_publ_contact_author_name 'Dr. Yvan Guindon' _publ_contact_author_address ; IRCM 110 ouest, Avenue des Pins Montr\'eal, Qu\'ebec Canada H2W 1R7 ; _publ_contact_author_phone '+1 514 987 5788' _publ_contact_author_fax '+1 514 987 5789' _publ_contact_author_email 'guindoy@ircm.qc.ca' _publ_section_title ; Structure of Guin57 ; loop_ _publ_author_name _publ_author_address 'Guindon, Yvan' ; IRCM 110 ouest, Avenue des Pins Montr\'eal, Qu\'ebec Canada H2W 1R7 ; 'Michael' ; IRCM 110 ouest, Avenue des Pins Montr\'eal, Qu\'ebec Canada H2W 1R7 ; 'B\'elanger-Gari\'epy, Francine' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; _publ_section_references ; Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388. Flack, H.D. (1983). Acta Cryst. A39, 876-881. Flack, H.D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. APEX2 (2006) version 2.1-0; Bruker Molecular Analysis Research Tool. Bruker AXS Inc., Madison, WI 53719-1173. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, WI 53719-1173. SHELXTL (2001) version 6.12; Bruker Analytical X-ray Systems Inc., Madison, WI 53719-1173. Spek, A.L. (2008). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Maris, T. (2004). UdMX, University of Montr\'eal, Montr\'eal, QC, Canada. XPREP (2005) Version 2005/2; X-ray data Preparation and Reciprocal space Exploration Program. Bruker AXS Inc., Madison, WI 53719-1173. ; # ======================================================== # STRUCTURAL DATA # ======================================================== data_guin57 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H45 N O13' _chemical_formula_sum 'C42 H45 N O13' _chemical_formula_weight 771.79 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0000 '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' 0.0311 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0000 '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 _symmetry_space_group_name_hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.5024(16) _cell_length_b 6.2258(8) _cell_length_c 20.953(2) _cell_angle_alpha 90 _cell_angle_beta 101.598(5) _cell_angle_gamma 90 _cell_volume 1981.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 5432 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 53.18 _exptl_crystal_description 'Chunk' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.2711 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker microstar diffractometer equiped with a Platinum 135 CCD Detector, a Helios optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over three different parts of the reciprocal space (99 frames total). Due to geometrical constraints of the instrument and the use of copper radiation, we obtain consistently a data completeness lower than 100% in dependence of the crystal system and the orientation of the mounted crystal, even with appropriate data collection routines. Typical values for data completeness range from 83-92% for triclinic, 85-97% for monoclinic and 85-98% for all other crystal systems. Disordered was found for one OBn and the isopropyl group. Absolute parameter (Flack) refined to -0.1(4). It was too high and the Friedel pairs were merged in last crefinement cycles. The poor data quality (low theta max and low ratio of reflections to parameters) was due to the very thin sample (.02 x .04 x .1). It was not possible to find a bigger crystal. ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios optics' _diffrn_measurement_device_type 'Bruker Microstar' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 203 _diffrn_standards_interval_time 900 _diffrn_standards_decay_% 2.20 _diffrn_reflns_number 31918 _diffrn_reflns_av_R_equivalents 0.092 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 60.55 _reflns_number_total 3171 _reflns_number_gt 2070 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'APEX2 v2.1-0 (Bruker AXS, 2006a)' _computing_cell_refinement 'SAINT V7.34A (Bruker AXS, 2006b)' _computing_data_reduction 'SAINT V7.34A (Bruker AXS, 2006b)' _computing_structure_solution 'SIR2004 (Burla et al., 2004)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'UdMX (Maris, 2004)' _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. ; _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^)+(0.1241P)^2^] 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_abs_structure_details 'Friedel Pairs merged' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3171 _refine_ls_number_parameters 538 _refine_ls_number_restraints 605 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.069 _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 C1 C 0.8436(4) 0.309(2) 0.9179(3) 0.0570(19) Uani 1 1 d U . . O1 O 0.8726(3) 0.4750(15) 0.9014(2) 0.0680(15) Uani 1 1 d U . . C2 C 0.7778(4) 0.1672(18) 0.8716(3) 0.0571(19) Uani 1 1 d U . . H2 H 0.7657 0.0328 0.8944 0.069 Uiso 1 1 calc R . . C3 C 0.6917(4) 0.2917(18) 0.8478(3) 0.0595(19) Uani 1 1 d U . . H3 H 0.7040 0.4266 0.8253 0.071 Uiso 1 1 calc R . . C4 C 0.6461(5) 0.345(2) 0.9034(4) 0.071(2) Uani 1 1 d U . . O4 O 0.5920(4) 0.2260(17) 0.9195(3) 0.100(2) Uani 1 1 d U . . O5 O 0.6761(3) 0.5218(15) 0.9332(2) 0.0674(14) Uani 1 1 d U A . C6 C 0.6421(4) 0.5852(8) 0.9906(3) 0.072(2) Uani 1 1 d DU . . H6A H 0.6387 0.4590 1.0195 0.087 Uiso 0.833(7) 1 calc PR A -1 H6B H 0.5764 0.5724 0.9813 0.087 Uiso 0.167(7) 1 calc PR A -2 C7 C 0.5517(5) 0.686(2) 0.9676(4) 0.087(2) Uani 0.833(7) 1 d PDU A -1 H7A H 0.5105 0.5771 0.9458 0.130 Uiso 0.833(7) 1 calc PR A -1 H7B H 0.5560 0.8030 0.9371 0.130 Uiso 0.833(7) 1 calc PR A -1 H7C H 0.5304 0.7433 1.0052 0.130 Uiso 0.833(7) 1 calc PR A -1 C8 C 0.7072(6) 0.7516(16) 1.0249(5) 0.087(2) Uani 0.833(7) 1 d PDU A -1 H8A H 0.7647 0.6838 1.0399 0.130 Uiso 0.833(7) 1 calc PR A -1 H8B H 0.6859 0.8100 1.0623 0.130 Uiso 0.833(7) 1 calc PR A -1 H8C H 0.7128 0.8680 0.9945 0.130 Uiso 0.833(7) 1 calc PR A -1 C9 C 0.669(3) 0.8195(17) 1.002(2) 0.087(2) Uani 0.167(7) 1 d PDU A -2 H9A H 0.6473 0.9018 0.9619 0.130 Uiso 0.167(7) 1 calc PR A -2 H9B H 0.7332 0.8298 1.0135 0.130 Uiso 0.167(7) 1 calc PR A -2 H9C H 0.6433 0.8779 1.0373 0.130 Uiso 0.167(7) 1 calc PR A -2 C10 C 0.682(3) 0.454(6) 1.0506(14) 0.087(2) Uani 0.167(7) 1 d PDU A -2 H10A H 0.6551 0.3101 1.0469 0.130 Uiso 0.167(7) 1 calc PR A -2 H10B H 0.6698 0.5250 1.0896 0.130 Uiso 0.167(7) 1 calc PR A -2 H10C H 0.7453 0.4410 1.0538 0.130 Uiso 0.167(7) 1 calc PR A -2 O11 O 0.8610(3) 0.2256(15) 0.9764(2) 0.0658(14) Uani 1 1 d U . . C12 C 0.9227(5) 0.347(2) 1.0256(3) 0.081(3) Uani 1 1 d U . . H12A H 0.9832 0.3061 1.0239 0.121 Uiso 1 1 calc R . . H12B H 0.9113 0.3157 1.0690 0.121 Uiso 1 1 calc R . . H12C H 0.9148 0.5013 1.0167 0.121 Uiso 1 1 calc R . . O21 O 0.8097(2) 0.1155(13) 0.81445(19) 0.0556(12) Uani 1 1 d U . . C22 C 0.8790(4) -0.0392(18) 0.8266(3) 0.0579(19) Uani 1 1 d U . . H22 H 0.8627 -0.1564 0.8546 0.069 Uiso 1 1 calc R . . O23 O 0.9593(2) 0.0563(15) 0.85865(19) 0.0617(13) Uani 1 1 d U . . C24 C 0.9914(4) 0.2205(18) 0.8205(3) 0.060(2) Uani 1 1 d U . . H24 H 0.9460 0.3364 0.8106 0.071 Uiso 1 1 calc R . . C25 C 1.0068(4) 0.1304(19) 0.7574(3) 0.067(2) Uani 1 1 d U A . H25 H 1.0277 0.2462 0.7311 0.081 Uiso 1 1 calc R . . C26 C 0.9209(4) 0.0295(18) 0.7186(3) 0.0576(19) Uani 1 1 d U . . H26 H 0.8760 0.1466 0.7088 0.069 Uiso 1 1 calc R . . C27 C 0.8875(4) -0.1326(17) 0.7614(3) 0.0575(19) Uani 1 1 d U . . H27 H 0.9299 -0.2553 0.7694 0.069 Uiso 1 1 calc R . . O31 O 0.6383(2) 0.1497(14) 0.8020(2) 0.0639(14) Uani 1 1 d U . . C32 C 0.5626(4) 0.238(2) 0.7680(4) 0.068(2) Uani 1 1 d U . . O32 O 0.5419(3) 0.4210(16) 0.7780(3) 0.0852(18) Uani 1 1 d U . . C33 C 0.5129(4) 0.0906(19) 0.7206(4) 0.066(2) Uani 1 1 d U . . C34 C 0.5450(4) -0.1104(19) 0.7070(4) 0.073(2) Uani 1 1 d U . . H34 H 0.6014 -0.1556 0.7295 0.088 Uiso 1 1 calc R . . C35 C 0.4959(4) -0.243(2) 0.6615(4) 0.079(2) Uani 1 1 d U . . H35 H 0.5186 -0.3769 0.6505 0.095 Uiso 1 1 calc R . . C36 C 0.4115(5) -0.175(2) 0.6317(4) 0.077(2) Uani 1 1 d U . . N36 N 0.3576(4) -0.324(2) 0.5847(4) 0.092(2) Uani 1 1 d U . . O36 O 0.3871(4) -0.4942(19) 0.5726(4) 0.118(3) Uani 1 1 d U . . C37 C 0.3796(4) 0.020(2) 0.6432(4) 0.088(3) Uani 1 1 d U . . H37 H 0.3229 0.0634 0.6205 0.106 Uiso 1 1 calc R . . O37 O 0.2840(4) -0.2635(17) 0.5589(3) 0.116(2) Uani 1 1 d U . . C38 C 0.4290(4) 0.157(2) 0.6877(4) 0.082(3) Uani 1 1 d U . . H38 H 0.4068 0.2939 0.6962 0.098 Uiso 1 1 calc R . . C41 C 1.0736(4) 0.314(2) 0.8636(4) 0.080(2) Uani 1 1 d U . . H41A H 1.0612 0.3497 0.9063 0.120 Uiso 1 1 calc R . . H41B H 1.0914 0.4440 0.8432 0.120 Uiso 1 1 calc R . . H41C H 1.1213 0.2080 0.8688 0.120 Uiso 1 1 calc R . . O51 O 1.0737(3) -0.0345(16) 0.7734(2) 0.0780(16) Uani 1 1 d DU . . C52 C 1.1300(5) -0.067(3) 0.7281(4) 0.104(3) Uani 0.833(7) 1 d PDU A -1 H22A H 1.1368 0.0699 0.7054 0.125 Uiso 0.833(7) 1 calc PR A -1 H22B H 1.1034 -0.1737 0.6949 0.125 Uiso 0.833(7) 1 calc PR A -1 C53 C 1.2148(4) -0.141(2) 0.7615(3) 0.078(3) Uani 0.833(7) 1 d PGDU A -1 C54 C 1.2432(6) -0.3509(19) 0.7560(4) 0.146(5) Uani 0.833(7) 1 d PGU A -1 H54 H 1.2043 -0.4540 0.7322 0.175 Uiso 0.833(7) 1 calc PR A -1 C55 C 1.3285(6) -0.4098(19) 0.7852(5) 0.146(5) Uani 0.833(7) 1 d PGU A -1 H55 H 1.3479 -0.5531 0.7814 0.175 Uiso 0.833(7) 1 calc PR A -1 C56 C 1.3854(4) -0.259(2) 0.8200(4) 0.126(5) Uani 0.833(7) 1 d PGU A -1 H56 H 1.4436 -0.2993 0.8400 0.152 Uiso 0.833(7) 1 calc PR A -1 C57 C 1.3570(5) -0.049(2) 0.8256(4) 0.142(5) Uani 0.833(7) 1 d PGU A -1 H57 H 1.3958 0.0537 0.8494 0.171 Uiso 0.833(7) 1 calc PR A -1 C58 C 1.2717(5) 0.0096(18) 0.7963(4) 0.123(4) Uani 0.833(7) 1 d PGU A -1 H58 H 1.2523 0.1529 0.8001 0.148 Uiso 0.833(7) 1 calc PR A -1 O61 O 0.9276(3) -0.0646(16) 0.6600(2) 0.0701(14) Uani 1 1 d U . . C62 C 0.9119(4) 0.068(2) 0.6039(3) 0.081(3) Uani 1 1 d U . . H62A H 0.8730 0.1880 0.6108 0.097 Uiso 1 1 calc R . . H62B H 0.8807 -0.0169 0.5663 0.097 Uiso 1 1 calc R . . C63 C 0.9952(4) 0.158(2) 0.5880(3) 0.064(2) Uani 1 1 d U . . C64 C 1.0441(4) 0.024(2) 0.5574(3) 0.074(2) Uani 1 1 d U . . H64 H 1.0235 -0.1166 0.5457 0.089 Uiso 1 1 calc R . . C65 C 1.1251(5) 0.094(2) 0.5430(4) 0.085(3) Uani 1 1 d U . . H65 H 1.1591 0.0026 0.5215 0.101 Uiso 1 1 calc R . . C66 C 1.1527(6) 0.296(2) 0.5611(4) 0.090(3) Uani 1 1 d U . . H66 H 1.2080 0.3413 0.5528 0.109 Uiso 1 1 calc R . . C67 C 1.1055(5) 0.440(2) 0.5906(4) 0.081(3) Uani 1 1 d U . . H67 H 1.1265 0.5810 0.6014 0.097 Uiso 1 1 calc R . . C68 C 1.0243(5) 0.368(2) 0.6044(4) 0.086(3) Uani 1 1 d U . . H68 H 0.9897 0.4622 0.6246 0.103 Uiso 1 1 calc R . . O71 O 0.8024(2) -0.2141(15) 0.7293(2) 0.0611(13) Uani 1 1 d U . . C72 C 0.8064(4) -0.4259(18) 0.7054(3) 0.062(2) Uani 1 1 d U . . H72A H 0.8061 -0.5301 0.7410 0.074 Uiso 1 1 calc R . . H72B H 0.8617 -0.4453 0.6893 0.074 Uiso 1 1 calc R . . C73 C 0.7280(4) -0.4675(18) 0.6503(3) 0.0557(18) Uani 1 1 d U . . C74 C 0.6863(4) -0.664(2) 0.6470(4) 0.070(2) Uani 1 1 d U . . H74 H 0.7036 -0.7676 0.6805 0.084 Uiso 1 1 calc R . . C75 C 0.6174(4) -0.712(2) 0.5931(4) 0.080(3) Uani 1 1 d U . . H75 H 0.5870 -0.8448 0.5908 0.096 Uiso 1 1 calc R . . C76 C 0.5956(5) -0.563(2) 0.5445(4) 0.083(3) Uani 1 1 d U . . H76 H 0.5511 -0.5957 0.5075 0.099 Uiso 1 1 calc R . . C77 C 0.6365(5) -0.369(2) 0.5480(4) 0.081(3) Uani 1 1 d U . . H77 H 0.6194 -0.2665 0.5142 0.098 Uiso 1 1 calc R . . C78 C 0.7046(4) -0.3199(18) 0.6019(3) 0.070(2) Uani 1 1 d U . . H78 H 0.7337 -0.1850 0.6044 0.084 Uiso 1 1 calc R . . C82 C 1.1305(4) -0.0613(18) 0.7281(3) 0.104(3) Uani 0.167(7) 1 d PRDU A -2 H82A H 1.1458 0.0809 0.7124 0.125 Uiso 0.167(7) 1 calc PR A -2 H82B H 1.0998 -0.1448 0.6900 0.125 Uiso 0.167(7) 1 calc PR A -2 C83 C 1.2093(15) -0.172(7) 0.7587(10) 0.104(9) Uani 0.167(7) 1 d PGDU A -2 C84 C 1.2186(17) -0.212(7) 0.8250(10) 0.093(11) Uani 0.167(7) 1 d PGU A -2 H84 H 1.1744 -0.1659 0.8474 0.111 Uiso 0.167(7) 1 calc PR A -2 C85 C 1.2927(18) -0.319(7) 0.8585(9) 0.098(13) Uani 0.167(7) 1 d PGU A -2 H85 H 1.2991 -0.3464 0.9038 0.117 Uiso 0.167(7) 1 calc PR A -2 C86 C 1.3574(15) -0.386(6) 0.8257(14) 0.068(9) Uani 0.167(7) 1 d PGU A -2 H86 H 1.4080 -0.4595 0.8486 0.082 Uiso 0.167(7) 1 calc PR A -2 C87 C 1.3481(15) -0.346(7) 0.7594(14) 0.103(10) Uani 0.167(7) 1 d PGU A -2 H87 H 1.3923 -0.3921 0.7370 0.123 Uiso 0.167(7) 1 calc PR A -2 C88 C 1.2740(16) -0.239(8) 0.7259(10) 0.109(11) Uani 0.167(7) 1 d PGU A -2 H88 H 1.2677 -0.2117 0.6806 0.131 Uiso 0.167(7) 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 C1 0.051(4) 0.070(6) 0.050(4) -0.004(4) 0.012(3) 0.008(4) O1 0.059(3) 0.065(4) 0.079(3) 0.003(3) 0.014(2) 0.000(3) C2 0.056(3) 0.063(5) 0.051(3) -0.004(4) 0.008(3) -0.001(4) C3 0.054(3) 0.060(5) 0.064(4) -0.006(4) 0.010(3) 0.000(4) C4 0.057(4) 0.087(7) 0.071(5) -0.003(5) 0.019(4) 0.006(5) O4 0.107(4) 0.085(5) 0.124(5) -0.012(4) 0.063(4) -0.017(4) O5 0.055(2) 0.080(4) 0.069(3) -0.015(3) 0.017(2) 0.003(3) C6 0.069(4) 0.081(7) 0.069(4) -0.017(5) 0.016(3) 0.009(4) C7 0.060(4) 0.111(7) 0.090(5) -0.015(5) 0.018(3) 0.012(4) C8 0.060(4) 0.111(7) 0.090(5) -0.015(5) 0.018(3) 0.012(4) C9 0.060(4) 0.111(7) 0.090(5) -0.015(5) 0.018(3) 0.012(4) C10 0.060(4) 0.111(7) 0.090(5) -0.015(5) 0.018(3) 0.012(4) O11 0.059(2) 0.076(4) 0.058(3) -0.003(3) 0.003(2) -0.005(3) C12 0.076(5) 0.089(7) 0.068(4) -0.013(5) -0.011(4) -0.009(5) O21 0.047(2) 0.056(3) 0.062(3) 0.002(2) 0.0061(19) 0.007(2) C22 0.047(3) 0.048(5) 0.074(4) 0.001(4) 0.001(3) -0.003(3) O23 0.050(2) 0.066(4) 0.064(2) 0.006(3) -0.0011(19) 0.000(3) C24 0.055(3) 0.057(6) 0.063(4) 0.004(4) 0.001(3) -0.006(4) C25 0.049(3) 0.075(6) 0.078(4) -0.002(4) 0.012(3) -0.001(4) C26 0.045(3) 0.068(6) 0.056(4) -0.003(4) 0.002(3) 0.000(4) C27 0.040(3) 0.063(6) 0.066(4) 0.000(4) 0.001(3) 0.005(3) O31 0.044(2) 0.068(4) 0.078(3) -0.009(3) 0.009(2) 0.004(2) C32 0.042(4) 0.076(7) 0.088(5) -0.006(5) 0.016(3) 0.011(4) O32 0.037(2) 0.086(5) 0.128(4) -0.022(4) 0.007(2) 0.009(3) C33 0.036(3) 0.071(6) 0.090(5) -0.014(5) 0.010(3) 0.003(4) C34 0.047(4) 0.071(7) 0.101(5) -0.008(5) 0.010(4) -0.001(4) C35 0.047(4) 0.082(7) 0.104(5) -0.012(5) 0.004(4) 0.006(4) C36 0.058(4) 0.065(7) 0.102(6) -0.012(5) 0.006(4) -0.007(5) N36 0.058(4) 0.091(7) 0.120(6) -0.005(5) -0.001(4) -0.009(4) O36 0.084(4) 0.093(7) 0.166(6) -0.044(5) -0.006(4) -0.002(4) C37 0.043(4) 0.093(8) 0.121(6) -0.020(6) -0.004(4) -0.009(5) O37 0.058(3) 0.109(6) 0.165(6) -0.014(5) -0.013(3) -0.011(3) C38 0.053(4) 0.082(7) 0.107(6) -0.011(5) 0.008(4) 0.008(4) C41 0.064(4) 0.093(7) 0.080(5) -0.006(5) 0.004(3) -0.016(5) O51 0.048(2) 0.102(5) 0.085(3) -0.006(3) 0.015(2) 0.011(3) C52 0.088(4) 0.126(6) 0.100(4) 0.004(5) 0.024(4) 0.024(4) C53 0.058(4) 0.107(7) 0.067(5) 0.001(5) 0.010(4) 0.011(5) C54 0.137(8) 0.159(9) 0.137(8) -0.006(7) 0.017(6) 0.007(7) C55 0.142(8) 0.165(9) 0.141(8) -0.029(7) 0.052(7) 0.031(7) C56 0.108(7) 0.144(9) 0.132(7) 0.010(7) 0.036(6) 0.025(7) C57 0.108(7) 0.172(10) 0.147(8) -0.013(8) 0.027(6) -0.006(7) C58 0.094(6) 0.150(9) 0.126(7) -0.007(7) 0.022(6) 0.000(7) O61 0.058(2) 0.093(4) 0.060(3) -0.008(3) 0.015(2) -0.007(3) C62 0.045(3) 0.138(9) 0.059(4) -0.009(5) 0.007(3) -0.008(5) C63 0.047(3) 0.088(7) 0.052(4) 0.001(4) 0.000(3) 0.005(4) C64 0.048(3) 0.094(7) 0.079(4) 0.010(5) 0.007(3) -0.001(4) C65 0.058(4) 0.101(9) 0.090(5) -0.001(6) 0.004(4) 0.011(5) C66 0.068(5) 0.100(9) 0.091(6) 0.005(6) -0.015(4) -0.006(6) C67 0.073(5) 0.084(7) 0.080(5) 0.012(5) -0.001(4) -0.017(5) C68 0.081(5) 0.110(9) 0.064(4) -0.004(5) 0.010(4) 0.014(6) O71 0.038(2) 0.061(4) 0.080(3) -0.011(3) 0.0011(19) 0.003(2) C72 0.047(3) 0.061(6) 0.076(4) -0.007(4) 0.009(3) 0.006(4) C73 0.051(3) 0.051(5) 0.065(4) -0.002(4) 0.011(3) -0.001(4) C74 0.050(4) 0.079(7) 0.080(5) 0.000(5) 0.012(3) 0.004(4) C75 0.052(4) 0.089(7) 0.096(5) -0.014(6) 0.006(4) -0.008(5) C76 0.063(4) 0.087(7) 0.089(5) 0.000(6) -0.008(4) -0.012(5) C77 0.060(4) 0.089(8) 0.088(5) 0.008(5) -0.004(4) 0.006(5) C78 0.059(4) 0.070(6) 0.077(5) 0.004(5) 0.005(3) 0.001(4) C82 0.088(4) 0.126(6) 0.100(4) 0.004(5) 0.024(4) 0.024(4) C83 0.098(11) 0.113(11) 0.102(11) 0.003(8) 0.020(8) 0.005(8) C84 0.089(13) 0.093(14) 0.097(13) -0.001(9) 0.019(9) 0.004(9) C85 0.092(14) 0.098(15) 0.102(15) -0.003(9) 0.016(9) 0.000(9) C86 0.041(11) 0.084(12) 0.081(12) 0.001(9) 0.015(8) -0.008(9) C87 0.090(12) 0.110(12) 0.111(12) 0.002(9) 0.029(8) 0.006(9) C88 0.105(13) 0.112(13) 0.111(13) 0.001(9) 0.022(9) 0.007(9) _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_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 O1 . . 1.204(9) Y C1 O11 . . 1.309(8) Y C1 C2 . . 1.539(10) Y C2 O21 . . 1.421(7) Y C2 C3 . . 1.537(9) Y C2 H2 . . 1 ? C3 O31 . . 1.438(8) Y C3 C4 . . 1.518(10) Y C3 H3 . . 1 ? C4 O4 . . 1.214(10) Y C4 O5 . . 1.306(11) Y O5 C6 . . 1.461(8) Y C6 C7 . . 1.522(8) Y C6 C9 . . 1.522(8) Y C6 C10 . . 1.522(8) Y C6 C8 . . 1.522(8) Y C6 H6a . . 1 ? C6 H6b . . 1 ? C7 H7a . . 0.98 ? C7 H7b . . 0.98 ? C7 H7c . . 0.98 ? C8 H8a . . 0.98 ? C8 H8b . . 0.98 ? C8 H8c . . 0.98 ? C9 H9a . . 0.98 ? C9 H9b . . 0.98 ? C9 H9c . . 0.98 ? C10 H10a . . 0.98 ? C10 H10b . . 0.98 ? C10 H10c . . 0.98 ? O11 C12 . . 1.468(8) Y C12 H12a . . 0.98 ? C12 H12b . . 0.98 ? C12 H12c . . 0.98 ? O21 C22 . . 1.427(8) Y C22 O23 . . 1.421(7) Y C22 C27 . . 1.514(9) Y C22 H22 . . 1 ? O23 C24 . . 1.446(8) Y C24 C25 . . 1.499(10) Y C24 C41 . . 1.522(9) Y C24 H24 . . 1 ? C25 O51 . . 1.45(1) Y C25 C26 . . 1.548(9) Y C25 H25 . . 1 ? C26 O61 . . 1.382(8) Y C26 C27 . . 1.51(1) Y C26 H26 . . 1 ? C27 O71 . . 1.447(7) Y C27 H27 . . 1 ? O31 C32 . . 1.360(9) Y C32 O32 . . 1.215(10) Y C32 C33 . . 1.452(11) Y C33 C34 . . 1.397(11) Y C33 C38 . . 1.406(10) Y C34 C35 . . 1.370(11) Y C34 H34 . . 0.95 ? C35 C36 . . 1.397(10) Y C35 H35 . . 0.95 ? C36 C37 . . 1.353(13) Y C36 N36 . . 1.481(12) Y N36 O36 . . 1.204(10) Y N36 O37 . . 1.219(9) Y C37 C38 . . 1.375(12) Y C37 H37 . . 0.95 ? C38 H38 . . 0.95 ? C41 H41a . . 0.98 ? C41 H41b . . 0.98 ? C41 H41c . . 0.98 ? O51 C52 . . 1.428(7) Y O51 C82 . . 1.428(7) Y C52 C53 . . 1.436(9) Y C52 H22a . . 0.99 ? C52 H22b . . 0.99 ? C53 C54 . . 1.39 Y C53 C58 . . 1.39 Y C54 C55 . . 1.39 Y C54 H54 . . 0.95 ? C55 C56 . . 1.39 Y C55 H55 . . 0.95 ? C56 C57 . . 1.39 Y C56 H56 . . 0.95 ? C57 C58 . . 1.39 Y C57 H57 . . 0.95 ? C58 H58 . . 0.95 ? O61 C62 . . 1.417(10) Y C62 C63 . . 1.505(10) Y C62 H62a . . 0.99 ? C62 H62b . . 0.99 ? C63 C64 . . 1.367(11) Y C63 C68 . . 1.405(13) Y C64 C65 . . 1.419(11) Y C64 H64 . . 0.95 ? C65 C66 . . 1.356(14) Y C65 H65 . . 0.95 ? C66 C67 . . 1.379(14) Y C66 H66 . . 0.95 ? C67 C68 . . 1.418(12) Y C67 H67 . . 0.95 ? C68 H68 . . 0.95 ? O71 C72 . . 1.416(10) Y C72 C73 . . 1.520(9) Y C72 H72a . . 0.99 ? C72 H72b . . 0.99 ? C73 C78 . . 1.362(10) Y C73 C74 . . 1.382(11) Y C74 C75 . . 1.42(1) Y C74 H74 . . 0.95 ? C75 C76 . . 1.369(13) Y C75 H75 . . 0.95 ? C76 C77 . . 1.357(13) Y C76 H76 . . 0.95 ? C77 C78 . . 1.417(10) Y C77 H77 . . 0.95 ? C78 H78 . . 0.95 ? C82 C83 . . 1.436(9) Y C82 H82a . . 0.99 ? C82 H82b . . 0.99 ? C83 C84 . . 1.39 Y C83 C88 . . 1.39 Y C84 C85 . . 1.39 Y C84 H84 . . 0.95 ? C85 C86 . . 1.39 Y C85 H85 . . 0.95 ? C86 C87 . . 1.39 Y C86 H86 . . 0.95 ? C87 C88 . . 1.39 Y C87 H87 . . 0.95 ? C88 H88 . . 0.95 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 C1 O11 . . . 126.3(7) Y O1 C1 C2 . . . 123.3(6) Y O11 C1 C2 . . . 110.4(8) Y O21 C2 C3 . . . 105.5(5) Y O21 C2 C1 . . . 111.3(5) Y C3 C2 C1 . . . 109.7(7) Y O21 C2 H2 . . . 110.1 ? C3 C2 H2 . . . 110.1 ? C1 C2 H2 . . . 110.1 ? O31 C3 C4 . . . 110.5(6) Y O31 C3 C2 . . . 104.6(6) Y C4 C3 C2 . . . 111.6(5) Y O31 C3 H3 . . . 110 ? C4 C3 H3 . . . 110 ? C2 C3 H3 . . . 110 ? O4 C4 O5 . . . 125.6(7) Y O4 C4 C3 . . . 122.4(9) Y O5 C4 C3 . . . 111.9(7) Y C4 O5 C6 . . . 117.9(6) Y O5 C6 C7 . . . 108.3(6) Y O5 C6 C9 . . . 105(2) Y C7 C6 C9 . . . 81.9(17) Y O5 C6 C10 . . . 112.5(17) Y C7 C6 C10 . . . 132.5(17) Y C9 C6 C10 . . . 109.6(14) Y O5 C6 C8 . . . 104.9(6) Y C7 C6 C8 . . . 110.4(8) Y C9 C6 C8 . . . 30.7(16) Y C10 C6 C8 . . . 81.8(17) Y O5 C6 H6A . . . 111 ? C7 C6 H6A . . . 111 ? C9 C6 H6A . . . 134.8 ? C10 C6 H6A . . . 30.5 ? C8 C6 H6A . . . 111 ? O5 C6 H6B . . . 110 ? C7 C6 H6B . . . 30.2 ? C9 C6 H6B . . . 110 ? C10 C6 H6B . . . 110 ? C8 C6 H6B . . . 134.2 ? H6A C6 H6B . . . 83 ? C6 C7 H7A . . . 109.5 ? C6 C7 H7B . . . 109.5 ? H7A C7 H7B . . . 109.5 ? C6 C7 H7C . . . 109.5 ? H7A C7 H7C . . . 109.5 ? H7B C7 H7C . . . 109.5 ? C6 C8 H8A . . . 109.5 ? C6 C8 H8B . . . 109.5 ? H8A C8 H8B . . . 109.5 ? C6 C8 H8C . . . 109.5 ? H8A C8 H8C . . . 109.5 ? H8B C8 H8C . . . 109.5 ? C6 C9 H9A . . . 109.5 ? C6 C9 H9B . . . 109.5 ? H9A C9 H9B . . . 109.5 ? C6 C9 H9C . . . 109.5 ? H9A C9 H9C . . . 109.5 ? H9B C9 H9C . . . 109.5 ? C6 C10 H10A . . . 109.5 ? C6 C10 H10B . . . 109.5 ? H10A C10 H10B . . . 109.5 ? C6 C10 H10C . . . 109.5 ? H10A C10 H10C . . . 109.5 ? H10B C10 H10C . . . 109.5 ? C1 O11 C12 . . . 115.7(6) Y O11 C12 H12A . . . 109.5 ? O11 C12 H12B . . . 109.5 ? H12A C12 H12B . . . 109.5 ? O11 C12 H12C . . . 109.5 ? H12A C12 H12C . . . 109.5 ? H12B C12 H12C . . . 109.5 ? C2 O21 C22 . . . 112.3(5) Y O23 C22 O21 . . . 111.0(6) Y O23 C22 C27 . . . 111.1(5) Y O21 C22 C27 . . . 107.3(5) Y O23 C22 H22 . . . 109.1 ? O21 C22 H22 . . . 109.1 ? C27 C22 H22 . . . 109.1 ? C22 O23 C24 . . . 113.6(5) Y O23 C24 C25 . . . 110.9(6) Y O23 C24 C41 . . . 106.4(5) Y C25 C24 C41 . . . 113.7(6) Y O23 C24 H24 . . . 108.6 ? C25 C24 H24 . . . 108.6 ? C41 C24 H24 . . . 108.6 ? O51 C25 C24 . . . 107.1(5) Y O51 C25 C26 . . . 109.6(7) Y C24 C25 C26 . . . 110.1(5) Y O51 C25 H25 . . . 110 ? C24 C25 H25 . . . 110 ? C26 C25 H25 . . . 110 ? O61 C26 C27 . . . 109.9(6) Y O61 C26 C25 . . . 115.4(5) Y C27 C26 C25 . . . 108.6(5) Y O61 C26 H26 . . . 107.5 ? C27 C26 H26 . . . 107.5 ? C25 C26 H26 . . . 107.5 ? O71 C27 C26 . . . 110.3(5) Y O71 C27 C22 . . . 108.5(5) Y C26 C27 C22 . . . 112.5(6) Y O71 C27 H27 . . . 108.5 ? C26 C27 H27 . . . 108.5 ? C22 C27 H27 . . . 108.5 ? C32 O31 C3 . . . 115.0(7) Y O32 C32 O31 . . . 121.1(8) Y O32 C32 C33 . . . 126.1(7) Y O31 C32 C33 . . . 112.8(8) Y C34 C33 C38 . . . 119.7(7) Y C34 C33 C32 . . . 122.9(6) Y C38 C33 C32 . . . 117.4(8) Y C35 C34 C33 . . . 120.8(7) Y C35 C34 H34 . . . 119.6 ? C33 C34 H34 . . . 119.6 ? C34 C35 C36 . . . 117.8(8) Y C34 C35 H35 . . . 121.1 ? C36 C35 H35 . . . 121.1 ? C37 C36 C35 . . . 122.4(8) Y C37 C36 N36 . . . 120.2(7) Y C35 C36 N36 . . . 117.4(9) Y O36 N36 O37 . . . 122.6(9) Y O36 N36 C36 . . . 120.2(7) Y O37 N36 C36 . . . 117.2(1) Y C36 C37 C38 . . . 120.2(8) Y C36 C37 H37 . . . 119.9 ? C38 C37 H37 . . . 119.9 ? C37 C38 C33 . . . 119.0(9) Y C37 C38 H38 . . . 120.5 ? C33 C38 H38 . . . 120.5 ? C24 C41 H41A . . . 109.5 ? C24 C41 H41B . . . 109.5 ? H41A C41 H41B . . . 109.5 ? C24 C41 H41C . . . 109.5 ? H41A C41 H41C . . . 109.5 ? H41B C41 H41C . . . 109.5 ? C52 O51 C82 . . . 1.4(8) Y C52 O51 C25 . . . 116.7(7) Y C82 O51 C25 . . . 115.9(6) Y O51 C52 C53 . . . 110.0(6) Y O51 C52 H22A . . . 109.7 ? C53 C52 H22A . . . 109.7 ? O51 C52 H22B . . . 109.7 ? C53 C52 H22B . . . 109.7 ? H22A C52 H22B . . . 108.2 ? C54 C53 C58 . . . 120 Y C54 C53 C52 . . . 122.4(9) Y C58 C53 C52 . . . 117.4(9) Y C53 C54 C55 . . . 120 Y C53 C54 H54 . . . 120 ? C55 C54 H54 . . . 120 ? C56 C55 C54 . . . 120 Y C56 C55 H55 . . . 120 ? C54 C55 H55 . . . 120 ? C57 C56 C55 . . . 120 Y C57 C56 H56 . . . 120 ? C55 C56 H56 . . . 120 ? C58 C57 C56 . . . 120 Y C58 C57 H57 . . . 120 ? C56 C57 H57 . . . 120 ? C57 C58 C53 . . . 120 Y C57 C58 H58 . . . 120 ? C53 C58 H58 . . . 120 ? C26 O61 C62 . . . 117.3(7) Y O61 C62 C63 . . . 112.8(5) Y O61 C62 H62A . . . 109 ? C63 C62 H62A . . . 109 ? O61 C62 H62B . . . 109 ? C63 C62 H62B . . . 109 ? H62A C62 H62B . . . 107.8 ? C64 C63 C68 . . . 119.9(7) Y C64 C63 C62 . . . 117.3(9) Y C68 C63 C62 . . . 122.7(8) Y C63 C64 C65 . . . 120.8(9) Y C63 C64 H64 . . . 119.6 ? C65 C64 H64 . . . 119.6 ? C66 C65 C64 . . . 117.9(9) Y C66 C65 H65 . . . 121 ? C64 C65 H65 . . . 121 ? C65 C66 C67 . . . 124.0(9) Y C65 C66 H66 . . . 118 ? C67 C66 H66 . . . 118 ? C66 C67 C68 . . . 117.5(1) Y C66 C67 H67 . . . 121.3 ? C68 C67 H67 . . . 121.3 ? C63 C68 C67 . . . 119.9(9) Y C63 C68 H68 . . . 120.1 ? C67 C68 H68 . . . 120.1 ? C72 O71 C27 . . . 113.0(5) Y O71 C72 C73 . . . 110.0(6) Y O71 C72 H72A . . . 109.7 ? C73 C72 H72A . . . 109.7 ? O71 C72 H72B . . . 109.7 ? C73 C72 H72B . . . 109.7 ? H72A C72 H72B . . . 108.2 ? C78 C73 C74 . . . 120.6(7) Y C78 C73 C72 . . . 120.2(7) Y C74 C73 C72 . . . 118.9(7) Y C73 C74 C75 . . . 119.5(8) Y C73 C74 H74 . . . 120.2 ? C75 C74 H74 . . . 120.2 ? C76 C75 C74 . . . 119.0(9) Y C76 C75 H75 . . . 120.5 ? C74 C75 H75 . . . 120.5 ? C77 C76 C75 . . . 121.3(8) Y C77 C76 H76 . . . 119.4 ? C75 C76 H76 . . . 119.4 ? C76 C77 C78 . . . 120.0(8) Y C76 C77 H77 . . . 120 ? C78 C77 H77 . . . 120 ? C73 C78 C77 . . . 119.5(8) Y C73 C78 H78 . . . 120.3 ? C77 C78 H78 . . . 120.3 ? O51 C82 C83 . . . 109.9(6) Y O51 C82 H82A . . . 109.7 ? C83 C82 H82A . . . 109.7 ? O51 C82 H82B . . . 109.7 ? C83 C82 H82B . . . 109.7 ? H82A C82 H82B . . . 108.2 ? C84 C83 C88 . . . 120 Y C84 C83 C82 . . . 116.2(11) Y C88 C83 C82 . . . 123.8(11) Y C83 C84 C85 . . . 120 Y C83 C84 H84 . . . 120 ? C85 C84 H84 . . . 120 ? C86 C85 C84 . . . 120 Y C86 C85 H85 . . . 120 ? C84 C85 H85 . . . 120 ? C85 C86 C87 . . . 120 Y C85 C86 H86 . . . 120 ? C87 C86 H86 . . . 120 ? C88 C87 C86 . . . 120 Y C88 C87 H87 . . . 120 ? C86 C87 H87 . . . 120 ? C87 C88 C83 . . . 120 Y C87 C88 H88 . . . 120 ? C83 C88 H88 . . . 120 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C1 C2 O21 . . . . 53.7(9) Y O11 C1 C2 O21 . . . . -127.5(6) Y O1 C1 C2 C3 . . . . -62.7(8) Y O11 C1 C2 C3 . . . . 116.2(6) Y O21 C2 C3 O31 . . . . 56.3(7) Y C1 C2 C3 O31 . . . . 176.3(5) Y O21 C2 C3 C4 . . . . 175.9(7) Y C1 C2 C3 C4 . . . . -64.1(9) Y O31 C3 C4 O4 . . . . 25.4(1) Y C2 C3 C4 O4 . . . . -90.6(9) Y O31 C3 C4 O5 . . . . -158.6(6) Y C2 C3 C4 O5 . . . . 85.3(8) Y O4 C4 O5 C6 . . . . -0.3(11) Y C3 C4 O5 C6 . . . . -176.1(6) Y C4 O5 C6 C7 . . . . -78.6(9) Y C4 O5 C6 C9 . . . . -164.7(17) Y C4 O5 C6 C10 . . . . 76.3(19) Y C4 O5 C6 C8 . . . . 163.5(7) Y O1 C1 O11 C12 . . . . -0.7(1) Y C2 C1 O11 C12 . . . . -179.5(6) Y C3 C2 O21 C22 . . . . -167.4(6) Y C1 C2 O21 C22 . . . . 73.7(8) Y C2 O21 C22 O23 . . . . -76.0(6) Y C2 O21 C22 C27 . . . . 162.4(6) Y O21 C22 O23 C24 . . . . -62.9(7) Y C27 C22 O23 C24 . . . . 56.4(8) Y C22 O23 C24 C25 . . . . -59.4(7) Y C22 O23 C24 C41 . . . . 176.5(6) Y O23 C24 C25 O51 . . . . -61.7(7) Y C41 C24 C25 O51 . . . . 58.2(9) Y O23 C24 C25 C26 . . . . 57.4(8) Y C41 C24 C25 C26 . . . . 177.2(7) Y O51 C25 C26 O61 . . . . -60.7(8) Y C24 C25 C26 O61 . . . . -178.3(7) Y O51 C25 C26 C27 . . . . 63.2(7) Y C24 C25 C26 C27 . . . . -54.4(9) Y O61 C26 C27 O71 . . . . -58.9(7) Y C25 C26 C27 O71 . . . . 174.0(6) Y O61 C26 C27 C22 . . . . 179.8(5) Y C25 C26 C27 C22 . . . . 52.7(7) Y O23 C22 C27 O71 . . . . -176.2(6) Y O21 C22 C27 O71 . . . . -54.7(7) Y O23 C22 C27 C26 . . . . -53.8(7) Y O21 C22 C27 C26 . . . . 67.7(6) Y C4 C3 O31 C32 . . . . 67.9(8) Y C2 C3 O31 C32 . . . . -171.8(5) Y C3 O31 C32 O32 . . . . -2.2(1) Y C3 O31 C32 C33 . . . . 177.6(6) Y O32 C32 C33 C34 . . . . 173.2(8) Y O31 C32 C33 C34 . . . . -6.6(1) Y O32 C32 C33 C38 . . . . -7(12) Y O31 C32 C33 C38 . . . . 173.3(7) Y C38 C33 C34 C35 . . . . 0.6(12) Y C32 C33 C34 C35 . . . . -179.5(8) Y C33 C34 C35 C36 . . . . -3(12) Y C34 C35 C36 C37 . . . . 4.2(14) Y C34 C35 C36 N36 . . . . -177.4(8) Y C37 C36 N36 O36 . . . . 177.3(9) Y C35 C36 N36 O36 . . . . -1.1(13) Y C37 C36 N36 O37 . . . . -1.6(13) Y C35 C36 N36 O37 . . . . -180.0(8) Y C35 C36 C37 C38 . . . . -2.9(14) Y N36 C36 C37 C38 . . . . 178.8(8) Y C36 C37 C38 C33 . . . . 0.3(13) Y C34 C33 C38 C37 . . . . 0.8(12) Y C32 C33 C38 C37 . . . . -179.0(8) Y C24 C25 O51 C52 . . . . -149.4(8) Y C26 C25 O51 C52 . . . . 91.3(9) Y C24 C25 O51 C82 . . . . -148.2(6) Y C26 C25 O51 C82 . . . . 92.4(7) Y C82 O51 C52 C53 . . . . 99(18) Y C25 O51 C52 C53 . . . . 150.4(9) Y O51 C52 C53 C54 . . . . 108.4(1) Y O51 C52 C53 C58 . . . . -76.6(12) Y C58 C53 C54 C55 . . . . 0 Y C52 C53 C54 C55 . . . . 174.8(6) Y C53 C54 C55 C56 . . . . 0 Y C54 C55 C56 C57 . . . . 0 Y C55 C56 C57 C58 . . . . 0 Y C56 C57 C58 C53 . . . . 0 Y C54 C53 C58 C57 . . . . 0 Y C52 C53 C58 C57 . . . . -175.1(6) Y C27 C26 O61 C62 . . . . 147.4(5) Y C25 C26 O61 C62 . . . . -89.3(7) Y C26 O61 C62 C63 . . . . 95.7(8) Y O61 C62 C63 C64 . . . . 78.7(8) Y O61 C62 C63 C68 . . . . -100.2(1) Y C68 C63 C64 C65 . . . . 1.3(1) Y C62 C63 C64 C65 . . . . -177.6(7) Y C63 C64 C65 C66 . . . . 0.5(11) Y C64 C65 C66 C67 . . . . -2.1(13) Y C65 C66 C67 C68 . . . . 1.8(13) Y C64 C63 C68 C67 . . . . -1.7(11) Y C62 C63 C68 C67 . . . . 177.1(7) Y C66 C67 C68 C63 . . . . 0.2(11) Y C26 C27 O71 C72 . . . . 105.6(7) Y C22 C27 O71 C72 . . . . -130.8(6) Y C27 O71 C72 C73 . . . . -156.6(5) Y O71 C72 C73 C78 . . . . 46.4(8) Y O71 C72 C73 C74 . . . . -139.5(6) Y C78 C73 C74 C75 . . . . -1(1) Y C72 C73 C74 C75 . . . . -175.1(6) Y C73 C74 C75 C76 . . . . 1.9(11) Y C74 C75 C76 C77 . . . . -2.2(13) Y C75 C76 C77 C78 . . . . 1.6(13) Y C74 C73 C78 C77 . . . . 0.4(1) Y C72 C73 C78 C77 . . . . 174.4(6) Y C76 C77 C78 C73 . . . . -0.6(11) Y C52 O51 C82 C83 . . . . -70(18) Y C25 O51 C82 C83 . . . . 161(2) Y O51 C82 C83 C84 . . . . -6(3) Y O51 C82 C83 C88 . . . . 174(2) Y C88 C83 C84 C85 . . . . 0 Y C82 C83 C84 C85 . . . . 180(4) Y C83 C84 C85 C86 . . . . 0 Y C84 C85 C86 C87 . . . . 0 Y C85 C86 C87 C88 . . . . 0 Y C86 C87 C88 C83 . . . . 0 Y C84 C83 C88 C87 . . . . 0 Y C82 C83 C88 C87 . . . . -180(4) Y _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 60.55 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.315 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.078