Electronic SUpplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_re81lt _database_code_depnum_ccdc_archive 'CCDC 268064' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (R,S)-2,2-bis-(4-pyridinoxy)-(4,4:6,6)-bis-(2',2''-dioxybiphenyl)cyclotri- phosphazene 1,4-diiodo-2,3,5,6-tetrafluorobenzene hemi-carbontetrachloride ; _chemical_formula_moiety '2(C34 H24 N5 O6 P3), C Cl4, 2(C6 F4 I2)' _chemical_formula_sum 'C81 H48 Cl4 F8 I4 N10 O12 P6' _chemical_formula_weight 2340.51 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.254(3) _cell_length_b 11.6963(12) _cell_length_c 31.383(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.60(3) _cell_angle_gamma 90.00 _cell_volume 8762(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8313 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 28.40 _exptl_crystal_description 'elongated prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4568 _exptl_absorpt_coefficient_mu 1.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 1997' _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; The material losses slowly the solvent. A first data collection at room temperature suffered for large intensity decay. A second data collection at room temperature was undertaken with a new crystal sealed in a glass capillary. The structure was solved but it was impossible to understand exactly what the solvent was; later we analyzed the gas developed by eating the material and we found that it was only carbontetrachloride. Data were then recollected at 90 K, the avoid decay and to reduce the refinement noise due to the carbontetrachloride disorder. The crystal temperature was controlled by an OXFORD low temperature device. During the data collection the temperature deviation from the fixed value was less than 0.2 K, but we evaluate that the real error on the crystal temperature was probably around 2 K. ; _diffrn_ambient_temperature 90(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 'Bruker APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 104489 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.95 _reflns_number_total 11023 _reflns_number_gt 9113 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92, (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson,1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 11023 _refine_ls_number_parameters 585 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1S C 0.5000 0.2544(4) 0.2500 0.0359(11) Uani 0.6918(19) d SP . 1 Cl1A Cl 0.49509(3) 0.16751(7) 0.20233(3) 0.0338(2) Uani 0.6918(19) d P . 1 Cl1B Cl 0.43916(5) 0.34118(9) 0.23153(4) 0.0588(4) Uani 0.6918(19) d P . 1 C2S C 0.5134(5) 0.3339(10) 0.2520(4) 0.062(5) Uiso 0.1541(9) d PD . -2 Cl2A Cl 0.4680(3) 0.3872(7) 0.2729(3) 0.091(2) Uiso 0.1541(9) d PD . -2 Cl2B Cl 0.4873(2) 0.2150(5) 0.21813(19) 0.0605(13) Uiso 0.1541(9) d PD . -2 Cl2C Cl 0.5786(3) 0.2949(6) 0.2967(3) 0.107(2) Uiso 0.1541(9) d PD . -2 Cl2D Cl 0.5237(2) 0.4354(5) 0.21599(19) 0.0603(14) Uiso 0.1541(9) d PD . -2 I1 I 0.467428(5) 1.031980(9) 0.086066(4) 0.01889(4) Uani 1 d . . . I2 I 0.545071(5) 0.465769(9) 0.070145(4) 0.02000(4) Uani 1 d . . . F1 F 0.45656(5) 0.80011(9) 0.13730(4) 0.0306(3) Uani 1 d . . . F2 F 0.48650(5) 0.58501(9) 0.13261(4) 0.0267(2) Uani 1 d . . . F3 F 0.56360(4) 0.69892(9) 0.02733(4) 0.0231(2) Uani 1 d . . . F4 F 0.53500(4) 0.91299(8) 0.03310(4) 0.0217(2) Uani 1 d . . . C1 C 0.49347(7) 0.86338(14) 0.08452(6) 0.0162(4) Uani 1 d . . . C2 C 0.48261(7) 0.77628(16) 0.10943(6) 0.0194(4) Uani 1 d . . . C3 C 0.49798(7) 0.66462(15) 0.10682(6) 0.0188(4) Uani 1 d . . . C4 C 0.52494(7) 0.63455(14) 0.07861(6) 0.0169(4) Uani 1 d . . . C5 C 0.53670(7) 0.72127(15) 0.05447(6) 0.0162(4) Uani 1 d . . . C6 C 0.52176(7) 0.83278(14) 0.05746(6) 0.0161(3) Uani 1 d . . . P1 P 0.752125(19) 1.02750(3) 0.051656(15) 0.01310(9) Uani 1 d . . . O1 O 0.79227(5) 1.00783(10) 0.02599(4) 0.0158(3) Uani 1 d . . . C11 C 0.83258(7) 0.92115(14) 0.04105(6) 0.0155(3) Uani 1 d . . . C12 C 0.87969(8) 0.93294(15) 0.08285(7) 0.0209(4) Uani 1 d . . . H12 H 0.8852 0.9969 0.1019 0.025 Uiso 1 calc R . . C13 C 0.91842(8) 0.84394(15) 0.09491(7) 0.0233(4) Uani 1 d . . . H13 H 0.9507 0.8508 0.1226 0.028 Uiso 1 calc R . . N14 N 0.91233(6) 0.74992(13) 0.06953(5) 0.0208(3) Uani 1 d . . . C15 C 0.86632(7) 0.74381(15) 0.02891(6) 0.0209(4) Uani 1 d . . . H15 H 0.8617 0.6794 0.0103 0.025 Uiso 1 calc R . . C16 C 0.82549(8) 0.82719(15) 0.01313(6) 0.0199(4) Uani 1 d . . . H16 H 0.7944 0.8199 -0.0153 0.024 Uiso 1 calc R . . O2 O 0.70203(5) 1.08176(10) 0.00697(4) 0.0155(2) Uani 1 d . . . C21 C 0.66133(7) 1.14300(14) 0.01527(6) 0.0147(3) Uani 1 d . . . C22 C 0.65633(7) 1.25852(15) 0.00554(6) 0.0192(4) Uani 1 d . . . H22 H 0.6781 1.2945 -0.0075 0.023 Uiso 1 calc R . . C23 C 0.61757(7) 1.31847(15) 0.01593(6) 0.0204(4) Uani 1 d . . . H23 H 0.6137 1.3963 0.0094 0.025 Uiso 1 calc R . . N24 N 0.58535(6) 1.27151(13) 0.03485(5) 0.0199(3) Uani 1 d . . . C25 C 0.59009(7) 1.15896(15) 0.04197(6) 0.0178(4) Uani 1 d . . . H25 H 0.5670 1.1244 0.0540 0.021 Uiso 1 calc R . . C26 C 0.62692(7) 1.09045(14) 0.03271(6) 0.0163(4) Uani 1 d . . . H26 H 0.6286 1.0120 0.0380 0.020 Uiso 1 calc R . . N2 N 0.73484(6) 0.90809(11) 0.06513(5) 0.0140(3) Uani 1 d . . . P3 P 0.734958(18) 0.88680(4) 0.114978(15) 0.01322(9) Uani 1 d . . . O3 O 0.77643(5) 0.78720(9) 0.14267(4) 0.0141(2) Uani 1 d . . . C31 C 0.76751(7) 0.67524(14) 0.12420(6) 0.0141(3) Uani 1 d . . . C32 C 0.80582(7) 0.63259(15) 0.10859(6) 0.0170(4) Uani 1 d . . . H32 H 0.8348 0.6782 0.1086 0.020 Uiso 1 calc R . . C33 C 0.80016(8) 0.52059(15) 0.09299(6) 0.0193(4) Uani 1 d . . . H33 H 0.8257 0.4902 0.0826 0.023 Uiso 1 calc R . . C34 C 0.75687(8) 0.45405(14) 0.09285(6) 0.0189(4) Uani 1 d . . . H34 H 0.7530 0.3790 0.0821 0.023 Uiso 1 calc R . . C35 C 0.71892(7) 0.49887(15) 0.10871(6) 0.0171(4) Uani 1 d . . . H35 H 0.6897 0.4532 0.1083 0.021 Uiso 1 calc R . . C36 C 0.72350(7) 0.61069(14) 0.12528(6) 0.0147(3) Uani 1 d . . . O4 O 0.67485(5) 0.83459(9) 0.10363(4) 0.0150(2) Uani 1 d . . . C41 C 0.66547(7) 0.76815(14) 0.13722(6) 0.0146(3) Uani 1 d . . . C42 C 0.63314(7) 0.81465(15) 0.15778(6) 0.0171(4) Uani 1 d . . . H42 H 0.6208 0.8899 0.1517 0.020 Uiso 1 calc R . . C43 C 0.61917(7) 0.74748(16) 0.18783(6) 0.0204(4) Uani 1 d . . . H43 H 0.5975 0.7776 0.2022 0.025 Uiso 1 calc R . . C44 C 0.63769(7) 0.63509(16) 0.19628(6) 0.0197(4) Uani 1 d . . . H44 H 0.6279 0.5894 0.2159 0.024 Uiso 1 calc R . . C45 C 0.67063(7) 0.59108(15) 0.17559(6) 0.0178(4) Uani 1 d . . . H45 H 0.6830 0.5158 0.1817 0.021 Uiso 1 calc R . . C46 C 0.68585(7) 0.65755(14) 0.14560(6) 0.0140(3) Uani 1 d . . . N4 N 0.74920(6) 0.99007(12) 0.15032(5) 0.0151(3) Uani 1 d . . . P5 P 0.766188(18) 1.11097(4) 0.137891(15) 0.01339(9) Uani 1 d . . . O5 O 0.81940(5) 1.14856(9) 0.18329(4) 0.0147(2) Uani 1 d . . . C51 C 0.83502(7) 1.26437(14) 0.19339(6) 0.0158(3) Uani 1 d . . . C52 C 0.88560(7) 1.29637(16) 0.19391(6) 0.0205(4) Uani 1 d . . . H52 H 0.9065 1.2445 0.1853 0.025 Uiso 1 calc R . . C53 C 0.90530(8) 1.40598(17) 0.20731(7) 0.0263(4) Uani 1 d . . . H53 H 0.9392 1.4287 0.2073 0.032 Uiso 1 calc R . . C54 C 0.87421(9) 1.48188(16) 0.22073(7) 0.0257(4) Uani 1 d . . . H54 H 0.8875 1.5556 0.2300 0.031 Uiso 1 calc R . . C55 C 0.82340(8) 1.44831(14) 0.22038(6) 0.0201(4) Uani 1 d . . . H55 H 0.8028 1.5004 0.2292 0.024 Uiso 1 calc R . . C56 C 0.80240(7) 1.33735(14) 0.20703(6) 0.0160(3) Uani 1 d . . . O6 O 0.72129(5) 1.20672(9) 0.13300(4) 0.0144(2) Uani 1 d . . . N6 N 0.77661(6) 1.12062(11) 0.09176(5) 0.0146(3) Uani 1 d . . . C61 C 0.71016(7) 1.23651(14) 0.17169(6) 0.0155(4) Uani 1 d . . . C62 C 0.65849(7) 1.20533(16) 0.17037(6) 0.0215(4) Uani 1 d . . . H62 H 0.6336 1.1614 0.1458 0.026 Uiso 1 calc R . . C63 C 0.64482(8) 1.24117(17) 0.20640(7) 0.0264(4) Uani 1 d . . . H63 H 0.6104 1.2213 0.2062 0.032 Uiso 1 calc R . . C64 C 0.68235(8) 1.30655(17) 0.24269(6) 0.0263(4) Uani 1 d . . . H64 H 0.6729 1.3308 0.2667 0.032 Uiso 1 calc R . . C65 C 0.73358(7) 1.33592(15) 0.24355(6) 0.0201(4) Uani 1 d . . . H65 H 0.7586 1.3788 0.2684 0.024 Uiso 1 calc R . . C66 C 0.74863(7) 1.30205(14) 0.20749(6) 0.0156(3) Uani 1 d . . . 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 C1S 0.040(3) 0.023(2) 0.057(3) 0.000 0.031(3) 0.000 Cl1A 0.0331(4) 0.0358(5) 0.0345(5) 0.0014(4) 0.0163(4) 0.0005(3) Cl1B 0.0698(8) 0.0487(6) 0.0854(10) 0.0227(6) 0.0596(7) 0.0232(5) I1 0.01860(7) 0.01480(6) 0.02461(7) -0.00235(5) 0.01033(5) 0.00272(4) I2 0.01869(6) 0.01320(6) 0.02508(7) -0.00307(5) 0.00610(5) 0.00121(4) F1 0.0417(7) 0.0248(6) 0.0427(7) -0.0017(5) 0.0348(6) 0.0013(5) F2 0.0347(6) 0.0203(6) 0.0316(6) 0.0017(5) 0.0203(5) -0.0048(5) F3 0.0275(6) 0.0204(6) 0.0297(6) -0.0031(5) 0.0200(5) 0.0012(5) F4 0.0269(6) 0.0163(5) 0.0268(6) 0.0028(4) 0.0161(5) 0.0005(4) C1 0.0140(8) 0.0143(8) 0.0185(9) -0.0019(7) 0.0050(7) 0.0000(7) C2 0.0168(9) 0.0239(10) 0.0207(9) -0.0034(8) 0.0111(8) -0.0003(7) C3 0.0168(9) 0.0171(9) 0.0223(9) 0.0016(7) 0.0078(8) -0.0006(7) C4 0.0143(8) 0.0137(8) 0.0192(9) -0.0031(7) 0.0036(7) -0.0008(7) C5 0.0142(8) 0.0168(9) 0.0178(9) -0.0040(7) 0.0067(7) 0.0016(7) C6 0.0159(8) 0.0150(9) 0.0168(9) 0.0007(7) 0.0062(7) -0.0010(7) P1 0.0171(2) 0.0107(2) 0.0129(2) 0.00097(16) 0.00760(18) 0.00156(17) O1 0.0203(6) 0.0136(6) 0.0174(6) 0.0024(5) 0.0117(5) 0.0047(5) C11 0.0181(9) 0.0132(8) 0.0186(9) 0.0021(7) 0.0111(7) 0.0020(7) C12 0.0213(9) 0.0156(9) 0.0249(10) -0.0045(7) 0.0089(8) 0.0009(7) C13 0.0167(9) 0.0225(10) 0.0273(10) 0.0007(8) 0.0057(8) 0.0011(7) N14 0.0186(8) 0.0198(8) 0.0269(9) 0.0015(7) 0.0123(7) 0.0034(6) C15 0.0246(10) 0.0168(9) 0.0250(10) -0.0024(7) 0.0142(8) 0.0035(7) C16 0.0213(9) 0.0223(10) 0.0170(9) -0.0023(7) 0.0088(8) 0.0017(7) O2 0.0201(6) 0.0144(6) 0.0133(6) 0.0020(5) 0.0081(5) 0.0052(5) C21 0.0152(8) 0.0135(8) 0.0138(8) -0.0005(6) 0.0045(7) 0.0029(7) C22 0.0206(9) 0.0164(9) 0.0197(9) 0.0038(7) 0.0075(8) 0.0021(7) C23 0.0228(9) 0.0126(9) 0.0242(10) -0.0004(7) 0.0081(8) 0.0013(7) N24 0.0175(8) 0.0179(8) 0.0203(8) -0.0021(6) 0.0038(6) 0.0031(6) C25 0.0161(9) 0.0176(9) 0.0168(9) 0.0003(7) 0.0040(7) -0.0002(7) C26 0.0198(9) 0.0120(8) 0.0162(9) -0.0007(7) 0.0066(7) 0.0009(7) N2 0.0186(7) 0.0097(7) 0.0142(7) -0.0010(5) 0.0074(6) 0.0001(6) P3 0.0167(2) 0.0103(2) 0.0133(2) 0.00083(16) 0.00687(18) -0.00002(16) O3 0.0159(6) 0.0094(6) 0.0154(6) 0.0002(5) 0.0050(5) -0.0002(5) C31 0.0185(9) 0.0110(8) 0.0113(8) 0.0004(6) 0.0049(7) 0.0021(6) C32 0.0174(9) 0.0180(9) 0.0151(9) 0.0034(7) 0.0063(7) 0.0008(7) C33 0.0223(9) 0.0211(10) 0.0141(9) 0.0022(7) 0.0071(8) 0.0078(7) C34 0.0289(10) 0.0111(8) 0.0159(9) -0.0002(7) 0.0086(8) 0.0018(7) C35 0.0202(9) 0.0149(8) 0.0149(9) 0.0006(7) 0.0060(7) -0.0027(7) C36 0.0189(9) 0.0123(8) 0.0128(8) 0.0034(6) 0.0064(7) 0.0020(7) O4 0.0167(6) 0.0124(6) 0.0155(6) 0.0024(5) 0.0063(5) 0.0003(5) C41 0.0148(8) 0.0147(8) 0.0130(8) 0.0006(7) 0.0045(7) -0.0043(7) C42 0.0147(8) 0.0166(9) 0.0159(9) -0.0037(7) 0.0024(7) -0.0020(7) C43 0.0151(9) 0.0295(10) 0.0171(9) -0.0052(8) 0.0071(7) -0.0026(7) C44 0.0198(9) 0.0254(10) 0.0147(9) 0.0001(7) 0.0079(7) -0.0062(7) C45 0.0189(9) 0.0150(9) 0.0171(9) 0.0023(7) 0.0053(7) -0.0013(7) C46 0.0141(8) 0.0130(8) 0.0139(8) -0.0007(6) 0.0049(7) -0.0012(7) N4 0.0232(8) 0.0116(7) 0.0121(7) 0.0003(6) 0.0088(6) -0.0006(6) P5 0.0173(2) 0.0103(2) 0.0132(2) -0.00054(16) 0.00705(18) 0.00036(17) O5 0.0168(6) 0.0109(6) 0.0145(6) -0.0012(5) 0.0047(5) 0.0011(5) C51 0.0194(9) 0.0145(8) 0.0108(8) 0.0002(6) 0.0036(7) -0.0011(7) C52 0.0216(9) 0.0230(10) 0.0177(9) -0.0002(7) 0.0090(8) 0.0004(7) C53 0.0277(11) 0.0294(11) 0.0254(10) 0.0003(8) 0.0147(9) -0.0073(8) C54 0.0352(12) 0.0168(9) 0.0235(10) -0.0037(8) 0.0105(9) -0.0083(8) C55 0.0262(10) 0.0156(9) 0.0156(9) -0.0019(7) 0.0060(8) 0.0014(7) C56 0.0205(9) 0.0156(8) 0.0092(8) 0.0003(6) 0.0035(7) 0.0003(7) O6 0.0166(6) 0.0127(6) 0.0138(6) -0.0008(5) 0.0062(5) 0.0011(5) N6 0.0192(7) 0.0122(7) 0.0134(7) -0.0001(5) 0.0077(6) -0.0005(6) C61 0.0217(9) 0.0126(8) 0.0146(8) 0.0028(7) 0.0098(7) 0.0049(7) C62 0.0201(9) 0.0249(10) 0.0191(9) -0.0002(8) 0.0078(8) -0.0010(8) C63 0.0210(10) 0.0391(12) 0.0225(10) 0.0042(9) 0.0125(8) 0.0019(9) C64 0.0294(11) 0.0375(12) 0.0150(9) 0.0008(8) 0.0123(8) 0.0078(9) C65 0.0221(9) 0.0215(9) 0.0148(9) 0.0015(7) 0.0058(8) 0.0069(8) C66 0.0192(9) 0.0127(8) 0.0130(8) 0.0034(7) 0.0049(7) 0.0045(7) _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 C1S Cl1A 1.768(3) 2_655 NO C1S Cl1A 1.768(3) . NO C1S Cl1B 1.774(3) . NO C1S Cl1B 1.774(3) 2_655 NO C2S Cl2A 1.700(11) . NO C2S Cl2B 1.710(11) . NO C2S Cl2D 1.735(11) . NO C2S Cl2C 1.763(12) . NO I1 C1 2.0943(17) . NO I2 C4 2.0890(17) . NO F1 C2 1.3449(19) . NO F2 C3 1.3478(19) . NO F3 C5 1.3390(18) . NO F4 C6 1.3441(19) . NO C1 C2 1.384(2) . NO C1 C6 1.388(2) . NO C2 C3 1.379(2) . NO C3 C4 1.389(2) . NO C4 C5 1.376(2) . NO C5 C6 1.376(2) . NO P1 N2 1.5796(14) . NO P1 N6 1.5844(14) . NO P1 O1 1.5874(12) . NO P1 O2 1.6011(13) . NO O1 C11 1.398(2) . NO C11 C16 1.369(2) . NO C11 C12 1.385(3) . NO C12 C13 1.393(2) . NO C12 H12 0.9300 . NO C13 N14 1.328(2) . NO C13 H13 0.9300 . NO N14 C15 1.344(2) . NO C15 C16 1.380(2) . NO C15 H15 0.9300 . NO C16 H16 0.9300 . NO O2 C21 1.3978(19) . NO C21 C22 1.379(2) . NO C21 C26 1.380(2) . NO C22 C23 1.382(2) . NO C22 H22 0.9300 . NO C23 N24 1.337(2) . NO C23 H23 0.9300 . NO N24 C25 1.332(2) . NO C25 C26 1.377(2) . NO C25 H25 0.9300 . NO C26 H26 0.9300 . NO N2 P3 1.5828(14) . NO P3 N4 1.5760(15) . NO P3 O3 1.5843(12) . NO P3 O4 1.5882(12) . NO O3 C31 1.4116(19) . NO C31 C32 1.382(2) . NO C31 C36 1.392(2) . NO C32 C33 1.385(2) . NO C32 H32 0.9300 . NO C33 C34 1.376(2) . NO C33 H33 0.9300 . NO C34 C35 1.389(2) . NO C34 H34 0.9300 . NO C35 C36 1.394(2) . NO C35 H35 0.9300 . NO C36 C46 1.487(2) . NO O4 C41 1.4113(19) . NO C41 C42 1.374(2) . NO C41 C46 1.383(2) . NO C42 C43 1.389(2) . NO C42 H42 0.9300 . NO C43 C44 1.388(3) . NO C43 H43 0.9300 . NO C44 C45 1.379(2) . NO C44 H44 0.9300 . NO C45 C46 1.401(2) . NO C45 H45 0.9300 . NO N4 P5 1.5797(14) . NO P5 N6 1.5853(14) . NO P5 O6 1.5864(12) . NO P5 O5 1.5867(13) . NO O5 C51 1.4126(19) . NO C51 C52 1.373(2) . NO C51 C56 1.396(2) . NO C52 C53 1.381(3) . NO C52 H52 0.9300 . NO C53 C54 1.385(3) . NO C53 H53 0.9300 . NO C54 C55 1.386(3) . NO C54 H54 0.9300 . NO C55 C56 1.404(2) . NO C55 H55 0.9300 . NO C56 C66 1.477(2) . NO O6 C61 1.4058(19) . NO C61 C66 1.388(2) . NO C61 C62 1.388(2) . NO C62 C63 1.386(2) . NO C62 H62 0.9300 . NO C63 C64 1.385(3) . NO C63 H63 0.9300 . NO C64 C65 1.378(3) . NO C64 H64 0.9300 . NO C65 C66 1.402(2) . NO C65 H65 0.9300 . NO 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 Cl1A C1S Cl1A 109.9(2) 2_655 . NO Cl1A C1S Cl1B 110.11(4) 2_655 . NO Cl1A C1S Cl1B 108.29(6) . . NO Cl1A C1S Cl1B 108.29(6) 2_655 2_655 NO Cl1A C1S Cl1B 110.11(4) . 2_655 NO Cl1B C1S Cl1B 110.2(3) . 2_655 NO Cl2A C2S Cl2B 112.0(7) . . NO Cl2A C2S Cl2D 108.9(6) . . NO Cl2B C2S Cl2D 106.4(7) . . NO Cl2A C2S Cl2C 113.1(7) . . NO Cl2B C2S Cl2C 106.8(6) . . NO Cl2D C2S Cl2C 109.4(7) . . NO C2 C1 C6 116.37(15) . . NO C2 C1 I1 122.29(13) . . NO C6 C1 I1 121.33(13) . . NO F1 C2 C3 118.38(16) . . NO F1 C2 C1 119.65(16) . . NO C3 C2 C1 121.96(16) . . NO F2 C3 C2 118.32(16) . . NO F2 C3 C4 120.57(15) . . NO C2 C3 C4 121.11(16) . . NO C5 C4 C3 117.06(16) . . NO C5 C4 I2 120.00(12) . . NO C3 C4 I2 122.90(13) . . NO F3 C5 C4 120.33(15) . . NO F3 C5 C6 117.97(15) . . NO C4 C5 C6 121.70(16) . . NO F4 C6 C5 118.30(15) . . NO F4 C6 C1 119.94(15) . . NO C5 C6 C1 121.76(16) . . NO N2 P1 N6 117.51(7) . . NO N2 P1 O1 109.46(7) . . NO N6 P1 O1 111.54(7) . . NO N2 P1 O2 111.24(7) . . NO N6 P1 O2 109.70(7) . . NO O1 P1 O2 95.15(6) . . NO C11 O1 P1 120.16(10) . . NO C16 C11 C12 121.06(16) . . NO C16 C11 O1 118.92(16) . . NO C12 C11 O1 119.99(15) . . NO C11 C12 C13 116.49(17) . . NO C11 C12 H12 121.8 . . NO C13 C12 H12 121.8 . . NO N14 C13 C12 124.33(17) . . NO N14 C13 H13 117.8 . . NO C12 C13 H13 117.8 . . NO C13 N14 C15 116.68(15) . . NO N14 C15 C16 124.06(17) . . NO N14 C15 H15 118.0 . . NO C16 C15 H15 118.0 . . NO C11 C16 C15 117.35(17) . . NO C11 C16 H16 121.3 . . NO C15 C16 H16 121.3 . . NO C21 O2 P1 116.93(10) . . NO C22 C21 C26 120.41(16) . . NO C22 C21 O2 118.06(15) . . NO C26 C21 O2 121.53(15) . . NO C21 C22 C23 117.16(17) . . NO C21 C22 H22 121.4 . . NO C23 C22 H22 121.4 . . NO N24 C23 C22 124.09(17) . . NO N24 C23 H23 118.0 . . NO C22 C23 H23 118.0 . . NO C25 N24 C23 116.64(15) . . NO N24 C25 C26 124.35(17) . . NO N24 C25 H25 117.8 . . NO C26 C25 H25 117.8 . . NO C25 C26 C21 117.24(16) . . NO C25 C26 H26 121.4 . . NO C21 C26 H26 121.4 . . NO P1 N2 P3 121.41(9) . . NO N4 P3 N2 118.51(7) . . NO N4 P3 O3 105.66(7) . . NO N2 P3 O3 112.09(7) . . NO N4 P3 O4 112.03(7) . . NO N2 P3 O4 104.24(7) . . NO O3 P3 O4 103.42(6) . . NO C31 O3 P3 119.88(10) . . NO C32 C31 C36 123.13(16) . . NO C32 C31 O3 117.37(15) . . NO C36 C31 O3 119.36(14) . . NO C31 C32 C33 118.67(16) . . NO C31 C32 H32 120.7 . . NO C33 C32 H32 120.7 . . NO C34 C33 C32 120.22(17) . . NO C34 C33 H33 119.9 . . NO C32 C33 H33 119.9 . . NO C33 C34 C35 120.01(16) . . NO C33 C34 H34 120.0 . . NO C35 C34 H34 120.0 . . NO C34 C35 C36 121.63(16) . . NO C34 C35 H35 119.2 . . NO C36 C35 H35 119.2 . . NO C31 C36 C35 116.32(15) . . NO C31 C36 C46 121.16(15) . . NO C35 C36 C46 122.44(15) . . NO C41 O4 P3 120.68(10) . . NO C42 C41 C46 123.13(16) . . NO C42 C41 O4 117.82(15) . . NO C46 C41 O4 118.91(15) . . NO C41 C42 C43 118.96(16) . . NO C41 C42 H42 120.5 . . NO C43 C42 H42 120.5 . . NO C44 C43 C42 119.66(17) . . NO C44 C43 H43 120.2 . . NO C42 C43 H43 120.2 . . NO C45 C44 C43 120.13(17) . . NO C45 C44 H44 119.9 . . NO C43 C44 H44 119.9 . . NO C44 C45 C46 121.27(16) . . NO C44 C45 H45 119.4 . . NO C46 C45 H45 119.4 . . NO C41 C46 C45 116.82(15) . . NO C41 C46 C36 122.48(15) . . NO C45 C46 C36 120.68(15) . . NO P3 N4 P5 121.39(9) . . NO N4 P5 N6 117.58(7) . . NO N4 P5 O6 112.40(7) . . NO N6 P5 O6 105.38(7) . . NO N4 P5 O5 105.06(7) . . NO N6 P5 O5 112.22(7) . . NO O6 P5 O5 103.43(6) . . NO C51 O5 P5 122.15(10) . . NO C52 C51 C56 122.89(16) . . NO C52 C51 O5 116.93(15) . . NO C56 C51 O5 119.82(15) . . NO C51 C52 C53 119.64(17) . . NO C51 C52 H52 120.2 . . NO C53 C52 H52 120.2 . . NO C52 C53 C54 119.62(18) . . NO C52 C53 H53 120.2 . . NO C54 C53 H53 120.2 . . NO C53 C54 C55 120.20(17) . . NO C53 C54 H54 119.9 . . NO C55 C54 H54 119.9 . . NO C54 C55 C56 121.41(17) . . NO C54 C55 H55 119.3 . . NO C56 C55 H55 119.3 . . NO C51 C56 C55 116.22(16) . . NO C51 C56 C66 122.87(15) . . NO C55 C56 C66 120.91(16) . . NO C61 O6 P5 120.30(10) . . NO P1 N6 P5 120.62(9) . . NO C66 C61 C62 122.82(16) . . NO C66 C61 O6 119.56(15) . . NO C62 C61 O6 117.44(15) . . NO C63 C62 C61 118.54(18) . . NO C63 C62 H62 120.7 . . NO C61 C62 H62 120.7 . . NO C64 C63 C62 120.04(18) . . NO C64 C63 H63 120.0 . . NO C62 C63 H63 120.0 . . NO C65 C64 C63 120.57(17) . . NO C65 C64 H64 119.7 . . NO C63 C64 H64 119.7 . . NO C64 C65 C66 120.96(17) . . NO C64 C65 H65 119.5 . . NO C66 C65 H65 119.5 . . NO C61 C66 C65 117.07(16) . . NO C61 C66 C56 121.53(15) . . NO C65 C66 C56 121.37(16) . . NO 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 C6 C1 C2 F1 178.38(15) . . . . NO I1 C1 C2 F1 -2.9(2) . . . . NO C6 C1 C2 C3 -1.3(3) . . . . NO I1 C1 C2 C3 177.44(14) . . . . NO F1 C2 C3 F2 -0.5(3) . . . . NO C1 C2 C3 F2 179.20(16) . . . . NO F1 C2 C3 C4 179.93(15) . . . . NO C1 C2 C3 C4 -0.4(3) . . . . NO F2 C3 C4 C5 -178.06(15) . . . . NO C2 C3 C4 C5 1.5(3) . . . . NO F2 C3 C4 I2 4.1(2) . . . . NO C2 C3 C4 I2 -176.32(13) . . . . NO C3 C4 C5 F3 178.69(15) . . . . NO I2 C4 C5 F3 -3.4(2) . . . . NO C3 C4 C5 C6 -0.9(3) . . . . NO I2 C4 C5 C6 176.96(13) . . . . NO F3 C5 C6 F4 -0.1(2) . . . . NO C4 C5 C6 F4 179.56(15) . . . . NO F3 C5 C6 C1 179.57(15) . . . . NO C4 C5 C6 C1 -0.8(3) . . . . NO C2 C1 C6 F4 -178.46(15) . . . . NO I1 C1 C6 F4 2.8(2) . . . . NO C2 C1 C6 C5 1.9(3) . . . . NO I1 C1 C6 C5 -176.87(13) . . . . NO N2 P1 O1 C11 -38.52(14) . . . . NO N6 P1 O1 C11 93.25(13) . . . . NO O2 P1 O1 C11 -153.20(12) . . . . NO P1 O1 C11 C16 109.79(16) . . . . NO P1 O1 C11 C12 -72.41(19) . . . . NO C16 C11 C12 C13 -0.9(3) . . . . NO O1 C11 C12 C13 -178.69(15) . . . . NO C11 C12 C13 N14 -1.1(3) . . . . NO C12 C13 N14 C15 2.3(3) . . . . NO C13 N14 C15 C16 -1.4(3) . . . . NO C12 C11 C16 C15 1.7(3) . . . . NO O1 C11 C16 C15 179.46(15) . . . . NO N14 C15 C16 C11 -0.5(3) . . . . NO N2 P1 O2 C21 83.93(13) . . . . NO N6 P1 O2 C21 -47.79(13) . . . . NO O1 P1 O2 C21 -162.87(12) . . . . NO P1 O2 C21 C22 115.35(15) . . . . NO P1 O2 C21 C26 -64.59(19) . . . . NO C26 C21 C22 C23 2.7(3) . . . . NO O2 C21 C22 C23 -177.20(15) . . . . NO C21 C22 C23 N24 0.4(3) . . . . NO C22 C23 N24 C25 -2.9(3) . . . . NO C23 N24 C25 C26 2.4(3) . . . . NO N24 C25 C26 C21 0.6(3) . . . . NO C22 C21 C26 C25 -3.2(2) . . . . NO O2 C21 C26 C25 176.76(15) . . . . NO N6 P1 N2 P3 7.22(13) . . . . NO O1 P1 N2 P3 135.77(9) . . . . NO O2 P1 N2 P3 -120.37(10) . . . . NO P1 N2 P3 N4 3.73(14) . . . . NO P1 N2 P3 O3 -119.77(10) . . . . NO P1 N2 P3 O4 129.05(9) . . . . NO N4 P3 O3 C31 167.72(12) . . . . NO N2 P3 O3 C31 -61.84(13) . . . . NO O4 P3 O3 C31 49.86(13) . . . . NO P3 O3 C31 C32 111.10(15) . . . . NO P3 O3 C31 C36 -73.08(17) . . . . NO C36 C31 C32 C33 0.4(3) . . . . NO O3 C31 C32 C33 176.04(14) . . . . NO C31 C32 C33 C34 0.5(3) . . . . NO C32 C33 C34 C35 -0.5(3) . . . . NO C33 C34 C35 C36 -0.4(3) . . . . NO C32 C31 C36 C35 -1.2(2) . . . . NO O3 C31 C36 C35 -176.75(14) . . . . NO C32 C31 C36 C46 175.46(15) . . . . NO O3 C31 C36 C46 -0.1(2) . . . . NO C34 C35 C36 C31 1.2(2) . . . . NO C34 C35 C36 C46 -175.44(16) . . . . NO N4 P3 O4 C41 -73.16(13) . . . . NO N2 P3 O4 C41 157.50(12) . . . . NO O3 P3 O4 C41 40.16(13) . . . . NO P3 O4 C41 C42 109.57(15) . . . . NO P3 O4 C41 C46 -74.66(17) . . . . NO C46 C41 C42 C43 -1.2(3) . . . . NO O4 C41 C42 C43 174.39(14) . . . . NO C41 C42 C43 C44 -0.4(2) . . . . NO C42 C43 C44 C45 1.2(3) . . . . NO C43 C44 C45 C46 -0.4(3) . . . . NO C42 C41 C46 C45 1.9(3) . . . . NO O4 C41 C46 C45 -173.62(14) . . . . NO C42 C41 C46 C36 -176.34(15) . . . . NO O4 C41 C46 C36 8.1(2) . . . . NO C44 C45 C46 C41 -1.1(2) . . . . NO C44 C45 C46 C36 177.19(15) . . . . NO C31 C36 C46 C41 42.7(2) . . . . NO C35 C36 C46 C41 -140.87(18) . . . . NO C31 C36 C46 C45 -135.49(17) . . . . NO C35 C36 C46 C45 40.9(2) . . . . NO N2 P3 N4 P5 -3.19(14) . . . . NO O3 P3 N4 P5 123.44(10) . . . . NO O4 P3 N4 P5 -124.64(10) . . . . NO P3 N4 P5 N6 -8.26(14) . . . . NO P3 N4 P5 O6 114.35(11) . . . . NO P3 N4 P5 O5 -133.88(10) . . . . NO N4 P5 O5 C51 -156.56(12) . . . . NO N6 P5 O5 C51 74.55(13) . . . . NO O6 P5 O5 C51 -38.53(13) . . . . NO P5 O5 C51 C52 -115.98(15) . . . . NO P5 O5 C51 C56 70.69(18) . . . . NO C56 C51 C52 C53 -1.6(3) . . . . NO O5 C51 C52 C53 -174.71(16) . . . . NO C51 C52 C53 C54 1.0(3) . . . . NO C52 C53 C54 C55 -0.5(3) . . . . NO C53 C54 C55 C56 0.6(3) . . . . NO C52 C51 C56 C55 1.7(2) . . . . NO O5 C51 C56 C55 174.60(14) . . . . NO C52 C51 C56 C66 -178.56(16) . . . . NO O5 C51 C56 C66 -5.6(2) . . . . NO C54 C55 C56 C51 -1.2(3) . . . . NO C54 C55 C56 C66 179.05(16) . . . . NO N4 P5 O6 C61 62.76(14) . . . . NO N6 P5 O6 C61 -167.98(12) . . . . NO O5 P5 O6 C61 -50.02(13) . . . . NO N2 P1 N6 P5 -19.22(13) . . . . NO O1 P1 N6 P5 -146.77(9) . . . . NO O2 P1 N6 P5 109.11(10) . . . . NO N4 P5 N6 P1 19.75(13) . . . . NO O6 P5 N6 P1 -106.38(10) . . . . NO O5 P5 N6 P1 141.76(9) . . . . NO P5 O6 C61 C66 74.69(17) . . . . NO P5 O6 C61 C62 -110.01(15) . . . . NO C66 C61 C62 C63 -0.1(3) . . . . NO O6 C61 C62 C63 -175.19(16) . . . . NO C61 C62 C63 C64 0.0(3) . . . . NO C62 C63 C64 C65 -0.4(3) . . . . NO C63 C64 C65 C66 1.0(3) . . . . NO C62 C61 C66 C65 0.6(2) . . . . NO O6 C61 C66 C65 175.64(14) . . . . NO C62 C61 C66 C56 -177.75(16) . . . . NO O6 C61 C66 C56 -2.7(2) . . . . NO C64 C65 C66 C61 -1.1(3) . . . . NO C64 C65 C66 C56 177.28(16) . . . . NO C51 C56 C66 C61 -41.4(2) . . . . NO C55 C56 C66 C61 138.38(17) . . . . NO C51 C56 C66 C65 140.35(17) . . . . NO C55 C56 C66 C65 -39.9(2) . . . . NO _diffrn_measured_fraction_theta_max 0.454 _diffrn_reflns_theta_full 28.95 _diffrn_measured_fraction_theta_full 0.454 _refine_diff_density_max 0.879 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.071 data_re138lt _database_code_depnum_ccdc_archive 'CCDC 268065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (R,S)-2,2-bis-(4-pyridinoxy)-(4,4:6,6)-bis-(2',2''-dioxybiphenyl)cyclotri- phosphazene ; _chemical_formula_moiety 'C34 H24 N5 O6 P3' _chemical_formula_sum 'C34 H24 N5 O6 P3' _chemical_formula_weight 691.49 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 P21/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 9.970(3) _cell_length_b 11.443(3) _cell_length_c 27.801(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.14(3) _cell_angle_gamma 90.00 _cell_volume 3163.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 749 _cell_measurement_theta_min 2.308 _cell_measurement_theta_max 17.667 _exptl_crystal_description wedge _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.244 _exptl_absorpt_correction_type none _exptl_special_details ; All crystal are very small, twinned, gypsum desert roses like. We carried on the x-ray crystal analysis on a small wedge cutted from a petal. because at room temperature the crystal diffraction was were poor, we collected data at 90 K by using of an OXFORD low temperature device; in spite of that, we could only collect incomplete data below 2\t < 41.3 \%. Moreover data were affected by large mosaicity. Notwithstanding, the structure solution was easyi and no disorder seems to be present. ; _diffrn_ambient_temperature 90(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 'Bruker APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 7244 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.1014 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 20.65 _reflns_number_total 2692 _reflns_number_gt 1703 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92, (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson,1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Due to the very low number of unique reflection only P atoms were refined with anisotropic atomic displacement parameterss and H atoms were calculated ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+16.8324P] 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 noref _refine_ls_extinction_method none _refine_ls_number_reflns 2692 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.3969(2) 0.81450(19) 0.41980(9) 0.0278(7) Uani 1 d . . . N2 N 0.2761(6) 0.8938(6) 0.3992(2) 0.0259(18) Uiso 1 d . . . P3 P 0.2168(2) 0.87496(19) 0.34543(9) 0.0288(7) Uani 1 d . . . N4 N 0.2364(6) 0.7510(6) 0.3221(2) 0.0281(19) Uiso 1 d . . . P5 P 0.3260(2) 0.65449(18) 0.34918(9) 0.0273(7) Uani 1 d . . . N6 N 0.4165(6) 0.6908(5) 0.3957(2) 0.0237(18) Uiso 1 d . . . O1 O 0.3964(5) 0.7979(5) 0.47635(19) 0.0278(15) Uiso 1 d . . . C11 C 0.3298(8) 0.7052(7) 0.4973(3) 0.030(2) Uiso 1 d . . . C12 C 0.1943(9) 0.7024(8) 0.4961(3) 0.035(2) Uiso 1 d . . . H12 H 0.1414 0.7583 0.4795 0.042 Uiso 1 calc R . . C13 C 0.1372(10) 0.6102(8) 0.5215(3) 0.042(3) Uiso 1 d . . . H13 H 0.0440 0.6080 0.5214 0.051 Uiso 1 calc R . . N14 N 0.2058(8) 0.5265(7) 0.5454(3) 0.046(2) Uiso 1 d . . . C15 C 0.3375(10) 0.5341(9) 0.5448(3) 0.053(3) Uiso 1 d . . . H15 H 0.3889 0.4770 0.5613 0.064 Uiso 1 calc R . . C16 C 0.4051(10) 0.6205(8) 0.5216(3) 0.048(3) Uiso 1 d . . . H16 H 0.4986 0.6213 0.5225 0.057 Uiso 1 calc R . . O2 O 0.5271(5) 0.8961(4) 0.41930(18) 0.0264(15) Uiso 1 d . . . C21 C 0.6526(8) 0.8713(7) 0.4412(3) 0.024(2) Uiso 1 d . . . C22 C 0.7263(8) 0.7760(7) 0.4291(3) 0.025(2) Uiso 1 d . . . H22 H 0.6907 0.7210 0.4071 0.030 Uiso 1 calc R . . C23 C 0.8542(9) 0.7638(8) 0.4503(3) 0.035(3) Uiso 1 d . . . H23 H 0.9050 0.6999 0.4418 0.042 Uiso 1 calc R . . N24 N 0.9103(7) 0.8412(6) 0.4833(2) 0.038(2) Uiso 1 d . . . C25 C 0.8325(8) 0.9317(8) 0.4949(3) 0.035(3) Uiso 1 d . . . H25 H 0.8676 0.9850 0.5177 0.042 Uiso 1 calc R . . C26 C 0.7048(8) 0.9495(7) 0.4749(3) 0.029(2) Uiso 1 d . . . H26 H 0.6545 1.0132 0.4839 0.034 Uiso 1 calc R . . O3 O 0.2784(5) 0.9759(4) 0.31461(19) 0.0296(15) Uiso 1 d . . . C31 C 0.2196(8) 1.0034(7) 0.2683(3) 0.030(2) Uiso 1 d . . . C32 C 0.2871(9) 0.9765(8) 0.2287(3) 0.040(3) Uiso 1 d . . . H32 H 0.3669 0.9342 0.2320 0.047 Uiso 1 calc R . . C33 C 0.2362(9) 1.0126(8) 0.1839(3) 0.042(3) Uiso 1 d . . . H33 H 0.2820 0.9955 0.1567 0.051 Uiso 1 calc R . . C34 C 0.1184(9) 1.0734(8) 0.1793(4) 0.048(3) Uiso 1 d . . . H34 H 0.0843 1.0979 0.1489 0.057 Uiso 1 calc R . . C35 C 0.0496(9) 1.0989(8) 0.2190(3) 0.043(3) Uiso 1 d . . . H35 H -0.0313 1.1394 0.2149 0.052 Uiso 1 calc R . . C36 C 0.0980(9) 1.0656(8) 0.2654(3) 0.035(3) Uiso 1 d . . . O4 O 0.0612(5) 0.9003(4) 0.34034(18) 0.0275(15) Uiso 1 d . . . C41 C 0.0143(8) 1.0185(7) 0.3458(3) 0.031(2) Uiso 1 d . . . C42 C -0.0470(9) 1.0424(8) 0.3858(3) 0.038(3) Uiso 1 d . . . H42 H -0.0552 0.9855 0.4092 0.045 Uiso 1 calc R . . C43 C -0.0987(9) 1.1549(8) 0.3917(4) 0.050(3) Uiso 1 d . . . H43 H -0.1405 1.1747 0.4194 0.060 Uiso 1 calc R . . C44 C -0.0864(10) 1.2342(9) 0.3561(4) 0.058(3) Uiso 1 d . . . H44 H -0.1193 1.3094 0.3600 0.069 Uiso 1 calc R . . C45 C -0.0272(9) 1.2076(8) 0.3147(3) 0.042(3) Uiso 1 d . . . H45 H -0.0233 1.2639 0.2907 0.051 Uiso 1 calc R . . C46 C 0.0284(8) 1.0951(8) 0.3077(3) 0.033(2) Uiso 1 d . . . O5 O 0.2237(5) 0.5524(5) 0.35912(18) 0.0268(15) Uiso 1 d . . . C51 C 0.2687(8) 0.4368(7) 0.3699(3) 0.027(2) Uiso 1 d . . . C52 C 0.2489(8) 0.3967(7) 0.4148(3) 0.032(2) Uiso 1 d . . . H52 H 0.2152 0.4454 0.4379 0.039 Uiso 1 calc R . . C53 C 0.2808(9) 0.2791(8) 0.4255(3) 0.046(3) Uiso 1 d . . . H53 H 0.2686 0.2490 0.4559 0.055 Uiso 1 calc R . . C54 C 0.3297(9) 0.2099(9) 0.3910(3) 0.043(3) Uiso 1 d . . . H54 H 0.3514 0.1324 0.3981 0.052 Uiso 1 calc R . . C55 C 0.3473(9) 0.2538(8) 0.3453(3) 0.042(3) Uiso 1 d . . . H55 H 0.3804 0.2049 0.3222 0.050 Uiso 1 calc R . . C56 C 0.3162(8) 0.3709(7) 0.3332(3) 0.026(2) Uiso 1 d . . . O6 O 0.4259(5) 0.5961(5) 0.31509(18) 0.0281(15) Uiso 1 d . . . C61 C 0.3758(8) 0.5279(7) 0.2755(3) 0.030(2) Uiso 1 d . . . C62 C 0.3846(8) 0.5718(8) 0.2303(3) 0.038(3) Uiso 1 d . . . H62 H 0.4144 0.6480 0.2263 0.046 Uiso 1 calc R . . C63 C 0.3495(9) 0.5035(8) 0.1904(4) 0.049(3) Uiso 1 d . . . H63 H 0.3554 0.5324 0.1594 0.059 Uiso 1 calc R . . C64 C 0.3051(10) 0.3902(9) 0.1980(4) 0.058(3) Uiso 1 d . . . H64 H 0.2824 0.3426 0.1715 0.069 Uiso 1 calc R . . C65 C 0.2940(9) 0.3471(8) 0.2438(3) 0.045(3) Uiso 1 d . . . H65 H 0.2635 0.2711 0.2476 0.054 Uiso 1 calc R . . C66 C 0.3275(8) 0.4149(7) 0.2844(3) 0.031(2) Uiso 1 d . . . 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 0.0310(16) 0.0134(13) 0.0380(17) -0.0015(13) -0.0047(12) 0.0002(12) P3 0.0334(16) 0.0095(13) 0.0423(17) -0.0002(13) -0.0057(12) -0.0009(12) P5 0.0307(15) 0.0119(13) 0.0385(17) -0.0010(12) -0.0028(12) 0.0003(12) _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 N2 1.582(7) . NO P1 O1 1.584(6) . NO P1 N6 1.584(7) . NO P1 O2 1.601(6) . NO N2 P3 1.581(7) . NO P3 O4 1.575(6) . NO P3 N4 1.577(7) . NO P3 O3 1.588(6) . NO N4 P5 1.576(7) . NO P5 O6 1.572(6) . NO P5 N6 1.578(7) . NO P5 O5 1.588(6) . NO O1 C11 1.400(9) . NO C11 C12 1.349(11) . NO C11 C16 1.374(11) . NO C12 C13 1.411(11) . NO C12 H12 0.9300 . NO C13 N14 1.327(10) . NO C13 H13 0.9300 . NO N14 C15 1.317(11) . NO C15 C16 1.383(12) . NO C15 H15 0.9300 . NO C16 H16 0.9300 . NO O2 C21 1.380(9) . NO C21 C26 1.371(10) . NO C21 C22 1.372(10) . NO C22 C23 1.372(11) . NO C22 H22 0.9300 . NO C23 N24 1.365(10) . NO C23 H23 0.9300 . NO N24 C25 1.347(10) . NO C25 C26 1.367(11) . NO C25 H25 0.9300 . NO C26 H26 0.9300 . NO O3 C31 1.412(9) . NO C31 C32 1.366(11) . NO C31 C36 1.403(11) . NO C32 C33 1.374(11) . NO C32 H32 0.9300 . NO C33 C34 1.363(11) . NO C33 H33 0.9300 . NO C34 C35 1.373(11) . NO C34 H34 0.9300 . NO C35 C36 1.398(11) . NO C35 H35 0.9300 . NO C36 C46 1.447(11) . NO O4 C41 1.443(9) . NO C41 C42 1.335(11) . NO C41 C46 1.390(11) . NO C42 C43 1.401(12) . NO C42 H42 0.9300 . NO C43 C44 1.356(12) . NO C43 H43 0.9300 . NO C44 C45 1.365(12) . NO C44 H44 0.9300 . NO C45 C46 1.420(11) . NO C45 H45 0.9300 . NO O5 C51 1.422(9) . NO C51 C52 1.358(10) . NO C51 C56 1.382(10) . NO C52 C53 1.409(11) . NO C52 H52 0.9300 . NO C53 C54 1.360(11) . NO C53 H53 0.9300 . NO C54 C55 1.389(11) . NO C54 H54 0.9300 . NO C55 C56 1.411(11) . NO C55 H55 0.9300 . NO C56 C66 1.458(11) . NO O6 C61 1.411(9) . NO C61 C62 1.361(11) . NO C61 C66 1.408(11) . NO C62 C63 1.382(11) . NO C62 H62 0.9300 . NO C63 C64 1.390(13) . NO C63 H63 0.9300 . NO C64 C65 1.377(12) . NO C64 H64 0.9300 . NO C65 C66 1.392(11) . NO C65 H65 0.9300 . NO 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 N2 P1 O1 111.8(3) . . NO N2 P1 N6 118.3(4) . . NO O1 P1 N6 108.8(3) . . NO N2 P1 O2 105.0(3) . . NO O1 P1 O2 98.0(3) . . NO N6 P1 O2 113.1(3) . . NO P3 N2 P1 119.1(4) . . NO O4 P3 N4 106.2(3) . . NO O4 P3 N2 111.0(3) . . NO N4 P3 N2 117.5(4) . . NO O4 P3 O3 103.6(3) . . NO N4 P3 O3 111.6(3) . . NO N2 P3 O3 106.1(3) . . NO P5 N4 P3 121.1(4) . . NO O6 P5 N4 111.8(3) . . NO O6 P5 N6 104.8(3) . . NO N4 P5 N6 118.5(4) . . NO O6 P5 O5 103.6(3) . . NO N4 P5 O5 104.4(3) . . NO N6 P5 O5 112.8(3) . . NO P5 N6 P1 120.1(4) . . NO C11 O1 P1 122.6(5) . . NO C12 C11 C16 120.4(9) . . NO C12 C11 O1 120.8(8) . . NO C16 C11 O1 118.7(8) . . NO C11 C12 C13 116.4(8) . . NO C11 C12 H12 121.8 . . NO C13 C12 H12 121.8 . . NO N14 C13 C12 125.3(9) . . NO N14 C13 H13 117.4 . . NO C12 C13 H13 117.4 . . NO C15 N14 C13 115.2(8) . . NO N14 C15 C16 124.9(10) . . NO N14 C15 H15 117.5 . . NO C16 C15 H15 117.5 . . NO C11 C16 C15 117.8(9) . . NO C11 C16 H16 121.1 . . NO C15 C16 H16 121.1 . . NO C21 O2 P1 125.9(5) . . NO C26 C21 C22 120.2(7) . . NO C26 C21 O2 117.1(7) . . NO C22 C21 O2 122.7(7) . . NO C21 C22 C23 118.2(8) . . NO C21 C22 H22 120.9 . . NO C23 C22 H22 120.9 . . NO N24 C23 C22 123.1(8) . . NO N24 C23 H23 118.4 . . NO C22 C23 H23 118.4 . . NO C25 N24 C23 116.4(7) . . NO N24 C25 C26 123.5(8) . . NO N24 C25 H25 118.2 . . NO C26 C25 H25 118.2 . . NO C25 C26 C21 118.5(8) . . NO C25 C26 H26 120.7 . . NO C21 C26 H26 120.7 . . NO C31 O3 P3 120.2(5) . . NO C32 C31 C36 122.9(8) . . NO C32 C31 O3 119.2(7) . . NO C36 C31 O3 117.7(7) . . NO C31 C32 C33 119.4(9) . . NO C31 C32 H32 120.3 . . NO C33 C32 H32 120.3 . . NO C34 C33 C32 119.8(9) . . NO C34 C33 H33 120.1 . . NO C32 C33 H33 120.1 . . NO C33 C34 C35 120.7(9) . . NO C33 C34 H34 119.7 . . NO C35 C34 H34 119.7 . . NO C34 C35 C36 121.7(9) . . NO C34 C35 H35 119.1 . . NO C36 C35 H35 119.1 . . NO C35 C36 C31 115.4(8) . . NO C35 C36 C46 122.2(8) . . NO C31 C36 C46 122.4(8) . . NO C41 O4 P3 119.2(5) . . NO C42 C41 C46 125.7(8) . . NO C42 C41 O4 116.8(8) . . NO C46 C41 O4 117.4(7) . . NO C41 C42 C43 118.8(9) . . NO C41 C42 H42 120.6 . . NO C43 C42 H42 120.6 . . NO C44 C43 C42 118.4(10) . . NO C44 C43 H43 120.8 . . NO C42 C43 H43 120.8 . . NO C43 C44 C45 122.3(10) . . NO C43 C44 H44 118.9 . . NO C45 C44 H44 118.9 . . NO C44 C45 C46 121.0(9) . . NO C44 C45 H45 119.5 . . NO C46 C45 H45 119.5 . . NO C41 C46 C45 113.9(8) . . NO C41 C46 C36 123.5(8) . . NO C45 C46 C36 122.5(8) . . NO C51 O5 P5 121.6(5) . . NO C52 C51 C56 125.2(8) . . NO C52 C51 O5 116.4(7) . . NO C56 C51 O5 118.1(7) . . NO C51 C52 C53 118.0(8) . . NO C51 C52 H52 121.0 . . NO C53 C52 H52 121.0 . . NO C54 C53 C52 119.7(9) . . NO C54 C53 H53 120.2 . . NO C52 C53 H53 120.2 . . NO C53 C54 C55 120.6(9) . . NO C53 C54 H54 119.7 . . NO C55 C54 H54 119.7 . . NO C54 C55 C56 121.5(9) . . NO C54 C55 H55 119.2 . . NO C56 C55 H55 119.2 . . NO C51 C56 C55 115.0(8) . . NO C51 C56 C66 123.5(7) . . NO C55 C56 C66 121.4(8) . . NO C61 O6 P5 120.1(5) . . NO C62 C61 C66 123.1(8) . . NO C62 C61 O6 118.2(7) . . NO C66 C61 O6 118.5(7) . . NO C61 C62 C63 120.2(9) . . NO C61 C62 H62 119.9 . . NO C63 C62 H62 119.9 . . NO C62 C63 C64 118.1(10) . . NO C62 C63 H63 121.0 . . NO C64 C63 H63 121.0 . . NO C65 C64 C63 121.5(10) . . NO C65 C64 H64 119.3 . . NO C63 C64 H64 119.3 . . NO C64 C65 C66 121.3(9) . . NO C64 C65 H65 119.3 . . NO C66 C65 H65 119.3 . . NO C65 C66 C61 115.8(8) . . NO C65 C66 C56 122.1(8) . . NO C61 C66 C56 122.1(8) . . NO 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 O1 P1 N2 P3 -151.5(4) . . . . NO N6 P1 N2 P3 -24.0(6) . . . . NO O2 P1 N2 P3 103.3(4) . . . . NO P1 N2 P3 O4 146.9(4) . . . . NO P1 N2 P3 N4 24.4(6) . . . . NO P1 N2 P3 O3 -101.3(5) . . . . NO O4 P3 N4 P5 -131.8(4) . . . . NO N2 P3 N4 P5 -7.0(6) . . . . NO O3 P3 N4 P5 115.9(4) . . . . NO P3 N4 P5 O6 -132.8(4) . . . . NO P3 N4 P5 N6 -10.7(6) . . . . NO P3 N4 P5 O5 115.8(4) . . . . NO O6 P5 N6 P1 136.7(4) . . . . NO N4 P5 N6 P1 11.2(6) . . . . NO O5 P5 N6 P1 -111.2(4) . . . . NO N2 P1 N6 P5 5.9(6) . . . . NO O1 P1 N6 P5 134.8(4) . . . . NO O2 P1 N6 P5 -117.4(4) . . . . NO N2 P1 O1 C11 91.0(6) . . . . NO N6 P1 O1 C11 -41.4(6) . . . . NO O2 P1 O1 C11 -159.2(6) . . . . NO P1 O1 C11 C12 -72.1(9) . . . . NO P1 O1 C11 C16 111.7(8) . . . . NO C16 C11 C12 C13 0.9(12) . . . . NO O1 C11 C12 C13 -175.2(7) . . . . NO C11 C12 C13 N14 -1.0(13) . . . . NO C12 C13 N14 C15 0.7(13) . . . . NO C13 N14 C15 C16 -0.2(14) . . . . NO C12 C11 C16 C15 -0.4(13) . . . . NO O1 C11 C16 C15 175.7(8) . . . . NO N14 C15 C16 C11 0.1(15) . . . . NO N2 P1 O2 C21 168.8(6) . . . . NO O1 P1 O2 C21 53.6(6) . . . . NO N6 P1 O2 C21 -60.9(7) . . . . NO P1 O2 C21 C26 -121.5(7) . . . . NO P1 O2 C21 C22 61.1(9) . . . . NO C26 C21 C22 C23 -2.2(12) . . . . NO O2 C21 C22 C23 175.1(7) . . . . NO C21 C22 C23 N24 0.9(12) . . . . NO C22 C23 N24 C25 0.7(12) . . . . NO C23 N24 C25 C26 -1.2(12) . . . . NO N24 C25 C26 C21 0.0(12) . . . . NO C22 C21 C26 C25 1.8(12) . . . . NO O2 C21 C26 C25 -175.7(7) . . . . NO O4 P3 O3 C31 -46.1(6) . . . . NO N4 P3 O3 C31 67.8(6) . . . . NO N2 P3 O3 C31 -163.0(6) . . . . NO P3 O3 C31 C32 -110.0(8) . . . . NO P3 O3 C31 C36 74.8(9) . . . . NO C36 C31 C32 C33 0.9(13) . . . . NO O3 C31 C32 C33 -174.1(7) . . . . NO C31 C32 C33 C34 -0.7(13) . . . . NO C32 C33 C34 C35 -0.2(14) . . . . NO C33 C34 C35 C36 1.1(14) . . . . NO C34 C35 C36 C31 -0.9(13) . . . . NO C34 C35 C36 C46 178.1(8) . . . . NO C32 C31 C36 C35 -0.1(13) . . . . NO O3 C31 C36 C35 175.0(7) . . . . NO C32 C31 C36 C46 -179.0(8) . . . . NO O3 C31 C36 C46 -3.9(12) . . . . NO N4 P3 O4 C41 -162.8(5) . . . . NO N2 P3 O4 C41 68.4(6) . . . . NO O3 P3 O4 C41 -45.1(6) . . . . NO P3 O4 C41 C42 -108.7(7) . . . . NO P3 O4 C41 C46 75.6(8) . . . . NO C46 C41 C42 C43 -2.3(14) . . . . NO O4 C41 C42 C43 -177.6(7) . . . . NO C41 C42 C43 C44 1.2(14) . . . . NO C42 C43 C44 C45 0.9(15) . . . . NO C43 C44 C45 C46 -2.0(15) . . . . NO C42 C41 C46 C45 1.2(13) . . . . NO O4 C41 C46 C45 176.5(7) . . . . NO C42 C41 C46 C36 178.8(8) . . . . NO O4 C41 C46 C36 -5.9(12) . . . . NO C44 C45 C46 C41 0.9(12) . . . . NO C44 C45 C46 C36 -176.7(8) . . . . NO C35 C36 C46 C41 139.3(9) . . . . NO C31 C36 C46 C41 -41.8(13) . . . . NO C35 C36 C46 C45 -43.4(13) . . . . NO C31 C36 C46 C45 135.5(9) . . . . NO O6 P5 O5 C51 44.1(6) . . . . NO N4 P5 O5 C51 161.3(6) . . . . NO N6 P5 O5 C51 -68.7(6) . . . . NO P5 O5 C51 C52 114.3(7) . . . . NO P5 O5 C51 C56 -71.9(8) . . . . NO C56 C51 C52 C53 1.1(12) . . . . NO O5 C51 C52 C53 174.3(7) . . . . NO C51 C52 C53 C54 -0.1(12) . . . . NO C52 C53 C54 C55 -0.5(13) . . . . NO C53 C54 C55 C56 0.3(13) . . . . NO C52 C51 C56 C55 -1.2(12) . . . . NO O5 C51 C56 C55 -174.4(7) . . . . NO C52 C51 C56 C66 175.6(8) . . . . NO O5 C51 C56 C66 2.5(12) . . . . NO C54 C55 C56 C51 0.5(12) . . . . NO C54 C55 C56 C66 -176.4(8) . . . . NO N4 P5 O6 C61 -66.0(6) . . . . NO N6 P5 O6 C61 164.4(6) . . . . NO O5 P5 O6 C61 45.9(6) . . . . NO P5 O6 C61 C62 109.0(7) . . . . NO P5 O6 C61 C66 -75.1(8) . . . . NO C66 C61 C62 C63 -2.2(13) . . . . NO O6 C61 C62 C63 173.5(7) . . . . NO C61 C62 C63 C64 0.2(13) . . . . NO C62 C63 C64 C65 1.0(14) . . . . NO C63 C64 C65 C66 -0.4(14) . . . . NO C64 C65 C66 C61 -1.5(13) . . . . NO C64 C65 C66 C56 179.9(8) . . . . NO C62 C61 C66 C65 2.7(12) . . . . NO O6 C61 C66 C65 -172.9(7) . . . . NO C62 C61 C66 C56 -178.6(8) . . . . NO O6 C61 C66 C56 5.8(12) . . . . NO C51 C56 C66 C65 -139.5(9) . . . . NO C55 C56 C66 C65 37.1(12) . . . . NO C51 C56 C66 C61 41.9(12) . . . . NO C55 C56 C66 C61 -141.4(8) . . . . NO _diffrn_measured_fraction_theta_max 0.781 _diffrn_reflns_theta_full 20.65 _diffrn_measured_fraction_theta_full 0.781 _refine_diff_density_max 0.430 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.079