# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_sc0897_shelxl _database_code_depnum_ccdc_archive 'CCDC 894956' #TrackingRef 'web_deposit_cif_file_0_shinichirokamino_1344261986.cis-ABPX010.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H37 N2 O6' _chemical_formula_weight 665.74 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8756(5) _cell_length_b 16.1912(7) _cell_length_c 20.1235(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.485(7) _cell_angle_gamma 90.00 _cell_volume 3532.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9355 _exptl_absorpt_correction_T_max 0.9355 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23504 _diffrn_reflns_av_R_equivalents 0.1035 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 45.00 _reflns_number_total 2843 _reflns_number_gt 1961 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.2450P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2843 _refine_ls_number_parameters 460 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.3082 _refine_ls_wR_factor_gt 0.2629 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2866(5) 0.5344(3) 0.5351(2) 0.0701(15) Uani 1 1 d . . . O2 O 0.2941(4) 0.7711(4) 0.5253(2) 0.0744(16) Uani 1 1 d . . . O3 O 0.3047(6) 0.9083(4) 0.5182(3) 0.098(2) Uani 1 1 d . . . O11 O -0.0461(5) 0.5138(3) 0.3737(3) 0.0705(15) Uani 1 1 d . . . O12 O -0.0814(5) 0.7624(3) 0.3651(2) 0.0748(16) Uani 1 1 d . . . O13 O -0.1131(5) 0.8979(4) 0.3716(3) 0.0925(18) Uani 1 1 d . . . N1 N 0.6402(6) 0.5243(4) 0.6868(3) 0.0720(18) Uani 1 1 d . . . N11 N -0.2969(7) 0.4823(6) 0.1725(4) 0.111(3) Uani 1 1 d D . . C1 C 0.3332(7) 0.6556(6) 0.6023(4) 0.061(2) Uani 1 1 d . . . C2 C 0.4130(8) 0.6891(5) 0.6523(4) 0.068(2) Uani 1 1 d . . . H2 H 0.3975 0.7434 0.6674 0.082 Uiso 1 1 calc R . . C3 C 0.5124(8) 0.6479(6) 0.6807(4) 0.071(2) Uani 1 1 d . . . H3 H 0.5652 0.6739 0.7143 0.086 Uiso 1 1 calc R . . C4 C 0.5379(7) 0.5655(6) 0.6604(4) 0.065(2) Uani 1 1 d . . . C5 C 0.4565(8) 0.5302(5) 0.6116(4) 0.062(2) Uani 1 1 d . . . H5 H 0.4684 0.4750 0.5976 0.074 Uiso 1 1 calc R . . C6 C 0.3596(7) 0.5753(6) 0.5842(3) 0.061(2) Uani 1 1 d . . . C7 C 0.1838(8) 0.5719(6) 0.5036(4) 0.062(2) Uani 1 1 d . . . C8 C 0.1173(8) 0.5291(5) 0.4562(4) 0.063(2) Uani 1 1 d . . . H8 H 0.1407 0.4741 0.4468 0.075 Uiso 1 1 calc R . . C9 C 0.0500(8) 0.6880(5) 0.4825(4) 0.066(2) Uani 1 1 d . . . H9 H 0.0270 0.7430 0.4922 0.079 Uiso 1 1 calc R . . C10 C 0.1525(7) 0.6543(6) 0.5181(3) 0.058(2) Uani 1 1 d . . . C11 C 0.2319(7) 0.7058(5) 0.5659(3) 0.068(2) Uani 1 1 d . . . C12 C 0.1615(7) 0.7607(6) 0.6106(3) 0.063(2) Uani 1 1 d . . . C13 C 0.0856(7) 0.7367(5) 0.6597(4) 0.076(2) Uani 1 1 d . . . H13 H 0.0727 0.6801 0.6694 0.091 Uiso 1 1 calc R . . C14 C 0.0296(8) 0.7988(7) 0.6938(4) 0.086(3) Uani 1 1 d . . . H14 H -0.0218 0.7841 0.7280 0.103 Uiso 1 1 calc R . . C15 C 0.0456(9) 0.8806(7) 0.6799(5) 0.094(3) Uani 1 1 d . . . H15 H 0.0049 0.9217 0.7038 0.113 Uiso 1 1 calc R . . C16 C 0.1207(9) 0.9031(5) 0.6314(5) 0.086(2) Uani 1 1 d . . . H16 H 0.1320 0.9597 0.6210 0.103 Uiso 1 1 calc R . . C17 C 0.1802(7) 0.8417(6) 0.5976(4) 0.067(2) Uani 1 1 d . . . C18 C 0.2637(8) 0.8474(7) 0.5437(4) 0.075(2) Uani 1 1 d . . . C19 C 0.7286(7) 0.5612(5) 0.7360(4) 0.078(2) Uani 1 1 d . . . H19A H 0.7727 0.5168 0.7619 0.093 Uiso 1 1 calc R . . H19B H 0.6838 0.5949 0.7674 0.093 Uiso 1 1 calc R . . C20 C 0.8222(7) 0.6155(5) 0.7042(4) 0.091(3) Uani 1 1 d . . . H20A H 0.7790 0.6598 0.6788 0.109 Uiso 1 1 calc R . . H20B H 0.8687 0.5820 0.6742 0.109 Uiso 1 1 calc R . . H20C H 0.8791 0.6396 0.7391 0.109 Uiso 1 1 calc R . . C21 C 0.6734(7) 0.4427(5) 0.6614(4) 0.077(2) Uani 1 1 d . . . H21A H 0.7642 0.4366 0.6672 0.092 Uiso 1 1 calc R . . H21B H 0.6489 0.4405 0.6130 0.092 Uiso 1 1 calc R . . C22 C 0.6154(8) 0.3702(5) 0.6947(4) 0.098(3) Uani 1 1 d . . . H22A H 0.6389 0.3716 0.7427 0.118 Uiso 1 1 calc R . . H22B H 0.6444 0.3185 0.6759 0.118 Uiso 1 1 calc R . . H22C H 0.5255 0.3735 0.6870 0.118 Uiso 1 1 calc R . . C31 C -0.1746(7) 0.6308(5) 0.3380(3) 0.057(2) Uani 1 1 d . . . C32 C -0.2638(7) 0.6576(5) 0.2885(4) 0.068(2) Uani 1 1 d . A . H32 H -0.2982 0.7111 0.2925 0.081 Uiso 1 1 calc R . . C33 C -0.3035(7) 0.6104(6) 0.2351(4) 0.069(2) Uani 1 1 d . . . H33 H -0.3611 0.6334 0.2023 0.082 Uiso 1 1 calc R A . C34 C -0.2629(8) 0.5296(6) 0.2267(4) 0.074(2) Uani 1 1 d . A . C35 C -0.1761(7) 0.5006(4) 0.2771(4) 0.068(2) Uani 1 1 d . . . H35 H -0.1459 0.4457 0.2749 0.082 Uiso 1 1 calc R A . C36 C -0.1350(7) 0.5502(6) 0.3289(4) 0.058(2) Uani 1 1 d . A . C37 C 0.0150(8) 0.5633(6) 0.4207(4) 0.061(2) Uani 1 1 d . . . C40 C -0.0205(7) 0.6451(6) 0.4333(3) 0.059(2) Uani 1 1 d . . . C41 C -0.1282(7) 0.6826(5) 0.3943(3) 0.063(2) Uani 1 1 d . . . C42 C -0.2276(7) 0.7165(5) 0.4359(3) 0.062(2) Uani 1 1 d . . . C43 C -0.3068(7) 0.6738(6) 0.4734(4) 0.075(2) Uani 1 1 d . . . H43 H -0.3029 0.6154 0.4773 0.090 Uiso 1 1 calc R . . C44 C -0.3931(7) 0.7199(7) 0.5056(4) 0.085(3) Uani 1 1 d . . . H44 H -0.4507 0.6923 0.5310 0.102 Uiso 1 1 calc R . . C45 C -0.3958(8) 0.8053(7) 0.5009(4) 0.096(3) Uani 1 1 d . . . H45 H -0.4562 0.8350 0.5227 0.115 Uiso 1 1 calc R . . C46 C -0.3140(5) 0.8479(3) 0.4657(2) 0.090(3) Uani 1 1 d . . . H46 H -0.3145 0.9065 0.4636 0.108 Uiso 1 1 calc R . . C47 C -0.2304(5) 0.8015(3) 0.4333(2) 0.070(2) Uani 1 1 d R . . C48 C -0.1362(5) 0.8289(3) 0.3886(2) 0.079(3) Uani 1 1 d R . . C49 C -0.3918(5) 0.5097(3) 0.1224(2) 0.092(3) Uani 1 1 d R A . H49A H -0.3847 0.4778 0.0809 0.110 Uiso 1 1 calc R . . H49B H -0.3781 0.5687 0.1123 0.110 Uiso 1 1 calc R . . C50 C -0.5187(8) 0.4992(6) 0.1446(4) 0.114(3) Uani 1 1 d . . . H50A H -0.5258 0.5299 0.1861 0.137 Uiso 1 1 calc R A . H50B H -0.5345 0.4405 0.1521 0.137 Uiso 1 1 calc R . . H50C H -0.5792 0.5204 0.1101 0.137 Uiso 1 1 calc R . . C51A C -0.2863(18) 0.3888(10) 0.1804(10) 0.068(6) Uani 0.50 1 d PD A 1 H51A H -0.3584 0.3613 0.1568 0.082 Uiso 0.50 1 calc PR A 1 H51B H -0.2834 0.3736 0.2282 0.082 Uiso 0.50 1 calc PR A 1 C52A C -0.167(2) 0.361(2) 0.1505(14) 0.134(12) Uani 0.50 1 d PD A 1 H52A H -0.1642 0.3849 0.1058 0.161 Uiso 0.50 1 calc PR A 1 H52B H -0.1653 0.3008 0.1477 0.161 Uiso 0.50 1 calc PR A 1 H52C H -0.0956 0.3804 0.1791 0.161 Uiso 0.50 1 calc PR A 1 C51B C -0.205(2) 0.4235(11) 0.1483(9) 0.100(8) Uani 0.50 1 d PD A 2 H51X H -0.1982 0.4290 0.0997 0.120 Uiso 0.50 1 calc PR A 2 H51Y H -0.1224 0.4311 0.1720 0.120 Uiso 0.50 1 calc PR A 2 C52B C -0.262(3) 0.3417(12) 0.1657(12) 0.083(7) Uani 0.50 1 d PD A 2 H52X H -0.3470 0.3391 0.1456 0.100 Uiso 0.50 1 calc PR A 2 H52Y H -0.2623 0.3369 0.2143 0.100 Uiso 0.50 1 calc PR A 2 H52Z H -0.2140 0.2963 0.1486 0.100 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.069(4) 0.093(4) 0.047(3) -0.001(3) 0.000(3) 0.012(3) O2 0.087(4) 0.091(4) 0.047(3) 0.002(3) 0.020(3) -0.003(3) O3 0.138(5) 0.097(5) 0.061(4) 0.013(3) 0.021(3) -0.009(4) O11 0.088(4) 0.079(4) 0.043(3) -0.013(3) 0.001(3) 0.001(3) O12 0.103(4) 0.074(4) 0.048(3) 0.008(3) 0.009(3) -0.003(3) O13 0.123(5) 0.079(4) 0.074(4) 0.005(3) 0.003(3) 0.010(4) N1 0.076(5) 0.090(6) 0.049(4) 0.001(4) -0.001(4) -0.002(4) N11 0.132(7) 0.137(8) 0.058(5) -0.041(5) -0.026(5) 0.053(6) C1 0.048(5) 0.090(7) 0.045(5) -0.010(5) 0.008(4) 0.002(5) C2 0.063(6) 0.084(6) 0.059(5) 0.004(5) 0.015(5) -0.001(5) C3 0.075(6) 0.092(7) 0.046(5) -0.009(5) -0.003(4) 0.009(5) C4 0.051(6) 0.103(8) 0.040(5) 0.006(5) -0.002(5) 0.001(5) C5 0.054(5) 0.089(6) 0.041(5) 0.010(5) 0.005(4) 0.013(5) C6 0.059(6) 0.099(8) 0.026(4) -0.012(5) 0.006(4) -0.009(6) C7 0.076(6) 0.085(7) 0.029(5) -0.015(5) 0.012(5) -0.012(6) C8 0.082(6) 0.075(6) 0.032(5) -0.004(5) 0.014(5) 0.002(5) C9 0.076(6) 0.080(6) 0.043(5) -0.006(5) 0.016(5) -0.009(5) C10 0.061(6) 0.088(7) 0.026(4) -0.014(5) 0.001(4) -0.014(5) C11 0.087(6) 0.084(6) 0.035(4) -0.001(5) 0.021(5) 0.006(5) C12 0.072(5) 0.084(7) 0.033(5) 0.001(5) 0.008(4) -0.002(5) C13 0.097(6) 0.076(6) 0.057(5) 0.004(5) 0.023(5) -0.001(5) C14 0.092(6) 0.099(8) 0.067(6) -0.013(6) 0.013(5) 0.003(6) C15 0.109(7) 0.101(9) 0.075(7) -0.022(6) 0.024(6) 0.014(6) C16 0.110(7) 0.077(7) 0.072(6) -0.012(5) 0.017(6) 0.000(6) C17 0.089(6) 0.076(7) 0.038(5) -0.002(5) 0.012(5) -0.004(5) C18 0.110(7) 0.063(7) 0.052(6) 0.007(5) 0.007(5) 0.005(6) C19 0.075(6) 0.107(6) 0.053(5) 0.011(5) 0.010(5) 0.006(5) C20 0.092(6) 0.130(7) 0.054(5) -0.011(5) 0.020(5) -0.006(5) C21 0.082(6) 0.093(7) 0.056(5) 0.009(5) 0.005(4) 0.009(5) C22 0.104(7) 0.092(7) 0.101(7) 0.006(5) 0.025(6) 0.004(5) C31 0.064(5) 0.078(6) 0.028(5) -0.013(4) 0.004(4) -0.009(4) C32 0.070(6) 0.084(6) 0.049(5) 0.002(5) 0.005(5) -0.010(4) C33 0.074(5) 0.085(7) 0.047(6) 0.010(5) 0.012(4) -0.002(5) C34 0.086(6) 0.095(8) 0.041(6) -0.015(6) 0.000(5) 0.001(5) C35 0.092(6) 0.070(6) 0.043(5) -0.018(5) 0.012(5) 0.001(5) C36 0.064(5) 0.083(7) 0.029(5) -0.006(5) 0.012(4) -0.004(5) C37 0.075(6) 0.076(7) 0.035(5) 0.003(5) 0.012(5) -0.002(5) C40 0.073(6) 0.073(7) 0.032(5) 0.003(4) 0.012(5) 0.001(5) C41 0.070(5) 0.079(6) 0.039(5) 0.004(5) 0.009(5) 0.003(5) C42 0.064(5) 0.080(6) 0.043(5) -0.007(4) 0.001(4) 0.003(5) C43 0.070(5) 0.105(7) 0.050(5) -0.004(5) 0.012(5) 0.000(5) C44 0.071(6) 0.117(9) 0.070(6) -0.020(6) 0.019(5) 0.003(5) C45 0.102(7) 0.100(8) 0.088(7) -0.016(6) 0.015(5) 0.020(6) C46 0.107(7) 0.079(7) 0.084(7) -0.012(5) 0.002(6) 0.020(6) C47 0.074(6) 0.089(8) 0.046(5) -0.003(5) -0.013(4) 0.004(6) C48 0.114(8) 0.057(7) 0.061(6) 0.002(5) -0.014(5) 0.011(6) C49 0.107(8) 0.127(8) 0.042(5) -0.010(5) 0.003(5) 0.004(5) C50 0.094(7) 0.146(8) 0.103(7) -0.034(6) 0.015(6) -0.003(6) C51A 0.094(14) 0.052(18) 0.057(12) -0.034(13) -0.003(10) 0.008(14) C52A 0.11(2) 0.19(3) 0.108(19) -0.09(2) 0.049(17) -0.01(2) C51B 0.120(18) 0.16(2) 0.031(10) -0.046(14) 0.046(11) -0.011(19) C52B 0.13(2) 0.043(17) 0.075(16) -0.008(12) -0.015(15) -0.011(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C7 1.382(9) . ? O1 C6 1.385(8) . ? O2 C18 1.340(9) . ? O2 C11 1.525(8) . ? O3 C18 1.212(9) . ? O11 C37 1.371(8) . ? O11 C36 1.398(8) . ? O12 C48 1.334(6) . ? O12 C41 1.523(8) . ? O13 C48 1.201(7) . ? N1 C4 1.368(9) . ? N1 C19 1.454(9) . ? N1 C21 1.472(9) . ? N11 C34 1.361(10) . ? N11 C49 1.455(8) . ? N11 C51B 1.490(16) . ? N11 C51A 1.525(16) . ? C1 C2 1.387(9) . ? C1 C6 1.387(10) . ? C1 C11 1.511(10) . ? C2 C3 1.358(10) . ? C3 C4 1.429(10) . ? C4 C5 1.392(10) . ? C5 C6 1.362(10) . ? C7 C8 1.344(9) . ? C7 C10 1.414(10) . ? C8 C37 1.389(9) . ? C9 C40 1.389(9) . ? C9 C10 1.389(9) . ? C10 C11 1.495(9) . ? C11 C12 1.514(10) . ? C12 C17 1.357(9) . ? C12 C13 1.392(10) . ? C13 C14 1.385(10) . ? C14 C15 1.367(11) . ? C15 C16 1.371(11) . ? C16 C17 1.392(10) . ? C17 C18 1.470(12) . ? C19 C20 1.523(10) . ? C21 C22 1.513(10) . ? C31 C36 1.392(9) . ? C31 C32 1.403(9) . ? C31 C41 1.467(9) . ? C32 C33 1.361(9) . ? C33 C34 1.395(10) . ? C34 C35 1.410(10) . ? C35 C36 1.364(9) . ? C37 C40 1.409(9) . ? C40 C41 1.488(9) . ? C41 C42 1.520(10) . ? C42 C43 1.375(10) . ? C42 C47 1.377(9) . ? C43 C44 1.397(10) . ? C44 C45 1.386(11) . ? C45 C46 1.367(11) . ? C46 C47 1.3806 . ? C47 C48 1.4837 . ? C49 C50 1.493(10) . ? C51A C52A 1.538(17) . ? C51B C52B 1.517(18) . ? 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 C7 O1 C6 121.0(7) . . ? C18 O2 C11 111.3(6) . . ? C37 O11 C36 118.2(6) . . ? C48 O12 C41 112.0(5) . . ? C4 N1 C19 122.6(7) . . ? C4 N1 C21 121.2(6) . . ? C19 N1 C21 116.0(6) . . ? C34 N11 C49 121.2(8) . . ? C34 N11 C51B 118.3(10) . . ? C49 N11 C51B 115.2(10) . . ? C34 N11 C51A 117.5(11) . . ? C49 N11 C51A 114.8(9) . . ? C51B N11 C51A 49.7(10) . . ? C2 C1 C6 115.2(7) . . ? C2 C1 C11 122.2(8) . . ? C6 C1 C11 122.3(7) . . ? C3 C2 C1 123.1(8) . . ? C2 C3 C4 120.3(7) . . ? N1 C4 C5 121.8(8) . . ? N1 C4 C3 120.9(7) . . ? C5 C4 C3 117.2(7) . . ? C6 C5 C4 119.8(8) . . ? C5 C6 O1 114.5(8) . . ? C5 C6 C1 124.4(7) . . ? O1 C6 C1 121.1(8) . . ? C8 C7 O1 118.1(8) . . ? C8 C7 C10 120.5(8) . . ? O1 C7 C10 121.3(7) . . ? C7 C8 C37 121.7(8) . . ? C40 C9 C10 123.2(7) . . ? C9 C10 C7 117.4(7) . . ? C9 C10 C11 120.9(8) . . ? C7 C10 C11 121.5(8) . . ? C1 C11 C10 112.0(7) . . ? C1 C11 C12 114.2(6) . . ? C10 C11 C12 114.6(7) . . ? C1 C11 O2 107.2(6) . . ? C10 C11 O2 107.5(5) . . ? C12 C11 O2 100.2(6) . . ? C17 C12 C13 120.9(8) . . ? C17 C12 C11 111.3(7) . . ? C13 C12 C11 127.9(9) . . ? C12 C13 C14 117.3(8) . . ? C15 C14 C13 122.3(8) . . ? C16 C15 C14 119.7(8) . . ? C15 C16 C17 119.0(8) . . ? C12 C17 C16 120.9(8) . . ? C12 C17 C18 108.3(8) . . ? C16 C17 C18 130.8(10) . . ? O3 C18 O2 121.8(8) . . ? O3 C18 C17 129.2(9) . . ? O2 C18 C17 109.0(8) . . ? N1 C19 C20 112.2(6) . . ? N1 C21 C22 114.9(6) . . ? C36 C31 C32 113.6(7) . . ? C36 C31 C41 123.1(7) . . ? C32 C31 C41 123.2(8) . . ? C33 C32 C31 123.1(8) . . ? C32 C33 C34 122.6(7) . . ? N11 C34 C33 123.8(9) . . ? N11 C34 C35 120.9(9) . . ? C33 C34 C35 115.2(7) . . ? C36 C35 C34 120.9(8) . . ? C35 C36 C31 124.5(7) . . ? C35 C36 O11 114.4(8) . . ? C31 C36 O11 121.0(7) . . ? O11 C37 C8 116.6(8) . . ? O11 C37 C40 123.3(8) . . ? C8 C37 C40 120.1(7) . . ? C9 C40 C37 117.0(7) . . ? C9 C40 C41 122.7(8) . . ? C37 C40 C41 120.3(8) . . ? C31 C41 C40 112.5(7) . . ? C31 C41 C42 114.5(6) . . ? C40 C41 C42 114.9(6) . . ? C31 C41 O12 106.9(5) . . ? C40 C41 O12 106.1(6) . . ? C42 C41 O12 100.4(6) . . ? C43 C42 C47 120.7(7) . . ? C43 C42 C41 128.5(8) . . ? C47 C42 C41 110.8(7) . . ? C42 C43 C44 117.2(8) . . ? C43 C44 C45 120.9(8) . . ? C46 C45 C44 121.8(8) . . ? C45 C46 C47 116.7(5) . . ? C46 C47 C42 122.6(4) . . ? C46 C47 C48 129.5 . . ? C42 C47 C48 107.9(4) . . ? O13 C48 O12 122.7(5) . . ? O13 C48 C47 128.3(4) . . ? O12 C48 C47 108.8(3) . . ? N11 C49 C50 112.4(6) . . ? N11 C51A C52A 107.8(18) . . ? C52B C51B N11 100.5(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 45.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.207 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.056