data_kw806 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 N O3 P, H2 O' _chemical_formula_sum 'C24 H26 N O4 P' _chemical_formula_weight 423.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.996(4) _cell_length_b 10.762(2) _cell_length_c 23.331(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.583(2) _cell_angle_gamma 90.00 _cell_volume 4371.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6630 _cell_measurement_theta_min 3.78 _cell_measurement_theta_max 27.37 _exptl_crystal_description cut-plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9105 _exptl_absorpt_correction_T_max 0.9846 _exptl_absorpt_process_details 'sadabs (Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'omega and phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42433 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 30.74 _reflns_number_total 12666 _reflns_number_gt 8859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0402P)^2^+2.0918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12666 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.71832(2) 0.25644(4) 0.855580(19) 0.01484(9) Uani 1 1 d . . . O1 O 0.73467(6) 0.47523(11) 0.90865(5) 0.0182(2) Uani 1 1 d . . . O2 O 0.89474(6) 0.42310(11) 0.80201(5) 0.0187(2) Uani 1 1 d . . . O3 O 0.92528(6) 0.57720(11) 0.87295(5) 0.0201(2) Uani 1 1 d . . . N1 N 0.92070(9) 0.78802(14) 1.03796(7) 0.0235(3) Uani 1 1 d . . . C1 C 0.90983(10) 0.57896(16) 0.99834(8) 0.0197(3) Uani 1 1 d . . . H1 H 0.9310 0.4977 1.0032 0.024 Uiso 1 1 calc R . . C2 C 0.94636(10) 0.67112(17) 1.04140(8) 0.0230(4) Uani 1 1 d . . . H2 H 0.9927 0.6501 1.0757 0.028 Uiso 1 1 calc R . . C3 C 0.85486(10) 0.81352(16) 0.98914(8) 0.0225(4) Uani 1 1 d . . . H3 H 0.8351 0.8956 0.9854 0.027 Uiso 1 1 calc R . . C4 C 0.81356(10) 0.72755(15) 0.94356(8) 0.0184(3) Uani 1 1 d . . . H4 H 0.7670 0.7507 0.9101 0.022 Uiso 1 1 calc R . . C5 C 0.84175(9) 0.60714(15) 0.94789(7) 0.0147(3) Uani 1 1 d . . . C6 C 0.79513(9) 0.50964(14) 0.90237(7) 0.0144(3) Uani 1 1 d . . . C7 C 0.81499(9) 0.45607(14) 0.85647(7) 0.0134(3) Uani 1 1 d . . . C8 C 0.87942(9) 0.48113(14) 0.84119(7) 0.0140(3) Uani 1 1 d . . . C9 C 0.98857(10) 0.60475(17) 0.85600(9) 0.0237(4) Uani 1 1 d . . . H9A H 1.0227 0.5324 0.8648 0.036 Uiso 1 1 calc R . . H9B H 1.0172 0.6761 0.8803 0.036 Uiso 1 1 calc R . . H9C H 0.9690 0.6245 0.8113 0.036 Uiso 1 1 calc R . . C10 C 0.75966(9) 0.36054(14) 0.81465(7) 0.0134(3) Uani 1 1 d . . . H10 H 0.7905 0.3065 0.7985 0.016 Uiso 1 1 calc R . . C11 C 0.69432(9) 0.41373(15) 0.75706(7) 0.0146(3) Uani 1 1 d . . . C12 C 0.66145(9) 0.52867(15) 0.75978(8) 0.0177(3) Uani 1 1 d . . . H12 H 0.6790 0.5736 0.7980 0.021 Uiso 1 1 calc R . . C13 C 0.60334(10) 0.57732(16) 0.70686(8) 0.0208(3) Uani 1 1 d . . . H13 H 0.5821 0.6563 0.7089 0.025 Uiso 1 1 calc R . . C14 C 0.57580(10) 0.51163(17) 0.65077(8) 0.0212(3) Uani 1 1 d . . . H14 H 0.5354 0.5447 0.6149 0.025 Uiso 1 1 calc R . . C15 C 0.60802(10) 0.39720(16) 0.64782(8) 0.0206(3) Uani 1 1 d . . . H15 H 0.5896 0.3516 0.6098 0.025 Uiso 1 1 calc R . . C16 C 0.66737(9) 0.34916(15) 0.70058(7) 0.0176(3) Uani 1 1 d . . . H16 H 0.6897 0.2715 0.6980 0.021 Uiso 1 1 calc R . . C17 C 0.78418(9) 0.21889(14) 0.93353(7) 0.0159(3) Uani 1 1 d . . . C18 C 0.75801(11) 0.19692(16) 0.98046(8) 0.0224(4) Uani 1 1 d . . . H18 H 0.7053 0.2090 0.9723 0.027 Uiso 1 1 calc R . . C19 C 0.80879(11) 0.15731(17) 1.03931(8) 0.0255(4) Uani 1 1 d . . . H19 H 0.7909 0.1423 1.0713 0.031 Uiso 1 1 calc R . . C20 C 0.88546(11) 0.13989(16) 1.05086(8) 0.0245(4) Uani 1 1 d . . . H20 H 0.9202 0.1127 1.0910 0.029 Uiso 1 1 calc R . . C21 C 0.91201(10) 0.16167(17) 1.00453(8) 0.0241(4) Uani 1 1 d . . . H21 H 0.9648 0.1498 1.0130 0.029 Uiso 1 1 calc R . . C22 C 0.86149(10) 0.20096(16) 0.94556(8) 0.0193(3) Uani 1 1 d . . . H22 H 0.8796 0.2155 0.9136 0.023 Uiso 1 1 calc R . . C23 C 0.62323(9) 0.28913(17) 0.84979(8) 0.0223(4) Uani 1 1 d . . . H23A H 0.5999 0.2127 0.8569 0.033 Uiso 1 1 calc R . . H23B H 0.5921 0.3214 0.8080 0.033 Uiso 1 1 calc R . . H23C H 0.6257 0.3512 0.8813 0.033 Uiso 1 1 calc R . . C24 C 0.70733(11) 0.11107(16) 0.81479(8) 0.0233(4) Uani 1 1 d . . . H24A H 0.7575 0.0833 0.8170 0.035 Uiso 1 1 calc R . . H24B H 0.6722 0.1221 0.7709 0.035 Uiso 1 1 calc R . . H24C H 0.6864 0.0487 0.8343 0.035 Uiso 1 1 calc R . . P2 P 0.10261(2) 0.19692(4) 0.774181(19) 0.01410(9) Uani 1 1 d . . . O4 O 0.08110(6) 0.38183(11) 0.69749(5) 0.0202(2) Uani 1 1 d . . . O5 O 0.33006(6) 0.22750(11) 0.76657(5) 0.0196(2) Uani 1 1 d . . . O6 O 0.28844(7) 0.33575(11) 0.67624(5) 0.0201(2) Uani 1 1 d . . . N2 N 0.08979(8) 0.46369(15) 0.49427(7) 0.0236(3) Uani 1 1 d . . . C25 C 0.11211(10) 0.30922(16) 0.57417(8) 0.0213(3) Uani 1 1 d . . . H25 H 0.1137 0.2237 0.5847 0.026 Uiso 1 1 calc R . . C26 C 0.09237(10) 0.34568(18) 0.51285(8) 0.0235(4) Uani 1 1 d . . . H26 H 0.0798 0.2826 0.4819 0.028 Uiso 1 1 calc R . . C27 C 0.10635(10) 0.55016(17) 0.53890(8) 0.0232(4) Uani 1 1 d . . . H27 H 0.1048 0.6349 0.5270 0.028 Uiso 1 1 calc R . . C28 C 0.12573(10) 0.52359(16) 0.60173(8) 0.0205(3) Uani 1 1 d . . . H28 H 0.1362 0.5887 0.6315 0.025 Uiso 1 1 calc R . . C29 C 0.12959(9) 0.40043(15) 0.62021(7) 0.0167(3) Uani 1 1 d . . . C30 C 0.14024(9) 0.36393(14) 0.68553(7) 0.0154(3) Uani 1 1 d . . . C31 C 0.20456(9) 0.30505(15) 0.72833(7) 0.0146(3) Uani 1 1 d . . . C32 C 0.27498(9) 0.29318(15) 0.71959(7) 0.0154(3) Uani 1 1 d . . . C33 C 0.40415(10) 0.21996(18) 0.76299(9) 0.0254(4) Uani 1 1 d . . . H33A H 0.3977 0.1877 0.7219 0.038 Uiso 1 1 calc R . . H33B H 0.4377 0.1641 0.7957 0.038 Uiso 1 1 calc R . . H33C H 0.4273 0.3029 0.7689 0.038 Uiso 1 1 calc R . . C34 C 0.19956(9) 0.25451(15) 0.78729(7) 0.0144(3) Uani 1 1 d . . . H34 H 0.2346 0.1810 0.8003 0.017 Uiso 1 1 calc R . . C35 C 0.22443(9) 0.34155(15) 0.84366(7) 0.0164(3) Uani 1 1 d . . . C36 C 0.21500(9) 0.46950(15) 0.83624(8) 0.0187(3) Uani 1 1 d . . . H36 H 0.1959 0.5046 0.7955 0.022 Uiso 1 1 calc R . . C37 C 0.23346(10) 0.54655(17) 0.88823(8) 0.0229(4) Uani 1 1 d . . . H37 H 0.2268 0.6339 0.8828 0.028 Uiso 1 1 calc R . . C38 C 0.26163(11) 0.49602(18) 0.94813(8) 0.0256(4) Uani 1 1 d . . . H38 H 0.2736 0.5485 0.9835 0.031 Uiso 1 1 calc R . . C39 C 0.27202(10) 0.36919(17) 0.95575(8) 0.0238(4) Uani 1 1 d . . . H39 H 0.2916 0.3345 0.9966 0.029 Uiso 1 1 calc R . . C40 C 0.25406(9) 0.29202(17) 0.90417(7) 0.0196(3) Uani 1 1 d . . . H40 H 0.2619 0.2050 0.9100 0.024 Uiso 1 1 calc R . . C41 C 0.06068(9) 0.11800(15) 0.70002(7) 0.0157(3) Uani 1 1 d . . . C42 C -0.01743(10) 0.12671(16) 0.66182(8) 0.0215(3) Uani 1 1 d . . . H42 H -0.0502 0.1766 0.6742 0.026 Uiso 1 1 calc R . . C43 C -0.04695(10) 0.06206(17) 0.60568(8) 0.0255(4) Uani 1 1 d . . . H43 H -0.1002 0.0672 0.5798 0.031 Uiso 1 1 calc R . . C44 C 0.00076(11) -0.00996(17) 0.58707(8) 0.0255(4) Uani 1 1 d . . . H44 H -0.0197 -0.0523 0.5481 0.031 Uiso 1 1 calc R . . C45 C 0.07825(10) -0.02034(16) 0.62522(8) 0.0231(4) Uani 1 1 d . . . H45 H 0.1107 -0.0707 0.6127 0.028 Uiso 1 1 calc R . . C46 C 0.10835(10) 0.04318(15) 0.68186(8) 0.0193(3) Uani 1 1 d . . . H46 H 0.1613 0.0357 0.7082 0.023 Uiso 1 1 calc R . . C47 C 0.04177(9) 0.30498(15) 0.79134(8) 0.0174(3) Uani 1 1 d . . . H47A H -0.0080 0.3099 0.7556 0.026 Uiso 1 1 calc R . . H47B H 0.0660 0.3872 0.7994 0.026 Uiso 1 1 calc R . . H47C H 0.0341 0.2769 0.8284 0.026 Uiso 1 1 calc R . . C48 C 0.11703(10) 0.07506(15) 0.83078(8) 0.0190(3) Uani 1 1 d . . . H48A H 0.1382 0.1106 0.8730 0.029 Uiso 1 1 calc R . . H48B H 0.1529 0.0135 0.8270 0.029 Uiso 1 1 calc R . . H48C H 0.0678 0.0349 0.8231 0.029 Uiso 1 1 calc R . . O7 O 0.85303(7) 0.31798(11) 0.67831(6) 0.0250(3) Uani 1 1 d . . . H7A H 0.8757 0.3718 0.6617 0.050(7) Uiso 1 1 d R . . H7B H 0.8538 0.3526 0.7107 0.063(9) Uiso 1 1 d R . . O8 O 0.93635(7) 0.48309(12) 0.63337(6) 0.0261(3) Uani 1 1 d . . . H8A H 0.9221 0.4944 0.5926 0.058(8) Uiso 1 1 d R . . H8B H 0.9855 0.4551 0.6503 0.059(8) Uiso 1 1 d 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 P1 0.0141(2) 0.01534(19) 0.01485(19) -0.00024(16) 0.00560(16) -0.00164(15) O1 0.0174(6) 0.0213(6) 0.0177(6) -0.0024(5) 0.0089(5) -0.0027(5) O2 0.0172(6) 0.0229(6) 0.0172(6) -0.0037(5) 0.0080(5) -0.0001(5) O3 0.0185(6) 0.0198(6) 0.0253(6) -0.0070(5) 0.0122(5) -0.0068(5) N1 0.0246(8) 0.0275(8) 0.0185(7) -0.0066(6) 0.0087(6) -0.0069(6) C1 0.0194(8) 0.0204(8) 0.0188(8) -0.0004(7) 0.0072(7) 0.0020(6) C2 0.0204(9) 0.0292(10) 0.0161(8) -0.0035(7) 0.0037(7) -0.0019(7) C3 0.0275(9) 0.0181(8) 0.0242(9) -0.0043(7) 0.0129(8) -0.0018(7) C4 0.0192(8) 0.0185(8) 0.0166(7) 0.0003(6) 0.0062(7) 0.0004(6) C5 0.0156(8) 0.0177(8) 0.0127(7) -0.0017(6) 0.0076(6) -0.0024(6) C6 0.0148(7) 0.0135(7) 0.0133(7) 0.0018(6) 0.0039(6) 0.0011(5) C7 0.0138(7) 0.0134(7) 0.0113(7) 0.0002(6) 0.0033(6) -0.0004(5) C8 0.0138(7) 0.0128(7) 0.0126(7) 0.0017(6) 0.0025(6) 0.0012(5) C9 0.0193(8) 0.0249(9) 0.0304(9) -0.0035(8) 0.0134(8) -0.0060(7) C10 0.0140(7) 0.0136(7) 0.0128(7) -0.0016(6) 0.0055(6) 0.0002(5) C11 0.0130(7) 0.0166(8) 0.0139(7) 0.0010(6) 0.0052(6) -0.0012(6) C12 0.0168(8) 0.0195(8) 0.0168(7) -0.0019(6) 0.0068(7) 0.0000(6) C13 0.0177(8) 0.0209(8) 0.0242(8) 0.0022(7) 0.0089(7) 0.0044(6) C14 0.0149(8) 0.0269(9) 0.0183(8) 0.0052(7) 0.0030(7) -0.0001(6) C15 0.0194(8) 0.0255(9) 0.0143(7) -0.0018(7) 0.0039(7) -0.0025(7) C16 0.0183(8) 0.0177(8) 0.0162(7) -0.0010(6) 0.0062(7) -0.0001(6) C17 0.0203(8) 0.0125(7) 0.0148(7) 0.0000(6) 0.0070(6) -0.0003(6) C18 0.0260(9) 0.0222(9) 0.0230(8) 0.0026(7) 0.0140(8) 0.0025(7) C19 0.0404(11) 0.0217(9) 0.0187(8) 0.0023(7) 0.0164(8) 0.0005(8) C20 0.0328(10) 0.0194(9) 0.0152(8) 0.0014(7) 0.0033(7) -0.0043(7) C21 0.0195(9) 0.0253(9) 0.0230(9) 0.0044(7) 0.0038(7) -0.0020(7) C22 0.0200(8) 0.0207(8) 0.0182(8) 0.0022(7) 0.0087(7) -0.0013(6) C23 0.0154(8) 0.0264(9) 0.0252(9) 0.0024(7) 0.0083(7) -0.0014(7) C24 0.0283(9) 0.0182(8) 0.0235(9) -0.0043(7) 0.0103(8) -0.0071(7) P2 0.0145(2) 0.01494(19) 0.01473(19) 0.00106(15) 0.00775(16) 0.00099(15) O4 0.0167(6) 0.0264(6) 0.0190(6) 0.0054(5) 0.0085(5) 0.0043(5) O5 0.0140(6) 0.0255(6) 0.0212(6) 0.0041(5) 0.0090(5) 0.0031(5) O6 0.0204(6) 0.0251(6) 0.0176(6) 0.0009(5) 0.0104(5) -0.0033(5) N2 0.0184(7) 0.0350(9) 0.0165(7) 0.0042(6) 0.0061(6) -0.0014(6) C25 0.0251(9) 0.0218(9) 0.0182(8) 0.0008(7) 0.0100(7) -0.0017(7) C26 0.0216(9) 0.0329(10) 0.0162(8) -0.0034(7) 0.0079(7) -0.0024(7) C27 0.0216(9) 0.0261(9) 0.0206(8) 0.0073(7) 0.0072(7) -0.0013(7) C28 0.0219(9) 0.0220(9) 0.0171(8) 0.0010(7) 0.0072(7) -0.0021(7) C29 0.0129(7) 0.0228(8) 0.0150(7) 0.0032(6) 0.0060(6) 0.0001(6) C30 0.0174(8) 0.0153(8) 0.0146(7) -0.0003(6) 0.0075(6) -0.0020(6) C31 0.0161(8) 0.0165(8) 0.0121(7) -0.0007(6) 0.0065(6) -0.0013(6) C32 0.0172(8) 0.0146(7) 0.0142(7) -0.0031(6) 0.0061(6) -0.0029(6) C33 0.0156(8) 0.0314(10) 0.0316(10) 0.0015(8) 0.0121(8) 0.0026(7) C34 0.0128(7) 0.0178(8) 0.0132(7) 0.0010(6) 0.0059(6) 0.0015(6) C35 0.0131(7) 0.0220(8) 0.0145(7) 0.0001(6) 0.0061(6) -0.0003(6) C36 0.0193(8) 0.0212(8) 0.0157(7) 0.0006(6) 0.0071(7) -0.0020(6) C37 0.0273(9) 0.0213(9) 0.0213(8) -0.0028(7) 0.0108(8) -0.0020(7) C38 0.0307(10) 0.0303(10) 0.0182(8) -0.0059(7) 0.0123(8) -0.0069(8) C39 0.0247(9) 0.0318(10) 0.0143(8) 0.0021(7) 0.0072(7) -0.0040(7) C40 0.0188(8) 0.0230(9) 0.0164(8) 0.0023(7) 0.0063(7) 0.0000(6) C41 0.0191(8) 0.0145(7) 0.0153(7) 0.0009(6) 0.0087(6) -0.0014(6) C42 0.0189(8) 0.0205(8) 0.0245(9) 0.0004(7) 0.0082(7) 0.0007(6) C43 0.0210(9) 0.0262(9) 0.0227(9) -0.0007(7) 0.0017(7) -0.0014(7) C44 0.0320(10) 0.0231(9) 0.0204(8) -0.0039(7) 0.0096(8) -0.0066(7) C45 0.0286(10) 0.0205(9) 0.0252(9) -0.0050(7) 0.0159(8) -0.0025(7) C46 0.0190(8) 0.0189(8) 0.0214(8) -0.0009(7) 0.0095(7) -0.0001(6) C47 0.0172(8) 0.0195(8) 0.0181(8) -0.0006(6) 0.0099(7) 0.0013(6) C48 0.0224(8) 0.0184(8) 0.0196(8) 0.0036(6) 0.0118(7) 0.0008(6) O7 0.0266(7) 0.0231(7) 0.0243(6) -0.0044(5) 0.0092(6) 0.0012(5) O8 0.0251(7) 0.0364(7) 0.0182(6) 0.0074(5) 0.0102(5) 0.0096(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 P1 C23 1.7916(17) . ? P1 C17 1.7931(17) . ? P1 C24 1.7994(18) . ? P1 C10 1.8395(16) . ? O1 C6 1.2697(19) . ? O2 C8 1.2340(18) . ? O3 C8 1.3640(19) . ? O3 C9 1.439(2) . ? N1 C2 1.340(2) . ? N1 C3 1.341(2) . ? C1 C2 1.385(2) . ? C1 C5 1.390(2) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.391(2) . ? C3 H3 0.9500 . ? C4 C5 1.390(2) . ? C4 H4 0.9500 . ? C5 C6 1.503(2) . ? C6 C7 1.395(2) . ? C7 C8 1.431(2) . ? C7 C10 1.514(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.529(2) . ? C10 H10 1.0000 . ? C11 C16 1.394(2) . ? C11 C12 1.398(2) . ? C12 C13 1.388(2) . ? C12 H12 0.9500 . ? C13 C14 1.392(2) . ? C13 H13 0.9500 . ? C14 C15 1.389(2) . ? C14 H14 0.9500 . ? C15 C16 1.394(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.392(2) . ? C17 C22 1.394(2) . ? C18 C19 1.392(2) . ? C18 H18 0.9500 . ? C19 C20 1.384(3) . ? C19 H19 0.9500 . ? C20 C21 1.383(2) . ? C20 H20 0.9500 . ? C21 C22 1.391(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? P2 C47 1.7940(16) . ? P2 C41 1.8019(17) . ? P2 C48 1.8027(16) . ? P2 C34 1.8488(16) . ? O4 C30 1.2758(19) . ? O5 C32 1.3704(19) . ? O5 C33 1.445(2) . ? O6 C32 1.2268(19) . ? N2 C26 1.337(2) . ? N2 C27 1.337(2) . ? C25 C26 1.383(2) . ? C25 C29 1.394(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.391(2) . ? C27 H27 0.9500 . ? C28 C29 1.387(2) . ? C28 H28 0.9500 . ? C29 C30 1.507(2) . ? C30 C31 1.384(2) . ? C31 C32 1.437(2) . ? C31 C34 1.517(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.527(2) . ? C34 H34 1.0000 . ? C35 C36 1.390(2) . ? C35 C40 1.399(2) . ? C36 C37 1.394(2) . ? C36 H36 0.9500 . ? C37 C38 1.392(2) . ? C37 H37 0.9500 . ? C38 C39 1.380(3) . ? C38 H38 0.9500 . ? C39 C40 1.388(2) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.395(2) . ? C41 C46 1.398(2) . ? C42 C43 1.388(2) . ? C42 H42 0.9500 . ? C43 C44 1.388(3) . ? C43 H43 0.9500 . ? C44 C45 1.387(3) . ? C44 H44 0.9500 . ? C45 C46 1.391(2) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O7 H7A 0.8960 . ? O7 H7B 0.8386 . ? O8 H8A 0.8867 . ? O8 H8B 0.9082 . ? 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 C23 P1 C17 113.21(8) . . ? C23 P1 C24 103.34(9) . . ? C17 P1 C24 103.10(8) . . ? C23 P1 C10 117.92(8) . . ? C17 P1 C10 113.22(7) . . ? C24 P1 C10 103.78(8) . . ? C8 O3 C9 115.41(13) . . ? C2 N1 C3 115.88(15) . . ? C2 C1 C5 118.99(16) . . ? C2 C1 H1 120.5 . . ? C5 C1 H1 120.5 . . ? N1 C2 C1 124.36(16) . . ? N1 C2 H2 117.8 . . ? C1 C2 H2 117.8 . . ? N1 C3 C4 124.23(16) . . ? N1 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? C5 C4 C3 118.78(16) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C1 C5 C4 117.76(15) . . ? C1 C5 C6 122.10(14) . . ? C4 C5 C6 119.89(14) . . ? O1 C6 C7 120.20(14) . . ? O1 C6 C5 115.24(13) . . ? C7 C6 C5 124.55(14) . . ? C6 C7 C8 129.39(14) . . ? C6 C7 C10 116.37(14) . . ? C8 C7 C10 114.20(13) . . ? O2 C8 O3 119.83(14) . . ? O2 C8 C7 124.60(14) . . ? O3 C8 C7 115.57(13) . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 C11 114.96(13) . . ? C7 C10 P1 114.17(11) . . ? C11 C10 P1 108.61(10) . . ? C7 C10 H10 106.1 . . ? C11 C10 H10 106.1 . . ? P1 C10 H10 106.1 . . ? C16 C11 C12 118.83(15) . . ? C16 C11 C10 120.40(14) . . ? C12 C11 C10 120.76(14) . . ? C13 C12 C11 120.26(15) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 120.71(16) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 119.30(15) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.12(16) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.76(15) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C18 C17 C22 119.81(15) . . ? C18 C17 P1 120.81(13) . . ? C22 C17 P1 119.14(12) . . ? C19 C18 C17 120.20(17) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 119.59(16) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.60(16) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 120.08(17) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 119.71(15) . . ? C21 C22 H22 120.1 . . ? C17 C22 H22 120.1 . . ? P1 C23 H23A 109.5 . . ? P1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P1 C24 H24A 109.5 . . ? P1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C47 P2 C41 116.30(8) . . ? C47 P2 C48 103.34(8) . . ? C41 P2 C48 103.87(8) . . ? C47 P2 C34 115.71(8) . . ? C41 P2 C34 110.20(7) . . ? C48 P2 C34 105.86(8) . . ? C32 O5 C33 115.62(13) . . ? C26 N2 C27 116.24(15) . . ? C26 C25 C29 118.69(16) . . ? C26 C25 H25 120.7 . . ? C29 C25 H25 120.7 . . ? N2 C26 C25 124.39(17) . . ? N2 C26 H26 117.8 . . ? C25 C26 H26 117.8 . . ? N2 C27 C28 123.95(16) . . ? N2 C27 H27 118.0 . . ? C28 C27 H27 118.0 . . ? C29 C28 C27 118.88(16) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C25 117.83(15) . . ? C28 C29 C30 122.18(15) . . ? C25 C29 C30 119.35(15) . . ? O4 C30 C31 120.78(14) . . ? O4 C30 C29 114.08(14) . . ? C31 C30 C29 124.86(14) . . ? C30 C31 C32 122.79(14) . . ? C30 C31 C34 117.45(14) . . ? C32 C31 C34 119.75(14) . . ? O6 C32 O5 120.51(14) . . ? O6 C32 C31 126.63(15) . . ? O5 C32 C31 112.86(13) . . ? O5 C33 H33A 109.5 . . ? O5 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O5 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 C35 116.79(13) . . ? C31 C34 P2 112.94(11) . . ? C35 C34 P2 107.01(10) . . ? C31 C34 H34 106.5 . . ? C35 C34 H34 106.5 . . ? P2 C34 H34 106.5 . . ? C36 C35 C40 118.85(15) . . ? C36 C35 C34 121.34(14) . . ? C40 C35 C34 119.74(15) . . ? C35 C36 C37 120.40(16) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C38 C37 C36 120.22(17) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C37 119.56(16) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 120.48(16) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C35 120.47(16) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? C42 C41 C46 119.82(15) . . ? C42 C41 P2 122.03(13) . . ? C46 C41 P2 118.12(13) . . ? C43 C42 C41 119.61(16) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 120.49(17) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.17(16) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 119.83(16) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 120.05(16) . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? P2 C47 H47A 109.5 . . ? P2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? P2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? P2 C48 H48A 109.5 . . ? P2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? P2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? H7A O7 H7B 105.3 . . ? H8A O8 H8B 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C2 C1 0.5(3) . . . . ? C5 C1 C2 N1 -0.3(3) . . . . ? C2 N1 C3 C4 -0.1(3) . . . . ? N1 C3 C4 C5 -0.5(3) . . . . ? C2 C1 C5 C4 -0.3(2) . . . . ? C2 C1 C5 C6 -174.50(15) . . . . ? C3 C4 C5 C1 0.6(2) . . . . ? C3 C4 C5 C6 174.96(15) . . . . ? C1 C5 C6 O1 104.36(18) . . . . ? C4 C5 C6 O1 -69.70(19) . . . . ? C1 C5 C6 C7 -74.4(2) . . . . ? C4 C5 C6 C7 111.49(18) . . . . ? O1 C6 C7 C8 179.57(15) . . . . ? C5 C6 C7 C8 -1.7(3) . . . . ? O1 C6 C7 C10 2.0(2) . . . . ? C5 C6 C7 C10 -179.22(14) . . . . ? C9 O3 C8 O2 1.5(2) . . . . ? C9 O3 C8 C7 -178.05(14) . . . . ? C6 C7 C8 O2 175.28(16) . . . . ? C10 C7 C8 O2 -7.1(2) . . . . ? C6 C7 C8 O3 -5.2(2) . . . . ? C10 C7 C8 O3 172.40(13) . . . . ? C6 C7 C10 C11 87.08(17) . . . . ? C8 C7 C10 C11 -90.83(16) . . . . ? C6 C7 C10 P1 -39.41(17) . . . . ? C8 C7 C10 P1 142.68(12) . . . . ? C23 P1 C10 C7 100.18(13) . . . . ? C17 P1 C10 C7 -35.26(13) . . . . ? C24 P1 C10 C7 -146.31(12) . . . . ? C23 P1 C10 C11 -29.55(13) . . . . ? C17 P1 C10 C11 -164.99(10) . . . . ? C24 P1 C10 C11 83.96(12) . . . . ? C7 C10 C11 C16 143.93(15) . . . . ? P1 C10 C11 C16 -86.79(16) . . . . ? C7 C10 C11 C12 -35.0(2) . . . . ? P1 C10 C11 C12 94.29(15) . . . . ? C16 C11 C12 C13 -0.4(2) . . . . ? C10 C11 C12 C13 178.58(15) . . . . ? C11 C12 C13 C14 1.3(2) . . . . ? C12 C13 C14 C15 -1.1(3) . . . . ? C13 C14 C15 C16 -0.1(2) . . . . ? C12 C11 C16 C15 -0.8(2) . . . . ? C10 C11 C16 C15 -179.78(14) . . . . ? C14 C15 C16 C11 1.1(2) . . . . ? C23 P1 C17 C18 10.63(17) . . . . ? C24 P1 C17 C18 -100.32(15) . . . . ? C10 P1 C17 C18 148.21(13) . . . . ? C23 P1 C17 C22 -175.03(13) . . . . ? C24 P1 C17 C22 74.02(15) . . . . ? C10 P1 C17 C22 -37.45(15) . . . . ? C22 C17 C18 C19 0.1(3) . . . . ? P1 C17 C18 C19 174.38(13) . . . . ? C17 C18 C19 C20 0.0(3) . . . . ? C18 C19 C20 C21 0.1(3) . . . . ? C19 C20 C21 C22 -0.3(3) . . . . ? C20 C21 C22 C17 0.3(3) . . . . ? C18 C17 C22 C21 -0.3(2) . . . . ? P1 C17 C22 C21 -174.65(13) . . . . ? C27 N2 C26 C25 -1.3(3) . . . . ? C29 C25 C26 N2 1.0(3) . . . . ? C26 N2 C27 C28 0.2(3) . . . . ? N2 C27 C28 C29 1.1(3) . . . . ? C27 C28 C29 C25 -1.3(2) . . . . ? C27 C28 C29 C30 -172.09(15) . . . . ? C26 C25 C29 C28 0.4(2) . . . . ? C26 C25 C29 C30 171.41(15) . . . . ? C28 C29 C30 O4 72.3(2) . . . . ? C25 C29 C30 O4 -98.37(18) . . . . ? C28 C29 C30 C31 -113.70(19) . . . . ? C25 C29 C30 C31 75.7(2) . . . . ? O4 C30 C31 C32 -173.98(15) . . . . ? C29 C30 C31 C32 12.4(2) . . . . ? O4 C30 C31 C34 4.5(2) . . . . ? C29 C30 C31 C34 -169.14(14) . . . . ? C33 O5 C32 O6 3.8(2) . . . . ? C33 O5 C32 C31 -175.64(14) . . . . ? C30 C31 C32 O6 3.0(3) . . . . ? C34 C31 C32 O6 -175.51(15) . . . . ? C30 C31 C32 O5 -177.67(14) . . . . ? C34 C31 C32 O5 3.9(2) . . . . ? C30 C31 C34 C35 -90.89(17) . . . . ? C32 C31 C34 C35 87.65(18) . . . . ? C30 C31 C34 P2 33.83(18) . . . . ? C32 C31 C34 P2 -147.63(12) . . . . ? C47 P2 C34 C31 -95.57(12) . . . . ? C41 P2 C34 C31 38.94(13) . . . . ? C48 P2 C34 C31 150.66(11) . . . . ? C47 P2 C34 C35 34.33(13) . . . . ? C41 P2 C34 C35 168.83(10) . . . . ? C48 P2 C34 C35 -79.44(12) . . . . ? C31 C34 C35 C36 31.4(2) . . . . ? P2 C34 C35 C36 -96.26(16) . . . . ? C31 C34 C35 C40 -151.62(15) . . . . ? P2 C34 C35 C40 80.71(16) . . . . ? C40 C35 C36 C37 -1.2(2) . . . . ? C34 C35 C36 C37 175.82(15) . . . . ? C35 C36 C37 C38 0.1(3) . . . . ? C36 C37 C38 C39 0.8(3) . . . . ? C37 C38 C39 C40 -0.5(3) . . . . ? C38 C39 C40 C35 -0.6(3) . . . . ? C36 C35 C40 C39 1.5(2) . . . . ? C34 C35 C40 C39 -175.59(15) . . . . ? C47 P2 C41 C42 -8.66(17) . . . . ? C48 P2 C41 C42 104.12(14) . . . . ? C34 P2 C41 C42 -142.88(13) . . . . ? C47 P2 C41 C46 173.29(12) . . . . ? C48 P2 C41 C46 -73.93(14) . . . . ? C34 P2 C41 C46 39.08(15) . . . . ? C46 C41 C42 C43 -0.8(2) . . . . ? P2 C41 C42 C43 -178.79(13) . . . . ? C41 C42 C43 C44 -0.7(3) . . . . ? C42 C43 C44 C45 1.5(3) . . . . ? C43 C44 C45 C46 -1.0(3) . . . . ? C44 C45 C46 C41 -0.5(3) . . . . ? C42 C41 C46 C45 1.3(2) . . . . ? P2 C41 C46 C45 179.43(13) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.507 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.062