# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email a.richards@latrobe.edu.au _publ_contact_author_phone ? _publ_contact_author_name A.Richards _publ_author_name A.Richards data_ar80cb _database_code_depnum_ccdc_archive 'CCDC 872675' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((PhtalMePO3)4Al5Cl6(thf)6)Cl(thf)1.5 _chemical_melting_point ? _chemical_formula_moiety ; C60 H72 Al5 Cl6 N4 O26 P4, 1.5(C4 H8 O), Cl ; _chemical_formula_sum 'C66 H84 Al5 Cl7 N4 O27.50 P4' _chemical_formula_weight 1880.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2 1 / c' 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 26.7048(4) _cell_length_b 15.5991(2) _cell_length_c 24.6674(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.990(2) _cell_angle_gamma 90.00 _cell_volume 10199.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9859 _cell_measurement_theta_min 2.5992 _cell_measurement_theta_max 73.6799 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.015 _exptl_crystal_size_mid 0.014 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 3.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9515 _exptl_absorpt_correction_T_max 0.9673 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.3281 _diffrn_reflns_number 18146 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 67.50 _reflns_number_total 18146 _reflns_number_gt 12523 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.40 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.40 ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.40 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; SHELXTL 5.1, XP (Sheldrick, 1994), OLEX2 (Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H.,2009) ; _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. The hydrogen atoms on carbon atoms were generated geometrically and refined as riding atoms with C-H = 0.95- 0.99 \%A and Uiso(H) =1.2 times Ueq(C) for CH and CH2 groups There are thre positions for a chloride ion- these positions were found in the difference map. The occupancies were allowed to refine while their thermal parameters were fixed. Once the occupancies converged, they were made to sum to 1, and the thermal parameters were allowed to refine. Thermal parameter similarity restraints were used to aide in the refinement of this disorder. Numerous THF molecules in this structure are disordered. To assist in the refinement of the disordered THFs, all the THF molecules were refined in a THF RESI. SADI commands were used to help optimize the geometry of the disordered molecules. The restrains used in this RESI are as follows: SADI_THF 0.01 O1 C1 O1 C4 SADI_THF 0.01 C1 C2 C4 C3 SADI_THF 0.01 C2 C3 SADI_THF 0.02 O1 C2 O1 C3 SADI_THF 0.02 C1 C4 SIMU_THF 0.02 O1 SIMU_THF 0.02 C1 C2 C3 C4 In one particularly bad case of disorder, one THF is disordered over three sites. The sites were identified, and restrained into the RESI, then their occupancies were made to sum to 0.5, due to this molecule's proximity to an inversion center. Two molecules of THF were very disordered and the disorder could not be modeled. These were omitted from the final refinment through the use of SQUEEZE. SQUEEZE RESULTS (APPEND TO CIF) Note: Data are Listed for all Voids in the P1 Unit Cell i.e. Centre of Gravity, Solvent Accessible Volume, Recovered number of Electrons in the Void and Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.016 0.000 706 167 ' ' 2 0.000 -0.012 0.500 706 167 ' ' 3 0.402 0.199 0.149 177 73 ' ' 4 0.598 -0.199 0.851 177 68 ' ' 5 0.402 0.301 0.649 177 73 ' ' 6 0.598 0.699 0.351 177 69 ' ' _platon_squeeze_details ; _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^)+(0.1303P)^2^+10.7827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18146 _refine_ls_number_parameters 1096 _refine_ls_number_restraints 1106 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.2396 _refine_ls_wR_factor_gt 0.2217 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.091 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.15601(6) 0.20979(13) 0.42600(7) 0.0797(5) Uani 1 1 d . . . Cl2 Cl 0.06699(8) 0.37064(18) 0.38659(10) 0.1092(7) Uani 1 1 d . . . Cl3 Cl 0.05607(7) 0.16815(15) 0.32421(10) 0.1070(8) Uani 1 1 d . . . Cl4 Cl 0.25292(6) 0.74809(16) 0.00327(6) 0.0914(6) Uani 1 1 d . . . Cl5 Cl 0.32524(7) 0.84878(10) 0.11318(7) 0.0757(5) Uani 1 1 d . . . Cl6 Cl 0.34802(6) 0.63478(11) 0.08155(6) 0.0653(4) Uani 1 1 d . . . Cl7 Cl 0.4387(3) 0.2537(5) 0.5550(4) 0.0993(19) Uani 0.409(4) 1 d PU A 1 Cl7' Cl 0.4405(2) 0.2087(5) 0.5438(2) 0.0987(17) Uani 0.491(6) 1 d PU B 2 Cl7" Cl 0.4248(8) 0.2581(14) 0.5976(10) 0.095(4) Uiso 0.101(5) 1 d PU C 3 P1 P 0.31336(4) 0.48358(7) 0.28201(4) 0.0333(2) Uani 1 1 d . . . P2 P 0.18949(4) 0.34555(7) 0.30227(5) 0.0371(3) Uani 1 1 d . . . P3 P 0.22160(4) 0.60584(7) 0.33918(4) 0.0334(2) Uani 1 1 d . . . P4 P 0.24101(4) 0.68184(7) 0.18445(5) 0.0370(3) Uani 1 1 d . D . Al1 Al 0.31708(5) 0.68257(8) 0.29022(5) 0.0358(3) Uani 1 1 d . . . Al2 Al 0.26567(5) 0.43419(8) 0.38961(5) 0.0355(3) Uani 1 1 d . . . Al4 Al 0.10638(6) 0.26241(13) 0.35965(8) 0.0631(5) Uani 1 1 d . . . Al3 Al 0.19894(5) 0.50571(8) 0.22565(5) 0.0335(3) Uani 1 1 d . . . Al5 Al 0.29143(6) 0.73154(10) 0.08265(6) 0.0469(4) Uani 1 1 d . . . O1 O 0.28840(12) 0.31318(19) 0.40399(12) 0.0406(7) Uani 1 1 d . . . O2 O 0.21856(16) 0.0876(2) 0.30297(15) 0.0588(10) Uani 1 1 d . . . O3 O 0.14088(12) 0.2967(2) 0.30860(14) 0.0484(8) Uani 1 1 d . . . O4 O 0.18297(11) 0.39897(19) 0.25159(12) 0.0375(7) Uani 1 1 d . . . O5 O 0.20709(12) 0.3934(2) 0.35458(12) 0.0392(7) Uani 1 1 d . . . O6 O 0.24745(11) 0.54646(19) 0.38346(12) 0.0358(7) Uani 1 1 d . . . O7 O 0.30332(11) 0.43378(18) 0.33243(12) 0.0358(7) Uani 1 1 d . . . O10 O 0.46015(14) 0.4900(3) 0.28565(18) 0.0664(11) Uani 1 1 d . . . O11 O 0.35850(14) 0.2639(2) 0.31455(17) 0.0565(9) Uani 1 1 d . . . O12 O 0.33668(11) 0.57065(19) 0.29717(12) 0.0362(7) Uani 1 1 d . D . O13 O 0.25809(11) 0.67051(19) 0.31930(12) 0.0373(7) Uani 1 1 d . D . O14 O 0.29206(11) 0.67545(19) 0.21786(12) 0.0374(7) Uani 1 1 d . D . O15 O 0.30350(12) 0.8067(2) 0.28620(13) 0.0424(7) Uani 1 1 d . D . O18 O 0.24703(13) 0.6999(2) 0.12484(13) 0.0453(8) Uani 1 1 d . . . O19 O 0.20673(11) 0.6063(2) 0.18867(12) 0.0389(7) Uani 1 1 d . . . O20 O 0.20697(14) 0.8427(2) 0.35634(18) 0.0619(10) Uani 1 1 d . . . O21 O 0.07948(14) 0.6527(3) 0.3098(2) 0.0687(12) Uani 1 1 d . . . O22 O 0.19258(11) 0.55911(19) 0.29183(12) 0.0361(7) Uani 1 1 d . . . O23 O 0.26811(11) 0.48822(19) 0.23907(12) 0.0359(7) Uani 1 1 d . . . O26 O 0.1948(2) 0.9326(3) 0.15157(17) 0.0740(12) Uani 1 1 d . . . N1 N 0.25186(15) 0.2147(2) 0.34006(15) 0.0397(9) Uani 1 1 d . . . N2 N 0.39898(14) 0.3880(3) 0.29266(16) 0.0414(9) Uani 1 1 d . . . N3 N 0.15101(15) 0.7316(3) 0.33902(17) 0.0434(9) Uani 1 1 d . . . N4 N 0.24119(17) 0.8492(2) 0.21771(16) 0.0469(10) Uani 1 1 d . D . C1 C 0.27835(17) 0.2399(3) 0.38867(18) 0.0367(10) Uani 1 1 d . . . C2 C 0.29237(18) 0.1611(3) 0.42016(19) 0.0416(10) Uani 1 1 d . . . C3 C 0.3218(2) 0.1508(3) 0.4699(2) 0.0489(12) Uani 1 1 d . . . H3 H 0.3371 0.1985 0.4894 0.059 Uiso 1 1 calc R . . C4 C 0.3279(2) 0.0676(4) 0.4902(2) 0.0578(14) Uani 1 1 d . . . H4A H 0.3482 0.0575 0.5240 0.069 Uiso 1 1 calc R . . C5 C 0.3041(3) -0.0010(4) 0.4610(2) 0.0635(15) Uani 1 1 d . . . H5A H 0.3082 -0.0571 0.4759 0.076 Uiso 1 1 calc R . . C6 C 0.2756(2) 0.0095(3) 0.4125(2) 0.0540(13) Uani 1 1 d . . . H6A H 0.2598 -0.0380 0.3933 0.065 Uiso 1 1 calc R . . C7 C 0.2703(2) 0.0911(3) 0.3918(2) 0.0461(11) Uani 1 1 d . . . C8 C 0.24336(19) 0.1242(3) 0.3399(2) 0.0453(11) Uani 1 1 d . . . C9 C 0.23711(18) 0.2672(3) 0.29277(19) 0.0412(10) Uani 1 1 d . . . H9A H 0.2243 0.2295 0.2619 0.049 Uiso 1 1 calc R . . H9B H 0.2673 0.2972 0.2827 0.049 Uiso 1 1 calc R . . C10 C 0.44598(18) 0.4262(3) 0.3068(2) 0.0461(11) Uani 1 1 d . . . C11 C 0.47252(18) 0.3710(3) 0.3503(2) 0.0473(12) Uani 1 1 d . . . C12 C 0.5195(2) 0.3807(4) 0.3800(2) 0.0612(15) Uani 1 1 d . . . H12A H 0.5410 0.4276 0.3744 0.073 Uiso 1 1 calc R . . C13 C 0.5332(2) 0.3177(5) 0.4186(3) 0.0707(17) Uani 1 1 d . . . H13A H 0.5653 0.3216 0.4398 0.085 Uiso 1 1 calc R . . C14 C 0.5027(3) 0.2503(5) 0.4275(3) 0.0698(17) Uani 1 1 d . . . H14A H 0.5138 0.2092 0.4548 0.084 Uiso 1 1 calc R . . C15 C 0.4555(2) 0.2408(4) 0.3971(2) 0.0574(14) Uani 1 1 d . . . H15 H 0.4340 0.1940 0.4030 0.069 Uiso 1 1 calc R . . C16 C 0.44171(18) 0.3017(3) 0.3587(2) 0.0455(11) Uani 1 1 d . . . C17 C 0.39493(19) 0.3108(3) 0.3211(2) 0.0445(11) Uani 1 1 d . . . C18 C 0.35984(17) 0.4210(3) 0.25198(18) 0.0386(10) Uani 1 1 d . . . H18A H 0.3428 0.3723 0.2315 0.046 Uiso 1 1 calc R . . H18B H 0.3755 0.4571 0.2257 0.046 Uiso 1 1 calc R . . C31 C 0.28258(19) 0.8607(3) 0.2550(2) 0.0448(11) Uani 1 1 d . . . C32 C 0.2989(2) 0.9508(3) 0.2516(2) 0.0555(14) Uani 1 1 d . D . C33 C 0.3385(2) 0.9936(4) 0.2810(2) 0.0620(15) Uani 1 1 d . . . H33 H 0.3595 0.9661 0.3097 0.074 Uiso 1 1 calc R D . C34 C 0.3463(3) 1.0781(4) 0.2672(3) 0.079(2) Uani 1 1 d . D . H34 H 0.3732 1.1095 0.2867 0.095 Uiso 1 1 calc R . . C35 C 0.3155(3) 1.1174(4) 0.2254(3) 0.086(2) Uani 1 1 d . . . H35 H 0.3221 1.1753 0.2166 0.104 Uiso 1 1 calc R D . C36 C 0.2746(3) 1.0746(4) 0.1951(2) 0.081(2) Uani 1 1 d . D . H36 H 0.2530 1.1021 0.1669 0.097 Uiso 1 1 calc R . . C37 C 0.2681(3) 0.9892(3) 0.2096(2) 0.0609(16) Uani 1 1 d . . . C38 C 0.2293(3) 0.9270(3) 0.1873(2) 0.0561(14) Uani 1 1 d . D . C39 C 0.2096(2) 0.7729(3) 0.2102(2) 0.0469(11) Uani 1 1 d . . . H39A H 0.1792 0.7865 0.1844 0.056 Uiso 1 1 calc R D . H39B H 0.1982 0.7573 0.2456 0.056 Uiso 1 1 calc R . . C40 C 0.16821(19) 0.8147(3) 0.3343(2) 0.0465(11) Uani 1 1 d . . . C41 C 0.1288(2) 0.8583(3) 0.2947(2) 0.0526(13) Uani 1 1 d . . . C42 C 0.1278(2) 0.9400(4) 0.2749(3) 0.0636(15) Uani 1 1 d . . . H42 H 0.1535 0.9801 0.2868 0.076 Uiso 1 1 calc R . . C43 C 0.0870(3) 0.9618(5) 0.2363(3) 0.082(2) Uani 1 1 d . . . H43 H 0.0853 1.0174 0.2205 0.098 Uiso 1 1 calc R . . C44 C 0.0496(3) 0.9038(5) 0.2212(3) 0.083(2) Uani 1 1 d . . . H44 H 0.0221 0.9207 0.1953 0.099 Uiso 1 1 calc R . . C45 C 0.0502(2) 0.8221(5) 0.2418(3) 0.0722(18) Uani 1 1 d . . . H45 H 0.0239 0.7826 0.2309 0.087 Uiso 1 1 calc R . . C46 C 0.09116(19) 0.7996(4) 0.2795(2) 0.0527(13) Uani 1 1 d . . . C47 C 0.10325(18) 0.7181(3) 0.3091(2) 0.0495(12) Uani 1 1 d . . . C48 C 0.17687(18) 0.6660(3) 0.37320(19) 0.0416(10) Uani 1 1 d . . . H48A H 0.1516 0.6260 0.3851 0.050 Uiso 1 1 calc R . . H48B H 0.1948 0.6933 0.4062 0.050 Uiso 1 1 calc R . . O1_1 O 0.12647(10) 0.5187(2) 0.20325(12) 0.0402(7) Uani 1 1 d D . . C1_1 C 0.08660(16) 0.4805(4) 0.2312(2) 0.0551(13) Uani 1 1 d DU . . H1A_1 H 0.0912 0.4953 0.2705 0.066 Uiso 1 1 calc R . . H1B_1 H 0.0865 0.4173 0.2274 0.066 Uiso 1 1 calc R . . C2_1 C 0.03875(18) 0.5180(5) 0.2034(2) 0.0712(17) Uani 1 1 d DU . . H2A_1 H 0.0108 0.4761 0.2017 0.085 Uiso 1 1 calc R . . H2B_1 H 0.0292 0.5701 0.2226 0.085 Uiso 1 1 calc R . . C3_1 C 0.05106(18) 0.5392(5) 0.1478(2) 0.0708(17) Uani 1 1 d DU . . H3A_1 H 0.0279 0.5834 0.1303 0.085 Uiso 1 1 calc R . . H3B_1 H 0.0493 0.4876 0.1242 0.085 Uiso 1 1 calc R . . C4_1 C 0.10380(18) 0.5723(4) 0.1585(2) 0.0640(16) Uani 1 1 d DU . . H4B_1 H 0.1217 0.5659 0.1259 0.077 Uiso 1 1 calc R . . H4C_1 H 0.1042 0.6335 0.1693 0.077 Uiso 1 1 calc R . . O1_2 O 0.20050(12) 0.4476(2) 0.15377(12) 0.0412(7) Uani 1 1 d D . . C1_2 C 0.1699(3) 0.3739(4) 0.1348(2) 0.082(2) Uani 1 1 d DU . . H1C_2 H 0.1336 0.3881 0.1331 0.099 Uiso 1 1 calc R . . H1D_2 H 0.1773 0.3249 0.1600 0.099 Uiso 1 1 calc R . . C2_2 C 0.1823(4) 0.3519(7) 0.0804(3) 0.132(3) Uani 1 1 d DU . . H2C_2 H 0.1904 0.2901 0.0787 0.159 Uiso 1 1 calc R . . H2D_2 H 0.1533 0.3643 0.0526 0.159 Uiso 1 1 calc R . . C3_2 C 0.2259(3) 0.4031(5) 0.0700(3) 0.098(2) Uani 1 1 d DU . . H3C_2 H 0.2191 0.4322 0.0342 0.117 Uiso 1 1 calc R . . H3D_2 H 0.2558 0.3659 0.0695 0.117 Uiso 1 1 calc R . . C4_2 C 0.2350(3) 0.4671(5) 0.1142(2) 0.079(2) Uani 1 1 d DU . . H4D_2 H 0.2704 0.4637 0.1316 0.094 Uiso 1 1 calc R . . H4E_2 H 0.2288 0.5257 0.0995 0.094 Uiso 1 1 calc R . . O1_3 O 0.32614(11) 0.4622(2) 0.43984(12) 0.0435(7) Uani 1 1 d D . . C1_3 C 0.3284(2) 0.5263(3) 0.4834(2) 0.0567(14) Uani 1 1 d DU . . H1E_3 H 0.3008 0.5172 0.5063 0.068 Uiso 1 1 calc R . . H1F_3 H 0.3254 0.5849 0.4679 0.068 Uiso 1 1 calc R . . C2_3 C 0.3781(3) 0.5139(6) 0.5158(3) 0.117(3) Uani 1 1 d DU . . H2E_3 H 0.3943 0.5701 0.5247 0.141 Uiso 1 1 calc R . . H2F_3 H 0.3741 0.4840 0.5504 0.141 Uiso 1 1 calc R . . C3_3 C 0.4095(2) 0.4624(5) 0.4833(2) 0.0729(17) Uani 1 1 d DU . . H3E_3 H 0.4280 0.4179 0.5063 0.088 Uiso 1 1 calc R . . H3F_3 H 0.4343 0.4993 0.4677 0.088 Uiso 1 1 calc R . . C4_3 C 0.3750(2) 0.4222(4) 0.4392(3) 0.079(2) Uani 1 1 d DU . . H4F_3 H 0.3874 0.4316 0.4034 0.095 Uiso 1 1 calc R . . H4G_3 H 0.3727 0.3598 0.4454 0.095 Uiso 1 1 calc R . . O1_4 O 0.23378(13) 0.4261(2) 0.45710(12) 0.0476(8) Uani 1 1 d D . . C1_4 C 0.2453(3) 0.3656(3) 0.50199(19) 0.0662(16) Uani 1 1 d DU . . H1G_4 H 0.2821 0.3639 0.5141 0.079 Uiso 1 1 calc R . . H1H_4 H 0.2336 0.3072 0.4910 0.079 Uiso 1 1 calc R . . C2_4 C 0.2172(3) 0.3998(5) 0.5464(2) 0.0771(19) Uani 1 1 d DU . . H2G_4 H 0.2101 0.3541 0.5723 0.092 Uiso 1 1 calc R . . H2H_4 H 0.2358 0.4470 0.5667 0.092 Uiso 1 1 calc R . . C3_4 C 0.1703(3) 0.4309(5) 0.5143(3) 0.086(2) Uani 1 1 d DU . . H3G_4 H 0.1529 0.4730 0.5356 0.103 Uiso 1 1 calc R . . H3H_4 H 0.1471 0.3828 0.5036 0.103 Uiso 1 1 calc R . . C4_4 C 0.1877(2) 0.4723(4) 0.4650(2) 0.0645(16) Uani 1 1 d DU . . H4H_4 H 0.1620 0.4660 0.4327 0.077 Uiso 1 1 calc R . . H4I_4 H 0.1947 0.5340 0.4715 0.077 Uiso 1 1 calc R . . O1_5 O 0.3842(4) 0.7094(6) 0.2675(5) 0.042(2) Uani 0.722(18) 1 d PD D 1 C1_5 C 0.4071(7) 0.6639(8) 0.2253(8) 0.052(5) Uani 0.722(18) 1 d PDU D 1 H1I_5 H 0.3809 0.6453 0.1957 0.062 Uiso 0.722(18) 1 calc PR D 1 H1J_5 H 0.4254 0.6126 0.2407 0.062 Uiso 0.722(18) 1 calc PR D 1 C2_5 C 0.4425(5) 0.7249(7) 0.2038(5) 0.076(3) Uani 0.722(18) 1 d PDU D 1 H2I_5 H 0.4776 0.7041 0.2118 0.091 Uiso 0.722(18) 1 calc PR D 1 H2J_5 H 0.4343 0.7314 0.1638 0.091 Uiso 0.722(18) 1 calc PR D 1 C3_5 C 0.4364(3) 0.8078(5) 0.2317(3) 0.059(3) Uani 0.722(18) 1 d PDU D 1 H3I_5 H 0.4130 0.8459 0.2086 0.071 Uiso 0.722(18) 1 calc PR D 1 H3J_5 H 0.4693 0.8371 0.2399 0.071 Uiso 0.722(18) 1 calc PR D 1 C4_5 C 0.4153(3) 0.7852(5) 0.2827(3) 0.052(2) Uani 0.722(18) 1 d PDU D 1 H4J_5 H 0.4425 0.7717 0.3124 0.062 Uiso 0.722(18) 1 calc PR D 1 H4K_5 H 0.3946 0.8327 0.2946 0.062 Uiso 0.722(18) 1 calc PR D 1 O1_9 O 0.3768(9) 0.7201(18) 0.2601(13) 0.043(8) Uiso 0.278(18) 1 d PD D 2 C1_9 C 0.4020(13) 0.665(2) 0.2243(18) 0.043(12) Uiso 0.278(18) 1 d PDU D 2 H1K_9 H 0.3827 0.6620 0.1874 0.051 Uiso 0.278(18) 1 calc PR D 2 H1L_9 H 0.4056 0.6057 0.2393 0.051 Uiso 0.278(18) 1 calc PR D 2 C2_9 C 0.4523(9) 0.7042(17) 0.2220(12) 0.064(8) Uiso 0.278(18) 1 d PDU D 2 H2K_9 H 0.4793 0.6627 0.2342 0.077 Uiso 0.278(18) 1 calc PR D 2 H2L_9 H 0.4559 0.7217 0.1840 0.077 Uiso 0.278(18) 1 calc PR D 2 C3_9 C 0.4561(8) 0.7801(19) 0.2582(16) 0.106(10) Uiso 0.278(18) 1 d PDU D 2 H3K_9 H 0.4741 0.8276 0.2423 0.127 Uiso 0.278(18) 1 calc PR D 2 H3L_9 H 0.4740 0.7658 0.2946 0.127 Uiso 0.278(18) 1 calc PR D 2 C4_9 C 0.4027(9) 0.8031(14) 0.2620(14) 0.086(11) Uiso 0.278(18) 1 d PDU D 2 H4L_9 H 0.3993 0.8335 0.2966 0.103 Uiso 0.278(18) 1 calc PR D 2 H4M_9 H 0.3890 0.8398 0.2310 0.103 Uiso 0.278(18) 1 calc PR D 2 O1_6 O 0.35293(11) 0.7096(2) 0.36167(12) 0.0426(7) Uani 1 1 d D D . C1_6 C 0.3391(2) 0.7733(4) 0.4003(2) 0.0643(15) Uani 1 1 d DU . . H1M_6 H 0.3049 0.7620 0.4102 0.077 Uiso 1 1 calc R D . H1N_6 H 0.3398 0.8317 0.3846 0.077 Uiso 1 1 calc R . . C2_6 C 0.3776(2) 0.7645(4) 0.4488(2) 0.0706(17) Uani 1 1 d DU D . H2M_6 H 0.3869 0.8214 0.4647 0.085 Uiso 1 1 calc R . . H2N_6 H 0.3646 0.7286 0.4770 0.085 Uiso 1 1 calc R . . C3_6 C 0.4218(2) 0.7231(5) 0.4286(2) 0.0712(17) Uani 1 1 d DU . . H3M_6 H 0.4419 0.6905 0.4581 0.085 Uiso 1 1 calc R D . H3N_6 H 0.4438 0.7660 0.4138 0.085 Uiso 1 1 calc R . . C4_6 C 0.39833(18) 0.6649(4) 0.3850(2) 0.0589(14) Uani 1 1 d DU D . H4N_6 H 0.4213 0.6551 0.3570 0.071 Uiso 1 1 calc R . . H4O_6 H 0.3898 0.6089 0.4005 0.071 Uiso 1 1 calc R . . C4_7 C 0.4774(6) 0.0150(18) 0.3347(6) 0.095(7) Uiso 0.45(3) 1 d PDU E 1 H4P_7 H 0.4741 0.0613 0.3070 0.114 Uiso 0.45(3) 1 calc PR E 1 H4Q_7 H 0.4809 -0.0406 0.3162 0.114 Uiso 0.45(3) 1 calc PR E 1 C1_7 C 0.4511(9) -0.013(2) 0.4212(7) 0.148(12) Uiso 0.45(3) 1 d PDU E 1 H1O_7 H 0.4487 -0.0765 0.4245 0.178 Uiso 0.45(3) 1 calc PR E 1 H1P_7 H 0.4308 0.0136 0.4475 0.178 Uiso 0.45(3) 1 calc PR E 1 C2_7 C 0.5043(9) 0.015(2) 0.4310(7) 0.125(8) Uiso 0.45(3) 1 d PDU E 1 H2O_7 H 0.5071 0.0686 0.4530 0.150 Uiso 0.45(3) 1 calc PR E 1 H2P_7 H 0.5255 -0.0293 0.4510 0.150 Uiso 0.45(3) 1 calc PR E 1 C3_7 C 0.5209(6) 0.031(2) 0.3768(9) 0.120(8) Uiso 0.45(3) 1 d PDU E 1 H3O_7 H 0.5490 -0.0083 0.3711 0.144 Uiso 0.45(3) 1 calc PR E 1 H3P_7 H 0.5328 0.0905 0.3743 0.144 Uiso 0.45(3) 1 calc PR E 1 O1_7 O 0.4341(5) 0.0143(15) 0.3658(6) 0.117(7) Uiso 0.45(3) 1 d PD E 1 C4_10 C 0.4735(9) -0.002(3) 0.3293(7) 0.224(17) Uiso 0.55(3) 1 d PDU E 2 H4R_10 H 0.4592 0.0535 0.3162 0.269 Uiso 0.55(3) 1 calc PR E 2 H4S_10 H 0.4751 -0.0406 0.2976 0.269 Uiso 0.55(3) 1 calc PR E 2 C1_10 C 0.4663(7) -0.0179(17) 0.4232(6) 0.123(7) Uiso 0.55(3) 1 d PDU E 2 H1Q_10 H 0.4609 -0.0637 0.4497 0.147 Uiso 0.55(3) 1 calc PR E 2 H1R_10 H 0.4519 0.0362 0.4354 0.147 Uiso 0.55(3) 1 calc PR E 2 C2_10 C 0.5208(7) -0.0076(18) 0.4188(9) 0.141(8) Uiso 0.55(3) 1 d PDU E 2 H2Q_10 H 0.5349 0.0412 0.4415 0.169 Uiso 0.55(3) 1 calc PR E 2 H2R_10 H 0.5395 -0.0602 0.4310 0.169 Uiso 0.55(3) 1 calc PR E 2 C3_10 C 0.5240(8) 0.009(2) 0.3605(10) 0.187(12) Uiso 0.55(3) 1 d PDU E 2 H3Q_10 H 0.5482 -0.0314 0.3468 0.224 Uiso 0.55(3) 1 calc PR E 2 H3R_10 H 0.5362 0.0680 0.3556 0.224 Uiso 0.55(3) 1 calc PR E 2 O1_10 O 0.4431(5) -0.0409(13) 0.3685(5) 0.127(6) Uiso 0.55(3) 1 d PD E 2 O1_8 O 0.0721(17) 0.1460(18) 0.0974(17) 0.16(2) Uiso 0.151(4) 1 d PD F 1 C1_8 C 0.0627(17) 0.227(2) 0.0675(11) 0.061(10) Uiso 0.151(4) 1 d PDU F 1 H1S_8 H 0.0328 0.2218 0.0397 0.074 Uiso 0.151(4) 1 calc PR F 1 H1T_8 H 0.0922 0.2435 0.0494 0.074 Uiso 0.151(4) 1 calc PR F 1 C2_8 C 0.0536(17) 0.2890(16) 0.1109(14) 0.071(9) Uiso 0.151(4) 1 d PDU F 1 H2S_8 H 0.0842 0.3242 0.1212 0.085 Uiso 0.151(4) 1 calc PR F 1 H2T_8 H 0.0254 0.3277 0.0977 0.085 Uiso 0.151(4) 1 calc PR F 1 C3_8 C 0.0412(18) 0.239(2) 0.1586(14) 0.064(9) Uiso 0.151(4) 1 d PDU F 1 H3S_8 H 0.0075 0.2561 0.1681 0.076 Uiso 0.151(4) 1 calc PR F 1 H3T_8 H 0.0665 0.2500 0.1906 0.076 Uiso 0.151(4) 1 calc PR F 1 C4_8 C 0.0414(15) 0.1478(18) 0.1424(15) 0.067(10) Uiso 0.151(4) 1 d PDU F 1 H4T_8 H 0.0565 0.1116 0.1731 0.081 Uiso 0.151(4) 1 calc PR F 1 H4U_8 H 0.0067 0.1273 0.1303 0.081 Uiso 0.151(4) 1 calc PR F 1 O1_11 O 0.1166(10) 0.196(2) 0.1154(12) 0.072(10) Uiso 0.148(12) 1 d PD G 2 C2_11 C 0.0323(10) 0.201(4) 0.1295(15) 0.093(13) Uiso 0.148(12) 1 d PDU G 2 H2U_11 H 0.0037 0.2407 0.1210 0.112 Uiso 0.148(12) 1 calc PR G 2 H2V_11 H 0.0188 0.1422 0.1334 0.112 Uiso 0.148(12) 1 calc PR G 2 C1_11 C 0.0659(12) 0.203(5) 0.0856(11) 0.097(16) Uiso 0.148(12) 1 d PDU G 2 H1U_11 H 0.0587 0.1539 0.0601 0.116 Uiso 0.148(12) 1 calc PR G 2 H1V_11 H 0.0618 0.2569 0.0647 0.116 Uiso 0.148(12) 1 calc PR G 2 C3_11 C 0.0636(12) 0.227(3) 0.1803(12) 0.057(10) Uiso 0.148(12) 1 d PDU G 2 H3U_11 H 0.0490 0.2079 0.2133 0.069 Uiso 0.148(12) 1 calc PR G 2 H3V_11 H 0.0694 0.2895 0.1819 0.069 Uiso 0.148(12) 1 calc PR G 2 C4_11 C 0.1101(12) 0.179(3) 0.1724(12) 0.072(12) Uiso 0.148(12) 1 d PDU G 2 H4V_11 H 0.1394 0.1995 0.1973 0.086 Uiso 0.148(12) 1 calc PR G 2 H4W_11 H 0.1058 0.1164 0.1786 0.086 Uiso 0.148(12) 1 calc PR G 2 O1_12 O 0.0983(13) 0.212(2) 0.0932(14) 0.135(13) Uiso 0.201(13) 1 d PD H 3 C2_12 C 0.0302(14) 0.263(3) 0.1345(17) 0.105(12) Uiso 0.201(13) 1 d PDU H 3 H2W_12 H 0.0391 0.3184 0.1525 0.126 Uiso 0.201(13) 1 calc PR H 3 H2X_12 H -0.0070 0.2565 0.1298 0.126 Uiso 0.201(13) 1 calc PR H 3 C1_12 C 0.0503(15) 0.257(3) 0.0811(13) 0.114(14) Uiso 0.201(13) 1 d PDU H 3 H1W_12 H 0.0270 0.2247 0.0543 0.136 Uiso 0.201(13) 1 calc PR H 3 H1X_12 H 0.0554 0.3151 0.0662 0.136 Uiso 0.201(13) 1 calc PR H 3 C3_12 C 0.0543(13) 0.191(3) 0.1670(13) 0.076(9) Uiso 0.201(13) 1 d PDU H 3 H3W_12 H 0.0286 0.1480 0.1735 0.091 Uiso 0.201(13) 1 calc PR H 3 H3X_12 H 0.0700 0.2127 0.2028 0.091 Uiso 0.201(13) 1 calc PR H 3 C4_12 C 0.0935(15) 0.151(2) 0.1372(18) 0.103(13) Uiso 0.201(13) 1 d PDU H 3 H4X_12 H 0.1258 0.1449 0.1612 0.124 Uiso 0.201(13) 1 calc PR H 3 H4Y_12 H 0.0825 0.0944 0.1225 0.124 Uiso 0.201(13) 1 calc PR H 3 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 Cl1 0.0728(10) 0.0998(13) 0.0649(9) 0.0299(9) 0.0024(8) -0.0157(9) Cl2 0.0771(12) 0.148(2) 0.1057(15) -0.0067(14) 0.0230(11) 0.0240(13) Cl3 0.0812(12) 0.1072(15) 0.1259(17) 0.0323(13) -0.0137(11) -0.0578(11) Cl4 0.0694(10) 0.163(2) 0.0403(7) 0.0292(10) 0.0031(7) 0.0091(11) Cl5 0.0853(10) 0.0533(8) 0.0923(12) 0.0006(8) 0.0266(9) -0.0218(8) Cl6 0.0710(9) 0.0750(10) 0.0489(7) -0.0103(7) 0.0039(6) 0.0126(7) Cl7 0.076(3) 0.115(5) 0.113(4) 0.018(4) 0.036(3) 0.011(4) Cl7' 0.064(2) 0.140(5) 0.092(3) -0.032(3) 0.0093(19) -0.004(3) P1 0.0335(5) 0.0313(6) 0.0348(6) -0.0033(4) 0.0026(4) -0.0016(4) P2 0.0401(6) 0.0331(6) 0.0368(6) 0.0019(5) 0.0003(5) -0.0081(5) P3 0.0368(5) 0.0302(5) 0.0334(6) -0.0012(4) 0.0051(4) -0.0019(4) P4 0.0444(6) 0.0334(6) 0.0335(6) 0.0030(5) 0.0057(5) -0.0035(5) Al1 0.0383(7) 0.0313(7) 0.0379(7) -0.0027(5) 0.0049(5) -0.0057(5) Al2 0.0427(7) 0.0316(7) 0.0312(6) -0.0004(5) 0.0012(5) -0.0018(5) Al4 0.0496(9) 0.0757(12) 0.0641(11) 0.0185(9) 0.0082(8) -0.0168(8) Al3 0.0353(6) 0.0319(6) 0.0324(6) 0.0015(5) 0.0010(5) -0.0037(5) Al5 0.0546(8) 0.0522(9) 0.0339(7) 0.0059(6) 0.0057(6) -0.0057(7) O1 0.0518(18) 0.0287(16) 0.0387(17) 0.0010(13) -0.0047(14) -0.0022(14) O2 0.078(3) 0.042(2) 0.054(2) -0.0030(17) -0.0041(19) -0.0143(18) O3 0.0451(18) 0.0467(19) 0.052(2) 0.0080(16) 0.0021(15) -0.0166(15) O4 0.0419(16) 0.0323(16) 0.0366(16) 0.0043(13) -0.0026(13) -0.0068(13) O5 0.0446(17) 0.0371(16) 0.0363(16) 0.0014(13) 0.0064(13) -0.0057(14) O6 0.0438(16) 0.0317(15) 0.0319(15) 0.0020(12) 0.0039(13) -0.0008(13) O7 0.0411(16) 0.0317(15) 0.0343(16) -0.0031(12) 0.0033(13) -0.0028(13) O10 0.046(2) 0.063(3) 0.087(3) 0.016(2) -0.0045(19) -0.0074(19) O11 0.048(2) 0.0361(18) 0.083(3) -0.0042(18) 0.0015(18) -0.0048(16) O12 0.0364(15) 0.0326(16) 0.0392(16) -0.0038(13) 0.0023(13) -0.0019(12) O13 0.0402(16) 0.0343(16) 0.0377(16) 0.0001(13) 0.0058(13) -0.0035(13) O14 0.0428(16) 0.0322(16) 0.0373(16) 0.0002(13) 0.0060(13) -0.0059(13) O15 0.0523(18) 0.0317(16) 0.0440(18) 0.0021(14) 0.0085(15) -0.0043(14) O18 0.0550(19) 0.0437(18) 0.0370(17) 0.0058(14) 0.0048(15) -0.0071(15) O19 0.0414(16) 0.0375(17) 0.0372(16) 0.0067(13) 0.0025(13) -0.0017(13) O20 0.053(2) 0.0396(19) 0.089(3) -0.0094(19) -0.005(2) -0.0033(17) O21 0.043(2) 0.051(2) 0.110(4) -0.005(2) 0.000(2) -0.0066(18) O22 0.0393(16) 0.0348(16) 0.0334(15) -0.0019(13) 0.0008(13) -0.0023(13) O23 0.0331(15) 0.0343(16) 0.0389(16) 0.0003(13) -0.0010(12) -0.0017(12) O26 0.115(4) 0.046(2) 0.056(2) 0.0054(19) -0.008(3) 0.013(2) N1 0.047(2) 0.0325(19) 0.038(2) 0.0016(16) -0.0037(17) -0.0056(16) N2 0.0376(19) 0.041(2) 0.045(2) -0.0073(18) 0.0014(17) 0.0043(17) N3 0.043(2) 0.039(2) 0.049(2) -0.0097(18) 0.0044(18) 0.0052(17) N4 0.073(3) 0.031(2) 0.038(2) -0.0005(17) 0.010(2) -0.0008(19) C1 0.043(2) 0.035(2) 0.032(2) 0.0021(18) 0.0035(18) -0.0025(19) C2 0.052(3) 0.034(2) 0.038(2) 0.0043(19) 0.000(2) -0.001(2) C3 0.057(3) 0.043(3) 0.044(3) 0.003(2) -0.003(2) 0.002(2) C4 0.076(4) 0.052(3) 0.044(3) 0.011(2) 0.000(3) 0.010(3) C5 0.089(4) 0.036(3) 0.064(4) 0.007(3) 0.006(3) 0.010(3) C6 0.073(4) 0.031(3) 0.056(3) 0.004(2) 0.000(3) 0.001(2) C7 0.061(3) 0.035(2) 0.042(3) -0.001(2) 0.006(2) -0.004(2) C8 0.052(3) 0.036(2) 0.046(3) 0.000(2) -0.001(2) -0.006(2) C9 0.050(3) 0.031(2) 0.040(3) -0.0007(19) -0.002(2) -0.007(2) C10 0.038(2) 0.047(3) 0.052(3) -0.004(2) 0.002(2) 0.000(2) C11 0.045(3) 0.047(3) 0.050(3) -0.007(2) 0.004(2) 0.006(2) C12 0.054(3) 0.063(4) 0.063(4) -0.010(3) -0.006(3) -0.004(3) C13 0.062(4) 0.084(5) 0.059(4) -0.011(3) -0.016(3) 0.006(3) C14 0.074(4) 0.075(4) 0.055(4) 0.006(3) -0.012(3) 0.003(3) C15 0.062(3) 0.054(3) 0.055(3) 0.001(3) 0.004(3) 0.007(3) C16 0.045(3) 0.043(3) 0.049(3) -0.008(2) 0.005(2) 0.006(2) C17 0.049(3) 0.036(2) 0.049(3) -0.009(2) 0.007(2) 0.006(2) C18 0.039(2) 0.038(2) 0.038(2) -0.0030(19) 0.0017(19) 0.0004(19) C31 0.055(3) 0.036(3) 0.044(3) -0.001(2) 0.009(2) 0.000(2) C32 0.084(4) 0.036(3) 0.049(3) -0.003(2) 0.018(3) 0.000(3) C33 0.085(4) 0.040(3) 0.061(3) -0.013(3) 0.008(3) -0.012(3) C34 0.122(6) 0.040(3) 0.074(4) -0.001(3) 0.009(4) -0.018(4) C35 0.151(7) 0.040(3) 0.073(4) -0.003(3) 0.030(5) -0.023(4) C36 0.156(7) 0.040(3) 0.044(3) 0.007(3) 0.005(4) 0.000(4) C37 0.109(5) 0.035(3) 0.038(3) -0.006(2) 0.007(3) -0.004(3) C38 0.089(4) 0.038(3) 0.041(3) 0.003(2) 0.005(3) 0.007(3) C39 0.054(3) 0.041(3) 0.045(3) 0.008(2) 0.003(2) 0.004(2) C40 0.045(3) 0.039(3) 0.056(3) -0.007(2) 0.006(2) 0.000(2) C41 0.055(3) 0.043(3) 0.060(3) -0.007(2) 0.007(3) 0.006(2) C42 0.064(3) 0.048(3) 0.078(4) 0.007(3) 0.003(3) 0.001(3) C43 0.087(5) 0.059(4) 0.099(5) 0.016(4) 0.007(4) 0.012(4) C44 0.072(4) 0.088(5) 0.083(5) 0.014(4) -0.010(4) 0.030(4) C45 0.060(4) 0.074(4) 0.079(4) -0.013(4) -0.005(3) 0.017(3) C46 0.045(3) 0.052(3) 0.060(3) -0.006(3) -0.001(2) 0.003(2) C47 0.038(2) 0.045(3) 0.065(3) -0.011(2) 0.005(2) 0.003(2) C48 0.046(3) 0.040(3) 0.040(2) -0.003(2) 0.008(2) 0.002(2) O1_1 0.0340(15) 0.0457(18) 0.0392(17) 0.0068(14) -0.0020(13) -0.0028(13) C1_1 0.039(3) 0.059(3) 0.067(3) 0.007(3) 0.008(2) -0.003(2) C2_1 0.042(3) 0.091(5) 0.081(4) 0.021(4) 0.009(3) 0.000(3) C3_1 0.047(3) 0.093(5) 0.070(4) 0.005(3) -0.004(3) 0.011(3) C4_1 0.050(3) 0.078(4) 0.063(4) 0.022(3) 0.000(3) 0.007(3) O1_2 0.0486(17) 0.0413(18) 0.0336(16) -0.0050(14) 0.0047(14) -0.0072(14) C1_2 0.105(5) 0.085(5) 0.058(4) -0.029(3) 0.015(4) -0.044(4) C2_2 0.183(8) 0.117(7) 0.108(6) -0.065(5) 0.061(6) -0.060(6) C3_2 0.123(6) 0.105(6) 0.075(4) -0.036(4) 0.046(4) -0.015(5) C4_2 0.086(4) 0.091(5) 0.065(4) -0.026(4) 0.032(3) -0.025(4) O1_3 0.0485(18) 0.0417(18) 0.0381(17) -0.0086(14) -0.0033(14) 0.0026(15) C1_3 0.063(3) 0.053(3) 0.052(3) -0.020(3) -0.003(3) -0.005(3) C2_3 0.111(6) 0.121(6) 0.104(6) -0.062(5) -0.051(5) 0.036(5) C3_3 0.053(3) 0.091(5) 0.070(4) -0.006(4) -0.012(3) 0.001(3) C4_3 0.060(4) 0.076(4) 0.095(5) -0.038(4) -0.019(3) 0.020(3) O1_4 0.063(2) 0.0460(19) 0.0349(17) 0.0036(15) 0.0094(15) 0.0000(16) C1_4 0.109(5) 0.051(3) 0.039(3) 0.010(2) 0.011(3) -0.006(3) C2_4 0.115(5) 0.071(4) 0.050(3) 0.011(3) 0.027(4) -0.001(4) C3_4 0.105(5) 0.089(5) 0.073(4) 0.005(4) 0.051(4) 0.008(4) C4_4 0.077(4) 0.072(4) 0.049(3) 0.008(3) 0.027(3) 0.011(3) O1_5 0.044(3) 0.038(4) 0.045(4) -0.005(3) 0.004(4) -0.011(3) C1_5 0.049(6) 0.053(7) 0.057(7) -0.006(3) 0.025(4) -0.004(4) C2_5 0.086(7) 0.076(6) 0.074(6) -0.007(6) 0.039(5) -0.028(5) C3_5 0.059(5) 0.058(5) 0.061(5) 0.003(4) 0.012(4) -0.029(4) C4_5 0.052(5) 0.043(4) 0.062(5) -0.014(4) 0.018(4) -0.023(3) O1_6 0.0443(17) 0.0420(18) 0.0408(17) -0.0090(14) 0.0030(14) -0.0020(14) C1_6 0.084(4) 0.063(4) 0.045(3) -0.010(3) 0.004(3) 0.006(3) C2_6 0.073(4) 0.072(4) 0.065(4) -0.024(3) 0.001(3) -0.012(3) C3_6 0.059(3) 0.093(5) 0.059(3) -0.017(3) -0.006(3) -0.006(3) C4_6 0.048(3) 0.076(4) 0.050(3) -0.004(3) -0.007(2) 0.000(3) _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 Cl1 Al4 2.140(2) . ? Cl2 Al4 2.137(3) . ? Cl3 Al4 2.108(3) . ? Cl4 Al5 2.114(2) . ? Cl5 Al5 2.136(2) . ? Cl6 Al5 2.138(2) . ? P1 O23 1.509(3) . ? P1 O7 1.518(3) . ? P1 O12 1.522(3) . ? P1 C18 1.807(5) . ? P2 O4 1.495(3) . ? P2 O5 1.515(3) . ? P2 O3 1.530(3) . ? P2 C9 1.800(5) . ? P3 O22 1.509(3) . ? P3 O13 1.525(3) . ? P3 O6 1.531(3) . ? P3 C48 1.804(5) . ? P4 O19 1.503(3) . ? P4 O14 1.508(3) . ? P4 O18 1.525(3) . ? P4 C39 1.804(5) . ? Al1 O13 1.818(3) . ? Al1 O12 1.825(3) . ? Al1 O14 1.831(3) . ? Al1 O1_9 1.930(19) . ? Al1 O1_6 1.947(3) . ? Al1 O15 1.971(3) . ? Al1 O1_5 1.986(7) . ? Al2 O5 1.808(3) . ? Al2 O6 1.819(3) . ? Al2 O7 1.829(3) . ? Al2 O1_3 1.961(3) . ? Al2 O1_4 1.964(3) . ? Al2 O1 2.001(3) . ? Al4 O3 1.733(4) . ? Al3 O19 1.840(3) . ? Al3 O4 1.852(3) . ? Al3 O23 1.857(3) . ? Al3 O22 1.859(3) . ? Al3 O1_1 1.957(3) . ? Al3 O1_2 1.997(3) . ? Al5 O18 1.742(3) . ? O1 C1 1.224(5) . ? O2 C8 1.204(6) . ? O10 C10 1.206(6) . ? O11 C17 1.212(6) . ? O15 C31 1.228(6) . ? O20 C40 1.193(6) . ? O21 C47 1.202(6) . ? O26 C38 1.198(7) . ? N1 C1 1.373(6) . ? N1 C8 1.430(6) . ? N1 C9 1.440(6) . ? N2 C10 1.394(6) . ? N2 C17 1.406(6) . ? N2 C18 1.452(6) . ? N3 C40 1.384(6) . ? N3 C47 1.410(6) . ? N3 C48 1.447(6) . ? N4 C31 1.361(7) . ? N4 C38 1.441(6) . ? N4 C39 1.458(6) . ? C1 C2 1.478(6) . ? C2 C3 1.384(7) . ? C2 C7 1.389(7) . ? C3 C4 1.393(7) . ? C3 H3 0.9500 . ? C4 C5 1.400(8) . ? C4 H4A 0.9500 . ? C5 C6 1.347(8) . ? C5 H5A 0.9500 . ? C6 C7 1.373(7) . ? C6 H6A 0.9500 . ? C7 C8 1.482(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.486(7) . ? C11 C12 1.383(7) . ? C11 C16 1.389(7) . ? C12 C13 1.386(9) . ? C12 H12A 0.9500 . ? C13 C14 1.365(9) . ? C13 H13A 0.9500 . ? C14 C15 1.392(8) . ? C14 H14A 0.9500 . ? C15 C16 1.362(8) . ? C15 H15 0.9500 . ? C16 C17 1.469(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C31 C32 1.477(7) . ? C32 C37 1.378(8) . ? C32 C33 1.379(8) . ? C33 C34 1.385(8) . ? C33 H33 0.9500 . ? C34 C35 1.382(10) . ? C34 H34 0.9500 . ? C35 C36 1.413(11) . ? C35 H35 0.9500 . ? C36 C37 1.396(8) . ? C36 H36 0.9500 . ? C37 C38 1.477(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.508(7) . ? C41 C42 1.363(8) . ? C41 C46 1.378(8) . ? C42 C43 1.398(9) . ? C42 H42 0.9500 . ? C43 C44 1.366(11) . ? C43 H43 0.9500 . ? C44 C45 1.372(10) . ? C44 H44 0.9500 . ? C45 C46 1.391(8) . ? C45 H45 0.9500 . ? C46 C47 1.482(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O1_1 C4_1 1.457(5) . ? O1_1 C1_1 1.464(5) . ? C1_1 C2_1 1.494(5) . ? C1_1 H1A_1 0.9900 . ? C1_1 H1B_1 0.9900 . ? C2_1 C3_1 1.487(6) . ? C2_1 H2A_1 0.9900 . ? C2_1 H2B_1 0.9900 . ? C3_1 C4_1 1.493(6) . ? C3_1 H3A_1 0.9900 . ? C3_1 H3B_1 0.9900 . ? C4_1 H4B_1 0.9900 . ? C4_1 H4C_1 0.9900 . ? O1_2 C4_2 1.453(5) . ? O1_2 C1_2 1.454(5) . ? C1_2 C2_2 1.461(6) . ? C1_2 H1C_2 0.9900 . ? C1_2 H1D_2 0.9900 . ? C2_2 C3_2 1.458(7) . ? C2_2 H2C_2 0.9900 . ? C2_2 H2D_2 0.9900 . ? C3_2 C4_2 1.477(6) . ? C3_2 H3C_2 0.9900 . ? C3_2 H3D_2 0.9900 . ? C4_2 H4D_2 0.9900 . ? C4_2 H4E_2 0.9900 . ? O1_3 C4_3 1.448(5) . ? O1_3 C1_3 1.464(5) . ? C1_3 C2_3 1.478(6) . ? C1_3 H1E_3 0.9900 . ? C1_3 H1F_3 0.9900 . ? C2_3 C3_3 1.468(7) . ? C2_3 H2E_3 0.9900 . ? C2_3 H2F_3 0.9900 . ? C3_3 C4_3 1.476(6) . ? C3_3 H3E_3 0.9900 . ? C3_3 H3F_3 0.9900 . ? C4_3 H4F_3 0.9900 . ? C4_3 H4G_3 0.9900 . ? O1_4 C1_4 1.458(5) . ? O1_4 C4_4 1.459(5) . ? C1_4 C2_4 1.500(6) . ? C1_4 H1G_4 0.9900 . ? C1_4 H1H_4 0.9900 . ? C2_4 C3_4 1.478(7) . ? C2_4 H2G_4 0.9900 . ? C2_4 H2H_4 0.9900 . ? C3_4 C4_4 1.500(6) . ? C3_4 H3G_4 0.9900 . ? C3_4 H3H_4 0.9900 . ? C4_4 H4H_4 0.9900 . ? C4_4 H4I_4 0.9900 . ? O1_5 C1_5 1.455(6) . ? O1_5 C4_5 1.468(6) . ? C1_5 C2_5 1.484(7) . ? C1_5 H1I_5 0.9900 . ? C1_5 H1J_5 0.9900 . ? C2_5 C3_5 1.483(7) . ? C2_5 H2I_5 0.9900 . ? C2_5 H2J_5 0.9900 . ? C3_5 C4_5 1.483(6) . ? C3_5 H3I_5 0.9900 . ? C3_5 H3J_5 0.9900 . ? C4_5 H4J_5 0.9900 . ? C4_5 H4K_5 0.9900 . ? O1_9 C1_9 1.460(7) . ? O1_9 C4_9 1.466(7) . ? C1_9 C2_9 1.485(8) . ? C1_9 H1K_9 0.9900 . ? C1_9 H1L_9 0.9900 . ? C2_9 C3_9 1.480(9) . ? C2_9 H2K_9 0.9900 . ? C2_9 H2L_9 0.9900 . ? C3_9 C4_9 1.486(8) . ? C3_9 H3K_9 0.9900 . ? C3_9 H3L_9 0.9900 . ? C4_9 H4L_9 0.9900 . ? C4_9 H4M_9 0.9900 . ? O1_6 C4_6 1.455(5) . ? O1_6 C1_6 1.455(5) . ? C1_6 C2_6 1.485(6) . ? C1_6 H1M_6 0.9900 . ? C1_6 H1N_6 0.9900 . ? C2_6 C3_6 1.483(6) . ? C2_6 H2M_6 0.9900 . ? C2_6 H2N_6 0.9900 . ? C3_6 C4_6 1.487(6) . ? C3_6 H3M_6 0.9900 . ? C3_6 H3N_6 0.9900 . ? C4_6 H4N_6 0.9900 . ? C4_6 H4O_6 0.9900 . ? C4_7 O1_7 1.462(7) . ? C4_7 C3_7 1.480(8) . ? C4_7 H4P_7 0.9900 . ? C4_7 H4Q_7 0.9900 . ? C1_7 O1_7 1.454(7) . ? C1_7 C2_7 1.481(8) . ? C1_7 H1O_7 0.9900 . ? C1_7 H1P_7 0.9900 . ? C2_7 C3_7 1.479(8) . ? C2_7 H2O_7 0.9900 . ? C2_7 H2P_7 0.9900 . ? C3_7 H3O_7 0.9900 . ? C3_7 H3P_7 0.9900 . ? C4_10 O1_10 1.464(7) . ? C4_10 C3_10 1.480(8) . ? C4_10 H4R_10 0.9900 . ? C4_10 H4S_10 0.9900 . ? C1_10 O1_10 1.460(7) . ? C1_10 C2_10 1.480(8) . ? C1_10 H1Q_10 0.9900 . ? C1_10 H1R_10 0.9900 . ? C2_10 C3_10 1.475(8) . ? C2_10 H2Q_10 0.9900 . ? C2_10 H2R_10 0.9900 . ? C3_10 H3Q_10 0.9900 . ? C3_10 H3R_10 0.9900 . ? O1_8 C4_8 1.459(8) . ? O1_8 C1_8 1.464(8) . ? C1_8 C2_8 1.489(8) . ? C1_8 H1S_8 0.9900 . ? C1_8 H1T_8 0.9900 . ? C2_8 C3_8 1.479(9) . ? C2_8 H2S_8 0.9900 . ? C2_8 H2T_8 0.9900 . ? C3_8 C4_8 1.485(8) . ? C3_8 H3S_8 0.9900 . ? C3_8 H3T_8 0.9900 . ? C4_8 H4T_8 0.9900 . ? C4_8 H4U_8 0.9900 . ? O1_11 C4_11 1.463(8) . ? O1_11 C1_11 1.465(8) . ? C2_11 C3_11 1.476(9) . ? C2_11 C1_11 1.487(8) . ? C2_11 H2U_11 0.9900 . ? C2_11 H2V_11 0.9900 . ? C1_11 H1U_11 0.9900 . ? C1_11 H1V_11 0.9900 . ? C3_11 C4_11 1.486(8) . ? C3_11 H3U_11 0.9900 . ? C3_11 H3V_11 0.9900 . ? C4_11 H4V_11 0.9900 . ? C4_11 H4W_11 0.9900 . ? O1_12 C4_12 1.459(8) . ? O1_12 C1_12 1.462(8) . ? C2_12 C3_12 1.475(9) . ? C2_12 C1_12 1.485(8) . ? C2_12 H2W_12 0.9900 . ? C2_12 H2X_12 0.9900 . ? C1_12 H1W_12 0.9900 . ? C1_12 H1X_12 0.9900 . ? C3_12 C4_12 1.486(8) . ? C3_12 H3W_12 0.9900 . ? C3_12 H3X_12 0.9900 . ? C4_12 H4X_12 0.9900 . ? C4_12 H4Y_12 0.9900 . ? 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 O23 P1 O7 113.18(17) . . ? O23 P1 O12 113.48(17) . . ? O7 P1 O12 111.31(17) . . ? O23 P1 C18 105.63(19) . . ? O7 P1 C18 104.9(2) . . ? O12 P1 C18 107.59(19) . . ? O4 P2 O5 115.49(18) . . ? O4 P2 O3 110.44(18) . . ? O5 P2 O3 109.74(19) . . ? O4 P2 C9 106.4(2) . . ? O5 P2 C9 107.1(2) . . ? O3 P2 C9 107.3(2) . . ? O22 P3 O13 111.04(17) . . ? O22 P3 O6 113.86(17) . . ? O13 P3 O6 112.30(17) . . ? O22 P3 C48 107.7(2) . . ? O13 P3 C48 106.9(2) . . ? O6 P3 C48 104.4(2) . . ? O19 P4 O14 115.33(17) . . ? O19 P4 O18 110.36(18) . . ? O14 P4 O18 110.18(18) . . ? O19 P4 C39 106.2(2) . . ? O14 P4 C39 106.7(2) . . ? O18 P4 C39 107.6(2) . . ? O13 Al1 O12 96.67(14) . . ? O13 Al1 O14 98.47(15) . . ? O12 Al1 O14 95.74(15) . . ? O13 Al1 O1_9 168.3(9) . . ? O12 Al1 O1_9 94.9(9) . . ? O14 Al1 O1_9 82.2(10) . . ? O13 Al1 O1_6 91.11(14) . . ? O12 Al1 O1_6 91.04(14) . . ? O14 Al1 O1_6 167.52(15) . . ? O1_9 Al1 O1_6 86.8(10) . . ? O13 Al1 O15 87.63(14) . . ? O12 Al1 O15 173.71(15) . . ? O14 Al1 O15 88.14(14) . . ? O1_9 Al1 O15 80.7(9) . . ? O1_6 Al1 O15 84.26(14) . . ? O13 Al1 O1_5 171.0(3) . . ? O12 Al1 O1_5 88.3(4) . . ? O14 Al1 O1_5 88.4(4) . . ? O1_9 Al1 O1_5 8.7(13) . . ? O1_6 Al1 O1_5 81.3(4) . . ? O15 Al1 O1_5 86.9(3) . . ? O5 Al2 O6 95.28(15) . . ? O5 Al2 O7 98.91(14) . . ? O6 Al2 O7 96.06(14) . . ? O5 Al2 O1_3 167.99(16) . . ? O6 Al2 O1_3 91.70(14) . . ? O7 Al2 O1_3 90.03(14) . . ? O5 Al2 O1_4 86.74(15) . . ? O6 Al2 O1_4 89.63(14) . . ? O7 Al2 O1_4 171.54(15) . . ? O1_3 Al2 O1_4 83.54(15) . . ? O5 Al2 O1 88.78(14) . . ? O6 Al2 O1 174.37(15) . . ? O7 Al2 O1 87.13(14) . . ? O1_3 Al2 O1 83.65(14) . . ? O1_4 Al2 O1 86.70(14) . . ? O3 Al4 Cl3 106.39(16) . . ? O3 Al4 Cl2 107.91(16) . . ? Cl3 Al4 Cl2 111.53(12) . . ? O3 Al4 Cl1 109.84(15) . . ? Cl3 Al4 Cl1 110.71(11) . . ? Cl2 Al4 Cl1 110.34(12) . . ? O19 Al3 O4 169.39(15) . . ? O19 Al3 O23 92.50(14) . . ? O4 Al3 O23 94.14(14) . . ? O19 Al3 O22 94.66(14) . . ? O4 Al3 O22 92.86(14) . . ? O23 Al3 O22 96.00(14) . . ? O19 Al3 O1_1 86.54(14) . . ? O4 Al3 O1_1 85.93(14) . . ? O23 Al3 O1_1 173.47(15) . . ? O22 Al3 O1_1 90.51(14) . . ? O19 Al3 O1_2 86.05(14) . . ? O4 Al3 O1_2 85.93(14) . . ? O23 Al3 O1_2 87.92(14) . . ? O22 Al3 O1_2 175.98(14) . . ? O1_1 Al3 O1_2 85.58(14) . . ? O18 Al5 Cl4 107.36(14) . . ? O18 Al5 Cl5 108.75(14) . . ? Cl4 Al5 Cl5 111.05(11) . . ? O18 Al5 Cl6 109.93(14) . . ? Cl4 Al5 Cl6 109.84(10) . . ? Cl5 Al5 Cl6 109.86(9) . . ? C1 O1 Al2 140.9(3) . . ? P2 O3 Al4 139.5(2) . . ? P2 O4 Al3 141.4(2) . . ? P2 O5 Al2 137.8(2) . . ? P3 O6 Al2 137.30(19) . . ? P1 O7 Al2 143.0(2) . . ? P1 O12 Al1 136.63(19) . . ? P3 O13 Al1 144.5(2) . . ? P4 O14 Al1 136.6(2) . . ? C31 O15 Al1 140.6(3) . . ? P4 O18 Al5 142.0(2) . . ? P4 O19 Al3 144.0(2) . . ? P3 O22 Al3 143.4(2) . . ? P1 O23 Al3 145.8(2) . . ? C1 N1 C8 110.4(4) . . ? C1 N1 C9 127.3(4) . . ? C8 N1 C9 122.1(4) . . ? C10 N2 C17 111.3(4) . . ? C10 N2 C18 124.9(4) . . ? C17 N2 C18 123.8(4) . . ? C40 N3 C47 112.6(4) . . ? C40 N3 C48 124.9(4) . . ? C47 N3 C48 122.4(4) . . ? C31 N4 C38 110.5(4) . . ? C31 N4 C39 127.1(4) . . ? C38 N4 C39 122.2(4) . . ? O1 C1 N1 127.4(4) . . ? O1 C1 C2 125.7(4) . . ? N1 C1 C2 107.0(4) . . ? C3 C2 C7 121.1(5) . . ? C3 C2 C1 130.0(4) . . ? C7 C2 C1 108.9(4) . . ? C2 C3 C4 117.1(5) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C3 C4 C5 120.1(5) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 122.4(5) . . ? C6 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C5 C6 C7 117.7(5) . . ? C5 C6 H6A 121.2 . . ? C7 C6 H6A 121.2 . . ? C6 C7 C2 121.5(5) . . ? C6 C7 C8 131.4(5) . . ? C2 C7 C8 107.0(4) . . ? O2 C8 N1 122.9(5) . . ? O2 C8 C7 130.8(5) . . ? N1 C8 C7 106.4(4) . . ? N1 C9 P2 114.1(3) . . ? N1 C9 H9A 108.7 . . ? P2 C9 H9A 108.7 . . ? N1 C9 H9B 108.7 . . ? P2 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? O10 C10 N2 124.4(5) . . ? O10 C10 C11 130.0(5) . . ? N2 C10 C11 105.6(4) . . ? C12 C11 C16 121.4(5) . . ? C12 C11 C10 130.0(5) . . ? C16 C11 C10 108.6(4) . . ? C11 C12 C13 115.7(6) . . ? C11 C12 H12A 122.1 . . ? C13 C12 H12A 122.1 . . ? C14 C13 C12 122.9(6) . . ? C14 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C13 C14 C15 121.0(6) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C16 C15 C14 116.8(6) . . ? C16 C15 H15 121.6 . . ? C14 C15 H15 121.6 . . ? C15 C16 C11 122.1(5) . . ? C15 C16 C17 130.1(5) . . ? C11 C16 C17 107.8(4) . . ? O11 C17 N2 124.0(5) . . ? O11 C17 C16 129.4(5) . . ? N2 C17 C16 106.6(4) . . ? N2 C18 P1 112.4(3) . . ? N2 C18 H18A 109.1 . . ? P1 C18 H18A 109.1 . . ? N2 C18 H18B 109.1 . . ? P1 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? O15 C31 N4 127.1(5) . . ? O15 C31 C32 125.0(5) . . ? N4 C31 C32 107.9(4) . . ? C37 C32 C33 122.3(5) . . ? C37 C32 C31 107.7(5) . . ? C33 C32 C31 130.0(5) . . ? C32 C33 C34 117.4(6) . . ? C32 C33 H33 121.3 . . ? C34 C33 H33 121.3 . . ? C35 C34 C33 120.9(7) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 122.4(6) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C37 C36 C35 115.3(6) . . ? C37 C36 H36 122.3 . . ? C35 C36 H36 122.3 . . ? C32 C37 C36 121.7(6) . . ? C32 C37 C38 108.8(5) . . ? C36 C37 C38 129.4(6) . . ? O26 C38 N4 123.1(5) . . ? O26 C38 C37 131.9(5) . . ? N4 C38 C37 105.0(5) . . ? N4 C39 P4 113.6(4) . . ? N4 C39 H39A 108.8 . . ? P4 C39 H39A 108.8 . . ? N4 C39 H39B 108.8 . . ? P4 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? O20 C40 N3 125.7(5) . . ? O20 C40 C41 128.9(5) . . ? N3 C40 C41 105.3(4) . . ? C42 C41 C46 122.8(5) . . ? C42 C41 C40 129.5(5) . . ? C46 C41 C40 107.7(5) . . ? C41 C42 C43 116.8(6) . . ? C41 C42 H42 121.6 . . ? C43 C42 H42 121.6 . . ? C44 C43 C42 120.5(6) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 122.5(6) . . ? C43 C44 H44 118.7 . . ? C45 C44 H44 118.7 . . ? C44 C45 C46 117.1(7) . . ? C44 C45 H45 121.4 . . ? C46 C45 H45 121.4 . . ? C41 C46 C45 120.1(6) . . ? C41 C46 C47 109.2(5) . . ? C45 C46 C47 130.7(6) . . ? O21 C47 N3 124.4(5) . . ? O21 C47 C46 130.6(5) . . ? N3 C47 C46 105.0(4) . . ? N3 C48 P3 113.1(3) . . ? N3 C48 H48A 108.9 . . ? P3 C48 H48A 108.9 . . ? N3 C48 H48B 108.9 . . ? P3 C48 H48B 108.9 . . ? H48A C48 H48B 107.8 . . ? C4_1 O1_1 C1_1 109.4(3) . . ? C4_1 O1_1 Al3 125.4(3) . . ? C1_1 O1_1 Al3 125.2(3) . . ? O1_1 C1_1 C2_1 104.8(4) . . ? O1_1 C1_1 H1A_1 110.8 . . ? C2_1 C1_1 H1A_1 110.8 . . ? O1_1 C1_1 H1B_1 110.8 . . ? C2_1 C1_1 H1B_1 110.8 . . ? H1A_1 C1_1 H1B_1 108.9 . . ? C3_1 C2_1 C1_1 103.7(4) . . ? C3_1 C2_1 H2A_1 111.0 . . ? C1_1 C2_1 H2A_1 111.0 . . ? C3_1 C2_1 H2B_1 111.0 . . ? C1_1 C2_1 H2B_1 111.0 . . ? H2A_1 C2_1 H2B_1 109.0 . . ? C2_1 C3_1 C4_1 102.9(4) . . ? C2_1 C3_1 H3A_1 111.2 . . ? C4_1 C3_1 H3A_1 111.2 . . ? C2_1 C3_1 H3B_1 111.2 . . ? C4_1 C3_1 H3B_1 111.2 . . ? H3A_1 C3_1 H3B_1 109.1 . . ? O1_1 C4_1 C3_1 103.4(4) . . ? O1_1 C4_1 H4B_1 111.1 . . ? C3_1 C4_1 H4B_1 111.1 . . ? O1_1 C4_1 H4C_1 111.1 . . ? C3_1 C4_1 H4C_1 111.1 . . ? H4B_1 C4_1 H4C_1 109.1 . . ? C4_2 O1_2 C1_2 109.1(4) . . ? C4_2 O1_2 Al3 125.7(3) . . ? C1_2 O1_2 Al3 125.0(3) . . ? O1_2 C1_2 C2_2 107.4(5) . . ? O1_2 C1_2 H1C_2 110.2 . . ? C2_2 C1_2 H1C_2 110.2 . . ? O1_2 C1_2 H1D_2 110.2 . . ? C2_2 C1_2 H1D_2 110.2 . . ? H1C_2 C1_2 H1D_2 108.5 . . ? C3_2 C2_2 C1_2 108.0(5) . . ? C3_2 C2_2 H2C_2 110.1 . . ? C1_2 C2_2 H2C_2 110.1 . . ? C3_2 C2_2 H2D_2 110.1 . . ? C1_2 C2_2 H2D_2 110.1 . . ? H2C_2 C2_2 H2D_2 108.4 . . ? C2_2 C3_2 C4_2 107.7(5) . . ? C2_2 C3_2 H3C_2 110.2 . . ? C4_2 C3_2 H3C_2 110.2 . . ? C2_2 C3_2 H3D_2 110.2 . . ? C4_2 C3_2 H3D_2 110.2 . . ? H3C_2 C3_2 H3D_2 108.5 . . ? O1_2 C4_2 C3_2 107.0(4) . . ? O1_2 C4_2 H4D_2 110.3 . . ? C3_2 C4_2 H4D_2 110.3 . . ? O1_2 C4_2 H4E_2 110.3 . . ? C3_2 C4_2 H4E_2 110.3 . . ? H4D_2 C4_2 H4E_2 108.6 . . ? C4_3 O1_3 C1_3 110.3(3) . . ? C4_3 O1_3 Al2 124.8(3) . . ? C1_3 O1_3 Al2 124.9(3) . . ? O1_3 C1_3 C2_3 105.1(4) . . ? O1_3 C1_3 H1E_3 110.7 . . ? C2_3 C1_3 H1E_3 110.7 . . ? O1_3 C1_3 H1F_3 110.7 . . ? C2_3 C1_3 H1F_3 110.7 . . ? H1E_3 C1_3 H1F_3 108.8 . . ? C3_3 C2_3 C1_3 108.1(5) . . ? C3_3 C2_3 H2E_3 110.1 . . ? C1_3 C2_3 H2E_3 110.1 . . ? C3_3 C2_3 H2F_3 110.1 . . ? C1_3 C2_3 H2F_3 110.1 . . ? H2E_3 C2_3 H2F_3 108.4 . . ? C2_3 C3_3 C4_3 106.8(5) . . ? C2_3 C3_3 H3E_3 110.4 . . ? C4_3 C3_3 H3E_3 110.4 . . ? C2_3 C3_3 H3F_3 110.4 . . ? C4_3 C3_3 H3F_3 110.4 . . ? H3E_3 C3_3 H3F_3 108.6 . . ? O1_3 C4_3 C3_3 106.9(4) . . ? O1_3 C4_3 H4F_3 110.3 . . ? C3_3 C4_3 H4F_3 110.3 . . ? O1_3 C4_3 H4G_3 110.3 . . ? C3_3 C4_3 H4G_3 110.3 . . ? H4F_3 C4_3 H4G_3 108.6 . . ? C1_4 O1_4 C4_4 108.8(4) . . ? C1_4 O1_4 Al2 127.7(3) . . ? C4_4 O1_4 Al2 122.7(3) . . ? O1_4 C1_4 C2_4 104.2(4) . . ? O1_4 C1_4 H1G_4 110.9 . . ? C2_4 C1_4 H1G_4 110.9 . . ? O1_4 C1_4 H1H_4 110.9 . . ? C2_4 C1_4 H1H_4 110.9 . . ? H1G_4 C1_4 H1H_4 108.9 . . ? C3_4 C2_4 C1_4 101.2(5) . . ? C3_4 C2_4 H2G_4 111.5 . . ? C1_4 C2_4 H2G_4 111.5 . . ? C3_4 C2_4 H2H_4 111.5 . . ? C1_4 C2_4 H2H_4 111.5 . . ? H2G_4 C2_4 H2H_4 109.4 . . ? C2_4 C3_4 C4_4 104.5(5) . . ? C2_4 C3_4 H3G_4 110.9 . . ? C4_4 C3_4 H3G_4 110.9 . . ? C2_4 C3_4 H3H_4 110.9 . . ? C4_4 C3_4 H3H_4 110.9 . . ? H3G_4 C3_4 H3H_4 108.9 . . ? O1_4 C4_4 C3_4 104.2(4) . . ? O1_4 C4_4 H4H_4 110.9 . . ? C3_4 C4_4 H4H_4 110.9 . . ? O1_4 C4_4 H4I_4 110.9 . . ? C3_4 C4_4 H4I_4 110.9 . . ? H4H_4 C4_4 H4I_4 108.9 . . ? C1_5 O1_5 C4_5 107.6(5) . . ? C1_5 O1_5 Al1 124.9(6) . . ? C4_5 O1_5 Al1 126.8(6) . . ? O1_5 C1_5 C2_5 106.5(6) . . ? O1_5 C1_5 H1I_5 110.4 . . ? C2_5 C1_5 H1I_5 110.4 . . ? O1_5 C1_5 H1J_5 110.4 . . ? C2_5 C1_5 H1J_5 110.4 . . ? H1I_5 C1_5 H1J_5 108.6 . . ? C3_5 C2_5 C1_5 106.4(6) . . ? C3_5 C2_5 H2I_5 110.4 . . ? C1_5 C2_5 H2I_5 110.4 . . ? C3_5 C2_5 H2J_5 110.4 . . ? C1_5 C2_5 H2J_5 110.4 . . ? H2I_5 C2_5 H2J_5 108.6 . . ? C2_5 C3_5 C4_5 105.1(6) . . ? C2_5 C3_5 H3I_5 110.7 . . ? C4_5 C3_5 H3I_5 110.7 . . ? C2_5 C3_5 H3J_5 110.7 . . ? C4_5 C3_5 H3J_5 110.7 . . ? H3I_5 C3_5 H3J_5 108.8 . . ? O1_5 C4_5 C3_5 103.7(6) . . ? O1_5 C4_5 H4J_5 111.0 . . ? C3_5 C4_5 H4J_5 111.0 . . ? O1_5 C4_5 H4K_5 111.0 . . ? C3_5 C4_5 H4K_5 111.0 . . ? H4J_5 C4_5 H4K_5 109.0 . . ? C1_9 O1_9 C4_9 107.0(10) . . ? C1_9 O1_9 Al1 121.1(16) . . ? C4_9 O1_9 Al1 131.6(18) . . ? O1_9 C1_9 C2_9 105.1(10) . . ? O1_9 C1_9 H1K_9 110.7 . . ? C2_9 C1_9 H1K_9 110.7 . . ? O1_9 C1_9 H1L_9 110.7 . . ? C2_9 C1_9 H1L_9 110.7 . . ? H1K_9 C1_9 H1L_9 108.8 . . ? C3_9 C2_9 C1_9 107.9(10) . . ? C3_9 C2_9 H2K_9 110.1 . . ? C1_9 C2_9 H2K_9 110.1 . . ? C3_9 C2_9 H2L_9 110.1 . . ? C1_9 C2_9 H2L_9 110.1 . . ? H2K_9 C2_9 H2L_9 108.4 . . ? C2_9 C3_9 C4_9 103.5(15) . . ? C2_9 C3_9 H3K_9 111.1 . . ? C4_9 C3_9 H3K_9 111.1 . . ? C2_9 C3_9 H3L_9 111.1 . . ? C4_9 C3_9 H3L_9 111.1 . . ? H3K_9 C3_9 H3L_9 109.0 . . ? O1_9 C4_9 C3_9 103.7(10) . . ? O1_9 C4_9 H4L_9 111.0 . . ? C3_9 C4_9 H4L_9 111.0 . . ? O1_9 C4_9 H4M_9 111.0 . . ? C3_9 C4_9 H4M_9 111.0 . . ? H4L_9 C4_9 H4M_9 109.0 . . ? C4_6 O1_6 C1_6 109.5(3) . . ? C4_6 O1_6 Al1 123.3(3) . . ? C1_6 O1_6 Al1 127.2(3) . . ? O1_6 C1_6 C2_6 104.9(4) . . ? O1_6 C1_6 H1M_6 110.8 . . ? C2_6 C1_6 H1M_6 110.8 . . ? O1_6 C1_6 H1N_6 110.8 . . ? C2_6 C1_6 H1N_6 110.8 . . ? H1M_6 C1_6 H1N_6 108.8 . . ? C3_6 C2_6 C1_6 105.8(4) . . ? C3_6 C2_6 H2M_6 110.6 . . ? C1_6 C2_6 H2M_6 110.6 . . ? C3_6 C2_6 H2N_6 110.6 . . ? C1_6 C2_6 H2N_6 110.6 . . ? H2M_6 C2_6 H2N_6 108.7 . . ? C2_6 C3_6 C4_6 103.0(4) . . ? C2_6 C3_6 H3M_6 111.2 . . ? C4_6 C3_6 H3M_6 111.2 . . ? C2_6 C3_6 H3N_6 111.2 . . ? C4_6 C3_6 H3N_6 111.2 . . ? H3M_6 C3_6 H3N_6 109.1 . . ? O1_6 C4_6 C3_6 104.6(4) . . ? O1_6 C4_6 H4N_6 110.8 . . ? C3_6 C4_6 H4N_6 110.8 . . ? O1_6 C4_6 H4O_6 110.8 . . ? C3_6 C4_6 H4O_6 110.8 . . ? H4N_6 C4_6 H4O_6 108.9 . . ? O1_7 C4_7 C3_7 103.7(9) . . ? O1_7 C4_7 H4P_7 111.0 . . ? C3_7 C4_7 H4P_7 111.0 . . ? O1_7 C4_7 H4Q_7 111.0 . . ? C3_7 C4_7 H4Q_7 111.0 . . ? H4P_7 C4_7 H4Q_7 109.0 . . ? O1_7 C1_7 C2_7 104.3(9) . . ? O1_7 C1_7 H1O_7 110.9 . . ? C2_7 C1_7 H1O_7 110.9 . . ? O1_7 C1_7 H1P_7 110.9 . . ? C2_7 C1_7 H1P_7 110.9 . . ? H1O_7 C1_7 H1P_7 108.9 . . ? C3_7 C2_7 C1_7 106.8(11) . . ? C3_7 C2_7 H2O_7 110.4 . . ? C1_7 C2_7 H2O_7 110.4 . . ? C3_7 C2_7 H2P_7 110.4 . . ? C1_7 C2_7 H2P_7 110.4 . . ? H2O_7 C2_7 H2P_7 108.6 . . ? C2_7 C3_7 C4_7 108.1(10) . . ? C2_7 C3_7 H3O_7 110.1 . . ? C4_7 C3_7 H3O_7 110.1 . . ? C2_7 C3_7 H3P_7 110.1 . . ? C4_7 C3_7 H3P_7 110.1 . . ? H3O_7 C3_7 H3P_7 108.4 . . ? C1_7 O1_7 C4_7 108.6(9) . . ? O1_10 C4_10 C3_10 104.5(9) . . ? O1_10 C4_10 H4R_10 110.9 . . ? C3_10 C4_10 H4R_10 110.9 . . ? O1_10 C4_10 H4S_10 110.9 . . ? C3_10 C4_10 H4S_10 110.9 . . ? H4R_10 C4_10 H4S_10 108.9 . . ? O1_10 C1_10 C2_10 105.7(9) . . ? O1_10 C1_10 H1Q_10 110.6 . . ? C2_10 C1_10 H1Q_10 110.6 . . ? O1_10 C1_10 H1R_10 110.6 . . ? C2_10 C1_10 H1R_10 110.6 . . ? H1Q_10 C1_10 H1R_10 108.7 . . ? C3_10 C2_10 C1_10 105.4(11) . . ? C3_10 C2_10 H2Q_10 110.7 . . ? C1_10 C2_10 H2Q_10 110.7 . . ? C3_10 C2_10 H2R_10 110.7 . . ? C1_10 C2_10 H2R_10 110.7 . . ? H2Q_10 C2_10 H2R_10 108.8 . . ? C2_10 C3_10 C4_10 109.1(11) . . ? C2_10 C3_10 H3Q_10 109.9 . . ? C4_10 C3_10 H3Q_10 109.9 . . ? C2_10 C3_10 H3R_10 109.9 . . ? C4_10 C3_10 H3R_10 109.9 . . ? H3Q_10 C3_10 H3R_10 108.3 . . ? C1_10 O1_10 C4_10 107.6(9) . . ? C4_8 O1_8 C1_8 106.7(11) . . ? O1_8 C1_8 C2_8 103.5(10) . . ? O1_8 C1_8 H1S_8 111.1 . . ? C2_8 C1_8 H1S_8 111.1 . . ? O1_8 C1_8 H1T_8 111.1 . . ? C2_8 C1_8 H1T_8 111.1 . . ? H1S_8 C1_8 H1T_8 109.0 . . ? C3_8 C2_8 C1_8 107.5(14) . . ? C3_8 C2_8 H2S_8 110.2 . . ? C1_8 C2_8 H2S_8 110.2 . . ? C3_8 C2_8 H2T_8 110.2 . . ? C1_8 C2_8 H2T_8 110.2 . . ? H2S_8 C2_8 H2T_8 108.5 . . ? C2_8 C3_8 C4_8 106.4(14) . . ? C2_8 C3_8 H3S_8 110.5 . . ? C4_8 C3_8 H3S_8 110.5 . . ? C2_8 C3_8 H3T_8 110.5 . . ? C4_8 C3_8 H3T_8 110.5 . . ? H3S_8 C3_8 H3T_8 108.6 . . ? O1_8 C4_8 C3_8 104.1(10) . . ? O1_8 C4_8 H4T_8 110.9 . . ? C3_8 C4_8 H4T_8 110.9 . . ? O1_8 C4_8 H4U_8 110.9 . . ? C3_8 C4_8 H4U_8 110.9 . . ? H4T_8 C4_8 H4U_8 109.0 . . ? C4_11 O1_11 C1_11 106.5(10) . . ? C3_11 C2_11 C1_11 106.5(18) . . ? C3_11 C2_11 H2U_11 110.4 . . ? C1_11 C2_11 H2U_11 110.4 . . ? C3_11 C2_11 H2V_11 110.4 . . ? C1_11 C2_11 H2V_11 110.4 . . ? H2U_11 C2_11 H2V_11 108.6 . . ? O1_11 C1_11 C2_11 103.6(10) . . ? O1_11 C1_11 H1U_11 111.0 . . ? C2_11 C1_11 H1U_11 111.0 . . ? O1_11 C1_11 H1V_11 111.0 . . ? C2_11 C1_11 H1V_11 111.0 . . ? H1U_11 C1_11 H1V_11 109.0 . . ? C2_11 C3_11 C4_11 98.3(18) . . ? C2_11 C3_11 H3U_11 112.1 . . ? C4_11 C3_11 H3U_11 112.1 . . ? C2_11 C3_11 H3V_11 112.1 . . ? C4_11 C3_11 H3V_11 112.1 . . ? H3U_11 C3_11 H3V_11 109.8 . . ? O1_11 C4_11 C3_11 103.4(10) . . ? O1_11 C4_11 H4V_11 111.1 . . ? C3_11 C4_11 H4V_11 111.1 . . ? O1_11 C4_11 H4W_11 111.1 . . ? C3_11 C4_11 H4W_11 111.1 . . ? H4V_11 C4_11 H4W_11 109.1 . . ? C4_12 O1_12 C1_12 108.1(11) . . ? C3_12 C2_12 C1_12 104.9(15) . . ? C3_12 C2_12 H2W_12 110.8 . . ? C1_12 C2_12 H2W_12 110.8 . . ? C3_12 C2_12 H2X_12 110.8 . . ? C1_12 C2_12 H2X_12 110.8 . . ? H2W_12 C2_12 H2X_12 108.9 . . ? O1_12 C1_12 C2_12 104.4(10) . . ? O1_12 C1_12 H1W_12 110.9 . . ? C2_12 C1_12 H1W_12 110.9 . . ? O1_12 C1_12 H1X_12 110.9 . . ? C2_12 C1_12 H1X_12 110.9 . . ? H1W_12 C1_12 H1X_12 108.9 . . ? C2_12 C3_12 C4_12 109.6(12) . . ? C2_12 C3_12 H3W_12 109.7 . . ? C4_12 C3_12 H3W_12 109.7 . . ? C2_12 C3_12 H3X_12 109.7 . . ? C4_12 C3_12 H3X_12 109.7 . . ? H3W_12 C3_12 H3X_12 108.2 . . ? O1_12 C4_12 C3_12 103.0(10) . . ? O1_12 C4_12 H4X_12 111.2 . . ? C3_12 C4_12 H4X_12 111.2 . . ? O1_12 C4_12 H4Y_12 111.2 . . ? C3_12 C4_12 H4Y_12 111.2 . . ? H4X_12 C4_12 H4Y_12 109.1 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.704 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.095 # Attachment '- 2_rev.cif' data_ar325acb _database_code_depnum_ccdc_archive 'CCDC 872676' #TrackingRef '- 2_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (((PhthalOH)In(H2O))ClO4)N _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 In N2 O12 P2, (Cl O4), 4(H2 O)' _chemical_formula_sum 'C18 H26 Cl In N2 O20 P2' _chemical_formula_weight 802.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.9622(2) _cell_length_b 10.0472(4) _cell_length_c 14.4552(6) _cell_angle_alpha 75.595(4) _cell_angle_beta 87.678(3) _cell_angle_gamma 89.821(3) _cell_volume 697.43(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5776 _cell_measurement_theta_min 3.1565 _cell_measurement_theta_max 73.9179 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 9.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8091 _exptl_absorpt_correction_T_max 0.9100 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.3281 _diffrn_reflns_number 12581 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 67.49 _reflns_number_total 2506 _reflns_number_gt 2356 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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. The hydrogen atoms on carbon atoms were generated geometrically and refined as riding atoms with C-H = 0.95- 0.99 \%A and Uiso(H) =1.2 times Ueq(C) for CH and CH2 groups and Uiso(H) =1.5 times Ueq(C) for CH3 groups. The hydrogens on water oxygens were found in the difference map, and restrained to known values (0.87Ang) using 1-2 and 1-3 restrained distances. The lone perchlorate anion in this structure has the chlorine atom near to an inversion center. this led to some disorder, which required the use of 1-2 and 1-3 restraints. the distance restraints are given below: SADI 0.01 Cl1 O7 Cl1 O8 Cl1 O9 Cl1 O10 Cl1 SADI 0.02 O7 O8 O7 O9 O7 O10 O8 O9 O8 O10 O9 O10 Due to the proximity of the perchlorate to its inversion-related self, thermal parameter restraints were used as well. ; _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^)+(0.0459P)^2^+0.7644P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2506 _refine_ls_number_parameters 242 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.078 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.5000 0.5000 0.0000 0.02530(13) Uani 1 2 d SD . . P1 P -0.00635(17) 0.36790(9) 0.15270(6) 0.0221(2) Uani 1 1 d . . . O1 O -0.4187(6) 0.1944(3) 0.3685(2) 0.0371(7) Uani 1 1 d . . . O2 O 0.2461(5) 0.5127(3) 0.35524(19) 0.0299(6) Uani 1 1 d . . . O3 O 0.2650(5) 0.4376(3) 0.12834(17) 0.0273(6) Uani 1 1 d . . . O4 O -0.1831(5) 0.3806(3) 0.06900(17) 0.0291(6) Uani 1 1 d . . . O5 O 0.0317(5) 0.2135(3) 0.20335(19) 0.0308(6) Uani 1 1 d . . . H5 H 0.0162 0.2028 0.2628 0.046 Uiso 1 1 calc R . . O6 O 0.3665(6) 0.3332(3) -0.0569(2) 0.0361(6) Uani 1 1 d D . . Cl1 Cl 0.0533(5) 1.0005(4) 0.0073(3) 0.0333(7) Uani 0.50 1 d PD A -1 O8 O 0.3406(10) 0.9954(7) 0.0007(5) 0.0488(16) Uani 0.50 1 d PD A -1 O7 O -0.0254(16) 1.1366(6) -0.0251(8) 0.087(3) Uani 0.50 1 d PDU A -1 O9 O -0.0300(15) 0.9520(9) 0.1056(4) 0.069(2) Uani 0.50 1 d PD A -1 O10 O -0.0526(17) 0.9136(11) -0.0441(7) 0.084(3) Uani 0.50 1 d PD A -1 O11 O 0.3474(7) 0.7362(3) 0.1915(2) 0.0478(8) Uani 1 1 d D . . O12 O 0.4801(6) 0.0890(3) 0.1889(2) 0.0445(7) Uani 1 1 d D . . N1 N -0.1066(6) 0.3708(3) 0.3403(2) 0.0242(6) Uani 1 1 d . . . C1 C -0.2349(7) 0.2511(4) 0.3954(3) 0.0266(8) Uani 1 1 d . . . C2 C -0.0993(7) 0.2177(4) 0.4880(3) 0.0262(8) Uani 1 1 d . . . C3 C -0.1461(8) 0.1122(4) 0.5685(3) 0.0341(9) Uani 1 1 d . . . H3 H -0.2817 0.0447 0.5710 0.041 Uiso 1 1 calc R . . C4 C 0.0139(9) 0.1087(5) 0.6461(3) 0.0394(10) Uani 1 1 d . . . H4A H -0.0137 0.0376 0.7029 0.047 Uiso 1 1 calc R . . C5 C 0.2120(9) 0.2066(5) 0.6421(3) 0.0373(10) Uani 1 1 d . . . H5A H 0.3189 0.2009 0.6960 0.045 Uiso 1 1 calc R . . C6 C 0.2582(8) 0.3134(4) 0.5607(3) 0.0304(8) Uani 1 1 d . . . H6 H 0.3930 0.3813 0.5582 0.036 Uiso 1 1 calc R . . C7 C 0.0994(7) 0.3163(4) 0.4839(2) 0.0248(8) Uani 1 1 d . . . C8 C 0.1002(7) 0.4138(4) 0.3880(2) 0.0227(7) Uani 1 1 d . . . C9 C -0.1828(7) 0.4369(4) 0.2433(2) 0.0248(8) Uani 1 1 d . . . H9B H -0.1441 0.5366 0.2302 0.030 Uiso 1 1 calc R . . H9A H -0.3795 0.4252 0.2387 0.030 Uiso 1 1 calc R . . H6A H 0.246(7) 0.273(3) -0.030(2) 0.037 Uiso 1 1 d D . . H11A H 0.290(7) 0.670(3) 0.239(2) 0.037 Uiso 1 1 d D . . H12A H 0.520(8) 0.080(4) 0.1324(14) 0.037 Uiso 1 1 d D . . H6B H 0.465(6) 0.302(3) -0.098(2) 0.037 Uiso 1 1 d D . . H11B H 0.210(5) 0.788(4) 0.171(3) 0.037 Uiso 1 1 d D . . H12B H 0.337(6) 0.138(4) 0.191(3) 0.037 Uiso 1 1 d 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 In1 0.0137(2) 0.0398(2) 0.01925(19) -0.00137(14) -0.00174(12) -0.00323(13) P1 0.0135(5) 0.0317(5) 0.0190(4) -0.0025(4) -0.0003(3) 0.0002(3) O1 0.0293(16) 0.0499(17) 0.0323(15) -0.0110(13) 0.0010(12) -0.0152(13) O2 0.0261(14) 0.0303(13) 0.0317(14) -0.0041(11) -0.0028(11) -0.0048(11) O3 0.0147(13) 0.0447(15) 0.0184(12) -0.0002(11) 0.0010(9) -0.0021(11) O4 0.0172(13) 0.0460(15) 0.0234(13) -0.0069(11) -0.0039(10) 0.0009(11) O5 0.0271(14) 0.0355(14) 0.0271(13) -0.0034(11) 0.0024(11) 0.0008(11) O6 0.0323(16) 0.0434(16) 0.0324(15) -0.0093(13) 0.0020(12) -0.0128(13) Cl1 0.029(3) 0.0285(8) 0.0455(15) -0.0126(9) -0.0111(15) 0.0046(17) O8 0.019(4) 0.057(4) 0.067(4) -0.011(3) -0.005(3) 0.002(3) O7 0.059(5) 0.042(4) 0.141(7) 0.020(5) -0.049(5) -0.020(3) O9 0.062(5) 0.104(6) 0.038(4) -0.010(4) -0.008(3) 0.027(5) O10 0.080(7) 0.111(8) 0.086(7) -0.077(7) 0.035(5) -0.051(6) O11 0.059(2) 0.0363(17) 0.0456(19) -0.0055(14) 0.0021(16) 0.0072(15) O12 0.0286(17) 0.0445(17) 0.062(2) -0.0164(16) -0.0074(15) 0.0054(13) N1 0.0196(16) 0.0328(16) 0.0184(14) -0.0031(12) 0.0001(11) -0.0001(12) C1 0.021(2) 0.035(2) 0.0234(18) -0.0073(15) 0.0044(14) -0.0012(16) C2 0.024(2) 0.0302(18) 0.0242(18) -0.0071(15) 0.0017(14) 0.0034(15) C3 0.033(2) 0.034(2) 0.031(2) -0.0013(16) 0.0050(16) -0.0002(17) C4 0.042(3) 0.041(2) 0.028(2) 0.0039(17) 0.0012(18) 0.0052(19) C5 0.037(2) 0.050(2) 0.0236(19) -0.0058(17) -0.0051(16) 0.0096(19) C6 0.024(2) 0.039(2) 0.0293(19) -0.0098(16) -0.0043(15) 0.0027(16) C7 0.0195(19) 0.0311(19) 0.0237(18) -0.0067(15) 0.0011(14) 0.0037(14) C8 0.0179(18) 0.0280(18) 0.0235(17) -0.0089(14) -0.0012(14) 0.0033(14) C9 0.0166(18) 0.037(2) 0.0190(17) -0.0034(15) -0.0012(13) 0.0037(15) _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 In1 O4 2.104(2) 2_565 ? In1 O4 2.104(2) 1_655 ? In1 O3 2.108(2) 2_665 ? In1 O3 2.108(2) . ? In1 O6 2.159(3) 2_665 ? In1 O6 2.159(3) . ? P1 O4 1.503(2) . ? P1 O3 1.507(3) . ? P1 O5 1.556(3) . ? P1 C9 1.821(4) . ? O1 C1 1.204(5) . ? O2 C8 1.216(4) . ? O4 In1 2.104(2) 1_455 ? O5 H5 0.8400 . ? O6 H6A 0.859(10) . ? O6 H6B 0.872(10) . ? Cl1 O7 1.391(7) . ? Cl1 O10 1.396(7) . ? Cl1 O8 1.427(5) . ? Cl1 O9 1.427(6) . ? O11 H11A 0.870(10) . ? O11 H11B 0.871(10) . ? O12 H12A 0.860(10) . ? O12 H12B 0.866(10) . ? N1 C8 1.387(5) . ? N1 C1 1.405(5) . ? N1 C9 1.459(4) . ? C1 C2 1.486(5) . ? C2 C3 1.377(5) . ? C2 C7 1.388(5) . ? C3 C4 1.394(6) . ? C3 H3 0.9500 . ? C4 C5 1.382(7) . ? C4 H4A 0.9500 . ? C5 C6 1.393(6) . ? C5 H5A 0.9500 . ? C6 C7 1.382(5) . ? C6 H6 0.9500 . ? C7 C8 1.484(5) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? 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 O4 In1 O4 180.00(13) 2_565 1_655 ? O4 In1 O3 88.30(10) 2_565 2_665 ? O4 In1 O3 91.70(10) 1_655 2_665 ? O4 In1 O3 91.71(10) 2_565 . ? O4 In1 O3 88.29(10) 1_655 . ? O3 In1 O3 180.0 2_665 . ? O4 In1 O6 91.35(11) 2_565 2_665 ? O4 In1 O6 88.65(11) 1_655 2_665 ? O3 In1 O6 94.41(10) 2_665 2_665 ? O3 In1 O6 85.59(10) . 2_665 ? O4 In1 O6 88.65(11) 2_565 . ? O4 In1 O6 91.35(11) 1_655 . ? O3 In1 O6 85.59(10) 2_665 . ? O3 In1 O6 94.41(10) . . ? O6 In1 O6 180.0 2_665 . ? O4 P1 O3 114.60(14) . . ? O4 P1 O5 109.75(15) . . ? O3 P1 O5 109.82(15) . . ? O4 P1 C9 109.22(15) . . ? O3 P1 C9 109.19(17) . . ? O5 P1 C9 103.71(16) . . ? P1 O3 In1 133.10(15) . . ? P1 O4 In1 140.94(16) . 1_455 ? P1 O5 H5 109.5 . . ? In1 O6 H6A 125.0(17) . . ? In1 O6 H6B 122.1(17) . . ? H6A O6 H6B 110(2) . . ? O7 Cl1 O10 113.4(5) . . ? O7 Cl1 O8 108.4(5) . . ? O10 Cl1 O8 109.0(5) . . ? O7 Cl1 O9 109.0(6) . . ? O10 Cl1 O9 109.0(5) . . ? O8 Cl1 O9 107.8(4) . . ? H11A O11 H11B 108(2) . . ? H12A O12 H12B 113(2) . . ? C8 N1 C1 112.1(3) . . ? C8 N1 C9 125.4(3) . . ? C1 N1 C9 122.4(3) . . ? O1 C1 N1 124.0(3) . . ? O1 C1 C2 130.5(4) . . ? N1 C1 C2 105.5(3) . . ? C3 C2 C7 121.7(4) . . ? C3 C2 C1 130.3(4) . . ? C7 C2 C1 108.0(3) . . ? C2 C3 C4 117.2(4) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 121.3(4) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 121.4(4) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C6 C5 117.1(4) . . ? C7 C6 H6 121.4 . . ? C5 C6 H6 121.4 . . ? C6 C7 C2 121.4(3) . . ? C6 C7 C8 130.2(4) . . ? C2 C7 C8 108.4(3) . . ? O2 C8 N1 125.1(3) . . ? O2 C8 C7 129.0(3) . . ? N1 C8 C7 105.9(3) . . ? N1 C9 P1 113.1(2) . . ? N1 C9 H9B 109.0 . . ? P1 C9 H9B 109.0 . . ? N1 C9 H9A 109.0 . . ? P1 C9 H9A 109.0 . . ? H9B C9 H9A 107.8 . . ? 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 O4 P1 O3 In1 -21.1(3) . . . . ? O5 P1 O3 In1 103.0(2) . . . . ? C9 P1 O3 In1 -144.0(2) . . . . ? O4 In1 O3 P1 55.8(2) 2_565 . . . ? O4 In1 O3 P1 -124.2(2) 1_655 . . . ? O3 In1 O3 P1 -165(3) 2_665 . . . ? O6 In1 O3 P1 147.1(2) 2_665 . . . ? O6 In1 O3 P1 -32.9(2) . . . . ? O3 P1 O4 In1 -96.6(3) . . . 1_455 ? O5 P1 O4 In1 139.3(2) . . . 1_455 ? C9 P1 O4 In1 26.2(3) . . . 1_455 ? C8 N1 C1 O1 -179.5(3) . . . . ? C9 N1 C1 O1 -1.1(5) . . . . ? C8 N1 C1 C2 1.6(4) . . . . ? C9 N1 C1 C2 179.9(3) . . . . ? O1 C1 C2 C3 0.3(7) . . . . ? N1 C1 C2 C3 179.2(4) . . . . ? O1 C1 C2 C7 -179.1(4) . . . . ? N1 C1 C2 C7 -0.2(4) . . . . ? C7 C2 C3 C4 0.3(6) . . . . ? C1 C2 C3 C4 -179.1(4) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C3 C4 C5 C6 0.6(7) . . . . ? C4 C5 C6 C7 -0.7(6) . . . . ? C5 C6 C7 C2 0.6(5) . . . . ? C5 C6 C7 C8 -179.2(4) . . . . ? C3 C2 C7 C6 -0.4(5) . . . . ? C1 C2 C7 C6 179.1(3) . . . . ? C3 C2 C7 C8 179.4(3) . . . . ? C1 C2 C7 C8 -1.1(4) . . . . ? C1 N1 C8 O2 178.3(3) . . . . ? C9 N1 C8 O2 0.0(5) . . . . ? C1 N1 C8 C7 -2.2(4) . . . . ? C9 N1 C8 C7 179.5(3) . . . . ? C6 C7 C8 O2 1.4(6) . . . . ? C2 C7 C8 O2 -178.5(3) . . . . ? C6 C7 C8 N1 -178.2(4) . . . . ? C2 C7 C8 N1 2.0(4) . . . . ? C8 N1 C9 P1 90.6(4) . . . . ? C1 N1 C9 P1 -87.5(4) . . . . ? O4 P1 C9 N1 150.2(3) . . . . ? O3 P1 C9 N1 -83.8(3) . . . . ? O5 P1 C9 N1 33.2(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 N1 0.84 2.31 2.886(4) 125.7 . O5 H5 O1 0.84 2.58 3.174(4) 128.5 . O6 H6A O7 0.859(10) 1.912(18) 2.719(8) 156(3) 1_545 O6 H6A O10 0.859(10) 2.127(19) 2.957(9) 163(4) 2_565 O6 H6A Cl1 0.859(10) 2.820(19) 3.581(5) 149(2) 1_545 O11 H11A O2 0.870(10) 2.001(13) 2.857(4) 167(4) . O12 H12A O8 0.860(10) 2.316(15) 3.159(7) 167(4) 2_665 O12 H12A O8 0.860(10) 2.46(3) 3.192(8) 143(4) 1_545 O12 H12A O9 0.860(10) 2.64(3) 3.134(8) 118(3) 1_645 O6 H6B O11 0.872(10) 1.730(12) 2.595(4) 172(4) 2_665 O11 H11B O9 0.871(10) 2.083(16) 2.928(8) 164(4) . O11 H11B O7 0.871(10) 2.28(3) 2.957(9) 134(4) 2_575 O11 H11B Cl1 0.871(10) 2.90(2) 3.613(5) 141(3) . O12 H12B O5 0.866(10) 1.716(13) 2.576(4) 172(5) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 67.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.887 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.091 # Attachment '- 4.cif' data_ar42 _database_code_depnum_ccdc_archive 'CCDC 885348' #TrackingRef '- 4.cif' _audit_creation_date 2012-06-06 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C17 H24 Cl3 In N O6 P' _chemical_formula_sum 'C17 H24 Cl3 In N O6 P' _chemical_formula_weight 590.51 _chemical_melting_point ? _chemical_oxdiff_formula 'C12 H12 N1 P1 O1 IN1 CL1' _chemical_oxdiff_usercomment 'PHTAL INCL3 THF' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 7.9265(3) _cell_length_b 8.0262(3) _cell_length_c 21.3673(9) _cell_angle_alpha 99.131(4) _cell_angle_beta 92.125(3) _cell_angle_gamma 117.475(4) _cell_volume 1181.30(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8670 _cell_measurement_temperature 173.2 _cell_measurement_theta_max 30.8700 _cell_measurement_theta_min 2.4553 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 15037 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.89 _diffrn_ambient_temperature 173.2 _diffrn_detector_area_resol_mean 10.3281 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -25.00 47.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 15.0885 -99.0000 67.0000 72 #__ type_ start__ end____ width___ exp.time_ 2 omega -19.00 94.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 15.0885 77.0000 -180.0000 113 #__ type_ start__ end____ width___ exp.time_ 3 omega -25.00 0.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -15.8697 -99.0000 6.0000 25 #__ type_ start__ end____ width___ exp.time_ 4 omega -64.00 49.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 15.0885 -77.0000 -150.0000 113 #__ type_ start__ end____ width___ exp.time_ 5 omega -19.00 94.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 15.0885 77.0000 -60.0000 113 #__ type_ start__ end____ width___ exp.time_ 6 omega -58.00 4.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -15.8697 99.0000 -67.0000 62 ; _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0426286000 _diffrn_orient_matrix_UB_12 -0.0520158000 _diffrn_orient_matrix_UB_13 -0.0163458000 _diffrn_orient_matrix_UB_21 -0.0666111000 _diffrn_orient_matrix_UB_22 -0.0271590000 _diffrn_orient_matrix_UB_23 -0.0275615000 _diffrn_orient_matrix_UB_31 0.0638912000 _diffrn_orient_matrix_UB_32 0.0829718000 _diffrn_orient_matrix_UB_33 -0.0110390000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4778 _reflns_number_total 5421 _reflns_odcompleteness_completeness 99.41 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.22 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.999 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.094 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 5421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0367 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+1.3222P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.0821 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 In1 In 0.03741(3) 0.10903(3) 0.354747(10) 0.02316(8) Uani 1 1 d . . . Cl1 Cl -0.19005(12) -0.12230(13) 0.26949(4) 0.0400(2) Uani 1 1 d . . . Cl2 Cl -0.01293(14) 0.36013(13) 0.40508(5) 0.0422(2) Uani 1 1 d . . . Cl3 Cl 0.29844(12) 0.06379(14) 0.38635(4) 0.0374(2) Uani 1 1 d . . . P1 P 0.26100(11) 0.31856(12) 0.22377(4) 0.02544(18) Uani 1 1 d . . . O1 O -0.0101(6) 0.3420(7) 0.07914(15) 0.0839(13) Uani 1 1 d . . . O2 O 0.3267(7) 0.0171(6) 0.08226(16) 0.0871(14) Uani 1 1 d . . . O3 O 0.2835(7) 0.5087(4) 0.21072(14) 0.0881(14) Uani 1 1 d . . . O4 O 0.1994(3) 0.2811(3) 0.28662(10) 0.0313(5) Uani 1 1 d . . . O5 O 0.4525(4) 0.3229(7) 0.21310(14) 0.0888(15) Uani 1 1 d . . . O6 O -0.1358(3) -0.0729(3) 0.42292(10) 0.0285(5) Uani 1 1 d . . . N1 N 0.1556(4) 0.1813(4) 0.09662(12) 0.0273(6) Uani 1 1 d . . . C1 C 0.0966(5) 0.2816(6) 0.06187(17) 0.0397(9) Uani 1 1 d . . . C2 C 0.1896(5) 0.2895(5) 0.00240(15) 0.0305(7) Uani 1 1 d . . . C3 C 0.1853(7) 0.3765(7) -0.04761(19) 0.0526(11) Uani 1 1 d . . . H3 H 0.1127 0.4431 -0.0485 0.063 Uiso 1 1 calc R . . C4 C 0.2906(6) 0.3636(6) -0.09665(18) 0.0446(10) Uani 1 1 d . . . H4 H 0.2923 0.4247 -0.1314 0.054 Uiso 1 1 calc R . . C5 C 0.3913(6) 0.2655(6) -0.09607(18) 0.0461(10) Uani 1 1 d . . . H5 H 0.4620 0.2586 -0.1304 0.055 Uiso 1 1 calc R . . C6 C 0.3922(7) 0.1747(7) -0.04570(19) 0.0518(11) Uani 1 1 d . . . H6 H 0.4608 0.1041 -0.0454 0.062 Uiso 1 1 calc R . . C7 C 0.2905(5) 0.1910(5) 0.00344(16) 0.0324(8) Uani 1 1 d . . . C8 C 0.2670(6) 0.1153(6) 0.06343(17) 0.0379(8) Uani 1 1 d . . . C9 C 0.0975(5) 0.1400(5) 0.15815(15) 0.0303(7) Uani 1 1 d . . . H9A H 0.0874 0.0143 0.1618 0.036 Uiso 1 1 calc R . . H9B H -0.0310 0.1303 0.1608 0.036 Uiso 1 1 calc R . . C10 C 0.5967(6) 0.3382(7) 0.2559(2) 0.0541(11) Uani 1 1 d . . . H10A H 0.5374 0.2509 0.2858 0.065 Uiso 1 1 calc R . . H10B H 0.6634 0.4705 0.2813 0.065 Uiso 1 1 calc R . . C11 C 0.7349(7) 0.2950(10) 0.2277(3) 0.0809(18) Uani 1 1 d . . . H11A H 0.8308 0.3090 0.2613 0.121 Uiso 1 1 calc R . . H11B H 0.7979 0.3832 0.1990 0.121 Uiso 1 1 calc R . . H11C H 0.6713 0.1630 0.2034 0.121 Uiso 1 1 calc R . . C12 C 0.2769(6) 0.6611(6) 0.25207(18) 0.0396(9) Uani 1 1 d . . . H12A H 0.4052 0.7480 0.2763 0.048 Uiso 1 1 calc R . . H12B H 0.1857 0.6095 0.2831 0.048 Uiso 1 1 calc R . . C13 C 0.2163(8) 0.7689(8) 0.2153(2) 0.0641(13) Uani 1 1 d . . . H13A H 0.2132 0.8745 0.2445 0.096 Uiso 1 1 calc R . . H13B H 0.0881 0.6833 0.1920 0.096 Uiso 1 1 calc R . . H13C H 0.3071 0.8206 0.1848 0.096 Uiso 1 1 calc R . . C14 C -0.3277(5) -0.0963(6) 0.43009(19) 0.0404(9) Uani 1 1 d . . . H14A H -0.3702 -0.0449 0.3972 0.049 Uiso 1 1 calc R . . H14B H -0.3314 -0.0307 0.4730 0.049 Uiso 1 1 calc R . . C15 C -0.4520(6) -0.3124(6) 0.4212(2) 0.0577(13) Uani 1 1 d . . . H15A H -0.5645 -0.3444 0.4449 0.069 Uiso 1 1 calc R . . H15B H -0.4970 -0.3720 0.3755 0.069 Uiso 1 1 calc R . . C16 C -0.3215(6) -0.3769(6) 0.4479(2) 0.0476(10) Uani 1 1 d . . . H16A H -0.3651 -0.5140 0.4302 0.057 Uiso 1 1 calc R . . H16B H -0.3131 -0.3571 0.4951 0.057 Uiso 1 1 calc R . . C17 C -0.1325(5) -0.2520(5) 0.42705(18) 0.0379(8) Uani 1 1 d . . . H17A H -0.0251 -0.2278 0.4586 0.045 Uiso 1 1 calc R . . H17B H -0.1182 -0.3131 0.3850 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.02328(12) 0.02212(12) 0.02189(12) 0.00666(9) 0.00457(8) 0.00809(9) Cl1 0.0353(5) 0.0359(5) 0.0284(4) 0.0040(4) -0.0007(3) 0.0010(4) Cl2 0.0509(5) 0.0317(5) 0.0496(5) 0.0075(4) 0.0164(4) 0.0237(4) Cl3 0.0313(4) 0.0466(5) 0.0414(5) 0.0169(4) 0.0068(3) 0.0215(4) P1 0.0258(4) 0.0248(4) 0.0227(4) 0.0083(3) 0.0058(3) 0.0082(3) O1 0.112(3) 0.173(4) 0.0513(19) 0.052(2) 0.0382(19) 0.127(3) O2 0.169(4) 0.123(3) 0.064(2) 0.057(2) 0.063(2) 0.133(3) O3 0.204(4) 0.0341(17) 0.0392(17) 0.0198(14) 0.054(2) 0.060(2) O4 0.0331(12) 0.0303(12) 0.0246(12) 0.0110(10) 0.0076(9) 0.0083(10) O5 0.0343(17) 0.206(5) 0.0378(17) 0.043(2) 0.0112(13) 0.060(2) O6 0.0270(12) 0.0277(12) 0.0308(12) 0.0131(10) 0.0095(9) 0.0102(9) N1 0.0304(14) 0.0306(15) 0.0243(14) 0.0054(11) 0.0044(11) 0.0173(12) C1 0.042(2) 0.065(3) 0.0291(19) 0.0124(18) 0.0030(15) 0.038(2) C2 0.0354(18) 0.0362(19) 0.0235(17) 0.0036(14) 0.0001(13) 0.0208(15) C3 0.079(3) 0.076(3) 0.033(2) 0.019(2) 0.009(2) 0.059(3) C4 0.059(3) 0.048(2) 0.029(2) 0.0134(17) 0.0056(17) 0.025(2) C5 0.049(2) 0.060(3) 0.028(2) 0.0078(18) 0.0107(16) 0.025(2) C6 0.072(3) 0.072(3) 0.041(2) 0.020(2) 0.022(2) 0.055(3) C7 0.0374(19) 0.0337(19) 0.0279(18) 0.0023(14) 0.0039(14) 0.0196(16) C8 0.060(2) 0.040(2) 0.0308(19) 0.0110(16) 0.0140(16) 0.0358(19) C9 0.0285(17) 0.0301(18) 0.0288(17) 0.0068(14) 0.0055(13) 0.0106(14) C10 0.056(3) 0.077(3) 0.052(3) 0.029(2) 0.011(2) 0.046(3) C11 0.051(3) 0.125(5) 0.085(4) 0.034(4) 0.021(3) 0.052(3) C12 0.043(2) 0.039(2) 0.042(2) 0.0038(17) 0.0090(16) 0.0246(17) C13 0.090(4) 0.071(3) 0.057(3) 0.025(3) 0.022(3) 0.054(3) C14 0.0300(19) 0.051(2) 0.042(2) 0.0186(18) 0.0133(15) 0.0177(17) C15 0.033(2) 0.054(3) 0.064(3) 0.026(2) -0.0002(19) -0.0023(19) C16 0.046(2) 0.033(2) 0.048(2) 0.0139(18) 0.0094(18) 0.0039(17) C17 0.041(2) 0.0276(18) 0.041(2) 0.0142(16) 0.0050(16) 0.0109(16) _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 In1 Cl1 2.3686(9) . ? In1 Cl2 2.3374(9) . ? In1 Cl3 2.3529(9) . ? In1 O4 2.194(2) . ? In1 O6 2.261(2) . ? P1 O3 1.525(3) . ? P1 O4 1.474(2) . ? P1 O5 1.528(3) . ? P1 C9 1.793(3) . ? O1 C1 1.196(4) . ? O2 C8 1.199(4) . ? O3 C12 1.414(5) . ? O5 C10 1.385(5) . ? O6 C14 1.461(4) . ? O6 C17 1.466(4) . ? N1 C1 1.389(4) . ? N1 C8 1.387(4) . ? N1 C9 1.447(4) . ? C1 C2 1.488(5) . ? C2 C3 1.374(5) . ? C2 C7 1.361(5) . ? C3 H3 0.9500 . ? C3 C4 1.384(6) . ? C4 H4 0.9500 . ? C4 C5 1.356(6) . ? C5 H5 0.9500 . ? C5 C6 1.394(6) . ? C6 H6 0.9500 . ? C6 C7 1.373(5) . ? C7 C8 1.486(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.420(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.473(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.523(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.486(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.501(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? 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 Cl2 In1 Cl1 119.22(4) . . ? Cl2 In1 Cl3 123.66(4) . . ? Cl3 In1 Cl1 117.08(4) . . ? O4 In1 Cl1 90.21(6) . . ? O4 In1 Cl2 90.87(7) . . ? O4 In1 Cl3 90.92(7) . . ? O4 In1 O6 178.53(8) . . ? O6 In1 Cl1 88.35(6) . . ? O6 In1 Cl2 89.58(6) . . ? O6 In1 Cl3 90.00(6) . . ? O3 P1 O5 105.2(2) . . ? O3 P1 C9 105.38(19) . . ? O4 P1 O3 113.72(15) . . ? O4 P1 O5 114.57(15) . . ? O4 P1 C9 113.27(14) . . ? O5 P1 C9 103.69(19) . . ? C12 O3 P1 129.8(3) . . ? P1 O4 In1 156.29(15) . . ? C10 O5 P1 130.8(3) . . ? C14 O6 In1 119.2(2) . . ? C14 O6 C17 109.6(3) . . ? C17 O6 In1 119.94(19) . . ? C1 N1 C9 124.1(3) . . ? C8 N1 C1 111.8(3) . . ? C8 N1 C9 124.0(3) . . ? O1 C1 N1 123.8(3) . . ? O1 C1 C2 130.6(3) . . ? N1 C1 C2 105.7(3) . . ? C3 C2 C1 130.2(3) . . ? C7 C2 C1 108.2(3) . . ? C7 C2 C3 121.6(3) . . ? C2 C3 H3 121.2 . . ? C2 C3 C4 117.5(4) . . ? C4 C3 H3 121.2 . . ? C3 C4 H4 119.3 . . ? C5 C4 C3 121.4(4) . . ? C5 C4 H4 119.3 . . ? C4 C5 H5 119.6 . . ? C4 C5 C6 120.8(4) . . ? C6 C5 H5 119.6 . . ? C5 C6 H6 121.2 . . ? C7 C6 C5 117.6(4) . . ? C7 C6 H6 121.2 . . ? C2 C7 C6 121.1(3) . . ? C2 C7 C8 108.5(3) . . ? C6 C7 C8 130.4(3) . . ? O2 C8 N1 124.1(3) . . ? O2 C8 C7 130.3(3) . . ? N1 C8 C7 105.7(3) . . ? P1 C9 H9A 109.0 . . ? P1 C9 H9B 109.0 . . ? N1 C9 P1 112.9(2) . . ? N1 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? O5 C10 H10A 108.5 . . ? O5 C10 H10B 108.5 . . ? O5 C10 C11 114.9(4) . . ? H10A C10 H10B 107.5 . . ? C11 C10 H10A 108.5 . . ? C11 C10 H10B 108.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C12 H12A 109.6 . . ? O3 C12 H12B 109.6 . . ? O3 C12 C13 110.4(4) . . ? H12A C12 H12B 108.1 . . ? C13 C12 H12A 109.6 . . ? C13 C12 H12B 109.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O6 C14 H14A 111.0 . . ? O6 C14 H14B 111.0 . . ? O6 C14 C15 103.6(3) . . ? H14A C14 H14B 109.0 . . ? C15 C14 H14A 111.0 . . ? C15 C14 H14B 111.0 . . ? C14 C15 H15A 111.0 . . ? C14 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? C16 C15 C14 103.6(3) . . ? C16 C15 H15A 111.0 . . ? C16 C15 H15B 111.0 . . ? C15 C16 H16A 111.1 . . ? C15 C16 H16B 111.1 . . ? C15 C16 C17 103.3(3) . . ? H16A C16 H16B 109.1 . . ? C17 C16 H16A 111.1 . . ? C17 C16 H16B 111.1 . . ? O6 C17 C16 105.3(3) . . ? O6 C17 H17A 110.7 . . ? O6 C17 H17B 110.7 . . ? C16 C17 H17A 110.7 . . ? C16 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? 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 In1 O6 C14 C15 129.3(3) . . . . ? In1 O6 C17 C16 -152.5(2) . . . . ? Cl1 In1 O4 P1 -19.7(4) . . . . ? Cl1 In1 O6 C14 -66.5(2) . . . . ? Cl1 In1 O6 C17 73.5(2) . . . . ? Cl2 In1 O4 P1 -138.9(4) . . . . ? Cl2 In1 O6 C14 52.7(2) . . . . ? Cl2 In1 O6 C17 -167.3(2) . . . . ? Cl3 In1 O4 P1 97.4(4) . . . . ? Cl3 In1 O6 C14 176.4(2) . . . . ? Cl3 In1 O6 C17 -43.6(2) . . . . ? P1 O3 C12 C13 -153.6(4) . . . . ? P1 O5 C10 C11 166.6(5) . . . . ? O1 C1 C2 C3 3.5(8) . . . . ? O1 C1 C2 C7 -176.7(5) . . . . ? O3 P1 O4 In1 138.9(4) . . . . ? O3 P1 O5 C10 110.0(5) . . . . ? O3 P1 C9 N1 53.1(3) . . . . ? O4 In1 O6 C14 -55(3) . . . . ? O4 In1 O6 C17 85(3) . . . . ? O4 P1 O3 C12 8.5(5) . . . . ? O4 P1 O5 C10 -15.6(6) . . . . ? O4 P1 C9 N1 178.0(2) . . . . ? O5 P1 O3 C12 -117.6(5) . . . . ? O5 P1 O4 In1 -100.1(4) . . . . ? O5 P1 C9 N1 -57.2(3) . . . . ? O6 In1 O4 P1 -31(4) . . . . ? O6 C14 C15 C16 32.6(4) . . . . ? N1 C1 C2 C3 -177.7(4) . . . . ? N1 C1 C2 C7 2.1(4) . . . . ? C1 N1 C8 O2 -176.2(5) . . . . ? C1 N1 C8 C7 3.6(4) . . . . ? C1 N1 C9 P1 -92.2(4) . . . . ? C1 C2 C3 C4 178.5(4) . . . . ? C1 C2 C7 C6 -179.8(4) . . . . ? C1 C2 C7 C8 0.0(4) . . . . ? C2 C3 C4 C5 1.3(7) . . . . ? C2 C7 C8 O2 177.7(5) . . . . ? C2 C7 C8 N1 -2.2(4) . . . . ? C3 C2 C7 C6 0.0(6) . . . . ? C3 C2 C7 C8 179.8(4) . . . . ? C3 C4 C5 C6 -0.2(7) . . . . ? C4 C5 C6 C7 -1.0(7) . . . . ? C5 C6 C7 C2 1.1(6) . . . . ? C5 C6 C7 C8 -178.7(4) . . . . ? C6 C7 C8 O2 -2.5(8) . . . . ? C6 C7 C8 N1 177.6(4) . . . . ? C7 C2 C3 C4 -1.2(6) . . . . ? C8 N1 C1 O1 175.3(4) . . . . ? C8 N1 C1 C2 -3.6(4) . . . . ? C8 N1 C9 P1 92.0(4) . . . . ? C9 P1 O3 C12 133.2(4) . . . . ? C9 P1 O4 In1 18.6(4) . . . . ? C9 P1 O5 C10 -139.6(5) . . . . ? C9 N1 C1 O1 -0.9(6) . . . . ? C9 N1 C1 C2 -179.8(3) . . . . ? C9 N1 C8 O2 0.0(6) . . . . ? C9 N1 C8 C7 179.8(3) . . . . ? C14 O6 C17 C16 -9.1(4) . . . . ? C14 C15 C16 C17 -38.2(4) . . . . ? C15 C16 C17 O6 29.5(4) . . . . ? C17 O6 C14 C15 -14.4(4) . . . . ?