data_zs12_hyd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H36 N3 O12 P3 Pr' _chemical_formula_weight 972.53 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' 'Pr' 'Pr' -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 13.022(2) _cell_length_b 19.989(4) _cell_length_c 16.747(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.376(18) _cell_angle_gamma 90.00 _cell_volume 4136.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5499 _exptl_absorpt_correction_T_max 0.6125 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _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 19663 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7183 _reflns_number_gt 6531 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0419P)^2^+6.4417P] 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 7183 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.002 _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 Pr1 Pr 0.956216(13) 0.175626(8) 0.685688(10) 0.01230(8) Uani 1 1 d . . . P3 P 0.98779(7) -0.01107(4) 0.62799(5) 0.01370(17) Uani 1 1 d . . . P1 P 1.18119(6) 0.13700(4) 0.89522(5) 0.01336(17) Uani 1 1 d . . . O22 O 0.8579(2) 0.11470(11) 0.77893(15) 0.0233(5) Uani 1 1 d . . . C1F C 1.1180(3) -0.04665(17) 0.6834(2) 0.0180(7) Uani 1 1 d . . . O31 O 1.01818(18) 0.29613(12) 0.74581(14) 0.0206(5) Uani 1 1 d . . . O12 O 0.9772(2) 0.18281(12) 0.53680(15) 0.0239(6) Uani 1 1 d . . . O3 O 0.98322(18) 0.06115(11) 0.65195(13) 0.0167(5) Uani 1 1 d . . . N20 N 0.8262(2) 0.16756(13) 0.80510(17) 0.0163(6) Uani 1 1 d . . . O11 O 1.1144(2) 0.21562(13) 0.64027(15) 0.0270(6) Uani 1 1 d . . . O1 O 1.10166(18) 0.15209(11) 0.81010(13) 0.0173(5) Uani 1 1 d . . . O13 O 1.1130(2) 0.23176(15) 0.51166(17) 0.0367(7) Uani 1 1 d . . . C5A C 1.4362(4) 0.1469(2) 0.8053(3) 0.0426(11) Uani 1 1 d . . . H5AA H 1.4469 0.1567 0.7530 0.051 Uiso 1 1 calc R . . C1A C 1.3171(3) 0.13552(16) 0.8892(2) 0.0185(7) Uani 1 1 d . . . O23 O 0.7648(2) 0.16631(13) 0.84691(18) 0.0316(6) Uani 1 1 d . . . O2 O 0.77470(19) 0.16585(11) 0.59742(14) 0.0183(5) Uani 1 1 d . . . O32 O 0.8925(2) 0.29132(12) 0.62561(15) 0.0258(6) Uani 1 1 d . . . C6A C 1.3327(3) 0.1508(2) 0.8127(2) 0.0278(8) Uani 1 1 d . . . H6AA H 1.2732 0.1637 0.7657 0.033 Uiso 1 1 calc R . . C2A C 1.4050(3) 0.1168(2) 0.9577(2) 0.0335(9) Uani 1 1 d . . . H2AA H 1.3948 0.1061 1.0099 0.040 Uiso 1 1 calc R . . C4F C 1.3045(3) -0.1027(2) 0.7925(3) 0.0428(11) Uani 1 1 d . . . H4FA H 1.3665 -0.1221 0.8320 0.051 Uiso 1 1 calc R . . C6B C 1.2060(3) 0.03779(18) 1.0185(2) 0.0266(8) Uani 1 1 d . . . H6BA H 1.2572 0.0666 1.0557 0.032 Uiso 1 1 calc R . . C2B C 1.0763(3) 0.01604(17) 0.8828(2) 0.0214(7) Uani 1 1 d . . . H2BA H 1.0382 0.0300 0.8271 0.026 Uiso 1 1 calc R . . O33 O 0.9394(2) 0.38763(12) 0.68545(16) 0.0277(6) Uani 1 1 d . . . C3 C 0.9616(3) -0.02135(16) 0.51627(19) 0.0170(7) Uani 1 1 d . . . H3A H 0.9704 -0.0691 0.5039 0.020 Uiso 1 1 calc R . . H3B H 0.8858 -0.0084 0.4862 0.020 Uiso 1 1 calc R . . N30 N 0.9502(2) 0.32664(13) 0.68570(16) 0.0160(6) Uani 1 1 d . . . O21 O 0.8607(2) 0.22243(12) 0.78559(16) 0.0250(6) Uani 1 1 d . . . C4A C 1.5230(3) 0.1289(3) 0.8735(3) 0.0472(12) Uani 1 1 d . . . H4AA H 1.5935 0.1269 0.8683 0.057 Uiso 1 1 calc R . . N10 N 1.0695(2) 0.21073(14) 0.56119(18) 0.0220(6) Uani 1 1 d . . . C1 C 1.1740(3) 0.19814(16) 0.9720(2) 0.0167(7) Uani 1 1 d . . . H1A H 1.1040 0.1931 0.9830 0.020 Uiso 1 1 calc R . . H1B H 1.2324 0.1891 1.0253 0.020 Uiso 1 1 calc R . . C6F C 1.1946(3) -0.0060(2) 0.7380(2) 0.0304(9) Uani 1 1 d . . . H6FA H 1.1834 0.0409 0.7384 0.036 Uiso 1 1 calc R . . C3F C 1.2311(3) -0.1428(2) 0.7355(3) 0.0357(10) Uani 1 1 d . . . H3FA H 1.2442 -0.1894 0.7336 0.043 Uiso 1 1 calc R . . C5F C 1.2883(3) -0.0347(3) 0.7925(3) 0.0446(12) Uani 1 1 d . . . H5FA H 1.3414 -0.0070 0.8298 0.053 Uiso 1 1 calc R . . C2F C 1.1384(3) -0.11509(18) 0.6810(2) 0.0270(8) Uani 1 1 d . . . H2FA H 1.0879 -0.1428 0.6415 0.032 Uiso 1 1 calc R . . C3A C 1.5076(3) 0.1137(3) 0.9494(3) 0.0448(11) Uani 1 1 d . . . H3AA H 1.5676 0.1011 0.9962 0.054 Uiso 1 1 calc R . . C5B C 1.1838(3) -0.02411(19) 1.0460(2) 0.0314(9) Uani 1 1 d . . . H5BA H 1.2196 -0.0376 1.1024 0.038 Uiso 1 1 calc R . . C1B C 1.1532(3) 0.05798(16) 0.9357(2) 0.0165(7) Uani 1 1 d . . . C5E C 0.7979(3) -0.16467(17) 0.6615(2) 0.0236(8) Uani 1 1 d . . . H5EA H 0.7854 -0.2105 0.6464 0.028 Uiso 1 1 calc R . . C4E C 0.7447(3) -0.13507(18) 0.7122(2) 0.0256(8) Uani 1 1 d . . . H4EA H 0.6950 -0.1605 0.7308 0.031 Uiso 1 1 calc R . . C2E C 0.8365(3) -0.03185(17) 0.7089(2) 0.0192(7) Uani 1 1 d . . . H2EA H 0.8504 0.0135 0.7260 0.023 Uiso 1 1 calc R . . C6E C 0.8695(3) -0.12763(16) 0.6327(2) 0.0198(7) Uani 1 1 d . . . H6EA H 0.9045 -0.1475 0.5967 0.024 Uiso 1 1 calc R . . C3E C 0.7633(3) -0.06882(18) 0.7358(2) 0.0254(8) Uani 1 1 d . . . H3EA H 0.7263 -0.0487 0.7702 0.030 Uiso 1 1 calc R . . C1E C 0.8896(3) -0.06055(16) 0.65742(19) 0.0156(6) Uani 1 1 d . . . C4B C 1.1098(3) -0.06655(19) 0.9923(2) 0.0315(9) Uani 1 1 d . . . H4BA H 1.0965 -0.1096 1.0110 0.038 Uiso 1 1 calc R . . C3B C 1.0551(3) -0.04565(18) 0.9107(2) 0.0283(8) Uani 1 1 d . . . H3BA H 1.0027 -0.0741 0.8740 0.034 Uiso 1 1 calc R . . P2 P 0.67252(7) 0.17080(4) 0.52374(5) 0.01379(18) Uani 1 1 d . . . C2D C 0.5866(3) 0.23180(19) 0.6368(2) 0.0245(8) Uani 1 1 d . . . H2DA H 0.6588 0.2321 0.6740 0.029 Uiso 1 1 calc R . . C2 C 0.6845(3) 0.22962(16) 0.4452(2) 0.0185(7) Uani 1 1 d . . . H2A H 0.7555 0.2237 0.4362 0.022 Uiso 1 1 calc R . . H2B H 0.6273 0.2205 0.3912 0.022 Uiso 1 1 calc R . . C1D C 0.5634(3) 0.20195(16) 0.5578(2) 0.0153(6) Uani 1 1 d . . . C4D C 0.3991(3) 0.26030(19) 0.6078(2) 0.0282(8) Uani 1 1 d . . . H4DA H 0.3429 0.2796 0.6251 0.034 Uiso 1 1 calc R . . C1C C 0.6360(3) 0.09022(16) 0.4755(2) 0.0171(7) Uani 1 1 d . . . C6C C 0.6586(3) 0.03528(18) 0.5295(2) 0.0264(8) Uani 1 1 d . . . H6CA H 0.6913 0.0419 0.5882 0.032 Uiso 1 1 calc R . . C3D C 0.5049(3) 0.2610(2) 0.6613(2) 0.0305(9) Uani 1 1 d . . . H3DA H 0.5213 0.2816 0.7150 0.037 Uiso 1 1 calc R . . C5C C 0.6339(3) -0.02879(18) 0.4982(2) 0.0301(9) Uani 1 1 d . . . H5CA H 0.6491 -0.0659 0.5356 0.036 Uiso 1 1 calc R . . C4C C 0.5873(3) -0.03891(18) 0.4131(2) 0.0301(9) Uani 1 1 d . . . H4CA H 0.5714 -0.0830 0.3914 0.036 Uiso 1 1 calc R . . C5D C 0.3757(3) 0.2313(2) 0.5289(2) 0.0273(8) Uani 1 1 d . . . H5DA H 0.3034 0.2313 0.4919 0.033 Uiso 1 1 calc R . . C6D C 0.4567(3) 0.20259(18) 0.5036(2) 0.0230(7) Uani 1 1 d . . . H6DA H 0.4400 0.1832 0.4492 0.028 Uiso 1 1 calc R . . C2C C 0.5879(3) 0.07993(18) 0.3901(2) 0.0307(9) Uani 1 1 d . . . H2CA H 0.5717 0.1170 0.3527 0.037 Uiso 1 1 calc R . . C3C C 0.5635(4) 0.01579(19) 0.3590(2) 0.0373(10) Uani 1 1 d . . . H3CA H 0.5302 0.0090 0.3003 0.045 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 Pr1 0.01293(11) 0.01031(11) 0.01120(11) 0.00003(6) 0.00030(8) -0.00033(6) P3 0.0172(4) 0.0106(4) 0.0123(4) -0.0008(3) 0.0032(3) -0.0008(3) P1 0.0141(4) 0.0115(4) 0.0116(4) -0.0006(3) 0.0000(3) 0.0008(3) O22 0.0321(14) 0.0138(12) 0.0266(13) 0.0002(10) 0.0129(11) 0.0018(10) C1F 0.0171(16) 0.0211(18) 0.0152(16) 0.0003(13) 0.0040(14) 0.0027(14) O31 0.0205(12) 0.0160(12) 0.0193(12) -0.0007(9) -0.0023(10) -0.0002(10) O12 0.0275(14) 0.0236(13) 0.0191(13) -0.0011(10) 0.0052(11) -0.0070(10) O3 0.0202(12) 0.0119(11) 0.0165(11) -0.0017(9) 0.0037(10) -0.0013(9) N20 0.0195(14) 0.0155(15) 0.0153(14) 0.0034(11) 0.0074(12) 0.0023(11) O11 0.0241(13) 0.0355(15) 0.0194(13) -0.0024(11) 0.0040(11) -0.0043(11) O1 0.0194(12) 0.0153(11) 0.0127(11) 0.0002(9) -0.0012(9) 0.0003(9) O13 0.0455(17) 0.0403(17) 0.0337(15) -0.0011(13) 0.0258(14) -0.0054(14) C5A 0.042(3) 0.049(3) 0.045(3) 0.008(2) 0.026(2) -0.004(2) C1A 0.0202(17) 0.0132(16) 0.0188(17) -0.0031(13) 0.0016(14) -0.0020(13) O23 0.0396(16) 0.0227(14) 0.0411(16) 0.0075(11) 0.0252(14) 0.0071(12) O2 0.0173(12) 0.0183(12) 0.0163(12) 0.0012(9) 0.0013(10) -0.0011(9) O32 0.0293(13) 0.0140(12) 0.0235(13) 0.0011(10) -0.0066(11) -0.0002(10) C6A 0.0266(19) 0.028(2) 0.031(2) 0.0048(16) 0.0111(17) 0.0007(16) C2A 0.0219(19) 0.050(3) 0.026(2) -0.0042(18) 0.0046(17) 0.0026(18) C4F 0.031(2) 0.062(3) 0.033(2) 0.000(2) 0.0060(19) 0.026(2) C6B 0.034(2) 0.0193(18) 0.0190(18) 0.0002(14) -0.0018(16) -0.0001(16) C2B 0.0198(17) 0.0208(18) 0.0193(17) 0.0024(14) 0.0000(14) 0.0004(14) O33 0.0346(15) 0.0119(13) 0.0357(15) -0.0001(10) 0.0099(12) 0.0032(10) C3 0.0201(16) 0.0169(16) 0.0127(15) -0.0020(13) 0.0034(14) -0.0033(14) N30 0.0162(15) 0.0128(15) 0.0191(16) 0.0015(11) 0.0057(13) 0.0000(10) O21 0.0355(14) 0.0128(12) 0.0313(14) -0.0004(10) 0.0172(12) -0.0018(11) C4A 0.019(2) 0.064(3) 0.062(3) -0.005(2) 0.019(2) -0.006(2) N10 0.0291(16) 0.0154(14) 0.0256(16) -0.0008(12) 0.0145(14) -0.0010(12) C1 0.0234(17) 0.0082(15) 0.0166(16) -0.0004(12) 0.0037(14) 0.0024(13) C6F 0.0209(18) 0.032(2) 0.035(2) -0.0132(17) 0.0043(17) 0.0023(16) C3F 0.032(2) 0.036(2) 0.041(2) 0.0093(19) 0.0143(19) 0.0124(18) C5F 0.023(2) 0.062(3) 0.039(2) -0.027(2) -0.0044(19) 0.012(2) C2F 0.0228(18) 0.0226(19) 0.034(2) 0.0005(15) 0.0066(17) 0.0004(15) C3A 0.020(2) 0.068(3) 0.040(3) -0.009(2) -0.0006(19) 0.005(2) C5B 0.043(2) 0.026(2) 0.0190(18) 0.0082(15) 0.0008(17) 0.0001(18) C1B 0.0195(16) 0.0132(16) 0.0162(16) 0.0013(13) 0.0049(14) 0.0035(13) C5E 0.0273(19) 0.0142(17) 0.0219(18) -0.0003(14) -0.0026(16) -0.0068(14) C4E 0.0281(19) 0.0222(19) 0.0259(19) 0.0048(15) 0.0075(16) -0.0070(15) C2E 0.0200(17) 0.0145(16) 0.0196(17) -0.0028(13) 0.0010(14) -0.0037(13) C6E 0.0236(18) 0.0141(16) 0.0190(17) -0.0013(13) 0.0029(14) -0.0013(14) C3E 0.0265(19) 0.028(2) 0.0221(18) -0.0043(15) 0.0080(16) -0.0040(16) C1E 0.0150(15) 0.0149(16) 0.0126(15) 0.0031(12) -0.0018(13) -0.0025(13) C4B 0.042(2) 0.0167(19) 0.032(2) 0.0077(15) 0.0076(18) -0.0024(17) C3B 0.030(2) 0.0202(19) 0.028(2) -0.0002(15) 0.0004(17) -0.0066(16) P2 0.0135(4) 0.0116(4) 0.0132(4) 0.0020(3) -0.0001(3) -0.0011(3) C2D 0.0197(17) 0.030(2) 0.0195(18) 0.0017(15) 0.0003(15) 0.0010(15) C2 0.0239(17) 0.0155(17) 0.0150(16) 0.0025(13) 0.0044(14) -0.0013(14) C1D 0.0185(16) 0.0100(15) 0.0166(16) 0.0031(12) 0.0044(13) -0.0006(13) C4D 0.0265(19) 0.030(2) 0.030(2) -0.0010(16) 0.0115(17) 0.0029(16) C1C 0.0146(16) 0.0149(16) 0.0195(17) 0.0010(13) 0.0021(14) -0.0011(13) C6C 0.0279(19) 0.0202(18) 0.0228(19) 0.0033(14) -0.0041(16) -0.0020(15) C3D 0.033(2) 0.037(2) 0.0188(18) -0.0084(16) 0.0050(17) 0.0011(17) C5C 0.033(2) 0.0153(18) 0.033(2) 0.0035(15) -0.0022(17) -0.0002(16) C4C 0.039(2) 0.0128(17) 0.038(2) -0.0045(15) 0.0115(18) -0.0063(16) C5D 0.0165(17) 0.034(2) 0.027(2) -0.0001(16) -0.0002(15) 0.0013(15) C6D 0.0204(17) 0.0251(19) 0.0188(17) -0.0015(14) -0.0007(15) -0.0028(15) C2C 0.052(3) 0.0172(18) 0.0194(18) 0.0033(14) 0.0068(18) -0.0073(17) C3C 0.068(3) 0.022(2) 0.0182(19) -0.0040(15) 0.008(2) -0.014(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 Pr1 O2 2.368(2) . ? Pr1 O1 2.379(2) . ? Pr1 O3 2.409(2) . ? Pr1 O11 2.539(3) . ? Pr1 O32 2.554(2) . ? Pr1 O21 2.556(2) . ? Pr1 O12 2.596(2) . ? Pr1 O22 2.612(2) . ? Pr1 O31 2.637(2) . ? Pr1 N10 2.993(3) . ? Pr1 N20 3.004(3) . ? Pr1 N30 3.020(3) . ? P3 O3 1.504(2) . ? P3 C1F 1.802(3) . ? P3 C1E 1.804(3) . ? P3 C3 1.805(3) . ? P1 O1 1.505(2) . ? P1 C1 1.798(3) . ? P1 C1B 1.801(3) . ? P1 C1A 1.804(3) . ? O22 N20 1.262(3) . ? C1F C6F 1.384(5) . ? C1F C2F 1.396(5) . ? O31 N30 1.268(3) . ? O12 N10 1.271(4) . ? N20 O23 1.218(4) . ? N20 O21 1.266(3) . ? O11 N10 1.272(4) . ? O13 N10 1.217(4) . ? C5A C4A 1.378(7) . ? C5A C6A 1.393(6) . ? C1A C2A 1.393(5) . ? C1A C6A 1.393(5) . ? O2 P2 1.506(2) . ? O32 N30 1.264(4) . ? C2A C3A 1.387(6) . ? C4F C3F 1.375(6) . ? C4F C5F 1.377(7) . ? C6B C5B 1.383(5) . ? C6B C1B 1.398(5) . ? C2B C3B 1.377(5) . ? C2B C1B 1.390(5) . ? O33 N30 1.227(4) . ? C3 C3 1.539(6) 3_756 ? C4A C3A 1.382(7) . ? C1 C2 1.531(4) 4_666 ? C6F C5F 1.396(6) . ? C3F C2F 1.379(5) . ? C5B C4B 1.382(5) . ? C5E C4E 1.387(5) . ? C5E C6E 1.390(5) . ? C4E C3E 1.381(5) . ? C2E C1E 1.388(5) . ? C2E C3E 1.388(5) . ? C6E C1E 1.403(5) . ? C4B C3B 1.392(5) . ? P2 C1C 1.797(3) . ? P2 C1D 1.802(3) . ? P2 C2 1.808(3) . ? C2D C3D 1.384(5) . ? C2D C1D 1.394(5) . ? C2 C1 1.531(4) 4_565 ? C1D C6D 1.400(5) . ? C4D C5D 1.386(5) . ? C4D C3D 1.386(5) . ? C1C C2C 1.385(5) . ? C1C C6C 1.394(5) . ? C6C C5C 1.383(5) . ? C5C C4C 1.377(5) . ? C4C C3C 1.391(5) . ? C5D C6D 1.380(5) . ? C2C C3C 1.383(5) . ? 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 O2 Pr1 O1 153.21(8) . . ? O2 Pr1 O3 88.05(8) . . ? O1 Pr1 O3 83.27(7) . . ? O2 Pr1 O11 125.68(8) . . ? O1 Pr1 O11 80.07(8) . . ? O3 Pr1 O11 92.10(8) . . ? O2 Pr1 O32 72.09(8) . . ? O1 Pr1 O32 126.44(8) . . ? O3 Pr1 O32 145.18(8) . . ? O11 Pr1 O32 77.89(9) . . ? O2 Pr1 O21 80.96(8) . . ? O1 Pr1 O21 85.21(8) . . ? O3 Pr1 O21 129.67(7) . . ? O11 Pr1 O21 133.54(8) . . ? O32 Pr1 O21 76.22(8) . . ? O2 Pr1 O12 77.96(8) . . ? O1 Pr1 O12 123.80(8) . . ? O3 Pr1 O12 76.11(7) . . ? O11 Pr1 O12 49.77(8) . . ? O32 Pr1 O12 72.00(8) . . ? O21 Pr1 O12 145.94(8) . . ? O2 Pr1 O22 75.74(8) . . ? O1 Pr1 O22 77.83(8) . . ? O3 Pr1 O22 80.37(7) . . ? O11 Pr1 O22 157.32(8) . . ? O32 Pr1 O22 119.88(8) . . ? O21 Pr1 O22 49.30(8) . . ? O12 Pr1 O22 145.06(8) . . ? O2 Pr1 O31 116.03(7) . . ? O1 Pr1 O31 77.47(7) . . ? O3 Pr1 O31 155.14(7) . . ? O11 Pr1 O31 69.35(8) . . ? O32 Pr1 O31 49.12(8) . . ? O21 Pr1 O31 64.48(7) . . ? O12 Pr1 O31 101.77(7) . . ? O22 Pr1 O31 110.26(7) . . ? O2 Pr1 N10 101.46(8) . . ? O1 Pr1 N10 103.02(8) . . ? O3 Pr1 N10 85.34(8) . . ? O11 Pr1 N10 24.89(8) . . ? O32 Pr1 N10 71.54(8) . . ? O21 Pr1 N10 144.96(8) . . ? O12 Pr1 N10 25.01(8) . . ? O22 Pr1 N10 165.50(8) . . ? O31 Pr1 N10 83.87(8) . . ? O2 Pr1 N20 75.53(8) . . ? O1 Pr1 N20 82.33(8) . . ? O3 Pr1 N20 105.05(7) . . ? O11 Pr1 N20 153.74(8) . . ? O32 Pr1 N20 97.45(8) . . ? O21 Pr1 N20 24.68(7) . . ? O12 Pr1 N20 153.39(8) . . ? O22 Pr1 N20 24.73(7) . . ? O31 Pr1 N20 87.92(7) . . ? N10 Pr1 N20 168.92(7) . . ? O2 Pr1 N30 93.54(7) . . ? O1 Pr1 N30 102.19(7) . . ? O3 Pr1 N30 162.78(7) . . ? O11 Pr1 N30 73.07(8) . . ? O32 Pr1 N30 24.44(7) . . ? O21 Pr1 N30 67.42(7) . . ? O12 Pr1 N30 87.44(7) . . ? O22 Pr1 N30 116.64(7) . . ? O31 Pr1 N30 24.73(7) . . ? N10 Pr1 N30 77.54(7) . . ? N20 Pr1 N30 91.92(7) . . ? O3 P3 C1F 110.56(14) . . ? O3 P3 C1E 111.25(14) . . ? C1F P3 C1E 106.01(15) . . ? O3 P3 C3 112.04(14) . . ? C1F P3 C3 109.16(16) . . ? C1E P3 C3 107.59(15) . . ? O1 P1 C1 111.46(14) . . ? O1 P1 C1B 111.83(14) . . ? C1 P1 C1B 105.32(15) . . ? O1 P1 C1A 110.14(14) . . ? C1 P1 C1A 108.94(16) . . ? C1B P1 C1A 109.00(15) . . ? N20 O22 Pr1 95.33(17) . . ? C6F C1F C2F 119.3(3) . . ? C6F C1F P3 118.3(3) . . ? C2F C1F P3 121.9(3) . . ? N30 O31 Pr1 94.77(17) . . ? N10 O12 Pr1 95.22(18) . . ? P3 O3 Pr1 174.18(14) . . ? O23 N20 O22 121.9(3) . . ? O23 N20 O21 121.1(3) . . ? O22 N20 O21 117.0(3) . . ? O23 N20 Pr1 173.6(2) . . ? O22 N20 Pr1 59.95(15) . . ? O21 N20 Pr1 57.43(15) . . ? N10 O11 Pr1 97.93(18) . . ? P1 O1 Pr1 171.57(14) . . ? C4A C5A C6A 120.3(4) . . ? C2A C1A C6A 119.7(3) . . ? C2A C1A P1 121.6(3) . . ? C6A C1A P1 118.6(3) . . ? P2 O2 Pr1 163.01(14) . . ? N30 O32 Pr1 98.88(17) . . ? C5A C6A C1A 119.7(4) . . ? C3A C2A C1A 119.8(4) . . ? C3F C4F C5F 120.2(4) . . ? C5B C6B C1B 120.0(3) . . ? C3B C2B C1B 120.3(3) . . ? C3 C3 P3 111.9(3) 3_756 . ? O33 N30 O32 120.9(3) . . ? O33 N30 O31 122.1(3) . . ? O32 N30 O31 117.0(3) . . ? O33 N30 Pr1 175.0(2) . . ? O32 N30 Pr1 56.68(15) . . ? O31 N30 Pr1 60.50(15) . . ? N20 O21 Pr1 97.89(17) . . ? C5A C4A C3A 120.0(4) . . ? O13 N10 O12 122.0(3) . . ? O13 N10 O11 121.5(3) . . ? O12 N10 O11 116.5(3) . . ? O13 N10 Pr1 173.3(2) . . ? O12 N10 Pr1 59.77(15) . . ? O11 N10 Pr1 57.18(15) . . ? C2 C1 P1 113.7(2) 4_666 . ? C1F C6F C5F 119.4(4) . . ? C4F C3F C2F 119.8(4) . . ? C4F C5F C6F 120.5(4) . . ? C3F C2F C1F 120.6(4) . . ? C4A C3A C2A 120.4(4) . . ? C4B C5B C6B 120.5(3) . . ? C2B C1B C6B 119.2(3) . . ? C2B C1B P1 118.7(2) . . ? C6B C1B P1 122.1(3) . . ? C4E C5E C6E 120.3(3) . . ? C3E C4E C5E 120.5(3) . . ? C1E C2E C3E 120.6(3) . . ? C5E C6E C1E 119.3(3) . . ? C4E C3E C2E 119.6(3) . . ? C2E C1E C6E 119.7(3) . . ? C2E C1E P3 118.5(2) . . ? C6E C1E P3 121.7(3) . . ? C5B C4B C3B 119.4(3) . . ? C2B C3B C4B 120.4(3) . . ? O2 P2 C1C 110.46(14) . . ? O2 P2 C1D 110.15(14) . . ? C1C P2 C1D 109.21(15) . . ? O2 P2 C2 112.49(15) . . ? C1C P2 C2 109.08(15) . . ? C1D P2 C2 105.29(15) . . ? C3D C2D C1D 120.3(3) . . ? C1 C2 P2 111.3(2) 4_565 . ? C2D C1D C6D 119.1(3) . . ? C2D C1D P2 119.5(3) . . ? C6D C1D P2 121.2(3) . . ? C5D C4D C3D 119.7(3) . . ? C2C C1C C6C 119.2(3) . . ? C2C C1C P2 124.5(3) . . ? C6C C1C P2 116.3(3) . . ? C5C C6C C1C 120.5(3) . . ? C2D C3D C4D 120.3(3) . . ? C4C C5C C6C 120.1(3) . . ? C5C C4C C3C 119.6(3) . . ? C6D C5D C4D 120.5(3) . . ? C5D C6D C1D 120.2(3) . . ? C3C C2C C1C 120.1(3) . . ? C2C C3C C4C 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.174 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.105