data_03hur995 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H36 F12 N2 O8 P2' _chemical_formula_weight 746.47 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' 'F' 'F' 0.0171 0.0103 '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 P2(1)/c _symmetry_space_group_name_hall '-P 2ybc' 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 13.958(3) _cell_length_b 7.2460(13) _cell_length_c 32.562(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.70(2) _cell_angle_gamma 90.00 _cell_volume 3255.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Delft instruments FAST area detector' _diffrn_measurement_method 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)' _diffrn_standards_number 'None' _diffrn_standards_interval_count 'N/A' _diffrn_standards_interval_time 'N/A' _diffrn_standards_decay_% 'N/A' _diffrn_reflns_number 4742 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.88 _reflns_number_total 4742 _reflns_number_gt 3119 _reflns_threshold_expression >2\s(I) _computing_data_collection 'MADNES (Pflugrath & Messerschmidt, 1989)' _computing_cell_refinement REFINE _computing_data_reduction 'ABSURD (Karaulov, 1992)' _computing_structure_solution 'SIR2004 (Cascarano, Giacovazzo &et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^ > 2\s(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^)+(0.0811P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 4742 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _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 0.31404(7) -0.50499(13) 0.18341(3) 0.0299(3) Uani 1 1 d . . . P2 P -0.20949(7) -0.14590(15) 0.07174(3) 0.0366(3) Uani 1 1 d . . . O4 O 0.10747(17) -0.2933(3) 0.06258(7) 0.0300(6) Uani 1 1 d . . . O2 O 0.07085(16) -0.1047(3) 0.17784(7) 0.0282(6) Uani 1 1 d . . . O3 O 0.08523(17) -0.5938(3) 0.03635(7) 0.0328(6) Uani 1 1 d . . . F1 F -0.31703(19) -0.1758(5) 0.07708(12) 0.1012(12) Uani 1 1 d . . . F2 F -0.2307(2) 0.0567(5) 0.05497(12) 0.1183(15) Uani 1 1 d . . . F3 F -0.1004(2) -0.1155(4) 0.06856(16) 0.1314(19) Uani 1 1 d . . . F4 F -0.1824(2) -0.3381(4) 0.09288(12) 0.0923(12) Uani 1 1 d . . . F5 F -0.2230(4) -0.2253(9) 0.02862(13) 0.201(3) Uani 1 1 d . . . F6 F -0.1976(3) -0.0588(5) 0.11647(11) 0.1208(15) Uani 1 1 d . . . F7 F 0.26228(16) -0.4798(3) 0.22389(7) 0.0502(6) Uani 1 1 d . . . F8 F 0.36536(17) -0.5300(3) 0.14320(7) 0.0526(7) Uani 1 1 d . . . F9 F 0.22160(17) -0.6147(4) 0.16166(8) 0.0619(8) Uani 1 1 d . . . F10 F 0.40451(16) -0.3917(3) 0.20548(8) 0.0595(7) Uani 1 1 d . . . F11 F 0.36171(18) -0.6914(3) 0.20234(8) 0.0573(7) Uani 1 1 d . . . F12 F 0.26517(17) -0.3187(3) 0.16459(8) 0.0565(7) Uani 1 1 d . . . O1 O -0.00964(16) -0.2413(3) 0.22863(7) 0.0289(6) Uani 1 1 d . . . O8 O 0.70169(17) -0.4759(4) 0.20250(8) 0.0414(7) Uani 1 1 d . . . O5 O 0.35035(19) 0.0034(4) 0.06116(9) 0.0499(8) Uani 1 1 d . . . O6 O 0.42580(19) -0.2815(4) 0.05299(8) 0.0442(7) Uani 1 1 d . . . O7 O 0.62029(17) -0.5670(3) 0.13712(8) 0.0391(7) Uani 1 1 d . . . N1 N 0.03874(19) -0.3816(4) 0.12879(8) 0.0211(6) Uani 1 1 d . . . H1 H 0.0681 -0.2780 0.1240 0.025 Uiso 1 1 calc R . . N2 N 0.5228(2) -0.2690(4) 0.12603(9) 0.0288(7) Uani 1 1 d . . . H2 H 0.5259 -0.3539 0.1070 0.035 Uiso 1 1 calc R . . C1 C 0.0188(2) -0.5011(5) 0.09735(10) 0.0236(8) Uani 1 1 d . . . C9 C 0.0452(2) -0.4459(4) 0.05551(10) 0.0256(8) Uani 1 1 d . . . H9 H -0.0152 -0.4058 0.0372 0.031 Uiso 1 1 calc R . . C6 C 0.0538(3) -0.2651(5) 0.19970(11) 0.0267(8) Uani 1 1 d . . . H6 H 0.1173 -0.3089 0.2149 0.032 Uiso 1 1 calc R . . C2 C 0.0172(2) -0.4088(5) 0.16688(10) 0.0232(8) Uani 1 1 d . . . C3 C -0.0282(2) -0.5703(5) 0.17505(11) 0.0283(8) Uani 1 1 d . . . H3 H -0.0442 -0.5936 0.2019 0.034 Uiso 1 1 calc R . . C20 C 0.6657(3) -0.4232(5) 0.16160(12) 0.0341(9) Uani 1 1 d . . . H20 H 0.7207 -0.3756 0.1482 0.041 Uiso 1 1 calc R . . C13 C 0.5905(2) -0.2735(5) 0.16041(11) 0.0283(9) Uani 1 1 d . . . C12 C 0.4509(3) -0.1438(5) 0.11892(12) 0.0310(9) Uani 1 1 d . . . C5 C -0.0268(2) -0.6649(5) 0.10420(11) 0.0286(9) Uani 1 1 d . . . H5 H -0.0419 -0.7528 0.0825 0.034 Uiso 1 1 calc R . . C4 C -0.0501(3) -0.6980(5) 0.14353(12) 0.0322(9) Uani 1 1 d . . . H4 H -0.0815 -0.8099 0.1488 0.039 Uiso 1 1 calc R . . C16 C 0.4458(3) -0.0104(6) 0.14806(13) 0.0418(10) Uani 1 1 d . . . H16 H 0.3958 0.0796 0.1441 0.050 Uiso 1 1 calc R . . C11 C 0.1106(3) -0.1861(5) 0.02544(12) 0.0392(10) Uani 1 1 d . . . H11A H 0.1300 -0.2656 0.0038 0.059 Uiso 1 1 calc R . . H11B H 0.1578 -0.0858 0.0316 0.059 Uiso 1 1 calc R . . H11C H 0.0464 -0.1340 0.0158 0.059 Uiso 1 1 calc R . . C15 C 0.5134(3) -0.0079(5) 0.18305(14) 0.0441(11) Uani 1 1 d . . . H15 H 0.5102 0.0856 0.2033 0.053 Uiso 1 1 calc R . . C10 C 0.1720(3) -0.6716(6) 0.05989(13) 0.0427(10) Uani 1 1 d . . . H10A H 0.2131 -0.5720 0.0731 0.064 Uiso 1 1 calc R . . H10B H 0.2076 -0.7411 0.0412 0.064 Uiso 1 1 calc R . . H10C H 0.1542 -0.7545 0.0813 0.064 Uiso 1 1 calc R . . C7 C -0.0993(3) -0.1525(5) 0.21216(12) 0.0360(9) Uani 1 1 d . . . H7A H -0.0878 -0.0206 0.2084 0.054 Uiso 1 1 calc R . . H7B H -0.1460 -0.1684 0.2315 0.054 Uiso 1 1 calc R . . H7C H -0.1253 -0.2079 0.1853 0.054 Uiso 1 1 calc R . . C8 C 0.1382(3) 0.0196(6) 0.20225(13) 0.0448(11) Uani 1 1 d . . . H8A H 0.1088 0.0679 0.2255 0.067 Uiso 1 1 calc R . . H8B H 0.1536 0.1222 0.1847 0.067 Uiso 1 1 calc R . . H8C H 0.1978 -0.0472 0.2130 0.067 Uiso 1 1 calc R . . C17 C 0.3804(3) -0.1668(5) 0.07883(13) 0.0381(10) Uani 1 1 d . . . H17 H 0.3219 -0.2328 0.0856 0.046 Uiso 1 1 calc R . . C21 C 0.6876(3) -0.7067(6) 0.12700(17) 0.0569(13) Uani 1 1 d . . . H21A H 0.7287 -0.6543 0.1080 0.085 Uiso 1 1 calc R . . H21B H 0.6513 -0.8118 0.1136 0.085 Uiso 1 1 calc R . . H21C H 0.7283 -0.7481 0.1525 0.085 Uiso 1 1 calc R . . C14 C 0.5866(3) -0.1388(5) 0.18974(12) 0.0372(10) Uani 1 1 d . . . H14 H 0.6333 -0.1353 0.2142 0.045 Uiso 1 1 calc R . . C22 C 0.6318(3) -0.5603(6) 0.22513(14) 0.0484(11) Uani 1 1 d . . . H22A H 0.5667 -0.5475 0.2092 0.073 Uiso 1 1 calc R . . H22B H 0.6341 -0.4991 0.2521 0.073 Uiso 1 1 calc R . . H22C H 0.6472 -0.6915 0.2295 0.073 Uiso 1 1 calc R . . C19 C 0.3638(3) -0.3414(7) 0.01611(14) 0.0580(13) Uani 1 1 d . . . H19A H 0.3085 -0.4092 0.0239 0.087 Uiso 1 1 calc R . . H19B H 0.4002 -0.4222 -0.0001 0.087 Uiso 1 1 calc R . . H19C H 0.3403 -0.2337 -0.0007 0.087 Uiso 1 1 calc R . . C18 C 0.4268(3) 0.1113(7) 0.04794(18) 0.0721(16) Uani 1 1 d . . . H18A H 0.4726 0.1494 0.0723 0.108 Uiso 1 1 calc R . . H18B H 0.3990 0.2210 0.0330 0.108 Uiso 1 1 calc R . . H18C H 0.4607 0.0371 0.0295 0.108 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 P1 0.0256(5) 0.0317(5) 0.0324(6) 0.0008(4) 0.0043(4) -0.0022(4) P2 0.0364(6) 0.0452(6) 0.0291(6) 0.0035(5) 0.0080(5) 0.0079(5) O4 0.0358(14) 0.0358(15) 0.0184(14) 0.0026(11) 0.0040(11) -0.0032(11) O2 0.0315(13) 0.0289(14) 0.0239(14) -0.0035(11) 0.0038(11) -0.0073(11) O3 0.0414(15) 0.0352(15) 0.0209(14) -0.0073(11) 0.0015(12) 0.0091(12) F1 0.0386(16) 0.126(3) 0.141(3) 0.029(2) 0.0203(18) 0.0017(16) F2 0.114(3) 0.116(3) 0.141(3) 0.096(3) 0.074(2) 0.070(2) F3 0.0499(18) 0.077(2) 0.279(6) 0.081(3) 0.064(3) 0.0213(16) F4 0.077(2) 0.0413(16) 0.171(4) 0.0337(18) 0.061(2) 0.0221(14) F5 0.249(6) 0.303(7) 0.054(3) -0.080(4) 0.035(3) -0.014(5) F6 0.190(4) 0.087(3) 0.074(2) -0.0304(19) -0.016(3) 0.025(2) F7 0.0423(14) 0.0722(16) 0.0389(14) 0.0089(12) 0.0146(11) 0.0178(12) F8 0.0642(16) 0.0534(15) 0.0459(15) -0.0031(12) 0.0265(13) -0.0026(12) F9 0.0570(16) 0.0726(18) 0.0507(16) 0.0081(13) -0.0091(13) -0.0370(13) F10 0.0359(13) 0.0665(17) 0.0752(19) -0.0288(14) 0.0059(13) -0.0153(12) F11 0.0749(18) 0.0433(14) 0.0532(16) 0.0070(12) 0.0082(14) 0.0250(13) F12 0.0544(15) 0.0525(15) 0.0658(18) 0.0251(13) 0.0200(13) 0.0187(12) O1 0.0300(14) 0.0373(15) 0.0198(13) -0.0004(11) 0.0056(11) 0.0049(11) O8 0.0246(14) 0.0529(17) 0.0443(18) 0.0167(14) -0.0027(13) -0.0045(12) O5 0.0368(16) 0.0459(17) 0.065(2) 0.0210(15) 0.0000(15) 0.0104(13) O6 0.0410(16) 0.0583(18) 0.0305(16) -0.0004(13) -0.0033(13) 0.0121(13) O7 0.0291(14) 0.0342(15) 0.0524(18) -0.0085(13) 0.0010(13) 0.0079(12) N1 0.0254(15) 0.0195(14) 0.0183(16) -0.0006(12) 0.0031(12) 0.0000(12) N2 0.0324(17) 0.0291(17) 0.0257(17) 0.0015(13) 0.0065(14) 0.0048(14) C1 0.0246(18) 0.0275(19) 0.0172(19) -0.0027(15) -0.0012(15) 0.0040(15) C9 0.030(2) 0.030(2) 0.017(2) 0.0029(15) 0.0027(16) 0.0042(16) C6 0.029(2) 0.032(2) 0.0192(19) -0.0023(15) 0.0029(16) 0.0034(16) C2 0.0264(19) 0.029(2) 0.014(2) 0.0012(14) 0.0028(15) 0.0042(15) C3 0.033(2) 0.033(2) 0.019(2) 0.0049(15) 0.0049(16) 0.0027(17) C20 0.026(2) 0.040(2) 0.034(2) 0.0045(18) -0.0010(18) -0.0006(17) C13 0.0230(19) 0.033(2) 0.029(2) 0.0073(16) 0.0046(17) -0.0050(16) C12 0.028(2) 0.028(2) 0.037(2) 0.0067(17) 0.0072(17) 0.0030(16) C5 0.031(2) 0.024(2) 0.029(2) -0.0034(16) -0.0013(17) 0.0032(16) C4 0.034(2) 0.026(2) 0.037(2) 0.0066(17) 0.0059(18) -0.0015(16) C16 0.039(2) 0.038(2) 0.050(3) 0.001(2) 0.012(2) 0.0055(18) C11 0.041(2) 0.046(2) 0.030(2) 0.0158(18) 0.0054(19) -0.0053(19) C15 0.051(3) 0.030(2) 0.054(3) -0.012(2) 0.018(2) -0.003(2) C10 0.042(2) 0.048(3) 0.037(3) 0.0015(19) 0.005(2) 0.0159(19) C7 0.028(2) 0.041(2) 0.040(2) 0.0053(18) 0.0107(18) 0.0066(17) C8 0.040(2) 0.043(2) 0.050(3) -0.017(2) 0.004(2) -0.0095(19) C17 0.028(2) 0.039(2) 0.046(3) 0.0085(19) 0.0046(19) 0.0083(18) C21 0.039(2) 0.047(3) 0.085(4) -0.008(2) 0.010(2) 0.015(2) C14 0.040(2) 0.046(2) 0.025(2) -0.0049(18) 0.0032(18) -0.005(2) C22 0.040(2) 0.058(3) 0.048(3) 0.016(2) 0.008(2) -0.004(2) C19 0.055(3) 0.079(3) 0.036(3) -0.008(2) -0.007(2) 0.011(2) C18 0.063(3) 0.064(3) 0.089(4) 0.037(3) 0.012(3) 0.003(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F10 1.584(2) . ? P1 F9 1.588(2) . ? P1 F11 1.589(2) . ? P1 F12 1.593(2) . ? P1 F8 1.595(2) . ? P1 F7 1.606(2) . ? P2 F5 1.503(4) . ? P2 F1 1.552(3) . ? P2 F3 1.558(3) . ? P2 F6 1.573(3) . ? P2 F4 1.574(3) . ? P2 F2 1.579(3) . ? O4 C9 1.404(4) . ? O4 C11 1.444(4) . ? O2 C6 1.402(4) . ? O2 C8 1.450(4) . ? O3 C9 1.398(4) . ? O3 C10 1.447(4) . ? O1 C6 1.397(4) . ? O1 C7 1.437(4) . ? O8 C20 1.404(4) . ? O8 C22 1.444(5) . ? O5 C17 1.398(4) . ? O5 C18 1.440(5) . ? O6 C17 1.400(5) . ? O6 C19 1.437(5) . ? O7 C20 1.403(4) . ? O7 C21 1.453(4) . ? N1 C2 1.334(4) . ? N1 C1 1.338(4) . ? N1 H1 0.8800 . ? N2 C12 1.346(4) . ? N2 C13 1.351(4) . ? N2 H2 0.8800 . ? C1 C5 1.381(5) . ? C1 C9 1.518(5) . ? C9 H9 1.0000 . ? C6 C2 1.524(5) . ? C6 H6 1.0000 . ? C2 C3 1.376(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9500 . ? C20 C13 1.506(5) . ? C20 H20 1.0000 . ? C13 C14 1.372(5) . ? C12 C16 1.364(5) . ? C12 C17 1.520(5) . ? C5 C4 1.389(5) . ? C5 H5 0.9500 . ? C4 H4 0.9500 . ? C16 C15 1.365(6) . ? C16 H16 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C15 C14 1.387(5) . ? C15 H15 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C17 H17 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C14 H14 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 F10 P1 F9 178.56(15) . . ? F10 P1 F11 90.35(14) . . ? F9 P1 F11 90.68(15) . . ? F10 P1 F12 90.07(14) . . ? F9 P1 F12 88.89(14) . . ? F11 P1 F12 179.39(16) . . ? F10 P1 F8 90.28(14) . . ? F9 P1 F8 90.72(14) . . ? F11 P1 F8 90.47(13) . . ? F12 P1 F8 89.98(14) . . ? F10 P1 F7 89.75(14) . . ? F9 P1 F7 89.25(14) . . ? F11 P1 F7 89.56(13) . . ? F12 P1 F7 89.99(13) . . ? F8 P1 F7 179.96(17) . . ? F5 P2 F1 93.7(3) . . ? F5 P2 F3 88.7(3) . . ? F1 P2 F3 177.4(2) . . ? F5 P2 F6 178.4(3) . . ? F1 P2 F6 85.5(2) . . ? F3 P2 F6 92.1(3) . . ? F5 P2 F4 93.3(3) . . ? F1 P2 F4 90.02(17) . . ? F3 P2 F4 88.93(15) . . ? F6 P2 F4 88.0(2) . . ? F5 P2 F2 92.4(3) . . ? F1 P2 F2 91.97(18) . . ? F3 P2 F2 88.83(17) . . ? F6 P2 F2 86.3(2) . . ? F4 P2 F2 173.8(2) . . ? C9 O4 C11 112.5(3) . . ? C6 O2 C8 112.5(3) . . ? C9 O3 C10 114.9(3) . . ? C6 O1 C7 114.1(3) . . ? C20 O8 C22 115.3(3) . . ? C17 O5 C18 114.3(3) . . ? C17 O6 C19 114.3(3) . . ? C20 O7 C21 113.2(3) . . ? C2 N1 C1 124.4(3) . . ? C2 N1 H1 117.8 . . ? C1 N1 H1 117.8 . . ? C12 N2 C13 124.6(3) . . ? C12 N2 H2 117.7 . . ? C13 N2 H2 117.7 . . ? N1 C1 C5 118.7(3) . . ? N1 C1 C9 117.7(3) . . ? C5 C1 C9 123.5(3) . . ? O3 C9 O4 113.4(3) . . ? O3 C9 C1 111.5(3) . . ? O4 C9 C1 106.8(3) . . ? O3 C9 H9 108.3 . . ? O4 C9 H9 108.3 . . ? C1 C9 H9 108.3 . . ? O1 C6 O2 114.4(3) . . ? O1 C6 C2 112.2(3) . . ? O2 C6 C2 106.0(3) . . ? O1 C6 H6 108.0 . . ? O2 C6 H6 108.0 . . ? C2 C6 H6 108.0 . . ? N1 C2 C3 118.7(3) . . ? N1 C2 C6 116.9(3) . . ? C3 C2 C6 124.1(3) . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? O7 C20 O8 113.8(3) . . ? O7 C20 C13 105.5(3) . . ? O8 C20 C13 111.6(3) . . ? O7 C20 H20 108.6 . . ? O8 C20 H20 108.6 . . ? C13 C20 H20 108.6 . . ? N2 C13 C14 117.6(3) . . ? N2 C13 C20 115.8(3) . . ? C14 C13 C20 126.5(3) . . ? N2 C12 C16 118.3(4) . . ? N2 C12 C17 116.3(3) . . ? C16 C12 C17 125.5(3) . . ? C1 C5 C4 118.4(3) . . ? C1 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C3 C4 C5 120.9(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C12 C16 C15 119.2(4) . . ? C12 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? O4 C11 H11A 109.5 . . ? O4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C16 C15 C14 121.4(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C17 O6 114.3(3) . . ? O5 C17 C12 111.8(3) . . ? O6 C17 C12 106.8(3) . . ? O5 C17 H17 107.9 . . ? O6 C17 H17 107.9 . . ? C12 C17 H17 107.9 . . ? O7 C21 H21A 109.5 . . ? O7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C13 C14 C15 118.9(4) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? O8 C22 H22A 109.5 . . ? O8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O6 C19 H19A 109.5 . . ? O6 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O6 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C18 H18A 109.5 . . ? O5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 24.88 _diffrn_measured_fraction_theta_full 0.836 _refine_diff_density_max 0.634 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.074