data_sp02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H50 Cl4 N5 O13 P4 Pr' _chemical_formula_weight 1455.64 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 15.197(14) _cell_length_b 16.435(14) _cell_length_c 24.33(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6077(9) _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 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7239 _exptl_absorpt_correction_T_max 0.8024 _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 37297 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 24.99 _reflns_number_total 10645 _reflns_number_gt 8547 _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^)+(0.0513P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.481(15) _refine_ls_number_reflns 10645 _refine_ls_number_parameters 803 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.003 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 0.119530(15) 0.24688(2) 0.08876(4) 0.01544(8) Uani 1 1 d . . . P1 P 0.32934(11) 0.30591(10) 0.17704(8) 0.0167(4) Uani 1 1 d . . . P2 P 0.33021(11) 0.19778(10) -0.00146(8) 0.0165(4) Uani 1 1 d . . . P4 P 0.03266(10) 0.42689(10) 0.18216(8) 0.0163(4) Uani 1 1 d . . . P3 P 0.05284(11) 0.05865(10) -0.00365(8) 0.0191(4) Uani 1 1 d . . . O2 O 0.2510(3) 0.2296(3) 0.0293(2) 0.0191(11) Uani 1 1 d . . . O1 O 0.2532(3) 0.2720(3) 0.1463(2) 0.0197(12) Uani 1 1 d . . . C1A C 0.4238(6) 0.2385(4) 0.1778(4) 0.0191(18) Uani 1 1 d . . . O11 O 0.1456(3) 0.3902(3) 0.0487(2) 0.0257(12) Uani 1 1 d . . . N30 N -0.0812(3) 0.2511(4) 0.0954(5) 0.0338(18) Uani 1 1 d . . . O22 O 0.1397(3) 0.1036(3) 0.1306(2) 0.0317(13) Uani 1 1 d . . . C1B C 0.3053(5) 0.3305(4) 0.2479(3) 0.0215(17) Uani 1 1 d . . . O13 O 0.1249(4) 0.4361(3) -0.0343(2) 0.0491(17) Uani 1 1 d . . . N20 N 0.1260(4) 0.1138(3) 0.1815(3) 0.0242(14) Uani 1 1 d . . . O23 O 0.1302(5) 0.0576(3) 0.2124(3) 0.0579(19) Uani 1 1 d . . . N10 N 0.1231(4) 0.3795(3) -0.0009(3) 0.0237(14) Uani 1 1 d . . . O4 O 0.0644(3) 0.3563(3) 0.1499(2) 0.0230(11) Uani 1 1 d . . . C1D C 0.3075(5) 0.1808(4) -0.0718(3) 0.0190(16) Uani 1 1 d . . . C1C C 0.3679(4) 0.3985(4) 0.1438(3) 0.0181(16) Uani 1 1 d . . . N6C N 0.4231(3) 0.4466(3) 0.1708(2) 0.0159(12) Uani 1 1 d . . . C5C C 0.4507(4) 0.5127(4) 0.1445(3) 0.0161(15) Uani 1 1 d . . . C4C C 0.4252(4) 0.5347(3) 0.0915(4) 0.0228(14) Uani 1 1 d . . . H4CA H 0.4469 0.5828 0.0746 0.027 Uiso 1 1 calc R . . C3C C 0.3681(4) 0.4847(4) 0.0650(3) 0.0270(17) Uani 1 1 d . . . H3CA H 0.3483 0.4979 0.0291 0.032 Uiso 1 1 calc R . . C2C C 0.3388(4) 0.4141(3) 0.0906(3) 0.0229(13) Uani 1 1 d . . . H2CA H 0.3001 0.3776 0.0724 0.027 Uiso 1 1 calc R . . C1F C 0.3637(4) 0.1009(4) 0.0280(3) 0.0161(15) Uani 1 1 d . . . N6F N 0.4360(3) 0.0635(3) 0.0057(2) 0.0181(12) Uani 1 1 d . . . C1J C -0.0185(4) 0.3947(4) 0.2449(3) 0.0212(15) Uani 1 1 d . . . C4B C 0.2632(4) 0.3749(4) 0.3539(3) 0.0205(16) Uani 1 1 d . . . H4BA H 0.2484 0.3943 0.3895 0.025 Uiso 1 1 calc R . . O3 O 0.0768(3) 0.1346(3) 0.02726(19) 0.0200(11) Uani 1 1 d . . . O21 O 0.1103(3) 0.1840(3) 0.1958(2) 0.0343(14) Uani 1 1 d . . . C1I C 0.1170(4) 0.5003(4) 0.1946(3) 0.0198(15) Uani 1 1 d . . . C3A C 0.4799(5) 0.1017(4) 0.1802(3) 0.0357(18) Uani 1 1 d . . . H3AA H 0.4698 0.0447 0.1816 0.043 Uiso 1 1 calc R . . O31 O -0.0403(4) 0.2787(3) 0.0550(2) 0.0326(14) Uani 1 1 d . . . C6G C -0.0079(4) 0.1642(4) -0.0820(3) 0.0282(18) Uani 1 1 d . . . H6GA H -0.0014 0.2030 -0.0533 0.034 Uiso 1 1 calc R . . C5B C 0.3501(5) 0.3662(4) 0.3399(3) 0.0253(17) Uani 1 1 d . . . H5BA H 0.3951 0.3742 0.3665 0.030 Uiso 1 1 calc R . . C6B C 0.3714(5) 0.3453(4) 0.2853(3) 0.0205(17) Uani 1 1 d . . . H6BA H 0.4312 0.3414 0.2743 0.025 Uiso 1 1 calc R . . C6J C -0.0221(4) 0.3097(4) 0.2545(3) 0.0207(15) Uani 1 1 d . . . H6JA H 0.0006 0.2720 0.2285 0.025 Uiso 1 1 calc R . . C4G C -0.0503(5) 0.1311(6) -0.1714(3) 0.048(2) Uani 1 1 d . . . H4GA H -0.0727 0.1466 -0.2063 0.058 Uiso 1 1 calc R . . C3D C 0.3597(5) 0.1458(4) -0.1622(3) 0.0283(18) Uani 1 1 d . . . H3DA H 0.4062 0.1320 -0.1866 0.034 Uiso 1 1 calc R . . C3B C 0.1977(5) 0.3563(4) 0.3179(3) 0.0234(18) Uani 1 1 d . . . H3BA H 0.1383 0.3573 0.3300 0.028 Uiso 1 1 calc R . . C6D C 0.2221(4) 0.1827(4) -0.0905(3) 0.0179(15) Uani 1 1 d . . . H6DA H 0.1758 0.1963 -0.0660 0.021 Uiso 1 1 calc R . . O33 O -0.1602(3) 0.2585(3) 0.1002(4) 0.060(2) Uani 1 1 d . . . C5D C 0.2030(6) 0.1648(4) -0.1449(3) 0.032(2) Uani 1 1 d . . . H5DA H 0.1436 0.1642 -0.1571 0.038 Uiso 1 1 calc R . . O32 O -0.0356(3) 0.2103(3) 0.1289(2) 0.0318(13) Uani 1 1 d . . . C2D C 0.3777(5) 0.1636(4) -0.1087(3) 0.0282(19) Uani 1 1 d . . . H2DA H 0.4369 0.1645 -0.0961 0.034 Uiso 1 1 calc R . . C3J C -0.0916(5) 0.4193(4) 0.3310(3) 0.0359(17) Uani 1 1 d . . . H3JA H -0.1172 0.4562 0.3565 0.043 Uiso 1 1 calc R . . O12 O 0.0960(4) 0.3097(3) -0.0142(2) 0.0354(14) Uani 1 1 d . . . C2A C 0.4085(4) 0.1550(4) 0.1798(3) 0.0305(16) Uani 1 1 d . . . H2AA H 0.3501 0.1346 0.1809 0.037 Uiso 1 1 calc R . . C2B C 0.2159(5) 0.3360(4) 0.2640(3) 0.0257(18) Uani 1 1 d . . . H2BA H 0.1698 0.3261 0.2385 0.031 Uiso 1 1 calc R . . C5G C -0.0390(5) 0.1903(5) -0.1322(3) 0.040(2) Uani 1 1 d . . . H5GA H -0.0519 0.2459 -0.1392 0.048 Uiso 1 1 calc R . . C5J C -0.0605(5) 0.2834(4) 0.3041(3) 0.0305(18) Uani 1 1 d . . . H5JA H -0.0643 0.2267 0.3114 0.037 Uiso 1 1 calc R . . C2I C 0.1390(4) 0.5314(4) 0.2462(3) 0.0298(16) Uani 1 1 d . . . H2IA H 0.1108 0.5108 0.2782 0.036 Uiso 1 1 calc R . . C3I C 0.2023(5) 0.5928(4) 0.2512(3) 0.0370(18) Uani 1 1 d . . . H3IA H 0.2154 0.6138 0.2866 0.044 Uiso 1 1 calc R . . C6I C 0.1611(4) 0.5323(4) 0.1491(3) 0.0255(15) Uani 1 1 d . . . H6IA H 0.1477 0.5116 0.1137 0.031 Uiso 1 1 calc R . . C2J C -0.0542(4) 0.4491(4) 0.2833(3) 0.0259(15) Uani 1 1 d . . . H2JA H -0.0525 0.5060 0.2766 0.031 Uiso 1 1 calc R . . C4I C 0.2464(5) 0.6239(4) 0.2059(4) 0.041(2) Uani 1 1 d . . . H4IA H 0.2903 0.6646 0.2096 0.050 Uiso 1 1 calc R . . C6A C 0.5106(4) 0.2661(4) 0.1787(3) 0.0253(14) Uani 1 1 d . . . H6AA H 0.5224 0.3229 0.1795 0.030 Uiso 1 1 calc R . . C4A C 0.5642(5) 0.1303(4) 0.1786(3) 0.0264(16) Uani 1 1 d . . . H4AA H 0.6119 0.0929 0.1774 0.032 Uiso 1 1 calc R . . C6E C 0.4268(4) 0.3310(4) -0.0334(3) 0.0235(15) Uani 1 1 d . . . H6EA H 0.3820 0.3381 -0.0602 0.028 Uiso 1 1 calc R . . C4H C 0.2655(6) -0.1369(5) -0.0115(5) 0.058(3) Uani 1 1 d . . . H4HA H 0.3083 -0.1789 -0.0134 0.069 Uiso 1 1 calc R . . C2E C 0.4890(4) 0.2567(4) 0.0414(3) 0.0262(14) Uani 1 1 d . . . H2EA H 0.4865 0.2120 0.0660 0.031 Uiso 1 1 calc R . . C5F C 0.4605(4) -0.0080(4) 0.0286(3) 0.0153(15) Uani 1 1 d . . . C1H C 0.1364(4) -0.0170(4) -0.0083(3) 0.0248(17) Uani 1 1 d . . . C5H C 0.2630(5) -0.0798(4) -0.0515(4) 0.047(2) Uani 1 1 d . . . H5HA H 0.3050 -0.0807 -0.0804 0.056 Uiso 1 1 calc R . . C6H C 0.1980(4) -0.0195(4) -0.0501(3) 0.0365(18) Uani 1 1 d . . . H6HA H 0.1963 0.0204 -0.0783 0.044 Uiso 1 1 calc R . . C2H C 0.1435(4) -0.0752(4) 0.0327(3) 0.0364(18) Uani 1 1 d . . . H2HA H 0.1033 -0.0741 0.0626 0.044 Uiso 1 1 calc R . . C1E C 0.4239(5) 0.2661(4) 0.0006(4) 0.0205(18) Uani 1 1 d . . . C5A C 0.5806(4) 0.2106(4) 0.1785(3) 0.0268(14) Uani 1 1 d . . . H5AA H 0.6395 0.2297 0.1784 0.032 Uiso 1 1 calc R . . C5I C 0.2228(4) 0.5921(4) 0.1539(3) 0.0332(18) Uani 1 1 d . . . H5IA H 0.2504 0.6128 0.1218 0.040 Uiso 1 1 calc R . . C4D C 0.2712(5) 0.1477(4) -0.1816(3) 0.0269(19) Uani 1 1 d . . . H4DA H 0.2587 0.1375 -0.2192 0.032 Uiso 1 1 calc R . . C4J C -0.0925(4) 0.3372(4) 0.3422(3) 0.0309(17) Uani 1 1 d . . . H4JA H -0.1152 0.3179 0.3761 0.037 Uiso 1 1 calc R . . C1G C 0.0139(4) 0.0859(4) -0.0718(3) 0.0244(16) Uani 1 1 d . . . C3H C 0.2081(5) -0.1354(5) 0.0313(4) 0.048(2) Uani 1 1 d . . . H3HA H 0.2119 -0.1747 0.0598 0.058 Uiso 1 1 calc R . . C2G C 0.0024(5) 0.0274(4) -0.1134(3) 0.0389(18) Uani 1 1 d . . . H2GA H 0.0177 -0.0279 -0.1072 0.047 Uiso 1 1 calc R . . C3G C -0.0310(6) 0.0515(5) -0.1625(3) 0.057(3) Uani 1 1 d . . . H3GA H -0.0408 0.0127 -0.1908 0.068 Uiso 1 1 calc R . . C3E C 0.5573(5) 0.3136(4) 0.0455(3) 0.0349(16) Uani 1 1 d . . . H3EA H 0.6024 0.3070 0.0721 0.042 Uiso 1 1 calc R . . C2F C 0.3154(4) 0.0673(4) 0.0697(3) 0.0292(19) Uani 1 1 d . . . H2FA H 0.2642 0.0940 0.0829 0.035 Uiso 1 1 calc R . . C3F C 0.3417(4) -0.0049(3) 0.0922(3) 0.0271(15) Uani 1 1 d . . . H3FA H 0.3086 -0.0292 0.1210 0.033 Uiso 1 1 calc R . . C4F C 0.4174(5) -0.0427(4) 0.0725(3) 0.027(2) Uani 1 1 d . . . H4FA H 0.4388 -0.0913 0.0889 0.032 Uiso 1 1 calc R . . C5E C 0.4944(5) 0.3876(4) -0.0297(3) 0.0309(18) Uani 1 1 d . . . H5EA H 0.4964 0.4319 -0.0547 0.037 Uiso 1 1 calc R . . C4E C 0.5582(5) 0.3803(4) 0.0097(4) 0.036(2) Uani 1 1 d . . . H4EA H 0.6030 0.4204 0.0127 0.044 Uiso 1 1 calc R . . C100 C 0.3796(14) 0.6286(9) -0.0614(5) 0.193(11) Uani 1 1 d . . . H10A H 0.3917 0.6864 -0.0699 0.232 Uiso 1 1 calc R . . H10B H 0.4174 0.6137 -0.0298 0.232 Uiso 1 1 calc R . . Cl10 Cl 0.2756(3) 0.6229(3) -0.04014(16) 0.160(2) Uani 1 1 d . . . Cl11 Cl 0.41237(18) 0.57643(17) -0.11283(12) 0.0834(8) Uani 1 1 d . . . C200 C 0.1843(14) -0.0419(11) -0.2449(8) 0.053(5) Uiso 0.469(6) 1 d P A 1 H20A H 0.1479 0.0073 -0.2390 0.064 Uiso 0.469(6) 1 calc PR A 1 H20B H 0.2395 -0.0254 -0.2635 0.064 Uiso 0.469(6) 1 calc PR A 1 Cl20 Cl 0.1292(6) -0.1099(4) -0.2839(3) 0.085(3) Uani 0.469(6) 1 d P A 1 Cl21 Cl 0.2096(4) -0.0909(4) -0.1781(2) 0.088(2) Uani 0.469(6) 1 d P A 1 C300 C 0.2263(11) -0.0835(10) -0.2374(7) 0.055(4) Uiso 0.531(6) 1 d P A 2 H30A H 0.2673 -0.0414 -0.2513 0.066 Uiso 0.531(6) 1 calc PR A 2 H30B H 0.2567 -0.1153 -0.2086 0.066 Uiso 0.531(6) 1 calc PR A 2 Cl30 Cl 0.1342(4) -0.0387(3) -0.2109(3) 0.093(2) Uani 0.531(6) 1 d P A 2 Cl31 Cl 0.1946(4) -0.1457(3) -0.2897(2) 0.0598(16) Uani 0.531(6) 1 d P 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 Pr1 0.01423(12) 0.01426(13) 0.01782(13) -0.00288(14) 0.0000(2) 0.00034(16) P1 0.0173(10) 0.0177(9) 0.0150(11) -0.0001(8) 0.0001(8) -0.0025(7) P2 0.0164(9) 0.0155(9) 0.0175(11) 0.0001(8) 0.0009(8) 0.0035(7) P4 0.0188(8) 0.0142(8) 0.0158(9) 0.0006(7) 0.0004(7) 0.0014(6) P3 0.0203(9) 0.0182(8) 0.0188(10) -0.0025(7) 0.0040(8) -0.0075(7) O2 0.018(3) 0.028(2) 0.011(3) -0.008(2) 0.006(2) -0.003(2) O1 0.021(3) 0.019(2) 0.020(3) 0.001(2) 0.005(2) -0.010(2) C1A 0.029(5) 0.012(3) 0.017(5) -0.007(3) 0.001(4) -0.001(3) O11 0.035(3) 0.024(3) 0.019(3) -0.002(2) -0.011(2) 0.000(2) N30 0.025(3) 0.026(3) 0.051(6) -0.022(3) -0.003(4) -0.001(3) O22 0.040(3) 0.030(3) 0.025(3) 0.001(2) 0.004(3) 0.003(2) C1B 0.034(4) 0.009(3) 0.021(4) -0.002(3) 0.008(3) -0.001(3) O13 0.106(5) 0.030(3) 0.012(3) 0.002(2) 0.004(3) 0.012(3) N20 0.038(4) 0.020(3) 0.014(4) -0.004(3) 0.005(3) -0.005(3) O23 0.114(6) 0.020(3) 0.040(4) 0.008(3) -0.015(4) -0.015(3) N10 0.030(3) 0.014(3) 0.027(4) 0.002(3) 0.011(3) 0.009(3) O4 0.026(3) 0.022(2) 0.021(3) -0.002(2) -0.002(2) 0.003(2) C1D 0.030(4) 0.014(3) 0.013(4) 0.005(3) 0.007(3) 0.004(3) C1C 0.014(4) 0.017(3) 0.023(4) -0.002(3) 0.006(3) 0.003(3) N6C 0.013(3) 0.012(2) 0.023(3) -0.001(2) 0.001(2) 0.001(2) C5C 0.015(3) 0.014(3) 0.019(4) -0.001(3) 0.000(3) 0.000(3) C4C 0.025(3) 0.018(3) 0.026(4) 0.007(4) -0.001(4) 0.004(2) C3C 0.039(4) 0.027(4) 0.015(3) 0.006(3) -0.003(3) -0.009(3) C2C 0.019(3) 0.023(3) 0.026(4) 0.006(4) -0.002(4) -0.002(2) C1F 0.017(4) 0.017(3) 0.015(4) 0.000(3) -0.004(3) -0.002(3) N6F 0.021(3) 0.022(3) 0.012(3) -0.001(2) -0.004(2) 0.005(2) C1J 0.015(3) 0.035(4) 0.014(3) 0.003(3) -0.007(3) 0.003(3) C4B 0.031(4) 0.016(3) 0.015(4) -0.003(3) 0.000(3) -0.001(3) O3 0.024(3) 0.018(2) 0.019(3) 0.002(2) -0.003(2) -0.012(2) O21 0.040(3) 0.034(3) 0.029(3) -0.015(2) 0.012(2) -0.005(2) C1I 0.012(3) 0.019(3) 0.028(4) 0.001(3) 0.002(3) 0.007(3) C3A 0.059(5) 0.015(3) 0.033(4) 0.000(3) -0.002(4) 0.002(3) O31 0.030(3) 0.035(3) 0.032(4) -0.018(3) -0.012(3) 0.007(3) C6G 0.026(4) 0.036(4) 0.023(4) -0.012(3) 0.002(3) -0.006(3) C5B 0.028(4) 0.027(4) 0.021(5) -0.002(3) -0.014(3) -0.008(3) C6B 0.019(4) 0.025(4) 0.018(4) 0.009(3) 0.001(3) -0.010(3) C6J 0.026(4) 0.014(3) 0.022(4) -0.007(3) -0.001(3) 0.000(3) C4G 0.052(5) 0.070(6) 0.023(4) 0.010(4) -0.009(4) -0.023(5) C3D 0.037(4) 0.029(4) 0.020(5) -0.003(3) -0.003(4) 0.009(3) C3B 0.020(4) 0.031(4) 0.020(4) -0.008(3) 0.006(3) 0.001(3) C6D 0.027(4) 0.015(3) 0.012(4) -0.010(3) 0.004(3) -0.007(3) O33 0.016(2) 0.056(3) 0.109(7) -0.027(3) 0.002(3) 0.008(3) C5D 0.035(5) 0.031(4) 0.029(5) 0.003(3) -0.008(4) 0.002(4) O32 0.030(3) 0.027(3) 0.039(4) -0.005(3) 0.009(3) -0.003(2) C2D 0.028(4) 0.024(4) 0.033(5) -0.006(3) -0.004(4) 0.009(3) C3J 0.045(4) 0.038(4) 0.024(4) 0.004(3) 0.002(3) 0.014(3) O12 0.050(3) 0.015(3) 0.041(4) -0.008(2) -0.015(3) 0.005(2) C2A 0.027(4) 0.021(3) 0.043(5) 0.003(3) 0.001(3) 0.005(3) C2B 0.024(4) 0.014(3) 0.039(5) 0.008(3) -0.005(3) -0.002(3) C5G 0.038(5) 0.047(5) 0.035(5) 0.009(4) -0.013(4) -0.001(4) C5J 0.030(4) 0.029(4) 0.033(4) 0.002(3) -0.002(3) -0.007(3) C2I 0.035(4) 0.018(3) 0.037(4) -0.004(3) -0.012(3) -0.003(3) C3I 0.044(4) 0.027(4) 0.040(5) -0.006(3) -0.018(4) 0.003(3) C6I 0.020(3) 0.019(3) 0.038(4) -0.004(3) 0.001(3) 0.001(3) C2J 0.036(4) 0.022(3) 0.020(4) 0.004(3) -0.005(3) 0.012(3) C4I 0.039(5) 0.011(4) 0.074(7) 0.009(4) -0.014(5) 0.013(3) C6A 0.025(3) 0.021(3) 0.030(4) 0.003(3) 0.002(3) 0.001(3) C4A 0.026(4) 0.031(4) 0.022(4) -0.001(3) 0.007(3) 0.009(3) C6E 0.028(4) 0.028(4) 0.015(3) 0.004(3) -0.004(3) -0.001(3) C4H 0.037(5) 0.030(5) 0.107(9) -0.020(5) 0.016(5) 0.000(4) C2E 0.033(4) 0.025(3) 0.021(4) 0.003(3) 0.002(3) -0.007(3) C5F 0.014(3) 0.015(3) 0.017(4) 0.000(3) 0.003(3) -0.002(3) C1H 0.024(4) 0.013(3) 0.037(5) -0.008(3) -0.004(3) -0.005(3) C5H 0.040(5) 0.026(4) 0.076(7) -0.016(4) 0.027(4) 0.002(3) C6H 0.041(4) 0.019(3) 0.050(5) -0.001(3) 0.023(4) 0.000(3) C2H 0.017(4) 0.038(4) 0.054(5) -0.001(4) 0.003(3) -0.004(3) C1E 0.010(4) 0.026(4) 0.025(5) 0.004(4) 0.005(4) 0.000(3) C5A 0.027(3) 0.030(4) 0.023(4) 0.001(3) -0.002(3) 0.004(3) C5I 0.024(4) 0.026(4) 0.049(5) -0.002(3) 0.010(3) 0.001(3) C4D 0.048(5) 0.012(3) 0.021(4) 0.000(3) -0.006(3) 0.000(3) C4J 0.036(4) 0.037(4) 0.020(4) 0.003(3) 0.010(3) -0.001(3) C1G 0.026(4) 0.028(4) 0.019(4) -0.002(3) 0.006(3) -0.019(3) C3H 0.019(4) 0.043(5) 0.083(7) 0.010(4) -0.003(4) -0.001(3) C2G 0.064(5) 0.038(4) 0.015(4) 0.001(3) 0.000(4) -0.027(4) C3G 0.098(7) 0.058(6) 0.014(4) -0.007(4) 0.001(4) -0.048(5) C3E 0.040(4) 0.029(4) 0.036(4) -0.008(3) -0.005(3) -0.004(3) C2F 0.019(3) 0.025(4) 0.044(5) 0.005(3) 0.017(3) 0.004(3) C3F 0.029(3) 0.029(3) 0.024(4) 0.012(4) 0.012(4) 0.001(3) C4F 0.028(4) 0.010(3) 0.043(6) 0.002(3) -0.004(3) 0.010(3) C5E 0.051(5) 0.027(4) 0.015(4) 0.005(3) 0.012(3) -0.011(3) C4E 0.037(5) 0.023(4) 0.049(6) -0.008(4) 0.010(4) -0.012(3) C100 0.37(3) 0.154(14) 0.056(9) -0.013(9) 0.005(12) -0.197(17) Cl10 0.146(4) 0.246(5) 0.087(3) 0.079(3) 0.034(2) 0.126(4) Cl11 0.0805(18) 0.086(2) 0.084(2) -0.0076(16) 0.0089(16) 0.0160(15) Cl20 0.134(7) 0.067(4) 0.055(4) 0.011(3) -0.027(4) -0.020(4) Cl21 0.096(5) 0.109(5) 0.060(4) -0.027(3) -0.027(3) -0.004(4) Cl30 0.069(4) 0.067(4) 0.143(6) 0.006(3) 0.023(4) 0.007(3) Cl31 0.094(4) 0.030(2) 0.055(3) -0.0039(19) 0.010(3) -0.004(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 O3 2.463(5) . ? Pr1 O4 2.479(5) . ? Pr1 O2 2.484(5) . ? Pr1 O1 2.500(5) . ? Pr1 O11 2.579(5) . ? Pr1 O22 2.584(5) . ? Pr1 O31 2.617(6) . ? Pr1 O32 2.622(6) . ? Pr1 O12 2.735(6) . ? Pr1 O21 2.806(6) . ? P1 O1 1.487(5) . ? P1 C1B 1.808(8) . ? P1 C1A 1.813(8) . ? P1 C1C 1.821(7) . ? P2 O2 1.510(5) . ? P2 C1D 1.769(8) . ? P2 C1E 1.813(8) . ? P2 C1F 1.819(7) . ? P4 O4 1.482(5) . ? P4 C1I 1.786(6) . ? P4 C1J 1.793(7) . ? P4 C5C 1.838(7) 3_465 ? P3 O3 1.502(5) . ? P3 C1H 1.781(7) . ? P3 C5F 1.810(7) 3_455 ? P3 C1G 1.816(7) . ? C1A C2A 1.393(8) . ? C1A C6A 1.395(10) . ? O11 N10 1.267(7) . ? N30 O33 1.212(7) . ? N30 O31 1.249(11) . ? N30 O32 1.263(10) . ? O22 N20 1.265(7) . ? C1B C6B 1.376(10) . ? C1B C2B 1.417(9) . ? O13 N10 1.236(8) . ? N20 O23 1.194(8) . ? N20 O21 1.229(7) . ? N10 O12 1.261(7) . ? C1D C6D 1.376(9) . ? C1D C2D 1.423(9) . ? C1C N6C 1.327(8) . ? C1C C2C 1.390(10) . ? N6C C5C 1.328(8) . ? C5C C4C 1.394(10) . ? C5C P4 1.838(7) 3_565 ? C4C C3C 1.357(9) . ? C3C C2C 1.391(8) . ? C1F C2F 1.368(9) . ? C1F N6F 1.371(8) . ? N6F C5F 1.352(8) . ? C1J C2J 1.403(9) . ? C1J C6J 1.416(9) . ? C4B C3B 1.360(9) . ? C4B C5B 1.371(10) . ? C1I C2I 1.396(9) . ? C1I C6I 1.397(9) . ? C3A C4A 1.365(9) . ? C3A C2A 1.394(9) . ? C6G C1G 1.352(9) . ? C6G C5G 1.378(10) . ? C5B C6B 1.410(10) . ? C6J C5J 1.409(10) . ? C4G C3G 1.358(11) . ? C4G C5G 1.374(11) . ? C3D C2D 1.361(10) . ? C3D C4D 1.426(10) . ? C3B C2B 1.381(10) . ? C6D C5D 1.385(10) . ? C5D C4D 1.397(10) . ? C3J C4J 1.378(9) . ? C3J C2J 1.380(9) . ? C5J C4J 1.368(10) . ? C2I C3I 1.399(9) . ? C3I C4I 1.386(11) . ? C6I C5I 1.364(9) . ? C4I C5I 1.415(10) . ? C6A C5A 1.401(8) . ? C4A C5A 1.343(9) . ? C6E C1E 1.352(9) . ? C6E C5E 1.388(9) . ? C4H C5H 1.353(12) . ? C4H C3H 1.359(12) . ? C2E C3E 1.400(8) . ? C2E C1E 1.410(10) . ? C5F C4F 1.377(9) . ? C5F P3 1.810(7) 3 ? C1H C6H 1.383(9) . ? C1H C2H 1.387(10) . ? C5H C6H 1.399(9) . ? C2H C3H 1.393(9) . ? C1G C2G 1.407(9) . ? C2G C3G 1.359(10) . ? C3E C4E 1.400(10) . ? C2F C3F 1.367(8) . ? C3F C4F 1.394(9) . ? C5E C4E 1.368(10) . ? C100 Cl11 1.596(17) . ? C100 Cl10 1.67(2) . ? C200 Cl20 1.688(18) . ? C200 Cl21 1.85(2) . ? C300 Cl31 1.702(17) . ? C300 Cl30 1.707(17) . ? 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 O3 Pr1 O4 144.95(12) . . ? O3 Pr1 O2 76.85(16) . . ? O4 Pr1 O2 134.78(16) . . ? O3 Pr1 O1 132.68(16) . . ? O4 Pr1 O1 79.58(16) . . ? O2 Pr1 O1 72.05(12) . . ? O3 Pr1 O11 119.68(16) . . ? O4 Pr1 O11 67.43(17) . . ? O2 Pr1 O11 76.14(17) . . ? O1 Pr1 O11 86.32(16) . . ? O3 Pr1 O22 65.67(18) . . ? O4 Pr1 O22 117.68(17) . . ? O2 Pr1 O22 91.75(17) . . ? O1 Pr1 O22 80.42(17) . . ? O11 Pr1 O22 164.33(12) . . ? O3 Pr1 O31 73.38(16) . . ? O4 Pr1 O31 74.33(16) . . ? O2 Pr1 O31 125.90(18) . . ? O1 Pr1 O31 153.72(15) . . ? O11 Pr1 O31 80.88(17) . . ? O22 Pr1 O31 114.57(18) . . ? O3 Pr1 O32 79.49(16) . . ? O4 Pr1 O32 68.83(16) . . ? O2 Pr1 O32 156.13(15) . . ? O1 Pr1 O32 124.01(19) . . ? O11 Pr1 O32 119.23(17) . . ? O22 Pr1 O32 75.55(17) . . ? O31 Pr1 O32 47.82(16) . . ? O3 Pr1 O12 72.03(15) . . ? O4 Pr1 O12 103.39(16) . . ? O2 Pr1 O12 67.31(17) . . ? O1 Pr1 O12 123.86(16) . . ? O11 Pr1 O12 47.87(15) . . ? O22 Pr1 O12 136.15(16) . . ? O31 Pr1 O12 60.98(18) . . ? O32 Pr1 O12 108.09(18) . . ? O3 Pr1 O21 105.97(16) . . ? O4 Pr1 O21 72.14(16) . . ? O2 Pr1 O21 122.63(16) . . ? O1 Pr1 O21 65.26(16) . . ? O11 Pr1 O21 133.98(15) . . ? O22 Pr1 O21 45.92(15) . . ? O31 Pr1 O21 108.60(17) . . ? O32 Pr1 O21 61.61(17) . . ? O12 Pr1 O21 169.59(12) . . ? O1 P1 C1B 114.0(3) . . ? O1 P1 C1A 113.1(3) . . ? C1B P1 C1A 106.7(4) . . ? O1 P1 C1C 109.9(3) . . ? C1B P1 C1C 107.6(3) . . ? C1A P1 C1C 105.1(3) . . ? O2 P2 C1D 112.2(3) . . ? O2 P2 C1E 113.4(3) . . ? C1D P2 C1E 106.1(4) . . ? O2 P2 C1F 109.3(3) . . ? C1D P2 C1F 107.4(3) . . ? C1E P2 C1F 108.2(3) . . ? O4 P4 C1I 112.7(3) . . ? O4 P4 C1J 111.2(3) . . ? C1I P4 C1J 111.5(3) . . ? O4 P4 C5C 112.3(3) . 3_465 ? C1I P4 C5C 101.9(3) . 3_465 ? C1J P4 C5C 106.9(3) . 3_465 ? O3 P3 C1H 116.1(3) . . ? O3 P3 C5F 110.7(3) . 3_455 ? C1H P3 C5F 105.0(3) . 3_455 ? O3 P3 C1G 109.3(3) . . ? C1H P3 C1G 110.3(3) . . ? C5F P3 C1G 104.9(3) 3_455 . ? P2 O2 Pr1 165.7(3) . . ? P1 O1 Pr1 167.4(3) . . ? C2A C1A C6A 118.5(7) . . ? C2A C1A P1 118.1(6) . . ? C6A C1A P1 123.4(5) . . ? N10 O11 Pr1 101.0(3) . . ? O33 N30 O31 122.2(9) . . ? O33 N30 O32 122.2(9) . . ? O31 N30 O32 115.4(5) . . ? N20 O22 Pr1 104.2(4) . . ? C6B C1B C2B 120.4(7) . . ? C6B C1B P1 121.5(5) . . ? C2B C1B P1 118.1(6) . . ? O23 N20 O21 123.9(7) . . ? O23 N20 O22 120.3(6) . . ? O21 N20 O22 115.8(6) . . ? O13 N10 O12 121.4(7) . . ? O13 N10 O11 121.1(6) . . ? O12 N10 O11 117.4(6) . . ? P4 O4 Pr1 174.7(3) . . ? C6D C1D C2D 120.2(7) . . ? C6D C1D P2 120.1(5) . . ? C2D C1D P2 119.7(6) . . ? N6C C1C C2C 123.5(6) . . ? N6C C1C P1 118.8(5) . . ? C2C C1C P1 117.7(5) . . ? C1C N6C C5C 116.6(6) . . ? N6C C5C C4C 124.8(6) . . ? N6C C5C P4 114.5(5) . 3_565 ? C4C C5C P4 120.6(5) . 3_565 ? C3C C4C C5C 117.3(6) . . ? C4C C3C C2C 119.9(6) . . ? C3C C2C C1C 117.9(6) . . ? C2F C1F N6F 122.9(6) . . ? C2F C1F P2 119.7(5) . . ? N6F C1F P2 117.4(5) . . ? C5F N6F C1F 116.6(6) . . ? C2J C1J C6J 120.2(6) . . ? C2J C1J P4 123.2(5) . . ? C6J C1J P4 116.6(5) . . ? C3B C4B C5B 121.4(7) . . ? P3 O3 Pr1 172.2(3) . . ? N20 O21 Pr1 94.1(4) . . ? C2I C1I C6I 117.3(6) . . ? C2I C1I P4 124.9(5) . . ? C6I C1I P4 117.6(5) . . ? C4A C3A C2A 121.0(6) . . ? N30 O31 Pr1 98.2(5) . . ? C1G C6G C5G 122.9(7) . . ? C4B C5B C6B 118.7(6) . . ? C1B C6B C5B 119.9(7) . . ? C5J C6J C1J 117.4(6) . . ? C3G C4G C5G 123.0(7) . . ? C2D C3D C4D 120.1(7) . . ? C4B C3B C2B 121.3(7) . . ? C1D C6D C5D 120.6(7) . . ? C6D C5D C4D 119.9(7) . . ? N30 O32 Pr1 97.5(5) . . ? C3D C2D C1D 119.7(7) . . ? C4J C3J C2J 121.1(6) . . ? N10 O12 Pr1 93.6(4) . . ? C1A C2A C3A 119.3(7) . . ? C3B C2B C1B 118.0(7) . . ? C4G C5G C6G 116.0(8) . . ? C4J C5J C6J 121.9(7) . . ? C1I C2I C3I 120.4(7) . . ? C4I C3I C2I 122.0(7) . . ? C5I C6I C1I 122.3(7) . . ? C3J C2J C1J 119.6(6) . . ? C3I C4I C5I 116.8(7) . . ? C1A C6A C5A 120.4(6) . . ? C5A C4A C3A 120.7(6) . . ? C1E C6E C5E 120.9(7) . . ? C5H C4H C3H 121.4(8) . . ? C3E C2E C1E 119.9(6) . . ? N6F C5F C4F 123.3(6) . . ? N6F C5F P3 115.8(5) . 3 ? C4F C5F P3 120.9(5) . 3 ? C6H C1H C2H 117.1(6) . . ? C6H C1H P3 123.4(6) . . ? C2H C1H P3 119.4(6) . . ? C4H C5H C6H 119.6(7) . . ? C1H C6H C5H 121.1(7) . . ? C1H C2H C3H 121.8(7) . . ? C6E C1E C2E 119.6(7) . . ? C6E C1E P2 119.9(6) . . ? C2E C1E P2 120.2(6) . . ? C4A C5A C6A 120.0(6) . . ? C6I C5I C4I 121.1(7) . . ? C5D C4D C3D 119.5(7) . . ? C5J C4J C3J 119.7(7) . . ? C6G C1G C2G 119.2(7) . . ? C6G C1G P3 118.8(5) . . ? C2G C1G P3 121.9(5) . . ? C4H C3H C2H 118.9(8) . . ? C3G C2G C1G 118.7(7) . . ? C4G C3G C2G 120.1(7) . . ? C2E C3E C4E 119.1(7) . . ? C1F C2F C3F 119.4(6) . . ? C2F C3F C4F 119.3(6) . . ? C5F C4F C3F 118.4(6) . . ? C4E C5E C6E 120.8(6) . . ? C5E C4E C3E 119.8(7) . . ? Cl11 C100 Cl10 120.7(8) . . ? Cl20 C200 Cl21 107.9(10) . . ? Cl31 C300 Cl30 108.1(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.445 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.094