# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Enrico Dalcanale' 'Chiara Massera' 'Monica Melegari' 'Franco Ugozzoli' _publ_contact_author_name 'Enrico Dalcanale' _publ_contact_author_email ENRICO.DALCANALE@UNIPR.IT _publ_section_title ; Tetraphosphonate cavitands: Interplay between metal coordination and H-bonding in the formation of dimeric capsules ; # Attachment 'total.cif' data_TPOBa _database_code_depnum_ccdc_archive 'CCDC 767369' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H87 Ba Cl2 F9 O30 P8' _chemical_formula_weight 2131.48 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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' _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 12.595(3) _cell_length_b 17.501(5) _cell_length_c 23.862(6) _cell_angle_alpha 89.857(5) _cell_angle_beta 77.873(5) _cell_angle_gamma 69.836(5) _cell_volume 4813(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3657 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 23.36 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6072 _exptl_absorpt_correction_T_max 0.7449 _exptl_absorpt_process_details 'Bruker Apex-II SADABS' _exptl_special_details ; The calculated molar mass, density and absorption coefficient include two disordered trifluoroethanol molecules per cell which do not appear in the final files because of the refinements carried out with data subjected to SQUEEZE. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD area-detector' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45305 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 23.36 _reflns_number_total 13929 _reflns_number_gt 8821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (2008)' _computing_cell_refinement 'APEX-II (2008)' _computing_data_reduction 'SAINT (2008)' _computing_structure_solution 'SIR97 (Giacovazzo and co., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In view of the presence of disordered trifluoroethanol molecules which could not be properly modelled and refined, the structure was subjected to SQUEEZE (P. v.d. Sluis and A. L. Spek, Acta Crystallogr., Sect A 1990, 46, 194-201). The program calculated a void volume of 743.1 A^3^ and 130 electrons per unit cell, which correspond roughly to the two disordered TFE molecules found in the difference Fourier map. ; _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^)+(0.0982P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13929 _refine_ls_number_parameters 1051 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1642 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.7297(2) 0.22236(16) 0.40328(10) 0.0936(8) Uani 1 1 d . . . Cl2 Cl 0.7807(3) 0.2596(2) 0.10187(12) 0.1189(10) Uani 1 1 d . . . Ba1 Ba 0.84623(4) 0.21903(2) 0.739991(18) 0.04421(16) Uani 1 1 d . . . O1W O 0.7659(5) 0.1676(4) 0.8472(2) 0.0851(18) Uani 1 1 d . . . O2W O 0.6166(4) 0.2904(3) 0.7807(2) 0.0663(14) Uani 1 1 d . . . O3W O 0.7497(6) 0.3341(5) 0.6641(3) 0.116(3) Uani 1 1 d . . . P1A P 0.76017(17) 0.02771(11) 0.68504(8) 0.0484(5) Uani 1 1 d . . . O1A O 0.8598(4) -0.0161(3) 0.62965(19) 0.0508(12) Uani 1 1 d . . . O2A O 0.6418(4) 0.0550(3) 0.6644(2) 0.0538(13) Uani 1 1 d . . . O3A O 0.7816(4) 0.0945(3) 0.7116(2) 0.0549(13) Uani 1 1 d . . . P1B P 0.38060(17) 0.40792(12) 0.69756(9) 0.0532(5) Uani 1 1 d . . . O1B O 0.3646(4) 0.3266(3) 0.6769(2) 0.0551(13) Uani 1 1 d . . . O2B O 0.3610(4) 0.4671(3) 0.6471(2) 0.0553(13) Uani 1 1 d . . . O3B O 0.4927(4) 0.3927(3) 0.7124(2) 0.0629(14) Uani 1 1 d . . . P1C P 0.7698(2) 0.55470(13) 0.59770(9) 0.0603(6) Uani 1 1 d . . . O1C O 0.6591(4) 0.5760(3) 0.5703(2) 0.0564(13) Uani 1 1 d . . . O2C O 0.8796(4) 0.5118(3) 0.5469(2) 0.0572(13) Uani 1 1 d . . . O3C O 0.7648(5) 0.5048(3) 0.6466(2) 0.0742(16) Uani 1 1 d . . . P1D P 1.14321(17) 0.18197(12) 0.60474(8) 0.0506(5) Uani 1 1 d . . . O1D O 1.1496(4) 0.2449(3) 0.5572(2) 0.0559(13) Uani 1 1 d . . . O2D O 1.1556(4) 0.0996(3) 0.5716(2) 0.0524(12) Uani 1 1 d . . . O3D O 1.0397(4) 0.2120(3) 0.65218(19) 0.0529(12) Uani 1 1 d . . . P1E P 0.82608(16) 0.44058(11) 0.81139(8) 0.0439(5) Uani 1 1 d . . . O1E O 0.9359(4) 0.4215(3) 0.83948(18) 0.0450(11) Uani 1 1 d . . . O2E O 0.7155(4) 0.4887(3) 0.86003(19) 0.0473(12) Uani 1 1 d . . . O3E O 0.8221(4) 0.3660(3) 0.7858(2) 0.0546(13) Uani 1 1 d . . . P1F P 0.32909(17) 0.36569(12) 0.91327(8) 0.0500(5) Uani 1 1 d . . . O1F O 0.3675(4) 0.4351(3) 0.93632(19) 0.0484(12) Uani 1 1 d . . . O2F O 0.3226(4) 0.3065(3) 0.96304(19) 0.0506(12) Uani 1 1 d . . . O3F O 0.4017(5) 0.3244(3) 0.8586(2) 0.0678(15) Uani 1 1 d . . . P1G P 0.6683(2) -0.01832(12) 0.89683(9) 0.0578(6) Uani 1 1 d . . . O1G O 0.5641(4) 0.0243(3) 0.9502(2) 0.0570(13) Uani 1 1 d . . . O2G O 0.7819(4) -0.0558(3) 0.9217(2) 0.0618(14) Uani 1 1 d . . . O3G O 0.6808(5) 0.0360(3) 0.8518(2) 0.0651(15) Uani 1 1 d . . . P1H P 1.13714(17) 0.07329(12) 0.80552(9) 0.0533(5) Uani 1 1 d . . . O1H O 1.1200(4) 0.0132(3) 0.8537(2) 0.0551(13) Uani 1 1 d . . . O2H O 1.1748(4) 0.1396(3) 0.8346(2) 0.0540(13) Uani 1 1 d . . . O3H O 1.0365(4) 0.1107(3) 0.7804(2) 0.0570(13) Uani 1 1 d . . . C1A C 0.9043(7) 0.1113(4) 0.5114(3) 0.0520(19) Uani 1 1 d . . . H1A H 0.8700 0.1340 0.4815 0.046(7) Uiso 1 1 calc R . . C2A C 0.8537(6) 0.0668(4) 0.5492(3) 0.0475(18) Uani 1 1 d . . . C3A C 0.9087(6) 0.0326(4) 0.5922(3) 0.0471(18) Uani 1 1 d . . . C4A C 1.0089(6) 0.0397(4) 0.6018(3) 0.0473(18) Uani 1 1 d . . . C5A C 1.0541(6) 0.0881(4) 0.5641(3) 0.0487(18) Uani 1 1 d . . . C6A C 1.0070(6) 0.1227(4) 0.5175(3) 0.0480(18) Uani 1 1 d . . . C7A C 1.0692(7) -0.0005(4) 0.6478(3) 0.062(2) Uani 1 1 d . . . H7A1 H 1.0404 -0.0426 0.6621 0.122(5) Uiso 1 1 calc R . . H7A2 H 1.0545 0.0394 0.6787 0.122(5) Uiso 1 1 calc R . . H7A3 H 1.1512 -0.0241 0.6321 0.122(5) Uiso 1 1 calc R . . C8A C 0.7393(6) 0.0611(4) 0.5438(3) 0.0525(19) Uani 1 1 d . . . H8A1 H 0.7356 0.0091 0.5562 0.078(6) Uiso 1 1 calc R . . H8A2 H 0.7342 0.0634 0.5038 0.078(6) Uiso 1 1 calc R . . C9A C 0.7537(8) -0.0546(4) 0.7254(3) 0.069(2) Uani 1 1 d . . . H9A1 H 0.8280 -0.0824 0.7342 0.122(5) Uiso 1 1 calc R . . H9A2 H 0.7336 -0.0917 0.7038 0.122(5) Uiso 1 1 calc R . . H9A3 H 0.6961 -0.0350 0.7606 0.122(5) Uiso 1 1 calc R . . C1B C 0.5849(6) 0.2007(4) 0.5549(3) 0.0489(18) Uani 1 1 d . . . H1B H 0.6104 0.2035 0.5157 0.046(7) Uiso 1 1 calc R . . C2B C 0.4962(6) 0.2673(4) 0.5858(3) 0.0461(18) Uani 1 1 d . . . C3B C 0.4604(6) 0.2602(5) 0.6441(3) 0.0508(19) Uani 1 1 d . . . C4B C 0.5087(6) 0.1910(4) 0.6725(3) 0.0447(17) Uani 1 1 d . . . C5B C 0.5977(6) 0.1282(4) 0.6383(3) 0.0473(18) Uani 1 1 d . . . C6B C 0.6377(6) 0.1300(4) 0.5797(3) 0.0428(17) Uani 1 1 d . . . C7B C 0.4644(7) 0.1863(5) 0.7354(3) 0.059(2) Uani 1 1 d . . . H7B1 H 0.4334 0.1431 0.7406 0.122(5) Uiso 1 1 calc R . . H7B2 H 0.4046 0.2372 0.7511 0.122(5) Uiso 1 1 calc R . . H7B3 H 0.5269 0.1756 0.7549 0.122(5) Uiso 1 1 calc R . . C8B C 0.4430(6) 0.3429(4) 0.5557(3) 0.0547(19) Uani 1 1 d . . . H8B1 H 0.4505 0.3272 0.5157 0.078(6) Uiso 1 1 calc R . . H8B2 H 0.3610 0.3672 0.5733 0.078(6) Uiso 1 1 calc R . . C9B C 0.2565(7) 0.4532(5) 0.7522(4) 0.079(3) Uani 1 1 d . . . H9B1 H 0.2559 0.4176 0.7828 0.122(5) Uiso 1 1 calc R . . H9B2 H 0.1885 0.4626 0.7371 0.122(5) Uiso 1 1 calc R . . H9B3 H 0.2569 0.5042 0.7666 0.122(5) Uiso 1 1 calc R . . C1C C 0.5960(6) 0.4037(4) 0.5180(3) 0.0507(19) Uani 1 1 d . . . H1C H 0.6243 0.3644 0.4872 0.046(7) Uiso 1 1 calc R . . C2C C 0.6517(6) 0.4580(4) 0.5209(3) 0.0489(18) Uani 1 1 d . . . C3C C 0.6079(6) 0.5160(4) 0.5670(3) 0.0481(18) Uani 1 1 d . . . C4C C 0.5100(7) 0.5231(4) 0.6101(3) 0.0491(18) Uani 1 1 d . . . C5C C 0.4603(6) 0.4644(4) 0.6042(3) 0.0487(18) Uani 1 1 d . . . C6C C 0.4999(6) 0.4051(4) 0.5588(3) 0.0462(18) Uani 1 1 d . . . C7C C 0.4641(7) 0.5849(5) 0.6596(3) 0.067(2) Uani 1 1 d . . . H7C1 H 0.3836 0.5934 0.6747 0.122(5) Uiso 1 1 calc R . . H7C2 H 0.4719 0.6353 0.6473 0.122(5) Uiso 1 1 calc R . . H7C3 H 0.5068 0.5660 0.6889 0.122(5) Uiso 1 1 calc R . . C8C C 0.7607(6) 0.4520(4) 0.4766(3) 0.0524(19) Uani 1 1 d . . . H8C1 H 0.7646 0.5061 0.4716 0.078(6) Uiso 1 1 calc R . . H8C2 H 0.7577 0.4300 0.4399 0.078(6) Uiso 1 1 calc R . . C9C C 0.7786(9) 0.6515(5) 0.6073(4) 0.094(3) Uani 1 1 d . . . H9C1 H 0.7054 0.6882 0.6288 0.122(5) Uiso 1 1 calc R . . H9C2 H 0.7972 0.6717 0.5704 0.122(5) Uiso 1 1 calc R . . H9C3 H 0.8379 0.6476 0.6278 0.122(5) Uiso 1 1 calc R . . C1D C 0.9164(6) 0.3147(5) 0.4787(3) 0.0508(19) Uani 1 1 d . . . H1D H 0.8837 0.2934 0.4540 0.046(7) Uiso 1 1 calc R . . C2D C 1.0103(6) 0.2626(4) 0.4972(3) 0.0473(18) Uani 1 1 d . . . C3D C 1.0536(6) 0.2951(5) 0.5369(3) 0.0510(19) Uani 1 1 d . . . C4D C 1.0098(6) 0.3782(5) 0.5554(3) 0.0506(19) Uani 1 1 d . . . C5D C 0.9181(7) 0.4260(4) 0.5327(3) 0.056(2) Uani 1 1 d . . . C6D C 0.8688(7) 0.3972(5) 0.4953(3) 0.0518(19) Uani 1 1 d . . . C7D C 1.0615(7) 0.4100(5) 0.5970(3) 0.069(2) Uani 1 1 d . . . H7D1 H 1.0491 0.4666 0.5921 0.122(5) Uiso 1 1 calc R . . H7D2 H 1.1433 0.3796 0.5900 0.122(5) Uiso 1 1 calc R . . H7D3 H 1.0253 0.4040 0.6356 0.122(5) Uiso 1 1 calc R . . C8D C 1.0611(7) 0.1727(4) 0.4775(3) 0.0551(19) Uani 1 1 d . . . H8D1 H 1.0492 0.1655 0.4393 0.078(6) Uiso 1 1 calc R . . H8D2 H 1.1440 0.1531 0.4753 0.078(6) Uiso 1 1 calc R . . C9D C 1.2800(6) 0.1581(5) 0.6216(4) 0.070(2) Uani 1 1 d . . . H9D1 H 1.2843 0.2057 0.6395 0.122(5) Uiso 1 1 calc R . . H9D2 H 1.3396 0.1402 0.5870 0.122(5) Uiso 1 1 calc R . . H9D3 H 1.2906 0.1154 0.6475 0.122(5) Uiso 1 1 calc R . . C1E C 0.9488(6) 0.2762(4) 0.9504(3) 0.0445(17) Uani 1 1 d . . . H1E H 0.9139 0.2751 0.9887 0.046(7) Uiso 1 1 calc R . . C2E C 0.9149(6) 0.3474(4) 0.9235(3) 0.0438(17) Uani 1 1 d . . . C3E C 0.9698(6) 0.3487(4) 0.8678(3) 0.0425(17) Uani 1 1 d . . . C4E C 1.0587(6) 0.2803(4) 0.8359(3) 0.0434(17) Uani 1 1 d . . . C5E C 1.0859(6) 0.2103(4) 0.8650(3) 0.0448(17) Uani 1 1 d . . . C6E C 1.0346(6) 0.2056(4) 0.9214(3) 0.0493(18) Uani 1 1 d . . . C7E C 1.1180(6) 0.2832(4) 0.7751(3) 0.057(2) Uani 1 1 d . . . H7E1 H 1.2002 0.2664 0.7721 0.122(5) Uiso 1 1 calc R . . H7E2 H 1.0897 0.3379 0.7637 0.122(5) Uiso 1 1 calc R . . H7E3 H 1.1023 0.2472 0.7504 0.122(5) Uiso 1 1 calc R . . C8E C 0.8168(6) 0.4216(4) 0.9552(3) 0.0455(17) Uani 1 1 d . . . H8E1 H 0.8281 0.4707 0.9406 0.078(6) Uiso 1 1 calc R . . H8E2 H 0.8178 0.4223 0.9958 0.078(6) Uiso 1 1 calc R . . C9E C 0.8399(7) 0.5173(4) 0.7654(3) 0.062(2) Uani 1 1 d . . . H9E1 H 0.9071 0.4946 0.7346 0.122(5) Uiso 1 1 calc R . . H9E2 H 0.8482 0.5606 0.7867 0.122(5) Uiso 1 1 calc R . . H9E3 H 0.7720 0.5385 0.7498 0.122(5) Uiso 1 1 calc R . . C1F C 0.6327(6) 0.3903(4) 0.9900(3) 0.0449(17) Uani 1 1 d . . . H1F H 0.6620 0.3683 1.0215 0.046(7) Uiso 1 1 calc R . . C2F C 0.5236(6) 0.3917(4) 0.9857(3) 0.0422(16) Uani 1 1 d . . . C3F C 0.4831(6) 0.4254(4) 0.9385(3) 0.0407(16) Uani 1 1 d . . . C4F C 0.5440(6) 0.4571(4) 0.8952(3) 0.0435(17) Uani 1 1 d . . . C5F C 0.6538(6) 0.4524(4) 0.9014(3) 0.0409(16) Uani 1 1 d . . . C6F C 0.6993(6) 0.4212(4) 0.9480(3) 0.0429(17) Uani 1 1 d . . . C7F C 0.4933(7) 0.4986(4) 0.8462(3) 0.063(2) Uani 1 1 d . . . H7F1 H 0.4614 0.4643 0.8291 0.122(5) Uiso 1 1 calc R . . H7F2 H 0.5531 0.5077 0.8178 0.122(5) Uiso 1 1 calc R . . H7F3 H 0.4331 0.5499 0.8605 0.122(5) Uiso 1 1 calc R . . C8F C 0.4568(6) 0.3533(4) 1.0303(3) 0.0467(17) Uani 1 1 d . . . H8F1 H 0.4790 0.3555 1.0666 0.078(6) Uiso 1 1 calc R . . H8F2 H 0.3743 0.3838 1.0361 0.078(6) Uiso 1 1 calc R . . C9F C 0.1799(7) 0.4175(5) 0.9161(4) 0.071(2) Uani 1 1 d . . . H9F1 H 0.1714 0.4549 0.8865 0.122(5) Uiso 1 1 calc R . . H9F2 H 0.1433 0.4472 0.9530 0.122(5) Uiso 1 1 calc R . . H9F3 H 0.1441 0.3787 0.9105 0.122(5) Uiso 1 1 calc R . . C1G C 0.5719(6) 0.2032(4) 1.0252(3) 0.0485(18) Uani 1 1 d . . . H1G H 0.6141 0.2163 1.0489 0.046(7) Uiso 1 1 calc R . . C2G C 0.6031(7) 0.1218(4) 1.0060(3) 0.0500(18) Uani 1 1 d . . . C3G C 0.5374(7) 0.1062(4) 0.9701(3) 0.054(2) Uani 1 1 d . . . C4G C 0.4442(6) 0.1662(4) 0.9531(3) 0.0516(19) Uani 1 1 d . . . C5G C 0.4193(6) 0.2450(4) 0.9756(3) 0.0452(17) Uani 1 1 d . . . C6G C 0.4814(6) 0.2656(4) 1.0109(3) 0.0442(17) Uani 1 1 d . . . C7G C 0.3749(7) 0.1459(5) 0.9155(3) 0.070(2) Uani 1 1 d . . . H7G1 H 0.2938 0.1690 0.9335 0.122(5) Uiso 1 1 calc R . . H7G2 H 0.3974 0.0877 0.9099 0.122(5) Uiso 1 1 calc R . . H7G3 H 0.3890 0.1680 0.8790 0.122(5) Uiso 1 1 calc R . . C8G C 0.7035(7) 0.0565(4) 1.0210(3) 0.056(2) Uani 1 1 d . . . H8G1 H 0.6884 0.0057 1.0230 0.078(6) Uiso 1 1 calc R . . H8G2 H 0.7119 0.0711 1.0586 0.078(6) Uiso 1 1 calc R . . C9G C 0.6404(8) -0.1067(5) 0.8800(4) 0.079(3) Uani 1 1 d . . . H9G1 H 0.5689 -0.0912 0.8674 0.122(5) Uiso 1 1 calc R . . H9G2 H 0.6347 -0.1367 0.9135 0.122(5) Uiso 1 1 calc R . . H9G3 H 0.7026 -0.1402 0.8499 0.122(5) Uiso 1 1 calc R . . C1H C 0.8868(6) 0.0874(4) 0.9832(3) 0.0473(18) Uani 1 1 d . . . H1H H 0.8656 0.1237 1.0155 0.046(7) Uiso 1 1 calc R . . C2H C 0.9875(6) 0.0787(4) 0.9434(3) 0.0475(18) Uani 1 1 d . . . C3H C 1.0152(6) 0.0268(4) 0.8952(3) 0.0512(19) Uani 1 1 d . . . C4H C 0.9491(7) -0.0202(4) 0.8861(3) 0.054(2) Uani 1 1 d . . . C5H C 0.8498(7) -0.0084(4) 0.9282(3) 0.0535(19) Uani 1 1 d . . . C6H C 0.8162(6) 0.0441(4) 0.9769(3) 0.0486(19) Uani 1 1 d . . . C7H C 0.9830(7) -0.0770(5) 0.8334(3) 0.071(2) Uani 1 1 d . . . H7H1 H 0.9325 -0.1080 0.8368 0.122(5) Uiso 1 1 calc R . . H7H2 H 1.0617 -0.1134 0.8293 0.122(5) Uiso 1 1 calc R . . H7H3 H 0.9767 -0.0459 0.8002 0.122(5) Uiso 1 1 calc R . . C8H C 1.0655(6) 0.1254(4) 0.9510(3) 0.0524(19) Uani 1 1 d . . . H8H1 H 1.1457 0.0920 0.9349 0.078(6) Uiso 1 1 calc R . . H8H2 H 1.0575 0.1373 0.9917 0.078(6) Uiso 1 1 calc R . . C9H C 1.2683(7) 0.0112(5) 0.7584(3) 0.071(2) Uani 1 1 d . . . H9H1 H 1.2535 -0.0289 0.7370 0.122(5) Uiso 1 1 calc R . . H9H2 H 1.3243 -0.0157 0.7805 0.122(5) Uiso 1 1 calc R . . H9H3 H 1.2980 0.0447 0.7324 0.122(5) Uiso 1 1 calc R . . O1S O 0.6684(12) 0.1708(8) 0.1862(6) 0.247(3) Uiso 1 1 d D . . C1S C 0.5955(10) 0.2374(8) 0.2285(6) 0.157(5) Uiso 1 1 d D . . H1S1 H 0.6129 0.2867 0.2206 0.078(6) Uiso 1 1 calc R . . H1S2 H 0.6038 0.2233 0.2671 0.078(6) Uiso 1 1 calc R . . C2S C 0.4774(9) 0.2468(9) 0.2207(5) 0.247(3) Uiso 1 1 d D . . F1S F 0.4452(11) 0.1841(6) 0.2345(5) 0.247(3) Uiso 1 1 d D . . F2S F 0.3967(11) 0.3035(6) 0.2585(5) 0.247(3) Uiso 1 1 d D . . F3S F 0.4515(11) 0.2652(7) 0.1694(5) 0.247(3) Uiso 1 1 d D . . O2S O 0.9347(15) 0.1957(9) 0.2986(7) 0.291(3) Uiso 1 1 d D . . C3S C 0.8966(11) 0.2779(10) 0.2831(9) 0.291(3) Uiso 1 1 d D . . H3S1 H 0.8223 0.3099 0.3077 0.078(6) Uiso 1 1 calc R . . H3S2 H 0.8896 0.2801 0.2434 0.078(6) Uiso 1 1 calc R . . C4S C 0.9903(19) 0.3081(12) 0.2919(12) 0.291(3) Uiso 1 1 d D . . F4S F 1.0916(11) 0.2544(9) 0.2507(5) 0.291(3) Uiso 1 1 d D . . F5S F 0.9871(12) 0.3711(8) 0.2834(6) 0.291(3) Uiso 1 1 d D . . F6S F 1.0177(12) 0.2891(8) 0.3423(4) 0.291(3) 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 Cl1 0.105(2) 0.0936(18) 0.0740(16) 0.0114(13) -0.0143(14) -0.0285(16) Cl2 0.122(2) 0.163(3) 0.0814(19) 0.0134(19) -0.0238(17) -0.062(2) Ba1 0.0419(3) 0.0416(3) 0.0496(3) -0.00058(19) -0.0099(2) -0.0155(2) O1W 0.101(5) 0.088(4) 0.078(4) 0.035(3) -0.025(4) -0.044(4) O2W 0.051(3) 0.073(4) 0.067(3) 0.009(3) -0.007(3) -0.017(3) O3W 0.093(5) 0.175(7) 0.089(5) 0.068(5) -0.037(4) -0.048(5) P1A 0.0574(13) 0.0386(10) 0.0543(12) 0.0041(9) -0.0193(10) -0.0193(10) O1A 0.063(3) 0.040(3) 0.053(3) 0.001(2) -0.016(3) -0.021(2) O2A 0.062(3) 0.042(3) 0.065(3) 0.011(2) -0.022(3) -0.024(3) O3A 0.067(3) 0.043(3) 0.062(3) -0.005(2) -0.020(3) -0.026(3) P1B 0.0479(12) 0.0516(12) 0.0560(13) 0.0068(10) -0.0077(10) -0.0148(10) O1B 0.043(3) 0.058(3) 0.059(3) 0.002(3) -0.007(3) -0.014(3) O2B 0.042(3) 0.056(3) 0.056(3) 0.009(2) -0.004(3) -0.006(2) O3B 0.067(4) 0.075(4) 0.061(3) 0.019(3) -0.031(3) -0.032(3) P1C 0.0691(15) 0.0571(13) 0.0593(14) 0.0092(11) -0.0122(12) -0.0293(12) O1C 0.067(4) 0.048(3) 0.054(3) 0.015(2) -0.014(3) -0.020(3) O2C 0.064(3) 0.040(3) 0.066(3) 0.008(2) -0.006(3) -0.021(3) O3C 0.079(4) 0.093(4) 0.058(3) 0.025(3) -0.022(3) -0.036(3) P1D 0.0426(12) 0.0589(13) 0.0531(12) 0.0064(10) -0.0140(10) -0.0193(10) O1D 0.049(3) 0.062(3) 0.057(3) 0.012(3) -0.008(3) -0.022(3) O2D 0.039(3) 0.055(3) 0.061(3) -0.001(2) -0.011(2) -0.014(2) O3D 0.049(3) 0.061(3) 0.045(3) -0.001(2) -0.004(2) -0.020(3) P1E 0.0483(12) 0.0405(10) 0.0463(11) 0.0030(9) -0.0117(9) -0.0191(9) O1E 0.049(3) 0.042(3) 0.052(3) 0.013(2) -0.017(2) -0.022(2) O2E 0.059(3) 0.038(3) 0.048(3) 0.006(2) -0.008(2) -0.023(2) O3E 0.058(3) 0.049(3) 0.059(3) -0.007(2) -0.015(3) -0.022(3) P1F 0.0477(12) 0.0535(12) 0.0505(12) 0.0002(10) -0.0102(10) -0.0205(10) O1F 0.040(3) 0.047(3) 0.058(3) 0.000(2) -0.008(2) -0.017(2) O2F 0.041(3) 0.051(3) 0.057(3) 0.004(2) -0.005(2) -0.015(2) O3F 0.073(4) 0.078(4) 0.055(3) -0.014(3) 0.005(3) -0.041(3) P1G 0.0686(15) 0.0459(12) 0.0591(13) 0.0039(10) -0.0023(11) -0.0274(11) O1G 0.066(3) 0.047(3) 0.059(3) 0.004(2) 0.000(3) -0.029(3) O2G 0.064(4) 0.041(3) 0.078(4) 0.013(3) -0.008(3) -0.020(3) O3G 0.081(4) 0.059(3) 0.056(3) 0.012(3) -0.006(3) -0.031(3) P1H 0.0434(12) 0.0490(12) 0.0599(13) 0.0065(10) -0.0097(10) -0.0078(10) O1H 0.048(3) 0.049(3) 0.059(3) 0.009(2) -0.008(3) -0.007(2) O2H 0.043(3) 0.055(3) 0.065(3) 0.007(3) -0.016(3) -0.016(3) O3H 0.053(3) 0.054(3) 0.064(3) 0.011(3) -0.027(3) -0.011(3) C1A 0.061(5) 0.048(4) 0.041(4) -0.011(4) -0.018(4) -0.008(4) C2A 0.051(5) 0.035(4) 0.056(5) 0.000(4) -0.014(4) -0.012(4) C3A 0.052(5) 0.037(4) 0.053(5) -0.003(3) -0.014(4) -0.016(4) C4A 0.046(4) 0.037(4) 0.052(5) -0.008(3) -0.010(4) -0.006(4) C5A 0.041(4) 0.045(4) 0.060(5) -0.005(4) -0.017(4) -0.012(4) C6A 0.050(5) 0.040(4) 0.047(4) -0.011(3) -0.009(4) -0.009(4) C7A 0.062(5) 0.059(5) 0.071(5) 0.008(4) -0.033(4) -0.017(4) C8A 0.059(5) 0.054(5) 0.048(4) -0.006(4) -0.017(4) -0.021(4) C9A 0.091(7) 0.054(5) 0.072(6) 0.021(4) -0.026(5) -0.032(5) C1B 0.053(5) 0.062(5) 0.044(4) 0.004(4) -0.017(4) -0.032(4) C2B 0.033(4) 0.055(5) 0.053(5) -0.004(4) -0.012(4) -0.018(4) C3B 0.031(4) 0.059(5) 0.061(5) -0.009(4) -0.007(4) -0.017(4) C4B 0.039(4) 0.049(4) 0.052(5) 0.006(4) -0.014(4) -0.022(4) C5B 0.048(5) 0.050(5) 0.051(5) 0.004(4) -0.015(4) -0.024(4) C6B 0.047(4) 0.040(4) 0.049(5) -0.002(3) -0.018(4) -0.020(4) C7B 0.064(5) 0.070(5) 0.057(5) 0.012(4) -0.018(4) -0.036(4) C8B 0.049(5) 0.056(5) 0.062(5) 0.013(4) -0.024(4) -0.016(4) C9B 0.071(6) 0.068(6) 0.088(7) -0.003(5) 0.010(5) -0.027(5) C1C 0.057(5) 0.050(5) 0.037(4) 0.011(3) -0.015(4) -0.005(4) C2C 0.056(5) 0.051(5) 0.045(4) 0.019(4) -0.021(4) -0.020(4) C3C 0.054(5) 0.048(4) 0.051(5) 0.022(4) -0.025(4) -0.021(4) C4C 0.059(5) 0.042(4) 0.049(5) 0.014(4) -0.026(4) -0.014(4) C5C 0.042(4) 0.047(4) 0.049(5) 0.017(4) -0.017(4) -0.001(4) C6C 0.043(4) 0.047(4) 0.048(4) 0.016(4) -0.021(4) -0.008(4) C7C 0.068(6) 0.059(5) 0.066(5) -0.005(4) -0.004(4) -0.020(4) C8C 0.059(5) 0.051(4) 0.044(4) 0.015(4) -0.012(4) -0.015(4) C9C 0.089(7) 0.073(6) 0.126(9) -0.017(6) -0.019(6) -0.039(6) C1D 0.053(5) 0.071(5) 0.039(4) 0.016(4) -0.016(4) -0.032(4) C2D 0.047(5) 0.056(5) 0.035(4) 0.005(3) -0.001(4) -0.020(4) C3D 0.042(4) 0.060(5) 0.050(5) 0.016(4) -0.009(4) -0.017(4) C4D 0.044(4) 0.064(5) 0.047(4) 0.011(4) -0.009(4) -0.025(4) C5D 0.061(5) 0.048(5) 0.057(5) 0.018(4) -0.007(4) -0.022(4) C6D 0.057(5) 0.056(5) 0.045(4) 0.012(4) -0.010(4) -0.024(4) C7D 0.066(6) 0.077(6) 0.069(6) 0.006(5) -0.018(5) -0.031(5) C8D 0.055(5) 0.064(5) 0.039(4) 0.001(4) -0.005(4) -0.015(4) C9D 0.046(5) 0.084(6) 0.089(6) 0.009(5) -0.025(5) -0.027(5) C1E 0.042(4) 0.053(5) 0.038(4) 0.004(4) -0.015(3) -0.013(4) C2E 0.041(4) 0.043(4) 0.055(5) -0.002(4) -0.020(4) -0.018(4) C3E 0.038(4) 0.050(4) 0.050(5) 0.006(4) -0.019(4) -0.023(4) C4E 0.036(4) 0.046(4) 0.050(4) 0.012(4) -0.014(4) -0.014(4) C5E 0.031(4) 0.049(4) 0.052(5) 0.002(4) -0.014(4) -0.008(4) C6E 0.047(5) 0.055(5) 0.056(5) 0.011(4) -0.028(4) -0.021(4) C7E 0.047(5) 0.062(5) 0.059(5) 0.000(4) -0.002(4) -0.020(4) C8E 0.052(5) 0.051(4) 0.041(4) -0.001(3) -0.015(4) -0.025(4) C9E 0.082(6) 0.055(5) 0.053(5) 0.016(4) -0.017(4) -0.026(4) C1F 0.057(5) 0.040(4) 0.039(4) -0.003(3) -0.010(4) -0.018(4) C2F 0.044(4) 0.036(4) 0.047(4) -0.001(3) -0.009(3) -0.016(3) C3F 0.041(4) 0.034(4) 0.047(4) -0.002(3) -0.011(3) -0.012(3) C4F 0.051(5) 0.034(4) 0.047(4) 0.000(3) -0.017(4) -0.011(3) C5F 0.043(4) 0.031(4) 0.049(4) -0.006(3) -0.009(4) -0.014(3) C6F 0.043(4) 0.043(4) 0.040(4) -0.011(3) -0.005(3) -0.013(3) C7F 0.060(5) 0.056(5) 0.075(6) 0.006(4) -0.023(4) -0.019(4) C8F 0.046(4) 0.045(4) 0.042(4) -0.002(3) -0.004(3) -0.011(4) C9F 0.054(5) 0.093(6) 0.072(6) 0.012(5) -0.024(5) -0.027(5) C1G 0.054(5) 0.065(5) 0.034(4) 0.007(4) -0.006(4) -0.032(4) C2G 0.059(5) 0.049(5) 0.038(4) 0.010(4) -0.005(4) -0.018(4) C3G 0.071(6) 0.043(5) 0.046(5) 0.009(4) 0.004(4) -0.027(4) C4G 0.053(5) 0.049(5) 0.053(5) 0.003(4) 0.002(4) -0.025(4) C5G 0.041(4) 0.044(4) 0.046(4) 0.002(3) 0.001(3) -0.016(4) C6G 0.043(4) 0.046(4) 0.042(4) 0.008(3) 0.003(3) -0.021(4) C7G 0.067(6) 0.077(6) 0.080(6) -0.003(5) -0.019(5) -0.042(5) C8G 0.071(6) 0.047(4) 0.047(4) 0.011(4) -0.016(4) -0.015(4) C9G 0.096(7) 0.053(5) 0.083(6) -0.008(5) 0.006(5) -0.036(5) C1H 0.057(5) 0.042(4) 0.044(4) 0.018(3) -0.022(4) -0.014(4) C2H 0.050(5) 0.037(4) 0.053(5) 0.015(4) -0.018(4) -0.009(4) C3H 0.046(5) 0.044(4) 0.057(5) 0.018(4) -0.014(4) -0.005(4) C4H 0.059(5) 0.031(4) 0.067(5) 0.014(4) -0.021(4) -0.005(4) C5H 0.056(5) 0.040(4) 0.064(5) 0.013(4) -0.013(4) -0.016(4) C6H 0.051(5) 0.038(4) 0.048(5) 0.022(4) -0.010(4) -0.005(4) C7H 0.066(6) 0.056(5) 0.077(6) -0.008(4) 0.003(5) -0.012(4) C8H 0.046(4) 0.060(5) 0.052(5) 0.015(4) -0.024(4) -0.011(4) C9H 0.056(5) 0.071(6) 0.069(6) 0.012(5) -0.001(4) -0.009(4) _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 Ba1 O2W 2.684(5) . ? Ba1 O3E 2.691(4) . ? Ba1 O3A 2.709(4) . ? Ba1 O1W 2.812(5) . ? Ba1 O3D 2.826(5) . ? Ba1 O3W 2.834(6) . ? Ba1 O3H 2.846(4) . ? P1A O3A 1.460(5) . ? P1A O2A 1.584(5) . ? P1A O1A 1.598(5) . ? P1A C9A 1.747(7) . ? O1A C3A 1.427(8) . ? O2A C5B 1.410(8) . ? P1B O3B 1.463(5) . ? P1B O2B 1.589(5) . ? P1B O1B 1.597(5) . ? P1B C9B 1.751(8) . ? O1B C3B 1.436(8) . ? O2B C5C 1.427(8) . ? P1C O3C 1.460(5) . ? P1C O2C 1.591(5) . ? P1C O1C 1.592(5) . ? P1C C9C 1.754(8) . ? O1C C3C 1.419(8) . ? O2C C5D 1.426(8) . ? P1D O3D 1.473(5) . ? P1D O1D 1.587(5) . ? P1D O2D 1.589(5) . ? P1D C9D 1.760(7) . ? O1D C3D 1.408(8) . ? O2D C5A 1.407(8) . ? P1E O3E 1.462(5) . ? P1E O2E 1.585(5) . ? P1E O1E 1.595(5) . ? P1E C9E 1.763(7) . ? O1E C3E 1.416(7) . ? O2E C5F 1.414(8) . ? P1F O3F 1.452(5) . ? P1F O2F 1.581(5) . ? P1F O1F 1.591(5) . ? P1F C9F 1.769(8) . ? O1F C3F 1.419(8) . ? O2F C5G 1.408(8) . ? P1G O3G 1.453(5) . ? P1G O1G 1.590(5) . ? P1G O2G 1.593(6) . ? P1G C9G 1.764(7) . ? O1G C3G 1.414(8) . ? O2G C5H 1.410(8) . ? P1H O3H 1.462(5) . ? P1H O1H 1.587(5) . ? P1H O2H 1.604(5) . ? P1H C9H 1.778(8) . ? O1H C3H 1.418(8) . ? O2H C5E 1.421(8) . ? C1A C2A 1.387(10) . ? C1A C6A 1.410(10) . ? C1A H1A 0.9300 . ? C2A C3A 1.379(9) . ? C2A C8A 1.509(9) . ? C3A C4A 1.375(9) . ? C4A C5A 1.402(10) . ? C4A C7A 1.502(9) . ? C5A C6A 1.408(10) . ? C6A C8D 1.508(10) . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C8A C6B 1.520(9) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C1B C2B 1.382(9) . ? C1B C6B 1.386(9) . ? C1B H1B 0.9300 . ? C2B C3B 1.389(10) . ? C2B C8B 1.517(9) . ? C3B C4B 1.398(9) . ? C4B C5B 1.379(9) . ? C4B C7B 1.501(9) . ? C5B C6B 1.387(9) . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? C8B C6C 1.506(10) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C1C C2C 1.371(10) . ? C1C C6C 1.378(10) . ? C1C H1C 0.9300 . ? C2C C3C 1.381(10) . ? C2C C8C 1.518(10) . ? C3C C4C 1.398(10) . ? C4C C5C 1.394(10) . ? C4C C7C 1.479(10) . ? C5C C6C 1.386(10) . ? C7C H7C1 0.9600 . ? C7C H7C2 0.9600 . ? C7C H7C3 0.9600 . ? C8C C6D 1.525(10) . ? C8C H8C1 0.9700 . ? C8C H8C2 0.9700 . ? C9C H9C1 0.9600 . ? C9C H9C2 0.9600 . ? C9C H9C3 0.9600 . ? C1D C2D 1.378(9) . ? C1D C6D 1.380(10) . ? C1D H1D 0.9300 . ? C2D C3D 1.396(10) . ? C2D C8D 1.513(10) . ? C3D C4D 1.399(10) . ? C4D C5D 1.387(10) . ? C4D C7D 1.499(10) . ? C5D C6D 1.373(10) . ? C7D H7D1 0.9600 . ? C7D H7D2 0.9600 . ? C7D H7D3 0.9600 . ? C8D H8D1 0.9700 . ? C8D H8D2 0.9700 . ? C9D H9D1 0.9600 . ? C9D H9D2 0.9600 . ? C9D H9D3 0.9600 . ? C1E C2E 1.377(9) . ? C1E C6E 1.394(9) . ? C1E H1E 0.9300 . ? C2E C3E 1.366(9) . ? C2E C8E 1.514(9) . ? C3E C4E 1.411(9) . ? C4E C5E 1.381(9) . ? C4E C7E 1.495(9) . ? C5E C6E 1.379(9) . ? C6E C8H 1.534(9) . ? C7E H7E1 0.9600 . ? C7E H7E2 0.9600 . ? C7E H7E3 0.9600 . ? C8E C6F 1.529(9) . ? C8E H8E1 0.9700 . ? C8E H8E2 0.9700 . ? C9E H9E1 0.9600 . ? C9E H9E2 0.9600 . ? C9E H9E3 0.9600 . ? C1F C2F 1.391(9) . ? C1F C6F 1.399(9) . ? C1F H1F 0.9300 . ? C2F C3F 1.380(9) . ? C2F C8F 1.518(9) . ? C3F C4F 1.386(9) . ? C4F C5F 1.395(9) . ? C4F C7F 1.516(9) . ? C5F C6F 1.383(9) . ? C7F H7F1 0.9600 . ? C7F H7F2 0.9600 . ? C7F H7F3 0.9600 . ? C8F C6G 1.509(9) . ? C8F H8F1 0.9700 . ? C8F H8F2 0.9700 . ? C9F H9F1 0.9600 . ? C9F H9F2 0.9600 . ? C9F H9F3 0.9600 . ? C1G C6G 1.382(9) . ? C1G C2G 1.392(10) . ? C1G H1G 0.9300 . ? C2G C3G 1.395(10) . ? C2G C8G 1.492(10) . ? C3G C4G 1.412(10) . ? C4G C5G 1.387(9) . ? C4G C7G 1.496(10) . ? C5G C6G 1.387(9) . ? C7G H7G1 0.9600 . ? C7G H7G2 0.9600 . ? C7G H7G3 0.9600 . ? C8G C6H 1.526(10) . ? C8G H8G1 0.9700 . ? C8G H8G2 0.9700 . ? C9G H9G1 0.9600 . ? C9G H9G2 0.9600 . ? C9G H9G3 0.9600 . ? C1H C2H 1.377(10) . ? C1H C6H 1.382(10) . ? C1H H1H 0.9300 . ? C2H C3H 1.375(10) . ? C2H C8H 1.515(9) . ? C3H C4H 1.402(10) . ? C4H C5H 1.382(10) . ? C4H C7H 1.497(10) . ? C5H C6H 1.380(10) . ? C7H H7H1 0.9600 . ? C7H H7H2 0.9600 . ? C7H H7H3 0.9600 . ? C8H H8H1 0.9700 . ? C8H H8H2 0.9700 . ? C9H H9H1 0.9600 . ? C9H H9H2 0.9600 . ? C9H H9H3 0.9600 . ? O1S C1S 1.449(5) . ? C1S C2S 1.490(5) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S F1S 1.315(5) . ? C2S F2S 1.323(5) . ? C2S F3S 1.343(5) . ? O2S C3S 1.43(2) . ? C3S C4S 1.501(5) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S F5S 1.108(19) . ? C4S F6S 1.33(2) . ? C4S F4S 1.46(3) . ? 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 O2W Ba1 O3E 76.05(15) . . ? O2W Ba1 O3A 81.81(15) . . ? O3E Ba1 O3A 157.81(15) . . ? O2W Ba1 O1W 66.62(17) . . ? O3E Ba1 O1W 92.99(16) . . ? O3A Ba1 O1W 76.66(16) . . ? O2W Ba1 O3D 146.16(15) . . ? O3E Ba1 O3D 93.75(14) . . ? O3A Ba1 O3D 105.65(14) . . ? O1W Ba1 O3D 147.01(16) . . ? O2W Ba1 O3W 70.09(17) . . ? O3E Ba1 O3W 73.9(2) . . ? O3A Ba1 O3W 100.04(19) . . ? O1W Ba1 O3W 136.63(18) . . ? O3D Ba1 O3W 76.10(17) . . ? O2W Ba1 O3H 136.47(15) . . ? O3E Ba1 O3H 103.11(14) . . ? O3A Ba1 O3H 91.85(14) . . ? O1W Ba1 O3H 70.00(16) . . ? O3D Ba1 O3H 77.02(14) . . ? O3W Ba1 O3H 152.67(17) . . ? O3A P1A O2A 114.0(3) . . ? O3A P1A O1A 112.0(3) . . ? O2A P1A O1A 106.1(3) . . ? O3A P1A C9A 118.5(3) . . ? O2A P1A C9A 102.6(3) . . ? O1A P1A C9A 102.3(3) . . ? C3A O1A P1A 118.8(4) . . ? C5B O2A P1A 123.9(4) . . ? P1A O3A Ba1 168.7(3) . . ? O3B P1B O2B 112.7(3) . . ? O3B P1B O1B 113.1(3) . . ? O2B P1B O1B 106.1(3) . . ? O3B P1B C9B 116.9(4) . . ? O2B P1B C9B 103.7(4) . . ? O1B P1B C9B 103.3(3) . . ? C3B O1B P1B 121.5(4) . . ? C5C O2B P1B 117.9(4) . . ? O3C P1C O2C 112.5(3) . . ? O3C P1C O1C 113.3(3) . . ? O2C P1C O1C 106.3(3) . . ? O3C P1C C9C 119.5(4) . . ? O2C P1C C9C 102.1(4) . . ? O1C P1C C9C 101.5(4) . . ? C3C O1C P1C 119.0(4) . . ? C5D O2C P1C 120.5(4) . . ? O3D P1D O1D 114.2(3) . . ? O3D P1D O2D 113.4(3) . . ? O1D P1D O2D 106.3(3) . . ? O3D P1D C9D 117.9(4) . . ? O1D P1D C9D 101.1(3) . . ? O2D P1D C9D 102.4(3) . . ? C3D O1D P1D 124.4(4) . . ? C5A O2D P1D 118.4(4) . . ? P1D O3D Ba1 162.4(3) . . ? O3E P1E O2E 114.6(3) . . ? O3E P1E O1E 111.2(3) . . ? O2E P1E O1E 106.7(3) . . ? O3E P1E C9E 117.8(3) . . ? O2E P1E C9E 102.7(3) . . ? O1E P1E C9E 102.6(3) . . ? C3E O1E P1E 118.1(4) . . ? C5F O2E P1E 125.3(4) . . ? P1E O3E Ba1 171.9(3) . . ? O3F P1F O2F 113.9(3) . . ? O3F P1F O1F 113.5(3) . . ? O2F P1F O1F 107.0(3) . . ? O3F P1F C9F 117.5(4) . . ? O2F P1F C9F 100.9(3) . . ? O1F P1F C9F 102.6(3) . . ? C3F O1F P1F 124.6(4) . . ? C5G O2F P1F 124.5(4) . . ? O3G P1G O1G 113.4(3) . . ? O3G P1G O2G 113.0(3) . . ? O1G P1G O2G 106.7(3) . . ? O3G P1G C9G 118.5(4) . . ? O1G P1G C9G 102.0(3) . . ? O2G P1G C9G 101.8(4) . . ? C3G O1G P1G 121.2(4) . . ? C5H O2G P1G 120.6(4) . . ? O3H P1H O1H 114.6(3) . . ? O3H P1H O2H 112.6(3) . . ? O1H P1H O2H 106.0(3) . . ? O3H P1H C9H 117.3(4) . . ? O1H P1H C9H 101.7(3) . . ? O2H P1H C9H 103.2(4) . . ? C3H O1H P1H 124.3(4) . . ? C5E O2H P1H 118.2(4) . . ? P1H O3H Ba1 166.2(3) . . ? C2A C1A C6A 121.3(7) . . ? C2A C1A H1A 119.4 . . ? C6A C1A H1A 119.4 . . ? C3A C2A C1A 117.5(7) . . ? C3A C2A C8A 122.8(6) . . ? C1A C2A C8A 119.6(6) . . ? C4A C3A C2A 125.9(7) . . ? C4A C3A O1A 116.3(6) . . ? C2A C3A O1A 117.8(6) . . ? C3A C4A C5A 114.5(6) . . ? C3A C4A C7A 124.8(7) . . ? C5A C4A C7A 120.8(6) . . ? C4A C5A O2D 118.1(6) . . ? C4A C5A C6A 123.7(6) . . ? O2D C5A C6A 118.1(6) . . ? C5A C6A C1A 117.0(7) . . ? C5A C6A C8D 121.3(7) . . ? C1A C6A C8D 121.6(7) . . ? C4A C7A H7A1 109.5 . . ? C4A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C4A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C2A C8A C6B 111.3(5) . . ? C2A C8A H8A1 109.4 . . ? C6B C8A H8A1 109.4 . . ? C2A C8A H8A2 109.4 . . ? C6B C8A H8A2 109.4 . . ? H8A1 C8A H8A2 108.0 . . ? P1A C9A H9A1 109.5 . . ? P1A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? P1A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C2B C1B C6B 122.9(7) . . ? C2B C1B H1B 118.5 . . ? C6B C1B H1B 118.5 . . ? C1B C2B C3B 116.6(7) . . ? C1B C2B C8B 120.0(7) . . ? C3B C2B C8B 123.5(7) . . ? C2B C3B C4B 124.1(7) . . ? C2B C3B O1B 118.0(7) . . ? C4B C3B O1B 117.8(6) . . ? C5B C4B C3B 115.1(6) . . ? C5B C4B C7B 123.3(7) . . ? C3B C4B C7B 121.6(7) . . ? C4B C5B C6B 124.4(7) . . ? C4B C5B O2A 116.6(6) . . ? C6B C5B O2A 118.8(6) . . ? C1B C6B C5B 116.9(6) . . ? C1B C6B C8A 120.0(6) . . ? C5B C6B C8A 123.0(6) . . ? C4B C7B H7B1 109.5 . . ? C4B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C4B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C6C C8B C2B 112.2(6) . . ? C6C C8B H8B1 109.2 . . ? C2B C8B H8B1 109.2 . . ? C6C C8B H8B2 109.2 . . ? C2B C8B H8B2 109.2 . . ? H8B1 C8B H8B2 107.9 . . ? P1B C9B H9B1 109.5 . . ? P1B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? P1B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C2C C1C C6C 122.7(7) . . ? C2C C1C H1C 118.7 . . ? C6C C1C H1C 118.7 . . ? C1C C2C C3C 117.6(7) . . ? C1C C2C C8C 121.0(7) . . ? C3C C2C C8C 121.3(7) . . ? C2C C3C C4C 124.0(7) . . ? C2C C3C O1C 119.5(6) . . ? C4C C3C O1C 116.4(7) . . ? C5C C4C C3C 114.5(7) . . ? C5C C4C C7C 121.7(7) . . ? C3C C4C C7C 123.7(7) . . ? C6C C5C C4C 124.1(7) . . ? C6C C5C O2B 118.2(7) . . ? C4C C5C O2B 117.7(7) . . ? C1C C6C C5C 117.2(7) . . ? C1C C6C C8B 121.6(7) . . ? C5C C6C C8B 121.2(7) . . ? C4C C7C H7C1 109.5 . . ? C4C C7C H7C2 109.5 . . ? H7C1 C7C H7C2 109.5 . . ? C4C C7C H7C3 109.5 . . ? H7C1 C7C H7C3 109.5 . . ? H7C2 C7C H7C3 109.5 . . ? C2C C8C C6D 110.8(5) . . ? C2C C8C H8C1 109.5 . . ? C6D C8C H8C1 109.5 . . ? C2C C8C H8C2 109.5 . . ? C6D C8C H8C2 109.5 . . ? H8C1 C8C H8C2 108.1 . . ? P1C C9C H9C1 109.5 . . ? P1C C9C H9C2 109.5 . . ? H9C1 C9C H9C2 109.5 . . ? P1C C9C H9C3 109.5 . . ? H9C1 C9C H9C3 109.5 . . ? H9C2 C9C H9C3 109.5 . . ? C2D C1D C6D 122.7(7) . . ? C2D C1D H1D 118.6 . . ? C6D C1D H1D 118.6 . . ? C1D C2D C3D 117.5(7) . . ? C1D C2D C8D 121.2(7) . . ? C3D C2D C8D 121.2(7) . . ? C2D C3D C4D 122.6(7) . . ? C2D C3D O1D 120.0(7) . . ? C4D C3D O1D 117.3(7) . . ? C5D C4D C3D 115.4(7) . . ? C5D C4D C7D 124.3(7) . . ? C3D C4D C7D 120.3(7) . . ? C6D C5D C4D 124.7(7) . . ? C6D C5D O2C 119.1(7) . . ? C4D C5D O2C 116.0(7) . . ? C5D C6D C1D 116.9(7) . . ? C5D C6D C8C 121.8(7) . . ? C1D C6D C8C 121.2(7) . . ? C4D C7D H7D1 109.5 . . ? C4D C7D H7D2 109.5 . . ? H7D1 C7D H7D2 109.5 . . ? C4D C7D H7D3 109.5 . . ? H7D1 C7D H7D3 109.5 . . ? H7D2 C7D H7D3 109.5 . . ? C6A C8D C2D 112.3(6) . . ? C6A C8D H8D1 109.2 . . ? C2D C8D H8D1 109.2 . . ? C6A C8D H8D2 109.2 . . ? C2D C8D H8D2 109.2 . . ? H8D1 C8D H8D2 107.9 . . ? P1D C9D H9D1 109.5 . . ? P1D C9D H9D2 109.5 . . ? H9D1 C9D H9D2 109.5 . . ? P1D C9D H9D3 109.5 . . ? H9D1 C9D H9D3 109.5 . . ? H9D2 C9D H9D3 109.5 . . ? C2E C1E C6E 121.1(6) . . ? C2E C1E H1E 119.4 . . ? C6E C1E H1E 119.4 . . ? C3E C2E C1E 118.6(6) . . ? C3E C2E C8E 121.6(6) . . ? C1E C2E C8E 119.8(6) . . ? C2E C3E C4E 123.5(6) . . ? C2E C3E O1E 119.3(6) . . ? C4E C3E O1E 117.2(6) . . ? C5E C4E C3E 114.7(6) . . ? C5E C4E C7E 122.7(6) . . ? C3E C4E C7E 122.6(6) . . ? C6E C5E C4E 124.4(7) . . ? C6E C5E O2H 118.8(6) . . ? C4E C5E O2H 116.8(6) . . ? C5E C6E C1E 117.6(6) . . ? C5E C6E C8H 122.1(7) . . ? C1E C6E C8H 120.3(7) . . ? C4E C7E H7E1 109.5 . . ? C4E C7E H7E2 109.5 . . ? H7E1 C7E H7E2 109.5 . . ? C4E C7E H7E3 109.5 . . ? H7E1 C7E H7E3 109.5 . . ? H7E2 C7E H7E3 109.5 . . ? C2E C8E C6F 111.2(5) . . ? C2E C8E H8E1 109.4 . . ? C6F C8E H8E1 109.4 . . ? C2E C8E H8E2 109.4 . . ? C6F C8E H8E2 109.4 . . ? H8E1 C8E H8E2 108.0 . . ? P1E C9E H9E1 109.5 . . ? P1E C9E H9E2 109.5 . . ? H9E1 C9E H9E2 109.5 . . ? P1E C9E H9E3 109.5 . . ? H9E1 C9E H9E3 109.5 . . ? H9E2 C9E H9E3 109.5 . . ? C2F C1F C6F 121.4(6) . . ? C2F C1F H1F 119.3 . . ? C6F C1F H1F 119.3 . . ? C3F C2F C1F 117.4(6) . . ? C3F C2F C8F 122.6(6) . . ? C1F C2F C8F 119.9(6) . . ? C2F C3F C4F 124.5(6) . . ? C2F C3F O1F 118.2(6) . . ? C4F C3F O1F 117.1(6) . . ? C3F C4F C5F 115.4(6) . . ? C3F C4F C7F 122.8(6) . . ? C5F C4F C7F 121.7(6) . . ? C6F C5F C4F 123.5(6) . . ? C6F C5F O2E 119.2(6) . . ? C4F C5F O2E 117.0(6) . . ? C5F C6F C1F 117.8(6) . . ? C5F C6F C8E 122.1(6) . . ? C1F C6F C8E 120.1(6) . . ? C4F C7F H7F1 109.5 . . ? C4F C7F H7F2 109.5 . . ? H7F1 C7F H7F2 109.5 . . ? C4F C7F H7F3 109.5 . . ? H7F1 C7F H7F3 109.5 . . ? H7F2 C7F H7F3 109.5 . . ? C6G C8F C2F 110.4(5) . . ? C6G C8F H8F1 109.6 . . ? C2F C8F H8F1 109.6 . . ? C6G C8F H8F2 109.6 . . ? C2F C8F H8F2 109.6 . . ? H8F1 C8F H8F2 108.1 . . ? P1F C9F H9F1 109.5 . . ? P1F C9F H9F2 109.5 . . ? H9F1 C9F H9F2 109.5 . . ? P1F C9F H9F3 109.5 . . ? H9F1 C9F H9F3 109.5 . . ? H9F2 C9F H9F3 109.5 . . ? C6G C1G C2G 123.4(7) . . ? C6G C1G H1G 118.3 . . ? C2G C1G H1G 118.3 . . ? C1G C2G C3G 115.6(7) . . ? C1G C2G C8G 121.7(7) . . ? C3G C2G C8G 122.6(7) . . ? C2G C3G C4G 124.7(7) . . ? C2G C3G O1G 117.9(7) . . ? C4G C3G O1G 117.4(7) . . ? C5G C4G C3G 114.8(7) . . ? C5G C4G C7G 122.6(7) . . ? C3G C4G C7G 122.5(7) . . ? C4G C5G C6G 124.0(7) . . ? C4G C5G O2F 117.2(6) . . ? C6G C5G O2F 118.8(6) . . ? C1G C6G C5G 117.5(6) . . ? C1G C6G C8F 120.7(6) . . ? C5G C6G C8F 121.7(6) . . ? C4G C7G H7G1 109.5 . . ? C4G C7G H7G2 109.5 . . ? H7G1 C7G H7G2 109.5 . . ? C4G C7G H7G3 109.5 . . ? H7G1 C7G H7G3 109.5 . . ? H7G2 C7G H7G3 109.5 . . ? C2G C8G C6H 111.7(5) . . ? C2G C8G H8G1 109.3 . . ? C6H C8G H8G1 109.3 . . ? C2G C8G H8G2 109.3 . . ? C6H C8G H8G2 109.3 . . ? H8G1 C8G H8G2 107.9 . . ? P1G C9G H9G1 109.5 . . ? P1G C9G H9G2 109.5 . . ? H9G1 C9G H9G2 109.5 . . ? P1G C9G H9G3 109.5 . . ? H9G1 C9G H9G3 109.5 . . ? H9G2 C9G H9G3 109.5 . . ? C2H C1H C6H 122.2(7) . . ? C2H C1H H1H 118.9 . . ? C6H C1H H1H 118.9 . . ? C3H C2H C1H 117.9(7) . . ? C3H C2H C8H 120.1(7) . . ? C1H C2H C8H 122.0(7) . . ? C2H C3H C4H 123.2(7) . . ? C2H C3H O1H 120.3(7) . . ? C4H C3H O1H 116.3(7) . . ? C5H C4H C3H 115.3(7) . . ? C5H C4H C7H 123.1(7) . . ? C3H C4H C7H 121.6(7) . . ? C6H C5H C4H 124.1(7) . . ? C6H C5H O2G 118.5(7) . . ? C4H C5H O2G 117.4(7) . . ? C5H C6H C1H 117.2(7) . . ? C5H C6H C8G 121.6(7) . . ? C1H C6H C8G 121.1(7) . . ? C4H C7H H7H1 109.5 . . ? C4H C7H H7H2 109.5 . . ? H7H1 C7H H7H2 109.5 . . ? C4H C7H H7H3 109.5 . . ? H7H1 C7H H7H3 109.5 . . ? H7H2 C7H H7H3 109.5 . . ? C2H C8H C6E 111.2(5) . . ? C2H C8H H8H1 109.4 . . ? C6E C8H H8H1 109.4 . . ? C2H C8H H8H2 109.4 . . ? C6E C8H H8H2 109.4 . . ? H8H1 C8H H8H2 108.0 . . ? P1H C9H H9H1 109.5 . . ? P1H C9H H9H2 109.5 . . ? H9H1 C9H H9H2 109.5 . . ? P1H C9H H9H3 109.5 . . ? H9H1 C9H H9H3 109.5 . . ? H9H2 C9H H9H3 109.5 . . ? O1S C1S C2S 101.8(11) . . ? O1S C1S H1S1 111.4 . . ? C2S C1S H1S1 111.4 . . ? O1S C1S H1S2 111.4 . . ? C2S C1S H1S2 111.4 . . ? H1S1 C1S H1S2 109.3 . . ? F1S C2S F2S 99.4(5) . . ? F1S C2S F3S 105.1(12) . . ? F2S C2S F3S 105.6(12) . . ? F1S C2S C1S 114.6(13) . . ? F2S C2S C1S 110.8(12) . . ? F3S C2S C1S 119.2(11) . . ? O2S C3S C4S 103.6(11) . . ? O2S C3S H3S1 111.0 . . ? C4S C3S H3S1 111.0 . . ? O2S C3S H3S2 111.0 . . ? C4S C3S H3S2 111.0 . . ? H3S1 C3S H3S2 109.0 . . ? F5S C4S F6S 110.3(16) . . ? F5S C4S F4S 106(2) . . ? F6S C4S F4S 103.0(15) . . ? F5S C4S C3S 122.0(16) . . ? F6S C4S C3S 111.3(19) . . ? F4S C4S C3S 102.2(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.36 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.940 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.090 #Data for compound 2 data_tpoicacl2 _database_code_depnum_ccdc_archive 'CCDC 767370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H92 Ca Cl2 F12 O32 P8' _chemical_formula_weight 2152.28 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' 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' Ca Ca 0.2262 0.3064 '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 12.6644(17) _cell_length_b 13.9674(19) _cell_length_c 16.164(2) _cell_angle_alpha 106.558(2) _cell_angle_beta 112.004(2) _cell_angle_gamma 97.153(3) _cell_volume 2453.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8578 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 27.94 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1110 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758582 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Bruker AXS SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER AXS SMART 1000' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean '8.192 pixels/mm' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30502 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.94 _reflns_number_total 11663 _reflns_number_gt 5815 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement ? _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SIR97 (Giacovazzo et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11663 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1437 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2291 _refine_ls_wR_factor_gt 0.1974 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.5000 1.0000 0.5000 0.0656(5) Uani 1 2 d S . . Cl1 Cl 0.55665(13) 0.38620(12) 0.17148(11) 0.0613(4) Uani 1 1 d . . . O1W O 0.3706(4) 1.0872(3) 0.5366(3) 0.0746(12) Uani 1 1 d . . . O2W O 0.4400(8) 0.9916(7) 0.3408(6) 0.172(3) Uiso 1 1 d . . . P1A P 0.73966(10) 1.25725(9) 0.62317(8) 0.0330(3) Uani 1 1 d . . . O1A O 0.6943(2) 1.3590(2) 0.6282(2) 0.0296(6) Uani 1 1 d . . . O2A O 0.8364(2) 1.2654(2) 0.5829(2) 0.0322(7) Uani 1 1 d . . . O3A O 0.6449(3) 1.1607(2) 0.5659(2) 0.0437(8) Uani 1 1 d . . . C1A C 0.5228(4) 1.3859(3) 0.3996(3) 0.0281(9) Uani 1 1 d . . . H1A H 0.5335 1.3954 0.3484 0.030(6) Uiso 1 1 calc R . . C2A C 0.6180(3) 1.3788(3) 0.4744(3) 0.0260(8) Uani 1 1 d . . . C3A C 0.5976(3) 1.3637(3) 0.5490(3) 0.0265(9) Uani 1 1 d . . . C4A C 0.4903(4) 1.3581(3) 0.5553(3) 0.0294(9) Uani 1 1 d . . . C5A C 0.3991(3) 1.3658(3) 0.4771(3) 0.0292(9) Uani 1 1 d . . . C6A C 0.4117(3) 1.3793(3) 0.3988(3) 0.0282(9) Uani 1 1 d . . . C7A C 0.4756(4) 1.3511(4) 0.6416(3) 0.0381(10) Uani 1 1 d . . . H7A1 H 0.5192 1.3056 0.6650 0.096(5) Uiso 1 1 calc R . . H7A2 H 0.3936 1.3247 0.6242 0.096(5) Uiso 1 1 calc R . . H7A3 H 0.5046 1.4187 0.6905 0.096(5) Uiso 1 1 calc R . . C8A C 0.7388(3) 1.3908(3) 0.4749(3) 0.0291(9) Uani 1 1 d . . . H8A1 H 0.7987 1.4242 0.5403 0.065(5) Uiso 1 1 calc R . . H8A2 H 0.7467 1.4352 0.4399 0.065(5) Uiso 1 1 calc R . . C9A C 0.8263(5) 1.2802(4) 0.7445(4) 0.0505(13) Uani 1 1 d . . . H9A1 H 0.7764 1.2800 0.7769 0.096(5) Uiso 1 1 calc R . . H9A2 H 0.8828 1.3463 0.7732 0.096(5) Uiso 1 1 calc R . . H9A3 H 0.8668 1.2270 0.7495 0.096(5) Uiso 1 1 calc R . . P1B P 0.71536(12) 0.89709(10) 0.24710(10) 0.0480(4) Uani 1 1 d . . . O1B O 0.8160(3) 1.0027(2) 0.3052(2) 0.0427(8) Uani 1 1 d . . . O2B O 0.6457(3) 0.8942(2) 0.1418(2) 0.0418(8) Uani 1 1 d . . . O3B O 0.6397(3) 0.8831(3) 0.2933(3) 0.0635(11) Uani 1 1 d . . . C1B C 0.7318(3) 1.2492(3) 0.3336(3) 0.0307(9) Uani 1 1 d . . . H1B H 0.7023 1.2884 0.2968 0.030(6) Uiso 1 1 calc R . . C2B C 0.7465(3) 1.1536(3) 0.2897(3) 0.0330(10) Uani 1 1 d . . . C3B C 0.7934(3) 1.0974(3) 0.3467(3) 0.0341(10) Uani 1 1 d . . . C4B C 0.8247(3) 1.1321(3) 0.4453(3) 0.0338(10) Uani 1 1 d . . . C5B C 0.8042(3) 1.2269(3) 0.4838(3) 0.0290(9) Uani 1 1 d . . . C6B C 0.7595(3) 1.2874(3) 0.4301(3) 0.0269(9) Uani 1 1 d . . . C7B C 0.8815(4) 1.0733(4) 0.5071(4) 0.0456(12) Uani 1 1 d . . . H7B1 H 0.9636 1.1082 0.5457 0.096(5) Uiso 1 1 calc R . . H7B2 H 0.8738 1.0046 0.4672 0.096(5) Uiso 1 1 calc R . . H7B3 H 0.8434 1.0694 0.5478 0.096(5) Uiso 1 1 calc R . . C8B C 0.7057(4) 1.1121(4) 0.1829(3) 0.0383(11) Uani 1 1 d . . . H8B1 H 0.7560 1.0704 0.1672 0.065(5) Uiso 1 1 calc R . . H8B2 H 0.7116 1.1692 0.1606 0.065(5) Uiso 1 1 calc R . . C9B C 0.7982(6) 0.8061(5) 0.2296(5) 0.091(3) Uani 1 1 d . . . H9B1 H 0.8332 0.7911 0.2868 0.096(5) Uiso 1 1 calc R . . H9B2 H 0.8591 0.8343 0.2149 0.096(5) Uiso 1 1 calc R . . H9B3 H 0.7471 0.7436 0.1775 0.096(5) Uiso 1 1 calc R . . P1C P 0.15616(10) 0.87407(8) 0.07128(8) 0.0315(3) Uani 1 1 d . . . O1C O 0.2294(2) 0.8688(2) 0.0095(2) 0.0329(7) Uani 1 1 d . . . O2C O 0.0912(2) 0.9632(2) 0.0601(2) 0.0322(7) Uani 1 1 d . . . O3C O 0.2291(3) 0.8891(2) 0.1720(2) 0.0381(7) Uani 1 1 d . . . C1C C 0.4851(4) 1.0904(3) 0.1041(3) 0.0330(10) Uani 1 1 d . . . H1C H 0.5015 1.1602 0.1125 0.030(6) Uiso 1 1 calc R . . C2C C 0.3679(4) 1.0343(3) 0.0631(3) 0.0296(9) Uani 1 1 d . . . C3C C 0.3476(4) 0.9300(3) 0.0524(3) 0.0316(9) Uani 1 1 d . . . C4C C 0.4362(4) 0.8800(3) 0.0785(3) 0.0338(10) Uani 1 1 d . . . C5C C 0.5516(4) 0.9417(3) 0.1189(3) 0.0349(10) Uani 1 1 d . . . C6C C 0.5783(4) 1.0467(3) 0.1330(3) 0.0321(9) Uani 1 1 d . . . C7C C 0.4107(4) 0.7658(3) 0.0631(3) 0.0430(11) Uani 1 1 d . . . H7C1 H 0.4143 0.7570 0.1208 0.096(5) Uiso 1 1 calc R . . H7C2 H 0.4682 0.7370 0.0464 0.096(5) Uiso 1 1 calc R . . H7C3 H 0.3333 0.7309 0.0122 0.096(5) Uiso 1 1 calc R . . C8C C 0.2675(4) 1.0832(3) 0.0309(3) 0.0326(9) Uani 1 1 d . . . H8C1 H 0.2919 1.1381 0.0111 0.065(5) Uiso 1 1 calc R . . H8C2 H 0.2011 1.0316 -0.0241 0.065(5) Uiso 1 1 calc R . . C9C C 0.0376(4) 0.7619(3) 0.0001(4) 0.0458(12) Uani 1 1 d . . . H9C1 H 0.0677 0.7018 -0.0070 0.096(5) Uiso 1 1 calc R . . H9C2 H -0.0051 0.7652 -0.0618 0.096(5) Uiso 1 1 calc R . . H9C3 H -0.0143 0.7578 0.0303 0.096(5) Uiso 1 1 calc R . . P1D P 0.18079(10) 1.26676(9) 0.42943(9) 0.0370(3) Uani 1 1 d . . . O1D O 0.1178(2) 1.2538(2) 0.3200(2) 0.0360(7) Uani 1 1 d . . . O2D O 0.2891(2) 1.3669(2) 0.4815(2) 0.0344(7) Uani 1 1 d . . . O3D O 0.2133(3) 1.1729(3) 0.4415(2) 0.0519(9) Uani 1 1 d . . . C1D C 0.2774(4) 1.2307(3) 0.1703(3) 0.0308(9) Uani 1 1 d . . . H1D H 0.3343 1.2720 0.1630 0.030(6) Uiso 1 1 calc R . . C2D C 0.2442(3) 1.2736(3) 0.2421(3) 0.0301(9) Uani 1 1 d . . . C3D C 0.1594(3) 1.2102(3) 0.2514(3) 0.0307(9) Uani 1 1 d . . . C4D C 0.1083(3) 1.1055(3) 0.1937(3) 0.0321(9) Uani 1 1 d . . . C5D C 0.1456(3) 1.0681(3) 0.1234(3) 0.0298(9) Uani 1 1 d . . . C6D C 0.2285(3) 1.1272(3) 0.1081(3) 0.0303(9) Uani 1 1 d . . . C7D C 0.0202(4) 1.0388(4) 0.2110(3) 0.0407(11) Uani 1 1 d . . . H7D1 H 0.0611 1.0241 0.2674 0.096(5) Uiso 1 1 calc R . . H7D2 H -0.0193 0.9752 0.1570 0.096(5) Uiso 1 1 calc R . . H7D3 H -0.0367 1.0751 0.2195 0.096(5) Uiso 1 1 calc R . . C8D C 0.3083(4) 1.3823(3) 0.3137(3) 0.0334(10) Uani 1 1 d . . . H8D1 H 0.2545 1.4138 0.3351 0.065(5) Uiso 1 1 calc R . . H8D2 H 0.3365 1.4240 0.2837 0.065(5) Uiso 1 1 calc R . . C9D C 0.0801(4) 1.3104(4) 0.4731(4) 0.0551(15) Uani 1 1 d . . . H9D1 H 0.0048 1.2604 0.4375 0.096(5) Uiso 1 1 calc R . . H9D2 H 0.0718 1.3753 0.4659 0.096(5) Uiso 1 1 calc R . . H9D3 H 0.1088 1.3191 0.5395 0.096(5) Uiso 1 1 calc R . . C1S C 0.8617(9) 0.5347(7) 0.2600(7) 0.112(3) Uani 1 1 d . . . H1S1 H 0.9205 0.6008 0.2947 0.065(5) Uiso 1 1 calc R . . H1S2 H 0.8150 0.5334 0.1962 0.065(5) Uiso 1 1 calc R . . C2S C 0.9226(7) 0.4531(7) 0.2514(8) 0.107(3) Uani 1 1 d . . . O1S O 0.7929(6) 0.5302(6) 0.3023(5) 0.150(3) Uani 1 1 d . . . F1S F 0.8581(5) 0.3590(4) 0.2049(5) 0.166(2) Uani 1 1 d . . . F2S F 0.9942(7) 0.4580(7) 0.3381(6) 0.245(4) Uani 1 1 d . . . F3S F 0.9986(6) 0.4649(5) 0.2173(5) 0.1719(18) Uani 1 1 d . . . C3S C 0.3497(6) 0.4789(5) 0.0169(5) 0.079(2) Uani 1 1 d . . . H3S1 H 0.3458 0.5126 -0.0287 0.065(5) Uiso 1 1 calc R . . H3S2 H 0.4140 0.5224 0.0780 0.065(5) Uiso 1 1 calc R . . C4S C 0.2370(7) 0.4687(6) 0.0269(6) 0.081(2) Uani 1 1 d . . . O2S O 0.3731(5) 0.3841(4) -0.0136(4) 0.1043(18) Uani 1 1 d . . . F4S F 0.1449(4) 0.4063(4) -0.0546(4) 0.1234(18) Uani 1 1 d . . . F5S F 0.2384(5) 0.4310(4) 0.0919(4) 0.1191(17) Uani 1 1 d . . . F6S F 0.2113(4) 0.5608(4) 0.0486(4) 0.1182(17) Uani 1 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 Ca1 0.0534(10) 0.0324(8) 0.1069(15) 0.0093(9) 0.0450(10) 0.0017(7) Cl1 0.0583(8) 0.0632(9) 0.0690(10) 0.0316(8) 0.0280(7) 0.0178(7) O1W 0.072(3) 0.067(3) 0.095(3) 0.032(2) 0.042(3) 0.024(2) P1A 0.0317(6) 0.0314(6) 0.0375(7) 0.0153(5) 0.0140(5) 0.0095(5) O1A 0.0303(15) 0.0260(15) 0.0300(16) 0.0097(12) 0.0101(12) 0.0097(12) O2A 0.0265(15) 0.0347(16) 0.0321(17) 0.0107(13) 0.0101(13) 0.0082(12) O3A 0.0422(18) 0.0294(17) 0.059(2) 0.0129(15) 0.0239(16) 0.0072(14) C1A 0.034(2) 0.0172(19) 0.028(2) 0.0029(16) 0.0125(18) 0.0047(16) C2A 0.027(2) 0.0146(18) 0.031(2) 0.0044(16) 0.0103(17) 0.0050(15) C3A 0.026(2) 0.022(2) 0.027(2) 0.0060(17) 0.0085(17) 0.0076(16) C4A 0.030(2) 0.020(2) 0.031(2) 0.0031(17) 0.0110(18) 0.0033(16) C5A 0.026(2) 0.019(2) 0.035(2) 0.0006(17) 0.0127(18) 0.0028(16) C6A 0.027(2) 0.0169(19) 0.032(2) 0.0040(17) 0.0089(18) 0.0042(16) C7A 0.039(2) 0.039(3) 0.035(3) 0.011(2) 0.018(2) 0.006(2) C8A 0.026(2) 0.027(2) 0.029(2) 0.0085(18) 0.0092(17) 0.0021(16) C9A 0.056(3) 0.062(3) 0.045(3) 0.031(3) 0.022(3) 0.022(3) P1B 0.0415(7) 0.0361(7) 0.0515(9) 0.0089(6) 0.0089(6) 0.0133(6) O1B 0.0292(16) 0.0351(17) 0.050(2) 0.0010(15) 0.0119(15) 0.0136(13) O2B 0.0370(17) 0.0378(18) 0.0420(19) 0.0035(15) 0.0144(15) 0.0155(14) O3B 0.063(2) 0.054(2) 0.053(2) 0.0225(19) 0.007(2) -0.0028(19) C1B 0.023(2) 0.034(2) 0.033(2) 0.0109(19) 0.0116(18) 0.0032(17) C2B 0.024(2) 0.034(2) 0.037(2) 0.0056(19) 0.0151(19) 0.0031(17) C3B 0.022(2) 0.029(2) 0.043(3) 0.003(2) 0.0133(19) 0.0065(17) C4B 0.022(2) 0.032(2) 0.044(3) 0.011(2) 0.0124(19) 0.0075(17) C5B 0.0172(18) 0.031(2) 0.032(2) 0.0063(18) 0.0076(17) 0.0024(16) C6B 0.0198(18) 0.024(2) 0.033(2) 0.0074(17) 0.0096(17) 0.0039(15) C7B 0.038(3) 0.041(3) 0.048(3) 0.012(2) 0.010(2) 0.016(2) C8B 0.029(2) 0.041(3) 0.040(3) 0.005(2) 0.018(2) 0.0048(19) C9B 0.071(4) 0.050(4) 0.090(5) -0.010(3) -0.010(4) 0.034(3) P1C 0.0269(5) 0.0272(6) 0.0319(6) 0.0083(5) 0.0065(5) 0.0042(4) O1C 0.0288(15) 0.0306(16) 0.0270(16) 0.0031(13) 0.0062(12) 0.0029(12) O2C 0.0242(14) 0.0252(15) 0.0321(16) 0.0045(12) 0.0021(12) 0.0026(12) O3C 0.0370(17) 0.0428(18) 0.0327(17) 0.0164(14) 0.0107(14) 0.0117(14) C1C 0.040(2) 0.029(2) 0.028(2) 0.0049(18) 0.017(2) 0.0047(19) C2C 0.037(2) 0.030(2) 0.019(2) 0.0053(17) 0.0121(18) 0.0084(18) C3C 0.031(2) 0.034(2) 0.022(2) 0.0047(18) 0.0090(18) 0.0034(18) C4C 0.038(2) 0.031(2) 0.029(2) 0.0058(19) 0.0141(19) 0.0081(19) C5C 0.033(2) 0.037(2) 0.031(2) 0.0067(19) 0.0132(19) 0.0122(19) C6C 0.030(2) 0.035(2) 0.024(2) 0.0042(18) 0.0112(18) 0.0032(18) C7C 0.041(3) 0.034(3) 0.043(3) 0.006(2) 0.013(2) 0.006(2) C8C 0.037(2) 0.032(2) 0.025(2) 0.0095(18) 0.0090(18) 0.0068(18) C9C 0.035(2) 0.030(2) 0.056(3) 0.007(2) 0.011(2) 0.002(2) P1D 0.0300(6) 0.0318(6) 0.0404(7) 0.0051(5) 0.0138(5) 0.0022(5) O1D 0.0291(15) 0.0349(17) 0.0365(18) 0.0040(13) 0.0129(13) 0.0087(13) O2D 0.0260(15) 0.0301(16) 0.0386(18) 0.0021(13) 0.0139(13) 0.0039(12) O3D 0.051(2) 0.0391(19) 0.050(2) 0.0138(16) 0.0105(17) 0.0019(16) C1D 0.029(2) 0.028(2) 0.033(2) 0.0134(18) 0.0095(18) 0.0073(17) C2D 0.023(2) 0.028(2) 0.028(2) 0.0074(18) 0.0022(17) 0.0069(17) C3D 0.022(2) 0.033(2) 0.029(2) 0.0078(18) 0.0050(17) 0.0076(17) C4D 0.0179(19) 0.031(2) 0.036(2) 0.0077(19) 0.0039(17) 0.0022(16) C5D 0.024(2) 0.024(2) 0.026(2) 0.0048(17) -0.0015(17) 0.0041(16) C6D 0.028(2) 0.031(2) 0.027(2) 0.0116(18) 0.0051(17) 0.0081(17) C7D 0.026(2) 0.038(3) 0.044(3) 0.005(2) 0.011(2) -0.0003(19) C8D 0.033(2) 0.025(2) 0.036(2) 0.0080(19) 0.0100(19) 0.0091(18) C9D 0.034(3) 0.065(4) 0.050(3) 0.000(3) 0.022(2) -0.004(2) C1S 0.106(7) 0.108(7) 0.105(7) 0.016(6) 0.052(6) 0.000(6) C2S 0.046(4) 0.090(6) 0.161(9) 0.055(6) 0.019(5) -0.005(4) O1S 0.110(5) 0.162(7) 0.110(5) -0.030(4) 0.050(4) -0.017(4) F1S 0.115(4) 0.102(4) 0.208 -0.017(4) 0.065(4) -0.030(3) F2S 0.165(6) 0.239 0.210 0.116(4) -0.058(6) 0.012(6) F3S 0.128(5) 0.160 0.205 0.007(5) 0.103(4) 0.002(4) C3S 0.080(5) 0.065(4) 0.079(5) 0.029(4) 0.019(4) 0.018(4) C4S 0.089(5) 0.070(5) 0.081(5) 0.048(4) 0.021(4) 0.012(4) O2S 0.130(5) 0.075(3) 0.075(3) 0.006(3) 0.022(3) 0.037(3) F4S 0.086(3) 0.131(4) 0.109(4) 0.050(3) 0.004(3) -0.012(3) F5S 0.135(4) 0.134(4) 0.120(4) 0.083(3) 0.059(3) 0.034(3) F6S 0.116(4) 0.097(3) 0.178(5) 0.072(3) 0.076(4) 0.056(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 Ca1 O1W 2.309(4) . ? Ca1 O1W 2.309(4) 2_676 ? Ca1 O2W 2.356(8) 2_676 ? Ca1 O2W 2.356(8) . ? Ca1 O3A 2.385(3) 2_676 ? Ca1 O3A 2.385(3) . ? P1A O3A 1.472(3) . ? P1A O1A 1.591(3) . ? P1A O2A 1.595(3) . ? P1A C9A 1.759(5) . ? O1A C3A 1.427(5) . ? O2A C5B 1.409(5) . ? C1A C2A 1.390(6) . ? C1A C6A 1.393(6) . ? C1A H1A 0.9300 . ? C2A C3A 1.388(6) . ? C2A C8A 1.516(5) . ? C3A C4A 1.395(6) . ? C4A C5A 1.399(6) . ? C4A C7A 1.502(6) . ? C5A C6A 1.394(6) . ? C5A O2D 1.423(5) . ? C6A C8D 1.519(6) . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C8A C6B 1.523(5) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? P1B O3B 1.444(4) . ? P1B O2B 1.582(4) . ? P1B O1B 1.590(3) . ? P1B C9B 1.773(6) . ? O1B C3B 1.419(5) . ? O2B C5C 1.415(5) . ? C1B C6B 1.382(6) . ? C1B C2B 1.393(6) . ? C1B H1B 0.9300 . ? C2B C3B 1.392(6) . ? C2B C8B 1.506(6) . ? C3B C4B 1.404(6) . ? C4B C5B 1.394(6) . ? C4B C7B 1.507(6) . ? C5B C6B 1.399(6) . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? C8B C6C 1.526(6) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? P1C O3C 1.476(3) . ? P1C O2C 1.591(3) . ? P1C O1C 1.591(3) . ? P1C C9C 1.768(4) . ? O1C C3C 1.420(5) . ? O2C C5D 1.426(5) . ? C1C C6C 1.383(6) . ? C1C C2C 1.391(6) . ? C1C H1C 0.9300 . ? C2C C3C 1.396(6) . ? C2C C8C 1.509(6) . ? C3C C4C 1.389(6) . ? C4C C5C 1.399(6) . ? C4C C7C 1.516(6) . ? C5C C6C 1.395(6) . ? C7C H7C1 0.9600 . ? C7C H7C2 0.9600 . ? C7C H7C3 0.9600 . ? C8C C6D 1.510(6) . ? C8C H8C1 0.9700 . ? C8C H8C2 0.9700 . ? C9C H9C1 0.9600 . ? C9C H9C2 0.9600 . ? C9C H9C3 0.9600 . ? P1D O3D 1.465(4) . ? P1D O1D 1.589(3) . ? P1D O2D 1.592(3) . ? P1D C9D 1.766(5) . ? O1D C3D 1.418(5) . ? C1D C2D 1.384(6) . ? C1D C6D 1.401(6) . ? C1D H1D 0.9300 . ? C2D C3D 1.386(6) . ? C2D C8D 1.514(6) . ? C3D C4D 1.400(6) . ? C4D C5D 1.383(6) . ? C4D C7D 1.521(6) . ? C5D C6D 1.393(6) . ? C7D H7D1 0.9600 . ? C7D H7D2 0.9600 . ? C7D H7D3 0.9600 . ? C8D H8D1 0.9700 . ? C8D H8D2 0.9700 . ? C9D H9D1 0.9600 . ? C9D H9D2 0.9600 . ? C9D H9D3 0.9600 . ? C1S O1S 1.299(9) . ? C1S C2S 1.457(12) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S F3S 1.292(10) . ? C2S F1S 1.292(9) . ? C2S F2S 1.329(11) . ? C3S O2S 1.385(8) . ? C3S C4S 1.490(10) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S F5S 1.298(7) . ? C4S F4S 1.340(8) . ? C4S F6S 1.347(8) . ? 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 O1W Ca1 O1W 180.000(1) . 2_676 ? O1W Ca1 O2W 81.3(2) . 2_676 ? O1W Ca1 O2W 98.7(2) 2_676 2_676 ? O1W Ca1 O2W 98.7(2) . . ? O1W Ca1 O2W 81.3(2) 2_676 . ? O2W Ca1 O2W 180.000(2) 2_676 . ? O1W Ca1 O3A 90.37(13) . 2_676 ? O1W Ca1 O3A 89.63(13) 2_676 2_676 ? O2W Ca1 O3A 94.1(2) 2_676 2_676 ? O2W Ca1 O3A 85.9(2) . 2_676 ? O1W Ca1 O3A 89.63(13) . . ? O1W Ca1 O3A 90.37(13) 2_676 . ? O2W Ca1 O3A 85.9(2) 2_676 . ? O2W Ca1 O3A 94.1(2) . . ? O3A Ca1 O3A 180.000(1) 2_676 . ? O3A P1A O1A 113.76(17) . . ? O3A P1A O2A 112.17(17) . . ? O1A P1A O2A 106.50(16) . . ? O3A P1A C9A 118.4(2) . . ? O1A P1A C9A 102.3(2) . . ? O2A P1A C9A 102.3(2) . . ? C3A O1A P1A 121.7(2) . . ? C5B O2A P1A 121.0(2) . . ? P1A O3A Ca1 169.6(2) . . ? C2A C1A C6A 122.1(4) . . ? C2A C1A H1A 118.9 . . ? C6A C1A H1A 118.9 . . ? C1A C2A C3A 117.0(4) . . ? C1A C2A C8A 120.7(4) . . ? C3A C2A C8A 122.2(4) . . ? C2A C3A C4A 124.9(4) . . ? C2A C3A O1A 118.4(3) . . ? C4A C3A O1A 116.6(3) . . ? C3A C4A C5A 114.5(4) . . ? C3A C4A C7A 122.9(4) . . ? C5A C4A C7A 122.6(4) . . ? C6A C5A C4A 124.2(4) . . ? C6A C5A O2D 118.2(4) . . ? C4A C5A O2D 117.4(4) . . ? C1A C6A C5A 117.3(4) . . ? C1A C6A C8D 120.7(4) . . ? C5A C6A C8D 122.0(4) . . ? C4A C7A H7A1 109.5 . . ? C4A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C4A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C2A C8A C6B 112.3(3) . . ? C2A C8A H8A1 109.1 . . ? C6B C8A H8A1 109.1 . . ? C2A C8A H8A2 109.1 . . ? C6B C8A H8A2 109.1 . . ? H8A1 C8A H8A2 107.9 . . ? P1A C9A H9A1 109.5 . . ? P1A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? P1A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? O3B P1B O2B 113.0(2) . . ? O3B P1B O1B 112.6(2) . . ? O2B P1B O1B 107.69(19) . . ? O3B P1B C9B 118.9(3) . . ? O2B P1B C9B 101.7(3) . . ? O1B P1B C9B 101.7(3) . . ? C3B O1B P1B 122.3(3) . . ? C5C O2B P1B 121.1(3) . . ? C6B C1B C2B 122.2(4) . . ? C6B C1B H1B 118.9 . . ? C2B C1B H1B 118.9 . . ? C1B C2B C3B 117.8(4) . . ? C1B C2B C8B 119.7(4) . . ? C3B C2B C8B 122.4(4) . . ? C2B C3B C4B 123.0(4) . . ? C2B C3B O1B 119.2(4) . . ? C4B C3B O1B 117.8(4) . . ? C5B C4B C3B 116.0(4) . . ? C5B C4B C7B 121.6(4) . . ? C3B C4B C7B 122.4(4) . . ? C6B C5B C4B 123.3(4) . . ? C6B C5B O2A 118.9(4) . . ? C4B C5B O2A 117.7(4) . . ? C1B C6B C5B 117.7(4) . . ? C1B C6B C8A 120.5(4) . . ? C5B C6B C8A 121.8(4) . . ? C4B C7B H7B1 109.5 . . ? C4B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C4B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C2B C8B C6C 110.3(3) . . ? C2B C8B H8B1 109.6 . . ? C6C C8B H8B1 109.6 . . ? C2B C8B H8B2 109.6 . . ? C6C C8B H8B2 109.6 . . ? H8B1 C8B H8B2 108.1 . . ? P1B C9B H9B1 109.5 . . ? P1B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? P1B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? O3C P1C O2C 112.99(17) . . ? O3C P1C O1C 113.23(17) . . ? O2C P1C O1C 106.55(16) . . ? O3C P1C C9C 118.9(2) . . ? O2C P1C C9C 101.54(19) . . ? O1C P1C C9C 102.2(2) . . ? C3C O1C P1C 119.8(2) . . ? C5D O2C P1C 121.6(2) . . ? C6C C1C C2C 122.7(4) . . ? C6C C1C H1C 118.7 . . ? C2C C1C H1C 118.7 . . ? C1C C2C C3C 116.6(4) . . ? C1C C2C C8C 121.8(4) . . ? C3C C2C C8C 121.5(4) . . ? C4C C3C C2C 124.2(4) . . ? C4C C3C O1C 116.9(4) . . ? C2C C3C O1C 118.8(4) . . ? C3C C4C C5C 115.7(4) . . ? C3C C4C C7C 122.7(4) . . ? C5C C4C C7C 121.6(4) . . ? C4C C5C C6C 123.1(4) . . ? C4C C5C O2B 118.4(4) . . ? C6C C5C O2B 118.3(4) . . ? C1C C6C C5C 117.7(4) . . ? C1C C6C C8B 121.1(4) . . ? C5C C6C C8B 121.1(4) . . ? C4C C7C H7C1 109.5 . . ? C4C C7C H7C2 109.5 . . ? H7C1 C7C H7C2 109.5 . . ? C4C C7C H7C3 109.5 . . ? H7C1 C7C H7C3 109.5 . . ? H7C2 C7C H7C3 109.5 . . ? C6D C8C C2C 112.9(3) . . ? C6D C8C H8C1 109.0 . . ? C2C C8C H8C1 109.0 . . ? C6D C8C H8C2 109.0 . . ? C2C C8C H8C2 109.0 . . ? H8C1 C8C H8C2 107.8 . . ? P1C C9C H9C1 109.5 . . ? P1C C9C H9C2 109.5 . . ? H9C1 C9C H9C2 109.5 . . ? P1C C9C H9C3 109.5 . . ? H9C1 C9C H9C3 109.5 . . ? H9C2 C9C H9C3 109.5 . . ? O3D P1D O1D 112.14(18) . . ? O3D P1D O2D 113.98(18) . . ? O1D P1D O2D 107.38(17) . . ? O3D P1D C9D 117.9(3) . . ? O1D P1D C9D 102.4(2) . . ? O2D P1D C9D 101.8(2) . . ? C3D O1D P1D 123.9(3) . . ? C5A O2D P1D 122.5(2) . . ? C2D C1D C6D 122.5(4) . . ? C2D C1D H1D 118.8 . . ? C6D C1D H1D 118.8 . . ? C1D C2D C3D 117.5(4) . . ? C1D C2D C8D 120.5(4) . . ? C3D C2D C8D 121.7(4) . . ? C2D C3D C4D 123.5(4) . . ? C2D C3D O1D 118.7(4) . . ? C4D C3D O1D 117.7(4) . . ? C5D C4D C3D 115.7(4) . . ? C5D C4D C7D 123.5(4) . . ? C3D C4D C7D 120.8(4) . . ? C4D C5D C6D 124.3(4) . . ? C4D C5D O2C 117.3(4) . . ? C6D C5D O2C 118.3(4) . . ? C5D C6D C1D 116.5(4) . . ? C5D C6D C8C 122.7(4) . . ? C1D C6D C8C 120.8(4) . . ? C4D C7D H7D1 109.5 . . ? C4D C7D H7D2 109.5 . . ? H7D1 C7D H7D2 109.5 . . ? C4D C7D H7D3 109.5 . . ? H7D1 C7D H7D3 109.5 . . ? H7D2 C7D H7D3 109.5 . . ? C2D C8D C6A 109.8(3) . . ? C2D C8D H8D1 109.7 . . ? C6A C8D H8D1 109.7 . . ? C2D C8D H8D2 109.7 . . ? C6A C8D H8D2 109.7 . . ? H8D1 C8D H8D2 108.2 . . ? P1D C9D H9D1 109.5 . . ? P1D C9D H9D2 109.5 . . ? H9D1 C9D H9D2 109.5 . . ? P1D C9D H9D3 109.5 . . ? H9D1 C9D H9D3 109.5 . . ? H9D2 C9D H9D3 109.5 . . ? O1S C1S C2S 116.1(9) . . ? O1S C1S H1S1 108.2 . . ? C2S C1S H1S1 108.2 . . ? O1S C1S H1S2 108.2 . . ? C2S C1S H1S2 108.2 . . ? H1S1 C1S H1S2 107.4 . . ? F3S C2S F1S 106.8(10) . . ? F3S C2S F2S 99.6(7) . . ? F1S C2S F2S 107.1(8) . . ? F3S C2S C1S 114.8(8) . . ? F1S C2S C1S 117.2(7) . . ? F2S C2S C1S 109.6(10) . . ? O2S C3S C4S 112.3(6) . . ? O2S C3S H3S1 109.1 . . ? C4S C3S H3S1 109.1 . . ? O2S C3S H3S2 109.1 . . ? C4S C3S H3S2 109.1 . . ? H3S1 C3S H3S2 107.9 . . ? F5S C4S F4S 106.4(6) . . ? F5S C4S F6S 108.2(7) . . ? F4S C4S F6S 105.7(6) . . ? F5S C4S C3S 112.9(6) . . ? F4S C4S C3S 112.2(7) . . ? F6S C4S C3S 111.1(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.383 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.096 #Data for compound 3 data_tpozn _database_code_depnum_ccdc_archive 'CCDC 767371' #TrackingRef 'total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H109 Cl4 F15 O40 P8 Zn2' _chemical_formula_weight 2539.99 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' 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' Zn Zn 0.2839 1.4301 '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 12.7839(7) _cell_length_b 18.1535(10) _cell_length_c 26.2766(14) _cell_angle_alpha 78.8100(10) _cell_angle_beta 83.7300(10) _cell_angle_gamma 70.8910(10) _cell_volume 5645.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3691 _cell_measurement_theta_min 0.79 _cell_measurement_theta_max 28.00 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794958 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Bruker AXS SADABS' _exptl_special_details ; The calculated molar mass, density and absorption coefficient include six disordered trifluoroethanol molecules per cell which do not appear in the final files because of the refinements carried out with data subjected to SQUEEZE. See "_refine_special_details" below. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER AXS SMART 1000' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean '8.192 pixels/mm' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 71418 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 28.00 _reflns_number_total 26852 _reflns_number_gt 17102 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement ? _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SIR97 (Giacovazzo et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In view of the presence of disordered trifluoroethanol molecules which were found in the difference Fourier's map but which could not be properly modelled, the structure was subjected to SQUEEZE (P. v.d. Sluis and A. L. Spek, Acta Crystallogr., Sect A 1990, 46, 194-201). The program calculated a void volume of 1274.5 A^3^ and 330 electrons per unit cell, which corresponds roughly to six trifluoroethanol molecules per unit cell. ; _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^)+(0.0857P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26852 _refine_ls_number_parameters 1209 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.49565(3) 0.24776(2) 0.747886(13) 0.03363(9) Uani 1 1 d . . . O1W O 0.43594(19) 0.22928(16) 0.68376(9) 0.0505(6) Uani 1 1 d . . . O2W O 0.5591(2) 0.26842(15) 0.81198(10) 0.0604(7) Uani 1 1 d . . . O3W O 0.65795(17) 0.21501(13) 0.71182(8) 0.0425(5) Uani 1 1 d . . . O4W O 0.33834(19) 0.28242(14) 0.78515(8) 0.0462(5) Uani 1 1 d . . . O5W O 0.5214(2) 0.13025(14) 0.78528(9) 0.0522(6) Uani 1 1 d . . . O6W O 0.4752(2) 0.36443(13) 0.70883(9) 0.0512(6) Uani 1 1 d . . . Zn2 Zn 0.26473(4) 0.81588(2) 0.823857(14) 0.04762(12) Uani 1 1 d . . . Cl1 Cl 0.20074(9) 0.75569(6) 0.89739(4) 0.0688(3) Uani 1 1 d . . . Cl2 Cl 0.40610(8) 0.72706(5) 0.78623(4) 0.0600(3) Uani 1 1 d . . . Cl3 Cl 0.12238(9) 0.86648(9) 0.76814(4) 0.0967(5) Uani 1 1 d . . . Cl4 Cl 0.32599(15) 0.91228(7) 0.83836(5) 0.0994(5) Uani 1 1 d . . . P1A P -0.06572(6) 0.31984(4) 0.66690(3) 0.02926(16) Uani 1 1 d . . . O1A O -0.07887(15) 0.25129(11) 0.64065(7) 0.0308(4) Uani 1 1 d . . . O2A O -0.09217(15) 0.39745(11) 0.62365(8) 0.0329(4) Uani 1 1 d . . . O3A O 0.04446(15) 0.29873(12) 0.68791(7) 0.0338(4) Uani 1 1 d . . . P1B P 0.29391(6) 0.51159(4) 0.58966(3) 0.03003(16) Uani 1 1 d . . . O1B O 0.17351(16) 0.53619(11) 0.56745(8) 0.0332(4) Uani 1 1 d . . . O2B O 0.38125(16) 0.49300(11) 0.54203(7) 0.0318(4) Uani 1 1 d . . . O3B O 0.31266(17) 0.44689(12) 0.63418(8) 0.0367(5) Uani 1 1 d . . . P1C P 0.68423(6) 0.16811(4) 0.56843(3) 0.02982(16) Uani 1 1 d . . . O1C O 0.66510(15) 0.24699(11) 0.52626(8) 0.0317(4) Uani 1 1 d . . . O2C O 0.66718(15) 0.10396(11) 0.54010(8) 0.0306(4) Uani 1 1 d . . . O3C O 0.61425(18) 0.18033(13) 0.61632(8) 0.0403(5) Uani 1 1 d . . . P1D P 0.32085(6) -0.02159(4) 0.64444(3) 0.03173(17) Uani 1 1 d . . . O1D O 0.40331(15) -0.03473(11) 0.59506(7) 0.0313(4) Uani 1 1 d . . . O2D O 0.19950(15) 0.00344(11) 0.62395(7) 0.0311(4) Uani 1 1 d . . . O3D O 0.33514(17) 0.03665(13) 0.67257(8) 0.0401(5) Uani 1 1 d . . . P1E P 0.29922(6) 0.36021(5) 0.91856(3) 0.03290(17) Uani 1 1 d . . . O1E O 0.30903(16) 0.28402(12) 0.96158(8) 0.0361(5) Uani 1 1 d . . . O2E O 0.32402(15) 0.42315(12) 0.94573(8) 0.0329(4) Uani 1 1 d . . . O3E O 0.36905(18) 0.34309(13) 0.87151(8) 0.0419(5) Uani 1 1 d . . . P1F P 0.70758(7) 0.51330(5) 0.84800(3) 0.03528(18) Uani 1 1 d . . . O1F O 0.61884(17) 0.53513(11) 0.89410(8) 0.0363(5) Uani 1 1 d . . . O2F O 0.82613(17) 0.47973(12) 0.87182(8) 0.0368(5) Uani 1 1 d . . . O3F O 0.68795(18) 0.45719(12) 0.81921(8) 0.0405(5) Uani 1 1 d . . . P1G P 1.06190(6) 0.15197(6) 0.84229(3) 0.0404(2) Uani 1 1 d . . . O1G O 1.08122(16) 0.22009(14) 0.86700(8) 0.0409(5) Uani 1 1 d . . . O2G O 1.07486(16) 0.07758(13) 0.88792(8) 0.0413(5) Uani 1 1 d . . . O3G O 0.95436(17) 0.17752(14) 0.81795(8) 0.0426(5) Uani 1 1 d . . . P1H P 0.66448(7) 0.00038(5) 0.90960(3) 0.03511(18) Uani 1 1 d . . . O1H O 0.77939(18) -0.03498(12) 0.93735(8) 0.0398(5) Uani 1 1 d . . . O2H O 0.56984(18) 0.02648(12) 0.95310(8) 0.0379(5) Uani 1 1 d . . . O3H O 0.66430(17) 0.06409(12) 0.86564(8) 0.0389(5) Uani 1 1 d . . . C1A C 0.1041(2) 0.18673(16) 0.52997(10) 0.0277(6) Uani 1 1 d . . . H1A H 0.1171 0.2061 0.4952 0.038(3) Uiso 1 1 calc R . . C2A C 0.0253(2) 0.23522(16) 0.55921(11) 0.0275(6) Uani 1 1 d . . . C3A C 0.0083(2) 0.20529(16) 0.61107(10) 0.0267(6) Uani 1 1 d . . . C4A C 0.0643(2) 0.12876(17) 0.63433(10) 0.0275(6) Uani 1 1 d . . . C5A C 0.1433(2) 0.08281(16) 0.60251(11) 0.0276(6) Uani 1 1 d . . . C6A C 0.1651(2) 0.10940(16) 0.55057(11) 0.0270(6) Uani 1 1 d . . . C7A C 0.0375(3) 0.09721(18) 0.69010(11) 0.0380(7) Uani 1 1 d . . . H7A1 H 0.0313 0.1360 0.7114 0.091(2) Uiso 1 1 calc R . . H7A2 H 0.0956 0.0496 0.7020 0.091(2) Uiso 1 1 calc R . . H7A3 H -0.0313 0.0860 0.6923 0.091(2) Uiso 1 1 calc R . . C8A C -0.0384(2) 0.31898(17) 0.53497(11) 0.0324(6) Uani 1 1 d . . . H8A1 H -0.0420 0.3215 0.4980 0.051(2) Uiso 1 1 calc R . . H8A2 H -0.1136 0.3330 0.5500 0.051(2) Uiso 1 1 calc R . . C9A C -0.1843(3) 0.3397(2) 0.71006(13) 0.0419(8) Uani 1 1 d . . . H9A1 H -0.1763 0.2959 0.7381 0.091(2) Uiso 1 1 calc R . . H9A2 H -0.2491 0.3473 0.6918 0.091(2) Uiso 1 1 calc R . . H9A3 H -0.1919 0.3867 0.7237 0.091(2) Uiso 1 1 calc R . . C1B C 0.0966(2) 0.39589(16) 0.50806(10) 0.0299(6) Uani 1 1 d . . . H1B H 0.1142 0.3731 0.4782 0.038(3) Uiso 1 1 calc R . . C2B C 0.1516(2) 0.44700(16) 0.51561(11) 0.0296(6) Uani 1 1 d . . . C3B C 0.1231(2) 0.47998(16) 0.56048(11) 0.0298(6) Uani 1 1 d . . . C4B C 0.0415(2) 0.46637(16) 0.59689(11) 0.0311(6) Uani 1 1 d . . . C5B C -0.0079(2) 0.41309(16) 0.58781(11) 0.0298(6) Uani 1 1 d . . . C6B C 0.0159(2) 0.37736(16) 0.54365(11) 0.0296(6) Uani 1 1 d . . . C7B C 0.0038(3) 0.51083(19) 0.64203(12) 0.0405(7) Uani 1 1 d . . . H7B1 H -0.0748 0.5366 0.6415 0.091(2) Uiso 1 1 calc R . . H7B2 H 0.0411 0.5497 0.6392 0.091(2) Uiso 1 1 calc R . . H7B3 H 0.0213 0.4744 0.6740 0.091(2) Uiso 1 1 calc R . . C8B C 0.2387(2) 0.46502(17) 0.47636(10) 0.0311(6) Uani 1 1 d . . . H8B1 H 0.2384 0.5187 0.4759 0.051(2) Uiso 1 1 calc R . . H8B2 H 0.2214 0.4614 0.4421 0.051(2) Uiso 1 1 calc R . . C9B C 0.3008(3) 0.60410(18) 0.59786(14) 0.0430(8) Uani 1 1 d . . . H9B1 H 0.2490 0.6231 0.6253 0.091(2) Uiso 1 1 calc R . . H9B2 H 0.2827 0.6411 0.5662 0.091(2) Uiso 1 1 calc R . . H9B3 H 0.3744 0.5983 0.6065 0.091(2) Uiso 1 1 calc R . . C1C C 0.3944(2) 0.33798(17) 0.46827(10) 0.0295(6) Uani 1 1 d . . . H1C H 0.3516 0.3281 0.4455 0.038(3) Uiso 1 1 calc R . . C2C C 0.4964(2) 0.28333(16) 0.48032(10) 0.0269(6) Uani 1 1 d . . . C3C C 0.5578(2) 0.29922(16) 0.51513(10) 0.0276(6) Uani 1 1 d . . . C4C C 0.5215(2) 0.36808(16) 0.53732(11) 0.0296(6) Uani 1 1 d . . . C5C C 0.4180(2) 0.42040(16) 0.52359(10) 0.0277(6) Uani 1 1 d . . . C6C C 0.3534(2) 0.40767(16) 0.48920(10) 0.0287(6) Uani 1 1 d . . . C7C C 0.5915(2) 0.38368(18) 0.57428(12) 0.0366(7) Uani 1 1 d . . . H7C1 H 0.5707 0.4395 0.5743 0.091(2) Uiso 1 1 calc R . . H7C2 H 0.6683 0.3644 0.5634 0.091(2) Uiso 1 1 calc R . . H7C3 H 0.5799 0.3570 0.6087 0.091(2) Uiso 1 1 calc R . . C8C C 0.5351(2) 0.20704(16) 0.45816(11) 0.0300(6) Uani 1 1 d . . . H8C1 H 0.5042 0.2161 0.4245 0.051(2) Uiso 1 1 calc R . . H8C2 H 0.6153 0.1899 0.4533 0.051(2) Uiso 1 1 calc R . . C9C C 0.8280(3) 0.1350(2) 0.57507(16) 0.0522(9) Uani 1 1 d . . . H9C1 H 0.8478 0.1697 0.5928 0.091(2) Uiso 1 1 calc R . . H9C2 H 0.8653 0.1348 0.5413 0.091(2) Uiso 1 1 calc R . . H9C3 H 0.8497 0.0824 0.5947 0.091(2) Uiso 1 1 calc R . . C1D C 0.4001(2) 0.12984(16) 0.48922(11) 0.0278(6) Uani 1 1 d . . . H1D H 0.3554 0.1608 0.4624 0.038(3) Uiso 1 1 calc R . . C2D C 0.3654(2) 0.07213(16) 0.52263(10) 0.0274(6) Uani 1 1 d . . . C3D C 0.4331(2) 0.02809(15) 0.56257(11) 0.0275(6) Uani 1 1 d . . . C4D C 0.5330(2) 0.03815(16) 0.57106(11) 0.0288(6) Uani 1 1 d . . . C5D C 0.5621(2) 0.09590(16) 0.53593(11) 0.0271(6) Uani 1 1 d . . . C6D C 0.4990(2) 0.14300(15) 0.49440(10) 0.0262(6) Uani 1 1 d . . . C7D C 0.6046(2) -0.01159(18) 0.61435(12) 0.0371(7) Uani 1 1 d . . . H7D1 H 0.6808 -0.0165 0.6043 0.091(2) Uiso 1 1 calc R . . H7D2 H 0.5956 -0.0631 0.6217 0.091(2) Uiso 1 1 calc R . . H7D3 H 0.5834 0.0129 0.6448 0.091(2) Uiso 1 1 calc R . . C8D C 0.2547(2) 0.06035(17) 0.51728(11) 0.0294(6) Uani 1 1 d . . . H8D1 H 0.2352 0.0758 0.4812 0.051(2) Uiso 1 1 calc R . . H8D2 H 0.2609 0.0049 0.5279 0.051(2) Uiso 1 1 calc R . . C9D C 0.3421(3) -0.1192(2) 0.67654(15) 0.0545(10) Uani 1 1 d . . . H9D1 H 0.4160 -0.1408 0.6886 0.091(2) Uiso 1 1 calc R . . H9D2 H 0.3323 -0.1504 0.6530 0.091(2) Uiso 1 1 calc R . . H9D3 H 0.2897 -0.1196 0.7056 0.091(2) Uiso 1 1 calc R . . C1E C 0.5693(2) 0.17889(17) 1.02689(11) 0.0322(6) Uani 1 1 d . . . H1E H 0.6120 0.1863 1.0508 0.038(3) Uiso 1 1 calc R . . C2E C 0.4726(2) 0.23913(17) 1.01135(10) 0.0307(6) Uani 1 1 d . . . C3E C 0.4121(2) 0.22611(17) 0.97529(11) 0.0321(6) Uani 1 1 d . . . C4E C 0.4420(2) 0.15719(18) 0.95413(11) 0.0340(6) Uani 1 1 d . . . C5E C 0.5395(2) 0.09946(17) 0.97103(11) 0.0334(6) Uani 1 1 d . . . C6E C 0.6038(2) 0.10795(17) 1.00777(11) 0.0329(6) Uani 1 1 d . . . C7E C 0.3732(3) 0.14601(19) 0.91449(13) 0.0420(7) Uani 1 1 d . . . H7E1 H 0.2966 0.1608 0.9263 0.091(2) Uiso 1 1 calc R . . H7E2 H 0.3978 0.0915 0.9102 0.091(2) Uiso 1 1 calc R . . H7E3 H 0.3817 0.1786 0.8819 0.091(2) Uiso 1 1 calc R . . C8E C 0.4401(2) 0.31694(17) 1.03150(11) 0.0321(6) Uani 1 1 d . . . H8E1 H 0.3600 0.3389 1.0341 0.051(2) Uiso 1 1 calc R . . H8E2 H 0.4676 0.3079 1.0659 0.051(2) Uiso 1 1 calc R . . C9E C 0.1552(3) 0.4002(2) 0.91197(15) 0.0535(9) Uani 1 1 d . . . H9E1 H 0.1389 0.4497 0.8885 0.091(2) Uiso 1 1 calc R . . H9E2 H 0.1189 0.4087 0.9453 0.091(2) Uiso 1 1 calc R . . H9E3 H 0.1292 0.3641 0.8986 0.091(2) Uiso 1 1 calc R . . C1F C 0.5912(2) 0.38035(17) 1.00236(11) 0.0307(6) Uani 1 1 d . . . H1F H 0.6306 0.3484 1.0306 0.038(3) Uiso 1 1 calc R . . C2F C 0.6374(2) 0.43189(16) 0.96887(11) 0.0293(6) Uani 1 1 d . . . C3F C 0.5760(2) 0.47855(16) 0.92690(11) 0.0310(6) Uani 1 1 d . . . C4F C 0.4726(2) 0.47700(17) 0.91706(11) 0.0310(6) Uani 1 1 d . . . C5F C 0.4323(2) 0.42353(16) 0.95201(11) 0.0291(6) Uani 1 1 d . . . C6F C 0.4882(2) 0.37496(16) 0.99507(11) 0.0287(6) Uani 1 1 d . . . C7F C 0.4058(3) 0.53060(18) 0.87277(12) 0.0408(7) Uani 1 1 d . . . H7F1 H 0.4157 0.5027 0.8442 0.091(2) Uiso 1 1 calc R . . H7F2 H 0.4304 0.5762 0.8620 0.091(2) Uiso 1 1 calc R . . H7F3 H 0.3288 0.5472 0.8838 0.091(2) Uiso 1 1 calc R . . C8F C 0.7509(2) 0.43527(18) 0.97706(11) 0.0328(6) Uani 1 1 d . . . H8F1 H 0.7647 0.4213 1.0138 0.051(2) Uiso 1 1 calc R . . H8F2 H 0.7534 0.4887 0.9652 0.051(2) Uiso 1 1 calc R . . C9F C 0.7079(3) 0.6065(2) 0.81381(14) 0.0537(9) Uani 1 1 d . . . H9F1 H 0.7627 0.5999 0.7856 0.091(2) Uiso 1 1 calc R . . H9F2 H 0.7251 0.6357 0.8368 0.091(2) Uiso 1 1 calc R . . H9F3 H 0.6362 0.6349 0.8004 0.091(2) Uiso 1 1 calc R . . C1G C 0.8911(2) 0.30141(18) 0.97132(11) 0.0321(6) Uani 1 1 d . . . H1G H 0.8716 0.2857 1.0059 0.038(3) Uiso 1 1 calc R . . C2G C 0.9700(2) 0.24685(18) 0.94536(11) 0.0328(6) Uani 1 1 d . . . C3G C 0.9963(2) 0.27205(19) 0.89357(11) 0.0338(7) Uani 1 1 d . . . C4G C 0.9491(2) 0.34833(19) 0.86741(11) 0.0339(7) Uani 1 1 d . . . C5G C 0.8711(2) 0.40009(18) 0.89619(11) 0.0323(6) Uani 1 1 d . . . C6G C 0.8400(2) 0.37890(17) 0.94757(11) 0.0308(6) Uani 1 1 d . . . C7G C 0.9838(3) 0.3754(2) 0.81151(12) 0.0479(8) Uani 1 1 d . . . H7G1 H 1.0377 0.3318 0.7983 0.072 Uiso 1 1 calc R . . H7G2 H 1.0154 0.4170 0.8103 0.072 Uiso 1 1 calc R . . H7G3 H 0.9201 0.3947 0.7907 0.072 Uiso 1 1 calc R . . C8G C 1.0210(2) 0.16271(19) 0.97305(12) 0.0380(7) Uani 1 1 d . . . H8G1 H 1.0975 0.1426 0.9605 0.051(2) Uiso 1 1 calc R . . H8G2 H 1.0203 0.1626 1.0100 0.051(2) Uiso 1 1 calc R . . C9G C 1.1843(3) 0.1235(3) 0.80281(14) 0.0595(11) Uani 1 1 d . . . H9G1 H 1.1907 0.0747 0.7919 0.091(2) Uiso 1 1 calc R . . H9G2 H 1.2472 0.1166 0.8222 0.091(2) Uiso 1 1 calc R . . H9G3 H 1.1815 0.1638 0.7729 0.091(2) Uiso 1 1 calc R . . C1H C 0.8690(2) 0.09909(17) 0.99748(11) 0.0351(7) Uani 1 1 d . . . H1H H 0.8503 0.1243 1.0263 0.038(3) Uiso 1 1 calc R . . C2H C 0.8078(2) 0.05252(17) 0.98904(11) 0.0344(7) Uani 1 1 d . . . C3H C 0.8388(3) 0.01505(17) 0.94571(12) 0.0359(7) Uani 1 1 d . . . C4H C 0.9284(2) 0.01972(17) 0.91165(12) 0.0367(7) Uani 1 1 d . . . C5H C 0.9840(2) 0.06960(18) 0.92141(12) 0.0362(7) Uani 1 1 d . . . C6H C 0.9581(2) 0.10952(17) 0.96397(11) 0.0344(7) Uani 1 1 d . . . C7H C 0.9683(3) -0.0287(2) 0.86905(13) 0.0478(8) Uani 1 1 d . . . H7H1 H 0.9653 0.0059 0.8362 0.091(2) Uiso 1 1 calc R . . H7H2 H 0.9220 -0.0610 0.8692 0.091(2) Uiso 1 1 calc R . . H7H3 H 1.0434 -0.0618 0.8745 0.091(2) Uiso 1 1 calc R . . C8H C 0.7106(3) 0.04444(18) 1.02482(11) 0.0381(7) Uani 1 1 d . . . H8H1 H 0.7243 0.0479 1.0597 0.051(2) Uiso 1 1 calc R . . H8H2 H 0.7029 -0.0072 1.0256 0.051(2) Uiso 1 1 calc R . . C9H C 0.6413(3) -0.0851(2) 0.89625(15) 0.0559(10) Uani 1 1 d . . . H9H1 H 0.5705 -0.0702 0.8814 0.091(2) Uiso 1 1 calc R . . H9H2 H 0.6425 -0.1220 0.9279 0.091(2) Uiso 1 1 calc R . . H9H3 H 0.6984 -0.1092 0.8722 0.091(2) Uiso 1 1 calc R . . O7W O 0.80057(18) 0.11746(14) 0.78489(9) 0.0479(6) Uani 1 1 d . . . O8W O 0.7370(3) 0.2872(2) 0.83950(16) 0.0959(11) Uani 1 1 d . . . O9W O 0.19340(18) 0.37041(14) 0.71447(9) 0.0450(5) Uani 1 1 d . . . O10W O 0.2586(2) 0.19918(19) 0.66708(19) 0.1109(15) Uani 1 1 d . . . O11W O 0.4610(2) 0.00785(16) 0.75837(10) 0.0623(7) Uani 1 1 d . . . O1S O 0.5497(2) 0.46742(13) 0.74638(9) 0.0517(6) Uani 1 1 d . . . C1S C 0.5800(4) 0.5672(2) 0.67936(15) 0.0610(10) Uani 1 1 d . . . C2S C 0.5093(3) 0.5481(2) 0.72460(13) 0.0484(8) Uani 1 1 d . . . H2S1 H 0.5075 0.5801 0.7505 0.051(2) Uiso 1 1 calc R . . H2S2 H 0.4343 0.5604 0.7141 0.051(2) Uiso 1 1 calc R . . F1S F 0.6841(2) 0.5548(2) 0.69257(12) 0.1002(9) Uani 1 1 d . . . F2S F 0.5874(3) 0.52589(17) 0.64233(9) 0.0914(9) Uani 1 1 d . . . F3S F 0.5393(3) 0.64374(15) 0.65785(10) 0.0985(9) Uani 1 1 d . . . O2S O 0.2405(4) 0.6810(3) 0.72260(17) 0.1273(15) Uani 1 1 d . . . C3S C 0.1558(5) 0.5859(4) 0.7565(3) 0.0989(17) Uiso 1 1 d . . . C4S C 0.1681(6) 0.6573(4) 0.7628(3) 0.128(2) Uani 1 1 d . . . H4S1 H 0.1981 0.6511 0.7963 0.051(2) Uiso 1 1 calc R . . H4S2 H 0.0963 0.6979 0.7619 0.051(2) Uiso 1 1 calc R . . F4S F 0.1039(7) 0.5465(4) 0.7947(3) 0.110(2) Uiso 0.50 1 d P . . F5S F 0.2638(6) 0.5247(4) 0.7543(3) 0.112(2) Uiso 0.50 1 d P . . F6S F 0.1245(6) 0.5884(4) 0.7090(3) 0.0981(19) Uiso 0.50 1 d P . . F5S' F 0.2144(8) 0.5274(8) 0.7856(6) 0.231(6) Uiso 0.50 1 d PD . . F4S' F 0.0540(7) 0.5788(5) 0.7711(4) 0.136(3) Uiso 0.50 1 d PD . . F6S' F 0.1892(9) 0.5524(6) 0.7164(4) 0.148(3) Uiso 0.50 1 d P . . 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 Zn1 0.0369(2) 0.03576(19) 0.03022(18) -0.00648(14) -0.00933(14) -0.01109(15) O1W 0.0423(13) 0.0781(17) 0.0405(13) -0.0236(12) -0.0053(10) -0.0229(12) O2W 0.0771(18) 0.0595(16) 0.0485(15) -0.0164(12) -0.0191(13) -0.0173(14) O3W 0.0381(12) 0.0476(13) 0.0423(13) -0.0067(10) -0.0058(10) -0.0135(10) O4W 0.0481(13) 0.0537(14) 0.0339(12) -0.0098(10) 0.0008(10) -0.0119(11) O5W 0.0666(16) 0.0433(13) 0.0510(14) 0.0018(11) -0.0264(12) -0.0211(12) O6W 0.0631(15) 0.0382(13) 0.0543(15) 0.0037(11) -0.0271(12) -0.0173(11) Zn2 0.0610(3) 0.0419(2) 0.02705(19) 0.00041(16) 0.00237(17) -0.00378(19) Cl1 0.0851(7) 0.0710(7) 0.0347(5) 0.0093(4) 0.0098(5) -0.0182(6) Cl2 0.0613(6) 0.0394(5) 0.0605(6) -0.0029(4) 0.0089(5) 0.0025(4) Cl3 0.0592(7) 0.1423(12) 0.0414(5) 0.0039(6) 0.0018(5) 0.0191(7) Cl4 0.1877(15) 0.0686(7) 0.0576(7) -0.0182(6) 0.0261(8) -0.0672(9) P1A 0.0230(3) 0.0346(4) 0.0300(4) -0.0076(3) 0.0018(3) -0.0084(3) O1A 0.0228(9) 0.0368(11) 0.0343(11) -0.0106(9) 0.0044(8) -0.0104(8) O2A 0.0251(10) 0.0336(11) 0.0367(11) -0.0049(9) 0.0004(8) -0.0060(8) O3A 0.0276(10) 0.0408(12) 0.0324(11) -0.0046(9) -0.0034(8) -0.0104(9) P1B 0.0335(4) 0.0268(4) 0.0302(4) -0.0030(3) -0.0028(3) -0.0106(3) O1B 0.0343(11) 0.0245(10) 0.0386(11) -0.0021(8) -0.0034(9) -0.0077(8) O2B 0.0372(11) 0.0252(10) 0.0343(11) -0.0041(8) 0.0005(9) -0.0126(8) O3B 0.0363(11) 0.0380(11) 0.0341(11) 0.0020(9) -0.0060(9) -0.0126(9) P1C 0.0237(3) 0.0332(4) 0.0352(4) -0.0089(3) -0.0021(3) -0.0104(3) O1C 0.0232(9) 0.0338(11) 0.0403(11) -0.0087(9) 0.0016(8) -0.0117(8) O2C 0.0210(9) 0.0345(11) 0.0383(11) -0.0111(9) 0.0005(8) -0.0093(8) O3C 0.0454(13) 0.0445(13) 0.0321(11) -0.0110(10) 0.0007(9) -0.0137(10) P1D 0.0306(4) 0.0306(4) 0.0312(4) -0.0009(3) 0.0015(3) -0.0091(3) O1D 0.0304(10) 0.0290(10) 0.0348(11) -0.0046(8) 0.0043(8) -0.0120(8) O2D 0.0298(10) 0.0294(10) 0.0350(11) -0.0041(8) 0.0027(8) -0.0127(8) O3D 0.0385(12) 0.0449(13) 0.0367(12) -0.0093(10) -0.0063(9) -0.0100(10) P1E 0.0274(4) 0.0395(4) 0.0345(4) -0.0114(3) -0.0026(3) -0.0109(3) O1E 0.0292(10) 0.0412(12) 0.0396(12) -0.0091(9) 0.0011(9) -0.0130(9) O2E 0.0236(10) 0.0384(11) 0.0364(11) -0.0126(9) -0.0004(8) -0.0063(8) O3E 0.0440(12) 0.0491(13) 0.0349(12) -0.0142(10) 0.0012(10) -0.0147(10) P1F 0.0408(4) 0.0343(4) 0.0335(4) 0.0011(3) -0.0082(3) -0.0174(3) O1F 0.0408(12) 0.0304(11) 0.0391(12) -0.0012(9) -0.0045(9) -0.0150(9) O2F 0.0388(12) 0.0406(12) 0.0352(11) -0.0006(9) -0.0060(9) -0.0201(10) O3F 0.0460(13) 0.0421(12) 0.0361(12) -0.0048(10) -0.0121(10) -0.0151(10) P1G 0.0250(4) 0.0574(5) 0.0354(4) -0.0146(4) -0.0003(3) -0.0047(4) O1G 0.0254(10) 0.0601(14) 0.0368(12) -0.0150(10) 0.0023(9) -0.0100(10) O2G 0.0271(11) 0.0510(13) 0.0390(12) -0.0125(10) -0.0044(9) 0.0006(9) O3G 0.0326(11) 0.0577(14) 0.0353(12) -0.0075(10) -0.0058(9) -0.0102(10) P1H 0.0454(5) 0.0304(4) 0.0314(4) -0.0050(3) -0.0022(3) -0.0145(3) O1H 0.0505(13) 0.0272(11) 0.0388(12) -0.0031(9) -0.0106(10) -0.0069(9) O2H 0.0482(13) 0.0325(11) 0.0368(11) -0.0076(9) 0.0030(10) -0.0185(10) O3H 0.0388(12) 0.0433(12) 0.0339(11) 0.0018(9) -0.0067(9) -0.0151(10) C1A 0.0254(13) 0.0370(15) 0.0240(13) -0.0050(11) -0.0028(11) -0.0137(12) C2A 0.0222(13) 0.0348(15) 0.0301(14) -0.0075(12) -0.0050(11) -0.0126(11) C3A 0.0197(13) 0.0339(15) 0.0302(14) -0.0105(12) 0.0014(10) -0.0113(11) C4A 0.0245(13) 0.0359(15) 0.0270(14) -0.0061(12) -0.0011(11) -0.0155(12) C5A 0.0213(13) 0.0303(14) 0.0335(15) -0.0053(12) -0.0016(11) -0.0113(11) C6A 0.0238(13) 0.0320(14) 0.0311(14) -0.0100(12) -0.0023(11) -0.0139(11) C7A 0.0393(17) 0.0393(17) 0.0333(16) -0.0034(13) 0.0029(13) -0.0126(14) C8A 0.0258(14) 0.0401(16) 0.0297(15) -0.0026(12) -0.0069(11) -0.0084(12) C9A 0.0352(17) 0.0466(19) 0.0450(18) -0.0166(15) 0.0139(14) -0.0142(14) C1B 0.0307(15) 0.0311(15) 0.0234(14) -0.0020(11) -0.0062(11) -0.0037(12) C2B 0.0289(14) 0.0273(14) 0.0285(14) 0.0021(11) -0.0070(11) -0.0053(11) C3B 0.0297(14) 0.0249(14) 0.0320(15) 0.0013(11) -0.0080(12) -0.0064(11) C4B 0.0279(14) 0.0267(14) 0.0316(15) -0.0002(12) -0.0064(12) -0.0003(11) C5B 0.0212(13) 0.0318(15) 0.0309(15) -0.0016(12) -0.0012(11) -0.0029(11) C6B 0.0232(13) 0.0295(14) 0.0315(15) 0.0017(12) -0.0081(11) -0.0040(11) C7B 0.0398(17) 0.0401(18) 0.0400(18) -0.0115(14) 0.0016(14) -0.0088(14) C8B 0.0331(15) 0.0327(15) 0.0240(14) 0.0019(11) -0.0036(11) -0.0087(12) C9B 0.0482(19) 0.0323(16) 0.053(2) -0.0142(15) 0.0012(16) -0.0157(14) C1C 0.0351(15) 0.0359(15) 0.0208(13) 0.0000(11) -0.0010(11) -0.0186(13) C2C 0.0295(14) 0.0302(14) 0.0229(13) -0.0040(11) 0.0049(11) -0.0143(12) C3C 0.0256(14) 0.0302(14) 0.0288(14) -0.0046(11) 0.0024(11) -0.0124(11) C4C 0.0300(14) 0.0318(15) 0.0308(15) -0.0043(12) 0.0002(11) -0.0161(12) C5C 0.0330(15) 0.0243(13) 0.0274(14) -0.0046(11) 0.0026(11) -0.0122(11) C6C 0.0315(14) 0.0303(14) 0.0227(13) 0.0042(11) -0.0007(11) -0.0127(12) C7C 0.0346(16) 0.0363(16) 0.0461(18) -0.0116(14) -0.0037(13) -0.0176(13) C8C 0.0327(15) 0.0356(15) 0.0262(14) -0.0102(12) 0.0051(11) -0.0161(12) C9C 0.0353(18) 0.051(2) 0.074(3) -0.0066(18) -0.0164(17) -0.0163(16) C1D 0.0279(14) 0.0294(14) 0.0272(14) -0.0100(11) -0.0001(11) -0.0079(11) C2D 0.0266(14) 0.0314(14) 0.0279(14) -0.0130(12) 0.0043(11) -0.0114(11) C3D 0.0249(13) 0.0241(13) 0.0344(15) -0.0090(11) 0.0054(11) -0.0088(11) C4D 0.0275(14) 0.0288(14) 0.0304(15) -0.0089(12) 0.0021(11) -0.0080(11) C5D 0.0224(13) 0.0297(14) 0.0331(15) -0.0127(12) 0.0025(11) -0.0104(11) C6D 0.0271(14) 0.0264(14) 0.0271(14) -0.0097(11) 0.0045(11) -0.0101(11) C7D 0.0314(15) 0.0400(17) 0.0379(17) -0.0016(13) -0.0055(13) -0.0099(13) C8D 0.0316(15) 0.0332(15) 0.0301(14) -0.0118(12) -0.0009(11) -0.0157(12) C9D 0.050(2) 0.0411(19) 0.057(2) 0.0154(16) 0.0067(17) -0.0100(16) C1E 0.0395(16) 0.0363(16) 0.0234(14) -0.0040(12) 0.0013(12) -0.0169(13) C2E 0.0357(15) 0.0346(15) 0.0232(14) -0.0051(12) 0.0055(11) -0.0153(13) C3E 0.0289(14) 0.0362(16) 0.0323(15) -0.0035(12) 0.0025(12) -0.0143(12) C4E 0.0368(16) 0.0380(16) 0.0332(16) -0.0056(13) 0.0016(12) -0.0208(13) C5E 0.0418(17) 0.0314(15) 0.0295(15) -0.0040(12) 0.0059(13) -0.0178(13) C6E 0.0410(17) 0.0323(15) 0.0243(14) 0.0009(12) 0.0019(12) -0.0144(13) C7E 0.0428(18) 0.0432(18) 0.0464(19) -0.0079(15) -0.0055(15) -0.0209(15) C8E 0.0314(15) 0.0392(16) 0.0265(14) -0.0087(12) 0.0014(11) -0.0113(13) C9E 0.0341(18) 0.063(2) 0.066(2) -0.0115(19) -0.0114(16) -0.0161(17) C1F 0.0337(15) 0.0318(15) 0.0264(14) -0.0111(12) -0.0019(12) -0.0063(12) C2F 0.0316(15) 0.0306(15) 0.0287(14) -0.0114(12) -0.0019(11) -0.0099(12) C3F 0.0343(15) 0.0271(14) 0.0342(15) -0.0090(12) -0.0003(12) -0.0115(12) C4F 0.0307(15) 0.0293(14) 0.0329(15) -0.0107(12) -0.0054(12) -0.0048(12) C5F 0.0267(14) 0.0310(15) 0.0310(15) -0.0138(12) -0.0006(11) -0.0063(11) C6F 0.0294(14) 0.0323(15) 0.0279(14) -0.0133(12) -0.0002(11) -0.0099(12) C7F 0.0414(18) 0.0377(17) 0.0415(18) -0.0001(14) -0.0116(14) -0.0108(14) C8F 0.0345(15) 0.0396(16) 0.0286(15) -0.0093(12) -0.0047(12) -0.0145(13) C9F 0.063(2) 0.044(2) 0.054(2) 0.0111(17) -0.0129(18) -0.0246(18) C1G 0.0300(15) 0.0449(17) 0.0233(14) -0.0060(12) -0.0052(11) -0.0128(13) C2G 0.0238(14) 0.0443(17) 0.0312(15) -0.0071(13) -0.0080(11) -0.0092(12) C3G 0.0219(14) 0.0505(18) 0.0329(16) -0.0134(14) -0.0003(11) -0.0133(13) C4G 0.0271(14) 0.0508(19) 0.0281(15) -0.0054(13) -0.0030(12) -0.0183(13) C5G 0.0283(14) 0.0405(17) 0.0323(15) -0.0033(13) -0.0071(12) -0.0162(13) C6G 0.0290(14) 0.0409(16) 0.0288(14) -0.0087(12) -0.0049(11) -0.0170(13) C7G 0.0459(19) 0.071(2) 0.0316(17) -0.0086(16) 0.0020(14) -0.0262(18) C8G 0.0286(15) 0.0482(18) 0.0327(16) -0.0085(14) -0.0085(12) -0.0028(13) C9G 0.0345(18) 0.091(3) 0.050(2) -0.032(2) 0.0117(16) -0.0094(19) C1H 0.0383(16) 0.0343(16) 0.0255(14) -0.0035(12) -0.0104(12) 0.0001(13) C2H 0.0381(16) 0.0268(14) 0.0306(15) 0.0007(12) -0.0114(13) 0.0000(12) C3H 0.0416(17) 0.0266(15) 0.0336(16) -0.0013(12) -0.0153(13) -0.0007(13) C4H 0.0350(16) 0.0323(16) 0.0323(16) -0.0032(13) -0.0115(13) 0.0052(13) C5H 0.0299(15) 0.0359(16) 0.0347(16) -0.0052(13) -0.0087(12) 0.0022(13) C6H 0.0316(15) 0.0355(16) 0.0285(15) -0.0030(12) -0.0103(12) 0.0012(12) C7H 0.0460(19) 0.0420(18) 0.0455(19) -0.0145(15) -0.0083(15) 0.0055(15) C8H 0.0529(19) 0.0327(16) 0.0253(15) 0.0015(12) -0.0054(13) -0.0116(14) C9H 0.077(3) 0.045(2) 0.057(2) -0.0225(18) 0.007(2) -0.0306(19) O7W 0.0358(12) 0.0630(15) 0.0408(13) -0.0007(11) -0.0064(10) -0.0131(11) O8W 0.064(2) 0.084(2) 0.148(3) -0.037(2) -0.021(2) -0.0199(17) O9W 0.0392(12) 0.0542(14) 0.0415(13) -0.0028(11) -0.0056(10) -0.0164(11) O10W 0.0375(15) 0.077(2) 0.240(5) -0.082(3) -0.017(2) -0.0134(15) O11W 0.0731(18) 0.0670(17) 0.0559(16) -0.0078(13) -0.0226(14) -0.0295(15) O1S 0.0646(16) 0.0421(13) 0.0519(14) -0.0005(11) -0.0246(12) -0.0189(12) C1S 0.081(3) 0.056(2) 0.046(2) -0.0036(18) -0.004(2) -0.024(2) C2S 0.053(2) 0.046(2) 0.0433(19) -0.0064(16) -0.0084(16) -0.0105(16) F1S 0.086(2) 0.133(3) 0.096(2) -0.0087(19) 0.0070(17) -0.0642(19) F2S 0.138(3) 0.095(2) 0.0445(13) -0.0289(13) 0.0079(15) -0.0358(18) F3S 0.162(3) 0.0619(16) 0.0641(16) 0.0128(13) -0.0035(17) -0.0396(18) O2S 0.159(4) 0.124(4) 0.105(3) -0.028(3) 0.028(3) -0.059(3) C4S 0.130(6) 0.126(6) 0.153(7) -0.067(5) 0.025(5) -0.061(5) _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 Zn1 O1W 2.050(2) . ? Zn1 O2W 2.093(2) . ? Zn1 O4W 2.093(2) . ? Zn1 O5W 2.103(2) . ? Zn1 O6W 2.112(2) . ? Zn1 O3W 2.130(2) . ? Zn2 Cl1 2.2400(10) . ? Zn2 Cl4 2.2453(13) . ? Zn2 Cl2 2.2724(10) . ? Zn2 Cl3 2.2944(12) . ? P1A O3A 1.473(2) . ? P1A O2A 1.594(2) . ? P1A O1A 1.596(2) . ? P1A C9A 1.772(3) . ? O1A C3A 1.413(3) . ? O2A C5B 1.415(3) . ? P1B O3B 1.466(2) . ? P1B O2B 1.593(2) . ? P1B O1B 1.598(2) . ? P1B C9B 1.765(3) . ? O1B C3B 1.421(3) . ? O2B C5C 1.409(3) . ? P1C O3C 1.471(2) . ? P1C O2C 1.580(2) . ? P1C O1C 1.598(2) . ? P1C C9C 1.754(3) . ? O1C C3C 1.412(3) . ? O2C C5D 1.416(3) . ? P1D O3D 1.469(2) . ? P1D O1D 1.584(2) . ? P1D O2D 1.590(2) . ? P1D C9D 1.754(3) . ? O1D C3D 1.418(3) . ? O2D C5A 1.416(3) . ? P1E O3E 1.466(2) . ? P1E O1E 1.587(2) . ? P1E O2E 1.587(2) . ? P1E C9E 1.759(3) . ? O1E C3E 1.421(3) . ? O2E C5F 1.414(3) . ? P1F O3F 1.477(2) . ? P1F O1F 1.582(2) . ? P1F O2F 1.586(2) . ? P1F C9F 1.757(3) . ? O1F C3F 1.421(3) . ? O2F C5G 1.417(3) . ? P1G O3G 1.474(2) . ? P1G O2G 1.599(2) . ? P1G O1G 1.600(2) . ? P1G C9G 1.765(3) . ? O1G C3G 1.405(3) . ? O2G C5H 1.408(4) . ? P1H O3H 1.467(2) . ? P1H O2H 1.590(2) . ? P1H O1H 1.593(2) . ? P1H C9H 1.775(3) . ? O1H C3H 1.420(4) . ? O2H C5E 1.412(3) . ? C1A C2A 1.376(4) . ? C1A C6A 1.397(4) . ? C1A H1A 0.9300 . ? C2A C3A 1.388(4) . ? C2A C8A 1.519(4) . ? C3A C4A 1.390(4) . ? C4A C5A 1.396(4) . ? C4A C7A 1.512(4) . ? C5A C6A 1.387(4) . ? C6A C8D 1.512(4) . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C8A C6B 1.505(4) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C1B C2B 1.387(4) . ? C1B C6B 1.395(4) . ? C1B H1B 0.9300 . ? C2B C3B 1.385(4) . ? C2B C8B 1.506(4) . ? C3B C4B 1.386(4) . ? C4B C5B 1.384(4) . ? C4B C7B 1.511(4) . ? C5B C6B 1.395(4) . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? C8B C6C 1.523(4) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C1C C2C 1.381(4) . ? C1C C6C 1.396(4) . ? C1C H1C 0.9300 . ? C2C C3C 1.395(4) . ? C2C C8C 1.518(4) . ? C3C C4C 1.401(4) . ? C4C C5C 1.390(4) . ? C4C C7C 1.512(4) . ? C5C C6C 1.386(4) . ? C7C H7C1 0.9600 . ? C7C H7C2 0.9600 . ? C7C H7C3 0.9600 . ? C8C C6D 1.516(4) . ? C8C H8C1 0.9700 . ? C8C H8C2 0.9700 . ? C9C H9C1 0.9600 . ? C9C H9C2 0.9600 . ? C9C H9C3 0.9600 . ? C1D C6D 1.386(4) . ? C1D C2D 1.388(4) . ? C1D H1D 0.9300 . ? C2D C3D 1.382(4) . ? C2D C8D 1.523(4) . ? C3D C4D 1.395(4) . ? C4D C5D 1.376(4) . ? C4D C7D 1.495(4) . ? C5D C6D 1.397(4) . ? C7D H7D1 0.9600 . ? C7D H7D2 0.9600 . ? C7D H7D3 0.9600 . ? C8D H8D1 0.9700 . ? C8D H8D2 0.9700 . ? C9D H9D1 0.9600 . ? C9D H9D2 0.9600 . ? C9D H9D3 0.9600 . ? C1E C6E 1.392(4) . ? C1E C2E 1.394(4) . ? C1E H1E 0.9300 . ? C2E C3E 1.385(4) . ? C2E C8E 1.519(4) . ? C3E C4E 1.390(4) . ? C4E C5E 1.391(4) . ? C4E C7E 1.516(4) . ? C5E C6E 1.395(4) . ? C6E C8H 1.515(4) . ? C7E H7E1 0.9600 . ? C7E H7E2 0.9600 . ? C7E H7E3 0.9600 . ? C8E C6F 1.519(4) . ? C8E H8E1 0.9700 . ? C8E H8E2 0.9700 . ? C9E H9E1 0.9600 . ? C9E H9E2 0.9600 . ? C9E H9E3 0.9600 . ? C1F C6F 1.389(4) . ? C1F C2F 1.388(4) . ? C1F H1F 0.9300 . ? C2F C3F 1.393(4) . ? C2F C8F 1.512(4) . ? C3F C4F 1.385(4) . ? C4F C5F 1.389(4) . ? C4F C7F 1.504(4) . ? C5F C6F 1.395(4) . ? C7F H7F1 0.9600 . ? C7F H7F2 0.9600 . ? C7F H7F3 0.9600 . ? C8F C6G 1.515(4) . ? C8F H8F1 0.9700 . ? C8F H8F2 0.9700 . ? C9F H9F1 0.9600 . ? C9F H9F2 0.9600 . ? C9F H9F3 0.9600 . ? C1G C2G 1.386(4) . ? C1G C6G 1.394(4) . ? C1G H1G 0.9300 . ? C2G C3G 1.391(4) . ? C2G C8G 1.519(4) . ? C3G C4G 1.389(4) . ? C4G C5G 1.396(4) . ? C4G C7G 1.522(4) . ? C5G C6G 1.382(4) . ? C7G H7G1 0.9600 . ? C7G H7G2 0.9600 . ? C7G H7G3 0.9600 . ? C8G C6H 1.508(4) . ? C8G H8G1 0.9700 . ? C8G H8G2 0.9700 . ? C9G H9G1 0.9600 . ? C9G H9G2 0.9600 . ? C9G H9G3 0.9600 . ? C1H C2H 1.386(4) . ? C1H C6H 1.402(4) . ? C1H H1H 0.9300 . ? C2H C3H 1.394(4) . ? C2H C8H 1.503(4) . ? C3H C4H 1.389(4) . ? C4H C5H 1.394(4) . ? C4H C7H 1.499(4) . ? C5H C6H 1.401(4) . ? C7H H7H1 0.9600 . ? C7H H7H2 0.9600 . ? C7H H7H3 0.9600 . ? C8H H8H1 0.9700 . ? C8H H8H2 0.9700 . ? C9H H9H1 0.9600 . ? C9H H9H2 0.9600 . ? C9H H9H3 0.9600 . ? O1S C2S 1.407(4) . ? C1S F2S 1.317(4) . ? C1S F3S 1.344(5) . ? C1S F1S 1.348(5) . ? C1S C2S 1.470(5) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? O2S C4S 1.424(7) . ? C3S F6S' 1.283(10) . ? C3S F5S' 1.250(12) . ? C3S F6S 1.340(9) . ? C3S F4S 1.358(8) . ? C3S F4S' 1.356(9) . ? C3S C4S 1.399(8) . ? C3S F5S 1.465(10) . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? F4S F4S' 0.914(9) . ? F4S F5S' 1.345(10) . ? F5S F5S' 0.980(14) . ? F5S F6S' 1.360(11) . ? F6S F6S' 0.884(10) . ? F6S F4S' 1.781(10) . ? 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 O1W Zn1 O2W 178.40(10) . . ? O1W Zn1 O4W 93.25(9) . . ? O2W Zn1 O4W 87.82(10) . . ? O1W Zn1 O5W 92.70(10) . . ? O2W Zn1 O5W 88.48(10) . . ? O4W Zn1 O5W 90.45(10) . . ? O1W Zn1 O6W 87.01(10) . . ? O2W Zn1 O6W 91.78(10) . . ? O4W Zn1 O6W 91.56(10) . . ? O5W Zn1 O6W 177.98(10) . . ? O1W Zn1 O3W 88.87(9) . . ? O2W Zn1 O3W 90.04(10) . . ? O4W Zn1 O3W 177.70(8) . . ? O5W Zn1 O3W 90.34(9) . . ? O6W Zn1 O3W 87.66(9) . . ? Cl1 Zn2 Cl4 111.69(5) . . ? Cl1 Zn2 Cl2 110.31(4) . . ? Cl4 Zn2 Cl2 108.58(5) . . ? Cl1 Zn2 Cl3 107.40(5) . . ? Cl4 Zn2 Cl3 110.60(6) . . ? Cl2 Zn2 Cl3 108.21(4) . . ? O3A P1A O2A 112.84(11) . . ? O3A P1A O1A 112.28(11) . . ? O2A P1A O1A 106.43(11) . . ? O3A P1A C9A 118.72(14) . . ? O2A P1A C9A 102.90(14) . . ? O1A P1A C9A 102.39(13) . . ? C3A O1A P1A 122.46(16) . . ? C5B O2A P1A 120.71(17) . . ? O3B P1B O2B 113.66(12) . . ? O3B P1B O1B 113.30(11) . . ? O2B P1B O1B 106.82(11) . . ? O3B P1B C9B 118.95(15) . . ? O2B P1B C9B 101.10(13) . . ? O1B P1B C9B 101.40(14) . . ? C3B O1B P1B 122.94(17) . . ? C5C O2B P1B 124.48(17) . . ? O3C P1C O2C 114.08(12) . . ? O3C P1C O1C 113.00(12) . . ? O2C P1C O1C 106.29(11) . . ? O3C P1C C9C 116.53(16) . . ? O2C P1C C9C 102.39(14) . . ? O1C P1C C9C 103.27(15) . . ? C3C O1C P1C 121.76(16) . . ? C5D O2C P1C 123.19(16) . . ? O3D P1D O1D 113.02(12) . . ? O3D P1D O2D 112.45(11) . . ? O1D P1D O2D 106.10(11) . . ? O3D P1D C9D 119.12(17) . . ? O1D P1D C9D 101.46(14) . . ? O2D P1D C9D 103.26(15) . . ? C3D O1D P1D 122.33(17) . . ? C5A O2D P1D 121.34(16) . . ? O3E P1E O1E 113.19(12) . . ? O3E P1E O2E 113.92(12) . . ? O1E P1E O2E 106.67(11) . . ? O3E P1E C9E 117.43(16) . . ? O1E P1E C9E 102.24(15) . . ? O2E P1E C9E 101.96(15) . . ? C3E O1E P1E 122.97(17) . . ? C5F O2E P1E 123.36(17) . . ? O3F P1F O1F 113.36(12) . . ? O3F P1F O2F 111.68(12) . . ? O1F P1F O2F 107.44(11) . . ? O3F P1F C9F 118.37(16) . . ? O1F P1F C9F 102.68(16) . . ? O2F P1F C9F 102.11(15) . . ? C3F O1F P1F 122.70(18) . . ? C5G O2F P1F 122.72(17) . . ? O3G P1G O2G 112.55(13) . . ? O3G P1G O1G 112.70(13) . . ? O2G P1G O1G 106.60(12) . . ? O3G P1G C9G 118.46(16) . . ? O2G P1G C9G 103.71(17) . . ? O1G P1G C9G 101.54(16) . . ? C3G O1G P1G 122.78(18) . . ? C5H O2G P1G 121.12(18) . . ? O3H P1H O2H 113.37(12) . . ? O3H P1H O1H 112.90(12) . . ? O2H P1H O1H 107.33(12) . . ? O3H P1H C9H 117.26(16) . . ? O2H P1H C9H 101.78(15) . . ? O1H P1H C9H 102.98(16) . . ? C3H O1H P1H 121.07(17) . . ? C5E O2H P1H 124.67(18) . . ? C2A C1A C6A 122.4(3) . . ? C2A C1A H1A 118.8 . . ? C6A C1A H1A 118.8 . . ? C1A C2A C3A 117.7(3) . . ? C1A C2A C8A 120.2(2) . . ? C3A C2A C8A 122.0(2) . . ? C2A C3A C4A 123.5(2) . . ? C2A C3A O1A 118.7(2) . . ? C4A C3A O1A 117.4(2) . . ? C3A C4A C5A 115.8(2) . . ? C3A C4A C7A 121.5(2) . . ? C5A C4A C7A 122.7(3) . . ? C6A C5A C4A 123.5(3) . . ? C6A C5A O2D 118.5(2) . . ? C4A C5A O2D 117.8(2) . . ? C5A C6A C1A 117.0(2) . . ? C5A C6A C8D 122.9(3) . . ? C1A C6A C8D 119.9(2) . . ? C4A C7A H7A1 109.5 . . ? C4A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C4A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C6B C8A C2A 111.3(2) . . ? C6B C8A H8A1 109.4 . . ? C2A C8A H8A1 109.4 . . ? C6B C8A H8A2 109.4 . . ? C2A C8A H8A2 109.4 . . ? H8A1 C8A H8A2 108.0 . . ? P1A C9A H9A1 109.5 . . ? P1A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? P1A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C2B C1B C6B 122.4(3) . . ? C2B C1B H1B 118.8 . . ? C6B C1B H1B 118.8 . . ? C3B C2B C1B 117.2(3) . . ? C3B C2B C8B 122.1(3) . . ? C1B C2B C8B 120.7(3) . . ? C2B C3B C4B 123.8(3) . . ? C2B C3B O1B 118.1(2) . . ? C4B C3B O1B 117.9(3) . . ? C5B C4B C3B 116.1(3) . . ? C5B C4B C7B 121.8(3) . . ? C3B C4B C7B 122.0(3) . . ? C4B C5B C6B 123.7(3) . . ? C4B C5B O2A 118.4(2) . . ? C6B C5B O2A 117.9(2) . . ? C1B C6B C5B 116.7(3) . . ? C1B C6B C8A 120.6(3) . . ? C5B C6B C8A 122.6(3) . . ? C4B C7B H7B1 109.5 . . ? C4B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C4B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C2B C8B C6C 111.1(2) . . ? C2B C8B H8B1 109.4 . . ? C6C C8B H8B1 109.4 . . ? C2B C8B H8B2 109.4 . . ? C6C C8B H8B2 109.4 . . ? H8B1 C8B H8B2 108.0 . . ? P1B C9B H9B1 109.5 . . ? P1B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? P1B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C2C C1C C6C 122.0(3) . . ? C2C C1C H1C 119.0 . . ? C6C C1C H1C 119.0 . . ? C1C C2C C3C 117.7(3) . . ? C1C C2C C8C 119.9(2) . . ? C3C C2C C8C 122.3(2) . . ? C2C C3C C4C 123.0(3) . . ? C2C C3C O1C 119.4(2) . . ? C4C C3C O1C 117.4(2) . . ? C5C C4C C3C 116.2(2) . . ? C5C C4C C7C 122.4(3) . . ? C3C C4C C7C 121.4(3) . . ? C6C C5C C4C 123.2(3) . . ? C6C C5C O2B 118.3(2) . . ? C4C C5C O2B 118.3(2) . . ? C5C C6C C1C 117.8(3) . . ? C5C C6C C8B 121.8(3) . . ? C1C C6C C8B 120.3(2) . . ? C4C C7C H7C1 109.5 . . ? C4C C7C H7C2 109.5 . . ? H7C1 C7C H7C2 109.5 . . ? C4C C7C H7C3 109.5 . . ? H7C1 C7C H7C3 109.5 . . ? H7C2 C7C H7C3 109.5 . . ? C6D C8C C2C 110.5(2) . . ? C6D C8C H8C1 109.6 . . ? C2C C8C H8C1 109.6 . . ? C6D C8C H8C2 109.6 . . ? C2C C8C H8C2 109.6 . . ? H8C1 C8C H8C2 108.1 . . ? P1C C9C H9C1 109.5 . . ? P1C C9C H9C2 109.5 . . ? H9C1 C9C H9C2 109.5 . . ? P1C C9C H9C3 109.5 . . ? H9C1 C9C H9C3 109.5 . . ? H9C2 C9C H9C3 109.5 . . ? C6D C1D C2D 122.4(3) . . ? C6D C1D H1D 118.8 . . ? C2D C1D H1D 118.8 . . ? C3D C2D C1D 117.2(2) . . ? C3D C2D C8D 121.2(2) . . ? C1D C2D C8D 121.6(3) . . ? C2D C3D C4D 124.1(3) . . ? C2D C3D O1D 118.2(2) . . ? C4D C3D O1D 117.5(2) . . ? C5D C4D C3D 115.1(3) . . ? C5D C4D C7D 122.5(3) . . ? C3D C4D C7D 122.4(3) . . ? C4D C5D C6D 124.7(2) . . ? C4D C5D O2C 117.3(2) . . ? C6D C5D O2C 117.8(2) . . ? C1D C6D C5D 116.5(2) . . ? C1D C6D C8C 121.9(3) . . ? C5D C6D C8C 121.5(2) . . ? C4D C7D H7D1 109.5 . . ? C4D C7D H7D2 109.5 . . ? H7D1 C7D H7D2 109.5 . . ? C4D C7D H7D3 109.5 . . ? H7D1 C7D H7D3 109.5 . . ? H7D2 C7D H7D3 109.5 . . ? C6A C8D C2D 110.2(2) . . ? C6A C8D H8D1 109.6 . . ? C2D C8D H8D1 109.6 . . ? C6A C8D H8D2 109.6 . . ? C2D C8D H8D2 109.6 . . ? H8D1 C8D H8D2 108.1 . . ? P1D C9D H9D1 109.5 . . ? P1D C9D H9D2 109.5 . . ? H9D1 C9D H9D2 109.5 . . ? P1D C9D H9D3 109.5 . . ? H9D1 C9D H9D3 109.5 . . ? H9D2 C9D H9D3 109.5 . . ? C6E C1E C2E 122.0(3) . . ? C6E C1E H1E 119.0 . . ? C2E C1E H1E 119.0 . . ? C3E C2E C1E 117.2(3) . . ? C3E C2E C8E 122.4(3) . . ? C1E C2E C8E 120.3(3) . . ? C2E C3E C4E 124.0(3) . . ? C2E C3E O1E 118.4(3) . . ? C4E C3E O1E 117.4(3) . . ? C3E C4E C5E 116.0(3) . . ? C3E C4E C7E 122.0(3) . . ? C5E C4E C7E 122.0(3) . . ? C4E C5E C6E 123.2(3) . . ? C4E C5E O2H 118.1(3) . . ? C6E C5E O2H 118.5(3) . . ? C1E C6E C5E 117.6(3) . . ? C1E C6E C8H 120.4(3) . . ? C5E C6E C8H 121.9(3) . . ? C4E C7E H7E1 109.5 . . ? C4E C7E H7E2 109.5 . . ? H7E1 C7E H7E2 109.5 . . ? C4E C7E H7E3 109.5 . . ? H7E1 C7E H7E3 109.5 . . ? H7E2 C7E H7E3 109.5 . . ? C6F C8E C2E 110.1(2) . . ? C6F C8E H8E1 109.6 . . ? C2E C8E H8E1 109.6 . . ? C6F C8E H8E2 109.6 . . ? C2E C8E H8E2 109.6 . . ? H8E1 C8E H8E2 108.2 . . ? P1E C9E H9E1 109.5 . . ? P1E C9E H9E2 109.5 . . ? H9E1 C9E H9E2 109.5 . . ? P1E C9E H9E3 109.5 . . ? H9E1 C9E H9E3 109.5 . . ? H9E2 C9E H9E3 109.5 . . ? C6F C1F C2F 122.2(3) . . ? C6F C1F H1F 118.9 . . ? C2F C1F H1F 118.9 . . ? C1F C2F C3F 117.1(3) . . ? C1F C2F C8F 121.1(3) . . ? C3F C2F C8F 121.7(3) . . ? C4F C3F C2F 124.2(3) . . ? C4F C3F O1F 117.8(3) . . ? C2F C3F O1F 117.9(2) . . ? C3F C4F C5F 115.3(3) . . ? C3F C4F C7F 123.1(3) . . ? C5F C4F C7F 121.6(3) . . ? C4F C5F C6F 124.1(3) . . ? C4F C5F O2E 117.6(2) . . ? C6F C5F O2E 118.1(2) . . ? C1F C6F C5F 117.1(3) . . ? C1F C6F C8E 121.4(3) . . ? C5F C6F C8E 121.5(2) . . ? C4F C7F H7F1 109.5 . . ? C4F C7F H7F2 109.5 . . ? H7F1 C7F H7F2 109.5 . . ? C4F C7F H7F3 109.5 . . ? H7F1 C7F H7F3 109.5 . . ? H7F2 C7F H7F3 109.5 . . ? C2F C8F C6G 110.7(2) . . ? C2F C8F H8F1 109.5 . . ? C6G C8F H8F1 109.5 . . ? C2F C8F H8F2 109.5 . . ? C6G C8F H8F2 109.5 . . ? H8F1 C8F H8F2 108.1 . . ? P1F C9F H9F1 109.5 . . ? P1F C9F H9F2 109.5 . . ? H9F1 C9F H9F2 109.5 . . ? P1F C9F H9F3 109.5 . . ? H9F1 C9F H9F3 109.5 . . ? H9F2 C9F H9F3 109.5 . . ? C2G C1G C6G 122.5(3) . . ? C2G C1G H1G 118.8 . . ? C6G C1G H1G 118.8 . . ? C1G C2G C3G 117.3(3) . . ? C1G C2G C8G 120.0(3) . . ? C3G C2G C8G 122.7(3) . . ? C4G C3G C2G 123.5(3) . . ? C4G C3G O1G 117.5(3) . . ? C2G C3G O1G 118.9(3) . . ? C3G C4G C5G 116.0(3) . . ? C3G C4G C7G 122.3(3) . . ? C5G C4G C7G 121.6(3) . . ? C6G C5G C4G 123.7(3) . . ? C6G C5G O2F 118.6(3) . . ? C4G C5G O2F 117.6(3) . . ? C5G C6G C1G 117.1(3) . . ? C5G C6G C8F 122.5(3) . . ? C1G C6G C8F 120.4(3) . . ? C4G C7G H7G1 109.5 . . ? C4G C7G H7G2 109.5 . . ? H7G1 C7G H7G2 109.5 . . ? C4G C7G H7G3 109.5 . . ? H7G1 C7G H7G3 109.5 . . ? H7G2 C7G H7G3 109.5 . . ? C6H C8G C2G 111.1(2) . . ? C6H C8G H8G1 109.4 . . ? C2G C8G H8G1 109.4 . . ? C6H C8G H8G2 109.4 . . ? C2G C8G H8G2 109.4 . . ? H8G1 C8G H8G2 108.0 . . ? P1G C9G H9G1 109.5 . . ? P1G C9G H9G2 109.5 . . ? H9G1 C9G H9G2 109.5 . . ? P1G C9G H9G3 109.5 . . ? H9G1 C9G H9G3 109.5 . . ? H9G2 C9G H9G3 109.5 . . ? C2H C1H C6H 122.2(3) . . ? C2H C1H H1H 118.9 . . ? C6H C1H H1H 118.9 . . ? C1H C2H C3H 117.3(3) . . ? C1H C2H C8H 120.9(3) . . ? C3H C2H C8H 121.8(3) . . ? C4H C3H C2H 124.3(3) . . ? C4H C3H O1H 117.5(3) . . ? C2H C3H O1H 118.1(3) . . ? C3H C4H C5H 115.4(3) . . ? C3H C4H C7H 123.2(3) . . ? C5H C4H C7H 121.3(3) . . ? C4H C5H C6H 123.9(3) . . ? C4H C5H O2G 118.2(3) . . ? C6H C5H O2G 117.9(3) . . ? C5H C6H C1H 116.8(3) . . ? C5H C6H C8G 122.0(3) . . ? C1H C6H C8G 121.2(3) . . ? C4H C7H H7H1 109.5 . . ? C4H C7H H7H2 109.5 . . ? H7H1 C7H H7H2 109.5 . . ? C4H C7H H7H3 109.5 . . ? H7H1 C7H H7H3 109.5 . . ? H7H2 C7H H7H3 109.5 . . ? C2H C8H C6E 111.8(2) . . ? C2H C8H H8H1 109.3 . . ? C6E C8H H8H1 109.3 . . ? C2H C8H H8H2 109.3 . . ? C6E C8H H8H2 109.3 . . ? H8H1 C8H H8H2 107.9 . . ? P1H C9H H9H1 109.5 . . ? P1H C9H H9H2 109.5 . . ? H9H1 C9H H9H2 109.5 . . ? P1H C9H H9H3 109.5 . . ? H9H1 C9H H9H3 109.5 . . ? H9H2 C9H H9H3 109.5 . . ? F2S C1S F3S 106.4(3) . . ? F2S C1S F1S 107.1(4) . . ? F3S C1S F1S 107.4(4) . . ? F2S C1S C2S 113.4(4) . . ? F3S C1S C2S 110.4(4) . . ? F1S C1S C2S 111.7(3) . . ? O1S C2S C1S 110.7(3) . . ? O1S C2S H2S1 109.5 . . ? C1S C2S H2S1 109.5 . . ? O1S C2S H2S2 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 108.1 . . ? F6S' C3S F5S' 92.2(9) . . ? F6S' C3S F6S 39.3(5) . . ? F5S' C3S F6S 127.6(9) . . ? F6S' C3S F4S 114.5(7) . . ? F5S' C3S F4S 61.9(6) . . ? F6S C3S F4S 112.8(6) . . ? F6S' C3S F4S' 106.4(8) . . ? F5S' C3S F4S' 100.2(7) . . ? F6S C3S F4S' 82.7(6) . . ? F4S C3S F4S' 39.4(4) . . ? F6S' C3S C4S 125.5(7) . . ? F5S' C3S C4S 113.0(9) . . ? F6S C3S C4S 112.6(6) . . ? F4S C3S C4S 120.0(6) . . ? F4S' C3S C4S 114.7(7) . . ? F6S' C3S F5S 58.9(6) . . ? F5S' C3S F5S 41.4(7) . . ? F6S C3S F5S 98.2(6) . . ? F4S C3S F5S 99.1(6) . . ? F4S' C3S F5S 129.9(7) . . ? C4S C3S F5S 110.9(6) . . ? C3S C4S O2S 110.2(6) . . ? C3S C4S H4S1 109.6 . . ? O2S C4S H4S1 109.6 . . ? C3S C4S H4S2 109.6 . . ? O2S C4S H4S2 109.6 . . ? H4S1 C4S H4S2 108.1 . . ? F4S' F4S F5S' 123.5(10) . . ? F4S' F4S C3S 70.2(7) . . ? F5S' F4S C3S 55.1(6) . . ? F5S' F5S F6S' 101.2(10) . . ? F5S' F5S C3S 57.4(8) . . ? F6S' F5S C3S 53.8(5) . . ? F6S' F6S C3S 66.8(8) . . ? F6S' F6S F4S' 99.3(9) . . ? C3S F6S F4S' 49.0(4) . . ? F5S F5S' F4S 134.5(13) . . ? F5S F5S' C3S 81.2(12) . . ? F4S F5S' C3S 63.0(5) . . ? F4S F4S' C3S 70.4(7) . . ? F4S F4S' F6S 108.6(8) . . ? C3S F4S' F6S 48.3(4) . . ? F6S F6S' C3S 73.9(9) . . ? F6S F6S' F5S 141.0(12) . . ? C3S F6S' F5S 67.3(7) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.833 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.080