# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Alessia Bacchi' _publ_contact_author_email ALESSIA.BACCHI@UNIPR.IT _publ_section_title ; Sampling rifamycin conformational variety by cruising through crystal forms: implications for polymorph screening and for biological models ; loop_ _publ_author_name 'Alessia Bacchi' 'Mauro Carcelli' 'Giancarlo Pelizzi' # Attachment 'B804746D_final.cif' ########################## # Sampling rifamycin conformational variety by cruising # through crystal froms: implications for polymorph screening # and for biological models # Alessia Bacchi, Mauro Carcelli, Giancarlo Pelizzi ################################# data_RSI _database_code_depnum_ccdc_archive 'CCDC 681840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H45 N O12' _chemical_formula_weight 695.74 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 0.0091 '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 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 24.605(6) _cell_length_b 14.569(4) _cell_length_c 10.318(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.82(2) _cell_angle_gamma 90.00 _cell_volume 3697(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method '\w/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14061 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 70.04 _reflns_number_total 13496 _reflns_number_gt 8227 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0911P)^2^+1.1464P] 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 SHELXL _refine_ls_extinction_coef 0.0045(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(2) _refine_ls_number_reflns 13496 _refine_ls_number_parameters 926 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.088 _refine_ls_shift/su_mean 0.002 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 N1 N 0.55177(15) 0.7384(3) 0.8557(4) 0.0693(10) Uani 1 1 d . . . H1 H 0.5428 0.7787 0.9120 0.083 Uiso 1 1 calc R . . O1 O 0.61539(13) 0.8648(2) 0.9614(3) 0.0720(9) Uani 1 1 d . . . O2 O 0.70540(15) 0.9486(3) 1.0006(4) 0.0880(11) Uani 1 1 d . . . H2 H 0.6724 0.9412 1.0018 0.132 Uiso 1 1 calc R . . O3 O 0.85582(14) 0.8416(3) 0.7741(3) 0.0793(10) Uani 1 1 d . . . O4 O 0.80296(16) 0.6686(3) 0.5697(4) 0.0928(12) Uani 1 1 d . . . O5 O 0.89767(14) 0.7942(3) 0.5855(4) 0.0853(10) Uani 1 1 d . . . O6 O 0.82838(17) 1.0426(3) 0.3561(5) 0.1054(14) Uani 1 1 d . . . O7 O 0.72935(15) 1.0838(2) 0.4417(4) 0.0790(10) Uani 1 1 d . . . O8 O 0.7612(3) 1.0890(4) 0.6474(6) 0.135(2) Uani 1 1 d . . . O9 O 0.64764(15) 1.0131(3) 0.6646(4) 0.0880(11) Uani 1 1 d . . . H9 H 0.6804 1.0235 0.6696 0.132 Uiso 1 1 calc R . . O10 O 0.55276(18) 0.9427(3) 0.7383(4) 0.1008(13) Uani 1 1 d . . . H10 H 0.5842 0.9574 0.7567 0.151 Uiso 1 1 calc R . . O11 O 0.52389(15) 0.6062(3) 0.7584(4) 0.0847(10) Uani 1 1 d . . . O12 O 0.69058(15) 0.6866(3) 0.5573(4) 0.0916(12) Uani 1 1 d . . . C1 C 0.63636(19) 0.8189(3) 0.8738(5) 0.0610(11) Uani 1 1 d . . . C2 C 0.60327(18) 0.7473(3) 0.8076(5) 0.0621(11) Uani 1 1 d . . . C3 C 0.62307(19) 0.6992(3) 0.7090(5) 0.0664(12) Uani 1 1 d . . . H3 H 0.6020 0.6536 0.6692 0.080 Uiso 1 1 calc R . . C4 C 0.67732(19) 0.7179(3) 0.6640(5) 0.0661(12) Uani 1 1 d . . . C5 C 0.77048(19) 0.7823(3) 0.7235(4) 0.0609(11) Uani 1 1 d . . . C6 C 0.80131(19) 0.8434(4) 0.7983(5) 0.0681(12) Uani 1 1 d . . . C7 C 0.7816(2) 0.9021(4) 0.8894(5) 0.0699(13) Uani 1 1 d . . . C8 C 0.7262(2) 0.8943(3) 0.9085(5) 0.0690(12) Uani 1 1 d . . . C9 C 0.69246(18) 0.8320(3) 0.8372(4) 0.0574(10) Uani 1 1 d . . . C10 C 0.71461(18) 0.7771(3) 0.7415(4) 0.0581(10) Uani 1 1 d . . . C11 C 0.8089(2) 0.7310(4) 0.6463(5) 0.0719(13) Uani 1 1 d . . . C12 C 0.8651(2) 0.7654(4) 0.6884(5) 0.0765(14) Uani 1 1 d . . . C13 C 0.8962(3) 0.6902(5) 0.7606(7) 0.108(2) Uani 1 1 d . . . H13A H 0.9319 0.7119 0.7848 0.161 Uiso 1 1 calc R . . H13B H 0.8991 0.6374 0.7055 0.161 Uiso 1 1 calc R . . H13C H 0.8773 0.6736 0.8371 0.161 Uiso 1 1 calc R . . C14 C 0.8181(3) 0.9658(6) 0.9644(7) 0.127(3) Uani 1 1 d . . . H14A H 0.8195 1.0238 0.9204 0.190 Uiso 1 1 calc R . . H14B H 0.8540 0.9400 0.9715 0.190 Uiso 1 1 calc R . . H14C H 0.8043 0.9747 1.0495 0.190 Uiso 1 1 calc R . . C15 C 0.5134(2) 0.6739(4) 0.8250(5) 0.0682(12) Uani 1 1 d . . . C16 C 0.4591(2) 0.6876(4) 0.8813(5) 0.0748(13) Uani 1 1 d . . . C17 C 0.4289(2) 0.7605(4) 0.8514(6) 0.0888(17) Uani 1 1 d . . . H17 H 0.3956 0.7641 0.8916 0.107 Uiso 1 1 calc R . . C18 C 0.4411(2) 0.8364(4) 0.7631(6) 0.0895(17) Uani 1 1 d . . . H18 H 0.4271 0.8935 0.7844 0.107 Uiso 1 1 calc R . . C19 C 0.4698(2) 0.8329(4) 0.6565(6) 0.0821(15) Uani 1 1 d . . . H19 H 0.4812 0.7753 0.6296 0.099 Uiso 1 1 calc R . . C20 C 0.4854(2) 0.9126(4) 0.5764(6) 0.0772(14) Uani 1 1 d . . . H20 H 0.4635 0.9652 0.6026 0.093 Uiso 1 1 calc R . . C21 C 0.5453(2) 0.9376(4) 0.6001(5) 0.0715(13) Uani 1 1 d . . . H21 H 0.5674 0.8866 0.5691 0.086 Uiso 1 1 calc R . . C22 C 0.5647(2) 1.0248(3) 0.5366(6) 0.0743(13) Uani 1 1 d . . . H22 H 0.5518 1.0222 0.4458 0.089 Uiso 1 1 calc R . . C23 C 0.6273(2) 1.0335(4) 0.5351(5) 0.0718(13) Uani 1 1 d . . . H23 H 0.6358 1.0979 0.5173 0.086 Uiso 1 1 calc R . . C24 C 0.6555(2) 0.9753(4) 0.4347(5) 0.0709(13) Uani 1 1 d . . . H24 H 0.6463 0.9108 0.4504 0.085 Uiso 1 1 calc R . . C25 C 0.7176(2) 0.9854(3) 0.4489(5) 0.0695(13) Uani 1 1 d . . . H25 H 0.7296 0.9625 0.5343 0.083 Uiso 1 1 calc R . . C26 C 0.7513(2) 0.9402(4) 0.3456(5) 0.0739(13) Uani 1 1 d . . . H26 H 0.7417 0.9710 0.2636 0.089 Uiso 1 1 calc R . . C27 C 0.8129(2) 0.9491(4) 0.3645(6) 0.0819(15) Uani 1 1 d . . . H27 H 0.8293 0.9170 0.2920 0.098 Uiso 1 1 calc R . . C28 C 0.8353(2) 0.9058(4) 0.4872(6) 0.0809(15) Uani 1 1 d . . . H28 H 0.8213 0.9233 0.5661 0.097 Uiso 1 1 calc R . . C29 C 0.8736(2) 0.8447(4) 0.4861(6) 0.0853(15) Uani 1 1 d . . . H29 H 0.8872 0.8329 0.4047 0.102 Uiso 1 1 calc R . . C30 C 0.4417(3) 0.6122(5) 0.9697(6) 0.1004(19) Uani 1 1 d . . . H30A H 0.4396 0.5555 0.9224 0.151 Uiso 1 1 calc R . . H30B H 0.4067 0.6265 1.0029 0.151 Uiso 1 1 calc R . . H30C H 0.4678 0.6062 1.0404 0.151 Uiso 1 1 calc R . . C31 C 0.4730(3) 0.8949(5) 0.4309(7) 0.110(2) Uani 1 1 d . . . H31A H 0.4376 0.8677 0.4201 0.165 Uiso 1 1 calc R . . H31B H 0.4998 0.8540 0.3978 0.165 Uiso 1 1 calc R . . H31C H 0.4739 0.9520 0.3845 0.165 Uiso 1 1 calc R . . C32 C 0.5400(3) 1.1103(4) 0.5945(7) 0.0967(19) Uani 1 1 d . . . H32A H 0.5012 1.1087 0.5814 0.145 Uiso 1 1 calc R . . H32B H 0.5542 1.1638 0.5530 0.145 Uiso 1 1 calc R . . H32C H 0.5489 1.1127 0.6857 0.145 Uiso 1 1 calc R . . C33 C 0.6337(3) 1.0011(6) 0.2972(6) 0.105(2) Uani 1 1 d . . . H33A H 0.6559 0.9726 0.2337 0.157 Uiso 1 1 calc R . . H33B H 0.6349 1.0665 0.2867 0.157 Uiso 1 1 calc R . . H33C H 0.5969 0.9801 0.2857 0.157 Uiso 1 1 calc R . . C34 C 0.7365(3) 0.8396(4) 0.3274(7) 0.0923(17) Uani 1 1 d . . . H34A H 0.7398 0.8084 0.4093 0.138 Uiso 1 1 calc R . . H34B H 0.7606 0.8119 0.2673 0.138 Uiso 1 1 calc R . . H34C H 0.6997 0.8348 0.2942 0.138 Uiso 1 1 calc R . . C35 C 0.7546(3) 1.1242(4) 0.5423(8) 0.0897(17) Uani 1 1 d . . . C36 C 0.7731(3) 1.2193(4) 0.5073(9) 0.122(3) Uani 1 1 d . . . H36A H 0.7821 1.2530 0.5850 0.183 Uiso 1 1 calc R . . H36B H 0.7445 1.2502 0.4594 0.183 Uiso 1 1 calc R . . H36C H 0.8047 1.2151 0.4551 0.183 Uiso 1 1 calc R . . C37 C 0.8820(3) 1.0558(7) 0.3198(9) 0.141(3) Uani 1 1 d . . . H37A H 0.8881 1.1199 0.3047 0.211 Uiso 1 1 calc R . . H37B H 0.8883 1.0220 0.2418 0.211 Uiso 1 1 calc R . . H37C H 0.9064 1.0346 0.3878 0.211 Uiso 1 1 calc R . . N1A N 0.94837(15) 0.6480(3) 0.3538(4) 0.0694(10) Uani 1 1 d . . . H1A H 0.9595 0.6087 0.4109 0.083 Uiso 1 1 calc R . . O1A O 0.88733(13) 0.5240(2) 0.4658(3) 0.0735(9) Uani 1 1 d . . . O2A O 0.79767(15) 0.4460(3) 0.5158(4) 0.0786(10) Uani 1 1 d . . . H2A H 0.8292 0.4628 0.5282 0.118 Uiso 1 1 calc R . . O3A O 0.64177(13) 0.5410(2) 0.2720(3) 0.0703(8) Uani 1 1 d . . . O4A O 0.69086(14) 0.7015(3) 0.0488(4) 0.0866(11) Uani 1 1 d . . . O5A O 0.59684(13) 0.5768(3) 0.0758(4) 0.0753(9) Uani 1 1 d . . . O6A O 0.65940(17) 0.3179(3) -0.1061(4) 0.0935(12) Uani 1 1 d . . . O7A O 0.76249(15) 0.2894(2) -0.0114(4) 0.0765(9) Uani 1 1 d . . . O8A O 0.7439(2) 0.3175(4) 0.1969(5) 0.1230(17) Uani 1 1 d . . . O9A O 0.85387(16) 0.3837(4) 0.1786(4) 0.0990(13) Uani 1 1 d . . . H9A H 0.8261 0.3579 0.2012 0.148 Uiso 1 1 calc R . . O10A O 0.95298(18) 0.4363(4) 0.2546(4) 0.0986(13) Uani 1 1 d . . . H10A H 0.9246 0.4113 0.2747 0.148 Uiso 1 1 calc R . . O11A O 0.97112(17) 0.7800(3) 0.2516(4) 0.0946(12) Uani 1 1 d . . . O12A O 0.80236(16) 0.6846(3) 0.0456(4) 0.0973(13) Uani 1 1 d . . . C1A C 0.86379(18) 0.5671(3) 0.3758(5) 0.0604(11) Uani 1 1 d . . . C2A C 0.89563(18) 0.6367(3) 0.3045(5) 0.0623(11) Uani 1 1 d . . . C3A C 0.8734(2) 0.6795(4) 0.2004(5) 0.0705(12) Uani 1 1 d . . . H3A H 0.8936 0.7234 0.1576 0.085 Uiso 1 1 calc R . . C4A C 0.81832(19) 0.6588(3) 0.1531(5) 0.0664(12) Uani 1 1 d . . . C5A C 0.72649(18) 0.5988(3) 0.2175(4) 0.0594(11) Uani 1 1 d . . . C6A C 0.69679(18) 0.5414(3) 0.2994(4) 0.0600(11) Uani 1 1 d . . . C7A C 0.7186(2) 0.4884(3) 0.3977(5) 0.0629(11) Uani 1 1 d . . . C8A C 0.7743(2) 0.4956(3) 0.4175(4) 0.0612(11) Uani 1 1 d . . . C9A C 0.80705(18) 0.5535(3) 0.3415(4) 0.0566(10) Uani 1 1 d . . . C10A C 0.78306(18) 0.6040(3) 0.2381(4) 0.0594(10) Uani 1 1 d . . . C11A C 0.6865(2) 0.6443(3) 0.1335(5) 0.0672(12) Uani 1 1 d . . . C12A C 0.6302(2) 0.6122(4) 0.1745(5) 0.0682(12) Uani 1 1 d . . . C13A C 0.5995(2) 0.6879(4) 0.2404(6) 0.0864(16) Uani 1 1 d . . . H13D H 0.6187 0.7052 0.3191 0.130 Uiso 1 1 calc R . . H13E H 0.5638 0.6666 0.2603 0.130 Uiso 1 1 calc R . . H13F H 0.5965 0.7400 0.1837 0.130 Uiso 1 1 calc R . . C14A C 0.6830(2) 0.4308(4) 0.4809(6) 0.0841(16) Uani 1 1 d . . . H14D H 0.6705 0.3781 0.4326 0.126 Uiso 1 1 calc R . . H14E H 0.6523 0.4663 0.5064 0.126 Uiso 1 1 calc R . . H14F H 0.7034 0.4111 0.5567 0.126 Uiso 1 1 calc R . . C15A C 0.9844(2) 0.7147(4) 0.3212(5) 0.0733(13) Uani 1 1 d . . . C16A C 1.0410(2) 0.7051(4) 0.3786(6) 0.0808(15) Uani 1 1 d . . . C17A C 1.0726(2) 0.6355(5) 0.3487(6) 0.0875(16) Uani 1 1 d . . . H17A H 1.1078 0.6374 0.3842 0.105 Uiso 1 1 calc R . . C18A C 1.0597(2) 0.5561(5) 0.2674(7) 0.0909(17) Uani 1 1 d . . . H18A H 1.0747 0.5003 0.2936 0.109 Uiso 1 1 calc R . . C19A C 1.0289(2) 0.5556(4) 0.1609(6) 0.0784(14) Uani 1 1 d . . . H19A H 1.0167 0.6122 0.1301 0.094 Uiso 1 1 calc R . . C20A C 1.0118(2) 0.4725(4) 0.0842(6) 0.0782(14) Uani 1 1 d . . . H20A H 1.0359 0.4216 0.1095 0.094 Uiso 1 1 calc R . . C21A C 0.9538(2) 0.4457(4) 0.1160(5) 0.0722(13) Uani 1 1 d . . . H21A H 0.9298 0.4968 0.0908 0.087 Uiso 1 1 calc R . . C22A C 0.9323(2) 0.3593(4) 0.0485(6) 0.0801(15) Uani 1 1 d . . . H22A H 0.9408 0.3645 -0.0433 0.096 Uiso 1 1 calc R . . C23A C 0.8698(2) 0.3473(4) 0.0557(5) 0.0732(13) Uani 1 1 d . . . H23A H 0.8621 0.2813 0.0558 0.088 Uiso 1 1 calc R . . C24A C 0.8370(2) 0.3899(4) -0.0567(5) 0.0743(13) Uani 1 1 d . . . H24A H 0.8474 0.4546 -0.0626 0.089 Uiso 1 1 calc R . . C25A C 0.7758(2) 0.3859(3) -0.0351(5) 0.0673(12) Uani 1 1 d . . . H25A H 0.7681 0.4212 0.0431 0.081 Uiso 1 1 calc R . . C26A C 0.7379(2) 0.4196(4) -0.1451(5) 0.0709(13) Uani 1 1 d . . . H26A H 0.7457 0.3830 -0.2220 0.085 Uiso 1 1 calc R . . C27A C 0.6774(2) 0.4105(4) -0.1226(5) 0.0747(13) Uani 1 1 d . . . H27A H 0.6579 0.4355 -0.1992 0.090 Uiso 1 1 calc R . . C28A C 0.6587(2) 0.4621(4) -0.0074(5) 0.0700(12) Uani 1 1 d . . . H28A H 0.6753 0.4515 0.0735 0.084 Uiso 1 1 calc R . . C29A C 0.6187(2) 0.5225(4) -0.0186(5) 0.0740(13) Uani 1 1 d . . . H29A H 0.6033 0.5292 -0.1015 0.089 Uiso 1 1 calc R . . C30A C 1.0588(3) 0.7850(5) 0.4609(7) 0.105(2) Uani 1 1 d . . . H30D H 1.0947 0.7738 0.4966 0.158 Uiso 1 1 calc R . . H30E H 1.0340 0.7930 0.5300 0.158 Uiso 1 1 calc R . . H30F H 1.0591 0.8396 0.4088 0.158 Uiso 1 1 calc R . . C31A C 1.0174(3) 0.4897(6) -0.0605(7) 0.114(2) Uani 1 1 d . . . H31D H 1.0178 0.4321 -0.1056 0.171 Uiso 1 1 calc R . . H31E H 1.0507 0.5221 -0.0746 0.171 Uiso 1 1 calc R . . H31F H 0.9872 0.5259 -0.0924 0.171 Uiso 1 1 calc R . . C32A C 0.9613(3) 0.2733(5) 0.1012(11) 0.143(3) Uani 1 1 d . . . H32D H 0.9473 0.2201 0.0563 0.214 Uiso 1 1 calc R . . H32E H 0.9550 0.2673 0.1922 0.214 Uiso 1 1 calc R . . H32F H 0.9996 0.2785 0.0882 0.214 Uiso 1 1 calc R . . C33A C 0.8517(3) 0.3429(7) -0.1844(6) 0.123(3) Uani 1 1 d . . . H33D H 0.8284 0.3655 -0.2536 0.184 Uiso 1 1 calc R . . H33E H 0.8470 0.2778 -0.1764 0.184 Uiso 1 1 calc R . . H33F H 0.8889 0.3561 -0.2030 0.184 Uiso 1 1 calc R . . C34A C 0.7512(3) 0.5199(4) -0.1773(6) 0.0918(17) Uani 1 1 d . . . H34D H 0.7850 0.5225 -0.2208 0.138 Uiso 1 1 calc R . . H34E H 0.7540 0.5549 -0.0986 0.138 Uiso 1 1 calc R . . H34F H 0.7228 0.5448 -0.2327 0.138 Uiso 1 1 calc R . . C35A C 0.7442(2) 0.2644(4) 0.1082(7) 0.0851(16) Uani 1 1 d . . . C36A C 0.7282(3) 0.1664(5) 0.1073(10) 0.138(3) Uani 1 1 d . . . H36D H 0.7330 0.1413 0.0224 0.207 Uiso 1 1 calc R . . H36E H 0.6908 0.1611 0.1296 0.207 Uiso 1 1 calc R . . H36F H 0.7506 0.1333 0.1693 0.207 Uiso 1 1 calc R . . C37A C 0.6537(7) 0.2646(11) -0.2057(9) 0.320(13) Uani 1 1 d . . . H37D H 0.6493 0.3010 -0.2829 0.479 Uiso 1 1 calc R . . H37E H 0.6222 0.2266 -0.1963 0.479 Uiso 1 1 calc R . . H37F H 0.6854 0.2265 -0.2120 0.479 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.061(2) 0.069(2) 0.078(3) -0.005(2) 0.0030(19) -0.008(2) O1 0.066(2) 0.071(2) 0.079(2) -0.0130(17) 0.0044(16) 0.0069(16) O2 0.085(2) 0.092(3) 0.088(2) -0.038(2) 0.015(2) -0.010(2) O3 0.062(2) 0.089(2) 0.088(2) -0.020(2) 0.0098(17) -0.0127(18) O4 0.077(2) 0.089(3) 0.112(3) -0.034(2) 0.013(2) 0.001(2) O5 0.064(2) 0.097(3) 0.096(3) -0.008(2) 0.0183(19) 0.0066(19) O6 0.097(3) 0.080(3) 0.142(4) 0.004(3) 0.049(3) -0.018(2) O7 0.083(2) 0.0514(18) 0.102(3) -0.0068(18) 0.002(2) -0.0047(16) O8 0.179(5) 0.116(4) 0.108(4) -0.024(3) -0.036(4) -0.014(4) O9 0.076(2) 0.116(3) 0.072(2) -0.008(2) -0.0024(17) 0.006(2) O10 0.111(3) 0.104(3) 0.086(3) 0.029(2) -0.017(2) -0.025(3) O11 0.076(2) 0.071(2) 0.107(3) -0.013(2) 0.008(2) -0.0049(18) O12 0.080(2) 0.108(3) 0.087(3) -0.039(2) 0.0128(19) -0.014(2) C1 0.063(3) 0.054(2) 0.066(3) 0.000(2) 0.001(2) 0.007(2) C2 0.052(2) 0.062(3) 0.071(3) -0.002(2) -0.006(2) 0.000(2) C3 0.063(3) 0.062(3) 0.073(3) -0.009(2) -0.001(2) 0.001(2) C4 0.063(3) 0.065(3) 0.070(3) -0.012(2) 0.001(2) -0.002(2) C5 0.062(3) 0.059(3) 0.062(3) -0.004(2) -0.003(2) -0.003(2) C6 0.059(3) 0.071(3) 0.075(3) -0.009(2) 0.009(2) -0.003(2) C7 0.068(3) 0.076(3) 0.066(3) -0.016(2) 0.007(2) -0.015(2) C8 0.078(3) 0.062(3) 0.067(3) -0.017(2) 0.003(2) -0.007(2) C9 0.058(2) 0.050(2) 0.064(3) -0.005(2) 0.002(2) 0.0007(19) C10 0.063(3) 0.051(2) 0.060(2) -0.004(2) -0.001(2) 0.001(2) C11 0.066(3) 0.066(3) 0.084(3) -0.017(3) 0.007(2) 0.001(2) C12 0.064(3) 0.083(4) 0.084(3) -0.010(3) 0.011(3) 0.001(3) C13 0.082(4) 0.112(5) 0.128(6) 0.008(4) -0.007(4) 0.010(4) C14 0.093(5) 0.160(7) 0.129(6) -0.071(5) 0.014(4) -0.052(5) C15 0.063(3) 0.063(3) 0.079(3) -0.001(2) -0.001(2) -0.004(2) C16 0.063(3) 0.077(3) 0.084(3) 0.002(3) 0.010(2) -0.006(3) C17 0.061(3) 0.088(4) 0.119(5) 0.010(4) 0.022(3) 0.002(3) C18 0.064(3) 0.083(4) 0.122(5) 0.021(4) 0.022(3) 0.009(3) C19 0.074(3) 0.070(3) 0.103(4) 0.003(3) 0.000(3) 0.001(3) C20 0.069(3) 0.068(3) 0.095(4) 0.006(3) 0.001(3) 0.005(2) C21 0.073(3) 0.064(3) 0.077(3) 0.007(2) -0.005(2) 0.002(2) C22 0.072(3) 0.057(3) 0.095(4) 0.010(3) 0.004(3) 0.006(2) C23 0.074(3) 0.064(3) 0.077(3) 0.004(2) 0.001(2) 0.001(2) C24 0.076(3) 0.067(3) 0.070(3) -0.005(2) 0.007(2) -0.004(2) C25 0.075(3) 0.048(2) 0.086(3) -0.005(2) 0.005(3) -0.003(2) C26 0.084(3) 0.059(3) 0.080(3) -0.003(2) 0.017(3) 0.003(2) C27 0.083(4) 0.067(3) 0.098(4) -0.004(3) 0.024(3) -0.005(3) C28 0.072(3) 0.083(4) 0.089(4) -0.012(3) 0.021(3) 0.004(3) C29 0.082(4) 0.082(4) 0.094(4) -0.003(3) 0.018(3) -0.002(3) C30 0.092(4) 0.103(5) 0.106(5) 0.027(4) 0.011(3) -0.014(4) C31 0.110(5) 0.117(5) 0.102(5) 0.016(4) -0.022(4) -0.026(4) C32 0.090(4) 0.063(3) 0.139(5) -0.002(3) 0.019(4) 0.015(3) C33 0.088(4) 0.153(7) 0.074(4) 0.004(4) -0.003(3) 0.003(4) C34 0.100(4) 0.071(3) 0.107(4) -0.021(3) 0.018(3) -0.007(3) C35 0.087(4) 0.074(4) 0.107(5) -0.020(4) -0.008(4) 0.002(3) C36 0.108(5) 0.067(4) 0.189(8) -0.019(4) -0.018(5) -0.012(3) C37 0.124(6) 0.139(7) 0.164(7) -0.015(6) 0.069(5) -0.053(5) N1A 0.057(2) 0.069(3) 0.082(3) 0.008(2) 0.0040(19) -0.0069(19) O1A 0.0638(19) 0.073(2) 0.083(2) 0.0096(18) 0.0009(16) 0.0086(16) O2A 0.079(2) 0.072(2) 0.083(2) 0.0240(19) -0.0083(18) -0.0054(18) O3A 0.0593(18) 0.072(2) 0.079(2) 0.0112(17) 0.0019(15) -0.0074(16) O4A 0.075(2) 0.082(3) 0.102(3) 0.034(2) 0.0005(19) 0.0012(19) O5A 0.0607(19) 0.079(2) 0.086(2) -0.0015(19) -0.0035(17) 0.0042(16) O6A 0.101(3) 0.071(2) 0.107(3) -0.022(2) -0.017(2) -0.008(2) O7A 0.087(2) 0.0529(18) 0.088(2) 0.0028(17) -0.0073(19) -0.0040(17) O8A 0.164(5) 0.098(4) 0.109(4) 0.020(3) 0.035(3) 0.000(3) O9A 0.073(3) 0.148(4) 0.076(2) -0.021(3) 0.0097(19) 0.004(2) O10A 0.103(3) 0.117(3) 0.076(2) -0.007(2) 0.012(2) -0.028(3) O11A 0.085(3) 0.073(2) 0.126(3) 0.014(2) 0.005(2) -0.010(2) O12A 0.083(2) 0.129(4) 0.078(2) 0.034(2) -0.007(2) -0.013(2) C1A 0.056(3) 0.056(2) 0.069(3) 0.001(2) 0.004(2) 0.004(2) C2A 0.059(3) 0.062(3) 0.065(3) 0.001(2) 0.002(2) -0.001(2) C3A 0.064(3) 0.067(3) 0.081(3) 0.002(3) 0.006(2) -0.004(2) C4A 0.061(3) 0.065(3) 0.072(3) 0.006(2) 0.004(2) -0.004(2) C5A 0.062(3) 0.051(2) 0.065(3) 0.004(2) 0.002(2) -0.006(2) C6A 0.060(3) 0.054(2) 0.066(3) 0.001(2) 0.002(2) -0.004(2) C7A 0.066(3) 0.060(3) 0.063(3) 0.005(2) 0.002(2) -0.006(2) C8A 0.068(3) 0.053(2) 0.063(3) 0.005(2) 0.002(2) -0.001(2) C9A 0.059(2) 0.048(2) 0.063(3) 0.0040(19) 0.0023(19) -0.0009(19) C10A 0.060(3) 0.052(2) 0.067(3) -0.002(2) 0.003(2) -0.001(2) C11A 0.070(3) 0.058(3) 0.074(3) 0.009(2) -0.001(2) 0.004(2) C12A 0.063(3) 0.065(3) 0.076(3) 0.008(2) 0.000(2) -0.002(2) C13A 0.076(3) 0.078(4) 0.105(4) -0.008(3) 0.012(3) 0.009(3) C14A 0.085(4) 0.084(4) 0.083(4) 0.026(3) 0.006(3) -0.020(3) C15A 0.071(3) 0.065(3) 0.084(3) 0.003(3) 0.014(3) -0.004(2) C16A 0.065(3) 0.084(4) 0.094(4) -0.009(3) 0.008(3) -0.014(3) C17A 0.062(3) 0.095(4) 0.106(4) -0.010(4) 0.000(3) -0.004(3) C18A 0.059(3) 0.085(4) 0.129(5) -0.012(4) 0.003(3) 0.006(3) C19A 0.072(3) 0.074(3) 0.089(4) -0.007(3) 0.010(3) -0.002(3) C20A 0.068(3) 0.077(3) 0.090(4) -0.004(3) 0.016(3) 0.000(3) C21A 0.077(3) 0.068(3) 0.071(3) 0.001(2) 0.007(2) 0.004(3) C22A 0.069(3) 0.074(3) 0.097(4) -0.019(3) 0.008(3) 0.003(3) C23A 0.076(3) 0.077(3) 0.068(3) -0.012(3) 0.009(2) 0.000(3) C24A 0.075(3) 0.078(3) 0.070(3) 0.000(3) 0.007(2) -0.005(3) C25A 0.077(3) 0.053(3) 0.072(3) 0.002(2) 0.000(2) -0.005(2) C26A 0.086(3) 0.070(3) 0.057(3) 0.001(2) -0.002(2) -0.001(3) C27A 0.080(3) 0.066(3) 0.077(3) 0.000(3) -0.009(3) 0.006(3) C28A 0.073(3) 0.069(3) 0.067(3) -0.009(2) -0.007(2) 0.002(2) C29A 0.071(3) 0.076(3) 0.074(3) -0.001(3) -0.007(2) 0.007(3) C30A 0.095(4) 0.100(5) 0.121(5) -0.031(4) 0.002(4) -0.018(4) C31A 0.124(5) 0.121(6) 0.100(5) -0.015(4) 0.042(4) -0.027(4) C32A 0.088(5) 0.072(4) 0.267(11) -0.023(6) -0.009(6) 0.021(4) C33A 0.104(5) 0.197(9) 0.068(4) -0.037(5) 0.000(3) 0.029(5) C34A 0.108(5) 0.070(4) 0.097(4) 0.017(3) -0.001(3) 0.003(3) C35A 0.082(4) 0.058(3) 0.116(5) 0.027(3) 0.011(3) -0.003(3) C36A 0.118(6) 0.078(4) 0.217(9) 0.055(5) -0.008(6) -0.019(4) C37A 0.56(3) 0.285(17) 0.107(7) 0.031(9) -0.094(12) -0.31(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C15 1.362(6) . ? N1 C2 1.381(6) . ? O1 C1 1.249(5) . ? O2 C8 1.349(6) . ? O3 C6 1.372(6) . ? O3 C12 1.442(6) . ? O4 C11 1.210(6) . ? O5 C29 1.380(7) . ? O5 C12 1.415(6) . ? O6 C37 1.395(8) . ? O6 C27 1.418(7) . ? O7 C35 1.330(7) . ? O7 C25 1.465(6) . ? O8 C35 1.206(8) . ? O9 C23 1.443(6) . ? O10 C21 1.434(6) . ? O11 C15 1.234(6) . ? O12 C4 1.245(6) . ? C1 C9 1.455(6) . ? C1 C2 1.478(6) . ? C2 C3 1.339(6) . ? C3 C4 1.453(7) . ? C4 C10 1.475(6) . ? C5 C6 1.388(6) . ? C5 C10 1.395(6) . ? C5 C11 1.461(7) . ? C6 C7 1.371(7) . ? C7 C8 1.387(7) . ? C7 C14 1.492(7) . ? C8 C9 1.419(6) . ? C9 C10 1.396(6) . ? C11 C12 1.520(7) . ? C12 C13 1.519(9) . ? C15 C16 1.489(7) . ? C16 C17 1.327(8) . ? C16 C30 1.499(8) . ? C17 C18 1.470(8) . ? C18 C19 1.327(8) . ? C19 C20 1.482(8) . ? C20 C21 1.531(7) . ? C20 C31 1.544(8) . ? C21 C22 1.513(7) . ? C22 C32 1.518(7) . ? C22 C23 1.544(7) . ? C23 C24 1.523(7) . ? C24 C25 1.537(7) . ? C24 C33 1.547(8) . ? C25 C26 1.522(7) . ? C26 C34 1.521(8) . ? C26 C27 1.527(8) . ? C27 C28 1.503(8) . ? C28 C29 1.297(8) . ? C35 C36 1.506(9) . ? N1A C15A 1.365(6) . ? N1A C2A 1.388(6) . ? O1A C1A 1.248(5) . ? O2A C8A 1.359(5) . ? O3A C6A 1.374(5) . ? O3A C12A 1.467(6) . ? O4A C11A 1.216(6) . ? O5A C29A 1.378(6) . ? O5A C12A 1.387(6) . ? O6A C37A 1.293(12) . ? O6A C27A 1.432(7) . ? O7A C35A 1.375(7) . ? O7A C25A 1.466(6) . ? O8A C35A 1.198(8) . ? O9A C23A 1.440(6) . ? O10A C21A 1.437(6) . ? O11A C15A 1.229(6) . ? O12A C4A 1.224(6) . ? C1A C9A 1.443(6) . ? C1A C2A 1.490(6) . ? C2A C3A 1.343(7) . ? C3A C4A 1.457(7) . ? C4A C10A 1.486(6) . ? C5A C10A 1.403(6) . ? C5A C6A 1.409(6) . ? C5A C11A 1.451(7) . ? C6A C7A 1.371(6) . ? C7A C8A 1.382(7) . ? C7A C14A 1.502(7) . ? C8A C9A 1.420(6) . ? C9A C10A 1.410(6) . ? C11A C12A 1.534(7) . ? C12A C13A 1.511(7) . ? C15A C16A 1.503(8) . ? C16A C17A 1.320(8) . ? C16A C30A 1.499(8) . ? C17A C18A 1.457(9) . ? C18A C19A 1.314(8) . ? C19A C20A 1.500(8) . ? C20A C31A 1.524(8) . ? C20A C21A 1.526(7) . ? C21A C22A 1.525(7) . ? C22A C32A 1.533(9) . ? C22A C23A 1.552(7) . ? C23A C24A 1.524(7) . ? C24A C25A 1.531(7) . ? C24A C33A 1.538(8) . ? C25A C26A 1.527(7) . ? C26A C27A 1.520(7) . ? C26A C34A 1.535(8) . ? C27A C28A 1.492(7) . ? C28A C29A 1.321(7) . ? C35A C36A 1.481(9) . ? 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 C15 N1 C2 128.1(4) . . ? C6 O3 C12 107.5(4) . . ? C29 O5 C12 118.4(4) . . ? C37 O6 C27 114.0(6) . . ? C35 O7 C25 118.8(5) . . ? O1 C1 C9 122.3(4) . . ? O1 C1 C2 118.6(4) . . ? C9 C1 C2 119.1(4) . . ? C3 C2 N1 125.7(4) . . ? C3 C2 C1 120.8(4) . . ? N1 C2 C1 113.4(4) . . ? C2 C3 C4 120.3(4) . . ? O12 C4 C3 118.9(4) . . ? O12 C4 C10 121.1(4) . . ? C3 C4 C10 119.9(4) . . ? C6 C5 C10 119.0(4) . . ? C6 C5 C11 106.2(4) . . ? C10 C5 C11 134.6(4) . . ? C7 C6 O3 120.4(4) . . ? C7 C6 C5 125.6(5) . . ? O3 C6 C5 114.0(4) . . ? C6 C7 C8 114.7(4) . . ? C6 C7 C14 121.5(5) . . ? C8 C7 C14 123.8(5) . . ? O2 C8 C7 116.6(4) . . ? O2 C8 C9 120.7(4) . . ? C7 C8 C9 122.7(4) . . ? C10 C9 C8 119.9(4) . . ? C10 C9 C1 120.2(4) . . ? C8 C9 C1 119.6(4) . . ? C5 C10 C9 118.1(4) . . ? C5 C10 C4 123.9(4) . . ? C9 C10 C4 117.9(4) . . ? O4 C11 C5 132.3(5) . . ? O4 C11 C12 121.6(5) . . ? C5 C11 C12 105.9(4) . . ? O5 C12 O3 109.6(4) . . ? O5 C12 C13 107.0(5) . . ? O3 C12 C13 110.0(5) . . ? O5 C12 C11 114.6(4) . . ? O3 C12 C11 105.6(4) . . ? C13 C12 C11 110.0(5) . . ? O11 C15 N1 121.8(5) . . ? O11 C15 C16 122.1(5) . . ? N1 C15 C16 116.1(5) . . ? C17 C16 C15 121.4(5) . . ? C17 C16 C30 124.1(5) . . ? C15 C16 C30 114.5(5) . . ? C16 C17 C18 128.4(5) . . ? C19 C18 C17 127.6(6) . . ? C18 C19 C20 125.9(6) . . ? C19 C20 C21 111.2(4) . . ? C19 C20 C31 111.4(5) . . ? C21 C20 C31 110.8(5) . . ? O10 C21 C22 110.8(4) . . ? O10 C21 C20 105.2(4) . . ? C22 C21 C20 116.5(4) . . ? C21 C22 C32 112.5(5) . . ? C21 C22 C23 113.7(4) . . ? C32 C22 C23 110.4(5) . . ? O9 C23 C24 111.2(4) . . ? O9 C23 C22 106.9(4) . . ? C24 C23 C22 115.9(4) . . ? C23 C24 C25 110.8(4) . . ? C23 C24 C33 109.7(5) . . ? C25 C24 C33 112.2(5) . . ? O7 C25 C26 105.9(4) . . ? O7 C25 C24 106.7(4) . . ? C26 C25 C24 117.1(4) . . ? C34 C26 C25 111.7(4) . . ? C34 C26 C27 109.3(5) . . ? C25 C26 C27 115.8(5) . . ? O6 C27 C28 111.3(5) . . ? O6 C27 C26 109.9(5) . . ? C28 C27 C26 114.1(5) . . ? C29 C28 C27 121.9(5) . . ? C28 C29 O5 130.8(6) . . ? O8 C35 O7 124.1(6) . . ? O8 C35 C36 125.0(7) . . ? O7 C35 C36 110.9(7) . . ? C15A N1A C2A 126.9(5) . . ? C6A O3A C12A 107.9(3) . . ? C29A O5A C12A 119.8(4) . . ? C37A O6A C27A 119.8(6) . . ? C35A O7A C25A 119.0(4) . . ? O1A C1A C9A 122.4(4) . . ? O1A C1A C2A 118.1(4) . . ? C9A C1A C2A 119.5(4) . . ? C3A C2A N1A 126.2(4) . . ? C3A C2A C1A 120.2(4) . . ? N1A C2A C1A 113.6(4) . . ? C2A C3A C4A 121.5(5) . . ? O12A C4A C3A 120.5(5) . . ? O12A C4A C10A 121.6(4) . . ? C3A C4A C10A 117.9(4) . . ? C10A C5A C6A 118.1(4) . . ? C10A C5A C11A 135.8(4) . . ? C6A C5A C11A 105.9(4) . . ? C7A C6A O3A 120.7(4) . . ? C7A C6A C5A 125.4(4) . . ? O3A C6A C5A 113.9(4) . . ? C6A C7A C8A 115.4(4) . . ? C6A C7A C14A 121.0(4) . . ? C8A C7A C14A 123.5(4) . . ? O2A C8A C7A 117.6(4) . . ? O2A C8A C9A 119.6(4) . . ? C7A C8A C9A 122.8(4) . . ? C10A C9A C8A 119.7(4) . . ? C10A C9A C1A 119.5(4) . . ? C8A C9A C1A 120.6(4) . . ? C5A C10A C9A 118.4(4) . . ? C5A C10A C4A 122.3(4) . . ? C9A C10A C4A 119.3(4) . . ? O4A C11A C5A 132.0(5) . . ? O4A C11A C12A 120.6(4) . . ? C5A C11A C12A 107.3(4) . . ? O5A C12A O3A 109.8(4) . . ? O5A C12A C13A 108.0(4) . . ? O3A C12A C13A 107.3(4) . . ? O5A C12A C11A 115.4(4) . . ? O3A C12A C11A 104.3(4) . . ? C13A C12A C11A 111.7(4) . . ? O11A C15A N1A 122.2(5) . . ? O11A C15A C16A 121.9(5) . . ? N1A C15A C16A 115.9(5) . . ? C17A C16A C30A 124.5(5) . . ? C17A C16A C15A 121.6(5) . . ? C30A C16A C15A 113.7(5) . . ? C16A C17A C18A 128.7(5) . . ? C19A C18A C17A 126.5(6) . . ? C18A C19A C20A 126.2(6) . . ? C19A C20A C31A 110.5(5) . . ? C19A C20A C21A 110.0(4) . . ? C31A C20A C21A 111.5(5) . . ? O10A C21A C22A 111.1(5) . . ? O10A C21A C20A 106.3(4) . . ? C22A C21A C20A 115.2(4) . . ? C21A C22A C32A 111.3(5) . . ? C21A C22A C23A 113.6(4) . . ? C32A C22A C23A 110.0(5) . . ? O9A C23A C24A 111.6(4) . . ? O9A C23A C22A 107.4(4) . . ? C24A C23A C22A 114.8(5) . . ? C23A C24A C25A 111.9(4) . . ? C23A C24A C33A 109.8(5) . . ? C25A C24A C33A 111.5(5) . . ? O7A C25A C26A 107.4(4) . . ? O7A C25A C24A 106.6(4) . . ? C26A C25A C24A 117.4(4) . . ? C27A C26A C25A 115.9(4) . . ? C27A C26A C34A 109.4(5) . . ? C25A C26A C34A 109.7(4) . . ? O6A C27A C28A 105.9(5) . . ? O6A C27A C26A 114.1(4) . . ? C28A C27A C26A 114.0(4) . . ? C29A C28A C27A 120.9(5) . . ? C28A C29A O5A 128.8(5) . . ? O8A C35A O7A 121.6(5) . . ? O8A C35A C36A 128.2(7) . . ? O7A C35A C36A 110.1(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 70.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.354 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.058 #===END data_RSIlowtemp _database_code_depnum_ccdc_archive 'CCDC 681841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H45 N O12' _chemical_formula_weight 695.74 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 0.0091 '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 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 24.618(5) _cell_length_b 14.588(5) _cell_length_c 10.278(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.48(5) _cell_angle_gamma 90.00 _cell_volume 3688(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4 _cell_measurement_theta_max 20 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method '\w/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7198 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.1587 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 70.47 _reflns_number_total 7057 _reflns_number_gt 3504 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0510P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(4) _refine_ls_number_reflns 7057 _refine_ls_number_parameters 925 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.873 _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 N1 N 0.5492(2) 0.7374(5) 0.8562(5) 0.0305(16) Uani 1 1 d . . . H1 H 0.5399 0.7785 0.9110 0.037 Uiso 1 1 calc R . . O1 O 0.6146(2) 0.8669(4) 0.9619(5) 0.0352(14) Uani 1 1 d . . . O2 O 0.7047(2) 0.9543(4) 0.9997(5) 0.0407(15) Uani 1 1 d . . . H2 H 0.6714 0.9555 0.9912 0.061 Uiso 1 1 calc R . . O3 O 0.8562(2) 0.8435(4) 0.7756(5) 0.0354(14) Uani 1 1 d . . . O4 O 0.8007(2) 0.6658(4) 0.5707(5) 0.0410(15) Uani 1 1 d . . . O5 O 0.8984(2) 0.7909(4) 0.5898(5) 0.0398(15) Uani 1 1 d . . . O6 O 0.8267(2) 1.0435(4) 0.3524(5) 0.0416(15) Uani 1 1 d . . . O7 O 0.7266(2) 1.0835(4) 0.4338(5) 0.0337(14) Uani 1 1 d . . . O8 O 0.7604(3) 1.0910(4) 0.6412(5) 0.059(2) Uani 1 1 d . . . O9 O 0.6469(2) 1.0126(4) 0.6611(5) 0.0395(15) Uani 1 1 d . . . H9 H 0.6775 1.0345 0.6695 0.059 Uiso 1 1 calc R . . O10 O 0.5522(2) 0.9366(4) 0.7338(5) 0.0442(16) Uani 1 1 d . . . H10 H 0.5831 0.9557 0.7498 0.066 Uiso 1 1 calc R . . O11 O 0.5205(2) 0.6015(4) 0.7611(5) 0.0373(14) Uani 1 1 d . . . O12 O 0.6870(2) 0.6882(4) 0.5541(5) 0.0404(15) Uani 1 1 d . . . C1 C 0.6349(3) 0.8206(5) 0.8741(7) 0.0274(18) Uani 1 1 d . . . C2 C 0.6011(3) 0.7466(5) 0.8091(7) 0.0263(18) Uani 1 1 d . . . C3 C 0.6202(3) 0.6984(5) 0.7082(7) 0.0293(19) Uani 1 1 d . . . H3 H 0.5989 0.6527 0.6690 0.035 Uiso 1 1 calc R . . C4 C 0.6740(3) 0.7176(5) 0.6607(7) 0.0284(19) Uani 1 1 d . . . C5 C 0.7693(3) 0.7838(6) 0.7229(7) 0.0261(18) Uani 1 1 d . . . C6 C 0.8013(3) 0.8464(5) 0.7958(7) 0.0263(18) Uani 1 1 d . . . C7 C 0.7814(3) 0.9064(6) 0.8885(8) 0.034(2) Uani 1 1 d . . . C8 C 0.7252(4) 0.8990(5) 0.9058(7) 0.033(2) Uani 1 1 d . . . C9 C 0.6900(3) 0.8343(5) 0.8367(7) 0.0231(17) Uani 1 1 d . . . C10 C 0.7127(3) 0.7787(5) 0.7404(6) 0.0230(17) Uani 1 1 d . . . C11 C 0.8074(3) 0.7286(6) 0.6460(8) 0.034(2) Uani 1 1 d . . . C12 C 0.8646(3) 0.7645(6) 0.6904(8) 0.035(2) Uani 1 1 d . . . C13 C 0.8957(4) 0.6901(7) 0.7674(8) 0.048(3) Uani 1 1 d . . . H13A H 0.9304 0.7138 0.7981 0.071 Uiso 1 1 calc R . . H13B H 0.9012 0.6382 0.7121 0.071 Uiso 1 1 calc R . . H13C H 0.8752 0.6717 0.8403 0.071 Uiso 1 1 calc R . . C14 C 0.8179(4) 0.9748(7) 0.9605(9) 0.057(3) Uani 1 1 d . . . H14A H 0.8146 1.0335 0.9189 0.086 Uiso 1 1 calc R . . H14B H 0.8550 0.9544 0.9593 0.086 Uiso 1 1 calc R . . H14C H 0.8074 0.9797 1.0491 0.086 Uiso 1 1 calc R . . C15 C 0.5105(3) 0.6711(6) 0.8268(7) 0.032(2) Uani 1 1 d . . . C16 C 0.4564(3) 0.6847(6) 0.8850(8) 0.037(2) Uani 1 1 d . . . C17 C 0.4256(4) 0.7593(6) 0.8515(8) 0.041(2) Uani 1 1 d . . . H17 H 0.3924 0.7630 0.8910 0.049 Uiso 1 1 calc R . . C18 C 0.4371(3) 0.8354(7) 0.7615(8) 0.046(2) Uani 1 1 d . . . H18 H 0.4234 0.8930 0.7811 0.055 Uiso 1 1 calc R . . C19 C 0.4661(3) 0.8279(6) 0.6532(8) 0.038(2) Uani 1 1 d . . . H19 H 0.4775 0.7700 0.6280 0.046 Uiso 1 1 calc R . . C20 C 0.4807(3) 0.9099(6) 0.5710(8) 0.034(2) Uani 1 1 d . . . H20 H 0.4593 0.9628 0.5977 0.041 Uiso 1 1 calc R . . C21 C 0.5420(4) 0.9324(6) 0.5951(8) 0.038(2) Uani 1 1 d . . . H21 H 0.5632 0.8815 0.5613 0.046 Uiso 1 1 calc R . . C22 C 0.5616(3) 1.0246(5) 0.5288(8) 0.036(2) Uani 1 1 d . . . H22 H 0.5481 1.0237 0.4377 0.043 Uiso 1 1 calc R . . C23 C 0.6242(3) 1.0319(6) 0.5291(7) 0.0294(19) Uani 1 1 d . . . H23 H 0.6331 1.0957 0.5088 0.035 Uiso 1 1 calc R . . C24 C 0.6525(3) 0.9705(6) 0.4295(7) 0.036(2) Uani 1 1 d . . . H24 H 0.6440 0.9064 0.4486 0.044 Uiso 1 1 calc R . . C25 C 0.7150(3) 0.9830(5) 0.4435(7) 0.0253(18) Uani 1 1 d . . . H25 H 0.7278 0.9612 0.5297 0.030 Uiso 1 1 calc R . . C26 C 0.7497(3) 0.9376(6) 0.3388(8) 0.031(2) Uani 1 1 d . . . H26 H 0.7404 0.9686 0.2562 0.038 Uiso 1 1 calc R . . C27 C 0.8111(3) 0.9469(6) 0.3621(8) 0.034(2) Uani 1 1 d . . . H27 H 0.8278 0.9153 0.2897 0.041 Uiso 1 1 calc R . . C28 C 0.8343(3) 0.9027(6) 0.4858(7) 0.038(2) Uani 1 1 d . . . H28 H 0.8195 0.9185 0.5644 0.046 Uiso 1 1 calc R . . C29 C 0.8750(4) 0.8422(6) 0.4874(8) 0.040(2) Uani 1 1 d . . . H29 H 0.8902 0.8327 0.4072 0.048 Uiso 1 1 calc R . . C30 C 0.4390(3) 0.6099(6) 0.9746(8) 0.042(2) Uani 1 1 d . . . H30A H 0.4429 0.5516 0.9329 0.063 Uiso 1 1 calc R . . H30B H 0.4017 0.6190 0.9949 0.063 Uiso 1 1 calc R . . H30C H 0.4614 0.6114 1.0535 0.063 Uiso 1 1 calc R . . C31 C 0.4671(4) 0.8904(7) 0.4259(8) 0.049(3) Uani 1 1 d . . . H31A H 0.4303 0.8689 0.4153 0.074 Uiso 1 1 calc R . . H31B H 0.4914 0.8444 0.3954 0.074 Uiso 1 1 calc R . . H31C H 0.4712 0.9456 0.3765 0.074 Uiso 1 1 calc R . . C32 C 0.5372(3) 1.1097(6) 0.5939(8) 0.041(2) Uani 1 1 d . . . H32A H 0.4984 1.1100 0.5784 0.061 Uiso 1 1 calc R . . H32B H 0.5524 1.1643 0.5578 0.061 Uiso 1 1 calc R . . H32C H 0.5456 1.1079 0.6860 0.061 Uiso 1 1 calc R . . C33 C 0.6293(4) 0.9929(6) 0.2938(8) 0.045(2) Uani 1 1 d . . . H33A H 0.6546 0.9744 0.2304 0.067 Uiso 1 1 calc R . . H33B H 0.6230 1.0577 0.2868 0.067 Uiso 1 1 calc R . . H33C H 0.5956 0.9608 0.2785 0.067 Uiso 1 1 calc R . . C34 C 0.7343(3) 0.8334(6) 0.3191(8) 0.042(2) Uani 1 1 d . . . H34A H 0.7429 0.8003 0.3980 0.063 Uiso 1 1 calc R . . H34B H 0.7544 0.8083 0.2496 0.063 Uiso 1 1 calc R . . H34C H 0.6960 0.8283 0.2978 0.063 Uiso 1 1 calc R . . C35 C 0.7532(3) 1.1256(6) 0.5351(8) 0.037(2) Uani 1 1 d . . . C36 C 0.7710(4) 1.2222(6) 0.4993(8) 0.042(2) Uani 1 1 d . . . H36A H 0.7729 1.2597 0.5760 0.063 Uiso 1 1 calc R . . H36B H 0.7452 1.2479 0.4368 0.063 Uiso 1 1 calc R . . H36C H 0.8061 1.2197 0.4625 0.063 Uiso 1 1 calc R . . C37 C 0.8828(4) 1.0537(7) 0.3261(9) 0.052(3) Uani 1 1 d . . . H37A H 0.8917 1.1177 0.3225 0.078 Uiso 1 1 calc R . . H37B H 0.8898 1.0256 0.2440 0.078 Uiso 1 1 calc R . . H37C H 0.9047 1.0248 0.3939 0.078 Uiso 1 1 calc R . . N1A N 0.9505(3) 0.6522(5) 0.3571(6) 0.0322(17) Uani 1 1 d . . . H1A H 0.9625 0.6132 0.4143 0.039 Uiso 1 1 calc R . . O1A O 0.8900(2) 0.5258(4) 0.4709(5) 0.0354(14) Uani 1 1 d . . . O2A O 0.7987(2) 0.4475(4) 0.5219(5) 0.0361(14) Uani 1 1 d . . . H2A H 0.8312 0.4599 0.5279 0.054 Uiso 1 1 calc R . . O3A O 0.6401(2) 0.5388(3) 0.2703(5) 0.0292(13) Uani 1 1 d . . . O4A O 0.6894(2) 0.6982(4) 0.0410(5) 0.0391(15) Uani 1 1 d . . . O5A O 0.5934(2) 0.5745(4) 0.0710(5) 0.0336(14) Uani 1 1 d . . . O6A O 0.6568(2) 0.3087(4) -0.1056(5) 0.0417(15) Uani 1 1 d . . . O7A O 0.7620(2) 0.2871(4) -0.0075(5) 0.0319(13) Uani 1 1 d . . . O8A O 0.7453(3) 0.3216(4) 0.2006(5) 0.0515(18) Uani 1 1 d . . . O9A O 0.8551(2) 0.3926(5) 0.1758(5) 0.054(2) Uani 1 1 d . . . H9A H 0.8219 0.3912 0.1790 0.081 Uiso 1 1 calc R . . O10A O 0.9560(2) 0.4391(5) 0.2567(5) 0.0454(16) Uani 1 1 d . . . H10A H 0.9278 0.4137 0.2759 0.068 Uiso 1 1 calc R . . O11A O 0.9708(2) 0.7879(4) 0.2533(5) 0.0406(15) Uani 1 1 d . . . O12A O 0.8028(2) 0.6758(4) 0.0368(5) 0.0418(16) Uani 1 1 d . . . C1A C 0.8654(3) 0.5675(6) 0.3791(7) 0.0283(19) Uani 1 1 d . . . C2A C 0.8973(3) 0.6384(5) 0.3072(7) 0.0295(19) Uani 1 1 d . . . C3A C 0.8739(3) 0.6800(6) 0.1979(7) 0.035(2) Uani 1 1 d . . . H3A H 0.8932 0.7242 0.1540 0.041 Uiso 1 1 calc R . . C4A C 0.8185(3) 0.6551(6) 0.1500(8) 0.032(2) Uani 1 1 d . . . C5A C 0.7267(3) 0.5961(5) 0.2148(7) 0.0254(18) Uani 1 1 d . . . C6A C 0.6954(3) 0.5402(5) 0.2974(7) 0.0273(18) Uani 1 1 d . . . C7A C 0.7184(3) 0.4890(5) 0.4003(7) 0.0266(18) Uani 1 1 d . . . C8A C 0.7746(3) 0.4966(5) 0.4231(7) 0.0254(18) Uani 1 1 d . . . C9A C 0.8077(3) 0.5534(5) 0.3416(7) 0.0277(19) Uani 1 1 d . . . C10A C 0.7830(3) 0.6012(5) 0.2364(6) 0.0220(17) Uani 1 1 d . . . C11A C 0.6856(3) 0.6433(6) 0.1267(7) 0.0301(19) Uani 1 1 d . . . C12A C 0.6281(3) 0.6115(6) 0.1710(7) 0.034(2) Uani 1 1 d . . . C13A C 0.5977(3) 0.6895(6) 0.2324(8) 0.036(2) Uani 1 1 d . . . H13D H 0.6174 0.7096 0.3099 0.055 Uiso 1 1 calc R . . H13E H 0.5622 0.6689 0.2543 0.055 Uiso 1 1 calc R . . H13F H 0.5942 0.7395 0.1719 0.055 Uiso 1 1 calc R . . C14A C 0.6825(3) 0.4342(6) 0.4854(8) 0.041(2) Uani 1 1 d . . . H14D H 0.6622 0.3906 0.4331 0.061 Uiso 1 1 calc R . . H14E H 0.6579 0.4746 0.5272 0.061 Uiso 1 1 calc R . . H14F H 0.7045 0.4025 0.5502 0.061 Uiso 1 1 calc R . . C15A C 0.9865(3) 0.7225(6) 0.3245(7) 0.031(2) Uani 1 1 d . . . C16A C 1.0429(3) 0.7158(6) 0.3813(8) 0.034(2) Uani 1 1 d . . . C17A C 1.0760(4) 0.6447(6) 0.3560(8) 0.041(2) Uani 1 1 d . . . H17A H 1.1106 0.6466 0.3959 0.049 Uiso 1 1 calc R . . C18A C 1.0636(3) 0.5640(6) 0.2721(8) 0.035(2) Uani 1 1 d . . . H18A H 1.0798 0.5087 0.2964 0.043 Uiso 1 1 calc R . . C19A C 1.0316(4) 0.5643(6) 0.1657(8) 0.037(2) Uani 1 1 d . . . H19A H 1.0181 0.6204 0.1358 0.044 Uiso 1 1 calc R . . C20A C 1.0150(3) 0.4781(6) 0.0883(7) 0.033(2) Uani 1 1 d . . . H20A H 1.0394 0.4275 0.1136 0.039 Uiso 1 1 calc R . . C21A C 0.9561(3) 0.4516(5) 0.1171(7) 0.032(2) Uani 1 1 d . . . H21A H 0.9324 0.5035 0.0937 0.039 Uiso 1 1 calc R . . C22A C 0.9331(3) 0.3642(6) 0.0462(8) 0.037(2) Uani 1 1 d . . . H22A H 0.9397 0.3719 -0.0465 0.044 Uiso 1 1 calc R . . C23A C 0.8711(4) 0.3506(6) 0.0564(7) 0.040(2) Uani 1 1 d . . . H23A H 0.8639 0.2847 0.0619 0.048 Uiso 1 1 calc R . . C24A C 0.8364(3) 0.3896(6) -0.0597(7) 0.034(2) Uani 1 1 d . . . H24A H 0.8467 0.4538 -0.0723 0.041 Uiso 1 1 calc R . . C25A C 0.7744(3) 0.3854(6) -0.0376(8) 0.034(2) Uani 1 1 d . . . H25A H 0.7668 0.4226 0.0389 0.041 Uiso 1 1 calc R . . C26A C 0.7357(3) 0.4147(5) -0.1493(7) 0.033(2) Uani 1 1 d . . . H26A H 0.7436 0.3769 -0.2251 0.039 Uiso 1 1 calc R . . C27A C 0.6740(4) 0.4045(6) -0.1250(8) 0.037(2) Uani 1 1 d . . . H27A H 0.6538 0.4281 -0.2020 0.044 Uiso 1 1 calc R . . C28A C 0.6564(3) 0.4585(6) -0.0082(7) 0.034(2) Uani 1 1 d . . . H28A H 0.6743 0.4511 0.0727 0.040 Uiso 1 1 calc R . . C29A C 0.6145(4) 0.5175(6) -0.0232(8) 0.040(2) Uani 1 1 d . . . H29A H 0.5977 0.5205 -0.1059 0.048 Uiso 1 1 calc R . . C30A C 1.0594(4) 0.7996(7) 0.4651(8) 0.050(3) Uani 1 1 d . . . H30D H 1.0967 0.7938 0.4947 0.075 Uiso 1 1 calc R . . H30E H 1.0368 0.8029 0.5389 0.075 Uiso 1 1 calc R . . H30F H 1.0549 0.8544 0.4141 0.075 Uiso 1 1 calc R . . C31A C 1.0194(4) 0.4982(6) -0.0606(8) 0.047(3) Uani 1 1 d . . . H31D H 1.0151 0.4421 -0.1088 0.070 Uiso 1 1 calc R . . H31E H 1.0544 0.5243 -0.0757 0.070 Uiso 1 1 calc R . . H31F H 0.9914 0.5406 -0.0885 0.070 Uiso 1 1 calc R . . C32A C 0.9644(4) 0.2767(7) 0.0922(12) 0.076(4) Uani 1 1 d . . . H32D H 0.9496 0.2243 0.0467 0.114 Uiso 1 1 calc R . . H32E H 0.9608 0.2687 0.1841 0.114 Uiso 1 1 calc R . . H32F H 1.0022 0.2831 0.0742 0.114 Uiso 1 1 calc R . . C33A C 0.8495(4) 0.3351(7) -0.1843(7) 0.049(3) Uani 1 1 d . . . H33D H 0.8336 0.3657 -0.2594 0.074 Uiso 1 1 calc R . . H33E H 0.8348 0.2744 -0.1790 0.074 Uiso 1 1 calc R . . H33F H 0.8882 0.3316 -0.1916 0.074 Uiso 1 1 calc R . . C34A C 0.7470(4) 0.5167(6) -0.1856(8) 0.041(2) Uani 1 1 d . . . H34D H 0.7830 0.5220 -0.2172 0.061 Uiso 1 1 calc R . . H34E H 0.7440 0.5546 -0.1098 0.061 Uiso 1 1 calc R . . H34F H 0.7210 0.5363 -0.2521 0.061 Uiso 1 1 calc R . . C35A C 0.7454(3) 0.2665(6) 0.1114(8) 0.037(2) Uani 1 1 d . . . C36A C 0.7287(4) 0.1668(6) 0.1206(9) 0.048(3) Uani 1 1 d . . . H36D H 0.7229 0.1420 0.0346 0.072 Uiso 1 1 calc R . . H36E H 0.6958 0.1623 0.1668 0.072 Uiso 1 1 calc R . . H36F H 0.7570 0.1329 0.1663 0.072 Uiso 1 1 calc R . . C37A C 0.6650(5) 0.2469(7) -0.2109(9) 0.068(3) Uani 1 1 d . . . H37D H 0.6570 0.2776 -0.2921 0.102 Uiso 1 1 calc R . . H37E H 0.6415 0.1949 -0.2036 0.102 Uiso 1 1 calc R . . H37F H 0.7022 0.2268 -0.2077 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.028(4) 0.042(4) 0.022(3) -0.002(3) 0.004(3) -0.008(3) O1 0.046(4) 0.032(3) 0.029(3) -0.006(3) 0.006(3) 0.005(3) O2 0.048(4) 0.041(4) 0.034(3) -0.015(3) 0.014(3) -0.005(3) O3 0.031(3) 0.040(4) 0.036(3) -0.008(3) 0.008(3) -0.005(3) O4 0.048(4) 0.039(4) 0.036(3) -0.015(3) 0.009(3) 0.003(3) O5 0.035(3) 0.052(4) 0.033(3) -0.002(3) 0.007(3) 0.002(3) O6 0.047(4) 0.040(4) 0.039(3) 0.005(3) 0.015(3) -0.012(3) O7 0.050(4) 0.027(3) 0.025(3) -0.002(2) 0.001(3) 0.003(3) O8 0.105(6) 0.040(4) 0.030(3) 0.001(3) -0.012(4) -0.009(4) O9 0.045(4) 0.043(4) 0.031(3) 0.000(3) 0.005(3) 0.001(3) O10 0.063(4) 0.040(4) 0.030(3) 0.006(3) 0.006(3) -0.009(4) O11 0.045(4) 0.033(3) 0.035(3) -0.005(3) 0.009(3) 0.002(3) O12 0.056(4) 0.038(4) 0.028(3) -0.013(3) 0.014(3) -0.006(3) C1 0.037(5) 0.016(4) 0.029(4) 0.004(3) 0.003(4) 0.006(4) C2 0.020(4) 0.027(4) 0.032(4) 0.005(4) -0.002(3) -0.001(4) C3 0.036(5) 0.021(5) 0.031(4) 0.001(4) -0.001(4) -0.001(4) C4 0.046(5) 0.023(4) 0.017(4) -0.001(3) 0.005(4) -0.001(4) C5 0.024(4) 0.034(5) 0.021(4) 0.002(4) 0.000(3) 0.000(4) C6 0.021(4) 0.029(5) 0.029(4) 0.003(4) 0.002(3) -0.005(4) C7 0.041(5) 0.031(5) 0.032(5) -0.008(4) 0.016(4) -0.008(4) C8 0.055(6) 0.022(4) 0.023(4) -0.002(4) 0.002(4) 0.006(4) C9 0.028(4) 0.018(4) 0.024(4) 0.001(3) 0.004(3) 0.003(3) C10 0.036(5) 0.020(4) 0.012(4) 0.001(3) -0.008(3) 0.004(4) C11 0.034(5) 0.036(5) 0.032(5) 0.009(4) 0.008(4) 0.008(4) C12 0.026(5) 0.045(6) 0.035(5) -0.004(4) 0.011(4) 0.009(4) C13 0.049(6) 0.062(7) 0.033(5) 0.009(5) 0.004(4) 0.007(5) C14 0.052(6) 0.069(8) 0.051(6) -0.028(6) 0.009(5) -0.006(6) C15 0.045(5) 0.026(5) 0.026(4) 0.008(4) -0.002(4) 0.004(4) C16 0.044(5) 0.035(5) 0.032(5) -0.003(4) 0.008(4) 0.000(5) C17 0.039(5) 0.044(6) 0.041(5) -0.004(4) 0.014(4) 0.000(5) C18 0.050(6) 0.039(6) 0.049(6) 0.008(5) 0.009(5) 0.015(5) C19 0.038(5) 0.034(5) 0.043(5) 0.005(4) 0.004(4) 0.004(4) C20 0.035(5) 0.030(5) 0.038(5) 0.003(4) 0.007(4) 0.013(4) C21 0.047(6) 0.023(5) 0.044(5) 0.005(4) 0.013(4) 0.007(4) C22 0.052(6) 0.019(4) 0.039(5) 0.007(4) 0.016(4) 0.009(4) C23 0.043(5) 0.023(4) 0.023(4) 0.003(4) 0.007(4) -0.003(4) C24 0.056(6) 0.025(5) 0.029(5) 0.002(4) 0.012(4) 0.000(4) C25 0.027(4) 0.032(5) 0.017(4) 0.000(3) 0.003(3) 0.005(4) C26 0.040(5) 0.025(5) 0.030(4) -0.001(4) 0.016(4) 0.009(4) C27 0.036(5) 0.038(5) 0.029(4) 0.000(4) 0.015(4) 0.001(4) C28 0.047(5) 0.045(6) 0.025(4) -0.006(4) 0.018(4) -0.002(5) C29 0.050(6) 0.035(5) 0.036(5) -0.014(4) 0.018(4) -0.002(5) C30 0.042(5) 0.047(6) 0.038(5) 0.004(5) 0.010(4) 0.005(5) C31 0.048(6) 0.052(6) 0.047(6) 0.007(5) -0.009(5) -0.008(5) C32 0.040(5) 0.041(6) 0.043(5) 0.007(4) 0.016(4) 0.008(4) C33 0.054(6) 0.041(6) 0.039(5) -0.003(4) 0.013(4) -0.004(5) C34 0.048(6) 0.034(5) 0.046(5) -0.010(4) 0.018(4) -0.001(5) C35 0.042(6) 0.038(5) 0.032(5) -0.004(4) 0.006(4) 0.003(4) C36 0.050(6) 0.036(5) 0.039(5) -0.004(4) 0.003(4) -0.006(5) C37 0.046(6) 0.043(6) 0.069(7) -0.013(5) 0.025(5) -0.008(5) N1A 0.030(4) 0.037(4) 0.030(4) 0.009(3) 0.005(3) -0.004(3) O1A 0.038(3) 0.042(4) 0.027(3) 0.009(3) 0.007(3) 0.002(3) O2A 0.048(4) 0.034(3) 0.026(3) 0.011(3) 0.002(3) -0.004(3) O3A 0.036(3) 0.027(3) 0.024(3) 0.004(2) -0.003(2) -0.001(3) O4A 0.046(4) 0.041(4) 0.031(3) 0.009(3) 0.004(3) -0.004(3) O5A 0.040(3) 0.031(3) 0.031(3) -0.001(3) 0.004(3) 0.005(3) O6A 0.061(4) 0.031(3) 0.034(3) -0.003(3) 0.016(3) -0.002(3) O7A 0.048(4) 0.021(3) 0.028(3) -0.001(2) 0.012(3) -0.005(3) O8A 0.088(5) 0.042(4) 0.026(3) 0.000(3) 0.020(3) 0.000(4) O9A 0.033(3) 0.101(6) 0.029(3) -0.022(4) 0.008(3) 0.004(4) O10A 0.057(4) 0.057(4) 0.022(3) 0.003(3) 0.005(3) -0.020(4) O11A 0.049(4) 0.040(4) 0.034(3) 0.004(3) 0.011(3) 0.000(3) O12A 0.054(4) 0.045(4) 0.026(3) 0.008(3) -0.002(3) -0.005(3) C1A 0.033(5) 0.032(5) 0.021(4) -0.002(4) 0.006(3) 0.005(4) C2A 0.029(5) 0.030(5) 0.030(4) -0.004(4) 0.008(4) 0.000(4) C3A 0.051(6) 0.028(5) 0.026(4) 0.004(4) 0.018(4) 0.001(4) C4A 0.032(5) 0.027(5) 0.037(5) 0.005(4) 0.000(4) 0.000(4) C5A 0.033(5) 0.028(4) 0.017(4) -0.001(3) 0.011(3) -0.004(4) C6A 0.032(5) 0.018(4) 0.032(4) -0.009(4) 0.004(4) 0.010(4) C7A 0.041(5) 0.021(4) 0.018(4) 0.000(3) 0.004(3) 0.005(4) C8A 0.029(4) 0.026(4) 0.021(4) -0.001(3) -0.001(3) 0.002(4) C9A 0.027(4) 0.026(4) 0.031(4) 0.006(4) 0.019(4) 0.006(4) C10A 0.032(5) 0.016(4) 0.018(4) -0.001(3) 0.002(3) 0.005(4) C11A 0.037(5) 0.027(5) 0.027(4) -0.004(4) 0.013(4) 0.005(4) C12A 0.045(5) 0.037(5) 0.021(4) 0.002(4) 0.006(4) 0.002(4) C13A 0.046(5) 0.028(5) 0.036(5) 0.004(4) 0.009(4) 0.003(4) C14A 0.055(6) 0.036(5) 0.032(5) 0.000(4) 0.003(4) -0.001(5) C15A 0.044(5) 0.023(4) 0.028(4) -0.010(4) 0.016(4) -0.005(4) C16A 0.036(5) 0.028(5) 0.038(5) 0.002(4) 0.011(4) -0.001(4) C17A 0.036(5) 0.044(6) 0.043(5) 0.002(4) 0.009(4) -0.006(5) C18A 0.036(5) 0.026(5) 0.044(5) -0.005(4) 0.010(4) 0.005(4) C19A 0.049(6) 0.032(5) 0.031(5) 0.002(4) 0.017(4) 0.005(4) C20A 0.041(5) 0.033(5) 0.024(4) 0.002(4) 0.008(4) 0.008(4) C21A 0.043(5) 0.022(4) 0.034(4) 0.001(4) 0.012(4) 0.008(4) C22A 0.043(5) 0.040(5) 0.027(4) -0.013(4) 0.002(4) -0.001(4) C23A 0.062(6) 0.030(5) 0.028(5) -0.001(4) 0.007(4) 0.012(5) C24A 0.045(5) 0.030(5) 0.027(4) -0.003(4) 0.004(4) -0.003(4) C25A 0.040(5) 0.032(5) 0.032(5) -0.007(4) 0.013(4) 0.002(4) C26A 0.045(5) 0.028(5) 0.026(4) -0.002(4) 0.013(4) 0.001(4) C27A 0.051(6) 0.032(5) 0.028(5) -0.002(4) 0.003(4) 0.010(4) C28A 0.045(5) 0.038(5) 0.017(4) -0.002(4) -0.001(4) -0.005(5) C29A 0.058(6) 0.028(5) 0.035(5) 0.003(4) 0.012(4) -0.002(5) C30A 0.053(6) 0.052(6) 0.045(5) -0.017(5) 0.011(5) -0.006(5) C31A 0.059(6) 0.045(6) 0.039(5) -0.009(5) 0.018(5) -0.004(5) C32A 0.043(6) 0.047(7) 0.139(11) -0.021(7) 0.011(7) 0.006(6) C33A 0.067(7) 0.056(6) 0.025(5) -0.008(5) 0.008(4) 0.021(6) C34A 0.053(6) 0.041(6) 0.028(4) 0.003(4) 0.015(4) 0.001(5) C35A 0.030(5) 0.041(6) 0.039(5) 0.005(5) 0.002(4) 0.005(4) C36A 0.053(6) 0.040(6) 0.053(6) 0.012(5) 0.015(5) -0.002(5) C37A 0.091(9) 0.069(8) 0.046(6) -0.017(6) 0.007(6) -0.014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C15 1.380(10) . ? N1 C2 1.394(9) . ? O1 C1 1.249(8) . ? O2 C8 1.371(9) . ? O3 C6 1.376(8) . ? O3 C12 1.468(9) . ? O4 C11 1.206(10) . ? O5 C29 1.396(10) . ? O5 C12 1.409(9) . ? O6 C37 1.427(9) . ? O6 C27 1.464(10) . ? O7 C35 1.352(10) . ? O7 C25 1.498(9) . ? O8 C35 1.207(9) . ? O9 C23 1.473(8) . ? O10 C21 1.438(9) . ? O11 C15 1.249(9) . ? O12 C4 1.231(8) . ? C1 C9 1.441(10) . ? C1 C2 1.501(10) . ? C2 C3 1.353(10) . ? C3 C4 1.459(10) . ? C4 C10 1.519(10) . ? C5 C6 1.401(10) . ? C5 C10 1.414(10) . ? C5 C11 1.489(10) . ? C6 C7 1.397(10) . ? C7 C8 1.408(11) . ? C7 C14 1.514(11) . ? C8 C9 1.446(11) . ? C9 C10 1.414(9) . ? C11 C12 1.553(12) . ? C12 C13 1.529(11) . ? C15 C16 1.499(11) . ? C16 C17 1.361(11) . ? C16 C30 1.503(11) . ? C17 C18 1.480(11) . ? C18 C19 1.352(10) . ? C19 C20 1.518(11) . ? C20 C31 1.541(11) . ? C20 C21 1.555(11) . ? C21 C22 1.592(11) . ? C22 C23 1.543(11) . ? C22 C32 1.545(10) . ? C23 C24 1.548(10) . ? C24 C33 1.519(11) . ? C24 C25 1.551(11) . ? C25 C26 1.552(9) . ? C26 C27 1.526(11) . ? C26 C34 1.577(11) . ? C27 C28 1.515(11) . ? C28 C29 1.333(11) . ? C35 C36 1.525(11) . ? N1A C2A 1.400(10) . ? N1A C15A 1.406(9) . ? O1A C1A 1.257(8) . ? O2A C8A 1.357(8) . ? O3A C6A 1.378(8) . ? O3A C12A 1.492(9) . ? O4A C11A 1.198(9) . ? O5A C29A 1.394(9) . ? O5A C12A 1.415(9) . ? O6A C37A 1.430(10) . ? O6A C27A 1.476(10) . ? O7A C35A 1.339(9) . ? O7A C25A 1.501(9) . ? O8A C35A 1.219(10) . ? O9A C23A 1.442(9) . ? O10A C21A 1.446(9) . ? O11A C15A 1.252(9) . ? O12A C4A 1.246(9) . ? C1A C9A 1.469(10) . ? C1A C2A 1.511(10) . ? C2A C3A 1.382(11) . ? C3A C4A 1.475(11) . ? C4A C10A 1.495(10) . ? C5A C10A 1.398(10) . ? C5A C6A 1.427(10) . ? C5A C11A 1.494(11) . ? C6A C7A 1.394(10) . ? C7A C8A 1.398(11) . ? C7A C14A 1.500(10) . ? C8A C9A 1.453(10) . ? C9A C10A 1.403(10) . ? C11A C12A 1.576(11) . ? C12A C13A 1.515(11) . ? C15A C16A 1.486(11) . ? C16A C17A 1.352(11) . ? C16A C30A 1.540(11) . ? C17A C18A 1.482(11) . ? C18A C19A 1.320(11) . ? C19A C20A 1.535(11) . ? C20A C21A 1.541(10) . ? C20A C31A 1.566(10) . ? C21A C22A 1.563(11) . ? C22A C23A 1.547(11) . ? C22A C32A 1.555(12) . ? C23A C24A 1.545(11) . ? C24A C33A 1.552(10) . ? C24A C25A 1.555(11) . ? C25A C26A 1.520(11) . ? C26A C27A 1.556(11) . ? C26A C34A 1.563(11) . ? C27A C28A 1.515(10) . ? C28A C29A 1.347(11) . ? C35A C36A 1.516(12) . ? 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 C15 N1 C2 128.7(7) . . ? C6 O3 C12 106.2(6) . . ? C29 O5 C12 117.5(6) . . ? C37 O6 C27 111.9(7) . . ? C35 O7 C25 118.7(6) . . ? O1 C1 C9 121.9(7) . . ? O1 C1 C2 118.7(7) . . ? C9 C1 C2 119.4(7) . . ? C3 C2 N1 124.8(7) . . ? C3 C2 C1 120.7(7) . . ? N1 C2 C1 114.4(7) . . ? C2 C3 C4 120.5(7) . . ? O12 C4 C3 120.3(7) . . ? O12 C4 C10 120.3(7) . . ? C3 C4 C10 119.3(6) . . ? C6 C5 C10 120.0(7) . . ? C6 C5 C11 106.6(7) . . ? C10 C5 C11 133.2(7) . . ? O3 C6 C7 119.8(7) . . ? O3 C6 C5 115.6(7) . . ? C7 C6 C5 124.6(7) . . ? C6 C7 C8 114.4(7) . . ? C6 C7 C14 121.9(8) . . ? C8 C7 C14 123.7(7) . . ? O2 C8 C7 116.0(7) . . ? O2 C8 C9 120.0(7) . . ? C7 C8 C9 124.0(7) . . ? C10 C9 C1 120.8(7) . . ? C10 C9 C8 118.2(7) . . ? C1 C9 C8 120.7(7) . . ? C9 C10 C5 118.7(7) . . ? C9 C10 C4 117.2(7) . . ? C5 C10 C4 124.1(7) . . ? O4 C11 C5 132.9(8) . . ? O4 C11 C12 122.8(7) . . ? C5 C11 C12 104.2(7) . . ? O5 C12 O3 109.0(7) . . ? O5 C12 C13 105.9(6) . . ? O3 C12 C13 109.2(7) . . ? O5 C12 C11 115.7(7) . . ? O3 C12 C11 106.9(6) . . ? C13 C12 C11 109.9(7) . . ? O11 C15 N1 122.5(8) . . ? O11 C15 C16 121.5(8) . . ? N1 C15 C16 115.9(7) . . ? C17 C16 C15 120.0(8) . . ? C17 C16 C30 124.5(8) . . ? C15 C16 C30 115.5(7) . . ? C16 C17 C18 129.6(8) . . ? C19 C18 C17 125.1(8) . . ? C18 C19 C20 122.7(8) . . ? C19 C20 C31 110.3(7) . . ? C19 C20 C21 109.3(7) . . ? C31 C20 C21 111.2(7) . . ? O10 C21 C20 107.1(6) . . ? O10 C21 C22 110.2(7) . . ? C20 C21 C22 114.8(7) . . ? C23 C22 C32 110.5(7) . . ? C23 C22 C21 112.2(7) . . ? C32 C22 C21 111.3(6) . . ? O9 C23 C22 109.1(6) . . ? O9 C23 C24 109.5(6) . . ? C22 C23 C24 115.9(7) . . ? C33 C24 C23 108.7(7) . . ? C33 C24 C25 113.1(6) . . ? C23 C24 C25 110.1(7) . . ? O7 C25 C24 107.5(6) . . ? O7 C25 C26 105.0(6) . . ? C24 C25 C26 117.4(6) . . ? C27 C26 C25 115.1(7) . . ? C27 C26 C34 109.8(7) . . ? C25 C26 C34 111.3(6) . . ? O6 C27 C28 112.1(7) . . ? O6 C27 C26 109.6(7) . . ? C28 C27 C26 115.3(7) . . ? C29 C28 C27 123.2(7) . . ? C28 C29 O5 130.5(8) . . ? O8 C35 O7 123.6(8) . . ? O8 C35 C36 124.8(8) . . ? O7 C35 C36 111.6(7) . . ? C2A N1A C15A 127.3(7) . . ? C6A O3A C12A 107.0(6) . . ? C29A O5A C12A 120.0(7) . . ? C37A O6A C27A 116.3(6) . . ? C35A O7A C25A 118.4(6) . . ? O1A C1A C9A 123.9(7) . . ? O1A C1A C2A 117.0(7) . . ? C9A C1A C2A 119.0(7) . . ? C3A C2A N1A 125.9(7) . . ? C3A C2A C1A 119.4(7) . . ? N1A C2A C1A 114.7(7) . . ? C2A C3A C4A 120.7(7) . . ? O12A C4A C3A 119.7(7) . . ? O12A C4A C10A 121.1(7) . . ? C3A C4A C10A 119.1(7) . . ? C10A C5A C6A 119.5(7) . . ? C10A C5A C11A 135.4(7) . . ? C6A C5A C11A 104.8(7) . . ? O3A C6A C7A 120.7(7) . . ? O3A C6A C5A 116.2(7) . . ? C7A C6A C5A 123.1(7) . . ? C6A C7A C8A 116.8(7) . . ? C6A C7A C14A 119.9(7) . . ? C8A C7A C14A 123.2(7) . . ? O2A C8A C7A 118.7(7) . . ? O2A C8A C9A 119.6(7) . . ? C7A C8A C9A 121.6(7) . . ? C10A C9A C8A 119.5(7) . . ? C10A C9A C1A 120.9(7) . . ? C8A C9A C1A 119.2(7) . . ? C5A C10A C9A 119.3(7) . . ? C5A C10A C4A 122.3(7) . . ? C9A C10A C4A 118.4(7) . . ? O4A C11A C5A 132.9(8) . . ? O4A C11A C12A 120.6(7) . . ? C5A C11A C12A 106.4(6) . . ? O5A C12A O3A 108.8(6) . . ? O5A C12A C13A 107.2(7) . . ? O3A C12A C13A 109.6(6) . . ? O5A C12A C11A 115.1(6) . . ? O3A C12A C11A 104.6(6) . . ? C13A C12A C11A 111.4(7) . . ? O11A C15A N1A 120.9(8) . . ? O11A C15A C16A 122.6(8) . . ? N1A C15A C16A 116.5(7) . . ? C17A C16A C15A 122.4(8) . . ? C17A C16A C30A 124.7(8) . . ? C15A C16A C30A 112.8(7) . . ? C16A C17A C18A 127.6(8) . . ? C19A C18A C17A 125.4(8) . . ? C18A C19A C20A 124.3(8) . . ? C19A C20A C21A 109.7(6) . . ? C19A C20A C31A 108.9(7) . . ? C21A C20A C31A 109.9(7) . . ? O10A C21A C20A 105.3(6) . . ? O10A C21A C22A 110.1(7) . . ? C20A C21A C22A 116.1(6) . . ? C23A C22A C32A 110.6(7) . . ? C23A C22A C21A 114.3(7) . . ? C32A C22A C21A 111.3(7) . . ? O9A C23A C24A 109.9(7) . . ? O9A C23A C22A 108.0(7) . . ? C24A C23A C22A 114.4(7) . . ? C23A C24A C33A 108.8(7) . . ? C23A C24A C25A 112.7(7) . . ? C33A C24A C25A 109.9(7) . . ? O7A C25A C26A 107.3(6) . . ? O7A C25A C24A 106.1(6) . . ? C26A C25A C24A 117.7(6) . . ? C25A C26A C27A 115.8(6) . . ? C25A C26A C34A 109.6(7) . . ? C27A C26A C34A 108.3(7) . . ? O6A C27A C28A 107.0(6) . . ? O6A C27A C26A 113.6(6) . . ? C28A C27A C26A 113.1(7) . . ? C29A C28A C27A 119.1(7) . . ? C28A C29A O5A 127.5(8) . . ? O8A C35A O7A 123.3(8) . . ? O8A C35A C36A 125.2(8) . . ? O7A C35A C36A 111.5(8) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 70.47 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.440 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.060 #===END data_RSII _database_code_depnum_ccdc_archive 'CCDC 681842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Cl3 N O14' _chemical_formula_weight 851.14 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 0.0091 '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 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.764(5) _cell_length_b 15.876(5) _cell_length_c 12.222(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.34(5) _cell_angle_gamma 90.00 _cell_volume 2111.3(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 4 _cell_measurement_theta_max 17 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 2.520 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method '\w/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4364 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 71.22 _reflns_number_total 4348 _reflns_number_gt 2115 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Restraints were necessary to fix water and hydroxyl geometry: DFIX 1.08 O13 H131 O13 H132 DFIX 1.08 O14 H141 O14 H142 dfix 0.93 o9 h9o o10 h10o o2 h2o dang 2.0 c8 h2o ; _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^)+(0.1900P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0085(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 4348 _refine_ls_number_parameters 542 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2529 _refine_ls_wR_factor_gt 0.1890 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.2778(4) 0.1207(3) 1.0447(4) 0.1543(16) Uani 1 1 d . . . Cl2 Cl 0.3060(4) -0.0548(3) 1.0902(4) 0.1496(14) Uani 1 1 d . . . Cl3 Cl 0.5190(4) 0.0489(4) 1.1663(4) 0.185(2) Uani 1 1 d . . . O1 O 0.5008(5) 0.2011(4) 0.9331(6) 0.0844(16) Uani 1 1 d . . . O2 O 0.2918(5) 0.2739(4) 0.8516(5) 0.0827(16) Uani 1 1 d D . . O3 O 0.2169(5) 0.4537(4) 0.5271(5) 0.0815(16) Uani 1 1 d . . . O4 O 0.4830(6) 0.4461(6) 0.4621(6) 0.108(2) Uani 1 1 d . . . O5 O 0.2156(5) 0.4733(4) 0.3372(5) 0.0869(17) Uani 1 1 d . . . O6 O 0.0314(6) 0.2282(5) 0.1695(6) 0.099(2) Uani 1 1 d . . . O7 O 0.0327(4) 0.1214(4) 0.3448(5) 0.0718(13) Uani 1 1 d . . . O8 O -0.0428(6) 0.2329(5) 0.4071(7) 0.101(2) Uani 1 1 d . . . O9 O 0.1889(5) 0.1261(4) 0.6528(6) 0.0803(15) Uani 1 1 d D . . O10 O 0.3758(5) 0.0457(4) 0.8085(5) 0.0849(17) Uani 1 1 d D . . O11 O 0.8669(5) 0.1203(5) 0.8695(6) 0.0916(18) Uani 1 1 d . . . O12 O 0.6200(6) 0.3142(5) 0.5821(7) 0.104(2) Uani 1 1 d . . . N N 0.6981(6) 0.1378(4) 0.9148(6) 0.0761(18) Uani 1 1 d . . . H0 H 0.6677 0.1237 0.9660 0.091 Uiso 1 1 calc R . . C1 C 0.5233(7) 0.2279(5) 0.8483(7) 0.0647(18) Uani 1 1 d . . . C2 C 0.6379(7) 0.2020(5) 0.8354(8) 0.073(2) Uani 1 1 d . . . C3 C 0.6736(7) 0.2345(6) 0.7533(8) 0.074(2) Uani 1 1 d . . . H3 H 0.7491 0.2192 0.7513 0.089 Uiso 1 1 calc R . . C4 C 0.5943(7) 0.2946(6) 0.6655(8) 0.072(2) Uani 1 1 d . . . C5 C 0.4000(7) 0.3795(5) 0.5969(7) 0.0680(19) Uani 1 1 d . . . C6 C 0.2862(6) 0.3957(5) 0.6067(7) 0.0652(18) Uani 1 1 d . . . C7 C 0.2457(7) 0.3612(6) 0.6872(7) 0.071(2) Uani 1 1 d . . . C8 C 0.3264(7) 0.3054(5) 0.7679(7) 0.0676(19) Uani 1 1 d D . . C9 C 0.4425(7) 0.2858(5) 0.7619(7) 0.0654(17) Uani 1 1 d . . . C10 C 0.4763(6) 0.3197(5) 0.6751(7) 0.0655(18) Uani 1 1 d . . . C11 C 0.4061(7) 0.4332(6) 0.5015(9) 0.081(2) Uani 1 1 d . . . C12 C 0.2851(8) 0.4854(6) 0.4588(8) 0.081(2) Uani 1 1 d . . . C13 C 0.3069(9) 0.5767(7) 0.4790(10) 0.100(3) Uani 1 1 d . . . H13A H 0.3611 0.5957 0.4421 0.151 Uiso 1 1 calc R . . H13B H 0.3435 0.5875 0.5625 0.151 Uiso 1 1 calc R . . H13C H 0.2301 0.6062 0.4457 0.151 Uiso 1 1 calc R . . C14 C 0.1203(8) 0.3802(7) 0.6870(9) 0.091(3) Uani 1 1 d . . . H14A H 0.1226 0.4328 0.7265 0.136 Uiso 1 1 calc R . . H14B H 0.0962 0.3361 0.7275 0.136 Uiso 1 1 calc R . . H14C H 0.0620 0.3838 0.6069 0.136 Uiso 1 1 calc R . . C15 C 0.8019(7) 0.0947(6) 0.9185(8) 0.077(2) Uani 1 1 d . . . C16 C 0.8258(7) 0.0144(5) 0.9870(8) 0.076(2) Uani 1 1 d . . . C17 C 0.7404(7) -0.0431(6) 0.9735(8) 0.080(2) Uani 1 1 d . . . H17 H 0.7639 -0.0901 1.0223 0.096 Uiso 1 1 calc R . . C18 C 0.6127(7) -0.0404(6) 0.8899(8) 0.082(2) Uani 1 1 d . . . H18 H 0.5878 0.0037 0.8359 0.098 Uiso 1 1 calc R . . C19 C 0.5309(8) -0.0984(7) 0.8879(9) 0.088(3) Uani 1 1 d . . . H19 H 0.5579 -0.1402 0.9454 0.105 Uiso 1 1 calc R . . C20 C 0.3992(7) -0.1040(6) 0.8031(8) 0.080(2) Uani 1 1 d . . . H20 H 0.3491 -0.1145 0.8500 0.096 Uiso 1 1 calc R . . C21 C 0.3486(7) -0.0248(5) 0.7294(7) 0.0702(19) Uani 1 1 d . . . H21 H 0.3923 -0.0169 0.6760 0.084 Uiso 1 1 calc R . . C22 C 0.2114(7) -0.0278(6) 0.6550(7) 0.074(2) Uani 1 1 d . . . H22 H 0.1978 -0.0755 0.6006 0.089 Uiso 1 1 calc R . . C23 C 0.1659(7) 0.0523(5) 0.5779(7) 0.072(2) Uani 1 1 d . . . H23 H 0.0768 0.0472 0.5361 0.087 Uiso 1 1 calc R . . C24 C 0.2212(6) 0.0687(5) 0.4862(7) 0.0662(18) Uani 1 1 d . . . H24 H 0.3080 0.0828 0.5292 0.079 Uiso 1 1 calc R . . C25 C 0.1606(6) 0.1453(5) 0.4106(7) 0.070(2) Uani 1 1 d . . . H25 H 0.1637 0.1933 0.4621 0.084 Uiso 1 1 calc R . . C26 C 0.2150(7) 0.1707(6) 0.3205(7) 0.074(2) Uani 1 1 d . . . H26 H 0.2042 0.1228 0.2669 0.089 Uiso 1 1 calc R . . C27 C 0.1563(8) 0.2478(6) 0.2435(8) 0.080(2) Uani 1 1 d . . . H27 H 0.2010 0.2579 0.1914 0.096 Uiso 1 1 calc R . . C28 C 0.1599(8) 0.3265(6) 0.3084(8) 0.077(2) Uani 1 1 d . . . H28 H 0.1231 0.3279 0.3636 0.093 Uiso 1 1 calc R . . C29 C 0.2133(8) 0.3946(6) 0.2908(8) 0.082(2) Uani 1 1 d . . . H29 H 0.2551 0.3887 0.2402 0.098 Uiso 1 1 calc R . . C30 C 0.9593(7) 0.0019(7) 1.0630(8) 0.086(3) Uani 1 1 d . . . H30A H 0.9702 -0.0520 1.1012 0.129 Uiso 1 1 calc R . . H30B H 0.9859 0.0455 1.1217 0.129 Uiso 1 1 calc R . . H30C H 1.0071 0.0043 1.0145 0.129 Uiso 1 1 calc R . . C31 C 0.3856(10) -0.1801(7) 0.7236(12) 0.112(4) Uani 1 1 d . . . H31A H 0.4303 -0.1706 0.6734 0.168 Uiso 1 1 calc R . . H31B H 0.3003 -0.1887 0.6758 0.168 Uiso 1 1 calc R . . H31C H 0.4176 -0.2291 0.7714 0.168 Uiso 1 1 calc R . . C32 C 0.1342(8) -0.0439(8) 0.7291(11) 0.100(3) Uani 1 1 d . . . H32A H 0.1528 -0.0989 0.7643 0.151 Uiso 1 1 calc R . . H32B H 0.0486 -0.0410 0.6793 0.151 Uiso 1 1 calc R . . H32C H 0.1528 -0.0021 0.7901 0.151 Uiso 1 1 calc R . . C33 C 0.2169(9) -0.0078(6) 0.4106(9) 0.086(2) Uani 1 1 d . . . H33A H 0.1342 -0.0284 0.3762 0.128 Uiso 1 1 calc R . . H33B H 0.2694 -0.0509 0.4588 0.128 Uiso 1 1 calc R . . H33C H 0.2446 0.0076 0.3488 0.128 Uiso 1 1 calc R . . C34 C 0.3533(8) 0.1865(7) 0.3812(10) 0.095(3) Uani 1 1 d . . . H34A H 0.3675 0.2318 0.4369 0.142 Uiso 1 1 calc R . . H34B H 0.3861 0.2012 0.3229 0.142 Uiso 1 1 calc R . . H34C H 0.3929 0.1364 0.4221 0.142 Uiso 1 1 calc R . . C35 C -0.0575(8) 0.1706(7) 0.3490(9) 0.083(2) Uani 1 1 d . . . C36 C -0.1781(9) 0.1366(8) 0.2664(13) 0.118(4) Uani 1 1 d . . . H36A H -0.2309 0.1273 0.3089 0.177 Uiso 1 1 calc R . . H36B H -0.1650 0.0844 0.2334 0.177 Uiso 1 1 calc R . . H36C H -0.2159 0.1764 0.2039 0.177 Uiso 1 1 calc R . . C37 C -0.0208(12) 0.2837(9) 0.0749(11) 0.133(5) Uani 1 1 d . . . H37A H -0.0226 0.3394 0.1047 0.200 Uiso 1 1 calc R . . H37B H -0.1031 0.2659 0.0283 0.200 Uiso 1 1 calc R . . H37C H 0.0273 0.2838 0.0267 0.200 Uiso 1 1 calc R . . C38 C 0.3765(10) 0.0346(8) 1.0629(9) 0.101(3) Uani 1 1 d . . . H38 H 0.3853 0.0258 0.9871 0.122 Uiso 1 1 calc R . . O13 O -0.1470(7) 0.2712(6) 0.5773(8) 0.123(3) Uani 1 1 d D . . O14 O 0.0072(8) 0.1582(8) 0.7277(10) 0.148(4) Uani 1 1 d D . . H2O H 0.332(13) 0.224(7) 0.888(12) 0.200 Uiso 1 1 d D . . H9O H 0.132(13) 0.129(12) 0.689(15) 0.20(7) Uiso 1 1 d D . . H10O H 0.323(10) 0.081(7) 0.829(12) 0.14(5) Uiso 1 1 d D . . H131 H -0.237(7) 0.286(10) 0.578(14) 0.17(5) Uiso 1 1 d D . . H132 H -0.121(15) 0.260(12) 0.502(10) 0.19(7) Uiso 1 1 d D . . H141 H -0.041(14) 0.131(10) 0.779(13) 0.20(7) Uiso 1 1 d D . . H142 H -0.049(9) 0.214(5) 0.700(10) 0.12(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.186(4) 0.141(3) 0.171(3) 0.031(3) 0.107(3) 0.054(3) Cl2 0.127(2) 0.149(3) 0.151(3) 0.037(3) 0.028(2) -0.005(2) Cl3 0.134(3) 0.238(5) 0.125(3) 0.021(3) -0.013(2) -0.040(4) O1 0.078(3) 0.094(4) 0.084(4) 0.005(3) 0.034(3) 0.010(3) O2 0.070(3) 0.096(4) 0.089(4) 0.001(3) 0.038(3) 0.001(3) O3 0.059(3) 0.085(4) 0.092(4) 0.021(3) 0.018(3) 0.012(3) O4 0.074(4) 0.135(6) 0.116(5) 0.044(5) 0.039(4) 0.015(4) O5 0.080(4) 0.078(4) 0.087(4) 0.011(3) 0.014(3) -0.001(3) O6 0.092(4) 0.096(4) 0.080(4) 0.008(4) -0.002(3) -0.009(4) O7 0.051(2) 0.079(3) 0.079(3) 0.000(3) 0.017(2) 0.005(2) O8 0.074(4) 0.108(5) 0.120(5) -0.015(5) 0.035(4) 0.015(4) O9 0.074(3) 0.082(4) 0.087(4) -0.002(3) 0.034(3) 0.000(3) O10 0.065(3) 0.094(4) 0.081(4) -0.011(3) 0.011(3) -0.005(3) O11 0.064(3) 0.107(4) 0.107(4) 0.014(4) 0.035(3) 0.009(3) O12 0.076(4) 0.137(6) 0.108(5) 0.034(5) 0.047(4) 0.027(4) N 0.074(4) 0.083(5) 0.075(4) 0.009(4) 0.032(3) 0.018(3) C1 0.065(4) 0.068(4) 0.063(4) -0.005(4) 0.027(4) -0.003(3) C2 0.059(4) 0.080(5) 0.075(5) -0.003(4) 0.019(4) 0.006(4) C3 0.056(4) 0.084(5) 0.081(5) 0.005(5) 0.023(4) 0.009(4) C4 0.059(4) 0.079(5) 0.079(5) 0.004(4) 0.027(4) 0.003(4) C5 0.059(4) 0.064(4) 0.079(5) 0.012(4) 0.024(4) 0.002(3) C6 0.057(4) 0.065(4) 0.070(4) -0.001(4) 0.019(3) 0.000(3) C7 0.053(4) 0.081(5) 0.078(5) 0.001(4) 0.025(4) 0.004(3) C8 0.058(4) 0.070(5) 0.078(5) -0.001(4) 0.029(4) -0.003(3) C9 0.056(4) 0.072(4) 0.069(4) 0.003(4) 0.024(3) 0.001(3) C10 0.054(3) 0.070(4) 0.069(4) -0.002(4) 0.019(3) 0.004(3) C11 0.058(4) 0.085(5) 0.091(6) 0.010(5) 0.018(4) -0.004(4) C12 0.066(4) 0.082(5) 0.086(5) 0.008(5) 0.019(4) 0.003(4) C13 0.081(6) 0.092(7) 0.109(7) 0.003(6) 0.014(5) -0.004(5) C14 0.061(4) 0.118(8) 0.098(6) 0.008(6) 0.035(4) 0.011(5) C15 0.058(4) 0.083(5) 0.084(5) 0.004(5) 0.019(4) 0.008(4) C16 0.060(4) 0.075(5) 0.087(5) 0.002(4) 0.022(4) 0.011(4) C17 0.058(4) 0.089(6) 0.083(5) 0.005(5) 0.016(4) 0.003(4) C18 0.062(4) 0.095(6) 0.082(5) 0.008(5) 0.021(4) 0.004(4) C19 0.066(5) 0.090(6) 0.090(6) 0.004(5) 0.010(4) 0.004(4) C20 0.061(4) 0.088(6) 0.079(5) 0.009(5) 0.012(4) 0.000(4) C21 0.062(4) 0.073(5) 0.072(4) -0.007(4) 0.020(4) -0.003(4) C22 0.052(3) 0.079(5) 0.077(5) 0.004(4) 0.010(4) -0.002(4) C23 0.061(4) 0.076(5) 0.077(5) -0.003(4) 0.023(4) -0.001(4) C24 0.048(3) 0.071(4) 0.071(4) -0.001(4) 0.013(3) 0.001(3) C25 0.050(4) 0.083(5) 0.068(4) -0.004(4) 0.013(3) -0.003(3) C26 0.062(4) 0.083(5) 0.075(5) -0.003(4) 0.022(4) 0.005(4) C27 0.074(5) 0.084(6) 0.074(5) 0.003(5) 0.021(4) -0.011(4) C28 0.076(5) 0.078(5) 0.078(5) 0.000(5) 0.030(4) 0.001(4) C29 0.082(5) 0.081(6) 0.080(5) 0.004(5) 0.029(4) -0.005(5) C30 0.051(4) 0.102(7) 0.089(6) 0.005(5) 0.009(4) 0.006(4) C31 0.081(6) 0.079(6) 0.138(9) 0.006(6) -0.001(6) -0.005(5) C32 0.065(5) 0.122(8) 0.115(7) 0.026(7) 0.035(5) -0.010(5) C33 0.086(6) 0.078(5) 0.095(6) 0.002(5) 0.037(5) 0.010(4) C34 0.065(5) 0.106(7) 0.112(7) 0.010(6) 0.033(5) 0.003(5) C35 0.064(5) 0.087(6) 0.099(6) 0.002(6) 0.032(4) 0.005(4) C36 0.061(5) 0.116(9) 0.155(10) -0.007(8) 0.017(6) 0.000(5) C37 0.135(10) 0.119(9) 0.090(7) 0.023(7) -0.020(7) -0.002(8) C38 0.098(7) 0.124(8) 0.074(5) 0.007(6) 0.024(5) 0.013(6) O13 0.087(4) 0.149(7) 0.137(7) 0.018(6) 0.047(5) 0.027(5) O14 0.113(6) 0.187(9) 0.181(8) 0.064(8) 0.097(6) 0.053(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C38 1.752(12) . ? Cl2 C38 1.739(13) . ? Cl3 C38 1.688(12) . ? O1 C1 1.238(9) . ? O2 C8 1.335(10) . ? O3 C6 1.362(9) . ? O3 C12 1.451(11) . ? O4 C11 1.193(10) . ? O5 C29 1.369(11) . ? O5 C12 1.410(11) . ? O6 C37 1.396(13) . ? O6 C27 1.437(10) . ? O7 C35 1.335(10) . ? O7 C25 1.461(9) . ? O8 C35 1.192(12) . ? O9 C23 1.447(10) . ? O10 C21 1.433(10) . ? O11 C15 1.207(10) . ? O12 C4 1.210(10) . ? N C15 1.384(10) . ? N C2 1.400(11) . ? C1 C9 1.449(11) . ? C1 C2 1.475(11) . ? C2 C3 1.330(12) . ? C3 C4 1.473(12) . ? C4 C10 1.491(10) . ? C5 C10 1.403(11) . ? C5 C6 1.413(10) . ? C5 C11 1.468(12) . ? C6 C7 1.361(11) . ? C7 C8 1.395(11) . ? C7 C14 1.505(11) . ? C8 C9 1.429(10) . ? C9 C10 1.376(11) . ? C11 C12 1.555(12) . ? C12 C13 1.477(15) . ? C15 C16 1.492(12) . ? C16 C17 1.321(12) . ? C16 C30 1.503(11) . ? C17 C18 1.462(11) . ? C18 C19 1.324(13) . ? C19 C20 1.504(12) . ? C20 C31 1.520(16) . ? C20 C21 1.530(12) . ? C21 C22 1.523(10) . ? C22 C32 1.528(13) . ? C22 C23 1.552(12) . ? C23 C24 1.517(11) . ? C24 C33 1.516(12) . ? C24 C25 1.529(11) . ? C25 C26 1.524(12) . ? C26 C34 1.531(12) . ? C26 C27 1.539(13) . ? C27 C28 1.473(12) . ? C28 C29 1.308(13) . ? C35 C36 1.495(14) . ? 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 C6 O3 C12 109.5(6) . . ? C29 O5 C12 118.2(7) . . ? C37 O6 C27 114.0(8) . . ? C35 O7 C25 119.6(7) . . ? C15 N C2 126.1(7) . . ? O1 C1 C9 122.6(7) . . ? O1 C1 C2 119.3(7) . . ? C9 C1 C2 118.2(7) . . ? C3 C2 N 125.7(7) . . ? C3 C2 C1 122.4(8) . . ? N C2 C1 111.8(7) . . ? C2 C3 C4 120.4(7) . . ? O12 C4 C3 119.2(7) . . ? O12 C4 C10 122.4(8) . . ? C3 C4 C10 117.8(7) . . ? C10 C5 C6 116.5(7) . . ? C10 C5 C11 136.3(7) . . ? C6 C5 C11 107.2(7) . . ? C7 C6 O3 120.7(6) . . ? C7 C6 C5 126.2(7) . . ? O3 C6 C5 113.1(7) . . ? C6 C7 C8 115.8(7) . . ? C6 C7 C14 122.0(8) . . ? C8 C7 C14 122.2(8) . . ? O2 C8 C7 117.1(7) . . ? O2 C8 C9 122.3(7) . . ? C7 C8 C9 120.6(7) . . ? C10 C9 C8 121.1(7) . . ? C10 C9 C1 120.5(7) . . ? C8 C9 C1 118.4(7) . . ? C9 C10 C5 119.5(7) . . ? C9 C10 C4 120.4(7) . . ? C5 C10 C4 120.0(7) . . ? O4 C11 C5 133.9(8) . . ? O4 C11 C12 120.8(8) . . ? C5 C11 C12 105.1(7) . . ? O5 C12 O3 109.5(7) . . ? O5 C12 C13 107.7(8) . . ? O3 C12 C13 110.0(9) . . ? O5 C12 C11 111.8(8) . . ? O3 C12 C11 105.0(7) . . ? C13 C12 C11 112.8(8) . . ? O11 C15 N 122.3(8) . . ? O11 C15 C16 123.1(7) . . ? N C15 C16 114.6(8) . . ? C17 C16 C15 123.2(7) . . ? C17 C16 C30 123.5(8) . . ? C15 C16 C30 112.9(7) . . ? C16 C17 C18 126.8(9) . . ? C19 C18 C17 122.6(9) . . ? C18 C19 C20 127.2(9) . . ? C19 C20 C31 108.6(8) . . ? C19 C20 C21 115.2(7) . . ? C31 C20 C21 110.7(7) . . ? O10 C21 C22 110.0(7) . . ? O10 C21 C20 107.9(6) . . ? C22 C21 C20 114.4(7) . . ? C21 C22 C32 112.6(7) . . ? C21 C22 C23 112.3(7) . . ? C32 C22 C23 110.6(7) . . ? O9 C23 C24 107.4(6) . . ? O9 C23 C22 109.9(6) . . ? C24 C23 C22 116.3(7) . . ? C33 C24 C23 112.9(7) . . ? C33 C24 C25 111.6(7) . . ? C23 C24 C25 110.5(6) . . ? O7 C25 C26 107.4(6) . . ? O7 C25 C24 105.8(6) . . ? C26 C25 C24 114.8(7) . . ? C25 C26 C34 110.7(7) . . ? C25 C26 C27 116.0(7) . . ? C34 C26 C27 108.2(7) . . ? O6 C27 C28 109.6(7) . . ? O6 C27 C26 109.0(7) . . ? C28 C27 C26 115.6(7) . . ? C29 C28 C27 121.9(8) . . ? C28 C29 O5 128.4(9) . . ? O8 C35 O7 124.9(8) . . ? O8 C35 C36 126.0(9) . . ? O7 C35 C36 109.1(9) . . ? Cl3 C38 Cl2 112.1(6) . . ? Cl3 C38 Cl1 114.3(7) . . ? Cl2 C38 Cl1 108.7(6) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 71.22 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.329 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.083 #===END data_RX4 _database_code_depnum_ccdc_archive 'CCDC 681843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H59 N3 O15' _chemical_formula_weight 857.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.8420(8) _cell_length_b 19.863(1) _cell_length_c 16.721(1) _cell_angle_alpha 90.00 _cell_angle_beta 91.709(1) _cell_angle_gamma 90.00 _cell_volume 4595.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 4 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.749617 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS procedure' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36988 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 22.47 _reflns_number_total 6178 _reflns_number_gt 5019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Restraints were applied to fix hydrogen geometry and avoid short H...H contacts dang 1.8 h1-1 c1' dfix 0.82 h1-1 o1' bump ; _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^)+(0.1186P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0071(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(13) _refine_ls_number_reflns 6178 _refine_ls_number_parameters 1130 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.007 _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 N1 N 1.0324(3) 0.9360(2) 1.1229(3) 0.0498(11) Uani 1 1 d . . . H1 H 1.0604 0.9224 1.0806 0.060 Uiso 1 1 calc R . . N2 N 0.9745(3) 0.8156(2) 1.2268(3) 0.0488(11) Uani 1 1 d . . . N3 N 0.8264(3) 0.7867(2) 1.2525(3) 0.0549(12) Uani 1 1 d . . . H3 H 0.7776 0.7655 1.2708 0.066 Uiso 1 1 calc R . . O1 O 0.8747(3) 1.0066(2) 1.0588(3) 0.0635(11) Uani 1 1 d . . . H1A H 0.8245 1.0169 1.0345 0.095 Uiso 1 1 calc R . . O2 O 0.7019(3) 1.0300(2) 1.0497(3) 0.0701(12) Uani 1 1 d . . . O3 O 0.4852(3) 0.9097(2) 1.2119(3) 0.0675(11) Uani 1 1 d . . . O4 O 0.6313(3) 0.7757(2) 1.2881(3) 0.0771(13) Uani 1 1 d . . . O5 O 0.4642(3) 0.8586(3) 1.3374(3) 0.0799(14) Uani 1 1 d . . . O6 O 0.6462(5) 1.0350(3) 1.4540(4) 0.117(2) Uani 1 1 d . . . O7 O 0.7843(3) 0.9198(2) 1.5735(2) 0.0598(10) Uani 1 1 d . . . O8 O 0.7507(4) 1.0153(3) 1.6384(3) 0.0930(16) Uani 1 1 d . . . O9 O 0.9905(3) 1.0194(2) 1.5794(3) 0.0733(12) Uani 1 1 d . . . H9 H 0.9387 1.0282 1.5996 0.110 Uiso 1 1 calc R . . O10 O 1.1485(4) 1.0294(2) 1.4897(3) 0.0750(12) Uani 1 1 d . . . H10 H 1.0969 1.0426 1.5067 0.112 Uiso 1 1 calc R . . O11 O 1.0372(3) 1.0021(3) 1.2305(3) 0.0966(18) Uani 1 1 d . . . C1 C 0.8581(4) 0.9541(3) 1.1071(3) 0.0492(13) Uani 1 1 d . . . C2 C 0.9358(4) 0.9170(3) 1.1369(3) 0.0470(13) Uani 1 1 d . . . C3 C 0.9138(4) 0.8618(3) 1.1858(3) 0.0491(13) Uani 1 1 d . . . C4 C 0.8211(4) 0.8434(3) 1.2040(3) 0.0488(13) Uani 1 1 d . . . C5 C 0.6434(4) 0.8732(3) 1.2007(3) 0.0513(13) Uani 1 1 d . . . C6 C 0.5744(4) 0.9209(3) 1.1773(4) 0.0579(15) Uani 1 1 d . . . C7 C 0.5886(4) 0.9741(3) 1.1256(4) 0.0578(15) Uani 1 1 d . . . C8 C 0.6829(4) 0.9818(3) 1.0988(4) 0.0594(15) Uani 1 1 d . . . C9 C 0.7607(4) 0.9378(3) 1.1273(3) 0.0473(13) Uani 1 1 d . . . C10 C 0.7404(4) 0.8829(3) 1.1768(3) 0.0480(13) Uani 1 1 d . . . C11 C 0.5998(4) 0.8259(3) 1.2521(4) 0.0599(15) Uani 1 1 d . . . C12 C 0.4932(4) 0.8478(4) 1.2592(4) 0.0666(17) Uani 1 1 d . . . C13 C 0.4233(5) 0.7972(4) 1.2230(5) 0.090(2) Uani 1 1 d . . . H13A H 0.4265 0.7563 1.2535 0.134 Uiso 1 1 calc R . . H13B H 0.4401 0.7882 1.1688 0.134 Uiso 1 1 calc R . . H13C H 0.3589 0.8151 1.2238 0.134 Uiso 1 1 calc R . . C14 C 0.5106(5) 1.0234(4) 1.1006(5) 0.079(2) Uani 1 1 d . . . H14A H 0.5363 1.0683 1.1021 0.119 Uiso 1 1 calc R . . H14B H 0.4579 1.0201 1.1365 0.119 Uiso 1 1 calc R . . H14C H 0.4877 1.0131 1.0472 0.119 Uiso 1 1 calc R . . C15 C 1.0802(4) 0.9757(3) 1.1764(3) 0.0525(14) Uani 1 1 d . . . C16 C 1.1874(4) 0.9825(3) 1.1673(3) 0.0530(14) Uani 1 1 d . . . C17 C 1.2451(4) 0.9768(3) 1.2329(4) 0.0597(15) Uani 1 1 d . . . H17 H 1.3108 0.9837 1.2260 0.072 Uiso 1 1 calc R . . C18 C 1.2166(4) 0.9612(3) 1.3122(4) 0.0633(16) Uani 1 1 d . . . H18 H 1.1512 0.9535 1.3193 0.076 Uiso 1 1 calc R . . C19 C 1.2737(4) 0.9568(4) 1.3759(4) 0.0718(18) Uani 1 1 d . . . H19 H 1.3374 0.9704 1.3703 0.086 Uiso 1 1 calc R . . C20 C 1.2463(4) 0.9318(4) 1.4579(4) 0.0683(17) Uani 1 1 d . . . H20 H 1.2937 0.9493 1.4973 0.082 Uiso 1 1 calc R . . C21 C 1.1455(4) 0.9577(3) 1.4803(3) 0.0595(15) Uani 1 1 d . . . H21 H 1.1011 0.9479 1.4351 0.071 Uiso 1 1 calc R . . C22 C 1.1014(4) 0.9275(3) 1.5548(3) 0.0586(15) Uani 1 1 d . . . H22 H 1.1020 0.8785 1.5482 0.070 Uiso 1 1 calc R . . C23 C 0.9958(4) 0.9486(3) 1.5640(4) 0.0613(15) Uani 1 1 d . . . H23 H 0.9725 0.9256 1.6115 0.074 Uiso 1 1 calc R . . C24 C 0.9271(4) 0.9293(3) 1.4937(4) 0.0633(16) Uani 1 1 d . . . H24 H 0.9513 0.9519 1.4463 0.076 Uiso 1 1 calc R . . C25 C 0.8237(4) 0.9559(3) 1.5053(3) 0.0576(14) Uani 1 1 d . . . H25 H 0.8267 1.0041 1.5177 0.069 Uiso 1 1 calc R . . C26 C 0.7564(4) 0.9450(3) 1.4323(4) 0.0646(16) Uani 1 1 d . . . H26 H 0.7572 0.8967 1.4200 0.078 Uiso 1 1 calc R . . C27 C 0.6506(5) 0.9642(4) 1.4488(4) 0.0755(19) Uani 1 1 d . . . H27 H 0.6322 0.9446 1.4999 0.091 Uiso 1 1 calc R . . C28 C 0.5812(5) 0.9391(4) 1.3824(4) 0.082(2) Uani 1 1 d . . . H28 H 0.5812 0.9605 1.3329 0.098 Uiso 1 1 calc R . . C29 C 0.5239(5) 0.8903(5) 1.3923(4) 0.079(2) Uani 1 1 d . . . H29 H 0.5220 0.8737 1.4442 0.095 Uiso 1 1 calc R . . C30 C 1.2220(4) 0.9922(4) 1.0837(4) 0.0702(18) Uani 1 1 d . . . H30A H 1.2907 0.9989 1.0854 0.105 Uiso 1 1 calc R . . H30B H 1.1909 1.0308 1.0601 0.105 Uiso 1 1 calc R . . H30C H 1.2066 0.9530 1.0523 0.105 Uiso 1 1 calc R . . C31 C 1.2512(6) 0.8546(4) 1.4599(5) 0.092(2) Uani 1 1 d . . . H31A H 1.2000 0.8363 1.4265 0.139 Uiso 1 1 calc R . . H31B H 1.2442 0.8391 1.5139 0.139 Uiso 1 1 calc R . . H31C H 1.3123 0.8399 1.4406 0.139 Uiso 1 1 calc R . . C32 C 1.1617(5) 0.9435(4) 1.6310(4) 0.0766(19) Uani 1 1 d . . . H32A H 1.2252 0.9245 1.6268 0.115 Uiso 1 1 calc R . . H32B H 1.1310 0.9245 1.6765 0.115 Uiso 1 1 calc R . . H32C H 1.1668 0.9914 1.6375 0.115 Uiso 1 1 calc R . . C33 C 0.9295(5) 0.8534(4) 1.4762(5) 0.092(2) Uani 1 1 d . . . H33A H 0.9942 0.8401 1.4645 0.138 Uiso 1 1 calc R . . H33B H 0.8873 0.8435 1.4311 0.138 Uiso 1 1 calc R . . H33C H 0.9084 0.8290 1.5221 0.138 Uiso 1 1 calc R . . C34 C 0.7923(6) 0.9812(5) 1.3605(4) 0.099(3) Uani 1 1 d . . . H34A H 0.7418 0.9831 1.3199 0.148 Uiso 1 1 calc R . . H34B H 0.8469 0.9577 1.3401 0.148 Uiso 1 1 calc R . . H34C H 0.8112 1.0261 1.3753 0.148 Uiso 1 1 calc R . . C35 C 0.7471(4) 0.9550(4) 1.6334(4) 0.0633(16) Uani 1 1 d . . . C36 C 0.7000(6) 0.9111(4) 1.6924(4) 0.087(2) Uani 1 1 d . . . H36A H 0.6776 0.9380 1.7357 0.14(4) Uiso 1 1 calc R . . H36B H 0.7457 0.8785 1.7127 0.216 Uiso 1 1 calc R . . H36C H 0.6462 0.8883 1.6669 0.216 Uiso 1 1 calc R . . C37 C 0.5620(12) 1.0575(8) 1.4958(7) 0.194(8) Uani 1 1 d . . . H37A H 0.5281 1.0192 1.5159 0.291 Uiso 1 1 calc R . . H37B H 0.5201 1.0821 1.4595 0.291 Uiso 1 1 calc R . . H37C H 0.5819 1.0861 1.5395 0.291 Uiso 1 1 calc R . . C211 C 1.0740(4) 0.8123(3) 1.2321(4) 0.0584(15) Uani 1 1 d . . . H211 H 1.1115 0.8436 1.2056 0.070 Uiso 1 1 calc R . . C311 C 1.1162(4) 0.7631(3) 1.2764(4) 0.0606(15) Uani 1 1 d . . . H311 H 1.1833 0.7613 1.2808 0.073 Uiso 1 1 calc R . . C411 C 1.0609(5) 0.7136(3) 1.3166(3) 0.0592(15) Uani 1 1 d . . . C511 C 0.9635(5) 0.7181(3) 1.3109(4) 0.0590(15) Uani 1 1 d . . . H511 H 0.9255 0.6866 1.3366 0.071 Uiso 1 1 calc R . . C611 C 0.9196(4) 0.7700(3) 1.2665(3) 0.0521(14) Uani 1 1 d . . . C711 C 1.1146(5) 0.6598(3) 1.3616(4) 0.0786(19) Uani 1 1 d . . . H71A H 1.0694 0.6307 1.3871 0.118 Uiso 1 1 calc R . . H71B H 1.1567 0.6800 1.4015 0.118 Uiso 1 1 calc R . . H71C H 1.1522 0.6341 1.3253 0.118 Uiso 1 1 calc R . . N1' N 1.0384(3) 0.7414(2) 0.9868(3) 0.0524(11) Uani 1 1 d . . . H1' H 1.0447 0.7080 0.9545 0.063 Uiso 1 1 calc R . . N2' N 0.9441(3) 0.8766(2) 0.9167(3) 0.0514(11) Uani 1 1 d . . . N3' N 0.7880(3) 0.8976(2) 0.9189(3) 0.0544(12) Uani 1 1 d . . . H3' H 0.7326 0.9163 0.9107 0.065 Uiso 1 1 calc R . . O1' O 0.9162(3) 0.6722(2) 1.0778(3) 0.0767(13) Uani 1 1 d D . . O2' O 0.7521(3) 0.6422(3) 1.1178(3) 0.0803(13) Uani 1 1 d . . . O3' O 0.4815(3) 0.7616(2) 1.0113(3) 0.0670(11) Uani 1 1 d . . . O4' O 0.5898(3) 0.8979(2) 0.9116(3) 0.0752(12) Uani 1 1 d . . . O5' O 0.4256(3) 0.8033(2) 0.8880(3) 0.0706(12) Uani 1 1 d . . . O6' O 0.5729(4) 0.6314(3) 0.7494(3) 0.0986(17) Uani 1 1 d . . . O7' O 0.7279(3) 0.7343(2) 0.6397(3) 0.0713(12) Uani 1 1 d . . . O8' O 0.6816(6) 0.6456(4) 0.5653(4) 0.124(2) Uani 1 1 d . . . O9' O 0.9060(3) 0.6024(2) 0.6441(3) 0.0718(12) Uani 1 1 d . . . H9' H 0.8526 0.5954 0.6231 0.108 Uiso 1 1 calc R . . O10' O 1.0862(5) 0.6032(3) 0.7345(4) 0.123(2) Uani 1 1 d . . . H10' H 1.0301 0.5916 0.7411 0.185 Uiso 1 1 calc R . . O11' O 1.1219(3) 0.8202(2) 1.0565(3) 0.0678(11) Uani 1 1 d . . . C1' C 0.8797(4) 0.7270(3) 1.0382(3) 0.0547(14) Uani 1 1 d D . . C2' C 0.9432(4) 0.7666(3) 0.9971(3) 0.0500(13) Uani 1 1 d . . . C3' C 0.9034(4) 0.8239(3) 0.9609(3) 0.0459(13) Uani 1 1 d . . . C4' C 0.8047(4) 0.8380(3) 0.9613(3) 0.0485(13) Uani 1 1 d . . . C5' C 0.6358(4) 0.8026(3) 0.9930(3) 0.0471(13) Uani 1 1 d . . . C6' C 0.5791(4) 0.7524(3) 1.0273(4) 0.0587(16) Uani 1 1 d . . . C7' C 0.6127(4) 0.6989(3) 1.0707(4) 0.0635(16) Uani 1 1 d . . . C8' C 0.7139(4) 0.6922(3) 1.0789(3) 0.0601(15) Uani 1 1 d . . . C9' C 0.7777(4) 0.7394(3) 1.0391(3) 0.0491(13) Uani 1 1 d . . . C10' C 0.7378(4) 0.7956(3) 0.9978(3) 0.0460(13) Uani 1 1 d . . . C11' C 0.5739(4) 0.8468(3) 0.9516(4) 0.0579(15) Uani 1 1 d . . . C12' C 0.4696(4) 0.8209(3) 0.9608(4) 0.0583(15) Uani 1 1 d . . . C13' C 0.4022(5) 0.8694(4) 1.0002(4) 0.0735(18) Uani 1 1 d . . . H13D H 0.3911 0.9075 0.9658 0.110 Uiso 1 1 calc R . . H13E H 0.4308 0.8843 1.0502 0.110 Uiso 1 1 calc R . . H13F H 0.3419 0.8474 1.0098 0.110 Uiso 1 1 calc R . . C14' C 0.5474(5) 0.6460(4) 1.1058(5) 0.090(2) Uani 1 1 d . . . H14D H 0.5589 0.6436 1.1626 0.135 Uiso 1 1 calc R . . H14E H 0.5607 0.6030 1.0822 0.135 Uiso 1 1 calc R . . H14F H 0.4811 0.6579 1.0947 0.135 Uiso 1 1 calc R . . C15' C 1.1197(4) 0.7653(3) 1.0235(3) 0.0512(13) Uani 1 1 d . . . C16' C 1.2053(4) 0.7199(3) 1.0217(4) 0.0573(15) Uani 1 1 d . . . C17' C 1.2423(4) 0.6960(3) 0.9553(4) 0.0581(15) Uani 1 1 d . . . H17' H 1.2950 0.6672 0.9614 0.070 Uiso 1 1 calc R . . C18' C 1.2089(5) 0.7102(4) 0.8742(4) 0.0690(17) Uani 1 1 d . . . H18' H 1.1638 0.7446 0.8672 0.083 Uiso 1 1 calc R . . C19' C 1.2364(4) 0.6790(4) 0.8097(4) 0.0667(16) Uani 1 1 d . . . H19' H 1.2836 0.6459 0.8152 0.080 Uiso 1 1 calc R . . C20' C 1.1952(4) 0.6942(4) 0.7262(4) 0.0693(17) Uani 1 1 d . . . H20' H 1.2303 0.6662 0.6886 0.083 Uiso 1 1 calc R . . C21' C 1.0895(4) 0.6725(3) 0.7210(4) 0.0620(16) Uani 1 1 d . . . H21' H 1.0570 0.6942 0.7654 0.074 Uiso 1 1 calc R . . C22' C 1.0325(4) 0.6903(4) 0.6449(4) 0.0703(18) Uani 1 1 d . . . H22' H 1.0374 0.7392 0.6390 0.084 Uiso 1 1 calc R . . C23' C 0.9237(5) 0.6743(3) 0.6479(4) 0.0652(16) Uani 1 1 d . . . H23' H 0.8936 0.6937 0.5994 0.078 Uiso 1 1 calc R . . C24' C 0.8700(4) 0.7036(3) 0.7182(4) 0.0627(16) Uani 1 1 d . . . H24' H 0.8913 0.6791 0.7665 0.075 Uiso 1 1 calc R . . C25' C 0.7607(4) 0.6915(3) 0.7058(3) 0.0583(15) Uani 1 1 d . . . H25' H 0.7498 0.6443 0.6911 0.070 Uiso 1 1 calc R . . C26' C 0.7005(4) 0.7086(3) 0.7785(4) 0.0623(16) Uani 1 1 d . . . H26' H 0.7126 0.7559 0.7923 0.075 Uiso 1 1 calc R . . C27' C 0.5917(5) 0.7008(4) 0.7586(4) 0.0746(19) Uani 1 1 d . . . H27' H 0.5742 0.7251 0.7093 0.089 Uiso 1 1 calc R . . C28' C 0.5299(6) 0.7246(6) 0.8272(6) 0.109(3) Uani 1 1 d . . . H28' H 0.5339 0.6978 0.8728 0.130 Uiso 1 1 calc R . . C29' C 0.4787(6) 0.7708(6) 0.8319(6) 0.112(3) Uani 1 1 d . . . H29' H 0.4717 0.7921 0.7826 0.135 Uiso 1 1 calc R . . C30' C 1.2456(5) 0.7027(5) 1.1036(5) 0.094(2) Uani 1 1 d . . . H30D H 1.3026 0.6756 1.0987 0.141 Uiso 1 1 calc R . . H30E H 1.1982 0.6781 1.1325 0.141 Uiso 1 1 calc R . . H30F H 1.2618 0.7434 1.1320 0.141 Uiso 1 1 calc R . . C31' C 1.2125(7) 0.7668(6) 0.7037(6) 0.123(4) Uani 1 1 d . . . H31D H 1.1943 0.7735 0.6484 0.185 Uiso 1 1 calc R . . H31E H 1.2798 0.7774 0.7119 0.185 Uiso 1 1 calc R . . H31F H 1.1745 0.7956 0.7364 0.185 Uiso 1 1 calc R . . C32' C 1.0758(6) 0.6599(6) 0.5704(4) 0.102(3) Uani 1 1 d . . . H32D H 1.1431 0.6715 0.5688 0.153 Uiso 1 1 calc R . . H32E H 1.0425 0.6773 0.5236 0.153 Uiso 1 1 calc R . . H32F H 1.0692 0.6118 0.5718 0.153 Uiso 1 1 calc R . . C33' C 0.8926(5) 0.7790(4) 0.7319(5) 0.083(2) Uani 1 1 d . . . H33D H 0.8812 0.8033 0.6829 0.124 Uiso 1 1 calc R . . H33E H 0.9591 0.7841 0.7490 0.124 Uiso 1 1 calc R . . H33F H 0.8517 0.7965 0.7724 0.124 Uiso 1 1 calc R . . C34' C 0.7312(5) 0.6662(5) 0.8500(4) 0.089(2) Uani 1 1 d . . . H34D H 0.6912 0.6767 0.8943 0.134 Uiso 1 1 calc R . . H34E H 0.7975 0.6755 0.8644 0.134 Uiso 1 1 calc R . . H34F H 0.7242 0.6194 0.8367 0.134 Uiso 1 1 calc R . . C35' C 0.6905(5) 0.7054(5) 0.5735(4) 0.079(2) Uani 1 1 d . . . C36' C 0.6627(9) 0.7580(6) 0.5120(6) 0.135(4) Uani 1 1 d . . . H36D H 0.7192 0.7723 0.4848 0.203 Uiso 1 1 calc R . . H36E H 0.6344 0.7960 0.5381 0.203 Uiso 1 1 calc R . . H36F H 0.6168 0.7393 0.4740 0.203 Uiso 1 1 calc R . . C37' C 0.4837(8) 0.6187(7) 0.7039(7) 0.152(5) Uani 1 1 d . . . H37D H 0.4298 0.6335 0.7342 0.228 Uiso 1 1 calc R . . H37E H 0.4778 0.5713 0.6933 0.228 Uiso 1 1 calc R . . H37F H 0.4846 0.6428 0.6542 0.228 Uiso 1 1 calc R . . C5A C 0.8945(5) 0.9790(3) 0.8498(4) 0.0636(16) Uani 1 1 d . . . H5A H 0.8460 1.0090 0.8340 0.076 Uiso 1 1 calc R . . C6A C 0.8727(4) 0.9209(3) 0.8931(3) 0.0537(14) Uani 1 1 d . . . C2A C 1.0396(4) 0.8890(3) 0.8980(4) 0.0597(15) Uani 1 1 d . . . H2A H 1.0886 0.8596 0.9145 0.072 Uiso 1 1 calc R . . C3A C 1.0596(5) 0.9454(4) 0.8550(4) 0.0686(17) Uani 1 1 d . . . H3A H 1.1232 0.9537 0.8413 0.082 Uiso 1 1 calc R . . C4A C 0.9887(5) 0.9907(3) 0.8310(3) 0.0611(15) Uani 1 1 d . . . C7A C 1.0156(6) 1.0528(4) 0.7852(4) 0.083(2) Uani 1 1 d . . . H7A1 H 0.9798 1.0906 0.8044 0.125 Uiso 1 1 calc R . . H7A2 H 1.0006 1.0461 0.7294 0.125 Uiso 1 1 calc R . . H7A3 H 1.0835 1.0612 0.7927 0.125 Uiso 1 1 calc R . . O1W O 0.9944(4) 0.6118(3) 0.9226(4) 0.1115(19) Uani 1 1 d . . . H11W H 0.9786 0.5742 0.9431 0.300 Uiso 1 1 d R . . H21W H 0.9925 0.6056 0.8647 0.300 Uiso 1 1 d R . . O2W O 0.3263(6) 0.5327(3) 0.1210(4) 0.140(3) Uani 1 1 d . . . H12W H 0.3141 0.5564 0.0794 0.300 Uiso 1 1 d R . . H22W H 0.3693 0.4964 0.1060 0.300 Uiso 1 1 d R . . O3W O 0.5202(6) 0.4744(5) 0.2052(6) 0.175(4) Uani 1 1 d . . . H13W H 0.5014 0.4646 0.1576 0.300 Uiso 1 1 d R . . H23W H 0.5878 0.4895 0.2056 0.300 Uiso 1 1 d R . . O4W O 0.3759(9) 0.5951(6) 0.2685(4) 0.231(7) Uani 1 1 d . . . H14W H 0.3672 0.5649 0.3143 0.300 Uiso 1 1 d R . . H24W H 0.3575 0.5715 0.2187 0.300 Uiso 1 1 d R . . O5W O 0.7630(9) 0.6410(7) 0.3110(11) 0.277(8) Uani 1 1 d . . . H25W H 0.7095 0.6519 0.3417 0.300 Uiso 1 1 d R . . H15W H 0.7385 0.6282 0.2573 0.300 Uiso 1 1 d R . . O6W O 0.5301(6) 0.6622(5) 0.3527(5) 0.165(3) Uani 1 1 d . . . H16W H 0.4986 0.6352 0.3101 0.300 Uiso 1 1 d R . . H26W H 0.5248 0.7102 0.3391 0.300 Uiso 1 1 d R . . O7W O 0.7118(7) 0.5175(7) 0.1870(12) 0.329(11) Uani 1 1 d . . . H17W H 0.7326 0.5511 0.1612 0.400 Uiso 1 1 d R . . H27W H 0.7386 0.5182 0.2421 0.400 Uiso 1 1 d R . . O8W O 0.6634(12) 0.5742(7) 0.4127(7) 0.243(6) Uani 1 1 d . . . H18W H 0.7036 0.5713 0.4521 0.300 Uiso 1 1 d R . . H28W H 0.5999 0.5634 0.4311 0.300 Uiso 1 1 d R . . H1-1 H 0.868(3) 0.649(3) 1.086(5) 0.13(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.046(2) 0.054(3) 0.051(2) -0.003(2) 0.014(2) 0.000(2) N2 0.050(3) 0.043(2) 0.054(3) 0.000(2) 0.015(2) 0.001(2) N3 0.053(3) 0.047(3) 0.066(3) 0.001(2) 0.017(2) -0.010(2) O1 0.054(2) 0.060(3) 0.077(3) 0.015(2) 0.001(2) -0.005(2) O2 0.058(2) 0.064(3) 0.087(3) 0.018(2) -0.003(2) -0.002(2) O3 0.041(2) 0.083(3) 0.079(3) -0.001(2) 0.009(2) -0.003(2) O4 0.058(2) 0.071(3) 0.104(3) 0.018(3) 0.023(2) -0.006(2) O5 0.048(2) 0.114(4) 0.079(3) 0.000(3) 0.016(2) -0.004(2) O6 0.144(5) 0.099(4) 0.106(4) -0.034(3) -0.030(4) 0.050(4) O7 0.063(2) 0.055(2) 0.062(2) -0.010(2) 0.0107(19) 0.0038(19) O8 0.120(4) 0.073(4) 0.088(3) -0.025(3) 0.035(3) -0.002(3) O9 0.067(3) 0.073(3) 0.079(3) -0.024(2) -0.001(2) 0.010(2) O10 0.088(3) 0.068(3) 0.070(3) 0.010(2) 0.016(2) 0.012(2) O11 0.047(2) 0.147(5) 0.096(3) -0.067(4) 0.011(2) 0.007(3) C1 0.053(3) 0.046(3) 0.049(3) -0.001(3) 0.009(2) -0.005(3) C2 0.044(3) 0.044(3) 0.054(3) -0.005(3) 0.012(2) 0.000(3) C3 0.050(3) 0.041(3) 0.056(3) -0.004(3) 0.015(3) 0.002(3) C4 0.050(3) 0.042(3) 0.055(3) -0.004(3) 0.013(3) -0.002(2) C5 0.039(3) 0.052(3) 0.063(3) -0.005(3) 0.004(3) -0.002(3) C6 0.050(3) 0.054(4) 0.070(4) -0.011(3) 0.007(3) -0.011(3) C7 0.047(3) 0.052(4) 0.074(4) -0.009(3) -0.002(3) -0.001(3) C8 0.062(4) 0.052(4) 0.064(4) -0.008(3) 0.003(3) -0.007(3) C9 0.043(3) 0.043(3) 0.056(3) -0.006(3) 0.004(2) -0.005(2) C10 0.044(3) 0.048(3) 0.053(3) -0.011(3) 0.004(2) -0.005(3) C11 0.052(3) 0.058(4) 0.069(4) -0.004(3) 0.009(3) -0.006(3) C12 0.051(3) 0.071(4) 0.078(4) 0.000(4) 0.016(3) -0.008(3) C13 0.058(4) 0.100(6) 0.111(6) 0.000(5) 0.001(4) -0.027(4) C14 0.051(4) 0.079(5) 0.107(5) 0.012(4) 0.003(4) 0.007(3) C15 0.047(3) 0.053(3) 0.058(3) 0.000(3) 0.011(3) 0.005(3) C16 0.045(3) 0.051(3) 0.063(4) -0.001(3) 0.013(3) 0.001(3) C17 0.042(3) 0.069(4) 0.068(4) 0.000(3) 0.015(3) -0.004(3) C18 0.039(3) 0.086(5) 0.065(4) 0.002(3) 0.006(3) -0.002(3) C19 0.048(3) 0.089(5) 0.080(4) 0.004(4) 0.018(3) 0.007(3) C20 0.049(3) 0.087(5) 0.069(4) 0.004(4) 0.001(3) 0.004(3) C21 0.059(3) 0.066(4) 0.054(3) -0.002(3) 0.005(3) 0.012(3) C22 0.064(4) 0.059(4) 0.053(3) 0.000(3) 0.010(3) 0.002(3) C23 0.066(4) 0.061(4) 0.057(3) -0.002(3) 0.008(3) 0.003(3) C24 0.063(4) 0.065(4) 0.063(4) -0.014(3) 0.012(3) 0.002(3) C25 0.056(3) 0.055(3) 0.062(3) -0.006(3) 0.014(3) -0.004(3) C26 0.063(4) 0.066(4) 0.064(4) -0.011(3) 0.004(3) -0.001(3) C27 0.075(4) 0.086(5) 0.064(4) -0.014(4) -0.005(3) 0.020(4) C28 0.074(5) 0.099(6) 0.071(4) 0.003(4) 0.000(4) 0.022(5) C29 0.050(4) 0.117(6) 0.070(4) 0.002(4) 0.008(3) 0.006(4) C30 0.053(3) 0.091(5) 0.067(4) 0.001(4) 0.019(3) -0.011(3) C31 0.088(5) 0.089(6) 0.102(6) 0.021(5) 0.032(4) 0.036(4) C32 0.077(4) 0.095(5) 0.058(4) 0.007(4) 0.004(3) 0.004(4) C33 0.071(4) 0.082(5) 0.124(6) -0.045(5) 0.015(4) 0.008(4) C34 0.098(5) 0.138(8) 0.061(4) -0.004(5) -0.002(4) -0.028(5) C35 0.060(4) 0.071(5) 0.058(4) -0.004(3) 0.006(3) 0.007(3) C36 0.095(5) 0.087(5) 0.080(5) 0.011(4) 0.033(4) 0.014(4) C37 0.245(15) 0.210(14) 0.125(8) -0.035(9) -0.013(9) 0.166(13) C211 0.048(3) 0.060(4) 0.068(4) 0.009(3) 0.015(3) 0.001(3) C311 0.055(3) 0.065(4) 0.062(4) 0.009(3) 0.011(3) 0.012(3) C411 0.073(4) 0.052(4) 0.053(3) -0.002(3) 0.013(3) 0.004(3) C511 0.067(4) 0.045(3) 0.065(4) 0.003(3) 0.012(3) -0.004(3) C611 0.057(4) 0.046(3) 0.054(3) -0.006(3) 0.015(3) -0.002(3) C711 0.091(5) 0.066(4) 0.079(4) 0.015(4) 0.005(4) 0.010(4) N1' 0.040(3) 0.051(3) 0.066(3) -0.008(2) 0.002(2) 0.004(2) N2' 0.046(3) 0.051(3) 0.057(3) -0.001(2) 0.003(2) 0.001(2) N3' 0.047(3) 0.054(3) 0.063(3) 0.002(2) 0.001(2) 0.008(2) O1' 0.063(3) 0.070(3) 0.097(3) 0.028(3) 0.005(2) 0.013(3) O2' 0.067(3) 0.079(3) 0.095(3) 0.032(3) 0.005(2) 0.003(2) O3' 0.045(2) 0.066(3) 0.091(3) 0.001(2) 0.012(2) 0.0009(19) O4' 0.054(2) 0.065(3) 0.106(3) 0.014(3) -0.006(2) 0.004(2) O5' 0.041(2) 0.090(3) 0.081(3) -0.022(3) 0.001(2) 0.007(2) O6' 0.096(4) 0.090(4) 0.111(4) -0.025(3) 0.021(3) -0.033(3) O7' 0.074(3) 0.065(3) 0.074(3) -0.001(2) -0.010(2) -0.002(2) O8' 0.184(7) 0.089(4) 0.094(4) -0.016(3) -0.050(4) -0.006(4) O9' 0.071(3) 0.069(3) 0.075(3) -0.021(2) -0.005(2) 0.005(2) O10' 0.156(6) 0.091(4) 0.121(5) 0.028(4) -0.035(5) -0.051(4) O11' 0.063(2) 0.056(3) 0.084(3) -0.016(2) -0.004(2) 0.008(2) C1' 0.060(4) 0.044(3) 0.060(3) 0.002(3) 0.000(3) 0.012(3) C2' 0.045(3) 0.052(3) 0.052(3) -0.007(3) 0.001(2) 0.003(3) C3' 0.044(3) 0.046(3) 0.048(3) -0.003(3) 0.003(2) -0.001(2) C4' 0.054(3) 0.044(3) 0.047(3) -0.002(3) 0.002(2) 0.004(3) C5' 0.043(3) 0.044(3) 0.055(3) -0.003(3) 0.001(2) 0.001(2) C6' 0.042(3) 0.061(4) 0.074(4) -0.012(3) 0.008(3) 0.004(3) C7' 0.053(4) 0.065(4) 0.073(4) 0.007(3) 0.017(3) 0.002(3) C8' 0.064(4) 0.057(4) 0.061(3) 0.010(3) 0.013(3) 0.006(3) C9' 0.044(3) 0.049(3) 0.055(3) -0.001(3) 0.003(2) 0.003(2) C10' 0.046(3) 0.046(3) 0.046(3) -0.008(2) 0.004(2) -0.002(2) C11' 0.053(3) 0.048(4) 0.074(4) -0.005(3) 0.007(3) -0.001(3) C12' 0.039(3) 0.065(4) 0.071(4) -0.007(3) 0.003(3) 0.003(3) C13' 0.058(4) 0.078(4) 0.085(4) -0.011(4) 0.009(3) 0.007(3) C14' 0.063(4) 0.089(5) 0.121(6) 0.027(5) 0.032(4) -0.009(4) C15' 0.052(3) 0.044(3) 0.057(3) -0.003(3) 0.004(3) 0.002(3) C16' 0.042(3) 0.056(4) 0.074(4) -0.012(3) -0.005(3) 0.005(3) C17' 0.049(3) 0.054(4) 0.071(4) -0.007(3) -0.003(3) 0.004(3) C18' 0.056(4) 0.068(4) 0.083(5) -0.003(4) 0.011(3) 0.013(3) C19' 0.048(3) 0.076(4) 0.077(4) -0.007(4) 0.011(3) 0.005(3) C20' 0.057(4) 0.081(5) 0.070(4) 0.005(4) 0.012(3) 0.001(3) C21' 0.061(4) 0.066(4) 0.060(4) -0.012(3) 0.017(3) 0.000(3) C22' 0.065(4) 0.086(5) 0.061(4) -0.003(3) 0.016(3) 0.004(4) C23' 0.072(4) 0.067(4) 0.057(3) -0.011(3) 0.006(3) 0.005(3) C24' 0.057(3) 0.067(4) 0.065(4) -0.014(3) 0.005(3) 0.000(3) C25' 0.061(3) 0.052(3) 0.062(3) -0.010(3) -0.002(3) 0.001(3) C26' 0.059(3) 0.062(4) 0.066(4) -0.022(3) 0.000(3) 0.004(3) C27' 0.061(4) 0.082(5) 0.081(4) -0.036(4) 0.010(3) -0.002(3) C28' 0.075(5) 0.120(8) 0.131(7) -0.046(6) 0.003(5) 0.002(5) C29' 0.058(4) 0.151(9) 0.127(7) -0.074(7) -0.012(5) 0.004(5) C30' 0.076(4) 0.108(6) 0.096(5) -0.028(5) -0.024(4) 0.035(4) C31' 0.109(7) 0.134(9) 0.126(7) 0.040(7) -0.013(6) -0.050(6) C32' 0.091(5) 0.157(8) 0.058(4) -0.017(5) 0.019(4) -0.005(5) C33' 0.065(4) 0.079(5) 0.104(6) -0.038(4) 0.003(4) -0.010(4) C34' 0.080(5) 0.123(7) 0.064(4) -0.021(4) 0.011(4) 0.018(5) C35' 0.079(5) 0.089(6) 0.069(4) -0.001(4) -0.020(4) -0.005(4) C36' 0.162(10) 0.128(8) 0.113(7) 0.026(7) -0.053(7) -0.007(7) C37' 0.129(9) 0.181(12) 0.147(9) -0.066(9) 0.014(7) -0.082(9) C5A 0.074(4) 0.051(4) 0.066(4) 0.009(3) 0.003(3) 0.002(3) C6A 0.057(4) 0.050(3) 0.054(3) 0.000(3) 0.004(3) -0.001(3) C2A 0.048(3) 0.064(4) 0.067(4) 0.002(3) 0.010(3) -0.007(3) C3A 0.060(4) 0.076(5) 0.071(4) 0.003(4) 0.011(3) -0.018(4) C4A 0.077(4) 0.055(4) 0.051(3) -0.004(3) 0.007(3) -0.006(3) C7A 0.115(6) 0.064(4) 0.072(4) 0.007(4) 0.015(4) -0.025(4) O1W 0.098(4) 0.063(3) 0.171(6) -0.028(3) -0.023(4) 0.003(3) O2W 0.204(8) 0.088(4) 0.129(5) 0.004(4) 0.020(5) -0.006(5) O3W 0.137(6) 0.187(9) 0.201(8) -0.049(7) -0.001(6) -0.049(6) O4W 0.300(13) 0.290(13) 0.101(5) 0.040(7) -0.008(6) -0.211(12) O5W 0.159(9) 0.209(12) 0.46(2) -0.118(15) -0.017(12) 0.010(8) O6W 0.168(7) 0.155(7) 0.171(7) 0.054(6) -0.033(6) -0.056(6) O7W 0.106(6) 0.247(14) 0.63(3) 0.265(18) -0.019(11) -0.016(7) O8W 0.341(18) 0.170(10) 0.217(11) -0.001(9) 0.027(11) 0.040(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 N1 C15 1.351(7) . ? N1 C2 1.415(7) . ? N2 C611 1.367(7) . ? N2 C211 1.379(7) . ? N2 C3 1.409(7) . ? N3 C611 1.346(7) . ? N3 C4 1.389(7) . ? O1 C1 1.344(7) . ? O2 C8 1.293(7) . ? O3 C6 1.397(7) . ? O3 C12 1.463(8) . ? O4 C11 1.237(7) . ? O5 C29 1.369(9) . ? O5 C12 1.397(8) . ? O6 C27 1.410(10) . ? O6 C37 1.448(14) . ? O7 C35 1.337(7) . ? O7 C25 1.467(7) . ? O8 C35 1.202(8) . ? O9 C23 1.433(8) . ? O10 C21 1.434(8) . ? O11 C15 1.216(7) . ? C1 C2 1.385(8) . ? C1 C9 1.436(7) . ? C2 C3 1.406(8) . ? C3 C4 1.376(7) . ? C4 C10 1.428(8) . ? C5 C6 1.393(9) . ? C5 C11 1.420(9) . ? C5 C10 1.425(8) . ? C6 C7 1.383(9) . ? C7 C8 1.402(8) . ? C7 C14 1.507(9) . ? C8 C9 1.456(8) . ? C9 C10 1.404(8) . ? C11 C12 1.547(9) . ? C12 C13 1.508(10) . ? C15 C16 1.502(8) . ? C16 C17 1.343(8) . ? C16 C30 1.504(8) . ? C17 C18 1.428(8) . ? C18 C19 1.310(9) . ? C19 C20 1.517(9) . ? C20 C31 1.536(11) . ? C20 C21 1.543(8) . ? C21 C22 1.526(8) . ? C22 C23 1.532(8) . ? C22 C32 1.535(9) . ? C23 C24 1.538(9) . ? C24 C33 1.537(10) . ? C24 C25 1.543(8) . ? C25 C26 1.530(8) . ? C26 C34 1.498(10) . ? C26 C27 1.545(9) . ? C27 C28 1.529(10) . ? C28 C29 1.267(11) . ? C35 C36 1.481(10) . ? C211 C311 1.349(8) . ? C311 C411 1.426(9) . ? C411 C511 1.352(9) . ? C411 C711 1.493(9) . ? C511 C611 1.398(8) . ? N1' C15' 1.352(7) . ? N1' C2' 1.426(7) . ? N2' C6A 1.372(7) . ? N2' C2A 1.389(7) . ? N2' C3' 1.409(7) . ? N3' C6A 1.344(7) . ? N3' C4' 1.394(7) . ? O1' C1' 1.362(7) . ? O2' C8' 1.292(7) . ? O3' C6' 1.382(7) . ? O3' C12' 1.454(8) . ? O4' C11' 1.237(7) . ? O5' C29' 1.371(10) . ? O5' C12' 1.389(7) . ? O6' C27' 1.410(9) . ? O6' C37' 1.452(12) . ? O7' C35' 1.336(8) . ? O7' C25' 1.457(7) . ? O8' C35' 1.202(10) . ? O9' C23' 1.450(8) . ? O10' C21' 1.396(9) . ? O11' C15' 1.222(7) . ? C1' C2' 1.378(8) . ? C1' C9' 1.434(8) . ? C2' C3' 1.395(8) . ? C3' C4' 1.396(8) . ? C4' C10' 1.406(8) . ? C5' C11' 1.396(8) . ? C5' C6' 1.401(8) . ? C5' C10' 1.419(7) . ? C6' C7' 1.363(9) . ? C7' C8' 1.409(9) . ? C7' C14' 1.516(10) . ? C8' C9' 1.462(8) . ? C9' C10' 1.415(8) . ? C11' C12' 1.545(8) . ? C12' C13' 1.507(9) . ? C15' C16' 1.491(8) . ? C16' C17' 1.325(8) . ? C16' C30' 1.502(9) . ? C17' C18' 1.447(9) . ? C18' C19' 1.309(9) . ? C19' C20' 1.523(9) . ? C20' C31' 1.512(12) . ? C20' C21' 1.525(9) . ? C21' C22' 1.518(9) . ? C22' C32' 1.524(9) . ? C22' C23' 1.542(9) . ? C23' C24' 1.525(9) . ? C24' C25' 1.540(8) . ? C24' C33' 1.546(10) . ? C25' C26' 1.533(8) . ? C26' C34' 1.513(10) . ? C26' C27' 1.540(9) . ? C27' C28' 1.527(12) . ? C28' C29' 1.163(13) . ? C35' C36' 1.508(13) . ? C5A C4A 1.371(9) . ? C5A C6A 1.400(8) . ? C2A C3A 1.365(9) . ? C3A C4A 1.382(9) . ? C4A C7A 1.503(9) . ? 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 C15 N1 C2 119.5(4) . . ? C611 N2 C211 120.4(5) . . ? C611 N2 C3 109.6(4) . . ? C211 N2 C3 130.0(5) . . ? C611 N3 C4 109.5(4) . . ? C6 O3 C12 107.8(4) . . ? C29 O5 C12 120.9(5) . . ? C27 O6 C37 112.0(10) . . ? C35 O7 C25 119.1(5) . . ? O1 C1 C2 119.0(5) . . ? O1 C1 C9 119.6(5) . . ? C2 C1 C9 121.3(5) . . ? C1 C2 C3 116.4(5) . . ? C1 C2 N1 121.7(5) . . ? C3 C2 N1 121.8(5) . . ? C4 C3 C2 123.7(5) . . ? C4 C3 N2 105.5(5) . . ? C2 C3 N2 130.8(5) . . ? C3 C4 N3 108.1(5) . . ? C3 C4 C10 120.7(5) . . ? N3 C4 C10 131.1(5) . . ? C6 C5 C11 108.7(5) . . ? C6 C5 C10 118.2(5) . . ? C11 C5 C10 132.8(5) . . ? C7 C6 C5 126.0(5) . . ? C7 C6 O3 121.6(6) . . ? C5 C6 O3 112.4(5) . . ? C6 C7 C8 115.7(6) . . ? C6 C7 C14 123.8(6) . . ? C8 C7 C14 120.5(6) . . ? O2 C8 C7 119.5(6) . . ? O2 C8 C9 119.4(5) . . ? C7 C8 C9 121.1(6) . . ? C10 C9 C1 121.3(5) . . ? C10 C9 C8 120.0(5) . . ? C1 C9 C8 118.6(5) . . ? C9 C10 C5 118.5(5) . . ? C9 C10 C4 116.4(5) . . ? C5 C10 C4 124.9(5) . . ? O4 C11 C5 132.7(5) . . ? O4 C11 C12 120.9(5) . . ? C5 C11 C12 106.4(5) . . ? O5 C12 O3 111.0(5) . . ? O5 C12 C13 106.2(5) . . ? O3 C12 C13 107.8(6) . . ? O5 C12 C11 114.5(5) . . ? O3 C12 C11 104.6(5) . . ? C13 C12 C11 112.6(6) . . ? O11 C15 N1 120.2(5) . . ? O11 C15 C16 122.9(5) . . ? N1 C15 C16 116.8(5) . . ? C17 C16 C15 118.4(5) . . ? C17 C16 C30 124.9(5) . . ? C15 C16 C30 116.7(5) . . ? C16 C17 C18 127.0(5) . . ? C19 C18 C17 126.3(5) . . ? C18 C19 C20 126.6(6) . . ? C19 C20 C31 109.6(6) . . ? C19 C20 C21 111.3(5) . . ? C31 C20 C21 111.5(6) . . ? O10 C21 C22 108.2(5) . . ? O10 C21 C20 109.5(5) . . ? C22 C21 C20 117.0(5) . . ? C21 C22 C23 112.4(5) . . ? C21 C22 C32 112.1(5) . . ? C23 C22 C32 110.9(5) . . ? O9 C23 C22 109.9(5) . . ? O9 C23 C24 110.4(5) . . ? C22 C23 C24 115.2(5) . . ? C33 C24 C23 112.0(6) . . ? C33 C24 C25 112.7(5) . . ? C23 C24 C25 111.9(5) . . ? O7 C25 C26 108.6(5) . . ? O7 C25 C24 107.3(5) . . ? C26 C25 C24 113.4(5) . . ? C34 C26 C25 111.3(5) . . ? C34 C26 C27 111.3(6) . . ? C25 C26 C27 112.4(5) . . ? O6 C27 C28 110.0(6) . . ? O6 C27 C26 107.5(6) . . ? C28 C27 C26 111.6(5) . . ? C29 C28 C27 122.5(7) . . ? C28 C29 O5 129.3(7) . . ? O8 C35 O7 123.8(6) . . ? O8 C35 C36 124.0(6) . . ? O7 C35 C36 112.2(6) . . ? C311 C211 N2 119.0(5) . . ? C211 C311 C411 121.9(6) . . ? C511 C411 C311 118.0(5) . . ? C511 C411 C711 124.3(6) . . ? C311 C411 C711 117.7(6) . . ? C411 C511 C611 120.1(5) . . ? N3 C611 N2 107.2(5) . . ? N3 C611 C511 132.2(5) . . ? N2 C611 C511 120.5(5) . . ? C15' N1' C2' 125.6(5) . . ? C6A N2' C2A 120.3(5) . . ? C6A N2' C3' 109.4(4) . . ? C2A N2' C3' 130.4(5) . . ? C6A N3' C4' 108.8(4) . . ? C6' O3' C12' 108.2(4) . . ? C29' O5' C12' 119.2(5) . . ? C27' O6' C37' 112.3(8) . . ? C35' O7' C25' 118.8(5) . . ? O1' C1' C2' 117.7(5) . . ? O1' C1' C9' 118.9(5) . . ? C2' C1' C9' 123.3(5) . . ? C1' C2' C3' 115.7(5) . . ? C1' C2' N1' 117.7(5) . . ? C3' C2' N1' 126.0(5) . . ? C2' C3' C4' 122.4(5) . . ? C2' C3' N2' 132.5(5) . . ? C4' C3' N2' 105.0(4) . . ? N3' C4' C3' 108.4(5) . . ? N3' C4' C10' 129.0(5) . . ? C3' C4' C10' 122.6(5) . . ? C11' C5' C6' 107.9(5) . . ? C11' C5' C10' 133.2(5) . . ? C6' C5' C10' 118.3(5) . . ? C7' C6' O3' 121.5(5) . . ? C7' C6' C5' 125.9(5) . . ? O3' C6' C5' 112.5(5) . . ? C6' C7' C8' 116.6(5) . . ? C6' C7' C14' 123.3(6) . . ? C8' C7' C14' 120.0(6) . . ? O2' C8' C7' 120.8(6) . . ? O2' C8' C9' 118.6(5) . . ? C7' C8' C9' 120.5(5) . . ? C10' C9' C1' 120.1(5) . . ? C10' C9' C8' 119.7(5) . . ? C1' C9' C8' 120.2(5) . . ? C4' C10' C9' 115.6(5) . . ? C4' C10' C5' 125.7(5) . . ? C9' C10' C5' 118.6(5) . . ? O4' C11' C5' 131.9(5) . . ? O4' C11' C12' 120.6(5) . . ? C5' C11' C12' 107.5(5) . . ? O5' C12' O3' 110.1(5) . . ? O5' C12' C13' 106.4(5) . . ? O3' C12' C13' 109.0(5) . . ? O5' C12' C11' 112.5(5) . . ? O3' C12' C11' 103.8(4) . . ? C13' C12' C11' 115.0(5) . . ? O11' C15' N1' 121.9(5) . . ? O11' C15' C16' 122.7(5) . . ? N1' C15' C16' 115.4(5) . . ? C17' C16' C15' 124.0(5) . . ? C17' C16' C30' 122.8(5) . . ? C15' C16' C30' 113.2(5) . . ? C16' C17' C18' 126.6(6) . . ? C19' C18' C17' 125.9(6) . . ? C18' C19' C20' 123.4(6) . . ? C31' C20' C19' 111.1(7) . . ? C31' C20' C21' 114.5(6) . . ? C19' C20' C21' 109.2(5) . . ? O10' C21' C22' 110.2(6) . . ? O10' C21' C20' 107.8(6) . . ? C22' C21' C20' 117.1(5) . . ? C21' C22' C32' 112.7(6) . . ? C21' C22' C23' 114.1(5) . . ? C32' C22' C23' 110.7(6) . . ? O9' C23' C24' 109.0(5) . . ? O9' C23' C22' 111.4(5) . . ? C24' C23' C22' 116.4(5) . . ? C23' C24' C25' 109.6(5) . . ? C23' C24' C33' 112.5(6) . . ? C25' C24' C33' 111.4(5) . . ? O7' C25' C26' 107.9(5) . . ? O7' C25' C24' 107.1(5) . . ? C26' C25' C24' 114.4(5) . . ? C34' C26' C25' 110.9(5) . . ? C34' C26' C27' 111.3(6) . . ? C25' C26' C27' 110.9(5) . . ? O6' C27' C28' 106.3(7) . . ? O6' C27' C26' 107.4(6) . . ? C28' C27' C26' 111.9(6) . . ? C29' C28' C27' 130.7(12) . . ? C28' C29' O5' 139.3(12) . . ? O8' C35' O7' 123.7(7) . . ? O8' C35' C36' 125.7(8) . . ? O7' C35' C36' 110.6(8) . . ? C4A C5A C6A 118.7(6) . . ? N3' C6A N2' 108.3(5) . . ? N3' C6A C5A 130.8(6) . . ? N2' C6A C5A 120.9(5) . . ? C3A C2A N2' 118.3(6) . . ? C2A C3A C4A 122.2(6) . . ? C5A C4A C3A 119.7(6) . . ? C5A C4A C7A 120.5(6) . . ? C3A C4A C7A 119.8(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.737 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.060