3 107.94(13) . . ? O14 Co3 O6 87.39(14) 2_455 1_545 ? O13 Co3 O6 98.51(15) . 1_545 ? O3 Co3 O6 95.94(12) . 1_545 ? O14 Co3 O3 91.54(13) 2_455 2_455 ? O13 Co3 O3 83.25(13) . 2_455 ? O3 Co3 O3 83.16(12) . 2_455 ? O6 Co3 O3 178.21(15) 1_545 2_455 ? Co1 O2 Co2 115.90(15) . . ? Co3 O3 Co2 105.55(15) . . ? Co3 O3 Co3 96.84(12) . 2_455 ? Co2 O3 Co3 126.58(14) . 2_455 ? C1 O4 Co1 128.6(3) . . ? C1 O5 Co2 128.8(3) . . ? C22 O6 Co3 131.1(3) . 1_565 ? C22 O7 Co2 124.9(3) . 1_565 ? C5 O8 C31 105.6(5) . . ? C10 O9 C34 111.9(4) . . ? C17 O10 C37 112.4(5) . . ? C25 O11 C40 114.0(4) . . ? C43 O12 Co2 138.6(4) . . ? C43 O13 Co3 119.4(3) . . ? C65 O14 Co3 143.3(3) . 2_455 ? C65 O15 Co2 124.6(3) . . ? C47 O16 C74 115.0(5) . . ? C72 O17 C77 115.8(6) . . ? C59 O18 C83 112.5(4) . . ? C56 O19 C80 109.2(8) . . ? C89 O21 C89A 38.5(8) . . ? C86 N1 C88 119.4(6) . . ? C86 N1 C87 123.0(6) . . ? C88 N1 C87 117.4(5) . . ? C89A N2 C89 35.5(7) . . ? C89A N2 C90 143.9(11) . . ? C89 N2 C90 127.8(11) . . ? C89A N2 C90A 124.2(11) . . ? C89 N2 C90A 91.3(11) . . ? C90 N2 C90A 72.1(11) . . ? C89A N2 C91 90.4(10) . . ? C89 N2 C91 115.1(11) . . ? C90 N2 C91 117.1(12) . . ? C90A N2 C91 106.9(12) . . ? C89A N2 C91A 119.9(9) . . ? C89 N2 C91A 141.5(10) . . ? C90 N2 C91A 46.5(8) . . ? C90A N2 C91A 114.1(10) . . ? C91 N2 C91A 85.9(10) . . ? O4 C1 O5 126.1(5) . . ? O4 C1 C2 117.9(4) . . ? O5 C1 C2 116.0(4) . . ? C3 C2 C7 120.8(5) . . ? C3 C2 C1 119.9(5) . . ? C7 C2 C1 119.2(4) . . ? C2 C3 C4 120.6(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 117.7(5) . . ? C5 C4 C30 120.7(5) . . ? C3 C4 C30 121.2(5) . . ? C4 C5 O8 118.4(5) . . ? C4 C5 C6 122.4(6) . . ? O8 C5 C6 119.0(5) . . ? C5 C6 C7 118.3(5) . . ? C5 C6 C8 120.4(6) . . ? C7 C6 C8 121.0(5) . . ? C2 C7 C6 119.8(5) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C6 110.5(4) . . ? C9 C8 H8A 109.5 . . ? C6 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C14 C9 C10 119.0(5) . . ? C14 C9 C8 119.8(6) . . ? C10 C9 C8 121.1(6) . . ? O9 C10 C9 120.8(5) . . ? O9 C10 C11 118.5(5) . . ? C9 C10 C11 120.7(6) . . ? C12 C11 C10 117.8(5) . . ? C12 C11 C15 119.2(5) . . ? C10 C11 C15 122.9(5) . . ? C11 C12 C13 121.7(5) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C14 C13 C12 118.8(7) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C9 C14 C13 121.7(6) . . ? C9 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C11 C15 C16 111.0(4) . . ? C11 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C11 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C21 C16 C17 118.6(4) . . ? C21 C16 C15 121.3(5) . . ? C17 C16 C15 119.9(4) . . ? O10 C17 C18 119.8(5) . . ? O10 C17 C16 118.8(4) . . ? C18 C17 C16 121.3(4) . . ? C17 C18 C19 118.7(5) . . ? C17 C18 C23 120.5(4) . . ? C19 C18 C23 120.1(5) . . ? C20 C19 C18 121.3(4) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 118.6(4) . . ? C19 C20 C22 122.1(4) . . ? C21 C20 C22 119.3(4) . . ? C16 C21 C20 121.5(5) . . ? C16 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? O6 C22 O7 124.6(4) . . ? O6 C22 C20 117.0(4) . . ? O7 C22 C20 118.4(4) . . ? C24 C23 C18 109.0(4) . . ? C24 C23 H23A 109.9 . . ? C18 C23 H23A 109.9 . . ? C24 C23 H23B 109.9 . . ? C18 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C29 C24 C25 118.3(5) . . ? C29 C24 C23 118.4(5) . . ? C25 C24 C23 123.2(5) . . ? C24 C25 C26 122.2(5) . . ? C24 C25 O11 119.0(5) . . ? C26 C25 O11 118.7(4) . . ? C27 C26 C25 118.0(5) . . ? C27 C26 C30 118.9(5) . . ? C25 C26 C30 123.0(5) . . ? C26 C27 C28 121.5(6) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C27 C28 C29 119.3(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C24 C29 C28 120.6(5) . . ? C24 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C4 C30 C26 108.6(4) . . ? C4 C30 H30A 110.0 . . ? C26 C30 H30A 110.0 . . ? C4 C30 H30B 110.0 . . ? C26 C30 H30B 110.0 . . ? H30A C30 H30B 108.3 . . ? C32 C31 O8 103.5(4) . . ? C32 C31 H31A 111.1 . . ? O8 C31 H31A 111.1 . . ? C32 C31 H31B 111.1 . . ? O8 C31 H31B 111.1 . . ? H31A C31 H31B 109.0 . . ? C31 C32 C33 103.2(5) . . ? C31 C32 H32A 111.1 . . ? C33 C32 H32A 111.1 . . ? C31 C32 H32B 111.1 . . ? C33 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O9 C34 C35A 112.4(6) . . ? O9 C34 C35 111.4(5) . . ? C35A C34 C35 115.3(13) . . ? O9 C34 H34A 109.3 . . ? C35A C34 H34A 98.1 . . ? C35 C34 H34A 109.3 . . ? O9 C34 H34B 109.3 . . ? C35A C34 H34B 10.0 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? O9 C34 H34C 109.1 . . ? C35A C34 H34C 109.1 . . ? C35 C34 H34C 9.6 . . ? H34A C34 H34C 118.4 . . ? H34B C34 H34C 102.2 . . ? O9 C34 H34D 109.1 . . ? C35A C34 H34D 109.1 . . ? C35 C34 H34D 98.4 . . ? H34A C34 H34D 12.6 . . ? H34B C34 H34D 118.7 . . ? H34C C34 H34D 107.9 . . ? C34 C35 C36 103.3(4) . . ? C34 C35 H35A 111.1 . . ? C36 C35 H35A 111.1 . . ? C34 C35 H35B 111.1 . . ? C36 C35 H35B 111.1 . . ? H35A C35 H35B 109.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O10 C37 C38 110.6(6) . . ? O10 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? O10 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C39 102.9(4) . . ? C37 C38 H38A 111.2 . . ? C39 C38 H38A 111.2 . . ? C37 C38 H38B 111.2 . . ? C39 C38 H38B 111.2 . . ? H38A C38 H38B 109.1 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O11 C40 C41 110.4(4) . . ? O11 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? O11 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42A 104.9(4) . . ? C40 C41 C42 104.3(4) . . ? C42A C41 C42 144.4(9) . . ? C40 C41 H41A 110.9 . . ? C42A C41 H41A 76.7 . . ? C42 C41 H41A 110.9 . . ? C40 C41 H41B 110.9 . . ? C42A C41 H41B 38.4 . . ? C42 C41 H41B 110.9 . . ? H41A C41 H41B 108.9 . . ? C40 C41 H41C 110.8 . . ? C42A C41 H41C 110.8 . . ? C42 C41 H41C 38.4 . . ? H41A C41 H41C 133.6 . . ? H41B C41 H41C 73.5 . . ? C40 C41 H41D 110.8 . . ? C42A C41 H41D 110.8 . . ? C42 C41 H41D 76.8 . . ? H41A C41 H41D 35.7 . . ? H41B C41 H41D 133.8 . . ? H41C C41 H41D 108.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O12 C43 O13 127.1(4) . . ? O12 C43 C44 117.7(4) . . ? O13 C43 C44 115.3(4) . . ? C49 C44 C45 118.9(5) . . ? C49 C44 C43 121.7(5) . . ? C45 C44 C43 119.3(4) . . ? C46 C45 C44 118.3(5) . . ? C46 C45 H45 120.8 . . ? C44 C45 H45 120.8 . . ? C45 C46 C47 120.4(6) . . ? C45 C46 C73 116.7(6) . . ? C47 C46 C73 122.6(6) . . ? O16 C47 C46 118.4(6) . . ? O16 C47 C48 119.6(6) . . ? C46 C47 C48 121.8(6) . . ? C49 C48 C47 118.2(5) . . ? C49 C48 C50 118.6(6) . . ? C47 C48 C50 123.0(6) . . ? C44 C49 C48 122.2(6) . . ? C44 C49 H49 118.9 . . ? C48 C49 H49 118.9 . . ? C51 C50 C48 108.5(5) . . ? C51 C50 H50A 110.0 . . ? C48 C50 H50A 110.0 . . ? C51 C50 H50B 110.0 . . ? C48 C50 H50B 110.0 . . ? H50A C50 H50B 108.4 . . ? C52 C51 C56 118.3(6) . . ? C52 C51 C50 122.2(6) . . ? C56 C51 C50 118.5(7) . . ? C53 C52 C51 120.8(6) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 119.3(7) . . ? C52 C53 H53 120.3 . . ? C54 C53 H53 120.3 . . ? C55 C54 C53 122.0(7) . . ? C55 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? C54 C55 C56 118.0(6) . . ? C54 C55 C57 121.4(6) . . ? C56 C55 C57 120.2(6) . . ? O19 C56 C55 119.9(6) . . ? O19 C56 C51 118.6(6) . . ? C55 C56 C51 121.3(7) . . ? C55 C57 C64 111.2(4) . . ? C55 C57 H57A 109.4 . . ? C64 C57 H57A 109.4 . . ? C55 C57 H57B 109.4 . . ? C64 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? C64 C59 C60 123.0(5) . . ? C64 C59 O18 118.3(5) . . ? C60 C59 O18 118.7(5) . . ? C61 C60 C59 117.7(5) . . ? C61 C60 C66 119.0(5) . . ? C59 C60 C66 123.2(5) . . ? C60 C61 C62 121.9(5) . . ? C60 C61 H61 119.0 . . ? C62 C61 H61 119.0 . . ? C61 C62 C63 118.4(5) . . ? C61 C62 C65 121.7(5) . . ? C63 C62 C65 119.9(5) . . ? C64 C63 C62 121.4(5) . . ? C64 C63 H63 119.3 . . ? C62 C63 H63 119.3 . . ? C63 C64 C59 117.5(5) . . ? C63 C64 C57 119.4(5) . . ? C59 C64 C57 123.1(5) . . ? O15 C65 O14 124.6(4) . . ? O15 C65 C62 118.8(5) . . ? O14 C65 C62 116.6(4) . . ? C67 C66 C60 110.2(4) . . ? C67 C66 H66A 109.6 . . ? C60 C66 H66A 109.6 . . ? C67 C66 H66B 109.6 . . ? C60 C66 H66B 109.6 . . ? H66A C66 H66B 108.1 . . ? C72 C67 C68 117.6(6) . . ? C72 C67 C66 119.7(6) . . ? C68 C67 C66 122.1(6) . . ? C69 C68 C67 121.6(7) . . ? C69 C68 H68 119.2 . . ? C67 C68 H68 119.2 . . ? C68 C69 C70 119.8(7) . . ? C68 C69 H69 120.1 . . ? C70 C69 H69 120.1 . . ? C69 C70 C71 120.0(7) . . ? C69 C70 H70 120.0 . . ? C71 C70 H70 120.0 . . ? C70 C71 C72 119.0(7) . . ? C70 C71 C73 121.5(6) . . ? C72 C71 C73 119.2(6) . . ? C67 C72 C71 121.7(6) . . ? C67 C72 O17 119.2(6) . . ? C71 C72 O17 118.8(6) . . ? C46 C73 C71 110.5(6) . . ? C46 C73 H73A 109.6 . . ? C71 C73 H73A 109.6 . . ? C46 C73 H73B 109.6 . . ? C71 C73 H73B 109.6 . . ? H73A C73 H73B 108.1 . . ? O16 C74 C75 108.0(6) . . ? O16 C74 H74A 110.1 . . ? C75 C74 H74A 110.1 . . ? O16 C74 H74B 110.1 . . ? C75 C74 H74B 110.1 . . ? H74A C74 H74B 108.4 . . ? C76 C75 C74 102.4(4) . . ? C76 C75 H75A 111.3 . . ? C74 C75 H75A 111.3 . . ? C76 C75 H75B 111.3 . . ? C74 C75 H75B 111.3 . . ? H75A C75 H75B 109.2 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O17 C77 C78 105.5(7) . . ? O17 C77 H77A 110.6 . . ? C78 C77 H77A 110.6 . . ? O17 C77 H77B 110.6 . . ? C78 C77 H77B 110.6 . . ? H77A C77 H77B 108.8 . . ? C77 C78 C79 103.2(4) . . ? C77 C78 H78A 111.1 . . ? C79 C78 H78A 111.1 . . ? C77 C78 H78B 111.1 . . ? C79 C78 H78B 111.1 . . ? H78A C78 H78B 109.1 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O19 C80 C81 110.1(7) . . ? O19 C80 H80A 109.6 . . ? C81 C80 H80A 109.6 . . ? O19 C80 H80B 109.6 . . ? C81 C80 H80B 109.6 . . ? H80A C80 H80B 108.2 . . ? C80 C81 C82 104.7(5) . . ? C80 C81 H81A 110.8 . . ? C82 C81 H81A 110.8 . . ? C80 C81 H81B 110.8 . . ? C82 C81 H81B 110.8 . . ? H81A C81 H81B 108.9 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O18 C83 C84 107.7(5) . . ? O18 C83 H83A 110.2 . . ? C84 C83 H83A 110.2 . . ? O18 C83 H83B 110.2 . . ? C84 C83 H83B 110.2 . . ? H83A C83 H83B 108.5 . . ? C85 C84 C83 105.4(4) . . ? C85 C84 H84A 110.7 . . ? C83 C84 H84A 110.7 . . ? C85 C84 H84B 110.7 . . ? C83 C84 H84B 110.7 . . ? H84A C84 H84B 108.8 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? O20 C86 N1 123.5(6) . . ? O20 C86 H86 118.2 . . ? N1 C86 H86 118.2 . . ? N1 C87 H87A 109.5 . . ? N1 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N1 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N1 C88 H88A 109.5 . . ? N1 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N1 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? O21 C89 N2 130.6(15) . . ? O21 C89 H89 114.7 . . ? N2 C89 H89 114.7 . . ? N2 C90 H90A 109.5 . . ? N2 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? N2 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N2 C91 H91A 109.5 . . ? N2 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? N2 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C34 C35A C36A 102.7(4) . . ? C34 C35A H35C 111.2 . . ? C36A C35A H35C 111.2 . . ? C34 C35A H35D 111.2 . . ? C36A C35A H35D 111.2 . . ? H35C C35A H35D 109.1 . . ? C35A C36A H36D 109.5 . . ? C35A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C35A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? C41 C42A H42D 109.5 . . ? C41 C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C41 C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? O21 C89A N2 125.8(11) . . ? O21 C89A H89A 117.1 . . ? N2 C89A H89A 117.1 . . ? N2 C90A H90D 109.5 . . ? N2 C90A H90E 109.5 . . ? H90D C90A H90E 109.5 . . ? N2 C90A H90F 109.5 . . ? H90D C90A H90F 109.5 . . ? H90E C90A H90F 109.5 . . ? N2 C91A H91D 109.5 . . ? N2 C91A H91E 109.5 . . ? H91D C91A H91E 109.5 . . ? N2 C91A H91F 109.5 . . ? H91D C91A H91F 109.5 . . ? H91E C91A H91F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Co1 O2 Co2 31.82(15) . . . . ? O4 Co1 O2 Co2 -148.18(15) 2 . . . ? O1 Co1 O2 Co2 122.50(15) . . . . ? O1 Co1 O2 Co2 -57.49(15) 2 . . . ? O2 Co1 O2 Co2 -178(5) 2 . . . ? O5 Co2 O2 Co1 -2.29(15) . . . . ? O3 Co2 O2 Co1 -120.4(16) . . . . ? O12 Co2 O2 Co1 177.87(17) . . . . ? O7 Co2 O2 Co1 82.08(16) 1_545 . . . ? O15 Co2 O2 Co1 -94.94(16) . . . . ? O14 Co3 O3 Co2 -140.28(14) 2_455 . . . ? O13 Co3 O3 Co2 50.42(16) . . . . ? O6 Co3 O3 Co2 -50.53(16) 1_545 . . . ? O3 Co3 O3 Co2 131.03(18) 2_455 . . . ? O14 Co3 O3 Co3 88.69(15) 2_455 . . 2_455 ? O13 Co3 O3 Co3 -80.60(15) . . . 2_455 ? O6 Co3 O3 Co3 178.44(14) 1_545 . . 2_455 ? O3 Co3 O3 Co3 0.0 2_455 . . 2_455 ? O5 Co2 O3 Co3 149.00(13) . . . . ? O12 Co2 O3 Co3 -31.64(15) . . . . ? O7 Co2 O3 Co3 64.74(15) 1_545 . . . ? O15 Co2 O3 Co3 -117.91(14) . . . . ? O2 Co2 O3 Co3 -92.8(16) . . . . ? O5 Co2 O3 Co3 -99.87(19) . . . 2_455 ? O12 Co2 O3 Co3 79.5(2) . . . 2_455 ? O7 Co2 O3 Co3 175.87(19) 1_545 . . 2_455 ? O15 Co2 O3 Co3 -6.8(2) . . . 2_455 ? O2 Co2 O3 Co3 18.4(18) . . . 2_455 ? O4 Co1 O4 C1 25(6) 2 . . . ? O1 Co1 O4 C1 -146.6(4) . . . . ? O1 Co1 O4 C1 33.4(4) 2 . . . ? O2 Co1 O4 C1 -51.8(4) . . . . ? O2 Co1 O4 C1 128.2(4) 2 . . . ? O3 Co2 O5 C1 127.2(4) . . . . ? O12 Co2 O5 C1 -47.8(12) . . . . ? O7 Co2 O5 C1 -139.4(4) 1_545 . . . ? O15 Co2 O5 C1 29.8(4) . . . . ? O2 Co2 O5 C1 -48.9(4) . . . . ? O5 Co2 O12 C43 170.0(8) . . . . ? O3 Co2 O12 C43 -5.0(5) . . . . ? O7 Co2 O12 C43 -99.1(5) 1_545 . . . ? O15 Co2 O12 C43 91.9(5) . . . . ? O2 Co2 O12 C43 171.1(5) . . . . ? O14 Co3 O13 C43 154.1(3) 2_455 . . . ? O3 Co3 O13 C43 -40.4(4) . . . . ? O6 Co3 O13 C43 58.7(4) 1_545 . . . ? O3 Co3 O13 C43 -120.9(4) 2_455 . . . ? O5 Co2 O15 C65 120.2(4) . . . . ? O3 Co2 O15 C65 30.8(5) . . . . ? O12 Co2 O15 C65 -66.9(4) . . . . ? O7 Co2 O15 C65 -163.1(7) 1_545 . . . ? O2 Co2 O15 C65 -147.3(5) . . . . ? Co1 O4 C1 O5 16.2(6) . . . . ? Co1 O4 C1 C2 -162.3(3) . . . . ? Co2 O5 C1 O4 50.7(6) . . . . ? Co2 O5 C1 C2 -130.8(4) . . . . ? O4 C1 C2 C3 18.4(6) . . . . ? O5 C1 C2 C3 -160.2(4) . . . . ? O4 C1 C2 C7 -157.8(4) . . . . ? O5 C1 C2 C7 23.5(6) . . . . ? C7 C2 C3 C4 -3.9(7) . . . . ? C1 C2 C3 C4 179.9(4) . . . . ? C2 C3 C4 C5 0.7(7) . . . . ? C2 C3 C4 C30 173.6(4) . . . . ? C3 C4 C5 O8 -179.1(5) . . . . ? C30 C4 C5 O8 8.0(8) . . . . ? C3 C4 C5 C6 4.4(8) . . . . ? C30 C4 C5 C6 -168.5(5) . . . . ? C31 O8 C5 C4 89.8(8) . . . . ? C31 O8 C5 C6 -93.6(8) . . . . ? C4 C5 C6 C7 -6.2(8) . . . . ? O8 C5 C6 C7 177.4(5) . . . . ? C4 C5 C6 C8 168.4(5) . . . . ? O8 C5 C6 C8 -8.0(8) . . . . ? C3 C2 C7 C6 2.2(7) . . . . ? C1 C2 C7 C6 178.3(4) . . . . ? C5 C6 C7 C2 2.8(7) . . . . ? C8 C6 C7 C2 -171.8(4) . . . . ? C5 C6 C8 C9 -72.7(8) . . . . ? C7 C6 C8 C9 101.7(6) . . . . ? C6 C8 C9 C14 -58.7(7) . . . . ? C6 C8 C9 C10 117.4(6) . . . . ? C34 O9 C10 C9 95.7(6) . . . . ? C34 O9 C10 C11 -84.3(6) . . . . ? C14 C9 C10 O9 -175.8(5) . . . . ? C8 C9 C10 O9 8.1(7) . . . . ? C14 C9 C10 C11 4.3(7) . . . . ? C8 C9 C10 C11 -171.8(4) . . . . ? O9 C10 C11 C12 176.6(4) . . . . ? C9 C10 C11 C12 -3.5(7) . . . . ? O9 C10 C11 C15 -7.2(7) . . . . ? C9 C10 C11 C15 172.8(4) . . . . ? C10 C11 C12 C13 -0.3(8) . . . . ? C15 C11 C12 C13 -176.7(5) . . . . ? C11 C12 C13 C14 3.1(10) . . . . ? C10 C9 C14 C13 -1.4(9) . . . . ? C8 C9 C14 C13 174.8(5) . . . . ? C12 C13 C14 C9 -2.3(10) . . . . ? C12 C11 C15 C16 58.1(6) . . . . ? C10 C11 C15 C16 -118.1(5) . . . . ? C11 C15 C16 C21 -101.2(6) . . . . ? C11 C15 C16 C17 73.1(7) . . . . ? C37 O10 C17 C18 -71.0(7) . . . . ? C37 O10 C17 C16 112.3(6) . . . . ? C21 C16 C17 O10 -179.6(5) . . . . ? C15 C16 C17 O10 5.9(8) . . . . ? C21 C16 C17 C18 3.7(9) . . . . ? C15 C16 C17 C18 -170.7(5) . . . . ? O10 C17 C18 C19 179.6(5) . . . . ? C16 C17 C18 C19 -3.8(9) . . . . ? O10 C17 C18 C23 -10.2(9) . . . . ? C16 C17 C18 C23 166.4(5) . . . . ? C17 C18 C19 C20 0.9(9) . . . . ? C23 C18 C19 C20 -169.3(5) . . . . ? C18 C19 C20 C21 1.9(9) . . . . ? C18 C19 C20 C22 -177.4(5) . . . . ? C17 C16 C21 C20 -0.8(9) . . . . ? C15 C16 C21 C20 173.5(5) . . . . ? C19 C20 C21 C16 -1.9(9) . . . . ? C22 C20 C21 C16 177.3(5) . . . . ? Co3 O6 C22 O7 40.6(8) 1_565 . . . ? Co3 O6 C22 C20 -139.2(4) 1_565 . . . ? Co2 O7 C22 O6 -13.5(8) 1_565 . . . ? Co2 O7 C22 C20 166.3(4) 1_565 . . . ? C19 C20 C22 O6 -170.3(5) . . . . ? C21 C20 C22 O6 10.5(8) . . . . ? C19 C20 C22 O7 9.9(8) . . . . ? C21 C20 C22 O7 -169.3(5) . . . . ? C17 C18 C23 C24 -68.1(7) . . . . ? C19 C18 C23 C24 102.0(6) . . . . ? C18 C23 C24 C29 -55.1(6) . . . . ? C18 C23 C24 C25 121.0(5) . . . . ? C29 C24 C25 C26 3.4(7) . . . . ? C23 C24 C25 C26 -172.7(5) . . . . ? C29 C24 C25 O11 -178.7(4) . . . . ? C23 C24 C25 O11 5.3(7) . . . . ? C40 O11 C25 C24 90.8(5) . . . . ? C40 O11 C25 C26 -91.2(5) . . . . ? C24 C25 C26 C27 -2.7(8) . . . . ? O11 C25 C26 C27 179.4(5) . . . . ? C24 C25 C26 C30 173.0(5) . . . . ? O11 C25 C26 C30 -4.9(7) . . . . ? C25 C26 C27 C28 -0.9(9) . . . . ? C30 C26 C27 C28 -176.7(6) . . . . ? C26 C27 C28 C29 3.5(10) . . . . ? C25 C24 C29 C28 -0.7(8) . . . . ? C23 C24 C29 C28 175.6(5) . . . . ? C27 C28 C29 C24 -2.6(9) . . . . ? C5 C4 C30 C26 70.7(7) . . . . ? C3 C4 C30 C26 -102.0(6) . . . . ? C27 C26 C30 C4 53.2(7) . . . . ? C25 C26 C30 C4 -122.4(5) . . . . ? C5 O8 C31 C32 152.0(12) . . . . ? O8 C31 C32 C33 -173.3(13) . . . . ? C10 O9 C34 C35A -58.3(15) . . . . ? C10 O9 C34 C35 170.5(9) . . . . ? O9 C34 C35 C36 177.7(9) . . . . ? C35A C34 C35 C36 48.0(16) . . . . ? C17 O10 C37 C38 -106.8(8) . . . . ? O10 C37 C38 C39 -172.8(8) . . . . ? C25 O11 C40 C41 175.9(4) . . . . ? O11 C40 C41 C42A 84.3(9) . . . . ? O11 C40 C41 C42 -75.1(8) . . . . ? Co2 O12 C43 O13 25.1(8) . . . . ? Co2 O12 C43 C44 -153.5(4) . . . . ? Co3 O13 C43 O12 1.9(7) . . . . ? Co3 O13 C43 C44 -179.4(3) . . . . ? O12 C43 C44 C49 160.2(5) . . . . ? O13 C43 C44 C49 -18.6(7) . . . . ? O12 C43 C44 C45 -17.3(7) . . . . ? O13 C43 C44 C45 163.9(4) . . . . ? C49 C44 C45 C46 2.7(7) . . . . ? C43 C44 C45 C46 -179.7(5) . . . . ? C44 C45 C46 C47 -2.0(8) . . . . ? C44 C45 C46 C73 -175.9(5) . . . . ? C74 O16 C47 C46 -90.2(8) . . . . ? C74 O16 C47 C48 92.9(8) . . . . ? C45 C46 C47 O16 -177.8(5) . . . . ? C73 C46 C47 O16 -4.3(9) . . . . ? C45 C46 C47 C48 -1.0(9) . . . . ? C73 C46 C47 C48 172.6(5) . . . . ? O16 C47 C48 C49 -180.0(5) . . . . ? C46 C47 C48 C49 3.2(8) . . . . ? O16 C47 C48 C50 5.0(8) . . . . ? C46 C47 C48 C50 -171.8(5) . . . . ? C45 C44 C49 C48 -0.5(7) . . . . ? C43 C44 C49 C48 -178.0(5) . . . . ? C47 C48 C49 C44 -2.4(8) . . . . ? C50 C48 C49 C44 172.9(5) . . . . ? C49 C48 C50 C51 -47.8(7) . . . . ? C47 C48 C50 C51 127.2(6) . . . . ? C48 C50 C51 C52 100.4(6) . . . . ? C48 C50 C51 C56 -68.2(7) . . . . ? C56 C51 C52 C53 0.7(9) . . . . ? C50 C51 C52 C53 -168.0(6) . . . . ? C51 C52 C53 C54 2.7(10) . . . . ? C52 C53 C54 C55 -2.1(10) . . . . ? C53 C54 C55 C56 -2.0(9) . . . . ? C53 C54 C55 C57 170.6(5) . . . . ? C80 O19 C56 C55 83.3(8) . . . . ? C80 O19 C56 C51 -102.0(8) . . . . ? C54 C55 C56 O19 -179.9(5) . . . . ? C57 C55 C56 O19 7.5(8) . . . . ? C54 C55 C56 C51 5.5(8) . . . . ? C57 C55 C56 C51 -167.2(5) . . . . ? C52 C51 C56 O19 -179.6(5) . . . . ? C50 C51 C56 O19 -10.5(8) . . . . ? C52 C51 C56 C55 -4.9(8) . . . . ? C50 C51 C56 C55 164.2(5) . . . . ? C54 C55 C57 C64 -103.1(6) . . . . ? C56 C55 C57 C64 69.3(7) . . . . ? C83 O18 C59 C64 -85.2(6) . . . . ? C83 O18 C59 C60 97.1(7) . . . . ? C64 C59 C60 C61 3.1(9) . . . . ? O18 C59 C60 C61 -179.3(5) . . . . ? C64 C59 C60 C66 -172.8(6) . . . . ? O18 C59 C60 C66 4.8(8) . . . . ? C59 C60 C61 C62 1.1(9) . . . . ? C66 C60 C61 C62 177.1(5) . . . . ? C60 C61 C62 C63 -3.8(8) . . . . ? C60 C61 C62 C65 179.1(5) . . . . ? C61 C62 C63 C64 2.5(8) . . . . ? C65 C62 C63 C64 179.6(5) . . . . ? C62 C63 C64 C59 1.4(8) . . . . ? C62 C63 C64 C57 -175.3(5) . . . . ? C60 C59 C64 C63 -4.3(9) . . . . ? O18 C59 C64 C63 178.1(5) . . . . ? C60 C59 C64 C57 172.3(5) . . . . ? O18 C59 C64 C57 -5.3(8) . . . . ? C55 C57 C64 C63 55.6(8) . . . . ? C55 C57 C64 C59 -120.9(6) . . . . ? Co2 O15 C65 O14 -46.5(7) . . . . ? Co2 O15 C65 C62 134.4(4) . . . . ? Co3 O14 C65 O15 34.9(10) 2_455 . . . ? Co3 O14 C65 C62 -145.9(5) 2_455 . . . ? C61 C62 C65 O15 11.6(8) . . . . ? C63 C62 C65 O15 -165.4(5) . . . . ? C61 C62 C65 O14 -167.6(5) . . . . ? C63 C62 C65 O14 15.3(7) . . . . ? C61 C60 C66 C67 -52.2(8) . . . . ? C59 C60 C66 C67 123.6(6) . . . . ? C60 C66 C67 C72 -66.4(7) . . . . ? C60 C66 C67 C68 104.5(7) . . . . ? C72 C67 C68 C69 1.5(10) . . . . ? C66 C67 C68 C69 -169.6(6) . . . . ? C67 C68 C69 C70 1.9(11) . . . . ? C68 C69 C70 C71 -1.5(11) . . . . ? C69 C70 C71 C72 -2.2(10) . . . . ? C69 C70 C71 C73 171.4(7) . . . . ? C68 C67 C72 C71 -5.4(9) . . . . ? C66 C67 C72 C71 165.9(5) . . . . ? C68 C67 C72 O17 -179.0(6) . . . . ? C66 C67 C72 O17 -7.7(8) . . . . ? C70 C71 C72 C67 5.8(10) . . . . ? C73 C71 C72 C67 -168.0(6) . . . . ? C70 C71 C72 O17 179.5(6) . . . . ? C73 C71 C72 O17 5.7(9) . . . . ? C77 O17 C72 C67 -112.3(7) . . . . ? C77 O17 C72 C71 73.9(7) . . . . ? C45 C46 C73 C71 49.6(7) . . . . ? C47 C46 C73 C71 -124.2(7) . . . . ? C70 C71 C73 C46 -108.4(7) . . . . ? C72 C71 C73 C46 65.2(7) . . . . ? C47 O16 C74 C75 169.7(8) . . . . ? O16 C74 C75 C76 179.4(12) . . . . ? C72 O17 C77 C78 93.2(11) . . . . ? O17 C77 C78 C79 172.7(11) . . . . ? C56 O19 C80 C81 128.3(14) . . . . ? O19 C80 C81 C82 -179.1(12) . . . . ? C59 O18 C83 C84 -179.5(5) . . . . ? O18 C83 C84 C85 -71.8(8) . . . . ? C88 N1 C86 O20 -175.3(6) . . . . ? C87 N1 C86 O20 -0.5(10) . . . . ? C89A O21 C89 N2 -48.1(16) . . . . ? C89A N2 C89 O21 50.3(17) . . . . ? C90 N2 C89 O21 -177.2(16) . . . . ? C90A N2 C89 O21 -109.0(19) . . . . ? C91 N2 C89 O21 0(2) . . . . ? C91A N2 C89 O21 117.9(18) . . . . ? O9 C34 C35A C36A 170.5(18) . . . . ? C35 C34 C35A C36A -60(3) . . . . ? C89 O21 C89A N2 45.6(16) . . . . ? C89 N2 C89A O21 -42.2(15) . . . . ? C90 N2 C89A O21 -124.6(18) . . . . ? C90A N2 C89A O21 -17.0(18) . . . . ? C91 N2 C89A O21 93.9(14) . . . . ? C91A N2 C89A O21 179.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.523 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.099 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.007 0.500 584 66 ' ' 2 0.268 0.475 0.784 13 1 ' ' 3 0.732 0.525 0.216 13 1 ' ' _platon_squeeze_details ; ; #===end